CN114367246B

CN114367246B - Continuous melting and multiphase separation system

Info

Publication number: CN114367246B
Application number: CN202210036704.9A
Authority: CN
Inventors: 沈齐晖; 赵雅晶; 沈立嵩
Original assignee: Individual
Current assignee: Individual
Priority date: 2022-01-13
Filing date: 2022-01-13
Publication date: 2024-07-16
Anticipated expiration: 2042-01-13
Also published as: CN114367246A

Abstract

A system and method for continuous melting and multiphase separation includes a heating unit, a heat exchanger bank, a multiphase separation tank, a liquid level holding mechanism, and a control system. The system is particularly suitable for separating liquid phase media which can be layered after melting, and is preferably suitable for purifying technology of aqueous sulfur particles in petrochemical industry, natural gas and metallurgical industry and related application of recovering solvent from sulfur solution.

Description

Continuous melting and multiphase separation system

Technical Field

The invention relates to a continuous melting and multiphase separation system and method, which are particularly suitable for separating layered liquid phase medium after melting, are preferably suitable for purification technology of aqueous sulfur particles in petrochemical industry, natural gas and metallurgical industry, and are applied to the field of energy conservation and environmental protection in the related recovery of solvent from sulfur solution.

Background

The aqueous sulfur particles are a mixture mainly comprising sulfur particles and a desulfurizing liquid (ammonia water solution or sodium carbonate solution, containing a minor amount of a wet oxidation catalyst), and may be mixed with a small amount of hydrocarbons or tar due to the difference in conditions at the ends of the sulfur particles.

When wet catalytic oxidation is adopted to purify H ₂ S in gas in industries such as petrifaction, steel, coking and the like, H ₂ S is converted into fine sulfur particles and separated from desulfurization liquid; the separated sulphur particles are mixed with a desulphurisation liquid and possibly with small amounts of hydrocarbons or tar, and industry practice calls such materials as: sulfur foam.

Typical compositions and individual component characteristics of sulfur foams are shown in table 1:

TABLE 1 typical composition and individual component characteristics of Sulfur foam

The prior art is that sulfur foam is heated in a melting kettle, and the implementation process of sulfur melting is as follows: charging sulfur foam, heating, separating clear liquid, heating again, converting sulfur crystal forms, continuously heating, melting sulfur particles into liquid sulfur, discharging the liquid sulfur, and discharging sulfur slag and oil.

The current intermittent sulfur melting technology is characterized in that each step in the sulfur melting implementation process is operated in batches in sequence, the steps cannot be parallel at the same time, and the heat supply amount and the heating time are required to be adjusted according to the temperature requirements of different steps.

The current continuous sulfur melting technology is characterized in that: the steps of simultaneously carrying out the "liquid sulfur removal", "sulfur slag removal and oil removal" in the sulfur melting process are batch-wise operations in sequence, so that the operating conditions of the "separated clear liquid" are destroyed at the time of the "liquid sulfur removal" and the "sulfur slag removal and oil removal", so that the "separated clear liquid" cannot be continuously carried out. Essentially, the current continuous sulfur melting technology realizes: 1) Continuous "sulfur foam charge"; 2) When the operations of 'discharging liquid sulfur' and 'discharging sulfur slag and oil' are not performed, the continuous 'heating, clear liquid separation, re-heating, sulfur crystal form transformation, continuous heating and sulfur particle melting into liquid sulfur' can be performed; 3) When the operations of 'discharging liquid sulfur' and 'discharging sulfur slag and oil' are carried out, the clear liquid cannot be separated in an equivalent amount; to prevent the drainage difficulties caused by the increase in viscosity of the liquid sulfur, it is also desirable to reduce or even stop the sulfur foam charge.

The prior sulfur melting technology adopts a jacketed kettle to melt sulfur particles into liquid sulfur. 1) Because the temperature gradient exists between the heating surface in the kettle and the center of the kettle, under the condition of no mechanical stirring, sulfur particles in the center area of the kettle cannot be reliably and completely melted, the discharged liquid sulfur is mixed with sulfur particles to be a multiple phenomenon, and the heating time is prolonged or the heating intensity is improved after the state of the discharged liquid sulfur is observed manually; 2) Because the density of the hydrocarbon or tar is lower than that of the liquid sulfur, the hydrocarbon or tar can be discharged out of the melting kettle only after the liquid sulfur is discharged; 3) Because of batch operation of the melting kettle, manual direct observation of liquid sulfur medium and the like, the field operation intensity is high and the operation environment is poor; 4) The temperature of the discharged gas and clear liquid is high due to the high operation pressure of the melting kettle; in addition, the equipment temperature reduction-heating process caused by batch operation of charging and discharging generates larger heating consumption and corresponding cooling consumption; as described in the related data, the minimum sulfur melting consumption is about 200Kg of steam/t of liquid sulfur.

At present, for the sulfur melting technology of sulfur foam generated in the wet catalytic oxidation method, a melting kettle is operated under the pressure of more than 0.2MPa (g); the heating strength of the sulfur-melted portion is low; the degree of automation is low; continuous operation is unstable.

To date, no continuous sulfur melting and multiphase separation technology for water-containing sulfur particles has the advantages of stable and continuous operation, low manual operation strength, high operation efficiency and environmental friendliness.

Disclosure of Invention

In view of this, the present invention aims to provide a continuous melting and multiphase separation system and method for continuously dewatering, degreasing and melting sulfur particles containing water, which addresses the above-mentioned deficiencies in the treatment of sulfur particles containing water. According to the system and method of the present invention, the liquid-meltable solid mixture can be continuously melted and separated in multiple phases, for example, the aqueous sulfur particles are continuously melted and separated in multiple phases to obtain non-condensable gases and solvent vapors, clear liquid (sulfur content <1 g/L), tar and liquid sulfur. Has the outstanding advantages of improving the color of liquid sulfur, stable and continuous operation, environmental protection, low manual operation strength and high operation efficiency, and greatly improves the technical level of disposal of the water-containing sulfur particles.

In one aspect, the present invention relates to a continuous melting and multiphase separation system comprising:

a heating unit for releasing energy from the heating medium to continuously provide driving force required for heating, evaporating and melting the liquid-meltable solid mixed material;

a heat exchanger set for heating a liquid-soluble solid mixture, the heat exchanger set comprising a melting heater 5 for heating a fusible solid;

A multiphase separation tank for standing and layering the continuously added liquid-meltable solid mixture; the multiphase separation tank comprises a multiphase separation tank 7, the multiphase separation tank 7 is connected with a melting heater 5 in the heat exchanger group in the vertical direction to form a melting-separation kettle body, and the melting-separation kettle body can completely melt soluble solid particles without mechanical stirring; and discharging the phase products from the system; the respective phase products include gas phase products and liquid phase products (e.g., liquid phase product YI, liquid phase product YII, and liquid phase product YIII);

A liquid level maintaining mechanism including a discharge system for each liquid phase product for stably discharging each liquid phase product continuously in equal amounts to the feed without providing an adjusting mechanism; and a control system for regulating the temperature of the liquid-meltable solid mixture and the respective phase products, the pressure and the level in the melt-separation tank during operation of the system.

In another aspect, the present invention also relates to a method for continuous fusion and multiphase separation using the above system, the method comprising:

S1, after the continuously added liquid-meltable solid mixed material exchanges heat with a heating medium which is used for heating, evaporating and melting the continuously added liquid-meltable solid mixed material, meltable solid particles are completely melted under the condition of no mechanical stirring;

S2, standing and layering the molten liquid-meltable solid mixture in a multiphase separation tank 7 to form products of each phase; the respective phase products include a gas phase product and a liquid phase product (liquid phase product YI, liquid phase product YII, and liquid phase product YIII);

s3, continuously discharging each liquid-phase product through the liquid level maintaining mechanism and keeping the liquid layer thickness of each layered product in the multiphase separation tank 7 unchanged;

S4, maintaining the operation pressure to be 0.01-0.8 MPa through a control system, and discharging a gas-phase product;

S5, continuously discharging a liquid phase product YI with the minimum density, a liquid phase product YII with the intermediate density and a liquid phase product YII from top to bottom along the height direction through the liquid level maintaining mechanism;

S6, regulating the temperature T2 in the multiphase separation tank 7 to be stably kept in a certain range lower than T1 through the control system; adjusting the outlet temperature T1 of said liquid phase product YIII to remain steadily above between the melting point and the boiling point of the meltable solid medium;

And S7, depositing solid slag with the density greater than that of the liquid phase product YIII at the bottom, gradually accumulating and intermittently discharging.

In another aspect, the present invention also relates to the use of the continuous melting and multiphase separation system described above in continuous melting and multiphase separation techniques for aqueous sulfur particles.

In another aspect, the present invention also relates to a continuous melting and multiphase separation system for aqueous sulfur particles, the system comprising: a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system,

The heating medium in the heating unit comprises a heating medium with a temperature higher than the melting point of the fusible solid, such as: steam F or heat transfer oil F'; the heat exchanger group provides heat for heating, evaporating and melting the sulfur foam raw material A;

The heat exchanger group includes a fusion heater 5, and a conduction oil heater 4 'when using conduction oil F';

The multiphase separation tank comprises a multiphase separation tank 7 which is vertically and coaxially connected with the heat exchanger group to form a melting-separation kettle, and simultaneously, the continuously added sulfur foam raw material A is stably discharged through the liquid level maintaining mechanism, and each phase of products comprises a gas phase product and a liquid phase product (such as a liquid phase product YI, a liquid phase product YII and a liquid phase product YIII);

The liquid level maintaining mechanism is a discharge pipe system, such as a discharge port I, a discharge port II and a discharge port III, which is arranged on the melting-separating kettle according to the height difference of the bottom of each liquid medium discharge pipe determined by the density difference of different liquid phase products;

the control system comprises a material level meter L1 and a temperature meter T1 which are arranged on the melting-separating kettle

T4, a pressure gauge P1, a regulating valve TV2 and a heating regulating device TC1 which are arranged on a sulfur foam feeding pipe line, and a pressure regulating device PV1 on the gas phase QI discharging pipe.

In another aspect, the present invention relates to a method for continuous melting and multiphase separation using the above system, the method comprising:

S1, after heat exchange is carried out on a continuously added sulfur foam raw material A and a heating medium for heating, evaporating and melting the sulfur foam raw material A, the sulfur foam raw material A enters a multiphase separation tank 7 of the melting-separation kettle from the top of the melting-separation kettle; sulfur particles descending from the multiphase separation tank 7 to the melting heater 5 are completely melted in the liquid sulfur flow passage of the melting heater 5 without mechanical agitation; the heat medium comprises steam F or heat conducting oil F';

s2, producing a product of each phase of the molten sulfur foam raw material A in the melting separation kettle, wherein the product comprises the following components: vapor phase QI, liquid phase product YI, liquid phase product YII, and liquid phase product YIII;

S3, adjusting a loop by controlling a PC1, keeping the operation pressure of the melting-separating kettle to be 0.01-0.8 MPa, and discharging a gas product QI; simultaneously, continuously discharging the liquid phase product YI from the melting-separating kettle through a discharge port I in a self-flowing manner;

s4, regulating the temperature T2 in the multiphase separation tank 7 to be stable and keeping the temperature at 85-130 ℃ through TC 2; regulating the outlet temperature T1 of the liquid sulfur E to be stable and keeping 130-150 ℃ through TC 1;

S5, gradually accumulating to form a YII liquid layer between the liquid layer of the liquid phase product YI and the liquid layer of the liquid phase product YII, wherein the liquid phase product YII, the liquid phase product YII and the liquid phase product YII are automatically discharged through a liquid level maintaining mechanism; stably maintaining the interface of the YI liquid layer, the YII liquid layer and the YIII liquid layer;

S6, sulfur slag with the density greater than that of the liquid-phase product YIII is deposited at the bottom, gradually accumulated and intermittently discharged.

In another aspect, the present invention relates to a system for continuous melting and multiphase separation of aqueous sulfur particles, the system comprising: a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system,

The heat exchanger group comprises a preheater 9, a heater 1, a melting heater 5, and a conduction oil heater 4 'when using conduction oil F';

The multiphase separation tank comprises a multiphase separation tank 7 which is vertically and coaxially connected with the melting heater 5 to form a melting-separation kettle, and the liquid level maintaining mechanism is used for stably discharging each phase of products while continuously adding the sulfur foam raw material A, wherein each phase of products comprises: non-condensable gas B, clear liquid C, tar D, and liquid sulfur E;

The heat medium in the heat supply unit comprises steam F or heat conduction oil F'; when the heating medium of the heating unit is steam F, the heating unit comprises a steam trap 2, an outlet at the bottom side of a cone below the melting heater 5 is connected with the steam trap 2, and the steam condensate G generated is discharged after heat exchange by the heater 1; or when the heating medium of the heating unit is heat conduction oil F ', the heating unit comprises a heat conduction oil expansion tank 2' and a heat conduction oil pump 3'; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat conduction oil heater 4' is connected with the inlet of the melting heater 5, a circulation loop is formed by the outlet of the multiphase separation tank 7 and the heat conduction oil pump 3' through the heater 1, and the heat conduction oil expansion tank 2 is externally connected with the circulation loop and is arranged at the front end of the heat conduction oil pump 3';

The liquid level holding mechanism comprises a discharge outlet I, a discharge outlet II and a discharge outlet III; determining the pipe bottom height differences of the discharge outlet I, the discharge outlet II and the discharge outlet III through different liquid phase product density differences;

the control system comprises a material level meter L1, temperature meters T1-T4, a pressure meter P1, a regulating valve TV2 and a heat supply regulating device TC1 which are arranged on a sulfur foam feeding pipe line and a pressure regulating device PV1 on a non-condensable gas B discharging pipe which are arranged on the melting-separating kettle.

In another aspect, the invention relates to a method for continuous phase separation using the above system, the method comprising:

S1, continuously adding a sulfur foam raw material A into a multiphase separation tank 7 of a melting-separation kettle after heat exchange of a preheater 9 and a heater 1, wherein after heat exchange of the sulfur foam raw material A and a heating medium for heating, evaporating and melting the sulfur foam raw material A, sulfur particles descending from the multiphase separation tank 7 to a melting heater 5 are completely melted in a liquid sulfur runner of the melting heater 5 under the condition of no mechanical stirring; the heat medium comprises steam F or heat conducting oil F'; when the heating medium is steam F, the steam F is firstly arranged in a jacket of the multiphase separation tank 7, steam or a steam-water mixture discharged from the jacket of the multiphase separation tank 7 is sent into the melting heater 5, and steam condensate G discharged from the melting heater 5 enters the steam trap 2 and is discharged after heat exchange by the heater 1; or when the heating medium is heat conduction oil F ', the heat conduction oil F ' is sent into the heat conduction oil heater 4 through the heat conduction oil pump 3, the heat conduction oil F ' in the heat conduction oil heater 4 is sent into the melting heater 5 after being heated, the heat conduction oil F ' which is discharged from the melting heater 5 enters the jacket of the multiphase separation tank 7, and the heat conduction oil F ' which is discharged from the jacket of the multiphase separation tank 7 returns to the inlet of the heat conduction oil pump 3 through the heater 1;

S2, producing a product of each phase of the molten sulfur foam raw material A in the melting-separating kettle, wherein the product comprises the following components:

non-condensable gas B, clear liquid C, tar D, and liquid sulfur E;

S3, adjusting a loop by controlling a PC1, keeping the operation pressure of the melting-separating kettle to be 0.01-0.8 MPa, and discharging a gas phase product QI; simultaneously, continuously discharging the clear liquid C from the melting-separating kettle through a discharge port I in a self-flowing way;

S5, gradually accumulating tar D between the liquid layer of the clear liquid C and the liquid layer of the liquid sulfur E, wherein the tar D is discharged through a discharge port II in a self-flowing manner; the liquid sulfur E is discharged through a discharge port III in a self-flowing way; stably maintaining the interface of the clear liquid C, the tar D and the liquid sulfur E;

s6, sulfur slag with the density greater than that of the liquid sulfur E is deposited at the bottom, gradually accumulated and intermittently discharged.

Compared with the prior art, the continuous operation multi-separation system and method have the following advantages:

1) The operation pressure of the continuous operation multi-separation system is obviously reduced;

2) The operation pressure, the temperature gradient and the interfaces of the material layers in the melting-separating kettle are continuously and stably maintained;

3) The addition of the heating medium corresponds to the feeding amount of the sulfur foam raw material and the self-adaptive adjustment of the components of the sulfur foam raw material;

4) The various mediums except the sulfur slag separated by the melting-separating kettle can be continuously discharged, and the discharge amount of each medium is adaptively matched with the feed amount of the sulfur foam raw material and the components thereof;

5) Because the invention adopts the dividing wall type heat exchanger except the jacket heat exchanger, the heat exchange area (tube bundle or multi-layer/ring plate) of the invention is much larger than that of the melting-separating kettle of the single-layer inner wall of the jacket, the heating strength is obviously improved, the center distance between the heat transfer wall surface and the flow channel is greatly reduced, and under the condition of no mechanical stirring, the sulfur particles in the center of the flow channel can be reliably and completely melted, so that the discharged liquid sulfur is prevented from being mixed with sulfur particles;

6) The measures of continuously separating and discharging tar and intermittently discharging sulfur slag lead the color of liquid sulfur to be improved and organic matters and ash to be reduced; meanwhile, the temperature gradient in the melting-separating kettle of the system avoids the problem that salt in residual desulfurizing liquid is transferred into liquid sulfur caused by batch temperature rise of the melting-separating kettle in the prior art, and further reduces liquid sulfur ash; the continuous melting and multiphase separation system of the water-containing sulfur particles avoids that the intermittent sulfur melting technology brings O ₂ into a melting-separating kettle in the charging and discharging processes, so that the acidity of the liquid sulfur is reduced;

7) The continuous operation multi-separation system and method have the advantages of high overall heat conductivity coefficient, low operation condition, high production efficiency and small equipment volume;

8) The material and energy consumption of the system are obviously reduced through the step heat exchange among the mediums;

9) The monitoring measures are indirect and complete, the operation conditions are good, the starting and stopping are convenient and quick, and the manual operation intensity is obviously reduced;

10 The closed continuous disposal mode avoids the volatilization and dissipation of gas and realizes the essential cleaning of the disposal process.

The continuous operation multi-separation system and method greatly improve the recycling utilization level of the water-containing sulfur particles in industries such as petrochemical industry, natural gas, metallurgy and the like, and have extremely high economic value and environmental protection value.

Drawings

FIG. 1 is a flow chart of a system of examples 1-2 and 4-6 of the present invention.

Fig. 2 is a flow chart of the system of embodiments 3, 4 to 6 of the present invention.

Symbol description of main devices, components and media:

The device comprises a heater 1, an expansion tank 2', a steam trap 2, a heat conduction oil pump 3', a heat conduction oil heater 4', a melting heater 5, a liquid collecting disc 6, a multiphase separation tank 7, a liquid collecting disc 8, a preheater 9, a distributor 10 and a valve 11.

Liquid-meltable solid mixture (preferably sulfur foam material A), non-condensable gas B, clear liquid C, tar D, liquid sulfur E, heating medium F and steam condensate G.

FIG. 3 is a schematic illustration of the bottom height of the discharge piping of the system for continuous melting and multiphase separation of aqueous sulfur particles according to the present invention.

Detailed Description

The advantages and various effects of the present invention will be more clearly apparent from the following detailed description and examples. It will be understood by those skilled in the art that these specific embodiments and examples are intended to illustrate the invention, not to limit the invention.

Throughout the specification, unless specifically indicated otherwise, the terms used herein should be understood as meaning as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification will control.

Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.

The continuous melting and multiphase separation system according to the present invention can be combined into several integrated components/devices or a set of integrated devices according to the medium flow sequence and the manner of butt joint of the process functions. Combinations and modifications thereof should be understood to be within the scope of the present application and equivalents thereof.

The term "fusion heater" as used herein means: a heat transfer member that indirectly heats the liquid-meltable solid mixture with a heat medium and melts the meltable solid.

The multi-phase separation tank refers to: and (3) a part for standing and layering the multilayer liquid and the non-condensable gas obtained by heating the liquid-meltable solid mixture.

The "melt-separation tank" according to the invention, i.e. any operable combination of the heater and the multiphase separation tank, is preferably a melt-separation tank in which the multiphase separation tank is coaxially connected to the melt heater in the vertical direction.

The present invention provides a system for continuous melting and multiphase separation, the system comprising:

A heat supply unit for releasing energy from the heat medium to continuously provide driving force required for heating, evaporating and melting the liquid-meltable solid mixed material;

a liquid level maintaining mechanism including a discharge system for each liquid phase product for stably discharging each liquid phase product continuously in equal amounts to the feed without providing an adjusting mechanism; and

And a control system for regulating the temperature of the sulfur foam raw material A and each phase product, the pressure in the melting-separating kettle and the material level during the operation of the system.

In some embodiments of the present invention, the heating medium used in the heating unit is heat conducting oil or steam.

The heating medium is used in parallel in the component equipment of the system or in cascade in series among the component equipment of the system.

In certain embodiments of the invention, the heat exchanger package comprises a fusion heater 5 and a heat transfer oil heater 4' when heat transfer oil is used as a heat medium, the fusion heater 5 being in the shape of a cylinder, preferably a cylindrical or rectangular cylinder. The liquid phase product YIIII and the meltable solid product flow vertically downwards in the cylinder and exchange heat with the heating medium indirectly, and reach the bottom of the melting heater 5 to be completely melted, and the liquid phase product YIIII is discharged from the conical bottom side of the melting heater 5 to the system.

Further, the conduction oil heater 4' is preferably a dividing wall type heat exchanger other than a jacket heat exchanger.

Further, the heat exchanger group comprises a preheater 9 for heating the liquid-meltable solid mixture, a heater 1, which are optional components of the system of the invention, in order to further reduce the energy medium consumption of the system.

Furthermore, the preheater 9 of the system is arranged in series with the heater 1, according to the different temperatures of the inlet heat sources, the liquid-meltable solid mixture fed into the system is firstly subjected to indirect heat exchange with the liquid-phase product YI (such as supernatant liquid) discharged from the melting-separating kettle with lower temperature in the preheater 9 to raise the temperature, and then is subjected to indirect heat exchange with the steam condensate G or heat conducting oil F' discharged from the melting-separating kettle with higher temperature in the heater 1 to raise the temperature, and then enters the multiphase separating tank 7 of the melting-separating kettle from the top of the melting-separating kettle; if the preheater 9 and the heater 1 are not arranged, the liquid-meltable solid mixture fed into the system directly enters the multiphase separation tank 7 of the melting-separation kettle from the top of the melting-separation kettle at a lower temperature; the preheater 9 and the heater 1 of the system can also be integrated into an integrated heat exchanger for sectional heat exchange.

In some embodiments of the invention, when the heating medium of the heating unit is steam F, the heating unit includes a steam trap 2, and an outlet below the melting heater 5 is connected to the steam trap 2, for discharging the generated steam condensate G.

In other embodiments of the present invention, when the heating medium of the heating unit is the heat transfer oil F ', the heating unit includes a heat transfer oil expansion tank 2', a heat transfer oil pump 3', and a heat transfer oil heater 4'; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat conduction oil heater 4 'is connected with the inlet of the melting heater 5, and forms a circulation loop with the heat conduction oil pump 3' through the outlet of the multiphase separation tank 7. The heat conduction oil expansion tank 2 is externally connected to the circulation loop and is arranged at the front end of the heat conduction oil pump 3'.

In some embodiments of the present invention, the multiphase separation tank 7 is a liquid containing tank body with a distributor 10, a liquid collecting disc 8 and a liquid collecting disc 6, and the multiphase separation tank 7 is coaxially connected with the vertical direction of the melting heater 5 in the heat exchanger group.

Further, the liquid-meltable solid mixture entering the multiphase separation tank 7 is in direct countercurrent contact with the rising gas in the multiphase separation tank 7 in the upper space of the distributor 10, the gas phase QII of the rising gas as condensable gas is condensed and cooled, and the gas phase QI of the non-condensable gas B is discharged from the system; the liquid phase products YI are collected by the liquid collecting disc 8 and continuously discharged through the discharge port I; the liquid phase product YII is collected by the liquid collecting disc 6 and continuously discharged; the liquid phase product YIII and meltable solid product flow vertically downward into the melting heater 5.

In certain embodiments of the invention, the liquid level maintaining mechanism is a bottom height difference of each liquid phase medium discharging pipe, which is determined according to different density differences of liquid phase products.

Further, the liquid level holding mechanism includes a plurality of discharge ports, such as discharge port I, discharge port II, and discharge port III, for discharging the separation medium out of the system.

Further, taking the three-phase separation as shown in fig. 3 as an example, the height difference of the bottom of each liquid medium discharge pipe can be calculated by the following formula:

H4 =h1+h2+h3 (formula I)

H5≡H2-H4-H1+ρ1++ρ2X1 (formula II)

H6 =h3+ρ1 ≡ρ3×h1+ρ2 ≡ρ3×h2 (formula III)

Wherein H1 is the liquid layer thickness of liquid phase I; h2 is the liquid layer thickness of liquid phase II; h3 is the liquid layer thickness of liquid phase III; h4 is the height of the discharge tube I (corresponding to the total liquid layer height); h5 is the height of the discharge pipe II; h6 is the height of the discharge tube III; ρ1 is the liquid phase I density; ρ2 is the liquid phase II density; ρ3 is the liquid phase III density.

In certain embodiments of the present invention, the drain piping may be fixed or movable.

In certain embodiments of the invention, the control system comprises meter measuring points arranged on the melting-separating kettle and used for monitoring the material level, the temperature and the pressure, and regulating valves and heating regulating devices arranged on a feeding pipe line.

The present invention also provides a method for continuous melting and multiphase separation using a system as described above, the method comprising:

In certain embodiments of the invention, the heating medium is a heating medium having a temperature above the melting point of the meltable solid, such as: heat transfer oil or steam; preferably, the heating medium is used in parallel in the constituent devices of the system or in cascade in series between the constituent devices of the system.

In some embodiments of the present invention, when the heating medium is steam F, the steam F is first introduced into the jacket of the multiphase separation tank 7, the steam or the steam-water mixture exiting the jacket of the multiphase separation tank 7 is fed into the fusion heater 5, and the steam condensate G exiting the fusion heater 5 is discharged through the steam trap 2.

In some embodiments of the present invention, when the heat medium is heat transfer oil F ', the heat transfer oil F ' is fed into the heat transfer oil heater 4 through the heat transfer oil pump 3, the heat transfer oil F ' in the heat transfer oil heater 4 is heated and then fed into the melting heater 5, the heat transfer oil F ' exiting the melting heater 5 enters the jacket of the multiphase separation tank 7, and the heat transfer oil F ' exiting the jacket of the multiphase separation tank 7 returns to the inlet of the heat transfer oil pump 3.

In certain embodiments of the present invention, the liquid-meltable solid mixture fed continuously into the system is fed at a lower temperature directly from the top of the melt-separation tank into the multiphase separation tank 7 of the melt-separation tank; simultaneously, a heating medium (steam/heat conducting oil) is sent into a melting heater 5 of the melting-separating kettle and/or a jacket of a multiphase separating tank 7, and the heating medium F or steam condensate G with reduced enthalpy value after heat exchange is discharged out of the melting-separating kettle in an equivalent way.

In certain embodiments of the present invention, the continuously added liquid-meltable solid mixture in S3 is heated in multiphase separator tank 7; because of the mutual incompatibility and density difference between the liquid phases of each medium, such as the liquid phase product YI, the liquid phase product YII and the liquid phase product YII, the liquid phase product YII and the liquid phase product YII are continuously discharged from the multiphase separation tank 7 at a set position after being layered in the multiphase separation tank 7, wherein the liquid phase product YI and the liquid phase product YII are discharged from a system through heat exchange condensation cooling or directly through the liquid level maintaining mechanism, and solid particles are discharged from the liquid phase product YII between the multiphase separation tank 7 and the melting heater 5 into the melting heater 5.

Or in other specific embodiments of the invention, when the system is provided with the preheater 9 and the heater 1, the liquid-fusible solid mixture fed into the system is firstly subjected to indirect heat exchange and temperature rise with the liquid-phase product YI (such as clear liquid C) discharged from the melting-separating kettle with lower temperature in the preheater 9, then subjected to indirect heat exchange and temperature rise with the steam condensate G or heat conducting oil F' discharged from the melting-separating kettle with higher temperature in the heater 1, and then enters the multiphase separating tank 7 of the melting-separating kettle from the top of the melting-separating kettle.

In certain embodiments of the present invention, the temperature of the heat medium entering the melt-separation tank in the system of the present invention is greater than 120 ℃.

In some embodiments of the present invention, the upper limit of the operating pressure of the melting-separating vessel is not limited in theory, and the lower limit of the operating pressure is higher than 85KPa (a), and the operating pressure of the present invention is determined to be 0.01 to 0.8MPa depending on the system pressure at the digestion side of the vapor phase product (non-condensable gas B), so that the vapor phase product (non-condensable gas B) saturated with the solvent vapor in the present system is discharged and the present system is kept stable.

Preferably, the absolute pressure is 0.09-0.18 MPa (a).

In certain embodiments of the invention, 85 ℃ < T2<95 ℃;135 ℃ < T1<142 ℃.

In certain embodiments of the present invention, a YII liquid layer is gradually formed between the liquid layer of the liquid phase product YI with the smallest density and the liquid layer of the liquid phase product YII with the largest density, wherein the liquid phase product YI, the liquid phase product YII and the liquid phase product YII are all discharged by self-flowing through a liquid level maintaining mechanism; liquid level holding mechanism the liquid level holding mechanism stably holds the interface of the YI liquid layer, the YII liquid layer and the YIII liquid layer.

In certain embodiments of the invention, the liquid level holding means is simply a combination of individual separated medium discharge pipes, by designing the height difference between individual separated medium discharge pipes in accordance with the density difference of the individual separated medium and the liquid layer thickness of the individual separated medium stably held in the multiphase separation tank. The liquid level maintaining mechanism of the invention can have the following functions: 1) Continuously discharging the corresponding separated medium with the same feed liquid amount at the liquid layer position of each separated medium in the multiphase separation tank; 2) The feed liquid is continuously fed and the respective separated media are continuously discharged in equal feed amounts such that the respective separated media continuously maintain the liquid layer thickness at a defined liquid layer position.

In certain embodiments of the invention, the continuous melting and multiphase separation system of the invention can be used for separation of emulsions. For example, emulsion a, which is formed by mixing media b, c and d, generally cannot be delaminated by standing and can only be demulsified by heating. With the system according to the invention, it is possible to continuously heat the emulsion a, to set aside and to layer it, and to continuously discharge the separated media b, c and d via the discharge line. If the multiphase separation tank top temperature T4 is higher than the boiling point of the separation medium b, the separated media c and d are continuously discharged through the liquid phase discharge piping.

The present invention also provides a system for continuous melting and multiphase separation of aqueous sulfur particles, the system comprising: a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system,

The heat medium in the heat supply unit comprises steam F or heat conduction oil F'; the heat exchanger group provides heat for heating, evaporating and melting the sulfur foam raw material A;

The liquid level maintaining mechanism is a discharge outlet I, a discharge outlet II and a discharge outlet III which are arranged on the melting-separating kettle according to the height difference of the bottom of each liquid phase medium discharge pipe determined by the density difference of different liquid phase products;

the control system comprises a material level meter L1, temperature meters T1-T4, a pressure meter P1, a regulating valve TV2 and a heat supply regulating device TC1 which are arranged on a sulfur foam feeding pipe and a pressure regulating device PV1 on a gas phase product discharging pipe which are arranged on the melting-separating kettle.

In certain embodiments of the present invention, the heating medium is a heat transfer oil or steam; preferably, the heating medium is used in parallel in the constituent devices of the system or in cascade in series between the constituent devices of the system.

In certain embodiments of the invention, the fusion heater 5 is a multi-plate side-by-side or multi-tube side-by-side dividing wall heater with a jacketed conical bottom; preferably, the fusion heater 5 is a cylindrical heater. The heat exchange area (tube bundle or multi-layer/ring plate) of the melting heater 5 is much larger than that of the melting-separating kettle with a single-layer inner wall of the jacket, the heating strength is obviously improved, and the center distance between the heat transfer wall surface and the flow channel is greatly reduced. The liquid phase product YIII (such as liquid sulfur E) and sulfur particles flow vertically downwards in the cylinder and indirectly exchange heat with the heating medium, reach the bottom of the melting heater 5 and are completely melted, and the liquid phase product YIII is discharged from the conical bottom side of the melting heater 5.

Further, the heat exchanger group also comprises a preheater 9 and a heater 1, which are optional components of the system, so as to further reduce the energy medium consumption of the system.

Furthermore, the preheater 9 of the system is arranged in series with the heater 1, according to the different temperatures of the inlet heat sources, the sulfur foam raw material A fed into the system firstly exchanges heat with the liquid phase product YI (clear liquid C) discharged from the melting-separating kettle with lower temperature in the preheater 9 for heating, then exchanges heat with the steam condensate water G or heat conducting oil F' discharged from the melting-separating kettle with higher temperature in the heater 1 for heating, and then enters the multiphase separating tank 7 of the melting-separating kettle from the top of the melting-separating kettle; if the preheater 9 and the heater 1 are not arranged, the sulfur foam raw material A fed into the system directly enters the multiphase separation tank 7 of the melting-separation kettle from the top of the melting-separation kettle at a lower temperature; the preheater 9 and the heater 1 of the system can also be integrated into an integrated heat exchanger for sectional heat exchange.

In some embodiments of the present invention, when the heating medium of the heating unit is steam F, the heating unit includes a steam trap 2, and an outlet on a bottom side of a cone below the melting heater 5 is connected to the steam trap 2, so as to drain the generated steam condensate G.

In other embodiments of the present invention, when the heating medium of the heating unit is heat transfer oil F ', the heating unit includes a heat transfer oil expansion tank 2' and a heat transfer oil pump 3'; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat conduction oil heater 4' is connected with the inlet of the melting heater 5, a circulation loop is formed by the outlet of the multiphase separation tank 7 and the heat conduction oil pump 3', and the heat conduction oil expansion tank 2 is externally connected with the circulation loop and is arranged at the front end of the heat conduction oil pump 3 '.

In some embodiments of the present invention, the multiphase separation tank 7 is a liquid container with a distributor 10, a liquid collecting disc 8 and a liquid collecting disc 6. The multiphase separation tank 7 is coaxially connected with the vertical direction of the melting heater 5 in the heat exchanger group. The heat required by the temperature rise of each medium in the multiphase separation tank 7 is conducted from bottom to top, and the heat is conducted in a heat conduction mode and a convection mode in the layers of each medium layer, so that the efficiency of the direct heat exchange mode is improved compared with that of the indirect heat exchange mode.

In certain embodiments of the invention, the liquid level maintaining means is an evacuation piping having a respective liquid medium evacuation piping bottom height differential determined based on the difference in density of the different liquid phase products.

H4 =h1+h2+h3 (formula I)

H5≡H2-H4-H1+ρ1++ρ2X1 (formula II)

H6 =h3+ρ1 ≡ρ3×h1+ρ2 ≡ρ3×h2 (formula III)

In certain embodiments of the invention, the drain piping may be fixed or movable.

In certain embodiments of the invention, the gas phase product is non-condensable gas B, the liquid phase product YI is clear liquid C, the liquid phase product YII is tar D, and the liquid phase product YIII is liquid sulfur E.

The invention also provides a method for continuous melting and multiphase separation using the system described above, the method comprising:

In certain embodiments of the present invention, the amount of S1 added to the heating medium is related to the amount of sulfur foam material A fed and the moisture content therein, and is adaptively adjusted by the TC1 loop.

In certain embodiments of the present invention, wherein the temperature of the heat medium entering the melt-separation tank in the system of the present invention is greater than 130 ℃.

According to certain embodiments of the present invention, it is preferred that the two heating mediums are used in parallel in the constituent devices of the system or in cascade in series between the constituent devices of the system.

According to some embodiments of the invention, when the heating medium is steam F, the steam F is first introduced into the jacket of the multiphase separation tank 7, the steam or steam-water mixture exiting the jacket of the multiphase separation tank 7 is fed into the fusion heater 5, and the steam condensate G exiting the fusion heater 5 is discharged through the steam trap 2.

According to other embodiments of the present invention, when the heating medium is heat transfer oil F ', the heat transfer oil F ' is fed into the heat transfer oil heater 4 through the heat transfer oil pump 3, the heat transfer oil F ' is heated in the heat transfer oil heater 4 and then fed into the melting heater 5, the heat transfer oil F ' exiting the melting heater 5 enters the jacket of the multiphase separation tank 7, and the heat transfer oil F ' exiting the jacket of the multiphase separation tank 7 returns to the inlet of the heat transfer oil pump 3.

According to certain embodiments of the present invention, the sulfur foam raw material a fed into the present system enters the multiphase separation tank 7 of the melt-separation tank directly from the top of the melt-separation tank at a lower temperature; simultaneously, a heating medium (steam/heat conducting oil) is sent into a melting heater 5 of the melting-separating kettle and/or a jacket of a multiphase separating tank 7, and the heating medium F or steam condensate G with reduced enthalpy value after heat exchange is discharged out of the melting-separating kettle in an equivalent way.

In some embodiments of the present invention, the upper limit of the operating pressure of the melting-separating vessel is not limited in theory, and the lower limit of the operating pressure is higher than 85KPa (a), and the operating pressure of the present invention is determined to be 0.01 to 0.8MPa depending on the system pressure at the digestion side of the vapor phase product (non-condensable gas B), so that the vapor phase product (non-condensable gas B) saturated with the solvent vapor in the present system is discharged and the present system is kept stable. Since the multiphase separator tank 7 according to the invention operates at a lower pressure than in the prior art, less heat is required for the temperature rise of the respective media.

Preferably, the absolute pressure is 0.09-0.18 MPa (a). Maintaining the operating pressure of the melt-separation tank by means of a PC1 regulation loop;

in certain embodiments of the invention, the temperature T2 at the bottom of the multiphase separation tank 7 of the melt-separation tank is maintained stable at a value between 85 and 130 ℃ in S4 by means of a TC2 regulation loop; meanwhile, the temperature T1 of the liquid sulfur at the outlet of the melting heater 5 of the melting-separating kettle is stably kept between 130 ℃ and 150 ℃ through a TC1 regulating loop.

The liquid phase product YIII and solid sulfur particles flow vertically downwards in the cylinder of the melting heater 5 and indirectly exchange heat with the heating medium F, and reach the bottom of the melting heater 5 to be completely melted, and the liquid phase product YIII is discharged out of the system through a discharge outlet III at the conical bottom side of the melting heater 5.

Specifically, a distributor 10, a liquid collecting disc 8 and a liquid collecting disc 6 are arranged in the multiphase separation tank 7; the sulfur foam raw material A entering the multiphase separation tank 7 is in direct countercurrent contact with rising gas in the multiphase separation tank 7 in the upper space of the distributor 10, gas phase products of the rising gas as condensable gas are condensed and cooled, and the gas phase products of the non-condensable gas B are discharged out of the system; the sulfur foam raw material a lowered by the distributor 10 is lowered to the lower position of the drip pan 8; the liquid phase products YI are collected by the liquid collecting disc 8 and continuously discharged through the discharge port I; the liquid phase product YII is collected by the liquid collecting disc 6 and continuously discharged through the discharge outlet II; the liquid phase product YIII and sulphur particles flow vertically downwards into the fusion heater 5.

In certain embodiments of the present invention, the continuous addition of a heat medium to the melt heater 5 of the melt-separation tank indirectly heats the liquid sulfur and sulfur particles entering the melt heater 5 to 130-150 ℃; the liquid phase product YIIII (liquid sulfur) and sulfur particles reach the bottom of the melting heater 5 and are completely melted, and the liquid phase product YIIII is continuously discharged from the conical bottom side part of the melting heater 5; the materials with the density larger than that of the liquid sulfur are deposited at the bottom of the conical bottom of the melting heater 5 and are intermittently discharged according to conditions; the material having a density less than the liquid phase product YIII floats on the liquid layer of the liquid phase product YIII. The heat transfer is carried out between the liquid phase product YIII and the sulfur particles in a heat conduction mode, meanwhile, the density difference caused by the temperature difference between the upper end and the lower end in the liquid sulfur layer causes convection of the liquid phase product YIII in the heat exchange tube bundle of the melting heater 5 or between the heat exchange plates, so that the stirring effect is realized, namely: under the condition of no mechanical stirring, the sulfur particles in the center of the flow channel can be reliably and completely melted by utilizing the thermal stirring effect in the heat exchange tube bundle or between the heat exchange plates, and the sulfur particles reach the bottom of the melting heater 5 and are completely melted, so that the discharged liquid phase product YIII is prevented from being mixed with the sulfur particles.

In certain embodiments of the present invention, the upper material of the liquid layer of the liquid phase product YIII is a liquid phase product YII having a density between that of the liquid phase product YIII and that of the liquid phase product YI, the liquid layer temperature of the liquid phase product YII is between 85 and 130 ℃, the liquid layer height of the liquid phase product YII is continuously pressed out of the multiphase separation tank 7 of the melting-separation tank at the lower edge of the liquid collecting tray 6, and the discharge amount of the liquid phase product YII is equal to the entry amount of the liquid phase product YII into the melting-separation tank.

The system for continuous melting and multiphase separation of aqueous sulfur particles according to the present invention, wherein the preheater 9, heater 1, melting heater 5 and conduction oil heater 4 are in the form of a dividing wall heat exchanger other than a jacket heat exchanger.

The present invention also provides a system for continuous melting and multiphase separation of aqueous sulfur particles, the system comprising: a heat supply unit consisting of a heat exchanger group, a multiphase separation tank, a liquid level holding mechanism and a control system,

The liquid level maintaining mechanism comprises a discharge outlet I, a discharge outlet II and a discharge outlet III, and the height difference of the pipe bottom is determined according to the density difference of different liquid phase products;

In certain embodiments of the invention, the fusion heater 5 is a multi-plate side-by-side or multi-tube side-by-side dividing wall heater with a jacketed conical bottom; preferably, the fusion heater 5 is a cylindrical heater. The heat exchange area (tube bundle or multi-layer/coil plate) of the fusion heater 5 is much larger than the heat exchange area (jacketed single-layer inner wall) of the multiphase separator tank 7, and the fusion heater 5 can be understood as a heat transfer "heart" component in the system of the present invention.

In certain embodiments of the present invention, the heat transfer oil or steam as the heating medium may be used in parallel in the constituent devices of the system or in series and in steps between the constituent devices of the system.

In certain embodiments of the invention, the fusion heater 5 is a multi-plate side-by-side or multi-tube side-by-side dividing wall heater with a jacketed conical bottom; preferably, the fusion heater 5 is a cylindrical heater. The heat exchange area (tube bundle or multi-layer/ring plate) of the melting heater 5 is much larger than that of the melting-separating kettle with a single-layer inner wall of the jacket, the heating strength is obviously improved, and the center distance between the heat transfer wall surface and the flow channel is greatly reduced. The liquid phase product YIII (liquid sulfur E) and sulfur particles flow vertically downwards in the cylinder and exchange heat with the heating medium indirectly, reach the bottom of the melting heater 5 and are completely melted, and the liquid sulfur E is discharged from the conical bottom side of the melting heater 5.

In certain embodiments of the invention, the drain piping may be a fixed height setting or an adjustable height setting.

S2, producing a product of each phase of the molten sulfur foam raw material A in the melting-separating kettle, wherein the product comprises the following components: non-condensable gas B, clear liquid C, tar D, and liquid sulfur E;

s4, regulating the temperature T2 in the multiphase separation tank 7 to be stable and keeping the temperature at 85-130 ℃ through TC 2;

regulating the outlet temperature T1 of the liquid sulfur E to be stable and keeping 130-150 ℃ through TC 1;

Preferably, the absolute pressure is 0.09-0.18 MPa (a).

In certain embodiments of the invention, the temperature T2 at the bottom of the multiphase separation tank 7 of the melt-separation tank is kept stable in S3 between 85 and 130 ℃ by means of a TC2 conditioning circuit, i.e.: controlling the feeding amount of the sulfur foam raw material A of the melting-separating kettle according to the temperature; meanwhile, the temperature T1 of the liquid sulfur at the outlet of the melting heater 5 of the melting-separating kettle is stably kept between 130 ℃ and 150 ℃ through a TC1 regulating loop, namely: and controlling the feeding amount of the heating medium of the melting-separating kettle according to the temperature.

The liquid sulfur E and the solid sulfur particles vertically flow downwards in the cylinder of the melting heater 5 and indirectly exchange heat with the heating medium F, reach the bottom of the melting heater 5 and are completely melted, and the liquid sulfur E is discharged out of the system through a discharge outlet III at the conical bottom side part of the melting heater 5.

Specifically, a distributor 10, a liquid collecting disc 8 and a liquid collecting disc 6 are arranged in the multiphase separation tank 7; the sulfur foam raw material A entering the multiphase separation tank 7 is in direct countercurrent contact with rising gas in the multiphase separation tank 7 in the upper space of the distributor 10, the rising gas is condensed and cooled as condensable gas, and the condensed gas is discharged out of the system as gas phase product of non-condensable gas B; the sulfur foam raw material a lowered by the distributor 10 is lowered to the lower position of the drip pan 8; the clear liquid C is collected by the liquid collecting disc 8 and is continuously discharged through the discharge port I; the tar D is collected by the liquid collecting disc 6 and is continuously discharged through the discharge outlet II; the liquid sulfur E and sulfur particles flow vertically downward into the fusion heater 5.

In certain embodiments of the present invention, the continuous addition of a heat medium to the melt heater 5 of the melt-separation tank indirectly heats the liquid sulfur E and sulfur particles entering the melt heater 5 to 130-150 ℃; the liquid sulfur E and sulfur particles reach the bottom of the melting heater 5 and are completely melted, and the liquid sulfur E is continuously discharged from the conical bottom side part of the melting heater 5; the materials with the density larger than the liquid sulfur E are deposited at the bottom of the conical bottom of the melting heater 5 and are intermittently discharged according to conditions; the material with the density less than the liquid sulfur E floats on the liquid layer of the liquid sulfur E.

In some embodiments of the invention, the upper material of the liquid layer of the liquid sulfur E is tar D with the density between the liquid sulfur E and clear liquid C, the temperature of the liquid layer of the tar D is between 85 ℃ and 130 ℃, the liquid layer of the tar D is continuously pressed out of the multiphase separation tank 7 of the melting-separation kettle at the lower edge of the liquid collecting disc 6, and the discharge amount of the tar D is equal to the entering amount of the tar D entering the melting-separation kettle.

In some embodiments of the invention, the upper material of tar D is a less dense clear liquid C, the temperature of the liquid layer of clear liquid C is between 85 and 95 ℃, the height of which is continuously discharged from the multiphase separation tank 7 of the melt-separation tank at the upper edge of the liquid collecting tray 8, and the discharge amount of clear liquid C is slightly smaller than that of clear liquid C entering the melt-separation tank (wherein the difference is the discharge amount of the gas phase product).

In certain embodiments of the invention, the preheater 9, heater 1, melt heater 5 and conduction oil heater 4 are in the form of a dividing wall heat exchanger other than a jacketed heat exchanger.

Specifically, the system of the invention heats the sulfur foam raw material A with lower temperature into the non-condensable gas B with higher temperature, clear liquid C, tar D and liquid sulfur E which are separated at different positions of the melting-separating kettle, and the required heat is provided by a heat medium; under the heat transfer and exchange actions of the melting heater 5, the preheater 9 and the heater 1, the clear liquid C, the tar D and the liquid sulfur E are in direct liquid-liquid contact in the multiphase separation tank 7, and heat is transferred between layers in a heat conduction mode and in a convection mode in the layers; because of the density differences between the non-condensable gas B, the clear liquid C, the tar D and the liquid sulfur E, the phase change heat absorption of the sulfur foam raw material a continuously fed from the top of the multiphase separation tank 7 and the continuous sulfur particles, a significant temperature gradient is formed in the melting-separation tank of the present invention, namely: the temperature gradually increases from top to bottom.

Continuously adding a heat medium into a melting heater 5 of the melting-separating kettle, and indirectly heating liquid sulfur E and sulfur particles entering the melting heater 5 to 130-150 ℃; the liquid sulfur and sulfur particles reach the bottom of the melting heater 5 and are completely melted, and the liquid sulfur is continuously discharged from the conical bottom side part of the melting heater 5; depositing a material with the density greater than that of liquid sulfur at the bottom of the conical bottom of the melting heater 5, and intermittently discharging according to conditions; the material with density less than that of liquid sulfur floats on the liquid sulfur layer. The liquid sulfur and the sulfur particles transfer heat in a heat conduction mode, meanwhile, the density difference caused by the temperature difference between the upper end and the lower end in the liquid sulfur layer causes convection in the heat exchange tube bundle of the melting heater 5 or between the heat exchange plates, so that the stirring effect is achieved, namely: under the condition of no mechanical stirring, the sulfur particles in the center of the flow channel can be reliably and completely melted by utilizing the thermal stirring effect in the heat exchange tube bundle or between the heat exchange plates, and the sulfur particles reach the bottom of the melting heater 5 and are completely melted, so that the discharged liquid sulfur is prevented from being mixed with the sulfur particles.

The bottom of the multiphase separation tank 7 is a liquid sulfur layer mixed with water vapor, tar and sulfur particles along with the gradual melting of the sulfur particles: when the sulfur particles are melted, moisture adhering to the surfaces and in micropores of the sulfur particles is vaporized and rises float in the air due to a density difference with the sulfur particles; tar adhering to the surface of the sulfur particles and in the micropores also rises float in the air due to the density difference between the sulfur particles and the liquid sulfur; the color of the liquid sulfur E discharged from the molten sulfur layer below the middle part of the melting heater 5 is improved because the moisture and tar adhering to the surfaces and micropores of the sulfur particles are separated; the material (non-melted slag) with a density greater than that of the liquid sulfur is deposited at the bottom of the cone bottom of the melting heater 5 and gradually accumulated.

The liquid sulfur E is continuously discharged from the conical bottom side part of the melting heater 5; the material with density less than that of liquid sulfur floats on the liquid sulfur layer.

Tar D can gradually accumulate between the clear liquid layer and the liquid sulfur layer to form a tar layer, and the tar D can be discharged from the melting-separating kettle in a self-flowing manner; liquid sulfur E is discharged from the melting-separating kettle in a self-flowing way; the interface of the clean liquid layer, the tar layer and the liquid sulfur layer can be stably maintained, and the feeding amount of the heating medium can be adaptively adjusted according to the feeding amount of the sulfur foam raw material A and the water content in the sulfur foam raw material A, so that the temperature gradient in the melting-separating kettle can be stably maintained.

Materials with density greater than that of liquid sulfur (such as non-melted ash and non-sulfur-soluble salts) are deposited at the bottom of the cone bottom of the melting heater 5, gradually accumulated and intermittently discharged through a valve 11 according to conditions, and are mixed with sulfur, namely sulfur slag and waste; when the sulfur slag is intermittently discharged, other valves and the feeding amount of the sulfur foam raw material A do not need to be manually adjusted.

In certain embodiments of the invention, the flow rate of the ascending liquid flow in the design layer is less than 0.2m/s and the standing time of the tar is more than 20min in order to avoid adverse effects on sedimentation of the tar droplets and sulfur particles due to convection in the layer.

In certain specific embodiments of the invention, in order to avoid sulfur particles from being mixed in the discharged liquid sulfur, the temperature of 95-150 ℃ is designed to be higher than 40min, so that the sulfur particles are fully ensured to realize crystal form transformation and complete melting.

In some embodiments of the present invention, since the temperature gradient in the multiphase separation tank 7 is gradually increased from top to bottom, the clear liquid C, tar D and liquid sulfur E in the tank are all liquids, the upper limit of the operating pressure of the multiphase separation tank 7 of the melt-separation tank is theoretically unlimited, and the lower limit of the operating pressure should be higher than 85KPa (a); the operating pressure of the melt-separation tank according to the invention can then be determined from the system pressure at the digestion side of the non-condensable gas B.

In certain embodiments of the invention, the sulfur color is darkened and the char content is increased due to the tar mixing with the liquid sulfur, and the sulfur color is improved and the impurities are reduced by continuously heating, layering by utilizing density differences and continuously discharging the tar.

In certain embodiments of the present invention, sulfur particles entrained in the exiting supernatant fluid C can be reliably avoided due to the supernatant layer temperature being between 85 and 95 ℃, below the sulfur melting point, and the ascending liquid flow rate being less than 0.2m/s in the layer.

According to the continuous melting and multiphase separation method of the aqueous sulfur particles, the upper limit of the operation pressure of the melting-separation kettle is not limited in theory, the lower limit of the operation pressure is higher than 85KPa (a), and the operation pressure of the melting-separation kettle is determined according to the system pressure of the absorption end of the non-condensable gas B; S1-S4 is generally carried out at relatively low absolute pressures, in the range from 0.01 to 0.8MPa (a).

Preferably, the absolute pressure is 0.09-0.18 MPa (a).

According to the continuous melting and multiphase separation method of the water-containing sulfur particles, the addition amount of the heating medium F of S1 is related to the addition amount of the sulfur foam raw material A and the water content therein, and is adaptively adjusted through a TC1 regulating loop.

According to the continuous melting and multiphase separation method of the water-containing sulfur particles, in S3, the temperature T2 at the bottom of a multiphase separation tank 7 of a melting-separating kettle is stably maintained at a certain value between 85 and 130 ℃ through a TC2 regulating loop; meanwhile, the temperature T1 of the liquid sulfur at the outlet of the melting heater 5 of the melting-separating kettle is stably kept at a certain value between 130 ℃ and 150 ℃ through a TC1 regulating loop. Preferably, 85 ℃ < T2<95 ℃;135 ℃ < T1<142 ℃.

According to the method for continuous melting and multiphase separation of aqueous sulfur particles of the present invention, non-condensable gas B saturated with solvent vapor in the system is discharged in S2, and the operating pressure of the melting-separating vessel is stably maintained.

Examples

Initial feed and establishment of normal operating conditions for the System of example 1

The raw material liquid is sulfur foam after filter pressing or centrifugal separation, the desulfurizing liquid is ammonia solution, and the ratio of the desulfurizing liquid to the ammonia solution is 30% (wt/%); sulfur particles at a ratio of 30% (wt/%); tar <1% (wt/%); the temperature was 25 ℃.

The system comprises: the device comprises a heating unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system.

Wherein the heat exchanger group comprises a heater 1, a melting heater 5 and a preheater 9; the heating unit comprises a steam trap 2; the outlet below the melting heater 5 is connected with the steam trap 2, and the steam condensate G generated is discharged after heat exchange by the heater 1.

The multiphase separation tank comprises a multiphase separation tank 7, wherein a distributor 10, a liquid collecting disc 8 and a liquid collecting disc 6 are arranged in the multiphase separation tank 7; the multiphase separation tank 7 is coaxially connected with the melting heater 5 in the vertical direction to form a melting-separation kettle body; the preheater 9 and the heater 1 are arranged in series along the feeding route of the sulfur foam raw material A, and the heater 1 is connected with the top of the melting-separating kettle, so that the materials subjected to heat exchange enter the multiphase separating tank 7 of the melting-separating kettle from the top of the melting-separating kettle.

The liquid level maintaining mechanism comprises a discharge outlet I, and the height of the discharge outlet I is 2000mm; a discharge outlet II having a height of 1948mm; and a discharge port III having a height of 1671mm.

The control system comprises an instrument measuring point arranged on the melting-separating kettle, and a regulating valve 11 and a heat supply regulating device which are arranged on a sulfur foam feeding pipe. The sulfur discharge pipe is provided with a standby port 12 for adding liquid sulfur or solid sulfur particles during primary casting. The melting heater 5 is a vertical pipe type heat exchanger, and the shell side passes through steam; the throughput of the system was 1t feed solution/h.

The normal working pressure of the melting-separating kettle of the system is 55KPa (g); the heating medium is saturated steam of 0.45MPa (g).

Introducing steam F into a melting-separating kettle, and discharging steam condensate G out of the system after passing through a jacket of a multiphase separating tank 7, a melting heater 5, a steam trap 2 and a heater 1;

When the temperature T1 of the liquid sulfur and the temperature T2 of the bottom of the multiphase separation tank 7 are higher than 130 ℃, adding the liquid sulfur to half of the height of the heat exchange tube bundle of the submerged fusion heater 5 through a standby port 12 on a sulfur discharge pipe, or adding solid sulfur particles, and after the liquid sulfur is melted to half of the height of the heat exchange tube bundle of the submerged fusion heater 5; closing the standby port 12;

Opening a valve of a clear liquid discharge pipeline to enable clear liquid to be discharged out of the melting-separating kettle when the liquid level in the melting-separating kettle reaches the upper edge of the liquid collecting disc 8, forming a route from the discharge of the melting-separating kettle to the discharge of the preheater 9 to the discharge of the system, and then;

The sulfur foam raw material A with the temperature of about 0.2t/h and 25 ℃ enters a multiphase separation tank 7 of the melting-separation kettle from the top of the melting-separation kettle through a preheater 9 to a heater 1, the pressure in the melting-separation kettle is increased due to the evaporation of liquid in the sulfur foam raw material A, the pressure in the kettle is kept at 55KPa (g) through a PC1, and non-condensable gas B is discharged out of the system; meanwhile, the temperature T2 at the bottom of the multiphase separation tank 7 can be rapidly reduced, and the steam with the maximum flow rate can be introduced into the melting-separation kettle when the temperature T2 at the bottom of the multiphase separation tank 7 is lower than 130 ℃; at this stage, the addition ratio of the "steam F/sulfur foam raw material A" is several times higher than that in the normal operation, so that a temperature gradient deviating from the normal operation state is established;

After the temperature measuring point T2 at the bottom of the multiphase separation tank 7 is higher than 100 ℃, gradually increasing the feeding quantity of the sulfur foam raw material A according to the temperature rising speed of the temperature until the normal feeding quantity (0.2T/h) is reached, and stably controlling the temperature at 112 ℃; simultaneously, the feeding amount of steam F is regulated according to a liquid sulfur temperature measuring point T1, and the temperature is stably controlled at 138 ℃; namely: gradually adjusting the adding ratio of the steam F/sulfur foam raw material A which is several times higher than that of the steam F/sulfur foam raw material A in normal operation to the adding ratio of the steam F/sulfur foam raw material A in normal operation;

when the liquid level in the melting-separating kettle reaches the position of the liquid collecting disc 8, the heated clear liquid is discharged out of the melting-separating kettle through the self-flowing way, and is discharged out of the system through the sulfur preheater 9, wherein the thickness H ₁ of the clear liquid layer is 700mm, and the specific gravity is 1.

The sulfur foam raw material A is heated to 85 ℃ in a melting-separating kettle, sulfur particles, tar and desulfurizing liquid are naturally layered according to density difference, the sulfur particles are settled to the bottom of a multi-phase separating tank 7 and enter a melting heater 5 to be heated and melted into liquid sulfur, and a tar layer is accumulated between the liquid sulfur layer and the desulfurizing liquid layer; the specific gravity of the liquid sulfur layer is 1.8, and the liquid sulfur layer can automatically flow out of the system when the specific gravity reaches 1255 mm; opening a discharge valve of a tar pipeline, closing the valve if the discharged material is desulfurization clear liquid, continuously waiting for accumulation of tar in a material layer in the melting-separation kettle, if the discharged material is tar, enabling each material layer (a liquid sulfur layer, a tar layer and a desulfurization liquid layer) to be self-maintained, wherein the specific gravity of the tar layer is 1.08, and the total liquid layer thickness is 2000mm when the specific gravity reaches 45mm, and continuously discharging various media (non-condensable gas B, desulfurization liquid C, tar D and liquid sulfur E) separated by the melting-separation kettle according to the self-adaptive matching of the feeding amount and the components thereof;

so far, a temperature system, a pressure system and a liquid layer thickness are stably established in the system, and the separation performance of discharging all materials in the same amount as the sulfur foam raw material A is realized.

Example 2: continuous feeding of the system and realization of continuous sulfur melting and multiphase separation

The system consists of a heater 1, a steam trap 2, a melting heater 5, a liquid collecting disc 6, a multiphase separation tank 7, a liquid collecting disc 8, a preheater 9, a distributor 10 and a valve 11, wherein a standby port 12 is reserved on a sulfur discharge pipe, the melting heater 5 is a vertical pipe type heat exchanger, and the shell pass passes through steam; the processing capacity of the system is 1t raw material liquid/h, and the primary feeding and the establishment of normal working conditions of the system are completed.

The heating medium is saturated steam of 0.45MPa (g).

Steam F is introduced into a melting-separating kettle, and steam condensate G is discharged out of the system after passing through a jacket of a multiphase separating tank 7, a melting heater 5, a steam trap 2 and a heater 1; the working pressure of a melting-separating kettle of the system is kept at 55KPa (g) through PC1, and non-condensable gas B is discharged out of the system;

The temperature measuring point T2 at the bottom of the multiphase separation tank 7 is kept at 112+/-2 ℃, and the temperature measuring point T1 of liquid sulfur is kept at 138+/-2 ℃;

The sulfur foam raw material A with the temperature of 1t/h and 25 ℃ enters a multiphase separation tank 7 of the melting-separation kettle from the top of the melting-separation kettle through a preheater 9 and a heater 1, and the temperature of the sulfur foam raw material A entering the multiphase separation tank 7 is 39.8 ℃; continuously discharging 0.3kg/h of non-condensable gas B (saturated by solvent vapor in the system) out of the system through a PC1, keeping the working pressure of a melting-separating kettle of the system at 55KPa (g), keeping the solvent vapor amount in the non-condensable gas B at 8g/h, and discharging the non-condensable gas B of the multiphase separating tank 7 at the temperature of about 52 ℃; the clear liquid C is discharged from a liquid collecting disc 8 in the multiphase separation tank 7 to a melting-separating kettle in a self-flowing way, the temperature of the discharged clear liquid (namely, the temperature T3 in the middle of the multiphase separation tank 7) is 92 ℃, and the clear liquid C is discharged from a system after heat exchange between the preheater 9 and the sulfur foam raw material A at 25 ℃ and the temperature of the clear liquid C discharged from the system is about 60 ℃ and the flow rate is 300kg/h; the tar D is discharged from a liquid collecting disc 6 in the multiphase separating tank 7 to a melting-separating kettle in a self-flowing way, the discharge temperature is 95-112 ℃ (namely, the temperature is between the display value of the middle temperature T3 and the bottom temperature T2 of the multiphase separating tank 7), and the flow rate of the tar D discharged from the system is less than 10kg/h; when the sulfur foam raw material A is heated to between 85 and 95 ℃ in a melting-separating kettle, sulfur particles, tar and a desulfurizing liquid are naturally layered according to density difference, the sulfur particles are settled in a liquid sulfur layer at the bottom of a multiphase separating tank 7, the sulfur particles are settled in a heat exchange tube bundle of a melting heater 5 of the melting-separating kettle in the liquid sulfur layer due to the density difference between the sulfur particles and the liquid sulfur and heated to be melted, when the temperature reaches a liquid sulfur discharge temperature T1 (namely, the temperature at the bottom of the melting heater 5) of 138+/-2 ℃, the sulfur particles are discharged from a flow-out system through a U-shaped liquid sulfur discharge tube, and the discharge amount of the liquid sulfur E is about 700kg/h;

the flow rate of steam F fed into the system is about 71kg/h; the temperature of the steam condensate G discharge system is 60 ℃;

The bottom of the multiphase separation tank 7 is a liquid sulfur layer mixed with water vapor, tar and sulfur particles along with the gradual melting of the sulfur particles: moisture adhering to the surface and in the micropores of the sulfur particles vaporizes and rises float in the air due to the density difference with the sulfur particles; tar adhering to the surface of the sulfur particles and in the micropores also rises float in the air due to the density difference between the sulfur particles and the liquid sulfur; the color of the liquid sulfur E discharged from the molten sulfur layer below the middle part of the melting heater 5 is improved because the moisture and tar adhering to the surfaces and micropores of the sulfur particles are separated; the materials (non-melted slag) with density greater than that of the liquid sulfur are deposited at the bottom of the cone bottom of the melting heater 5, gradually accumulated, intermittently discharged through a valve 11 according to the condition, and the discharged sulfur slag is discarded.

The system realizes the improvement of the color and luster of the liquid sulfur E and the separation performance of the materials discharged in the same amount as the sulfur foam raw material A through a stable temperature system, a stable pressure system and a stable liquid layer thickness.

Example 3: initial feed and establishment of normal operating conditions of a system

The system comprises: the heat supply unit, the heat exchanger group, the multiphase separation tank liquid level retaining mechanism and the control system.

Wherein the heat exchanger group comprises a heater 1, a melting heater 5, a preheater 9 and a heat conducting oil heater 4'; the heating unit comprises a steam trap 2; the outlet below the melting heater 5 is connected with the steam trap 2, and the steam condensate G generated is discharged after heat exchange by the heater 1.

The heat supply unit comprises a heat conduction oil expansion tank 2 'and a heat conduction oil pump 3'; the heat conduction oil pump 3 'is connected with the heat conduction oil heater 4'; the outlet of the heat conduction oil heater 4 'is connected with the inlet of the melting heater 5, a circulation loop is formed by the outlet of the multiphase separation tank 7 and the heat conduction oil pump 3' through the heater 1, and the heat conduction oil expansion tank 2 'is externally connected with the circulation loop and is arranged at the front end of the heat conduction oil pump 3'.

The multiphase separation tank comprises a multiphase separation tank 7, wherein a distributor 10, a liquid collecting disc 8 and a liquid collecting disc 6 are arranged in the multiphase separation tank 7; the multiphase separation tank 7 is coaxially connected with the melting heater 5 in the vertical direction to form a melting-separation kettle body; the preheater 9 and the heater 1 are arranged in series along the feeding route of the sulfur foam raw material A, and the heater 1 is connected with the top of the melting-separating kettle, so that the heat exchanged materials enter the multiphase separating tank 7 of the melting-separating kettle from the top of the melting-separating kettle.

The liquid level maintaining mechanism comprises a discharge outlet I, and the height of the discharge outlet I is 2000mm; a discharge outlet II having a height of 1948mm; and a discharge opening III having a height of 1732mm.

The control system comprises a material level meter L1, temperature meters T1-T4, a pressure meter P1, a regulating valve TV2, heating regulating devices TC 1-TC 2 and a pressure regulating device PV1 on a gas-phase QI discharge pipe, wherein the material level meter L1, the temperature meters T1-T4, the pressure meter P1, the regulating valve TV2 and the heating regulating devices TC 1-TC 2 are arranged on a sulfur foam feed pipe.

The sulfur discharge pipe is provided with a standby port 12 for adding liquid sulfur or solid sulfur particles during primary casting. The melting heater 5 is a vertical pipe type heat exchanger, and the shell side passes through heat conduction oil; the heat conducting oil heater 4' is an electric heater; the throughput of the system was 1t feed solution/h.

The normal working pressure of the melting-separating kettle of the system is 55KPa (g); the heat medium is heat conducting oil.

The heat conduction oil F forms a closed cycle of the heat conduction oil F through a heat conduction oil pump 3 '. Fwdarw.a heat conduction oil heater 4'. Fwdarw.a melting heater 5 '. Fwdarw.a jacket of a multiphase separation tank 7'. Fwdarw.a heater 1 '. Fwdarw.a heat conduction oil pump 3'; starting an electric heater of the heat conduction oil heater 4'; the heat conduction oil expansion tank 2' balances the volume expansion of the heat conduction oil from normal temperature to working temperature;

When the temperature T1 of the liquid sulfur and the temperature T2 of the bottom of the multiphase separation tank 7 'are higher than 130 ℃, adding liquid sulfur to half of the height of the heat exchange tube bundle of the submerged fusion heater 5' through a standby port 12 'on a sulfur discharge pipe, or adding solid sulfur particles, and after the liquid sulfur is melted to half of the height of the heat exchange tube bundle of the submerged fusion heater 5'; closing the standby port 12';

Opening a valve of a clear liquid discharge pipeline to enable clear liquid to be discharged out of the melting-separating kettle when the liquid level in the melting-separating kettle reaches the upper edge of the liquid collecting disc 8', forming a route from the discharge of the melting-separating kettle to the discharge of the preheater 9' - & gt to the discharge of the system, and then;

the sulfur foam raw material A with the temperature of 0.2t/h and 25 ℃ enters a multiphase separation tank 7 'of the melting-separation kettle from the top of the melting-separation kettle through a preheater 9'. Fwdarw.a heater 1 '. Fwdarw.due to the evaporation of liquid in the sulfur foam raw material A, the pressure in the melting-separation kettle is increased, the pressure in the kettle is kept at 55KPa (g) through a PC1', and the non-condensable gas B is discharged out of the system; meanwhile, the temperature T2 at the bottom of the multiphase separation tank 7 can be rapidly reduced, and the heat conduction oil with the maximum flow and the highest allowable temperature can be introduced into the melting-separation kettle when the temperature T2 at the bottom of the multiphase separation tank 7' is lower than 130 ℃; in this stage, the addition ratio of the heat conduction oil F/sulfur foam raw material A is several times higher than that in normal operation, and the melting-separating kettle can quickly establish a temperature gradient deviating from the normal operation state;

After the temperature measuring point T2 at the bottom of the multiphase separation tank 7' is higher than 100 ℃, gradually increasing the feeding amount of the sulfur foam raw material A according to the temperature rising speed of the temperature until the normal feeding amount is reached, and stably controlling the temperature at 112 ℃; simultaneously, the temperature of heat conducting oil F fed into the melting-separating kettle is regulated according to a liquid sulfur temperature measuring point T1, and the liquid sulfur temperature measuring point T1 is stably controlled to 138 ℃; namely: gradually adjusting the adding ratio of the heat-conducting oil F/sulfur foam raw material A which is several times higher than that of the heat-conducting oil F/sulfur foam raw material A in normal operation to the adding ratio of the heat-conducting oil F/sulfur foam raw material A in normal operation;

When the liquid level in the melting-separating kettle reaches the position of the liquid collecting disc 8', the heated clear liquid is discharged out of the melting-separating kettle through the self-flowing way, and is discharged out of the system through the preheater 9', wherein the thickness H ₁ of the clear liquid layer is 570mm, and the specific gravity is 1.

When the sulfur foam raw material A is heated to 95 ℃ in a melting-separating kettle, sulfur particles, tar and desulfurizing liquid in the sulfur foam raw material A are naturally layered according to density difference, the sulfur particles are settled to the bottom of a multi-phase separating tank 7 'and enter a melting heater 5' to be heated and melted into liquid sulfur, and a tar layer is accumulated between a liquid sulfur layer and a desulfurizing liquid layer; the specific gravity of the liquid sulfur layer is 1.6, and the liquid sulfur layer can automatically flow out of the system when the specific gravity reaches 1255 mm; opening a discharge valve of the tar pipeline, and closing the valve if the discharge is observed to be desulfurization clear liquid, and continuing to wait for tar to accumulate in a material layer in the melting-separating kettle; if the discharged material is tar, each material layer (liquid sulfur layer, tar layer and desulfurization liquid layer) can be kept, at the moment, the specific gravity of the tar layer is 1.1, when the specific gravity reaches 175mm, the tar layer can flow out of the discharge system, the total liquid layer thickness is 2000mm, and various media (non-condensable gas B, desulfurization liquid C, tar D and liquid sulfur E) separated by the melting-separating kettle can be continuously discharged according to the self-adaptive matching of the feeding amount and the components thereof;

After the initial feed of the system and establishment of normal operating conditions are completed,

The temperature measuring point T2 at the bottom of the multiphase separation tank 7' is kept at 112+/-2 ℃, and the temperature measuring point T1 of the liquid sulfur is kept at 138+/-2 ℃;

The sulfur foam raw material A with the temperature of 1t/h and 25 ℃ enters a multiphase separation tank 7' of the melting-separation kettle from the top of the melting-separation kettle through a preheater 9 '. Fwdarw.a heater 1 '. Fwdarw.; continuously discharging 0.3kg/h of non-condensable gas B (saturated by solvent vapor in the system) out of the system through a PC1, keeping the working pressure of a melting-separating kettle of the system at 55KPa (g), keeping the solvent vapor amount in the non-condensable gas B at 8g/h, and discharging the non-condensable gas B of a multiphase separating tank 7' (namely, keeping the upper temperature T4 of the multiphase separating tank 7) at about 52 ℃; the clear liquid C is discharged from a liquid collecting disc 8' in a multiphase separation tank 7' to a melting-separating kettle in a self-flowing way, the temperature of the discharged clear liquid (namely, the temperature T3 in the middle of the multiphase separation tank 7) is 92 ℃, and the clear liquid C is discharged from a system after heat exchange between the preheater 9' and a sulfur foam raw material A at 25 ℃ and the temperature of the clear liquid C discharged from the system is about 60 ℃ and the flow rate is 300kg/h; the tar D is discharged from the liquid collecting disc 6' in the multiphase separating tank 7' to the melting-separating kettle in a self-flowing way, the discharge temperature is 95-112 ℃ (namely, the temperature is between the display values of the middle temperature T3 and the bottom temperature T2 of the multiphase separating tank 7 '), and the flow rate of the tar D discharged from the system is less than 10kg/h; when the sulfur foam raw material A is heated to between 85 and 95 ℃ in a melting-separating kettle, sulfur particles, tar and desulfurization liquid are naturally layered according to density difference, the sulfur particles are precipitated into a liquid sulfur layer at the bottom of a multiphase separating tank 7', the sulfur particles are precipitated into a heat exchange tube bundle of a melting heater 5' of the melting-separating kettle in the liquid sulfur layer due to the density difference between the sulfur particles and the liquid sulfur, and are heated and melted, when the temperature reaches a liquid sulfur discharge temperature T1 (namely, the temperature at the bottom of the melting heater 5) of 138+/-2 ℃, the sulfur particles are discharged from a flowing-out discharge system through a U-shaped liquid sulfur discharge tube, and the discharge amount of the liquid sulfur E is about 700kg/h;

The temperature of the heat conduction oil F entering the melting-separating kettle is 242 ℃, the temperature of the heat conduction oil F exiting the melting-separating kettle is 120 ℃, the temperature of the heat conduction oil F exiting the heater 1' is 60 ℃, and the circulation quantity of the heat conduction oil F in the system is about 117kg/h; the power consumption of the heat conduction oil pump 3' is 0.01Kw: the consumption power of the electric heater of the conduction oil heater 4' is 49.33Kw;

The bottom of the multiphase separation tank 7' is a liquid sulfur layer mixed with water vapor, tar and sulfur particles, accompanied by gradual melting of the sulfur particles: moisture adhering to the surface and in the micropores of the sulfur particles vaporizes and rises float in the air due to the density difference with the sulfur particles; tar adhering to the surface of the sulfur particles and in the micropores also rises float in the air due to the density difference between the sulfur particles and the liquid sulfur; the color of the liquid sulfur E discharged from the molten sulfur layer below the middle part of the melting heater 5' is improved because the moisture and tar adhered to the surface and micropores of the sulfur particles are separated; the materials (non-melted ash) with density greater than that of the liquid sulfur are deposited at the bottom of the cone bottom of the melting heater 5', gradually accumulated, intermittently discharged through a valve 11 according to the condition, and the discharged sulfur slag is discarded.

Example 4: when the composition of the raw material liquid of the system changes:

The raw material liquid is sulfur foam from a sulfur foam tank, the desulfurizing liquid is ammonia solution, and the ratio of the desulfurizing liquid to the ammonia solution is 95% (wt/%); sulfur particles at a ratio of 5% (wt/%); tar <1% (wt/%); the temperature was 25 ℃. The system feed rate was 1t/h.

Compared to example 2, the changes are: the flow rate of the discharged clear liquid C is 950kg/h; the discharge amount of the liquid sulfur E is about 50kg/h; the flow rate of steam F fed into the system was about 66kg/h.

Compared to example 3, the changes are: the flow rate of the discharged clear liquid C is 950kg/h; the discharge amount of the liquid sulfur E is about 50kg/h; the circulation amount of the heat conduction oil F in the system is about 108kg/h; the power consumption of the heat conduction oil pump 3' is 0.01Kw: the consumed power of the electric heater of the conduction oil heater 4' is 45.86Kw.

The system realizes the self-adaptation of the composition change of the raw material liquid, the improvement of the color and luster of the liquid sulfur E and the separation performance of the materials discharged in the same amount as the sulfur foam raw material A through a stable temperature system, a stable pressure system and a stable liquid layer thickness.

Example 5:

non-condensable gas B (saturated by solvent vapor in the system) discharged from the system is sent into an uncleaned gas pipeline before a wet catalytic oxidation desulfurization (H ₂ S) unit; the discharged clear liquid C is sent to a desulfurization liquid circulation tank of a wet catalytic oxidation desulfurization (H ₂ S) unit; the tar D is sent to a tar ammonia water separation unit before a wet catalytic oxidation desulfurization (H ₂ S) unit.

Example 6:

If there is no need to improve the color and purity of the liquid sulfur E, the drip pan 6 may not be provided in the multiphase separation tank 7 of the system as compared with examples 1 to 5.

Example 7: height difference adjustment of exhaust piping

For solid-liquid mixture systems, when separating three layers according to the mutual density difference in a melt-separation tank, it can be obtained by the known conditions and common knowledge: the liquid layer thickness H ₁ of the liquid 1 is 700mm and the specific gravity is 1.1; the liquid layer thickness H ₂ of the liquid 2 is 50mm and the specific gravity is 1.5; the liquid layer thickness H ₃ of the liquid 3 is 1250mm and the specific gravity is 2; the total liquid layer height H ₄ is 2000mm.

The height of the discharge pipe, which can be determined from the density difference, is then: the discharge tube C (corresponding to liquid 1) H ₄ is 2000mm, the discharge tube D (corresponding to liquid 2) H ₅ is 1813mm, and the discharge tube E (corresponding to liquid 3) H ₆ is 1673mm.

If the specific gravity of the liquid 2 becomes 1.6 and the specific gravity of the liquid 3 becomes 1.8, that is, the density difference between the liquid 2 and the liquid 3 becomes small, at this time, the positions of the discharge pipes are not changed, and only H ₆ needs to be adjusted to 1735mm, and the liquid layer thickness of each liquid medium becomes adaptively: h ₁ is 645mm, H ₂ is 105mm, and H ₃ is 1250mm.

While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.

It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.

Claims

1. A continuous melting and multiphase separation system for aqueous sulfur particles, the system comprising: a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system,

The heat medium in the heat supply unit is steam F or heat conduction oil F'; the heat exchanger group provides heat for heating, evaporating and melting the sulfur foam raw material A;

the heat exchanger group comprises a melting heater (5) and a heat conduction oil heater (4 ') when the heat conduction oil F' is used;

The multiphase separating tank comprises a multiphase separating tank (7), wherein the multiphase separating tank (7) is a liquid containing tank body provided with a distributor (10), a liquid collecting disc (8) and a liquid collecting disc (6) inside; the multiphase separation tank (7) is vertically and coaxially connected with the heat exchanger group to form a melting-separation kettle, and the body of the melting-separation kettle can completely melt the sulfur foam raw material A without mechanical stirring; while continuously adding the sulfur foam raw material A, stably discharging each phase of products through the liquid level maintaining mechanism, wherein each phase of products comprises a gas phase product and a liquid phase product YI, a liquid phase product YII and a liquid phase product YIII; the gas phase product is discharged from the upper part of the melting-separating kettle body; the liquid phase product YI is clear liquid C, the liquid phase product YII is tar D, and the liquid phase product YIII is liquid sulfur E;

the liquid level maintaining mechanism is a discharge pipe system arranged on the melting-separating kettle according to the height difference of the bottom of each liquid phase medium discharge pipe determined by the density difference of different liquid phase products, and comprises a discharge port I, a discharge port II and a discharge port III; the height difference of the bottom of each liquid medium discharge pipe can be calculated by the following formula:

H4=H1+H2+H3

H5≈H4－H1＋ρ1÷ρ2×H1

H6=H3＋ρ1÷ρ3×H1＋ρ2÷ρ3×H2

Wherein H1 is the liquid layer thickness of the liquid phase product YI; h2 is the liquid layer thickness of the liquid phase product YII; h3 is the liquid layer thickness of the liquid phase product YIII; h4 is the height of the discharge pipe I and corresponds to the height of the total liquid layer; h5 is the height of the discharge pipe II; h6 is the height of the discharge tube III; ρ1 is the density of the liquid phase product YI; ρ2 is the density of the liquid phase product YII; ρ3 is the density of the liquid phase product YIII;

The control system comprises a material level meter L1, temperature meters T1-T4, a pressure meter P1, a regulating valve TV2 and a heat supply regulating device TC1 which are arranged on a sulfur foam feeding pipe line, and a pressure regulating device PV1 on a gas phase product QI discharging pipe, wherein the material level meter L1, the temperature meters T1-T4, the pressure meter P1 and the regulating valve TC1 are arranged on the melting-separating kettle; wherein, the operation pressure of the melting-separating kettle is kept to be 0.01-0.8 MPa by controlling the PC1 regulating loop, and the gaseous product is discharged; the temperature T2 in the multiphase separation tank (7) is regulated by TC2 and is stably kept at 85-130 ℃; regulating the outlet temperature T1 of the liquid sulfur E to be stable and keeping 130-150 ℃ through TC 1; the upper material of the liquid sulfur E liquid layer is tar D with the density between the liquid sulfur E and clear liquid C, the liquid layer temperature of the tar D is between 85 and 130 ℃, and the liquid layer height of the tar D is continuously pressed out of the multiphase separation tank (7) at the lower edge of the liquid collecting disc (6); the liquid layer temperature of the clear liquid C is 85-95 ℃, and the height of the clear liquid C is continuously discharged out of the multiphase separation tank (7) at the upper edge of the liquid collecting disc (8).

2. The continuous melting and multiphase separation system of claim 1, wherein the heating medium is used in parallel in the constituent devices of the system or in series in steps between the constituent devices of the system.

3. Continuous melting and multiphase separation system according to claim 1 or 2 wherein the melting heater (5) is a multi-plate side-by-side or multi-tube side-by-side dividing wall heater with jacketed conical bottom.

4. A continuous melting and multiphase separation system as claimed in claim 3, characterized in that the melting heater (5) is a cylindrical heater.

5. Continuous melting and multiphase separation system according to claim 1, characterized in that when the heating medium of the heating unit is steam F, the heating unit comprises a steam trap (2), and the jacket outlet of the cone bottom below the melting heater (5) is connected to the steam trap (2) for discharging the steam condensate G produced.

6. Continuous melting and multiphase separation system according to claim 1, characterized in that when the heating medium of the heating unit is heat transfer oil F ', the heating unit further comprises a heat transfer oil expansion tank (2 ') and a heat transfer oil pump (3 '); the heat conduction oil pump (3 ') is connected with the heat conduction oil heater (4'); the outlet of the heat conduction oil heater (4 ') is connected with the inlet of the melting heater (5), and a circulation loop is formed by the outlet of the multiphase separation tank (7) and the heat conduction oil pump (3').

7. Continuous melting and multiphase separation system according to claim 1 or 2, characterized in that the heat exchanger package further comprises a preheater (9) for heating the sulphur foam feedstock a, a heater (1), the preheater (9) being arranged in series with the heater (1) along the sulphur foam feedstock a feed route, the sulphur foam feedstock outlet of the heater (1) being connected to the multiphase separation tank (7) via a melt-separation tank top.

8. A method of continuous melting and multiphase separation using the system of any one of claims 1, the method comprising:

S1, after heat exchange is carried out on a continuously added sulfur foam raw material A and a heating medium for heating, evaporating and melting the sulfur foam raw material A, the sulfur foam raw material A enters a multiphase separation tank (7) of the melting-separation kettle from the top of the melting-separation kettle; sulfur particles descending from the multiphase separation tank (7) to the melting heater (5) are completely melted in a liquid sulfur runner of the melting heater (5) without mechanical stirring; the heat medium comprises steam F or heat conducting oil F';

S2, producing a product of each phase of the molten sulfur foam raw material A in the melting separation kettle, wherein the product comprises the following components: a gas phase product QI, a liquid phase product YI, a liquid phase product YII, and a liquid phase product YIII; a distributor (10), a liquid collecting disc (8) and a liquid collecting disc (6) are arranged in the multiphase separating tank (7); the sulfur foam raw material A entering the multiphase separation tank (7) is in direct countercurrent contact with rising gas in the multiphase separation tank (7) in the upper space of the distributor (10), the gas phase product of the rising gas as condensable gas is condensed and cooled, and the gas phase product of the non-condensable gas B is discharged out of the system;

S3, adjusting a loop by controlling a PC1, keeping the operation pressure of the melting-separating kettle to be 0.01-0.8 MPa, and discharging a gaseous product QI; simultaneously, the liquid phase product YI is collected at the liquid collecting disc (8) and continuously discharged in a self-flowing way through a discharge port I;

S4, regulating the temperature T2 in the multiphase separation tank (7) to be stable at 85-130 ℃ through TC 2; regulating the outlet temperature T1 of the liquid sulfur E to be stable and keeping 130-150 ℃ through TC 1;

S5, gradually accumulating a YII liquid layer between the liquid layer of the liquid phase product YI and the liquid layer of the liquid phase product YIII, and continuously discharging the YII liquid layer through the discharge outlet II after being collected at the liquid collecting disc (6); stably maintaining the interface of the YI liquid layer, the YII liquid layer and the YIII liquid layer;

s6, enabling the liquid-phase product YIII and sulfur particles to vertically flow downwards into the melting heater (5), and enabling sulfur slag with density larger than that of the liquid-phase product YIII to be deposited at the bottom, gradually accumulating and intermittently discharging.

9. The method of claim 8, wherein the heating medium is used in parallel in the constituent devices of the system or in series in steps between the constituent devices of the system.

10. A method according to claim 8, characterized in that when the heating medium is steam F, the steam F is first introduced into the jacket of the multiphase separation tank (7), the steam or steam-water mixture exiting the jacket of the multiphase separation tank (7) is fed into the fusion heater (5), and the steam condensate G exiting the fusion heater (5) is discharged after passing through the steam trap (2).

11. The method according to claim 8, wherein when the heating medium is heat transfer oil F ', the heat transfer oil F' is fed into the heat transfer oil heater (4 ') through the heat transfer oil pump (3'), and after being heated in the heat transfer oil heater (4 '), the heat transfer oil F' exiting the heat transfer oil heater (5) is fed into the jacket of the multiphase separation tank (7), and the heat transfer oil F 'exiting the jacket of the multiphase separation tank (7) is returned to the inlet of the heat transfer oil pump (3').

12. The method as claimed in claim 8, characterized in that the liquid sulfur E and solid sulfur particles flow vertically downwards in the cylinder of the melting heater (5) and indirectly exchange heat with a heating medium F, reaching the bottom of the melting heater (5) and having been completely melted, and the liquid sulfur E is discharged from a discharge port III at the conical bottom side of the melting heater (5) out of the system.

13. A system for continuous melting and multiphase separation of aqueous sulfur particles, the system comprising: a heat supply unit, a heat exchanger group, a multiphase separation tank, a liquid level maintaining mechanism and a control system,

The heat exchanger group comprises a preheater (9) and a heater (1) for heating the sulfur foam raw material A; a fusion heater (5); and a conduction oil heater (4 ') when using conduction oil F';

the multiphase separating tank comprises a multiphase separating tank (7), wherein the multiphase separating tank (7) is a liquid containing tank body provided with a distributor (10), a liquid collecting disc (8) and a liquid collecting disc (6) inside; the multiphase separation tank (7) is vertically and coaxially connected with the melting heater (5) to form a melting-separation kettle, and the melting-separation kettle can completely melt the sulfur foam raw material A without mechanical stirring; stably discharging each phase of product through the liquid level maintaining mechanism while continuously adding the sulfur foam raw material A, wherein each phase of product comprises: non-condensable gas B, clear liquid C, tar D and liquid sulfur E;

The heat medium in the heat supply unit comprises steam F or heat conduction oil F'; when the heating medium of the heating unit is steam F, the heating unit comprises a steam trap (2), a condensate water outlet of a jacket at the lower part of the melting heater (5) is connected with the steam trap (2), and the steam condensate water G generated is discharged after heat exchange of the heater (1); or when the heating medium of the heating unit is heat conduction oil F ', the heating unit comprises a heat conduction oil expansion tank (2 ') and a heat conduction oil pump (3 '); the heat conduction oil pump (3 ') is connected with the heat conduction oil heater (4'); the outlet of the heat conduction oil heater (4 ') is connected with the inlet of the melting heater (5), a circulation loop is formed by the outlet of the multiphase separation tank (7) and the heat conduction oil pump (3') through the heater (1), and the heat conduction oil expansion tank (2 ') is externally connected with the circulation loop and is arranged at the front end of the heat conduction oil pump (3');

The liquid level holding mechanism comprises a discharge outlet I, a discharge outlet II and a discharge outlet III; determining the pipe bottom height differences of the discharge outlet I, the discharge outlet II and the discharge outlet III through different liquid phase product density differences; the height difference of the bottom of each liquid medium discharge pipe can be calculated by the following formula:

H4=H1+H2+H3

H5≈H4－H1＋ρ1÷ρ2×H1

H6=H3＋ρ1÷ρ3×H1＋ρ2÷ρ3×H2

Wherein H1 is the liquid layer thickness of the liquid phase product YI; h2 is the liquid layer thickness of the liquid phase product YII; h3 is the liquid layer thickness of the liquid phase product YIII; h4 is the height of the discharge pipe I and corresponds to the height of the total liquid layer; h5 is the height of the discharge pipe II; h6 is the height of the discharge tube III; ρ1 is the density of the liquid phase product YI; ρ2 is the density of the liquid phase product YII; ρ3 is the density of the liquid phase product III;

The control system comprises a material level meter L1, temperature meters T1-T4, a pressure meter P1, a regulating valve TV2 and a heat supply regulating device TC1 which are arranged on a sulfur foam feeding pipe line, and a pressure regulating device PV1 on a non-condensable gas B discharging pipe, wherein the material level meter L1, the temperature meters T1-T4, the pressure meter P1 and the regulating valve TC1 are arranged on the melting-separating kettle; wherein, the operation pressure of the melting-separating kettle is kept to be 0.01-0.8 MPa by controlling the PC1 regulating loop, and the gaseous product is discharged; the temperature T2 in the multiphase separation tank (7) is regulated by TC2 and is stably kept at 85-130 ℃; regulating the outlet temperature T1 of the liquid sulfur E to be stable and keeping 130-150 ℃ through TC 1; the upper material of the liquid sulfur E liquid layer is tar D with the density between the liquid sulfur E and clear liquid C, the liquid layer temperature of the tar D is between 85 and 130 ℃, and the liquid layer height of the tar D is continuously pressed out of the multiphase separation tank (7) at the lower edge of the liquid collecting disc (6); the liquid layer temperature of the clear liquid C is 85-95 ℃, and the height of the clear liquid C is continuously discharged out of the multiphase separation tank (7) at the upper edge of the liquid collecting disc (8).

14. A method of continuous phase separation using the system of claim 13, the method comprising:

S1, continuously adding a sulfur foam raw material A into a multiphase separation tank (7) of a melting-separating kettle after heat exchange of a preheater (9) and a heater (1), and completely melting sulfur particles which descend from the multiphase separation tank (7) to the melting heater (5) in a liquid sulfur runner of the melting heater (5) under the condition of no mechanical stirring after heat exchange of the sulfur foam raw material A and a heating medium for heating, evaporating and melting the sulfur foam raw material A; a distributor (10), a liquid collecting disc (8) and a liquid collecting disc (6) are arranged in the multiphase separating tank (7); the sulfur foam raw material A entering the multiphase separation tank (7) is in direct countercurrent contact with rising gas in the multiphase separation tank (7) in the upper space of the distributor (10), the gas phase product which is taken as condensable gas in the rising gas is condensed and cooled, and the gas phase product which is taken as non-condensable gas B is discharged out of the system; the heat medium comprises steam F or heat conducting oil F'; when the heating medium is steam F, the steam F is firstly arranged in a jacket of a multiphase separation tank (7), steam or a steam-water mixture discharged from the jacket of the multiphase separation tank (7) is sent into a melting heater (5), and steam condensate G discharged from the melting heater (5) enters a steam trap (2) and is discharged after heat exchange by the heater 1; or when the heating medium is heat conduction oil F ', the heat conduction oil F ' is sent to a heat conduction oil heater (4 ') through a heat conduction oil pump (3 '), the heat conduction oil F ' in the heat conduction oil heater (4 ') is heated and then sent to a melting heater (5), the heat conduction oil F ' exiting the melting heater (5) enters a jacket of a multiphase separation tank (7), and the heat conduction oil F ' exiting the jacket of the multiphase separation tank (7) returns to an inlet of the heat conduction oil pump (3 ') through a heater (1);

s2, producing each phase of product in the melting-separating kettle by the melted sulfur foam raw material A;

S3, adjusting a loop by controlling a PC1, keeping the operation pressure of the melting-separating kettle to be 0.01-0.8 MPa, and discharging a gas phase product QI; meanwhile, the clear liquid C is collected by the liquid collecting disc (8) and continuously discharged in a self-flowing way through the discharge port I;

S5, gradually accumulating tar D between the liquid layer of the clear liquid C and the liquid layer of the liquid sulfur E, wherein the tar D is collected at the liquid collecting disc (6) and is discharged through a discharge port II in a self-flowing way; the liquid sulfur E is discharged through a discharge port III in a self-flowing way; stably maintaining the interface of the clear liquid C, the tar D and the liquid sulfur E;

s6, vertically downwards flowing the liquid sulfur E and sulfur particles into the melting heater (5), depositing sulfur slag with density greater than that of the liquid sulfur E at the bottom, gradually accumulating and intermittently discharging.

15. Use of the continuous melting and multiphase separation system according to any of claims 1-7 in continuous melting and multiphase separation technology of aqueous sulphur particles.