CN115852182A - A kind of aluminum amalgam preparation method of inert gas bubbling mercury injection - Google Patents

Abstract

The invention discloses an inert gas bubbling mercury-injecting aluminum amalgam preparation method, which relates to the technical field of non-ferrous metal smelting. The inert gas is used as a protective gas, and the mercury is heated by an evaporator to form mercury vapor. The pipeline and the feed pipe whose lower end is inserted below the liquid level of the reaction furnace lead into the interior of the aluminum soup, and the carried mercury vapor is diffused into the aluminum soup by bubbling to complete the preparation of the aluminum amalgam. Since mercury enters the molten aluminum soup in the form of vapor, the whole process is safe and controllable, and mercury bumping does not occur. Under the double action of bubbling and stirring, the present invention can obtain aluminum amalgam with relatively uniform components.

Description

A kind of aluminum amalgam preparation method of inert gas bubbling mercury injection

technical field

The invention relates to the technical field of non-ferrous metal smelting, in particular to an aluminum amalgam preparation method for inert gas bubbling mercury injection.

Background technique

Aluminum water hydrogen production technology is a very potential hydrogen production technology, and its reaction product is an important precursor for the preparation of another important industrial raw material, ultrafine alumina powder. Since a dense oxide film is easily formed on the surface of aluminum, which prevents the aluminum water from continuing to react, metal aluminum cannot be directly used to react with aluminum. Mercury in aluminum amalgam can prevent the surface of aluminum from being oxidized to form a dense oxide film, and mercury is easily separated by heating and evaporation, so aluminum amalgam is a good material for hydrogen production and ultrafine alumina powder.

Because the melting point of aluminum is much higher than the boiling point of mercury, aluminum amalgam is difficult to prepare by traditional methods. Most of the published aluminum amalgam preparation methods are chemical methods, which can only prepare a small amount of aluminum amalgam on the surface of aluminum, and do not have the value of large-scale industrial application.

Contents of the invention

The object of the present invention is to provide an inert gas bubbling mercury injection method for preparing aluminum amalgam, so as to solve the above-mentioned problems in the prior art, and to prepare a large amount of aluminum amalgam with uniform properties under safe and reliable conditions.

To achieve the above object, the present invention provides the following scheme:

The invention provides a method for preparing aluminum amalgam by inert gas bubbling mercury injection, which comprises the following steps:

Step 1, building a bubbling mercury-injecting aluminum amalgam preparation device;

Step 2, calculate the amount of required mercury raw material according to the mass of aluminum put into the reaction furnace at one time, and calculate the amount and flow rate of the inert gas required to transport mercury according to the preparation time requirement;

Step 3, putting the weighed aluminum into the smelting furnace for melting;

Step 4, put the weighed mercury raw material into the evaporator, and check the airtightness of the second pipeline from the evaporator to the reaction furnace;

Step 5, open the valve on the third pipeline of the inert gas direct-flow reaction furnace, and temporarily close the third pipeline of the inert gas direct-flow reaction furnace after blowing off the air in the third pipeline;

Step 6, after the aluminum is melted, the surface oxide slag is removed, and the molten aluminum is transferred to the reaction furnace;

Step 7: Insulate the molten aluminum in the reaction furnace so that the internal temperature of the furnace of the reaction furnace is above the melting point of aluminum, and open the stirring structure of the reaction furnace so that the oxide slag that sinks at the bottom of the furnace of the reaction furnace Float to the surface, and then carry out surface slag removal treatment;

Step 8, turn on the preheater on the first pipeline to heat the first pipeline, simultaneously turn on the heater on the second pipeline to heat up and keep warm the second pipeline, and open the evaporator to heat the mercury raw material;

Step 9: After the slag removal is completed and the temperature of the evaporator reaches the rated value, the inert gas passes through the preheater and the evaporator in turn, and the inert gas with mercury vapor enters the furnace of the reaction furnace through the feed pipe of the reaction furnace. In molten aluminum;

Step ten, when the scheduled feeding time is reached, take the molten aluminum amalgam sample from the sampling port of the reaction furnace, and detect the components; if the components meet the requirements, stop the evaporator heating and close the valve of the first pipeline, open the second The three-pipeline valve allows the inert gas to directly enter the feed pipe, maintaining the delivery of clean, high-temperature inert gas for a period of time;

In step eleven, the aluminum amalgam produced in the reaction furnace is ventilated and casted, and the production of the hydrogen production material is completed.

Preferably, the bubbling mercury injection aluminum amalgam preparation device includes an inert gas storage structure, a preheater, an evaporator, a smelting furnace and a reaction furnace, and the inert gas storage structure is used to store the inert gas, so The evaporator is used to heat mercury raw material, the melting furnace is used to smelt aluminum, the inert gas storage structure is connected to the preheater through a first pipeline, and the preheater is connected to the preheater through a first pipeline. The evaporator is connected, the evaporator is connected with the feed pipe of the reaction furnace through the second pipeline, the preheater is connected with the feed pipe of the reaction furnace through the third pipeline, and the melting furnace is connected with the feed pipe of the reaction furnace The feed port of the reaction furnace is connected.

Preferably, heaters are provided on the first pipeline, the second pipeline and the third pipeline, and the heaters are cast copper heating rings or ceramic heating rings.

Preferably, in the second step, the mercury raw material is pure mercury or mercury-containing amalgam.

Preferably, the inert gas used is a gas with stable properties below 700°C and not easily reacting with aluminum.

Preferably, the inert gas used is nitrogen or an inert gas.

Preferably, the rated operating temperatures of the preheater, the evaporator and the heater of the second pipeline are all set above the boiling point of the mercury raw material.

Preferably, the second pipeline is a seamless pipe made of 310S or 316L material.

Preferably, the feed pipe is made of a material with a temperature resistance not lower than 700°C and not easily corroded by aluminum water.

Preferably, the lower end of the feed pipe is provided with an opening, and a plurality of through holes are opened on the side wall of the lower part of the feed pipe; the lower end of the feed pipe is located below the liquid level of the aluminum soup and is at a distance 1cm at the bottom.

Compared with the prior art, the present invention has achieved the following technical effects:

1, adopt the present invention to be able to prepare the aluminum amalgam of uniform composition safely in a large amount;

2. The present invention is also applicable to the melting method to prepare an alloy whose melting point of one component is higher than the boiling point of another component, so as to avoid the explosion that is extremely easy to occur during the preparation process;

3. The activity of the reaction between aluminum amalgam and water can be realized by adjusting the amount of mercury introduced and controlling the mercury content in the alloy;

4. The gaseous mercury is transported through the inert gas, and transported through the third heat-insulating pipeline to ensure that the mercury will not cause too intense phase change reaction (bumping) due to sudden boiling when it contacts aluminum water;

5. The feed pipe adopts a porous structure on the side wall. When the gas containing high concentration of mercury enters the aluminum water, it will be broken up into many small bubbles, which makes the mixing of aluminum and mercury elements more uniform and the process more gentle.

Description of drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the accompanying drawings required in the embodiments. Obviously, the accompanying drawings in the following description are only some of the present invention. Embodiments, for those of ordinary skill in the art, other drawings can also be obtained based on these drawings without any creative effort.

Fig. 1 is the aluminum amalgam preparation method flowchart of inert gas bubbling type mercury delivery of the present invention;

Fig. 2 is the schematic diagram of the bubbling type mercury injection aluminum amalgam preparation device of the present invention;

Among them: 1-inert gas storage structure, 2-preheater, 3-evaporator, 4-smelting furnace, 5-first pipeline, 6-second pipeline, 7-third pipeline, 8-reaction furnace.

Detailed ways

The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

The object of the present invention is to provide an inert gas bubbling mercury injection method for preparing aluminum amalgam, so as to solve the above-mentioned problems in the prior art, and to prepare a large amount of aluminum amalgam with uniform properties under safe and reliable conditions.

In order to make the above objects, features and advantages of the present invention more comprehensible, the present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.

As shown in Figure 1: the present embodiment provides a kind of aluminum amalgam preparation method of inert gas bubbling type mercury injection, and the production of 100kg of hydrogen production material with mercury content of 0.5% comprises the following steps:

Step 1, calculate the material, considering the loss, about 105kg of aluminum and 1kg of mercury raw materials are needed; weigh 105kg of aluminum block and about 1kg of mercury raw materials for use, and build a bubbling mercury-injecting aluminum amalgam preparation device according to Figure 2;

As shown in Figure 2, the bubbling mercury injection aluminum amalgam preparation device includes an inert gas storage structure 1, a preheater 2, an evaporator 3, a melting furnace 4 and a reaction furnace 8, and the inert gas storage structure 1 is used for storing Inert gas, the evaporator 3 is used to heat the mercury raw material, the mercury raw material is pure mercury or mercury-containing amalgam, the melting furnace 4 is used for melting aluminum, the inert gas storage structure 1 is connected to the preheater 2 through the first pipeline 5 , the preheater 2 is connected with the evaporator 3 through the first pipeline 5, the evaporator 3 is connected with the feed pipe of the reaction furnace 8 through the second pipeline 6, and the preheater 2 is connected with the reaction furnace 8 through the third pipeline 7 The feeding pipe is connected, and the smelting furnace 4 is connected with the feed port of the reaction furnace 8;

Step 2, calculate the amount of required mercury raw material according to the mass of aluminum put into reaction furnace 8 at one time, and calculate the amount and flow rate of the inert gas required to transport mercury according to the preparation time requirements;

Step 3, put the weighed aluminum into the smelting furnace 4 for melting, according to the time when the reaction furnace 8 is expected to heat up to the rated temperature (for example, 695±15° C.), choose an opportunity to start the reaction furnace 8 to preheat, and put the second Pipeline 6 is heated to 360±40°C;

Step 4, put the weighed mercury raw material into the evaporator 3, and check the airtightness of the evaporator 3 to the second pipeline 6 of the reaction furnace 8;

Step 5, according to the estimated time of aluminum conversion and the time required for temperature rise, select an opportunity to turn on the heater of the preheater 2 and the third pipeline 7; when the temperature of the third pipeline 7 rises to 400±40°C, blow it off with an inert gas The air in the hearth of the third pipeline 7 and the reaction furnace 8; select the opportunity to open the evaporator 3 heating according to the expected feeding time;

Step 6, after the aluminum is melted, the surface oxide slag is removed, and the molten aluminum is transferred to the reaction furnace 8;

Step 7: Insulate the molten aluminum in the reaction furnace 8, so that the internal temperature of the furnace chamber of the reaction furnace 8 is above the melting point of aluminum at 35±15° C., and open the stirring structure of the reaction furnace 8, so that the sinking in the reaction furnace The oxidized slag at the bottom of the hearth of the furnace 8 floats to the surface, and then the slag removal process is performed on the surface _{, and} the valve of the third pipeline 7 is closed after the slag removal;

Step 8, turn on the preheater 2 on the first pipeline 5 to heat the first pipeline 5, and at the same time turn on the heater of the second pipeline 6 to heat up and keep warm the second pipeline 6, and turn on the evaporator 3 pair Mercury raw material is heated;

Step 9: After the slag removal is completed and the temperature of the evaporator 3 reaches the rated value, open the valve of the first pipeline 5 so that the inert gas passes through the preheater 2 and the evaporator 3 in sequence, and the inert gas with mercury vapor passes through the reaction The feed pipe of the furnace 8 enters the aluminum in the molten state of the hearth of the reaction furnace 8;

Step 10: Estimate the starting time of casting aluminum and the heating time of the heating device of the aluminum outlet, and start heating the aluminum outlet at an appropriate time; when the scheduled feeding time is reached, take a sample of molten aluminum amalgam from the sampling port of reaction furnace 8, and detect the composition of the aluminum amalgam. Take a sample at regular intervals until the mercury content meets the requirements; if the components meet the requirements, stop the heating of the evaporator 3 and close the valve of the first pipeline 5, and open the valve of the third pipeline 7 to make the mercury inert. The gas directly enters the feed pipe, and maintains the delivery of clean, high-temperature inert gas for 3-5 minutes until the liquid level of the aluminum soup drops to out of contact with the feed pipe;

In this embodiment, the inert gas is always fed into the furnace through the feed pipe during the process of putting aluminum;

Step 11: When the temperature of the aluminum outlet reaches 660°C or higher, the aluminum amalgam produced in the reaction furnace 8 is vented and casted, and the production of the hydrogen production material is completed.

This embodiment discloses an inert gas bubbling mercury injection method for preparing aluminum amalgam. The inert gas is used as the protective gas, and after the mercury is heated by the evaporator 3 to form mercury vapor, it passes through the second pipeline 6 and the lower end The feed pipe inserted below the liquid level of the reaction furnace 8 is passed into the interior of the aluminum soup, and the carried mercury vapor is diffused into the aluminum soup by bubbling to complete the preparation of the aluminum amalgam. Since mercury enters the molten aluminum soup in the form of vapor, the whole process is safe and controllable, and mercury bumping does not occur. In this embodiment, under the double action of bubbling and stirring, aluminum amalgam with relatively uniform composition can be obtained.

In this embodiment, the inert gas used is a gas with stable properties below 700° C. and which is not easy to react with aluminum. The inert gas used is nitrogen or inert gas.

In this embodiment, the rated operating temperatures of the preheater 2, the evaporator 3 and the heaters of the second pipeline 6 are all set above the boiling point of the mercury raw material.

In this embodiment, the second pipeline 6 is a seamless pipe made of 310S or 316L material.

In this embodiment, heaters are provided on the first pipeline 5 , the second pipeline 6 and the third pipeline 7 , and the heaters are cast copper heating rings or ceramic heating rings.

In this embodiment, the feed pipe is made of a material with a temperature resistance not lower than 700° C. and not easily corroded by aluminum water, preferably graphite. The lower end of the feed tube was located below the liquid level of the aluminum soup and 1 cm from the bottom of the furnace. The lower end of the feed pipe is provided with an opening, and a plurality of through holes are opened on the side wall of the lower part of the feed pipe.

In this description, specific examples are used to illustrate the principle and implementation of the present invention. The description of the above embodiments is only used to help understand the method and core idea of the present invention; meanwhile, for those of ordinary skill in the art, according to this The idea of the invention will have changes in the specific implementation and scope of application. In summary, the contents of this specification should not be construed as limiting the present invention.

Claims (10)

1. A preparation method of an aluminum amalgam for conveying mercury in an inert gas bubbling mode is characterized by comprising the following steps: the method comprises the following steps:

step one, building a bubbling type mercury-conveying aluminum amalgam preparation device;

calculating the amount of the required mercury raw material according to the mass of the aluminum put into the reaction furnace at one time, and calculating the amount and the flow of the inactive gas required for conveying mercury according to the preparation time requirement;

step three, putting the weighed aluminum into a smelting furnace for smelting;

putting the weighed mercury raw materials into an evaporator, and checking the air tightness of a second pipeline from the evaporator to the reaction furnace;

step five, opening a valve on a third pipeline of the inert gas direct reaction furnace, and temporarily closing the third pipeline of the inert gas direct reaction furnace after blowing off air in the third pipeline;

sixthly, after the aluminum is melted, removing surface oxidation slag, and transferring the aluminum in a molten state into a reaction furnace;

step seven, preserving heat of the transferred molten aluminum in the reaction furnace to enable the temperature inside the hearth of the reaction furnace to be above the melting point of the aluminum, starting a stirring structure of the reaction furnace to enable the oxidation slag deposited at the bottom of the hearth of the reaction furnace to float to the surface, and then carrying out surface slag removing treatment;

step eight, starting a preheater on the first pipeline to heat the first pipeline, simultaneously starting a heater of the second pipeline to heat and insulate the second pipeline, and starting an evaporator to heat the mercury raw material;

step nine, finishing slag skimming, enabling the inert gas to sequentially pass through the preheater and the evaporator after the temperature of the evaporator reaches a rated value, and enabling the inert gas with mercury vapor to enter molten aluminum in a hearth of the reaction furnace through a material inlet pipe of the reaction furnace;

step ten, taking a molten aluminum amalgam sample from a sampling port of the reaction furnace after the preset feeding time is reached, and detecting the components in the molten aluminum amalgam sample; if the components meet the requirements, stopping heating the evaporator, closing the valve of the first pipeline, opening the valve of the third pipeline, enabling the inert gas to directly enter the material passing pipe, and maintaining the conveying of the clean and high-temperature inert gas for a period of time;

step eleven, the aluminum amalgam prepared in the reaction furnace is cast and molded in an empty mode, and the preparation work of the hydrogen production material is finished.

2. The method for preparing an aluminum amalgam for mercury delivery by bubbling inert gas as claimed in claim 1, wherein: the bubbling type mercury-conveying aluminum amalgam preparation device comprises an inactive gas storage structure, a preheater, an evaporator, a smelting furnace and a reaction furnace, wherein the inactive gas storage structure is used for storing inactive gas, the evaporator is used for heating mercury raw materials, the smelting furnace is used for smelting aluminum, the inactive gas storage structure is connected with the preheater through a first pipeline, the preheater is connected with the evaporator through a first pipeline, the evaporator is connected with the reaction furnace through a second pipeline through a material pipe, the preheater is connected with the reaction furnace through a material pipe through a third pipeline, and the smelting furnace is connected with a feed inlet of the reaction furnace.

3. The method for preparing an inert gas bubbling mercury transport aluminum amalgam according to claim 2, wherein the method comprises the following steps: the first pipeline, the second pipeline and the third pipeline are all provided with heaters, and the heaters are cast copper heating rings or ceramic heating rings.

4. The method for preparing an inert gas bubbling mercury transport aluminum amalgam according to claim 1, wherein the method comprises the following steps: in the second step, the mercury raw material is pure mercury or mercury-containing amalgam.

5. The method for preparing an inert gas bubbling mercury transport aluminum amalgam according to claim 1, wherein the method comprises the following steps: the inert gas is a gas which has stable properties below 700 ℃ and is not easy to react with aluminum.

6. The method for preparing an aluminum amalgam for mercury delivery by bubbling inert gas as claimed in claim 5, wherein: the inert gas is nitrogen or inert gas.

7. The method for preparing an inert gas bubbling mercury transport aluminum amalgam according to claim 1, wherein the method comprises the following steps: rated working temperatures of the preheater, the evaporator and the heater of the second pipeline are all set above the boiling point of the mercury raw material.

8. The method for preparing an inert gas bubbling mercury transport aluminum amalgam according to claim 1, wherein the method comprises the following steps: the second pipeline is a seamless pipe made of 310S or 316L materials.

9. The method for preparing an inert gas bubbling mercury transport aluminum amalgam according to claim 1, wherein the method comprises the following steps: the material passing pipe is made of a material which can resist temperature not lower than 700 ℃ and is not easy to be corroded by molten aluminum.

10. The method for preparing an aluminum amalgam for mercury delivery by bubbling inert gas as claimed in claim 1, wherein: the lower end of the material passing pipe is provided with an opening, and the side wall of the lower part of the material passing pipe is provided with a plurality of through holes; the lower end of the material passing pipe is located below the liquid level of the aluminum soup and is 1cm away from the bottom of the hearth.

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