CN101543736A - Visualization device for preparing gas hydrate in a spraying way - Google Patents

Abstract

The invention discloses a visualization device for preparing gas hydrate by spraying, which comprises a gas circulation loop, a reaction water circulation loop, a refrigerant liquid circulation loop, a jet reactor and a refrigerant constant temperature box. A gas pressure reducing valve, a gas cylinder and an air compressor are connected before the gas booster pump, a vacuum pump and a pressure gauge are connected outside the buffer tank; a plunger pump, a liquid flow meter, valves, a reactor and a storage tank are connected to the reaction water circulation circuit , the plunger pump is connected to a water tank and a valve; the refrigerant liquid circulation circuit is equipped with a low-temperature constant temperature tank, which can provide refrigerant liquid for buffer tanks, storage tanks and refrigerant constant temperature boxes; the invention can fully contact and mix the gas and reaction water before spraying Atomization can increase the gas-water contact area, shorten the induction time of hydration reaction, greatly increase the formation rate of gas hydrate, and realize the rapid formation of gas hydrate. It is an efficient device for preparing gas hydrate.

Description

A visualization device for gas hydrate preparation by spraying

technical field

The invention relates to a gas-liquid dispersion technology for synthesizing gas hydrates, in particular to a visualization device for preparing gas hydrates by jetting.

Background technique

Gas hydrate is a kind of cage-type enveloping crystal formed by certain gases (or volatile liquids) and water under low temperature and high pressure conditions. Different gases require different temperature and pressure conditions to form gas hydrates, and the types of gas hydrates formed are also different. Gas hydrates have the characteristics of large gas storage capacity, convenient transportation, and safe use. However, the technology for synthesizing gas hydrates is not yet mature, especially for gases that are difficult to form hydrates. The temperature and pressure conditions are not easy to control, and the hydration rate is also very slow. It is difficult to improve, so the application of this technology urgently needs a device for efficiently producing gas hydrate.

At present, there are four main techniques for preparing gas hydrates: static contact method, porous media filling method, bubble disturbance method and mechanical stirring method. (1) The static contact method is to directly contact the gas-liquid two phases at the phase interface without disturbance, and the gas diffuses into the water through the phase interface, undergoes crystal nucleation and growth, and finally forms a gas hydrate. (2) The porous media filling method is a technology that uses porous media to accelerate the formation of gas hydrates. The gas is passed into the porous media to increase the gas-liquid contact area and quickly generate gas hydrates. (3) The bubble disturbance method is to make the gas pass through the orifice in the reactor to generate bubbles. The bubbles rise and break in the water continuously, increasing the solubility of the gas in the water and shortening the hydration induction time, thereby accelerating the nucleation and growth of hydrates. (4) The mechanical stirring method is to install a stirrer in the reactor, which can accelerate the dissolution of gas in water, promote the full contact of gas and water, shorten the hydration induction time, and increase the hydration rate. There is also a method of combining the bubble disturbance method and the mechanical stirring method, which is to install an orifice plate and a stirrer in the reactor at the same time, which can further increase the contact area between gas and water and accelerate the formation of gas hydrate.

However, the above methods have disadvantages: ①The contact area between gas and water is very limited, which greatly affects the formation rate of gas hydrate; ②The synthesis of gas hydrate is not continuous, and the continuous generation of hydrate prevents the gas from hydrate The diffusion increases the blowing power and stirring power, which is not recommended economically; ③The thermal effect generated during mechanical stirring will inevitably affect the hydration conditions.

Contents of the invention

The purpose of the present invention is to overcome the shortcomings of the prior art, and to provide a visual device for preparing gas hydrate by spraying. The gas-liquid mixture is sprayed simultaneously to form a mist flow or foam flow, which increases the solubility of gas in water and increases the The gas-liquid contact area shortens the hydration induction time, which can realize the efficient and rapid generation of hydrates. At the same time, the state and reaction of the mixed fluid can be observed by using the visualization window.

The object of the present invention is achieved through the following technical solutions.

A device for efficiently preparing gas hydrates by visual spraying includes a gas circulation loop, a reaction water circulation loop, a refrigerant liquid circulation loop, a reactor, and a refrigerant constant temperature box.

A visualization device for preparing gas hydrate by spraying, including a gas circulation loop, a reaction water circulation loop, a refrigerant liquid circulation loop, a reactor and a refrigerant constant temperature box, wherein:

The gas circulation loop is connected with a gas cylinder 1, a gas booster pump 4, a buffer tank 5, a storage tank 9 and a water eliminator 8, and the gas circulation loop is connected to the gas inlet 37 of the reactor 7 through a pipeline, and in the reactor 7 The unreacted gas enters the storage tank 9 through the gas-liquid outlet 38 of the reactor 7, then returns to the gas booster pump 4 of the gas circulation circuit through the water eliminator 8, and finally uses the air compressor 3 to press into the buffer tank 5 for recycling;

The reaction water circulation loop is connected with a water tank 11, a plunger pump 12 and a storage tank 9, and the reaction water circulation loop is connected to the reaction water inlet 36 of the reactor 7 through a pipeline, and the unreacted water in the reactor 7 flows in from the gas-liquid outlet 38 In storage tank 9, pressurize to reactor 7 through plunger pump 12 and circulate then;

The low temperature constant temperature tank 10 is provided on the refrigerant liquid circulation circuit, and the low temperature constant temperature tank 10 provides the circulating refrigerant liquid for the buffer tank 5, the storage tank 9 and the refrigerant constant temperature box 29, and the buffer tank 5, the storage tank 9 and the reaction Device 7 carries out constant temperature control;

The needle valve 35 for adjusting the area of the nozzle 30 is provided in the water inlet pipe of the reactor 7, and the needle valve 35 is screwed forward by rotating the valve handle of the needle valve 35, and the gap between the needle head and the nozzle 30 is gradually reduced, and then To control the flow rate of incoming water, the reactor is provided with a gas inlet 37 communicating with the entrainment chamber 31, and the entrainment chamber 31 and the throat pipe 32 as well as the throat pipe 32 and the diffusion pipe 33 are connected as one by welding; the end of the throat pipe 32 is equipped with a flow A controller 39, an oval glass window 34 is provided at the diffuser 33;

The reactor 7 is placed in a refrigerant constant temperature box 29, and a glass window is opened on the front side of the refrigerant constant temperature box 29, corresponding to the window 34 on the reactor 7, for easy observation.

The gas is entrained by the high-pressure reaction water into the entrainment chamber 31 of the reactor 7, the gas-liquid is mixed at the throat 32, and finally sprayed and atomized at the diffuser 33 by the flow controller 39, under high-pressure and low-temperature environment Gas hydrates are formed.

The diffusion tube 33 of the reactor 7 is provided with a window 34 to observe the atomization effect and hydration condition in the reactor.

The end of the throat pipe 3 of the reactor 7 is connected to the flow controller 12 by threads, and the diameter of the end of the throat pipe 3 can be changed by replacing the flow controller 12 .

The entrainment chamber 31, throat 32 and diffuser 33 of the reactor 7 are equipped with temperature sensors (40, 41, 42) and pressure sensors (43, 44, 45) to measure the temperature and pressure everywhere.

Air valves (19, 21, 23), check valves (24, 25) and gas flowmeters (26, 27) are also installed on the gas circulation loop; valves (13, 16) are also installed in the reaction water circulation loop. , 17, 18) and liquid flow meter 28.

A vacuum pump 6 and a pressure gauge are connected to the branch of the buffer tank 5 .

The pipelines connecting the gas booster pump 4 and the plunger pump 12 are respectively provided with a gas safety valve 20 and a liquid safety valve 15 .

The buffer tank 5 is equipped with a refrigerant jacket externally, the storage tank 9 has a built-in refrigerant coil, and the stainless steel jacket of the refrigerant constant temperature box 29 has a built-in insulation cotton.

The operation steps of the whole device are: ① Turn on the vacuum pump 6 to realize the vacuum degree required by the buffer tank 5, the reactor 7, the storage tank 9 and each gas pipeline; ② Start the refrigerant liquid circulation loop to control the buffer tank 5 and the reactor 7 and the temperature of the storage tank 9; 3. Utilize the air compressor 3 and the gas booster pump 4 to pressurize the gas in the gas cylinder 1 into the buffer tank 5 to reach the required pressure (about 10MPa), and release part of the gas from the buffer tank 5 to In the reactor 7 and storage tank 9, then close the gas cylinder 1, so that the gas in the storage tank 9 is pressurized by the gas booster pump 4 into the buffer tank 5 to realize the gas circuit circulation; ④ appropriate amount of reaction water is passed through the plunger pump from the water tank 11 12 After pressurization, it is ejected through the nozzle 30 of the reactor 7, and the gas entrained in the entrainment chamber 31, after the gas and the reaction water are initially mixed, exchange energy and mass at the reactor throat 32 (including those caused by temperature differences) heat exchange), and finally spray and atomize at the diffusion tube 33, after the atomized mist drops and gas are fully contacted, the gas pressure in the reactor 7 is increased under low temperature conditions, and in a short time it can be seen in the window 34 Hydrate crystals are formed. The needle valve 35 on the reactor 7 can control the area of the nozzle 30, and then control the amount of reaction water entering; the end of the throat pipe 32 of the reactor 7 is equipped with a flow controller 39, which can change the diameter of the end aperture of the throat pipe 32; the outside of the reactor 7 The refrigerant constant temperature box 29 carries out constant temperature control on the interior of the reactor, and at the same time, the heat released in the hydration reaction process will be exchanged. The stainless steel jacket of the refrigerant constant temperature box has built-in insulation cotton; the gas circulation circuit is equipped with gas flowmeters (26, 27) Monitor the gas flow; the reactor 7 nozzle 30, the throat 32, and the diffuser 33 are equipped with temperature and pressure sensors to measure the reaction conditions; The dehumidification of the gas coming out in 9; the gas booster pump 4 and the plunger pump 12 are respectively provided with a gas safety valve 20 and a liquid safety valve 15 to prevent damage to the equipment caused by excessive air pressure or water pressure.

A visualization device for spraying and preparing gas hydrates of the present invention has the following characteristics:

(1) A glass window 34 is provided at the diffuser tube 33 of the reactor 7 to observe the atomization effect and hydration condition in the reactor 7 .

(2) A needle valve 25 is provided at the nozzle 30 of the reactor 7 to adjust the area of the nozzle 30, thereby controlling the amount of reaction water entering.

(3) The end of the throat 32 of the reactor 7 is equipped with a flow controller 39, which can change the diameter of the end of the throat 32.

(4) There are gas booster pumps 4, buffer tanks 5, gas valves (19, 21, 23), gas flow meters (26, 27), check valves (24, 25) and water eliminators 8 on the gas circulation circuit .

(5) There are plunger pump 12 , valves ( 13 , 16 , 17 , 18 ), liquid flow meter 28 and storage tank 8 in the reaction water circulation circuit.

(6) The low temperature constant temperature bath 9 can control the temperature of the buffer tank 5 , the reactor 7 and the storage tank 9 .

(7) The buffer tank 5 has an external refrigerant jacket, the storage tank 9 has a built-in refrigerant coil, and the refrigerant constant temperature box 29 has a jacket with built-in insulation cotton.

(8) The gas booster pump 4 and the plunger pump 12 are respectively provided with a gas safety valve 20 and a liquid safety valve 15 .

Compared with the prior art, the present invention has the following advantages and beneficial effects:

The existing jet atomization technology for preparing hydrate only sprays and atomizes the liquid, and then contacts and mixes it with the gas, and the flow rate of the influent liquid cannot be controlled, and the atomization effect and hydration reaction cannot be observed. A visualization device for preparing gas hydrate by spraying in the present invention, entrains gas through liquid, and then sprays the gas-liquid mixture simultaneously to form mist flow or foam flow, which can increase the solubility of gas in water and increase the contact area of gas and liquid , shortening the hydration induction time and increasing the hydration rate, etc., the effect is more obvious than that of the existing technology, and the efficient and rapid generation of hydrate can be realized. The design of the visualization window of the present invention realizes the observation of the state and reaction of the mixed fluid, and the camera and image processing software can be used to analyze the size of its foam or droplet, and then study its atomization effect and reaction rate, and improve the hydration reaction rate .

Description of drawings

Fig. 1 is the structural representation of device of the present invention;

Fig. 2 is a structural diagram of the reactor of the device of the present invention.

Gas cylinder 1, gas pressure reducing valve 2, air compressor 3, gas booster pump 4, buffer tank 5, vacuum pump 6, reactor 7, water eliminator 8, storage tank 9, low temperature constant temperature tank 10, water tank 11, column Plug pump 12, valve 13, valve 14, liquid safety valve 15, valve 16, valve 17, valve 18, gas valve 19, gas safety valve 20, gas valve 21, gas valve 22, gas valve 23, check valve 24, Check valve 25, gas flowmeter 26, gas flowmeter 27, liquid flowmeter 28, refrigerant thermostat 29, valve 18, gas valve 19, nozzle 30, entrainment chamber 31, throat 32, diffuser 33, window 34 , needle valve 35, reaction water inlet 36, gas inlet 37, gas-liquid outlet 38, flow controller 39, temperature sensor 40, temperature sensor 41, temperature sensor 42, pressure sensor 43, pressure sensor 44, pressure sensor 45.

Detailed ways

A visualization device for preparing gas hydrate by spraying, comprising a gas circulation loop, a reaction water circulation loop, a refrigerant liquid circulation loop, a jet reactor and a refrigerant constant temperature box 29 . A visualization device for preparing gas hydrate by spraying, which is characterized in that it includes a gas circulation loop, a reaction water circulation loop, a refrigerant liquid circulation loop, a reactor, and a refrigerant constant temperature box.

Reactor 7 is composed of nozzle 30, entrainment chamber 31, throat pipe 32, diffuser pipe 33, window 34 and needle valve 35, and its exterior is provided with reaction water inlet 36, gas inlet 37, gas-liquid outlet 38, temperature sensor (40,41,42) and pressure sensor (43,44,45), internal throat pipe 31 ends are equipped with flow controller 39; Gas booster pump 4, buffer tank 5, gas flowmeter ( 26, 27), air valves (19, 21, 23), check valves (24, 25), reactor 7, storage tank 9 and water eliminator 8, before gas booster pump 4, connect air compressor 3 and Gas cylinder 1, gas pressure reducing valve 2 is arranged behind gas cylinder 1, pressure gauge, gas valve 22 and vacuum pump 6 are connected outside buffer tank 5; plunger pump 12, valves (13, 16, 17 , 18), liquid flowmeter 28, reactor 7 and storage tank 9, before plunger pump 12, connect water tank 11 and valve 14 in addition; The low temperature constant temperature tank 9 is arranged on the refrigerant liquid circulation circuit, connects storage tank 9 and refrigerant constant temperature box 29; The gas booster pump 4 and the plunger pump 12 are respectively equipped with a gas safety valve 20 and a liquid safety valve 15; the gas-liquid outlet 38 is connected to the storage tank 9, and the gas flow meter 26 is equipped with a water eliminator 7.

Vacuumize the gas path: open the gas valves (19, 21, 22, 23), close the gas pressure reducing valve 2 and the valves (13, 17, 18), and turn on the vacuum pump 6 to evacuate the gas path system until the reactor 7, buffer Vacuum requirements for tank 5, storage tank 9 and each gas pipeline.

Start the refrigeration system: turn on the low temperature constant temperature tank 10 for refrigeration, and start the circulation of the refrigerant liquid, and control the temperature of the buffer tank 5, the reactor 7 and the storage tank 9.

Realize gas circulation: close gas valve (21,22) and gas decompression valve 2, open air compressor 3 and gas booster pump 4 and pressurize the gas in gas cylinder 1 into buffer tank 5, reach required pressure (10MPa left and right); open the gas valve (19,21,23), close the gas pressure reducing valve 2, valve (13,17,18), air compressor 3 and gas booster pump 4, so that 5 parts of the buffer tank gas are released to the reaction In the device 7 and the storage tank 9, the pressure of the two is controlled within the gas booster pump 4 inlet pressure range (less than 0.8MPa); the gas pressure reducing valve 2 is closed, and the air compressor 3 and the gas booster pump 4 are opened to make the storage tank The gas in 9 is pressurized by the gas booster pump 4 into the buffer tank 5 to realize the gas circulation;

Pass into high-pressure reaction water: close valve (13,17), open valve (14,16) and plunger pump 12, the water in the water tank 11 is pressurized until liquid safety valve 15 has water to overflow, then open valve 17, make The high-pressure water enters the reactor 7 through the reaction water inlet 36, sprays out at the nozzle 30, entrains and circulates the gas in the entrainment chamber 31, and after the gas and the reaction water are initially mixed, energy and mass are exchanged at the reactor throat 32. Exchange, and finally spray and atomize at the diffuser 33, after the atomized mist and gas fully contact, increase the opening of the gas valve 23 under low temperature conditions, so that the gas pressure in the reactor 7 increases to the reaction pressure (5 ~ 8MPa ), in a short period of time, it can be seen that hydrate crystals are generated in the window 34.

In addition, the area of the nozzle 30 can be controlled by adjusting the needle valve 35 on the reactor 7, thereby controlling the amount of reaction water entering; changing the flow controller 39 at the end of the throat 32 can change the aperture at the end of the throat 32, thereby adjusting the size of the droplet particle size. path. The temperature and pressure conditions of the hydration reaction process can be measured by the temperature sensors (40, 41, 42) and pressure sensors (43, 44, 45) at the entrainment chamber 31, the throat pipe 32 and the diffusion pipe 33 of the reactor 7.

In the process of preparing hydrate, the device can add gas through the gas cylinder 1 and add reaction water through the water tank 11; the unreacted gas can enter the storage tank, and circulate back to the gas booster pump 4 through the water eliminator 8, The unreacted water can be stored in the storage tank 9, and the water in the storage tank 9 can be pressurized and circulated by the plunger pump 12 while the valve 14 is closed and the valve 13 is opened.

The design of the visualization window of the present invention realizes the observation of the state of the mixed fluid and the reaction situation, and the atomization of the mixture in the reactor can be clearly seen through the window, and the order of magnitude of the particle size of the foam or droplet is analyzed by using a high-speed camera and image processing software At 10-10 ² μm, it is lower than the droplet size of 10 ^{2-10 3} μm formed by spraying in the prior art; when conducting the CH ₄ hydrate experiment, the temperature and pressure data are collected by the data collector, It is found that when the reaction temperature is 0-5°C and the pressure is within the range of 5-8MPa, the supercooling degree of the hydrate can be reduced to 3°C, and the induction time of the hydration experiment can be reduced to within 100-150min, which is better than the hydration in the existing stirring technology. The induction time (more than 200min) was reduced.

Claims (9)

1, a kind of visualization device that sprays the preparation gas hydrate is characterized in that, comprises gas circulation loop, reaction water closed circuit, cooling medium liquid circulating loop, reactor and refrigerant insulating box, wherein:

Described gas circulation loop is connected with gas cylinder (1), gas boosting pump (4), surge tank (5), storage tank (9) and dehydrater (8), gas circulation loop is connected to the gas feed (37) of reactor (7) by pipeline, unreacted gas enters storage tank (9) through the gas liquid outlet (38) of reactor (7) in the reactor (7), get back to the gas boosting pump (4) of gas circulation loop then through dehydrater (8), utilize air compressor (3) to be pressed into surge tank (5) at last and recycle;

Described reaction water closed circuit is connected with water tank (11), plunger displacement pump (12) and storage tank (9), the reaction water closed circuit is connected to the reaction water import (36) of reactor (7) by pipeline, unreacted water flows into the storage tank (9) from gas liquid outlet (38) in the reactor (7), is pressurized to reactor (7) through plunger displacement pump (12) then and recycles;

Described cooling medium liquid circulating loop is provided with low temperature thermostat bath (10), low temperature thermostat bath (10) is that surge tank (5), storage tank (9) and refrigerant insulating box (29) provide the circulation cooling medium liquid, by the circulation cooling medium liquid surge tank (5), storage tank (9) and reactor (7) is carried out thermostatic control;

Be provided with the needle-valve (35) of regulating nozzle (30) area in described reactor (7) inlet channel, valve handle by rotation needle-valve (35) makes needle-valve (35) precession forward, space between syringe needle and the nozzle (30) reduces gradually, and then the flow of control water inlet, reactor is provided with and entrainments the gas feed (37) that chamber (31) communicates, and entrainments chamber (31) and is connected as a single entity by welding with anemostat (33) with trunnion (32) and trunnion (32); Trunnion (32) end is equipped with Flow Control device (39), and anemostat (33) locates to have oval glass vision panel (34);

Described reactor (7) places refrigerant insulating box (29), and refrigerant insulating box (29) front side has a glass vision panel, and is corresponding with the form (34) on the reactor (7), is convenient to observe.

2, a kind of visualization device that sprays the preparation gas hydrate according to claim 1, it is characterized in that gas is entrainmented the into described chamber (31) of entrainmenting by reaction under high pressure water and locates, gas-liquid is located to mix at trunnion (32), locate jet atomization by Flow Control device (39) at anemostat (33) at last, under the high pressure low temperature environment, generate gas hydrate.

3, a kind of visualization device that sprays the preparation gas hydrate according to claim 1 is characterized in that the anemostat (33) of described reactor (7) locates to have form (34), with atomizing effect in the observing response device and hydration situation.

4, a kind of visualization device that sprays the preparation gas hydrate according to claim 1, it is characterized in that the terminal and Flow Control device (12) of the trunnion (3) of described reactor (7) is by being threaded, by changing the aperture that Flow Control device (12) changes trunnion (3) end.

5, a kind of visualization device that sprays the preparation gas hydrate according to claim 1 is characterized in that entrainment chamber (31), trunnion (32) and the anemostat (33) of described reactor (7) locates all to be equipped with temperature sensor (40,41,42) and pressure sensor (43,44,45) with measurement temperature and pressure everywhere.

6, a kind of visualization device that sprays the preparation gas hydrate according to claim 1 is characterized in that also being equipped with on the described gas circulation loop air valve (19,21,23), check-valves (24,25) and gas flowmeter (26,27); Described reaction water closed circuit also is equipped with valve (13,16,17,18) and fluid flowmeter (28).

7, a kind of visualization device that sprays the preparation gas hydrate according to claim 1 is characterized in that being connected with vavuum pump (6) and Pressure gauge on the branch road of described surge tank (5).

8, a kind of visualization device that sprays the preparation gas hydrate according to claim 1 is characterized in that the pipeline that is connected with plunger displacement pump (12) with described gas boosting pump (4) is respectively equipped with gas safety valve (20) and liquid safe valve (15).

9, a kind of visualization device that sprays the preparation gas hydrate according to claim 1 is characterized in that the external refrigerant chuck of described surge tank (5), the built-in refrigerant coil pipe of storage tank (9), the stainless steel chuck built-in heat insulation cotton of refrigerant insulating box (29).

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