Gas-liquid-solid reaction kettle

Abstract

The utility model discloses a gas-liquid-solid reaction kettle which comprises a reaction kettle body, a driving device arranged on the reaction kettle body, a kettle liquid lifting device used for lifting reaction liquid upwards, a liquid throwing and sucking device used for throwing the lifted liquid outwards, a filtering device used for filtering the liquid, a filtrate collecting loop and a gas-liquid separation tank. According to the utility model, liquid mixed with powder or fine particles is ingeniously circulated in the reaction kettle and is dispersed into extremely small particle sizes, so that feed gas is rapidly sucked while liquid drops are rapidly thrown out, and the gas-liquid-solid contact becomes simple and efficient. The problems that in a conventional gas-liquid-solid reaction, liquid and solid are not fully dispersed, and gas bubbles in a liquid-solid material are avoided, and contact of different phase states of the gas-liquid-solid reaction is in a macroscopic level are solved.

Description

Technical Field

[0001] The utility model belongs to the technical field of reaction kettles, in particular to a gas-liquid-solid reaction kettle. Background Art

[0002] Gas-liquid-solid reactions are widely used in the production of chemical products. For most gas-liquid-solid reactions, low mass transfer efficiency leads to slow reaction rates, large required reaction equipment, long material residence time, many side reactions, and low overall yields. For example, the traditional production process of pentachloropropane and tetrachloropropane, the raw materials for the preparation of the fourth-generation refrigerants R1234ze, R1233zd and R1234yf, has such problems. Utility Model Content

[0003] In view of the above problems, the utility model provides a reactor with high gas-liquid mass transfer efficiency, small equipment volume, short material residence time, few side reactions, high total yield and low energy consumption to solve the problems raised in the above background technology.

[0004] In order to achieve the above purpose, the utility model provides the following technical solutions:

[0005] A gas-liquid-solid reactor, comprising

[0006] The reactor body has a feed port, an air inlet and an air outlet at the top and a feed port at the bottom;

[0007] A driving device, mounted on the reactor body;

[0008] The kettle liquid lifting device is arranged in the reactor body and is connected to the driving device for lifting the liquid at the bottom of the reactor upwards;

[0009] The liquid-spinning and air-inhaling device is arranged in the reactor body, is connected to the driving device and is connected to the reactor liquid lifting device to throw the lifted liquid outwards;

[0010] The filtering device is installed along the inner wall of the reactor body and is used to filter the liquid thrown out from the liquid-throwing and air-inhaling device; when the liquid droplets mixed with powder or fine particles hit the filtering device, most of the liquid carries the powder and fine particles from the surface of the filtering device back into the reactor body, and part of the liquid flows out through the filtering device.

[0011] The filtrate collecting loop is installed along the inner wall of the reactor body and connected to the filtering device for collecting the filtrate;

[0012] The gas-liquid separation tank is arranged outside the reactor body and connected to the filtrate collection loop to store the filtrate.

[0013] Preferably, the driving device comprises a motor, a reducer and a rotating shaft, and the motor is transmission-connected to the rotating shaft via the reducer.

[0014] Preferably, the kettle liquid lifting device includes a guide tube, a lifting screw and a fixed rod, the guide tube is vertically installed through the fixed rod, the guide tube extends downward to the bottom of the reactor body, and the lifting screw is arranged in the guide tube and is connected to the lower end of the rotating shaft. The kettle liquid lifting device and the liquid-spinning and air-inhaling device are driven by a motor to rotate together, and are transferred to the liquid-spinning and air-inhaling device through the lifting screw. For powder and fine particle catalysts, additives and raw materials in liquid, the greater the difference between the density of solid and liquid, the more difficult it is to disperse them evenly. This kettle liquid lifting device can suck the liquid mixed with powder and fine particles from the bottom and lift it into the liquid-spinning and air-inhaling device through the kettle liquid lifting device, and the liquid is quickly dispersed and thrown out by centrifugal force in the liquid-spinning and air-inhaling device, and the powder and fine particles are thrown out together with the dispersed liquid droplets.

[0015] Preferably, the liquid-spinning and air-inhaling device comprises an air pipe and a filling plate, wherein the air pipe is fixed in the reactor body, the air pipe is connected to the air outlet, the filling plate is arranged below the air pipe, the filling plate is connected to the rotating shaft by transmission, the top of the filling plate is connected to the air pipe, the bottom is connected to the guide tube, and the outer peripheral side of the filling plate is provided with a liquid-spinning air port. Firstly, the liquid-spinning and air-inhaling device (such as the filling plate) can provide a very large contact area for materials of different phases; secondly, the liquid-spinning and air-inhaling device can accelerate the indirect contact and separation time of materials of different phases under the drive of a motor, and its effect is often tens, hundreds or even higher than that under normal conditions; thirdly, the droplets can be dispersed into micron-sized droplets or mist in the presence of centrifugal force, so that the contact between gas and liquid is deeper. During the rotation process, the liquid-swinging and air-absorption device generates centrifugal force to continuously throw the droplets to the surroundings. At the same time, a cavity is formed in the central area compared with the periphery of the packing disk, and the gas is sucked in from the outer edge of the packing disk. In the case of excess raw gas or gas generation, the gas is gathered in the central area of ​​the packing disk and discharged through the gas outlet. The discharged gas can be circulated externally into the reactor body for re-reaction, or the raw gas can be circulated externally after external separation treatment and then enter the reactor body for re-reaction. The generated gas is collected by the rear system.

[0016] Preferably, the bottom of the gas-liquid separation tank also has a drain port, and the top of the gas-liquid separation tank is connected to the reactor body through a gas phase balance pipe. By arranging a gas phase balance pipe at the top of the gas-liquid separation tank and the top of the reactor body, the liquid level of the gas-liquid separation tank is close to the liquid level of the loop, and the reaction liquid is collected from the bottom of the gas-liquid separation tank. During the operation, the liquid level of the gas-liquid separation tank must be controlled all the time, and the extraction volume can be reduced by controlling the liquid level of the gas-liquid separation tank to be higher. The reaction liquid is separated, and the raw materials or intermediates re-enter the reactor body through the external circulation gas phase balance pipe to participate in the reaction, and the target product and by-products are collected.

[0017] Preferably, a kettle bottom pipe aligned with and connected to the guide tube is provided at the bottom of the reactor body, a plurality of circulation ports are provided on the wall of the kettle bottom pipe, a control valve for controlling the circulation volume in the kettle is provided in the kettle bottom pipe, and a filler is provided at the bottom of the kettle bottom pipe.

[0018] Preferably, a jacket for heating or cooling is provided outside the reactor body.

[0019] Preferably, the lower part of the reactor body is in a conical structure.

[0020] Compared with the prior art, the beneficial effects of the utility model are:

[0021] The utility model ingeniously circulates the liquid mixed with powder or fine particles in the reactor and disperses them into extremely small particle sizes, so that the liquid droplets are quickly thrown out and the raw gas is rapidly sucked in, making the contact between gas, liquid and solid simple and efficient. It avoids the situation in conventional gas-liquid-solid reactions where the liquid and solid are not fully dispersed and the gas bubbles in the liquid and solid materials, so that the contact between different phases of the gas-liquid-solid reaction is at the macroscopic level. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a schematic diagram of the overall structure of the utility model;

[0023] Figure 2 for Figure 1 A magnified view of middle;

[0024] Figure 3 It is a schematic diagram of the operating status of Example 2 and Example 3;

[0025] Figure 4 This is a schematic diagram of the operating state of Example 4;

[0026] In the figure: 1. reactor body; 2. driving device; 3. reactor liquid lifting device; 4. liquid-spinning and air-inhaling device; 5. filtering device; 6. filtrate collecting loop; 7. gas-liquid separation tank; 8. jacket; 9. control valve; 10. stuffing; 11. feeding port; 12. air inlet; 13. air outlet; 14. feeding port; 15. reactor bottom pipe; 16. circulation port; 21. motor; 22. reducer; 23. rotating shaft; 31. guide tube; 32. lifting screw; 33. fixing rod; 41. air pipe; 42. stuffing tray; 43. liquid-spinning air port; 71. liquid discharge port; 72. gas phase balance pipe. DETAILED DESCRIPTION

[0027] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments in the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0028] Example 1

[0029] See also Figure 1 and Figure 2 This embodiment relates to a gas-liquid-solid reactor, which includes

[0030] The reactor body 1 has a feeding port 11, an air inlet 12 and an air outlet 13 at the top and a feeding port 14 at the bottom; the feeding port 11 is used for feeding powder or fine granular material, a jacket 8 for heating or cooling the reactor body 1 is provided outside the reactor body 1, and the lower part of the reactor body 1 is a conical structure.

[0031] The driving device 2 is installed on the reactor body 1 and includes a motor 21 , a reducer 22 and a rotating shaft 23 . The motor 21 is connected to the rotating shaft 23 through the reducer 22 .

[0032] The kettle liquid lifting device 3 is arranged in the reactor body 1 and is transmission-connected to the driving device 2 for lifting the liquid at the bottom of the reactor body 1 upwards; the kettle liquid lifting device 3 includes a guide tube 31, a lifting screw 32 and a fixing rod 33, the guide tube 31 is vertically installed through the fixing rod 33, the guide tube 31 extends downward to the bottom of the reactor body 1, and the lifting screw 32 is arranged in the guide tube 31 and is transmission-connected to the lower end of the rotating shaft 23.

[0033] The liquid-spinning and air-inhaling device 4 is arranged in the reactor body 1, and is connected to the driving device 2 and communicated with the reactor liquid lifting device 3 for throwing the lifted liquid outward; the liquid-spinning and air-inhaling device 4 comprises an air pipe 41 and a filling plate 42, the air pipe 41 is fixed in the reactor body 1, the air pipe 41 is communicated with the air outlet 13, the filling plate 42 is arranged below the air pipe 41, the filling plate 42 is connected to the rotating shaft 23, the top of the filling plate 42 is communicated with the air pipe 41 for exhaust, and the bottom is communicated with the guide tube 31, and the outer peripheral side of the filling plate 42 is provided with a liquid-spinning air port 43. When the motor 21 rotates, the lifting screw 32 and the filling plate 42 rotate synchronously.

[0034] The filtering device 5 is installed along the inner wall of the reactor body 1 and is used to filter the droplets thrown out from the liquid-throwing and air-absorbent device 4; when the droplets mixed with powder or fine particles hit the filtering device 5, most of the liquid carries the powder and fine particles from the surface of the filtering device 5 back into the reactor body 4, and part of the liquid flows out through the filtering device 5.

[0035] The filtrate collecting loop 6 is installed along the inner wall of the reactor body 1 and connected to the filtering device 5 for collecting the filtrate;

[0036] The gas-liquid separation tank 7 is arranged outside the reactor body 1 and connected to the filtrate collecting loop 6 for storing the filtrate.

[0037] In the present application, the kettle liquid lifting device 3 and the liquid-spinning air-inhaling device 4 are driven to rotate together by the motor 21, and the solid liquid is transferred to the liquid-spinning air-inhaling device 4 through the lifting screw 32. For powder and fine particle catalysts, additives and raw materials in liquid, the greater the difference between the solid and liquid density, the more difficult it is to disperse them uniformly. The kettle liquid lifting device 3 can suck the liquid mixed with powder and fine particles from the bottom and lift it through the kettle liquid lifting device 3 to the liquid-spinning air-inhaling device 4, and the liquid-spinning air-inhaling device 4 quickly disperses and throws out the powder and fine particles together with the dispersed liquid droplets.

[0038] First, the liquid-spinning and air-inhaling device 4 can provide a very large contact area for materials of different phases; secondly, the liquid-spinning and air-inhaling device 4 can accelerate the indirect contact and separation time of materials of different phases under the drive of the motor 21, and its effect is often tens, hundreds or even higher than that under normal conditions; thirdly, the droplets can be dispersed into micron-sized droplets or mist under the existence of centrifugal force, so that the contact between gas and liquid is deeper. During the rotation process, the liquid-spinning and air-inhaling device 4 generates centrifugal force to continuously throw the droplets around, and at the same time, the central area forms a cavity compared with the outer periphery of the packing disk 42, and the gas is sucked from the outer edge of the packing disk 42. For excessive raw gas or gas generation, the gas is collected in the central area of ​​the packing disk 42 and discharged through the air pipe 41 and the gas outlet 13. The discharged gas can enter the reactor body 1 through external circulation for re-reaction, or the raw gas can enter the reactor body 1 through external circulation for re-reaction after external separation treatment, and the generated gas is collected by the rear system.

[0039] In the embodiment of the present application, the bottom of the gas-liquid separation tank 7 also has a drain port 71, and the top of the gas-liquid separation tank 7 is connected to the reactor body 1 through a gas phase balance pipe 72. By setting the gas phase balance pipe 72 at the top of the gas-liquid separation tank 7 and the top of the reactor body 1, the liquid level of the gas-liquid separation tank 7 is close to the liquid level of the filtrate collection loop 6, and the reaction liquid is collected from the bottom of the gas-liquid separation tank 7. During the operation, the liquid level of the gas-liquid separation tank 7 must be controlled all the time, and the extraction volume can be reduced by controlling the liquid level of the gas-liquid separation tank 7 to be higher. The reaction liquid is separated, and the raw materials or intermediate products re-enter the reactor body 1 through the external circulation gas phase balance pipe 72 to participate in the reaction, and the target product and by-products are collected.

[0040] In addition, a bottom pipe 15 aligned with and connected to the guide tube 31 is provided at the bottom of the reactor body 1, and a plurality of circulation ports 16 are provided on the wall of the bottom pipe 15. The reaction liquid and solid particles in the reactor body 1 enter the bottom pipe 15 from the circulation ports 16, and then are lifted upward by the lifting screw 32. A control valve 9 for controlling the circulation amount in the reactor is provided in the bottom pipe 15, and a packing 10 is provided at the bottom of the bottom pipe 15. The packing 10 in the present application is made of foamed nickel.

[0041] Principle of the utility model

[0042] Liquid raw materials / solvents / priming materials and powders or fine particles are added to the reactor body 1, stirring is started, and the speed is adjusted to a certain level. A heating or cooling medium is passed through the jacket 8 to control the reaction start-up conditions, and the gas phase material is introduced to start the reaction. At the same time, fresh liquid raw materials are added from the bottom feed port 14 in a certain proportion according to the consumption rate of the gas material. The liquid product is extracted from the bottom of the gas-liquid separation tank 7. The excess raw materials or intermediate products in the liquid are separated by the rear system and then circulated back to the reactor body 1 to continue the reaction, and the purified products are collected; if all the gases introduced participate in the reaction, there is no need to discharge the gas during the reaction process. For reactions with excess gas raw materials or gas generation, or reactions with excess raw gas and gas generation, it is necessary to collect from the gas outlet 13, and the excess raw gas is directly circulated back to the reactor body 1 or the raw gas is separated and circulated back to the reactor body 1. The materials in the reactor body 1 include liquid, powder or fine particles, which are continuously rotated and transported to the central area of ​​the liquid-sweeping and air-inhaling device 4, and then thrown to the surroundings under the action of centrifugal force. During the process of being thrown out, they are forced to contact with the gas sucked in through the filler or sieve plate, and the thrown out droplets are dispersed into small droplets of micron size under the action of rapid centrifugal force. The closer to the outside of the filler disk 42, the smaller the droplet diameter, and the more sufficient the gas-liquid-solid contact. When the thrown out droplets hit the filter device 5, a large amount of liquid, powder and fine particles fall from the surface into the reactor of the reactor body 1. With the large inclination angle of the cone, the powder and fine particles are brought to the bottom and re-enter the kettle liquid lifting device 3 for internal circulation. Some liquid will flow into the filtrate collection loop 6 through the filter device 5. The function of the filler is to prevent the iron powder or fine particles from settling, and to keep the iron powder or fine particles suspended through the fresh material or circulating material at the bottom and then be transported upward by the kettle liquid lifting device 5. The purpose of the fixing rods 33 is to fix the guide tube 31 of the kettle liquid lifting device 3 to make it stable and not shake. Three or four fixing rods 33 can be evenly arranged around the guide tube 31.

[0043] Example 2

[0044] like Figure 3As shown, the preparation process of pentachloropropane is taken as an example. The white arrows in the figure indicate the gas flow direction, the black arrows indicate the kettle liquid flow direction, and the black dots indicate the droplets. Carbon tetrachloride preheated to the reaction temperature is added to the reactor body 1, and then additives such as (tributyl phosphate, triethyl phosphate) and iron powder are added. Stirring is turned on to circulate the kettle material, and gaseous vinyl chloride is continuously introduced from the air inlet 12. The amount of vinyl chloride feed is controlled to be lower than the ratio required for the reaction to make it react completely. Fresh carbon tetrachloride is continuously pumped in from the feed port 14, and pentachloropropane and excess carbon tetrachloride are continuously extracted from the discharge port 71 of the gas-liquid separation tank 7. After the system separates carbon tetrachloride from pentachloropropane, this part of carbon tetrachloride is circulated and continuously pumped into the reactor from the feed port 14. Pentachloropropane is collected after separation.

[0045] Example 3

[0046] like Figure 3 As shown, the preparation process of tetrachloropropane is taken as an example. In the figure, the white arrow indicates the gas flow direction, the black arrow indicates the kettle liquid flow direction, and the black dots indicate the droplets. Carbon tetrachloride preheated to the reaction temperature is added to the reactor body 1, and then the additives such as (tributyl phosphate, triethyl phosphate) and iron powder are added, and the stirring is turned on to circulate the kettle material. Gas phase ethylene is continuously introduced from the air inlet 12, and the ethylene feed amount is controlled to be lower than the ratio required for the reaction to make it react completely. Fresh carbon tetrachloride is continuously pumped in from the feed port 14, and tetrachloropropane and excess carbon tetrachloride are continuously extracted from the discharge port 71 of the gas-liquid separation tank 7. After the system separates carbon tetrachloride from tetrachloropropane, this part of carbon tetrachloride is circulated and continuously pumped into the reactor from the feed port 14. Tetrachloropropane is collected after separation.

[0047] Example 4

[0048] like Figure 4 The figure shows a state where the circulation amount in the reactor body 1 is relatively small. If the circulation amount in the reactor body 1 needs to be adjusted, the upper and lower positions of the valve core of the control valve 9 can be adjusted by rotating the hand wheel. The control valve 9 blocks the circulation port 16 to limit the feed amount of the tank wall of the bottom pipe 15, thereby controlling the feed amount entering the guide tube 31.

[0049] It is obvious to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be regarded as exemplary and non-restrictive from any point of view, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention. Any reference numeral in a claim should not be regarded as limiting the claim to which it relates.

Claims

1. A gas-liquid-solid reactor, characterized in that: It includes The reactor body has a feed port, an air inlet and an air outlet at the top and a feed port at the bottom; A driving device, mounted on the reactor body; The kettle liquid lifting device is arranged in the reactor body and is transmission-connected with the driving device to lift the liquid at the bottom of the reactor body upwards; The liquid-spinning and air-inhaling device is arranged in the reactor body, is connected to the driving device and is connected to the reactor liquid lifting device to throw the lifted liquid outwards; A filtering device is installed along the inner wall of the reactor body and is used to filter the liquid droplets thrown out from the liquid-throwing and air-absorbent device; The filtrate collecting loop is installed along the inner wall of the reactor body and connected to the filtering device for collecting the filtrate; The gas-liquid separation tank is arranged outside the reactor body and connected to the filtrate collection loop.

2. The gas-liquid-solid reactor according to claim 1, characterized in that: The driving device comprises a motor, a reducer and a rotating shaft, and the motor is transmission-connected to the rotating shaft via the reducer.

3. The gas-liquid-solid reactor according to claim 2, characterized in that: The kettle liquid lifting device includes a guide tube, a lifting screw and a fixed rod. The guide tube is vertically installed through the fixed rod and extends downward to the bottom of the reactor body. The lifting screw is arranged in the guide tube and is transmission-connected to the lower end of the rotating shaft.

4. The gas-liquid-solid reactor according to claim 3, characterized in that: The liquid-spinning and air-inhaling device comprises an air pipe and a filling plate. The air pipe is fixed in the reactor body, the air pipe is connected to the air outlet, the filling plate is arranged below the air pipe, the filling plate is connected to the rotating shaft by transmission, the top of the filling plate is connected to the air pipe, and the bottom is connected to the guide tube. The outer peripheral side of the filling plate is provided with a liquid-spinning air outlet.

5. The gas-liquid-solid reactor according to claim 1, characterized in that: The bottom of the gas-liquid separation tank is also provided with a liquid discharge port, and the top of the gas-liquid separation tank is connected with the reactor body through a gas phase balance pipe.

6. The gas-liquid-solid reactor according to claim 3, characterized in that: The bottom of the reactor body is provided with a bottom pipe aligned with and connected to the guide tube, a plurality of circulation ports are opened on the wall of the bottom pipe, a control valve for controlling the circulation volume in the reactor is arranged in the bottom pipe, and a filler is arranged at the bottom of the bottom pipe.

7. The gas-liquid-solid reactor according to claim 1, characterized in that: The outside of the reactor body is provided with a jacket for heating or cooling.

8. The gas-liquid-solid reactor according to claim 1, characterized in that: The lower part of the reactor body is in a conical structure.

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