Continuous preparation device for 1, 1, 1, 3, 3-pentachloropropane

Abstract

The utility model belongs to the technical field of acyclic compounds, and particularly relates to a continuous preparation device for 1, 1, 1, 3, 3-pentachloropropane, which comprises a reaction tower, a filler section arranged in an inner cavity of the reaction tower, a catalytic leakproof component arranged in the filler section, a liquid inlet pipe arranged at the top of the reaction tower, a carbon tetrachloride feeding pump connected with one end of the liquid inlet pipe, and a liquid outlet pipe connected with the other end of the liquid inlet pipe, the other end of the liquid inlet pipe penetrates through the top of the reaction tower and is connected with a first nozzle distributor, a first gas inlet pipe and a second gas inlet pipe are arranged on the side wall of the reaction tower, and one end of the first gas inlet pipe and one end of the second gas inlet pipe penetrate through the side wall of the reaction tower and are connected with a first gas distributor and a second gas distributor respectively. The other end of the first gas inlet pipe and the other end of the second gas inlet pipe are jointly connected with a gas inlet header pipe, the end, away from the second gas inlet pipe, of the gas inlet header pipe is connected with a vinyl chloride metering pump, and a circulation pipeline is arranged on the side wall of the reaction tower. According to the device, continuous and stable operation from raw material input to product output can be achieved, and the overall production efficiency is improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of acyclic compounds, and specifically relates to a continuous preparation device for 1,1,1,3,3-pentachloropropane. Background Art

[0002] As an acyclic compound, 1,1,1,3,3-pentachloropropane has a wide range of application needs. In the preparation of refrigerants, 1,1,1,3,3-pentachloropropane is a key intermediate for the synthesis of a variety of chlorine-containing organic compounds. It can generate refrigerants with specific properties through chemical reactions or replacement of functional groups. In terms of solvent applications, 1,1,1,3,3-pentachloropropane has excellent solubility and can be used as a solvent in the production of special coatings and inks to adjust viscosity, make the product adhere evenly and firmly, and improve the quality of coatings and printed products. In agriculture, 1,1,1,3,3-pentachloropropane is a raw material for pesticide synthesis and can be made into special-effect pesticides after participating in the reaction.

[0003] Chinese patent CN220467857U discloses a 1,1,1,3,3-pentachloropropane synthesis device, including a preheating reactor, a high-pressure reactor, a flash tank, a first distillation tower and a second distillation tower; the preheating reactor is connected to the high-pressure reactor, the high-pressure reactor is connected to the flash tank, the flash tank is connected to the first distillation tower, and the first distillation tower is connected to the second distillation tower; a filter is arranged between the high-pressure reactor and the flash tank; the flash tank is connected to the preheating reactor; the first distillation tower is connected to the preheating reactor. The above patent can avoid the catalyst from being deposited in the pipeline, but the operation process is cumbersome, and each batch of production requires a lot of manpower, which cannot meet the needs of large-scale production. Utility Model Content

[0004] The utility model aims to provide a 1,1,1,3,3-pentachloropropane continuous preparation device, which can realize continuous and stable operation from raw material input to product output, avoid manpower waste caused by frequent start and stop, improve overall production efficiency, and prevent catalyst deposition from clogging pipelines, thereby ensuring long-term stable operation of the equipment.

[0005] To achieve the above purpose, the technical solution of the utility model is:

[0006] The 1,1,1,3,3-pentachloropropane continuous preparation device comprises a reaction tower, wherein the inner cavity of the reaction tower is provided with a plurality of packing sections, the packing sections are provided with catalytic leak-proof components, a liquid inlet pipe is provided at the top of the reaction tower, one end of the liquid inlet pipe is connected to a carbon tetrachloride feed pump, the other end of the liquid inlet pipe penetrates the top of the reaction tower and is connected to a nozzle distributor 1, an air inlet pipe 1 and an air inlet pipe 2 are provided on the side wall of the reaction tower, one end of the air inlet pipe 1 and one end of the air inlet pipe 2 penetrate the side wall of the reaction tower and are connected to a gas distributor 1 and a gas distributor 2 respectively, the other end of the air inlet pipe 1 and the other end of the air inlet pipe 2 are commonly connected to an air inlet main pipe, one end of the air inlet main pipe away from the air inlet pipe 2 is connected to a vinyl chloride metering pump, a circulation pipeline is provided on the side wall of the reaction tower away from the air inlet pipe 1, one end of the circulation pipeline penetrates the upper part of the side wall of the reaction tower and is connected to the nozzle distributor 2, and the other end of the circulation pipeline is connected to the lower part of the side wall of the reaction tower.

[0007] in:

[0008] The liquid inlet pipe is provided with a preheater 1, which is located between the carbon tetrachloride feed pump and the reaction tower, and the end of the carbon tetrachloride feed pump away from the preheater 1 is connected to the carbon tetrachloride storage tank; the air inlet main pipe is provided with a preheater 2, which is located between the vinyl chloride metering pump and the reaction tower, and the end of the vinyl chloride metering pump away from the preheater 2 is connected to the vinyl chloride storage tank.

[0009] The circulation pipeline is provided with a preheater three, and a circulation pump is provided between the preheater three and the reaction tower.

[0010] The top of the reaction tower is provided with an air outlet pipe, and a gas cooler is provided on the air outlet pipe.

[0011] A discharge pipe is arranged at the bottom of the reaction tower, one end of the discharge pipe away from the reaction tower is connected to a product storage tank, and a discharge pump is arranged on the discharge pipe.

[0012] The catalytic leak-proof component comprises a leak-proof mesh bag, and a solid catalyst is arranged inside the leak-proof mesh bag.

[0013] The gas distributor 1 is located in the middle of the inner cavity of the reaction tower. The gas distributor 1 includes three groups of air inlet branch pipes 1 arranged in parallel with each other. Both ends of the air inlet branch pipes 1 are sealed and both ends of the air inlet branch pipes 1 are fixedly arranged on the inner wall of the reaction tower. A cross frame 1 is arranged at the bottom of the air inlet branch pipe 1, and both ends of the cross frame 1 are fixedly arranged on the inner wall of the reaction tower.

[0014] The three groups of air intake branch pipes 1 are all connected to the air intake pipe 1, and a plurality of air distribution holes 1 are evenly arranged on the three groups of air intake branch pipes 1.

[0015] The gas distributor 2 is located at the bottom of the inner cavity of the reaction tower. The gas distributor 2 includes three groups of air intake branch pipes 2 arranged in parallel with each other. Both ends of the air intake branch pipes 2 are sealed and both ends of the air intake branch pipes 2 are fixedly arranged on the inner wall of the reaction tower. A cross frame 2 is arranged at the bottom of the air intake branch pipes 2, and both ends of the cross frame 2 are fixedly arranged on the inner wall of the reaction tower.

[0016] The three groups of air intake branch pipes 2 are all connected to the air intake pipe 2, and a plurality of air distribution holes 2 are evenly arranged on the three groups of air intake branch pipes 2.

[0017] The beneficial effects of the utility model are:

[0018] The device can achieve continuous and stable operation from raw material input to product output, avoiding the waste of manpower caused by frequent start and stop; the catalytic leak-proof component can prevent the catalyst from depositing and clogging the pipeline, ensuring the long-term stable operation of the device; gas distributor 1 and gas distributor 2 can enhance the mixing degree of gas and liquid, making the reaction more uniform; this device improves the overall production efficiency and can meet the needs of large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a schematic diagram of the structure of the utility model;

[0020] Figure 2 It is a cross-sectional schematic diagram of a reaction tower, an air inlet pipe 1 and a gas distributor 1 in the utility model;

[0021] Figure 3 It is a cross-sectional schematic diagram of the reaction tower, the second air inlet pipe and the second gas distributor in the utility model;

[0022] Figure 4 This is a schematic diagram of the structure of the leak-proof mesh bag in the utility model;

[0023] Figure 5 It is a cross-sectional schematic diagram of the catalytic leak-proof component in the utility model;

[0024] In the figure:

[0025] 1. Reaction tower; 2. Packing section; 3. Catalytic leak-proof assembly; 301. Leak-proof mesh bag; 302. Solid catalyst; 4. Liquid inlet pipe; 5. Carbon tetrachloride storage tank; 6. Nozzle distributor 1; 7. Air inlet pipe 1; 8. Air inlet pipe 2; 9. Gas distributor 1; 901. Air inlet branch pipe 1; 902. Horizontal frame 1; 903. Air distribution hole 1; 10. Gas distributor 2; 1001. Air inlet branch pipe 2; 1002 , horizontal frame two; 1003, air distribution hole two; 11, air inlet main pipe; 12, vinyl chloride storage tank; 13, circulation pipeline; 14, nozzle distributor two; 15, carbon tetrachloride feed pump; 16, preheater one; 17, vinyl chloride metering pump; 18, preheater two; 19, circulation pump; 20, preheater three; 21, air outlet pipe; 22, gas cooler; 23, discharge pipe; 24, discharge pump; 25, product storage tank. DETAILED DESCRIPTION

[0026] The present invention will be specifically described and illustrated below in conjunction with the embodiments.

[0027] Example 1

[0028] like Figure 1-5 As shown, the 1,1,1,3,3-pentachloropropane continuous preparation device comprises a reaction tower 1, wherein the inner cavity of the reaction tower 1 is provided with a plurality of packing sections 2, wherein the packing sections 2 are provided with a catalytic leak-proof assembly 3, wherein the top of the reaction tower 1 is provided with a liquid inlet pipe 4, wherein one end of the liquid inlet pipe 4 is connected to a carbon tetrachloride feed pump 15, wherein the other end of the liquid inlet pipe 4 penetrates through the top of the reaction tower 1 and is connected to a nozzle distributor 16, wherein the side wall of the reaction tower 1 is provided with an air inlet pipe 17 and an air inlet pipe 28, wherein one end of the air inlet pipe 17 and one end of the air inlet pipe 28 are connected to each other. A gas distributor 1 9 and a gas distributor 2 10 are respectively connected to the side walls of the reaction tower 1, the other ends of the air inlet pipe 1 7 and the other ends of the air inlet pipe 2 8 are commonly connected to an air inlet main pipe 11, the end of the air inlet main pipe 11 away from the air inlet pipe 2 8 is connected to a vinyl chloride metering pump 17, a circulation pipeline 13 is arranged on the side wall of the reaction tower 1 away from the air inlet pipe 1 7, one end of the circulation pipeline 13 penetrates the upper part of the side wall of the reaction tower 1 and is connected to a nozzle distributor 2 14, and the other end of the circulation pipeline 13 is connected to the lower part of the side wall of the reaction tower 1.

[0029] The catalytic leak-proof component 3 can prevent the catalyst from depositing and clogging the pipeline, ensuring the long-term stable operation of the device; the gas distributor 1 9 and the gas distributor 2 10 can enhance the mixing degree of gas and liquid, making the reaction more uniform.

[0030] A preheater 16 is provided on the liquid inlet pipe 4, and the preheater 16 is located between the carbon tetrachloride feed pump 15 and the reaction tower 1, and the end of the carbon tetrachloride feed pump 15 away from the preheater 16 is connected to the carbon tetrachloride storage tank 5. A preheater 2 18 is provided on the air inlet main pipe 11, and the preheater 2 18 is located between the vinyl chloride metering pump 17 and the reaction tower 1, and the end of the vinyl chloride metering pump 17 away from the preheater 2 18 is connected to the vinyl chloride storage tank 12.

[0031] Preheater 16 can preheat carbon tetrachloride liquid to accelerate the reaction rate; preheater 2 18 can preheat vinyl chloride gas to enhance the reaction activity.

[0032] A preheater 3 20 is provided on the circulation pipeline 13, and a circulation pump 19 is provided between the preheater 3 20 and the reaction tower 1. The circulation pipeline 13 realizes material recycling and optimizes the reaction process; the preheater 3 20 can reheat the circulating material to compensate for the temperature loss caused by the circulation heat dissipation.

[0033] The top of the reaction tower 1 is provided with an outlet pipe 21, and the outlet pipe 21 is provided with a gas cooler 22. The outlet pipe 21 can discharge the gas of the reaction tower 1, and then collect, separate and perform other subsequent treatments on the gas.

[0034] A discharge pipe 23 is provided at the bottom of the reaction tower 1 , and one end of the discharge pipe 23 away from the reaction tower 1 is connected to a product storage tank 25 . A discharge pump 24 is provided on the discharge pipe 23 .

[0035] The catalytic leak-proof assembly 3 includes a leak-proof mesh bag 301, and a solid catalyst 302 is arranged inside the leak-proof mesh bag 301. The leak-proof mesh bag 301 wraps the solid catalyst 302, and in the case of liquid impact, the solid catalyst 302 can be confined in the packing section 2 to prevent it from scattering into the pipeline and causing blockage.

[0036] The gas distributor 9 is located in the middle of the inner cavity of the reaction tower 1. The gas distributor 9 includes three groups of air inlet branch pipes 901 arranged in parallel with each other. Both ends of the air inlet branch pipes 901 are sealed and fixedly arranged on the inner wall of the reaction tower 1. A cross frame 902 is arranged at the bottom of the air inlet branch pipe 901, and both ends of the cross frame 902 are fixedly arranged on the inner wall of the reaction tower 1.

[0037] The three groups of air inlet branch pipes 901 are all connected to the air inlet pipe 7, and a plurality of air distribution holes 903 are evenly arranged on the three groups of air inlet branch pipes 901. The gas distributor 9 can prevent the vinyl chloride gas from concentrating in a local area of ​​the reaction tower 1, improve the reaction uniformity, and enhance the reaction efficiency.

[0038] The gas distributor 10 is located at the bottom of the inner cavity of the reaction tower 1. The gas distributor 10 includes three groups of air inlet branch pipes 1001 arranged in parallel with each other. Both ends of the air inlet branch pipes 1001 are sealed and both ends of the air inlet branch pipes 1001 are fixedly arranged on the inner wall of the reaction tower 1. A cross frame 1002 is arranged at the bottom of the air inlet branch pipes 1001, and both ends of the cross frame 1002 are fixedly arranged on the inner wall of the reaction tower 1.

[0039] The three groups of air inlet branch pipes 1001 are all connected to the air inlet pipe 8, and a plurality of air distribution holes 1003 are evenly arranged on the three groups of air inlet branch pipes 1001. The gas distributor 10 cooperates with the gas distributor 9 to improve the reaction efficiency.

[0040] Working principle and process:

[0041] 1. Raw material pretreatment:

[0042] The vinyl chloride gas is stored in the vinyl chloride storage tank 12, compressed to 0.05-0.6MPa by the vinyl chloride metering pump 17 and enters the air intake main pipe 11. The preheater 2 18 on the air intake main pipe 11 preheats the vinyl chloride gas to 40-180°C. The treated vinyl chloride gas is diverted to the air intake pipe 1 7 and the air intake pipe 2 8 through the air intake main pipe 11.

[0043] The carbon tetrachloride liquid is stored in the carbon tetrachloride storage tank 5 and transported to the reaction tower 1 through the liquid inlet pipe 4. In this process, the preheater 16 on the liquid inlet pipe 4 heats the carbon tetrachloride liquid to 40-180°C.

[0044] 2. Mixing of reactants:

[0045] The air inlet pipe 7 delivers a portion of the vinyl chloride gas to the gas distributor 9 located in the middle of the inner cavity of the reaction tower 1, and is finely dispersed into tiny bubbles through the air distribution holes 903. At this time, the carbon tetrachloride liquid sprayed from the top of the reaction tower 1 through the nozzle distributor 6 contacts the vinyl chloride gas, and the reaction starts in the reaction tower 1.

[0046] The air inlet pipe 28 delivers another part of the vinyl chloride gas to the gas distributor 2 10. After the vinyl chloride gas flows out from the air distribution hole 2 1003, it moves from bottom to top and cooperates with the gas distributor 1 9 to ensure that the gas and liquid are fully mixed.

[0047] 3. Catalytic reaction:

[0048] The leak-proof net bag 301 in the catalytic leak-proof component 3 is a net bag made of tetrafluoroethylene or nylon, the solid catalyst 302 is a divalent iron compound, and the mass of a single catalytic leak-proof component 3 is 0.1-5 kg. When the vinyl chloride gas and the carbon tetrachloride liquid flow through the packing section 2, the catalytic leak-proof component 3 promotes the vinyl chloride gas and the carbon tetrachloride liquid to react in the direction of generating 1,1,1,3,3-pentachloropropane.

[0049] 4. Cycle stage:

[0050] In the case of insufficient conversion of raw materials in a single reaction, the incompletely reacted materials are returned to the reaction tower 1 for further reaction through the circulation pipeline 13. The preheater 3 20 can heat the recycled materials again to improve the overall conversion rate of the raw materials.

[0051] 5. Product Collection:

[0052] After the reaction is completed, the gaseous product is discharged through the gas outlet pipe 21 at the top of the reaction tower 1, and the 1,1,1,3,3-pentachloropropane product is transported to the product storage tank 25 through the discharge pipe 23 at the bottom of the reaction tower 1.

Claims

1. A continuous preparation device for 1,1,1,3,3-pentachloropropane, comprising a reaction tower (1), characterized in that: The reaction tower (1) is provided with a plurality of packing sections (2) in the inner cavity, and a catalytic leak-proof assembly (3) is provided in the packing section (2). The top of the reaction tower (1) is provided with a liquid inlet pipe (4), one end of which is connected to a carbon tetrachloride feed pump (15), and the other end of which passes through the top of the reaction tower (1) and is connected to a nozzle distributor 1 (6). The side wall of the reaction tower (1) is provided with an air inlet pipe 1 (7) and an air inlet pipe 2 (8), and one end of the air inlet pipe 1 (7) and one end of the air inlet pipe 2 (8) respectively pass through the side wall of the reaction tower (1) and are connected to a gas distributor 1 (6). The gas distributor 1 (9) and the gas distributor 2 (10), the other end of the air inlet pipe 1 (7) and the other end of the air inlet pipe 2 (8) are connected to an air inlet main pipe (11), the end of the air inlet main pipe (11) away from the air inlet pipe 2 (8) is connected to a vinyl chloride metering pump (17), a circulation pipeline (13) is arranged on the side wall of the reaction tower (1) away from the air inlet pipe 1 (7), one end of the circulation pipeline (13) passes through the upper part of the side wall of the reaction tower (1) and is connected to the nozzle distributor 2 (14), and the other end of the circulation pipeline (13) is connected to the lower part of the side wall of the reaction tower (1).

2. The continuous preparation device for 1,1,1,3,3-pentachloropropane according to claim 1, characterized in that: A preheater 1 (16) is provided on the liquid inlet pipe (4), the preheater 1 (16) is located between the carbon tetrachloride feed pump (15) and the reaction tower (1), and the end of the carbon tetrachloride feed pump (15) away from the preheater 1 (16) is connected to the carbon tetrachloride storage tank (5). A preheater 2 (18) is provided on the air inlet main pipe (11), the preheater 2 (18) is located between the vinyl chloride metering pump (17) and the reaction tower (1), and the end of the vinyl chloride metering pump (17) away from the preheater 2 (18) is connected to the vinyl chloride storage tank (12).

3. The continuous preparation device for 1,1,1,3,3-pentachloropropane according to claim 1, characterized in that: A preheater three (20) is provided on the circulation pipeline (13), and a circulation pump (19) is provided between the preheater three (20) and the reaction tower (1).

4. The continuous preparation device for 1,1,1,3,3-pentachloropropane according to claim 1, characterized in that: A gas outlet pipe (21) is arranged at the top of the reaction tower (1), and a gas cooler (22) is arranged on the gas outlet pipe (21).

5. The continuous preparation device for 1,1,1,3,3-pentachloropropane according to claim 1, characterized in that: A discharge pipe (23) is provided at the bottom of the reaction tower (1), one end of the discharge pipe (23) away from the reaction tower (1) is connected to a product storage tank (25), and a discharge pump (24) is provided on the discharge pipe (23).

6. The continuous preparation device for 1,1,1,3,3-pentachloropropane according to claim 1, characterized in that: The catalytic leak-proof component (3) comprises a leak-proof mesh bag (301), and a solid catalyst (302) is arranged inside the leak-proof mesh bag (301).

7. The continuous preparation device for 1,1,1,3,3-pentachloropropane according to claim 1, characterized in that: A gas distributor (9) is located in the middle of the inner cavity of the reaction tower (1). The gas distributor (9) comprises three groups of air inlet branch pipes (901) arranged in parallel with each other. Both ends of the air inlet branch pipes (901) are sealed and both ends of the air inlet branch pipes (901) are fixedly arranged on the inner wall of the reaction tower (1). A cross frame (902) is arranged at the bottom of the air inlet branch pipes (901). Both ends of the cross frame (902) are fixedly arranged on the inner wall of the reaction tower (1).

8. The continuous preparation device for 1,1,1,3,3-pentachloropropane according to claim 7, characterized in that: The three groups of air intake branch pipes 1 (901) are all connected to the air intake pipe 1 (7), and a plurality of air distribution holes 1 (903) are evenly arranged on the three groups of air intake branch pipes 1 (901).

9. The continuous preparation device for 1,1,1,3,3-pentachloropropane according to claim 1, characterized in that: The second gas distributor (10) is located at the bottom of the inner cavity of the reaction tower (1). The second gas distributor (10) includes three sets of gas inlet branch pipes (1001) arranged in parallel with each other. Both ends of the second gas inlet branch pipes (1001) are sealed and both ends of the second gas inlet branch pipes (1001) are fixedly arranged on the inner wall of the reaction tower (1). The bottom of the second gas inlet branch pipe (1001) is provided with a second cross frame (1002), and both ends of the second cross frame (1002) are fixedly arranged on the inner wall of the reaction tower (1).

10. The continuous preparation device for 1,1,1,3,3-pentachloropropane according to claim 9, characterized in that: The three groups of air intake branch pipes 2 (1001) are all connected to the air intake pipe 2 (8), and a plurality of air distribution holes 2 (1003) are evenly arranged on the three groups of air intake branch pipes 2 (1001).

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