Trickle bed reactor for synthesizing perchloromethyl mercaptan

Abstract

A trickle bed reactor for synthesizing perchloromethyl mercaptan relates to the technical field of synthesis devices and comprises a tank body, a plurality of distributors and fillers are arranged in the tank body from top to bottom in parallel, the top of the tank body is connected with a carbon disulfide inlet pipeline, the bottom of the tank body is connected with a chlorine inlet pipeline, and the top of the tank body is further connected with a heat exchanger. The outlet end of the heat exchanger is connected with a carbon disulfide receiving tank, and the outlet end of the carbon disulfide receiving tank is connected to the carbon disulfide inlet pipeline through a backflow pipeline. The utility model solves the problems that the device in the traditional technology is not timely in heat transfer, the traditional device controls the reaction temperature by controlling the feeding rate, the efficiency is low and certain instability exists in a certain range, and the selectivity is reduced if the heat transfer in the reaction is not timely.

Description

TECHNICAL FIELD

[0001] The utility model relates to synthetic device technical field, concretely relates to the trickle bed reactor for perchloromethylmercaptan synthesis. BACKGROUND

[0002] Perchloromethylmercaptan is also called trichlorothiochloromethane, colorless oily liquid, is the intermediate of pesticide captan, antidote and other fungicides.

[0003] The prior art discloses a patent with the publication number CN103360295A, which comprises the following steps: adding carbon disulfide and hydrochloric acid into two chlorination reaction kettles, taking 1# kettle as the main reaction kettle for chlorination reaction, controlling its temperature at 20-30 DEG C, and passing in chlorine for chlorination reaction; 2# kettle is used as the side reaction kettle during chlorination; when the density of the reaction liquid in 1# kettle reaches 1.65-1.68, the reaction is terminated, and after the reaction is finished, the reaction material is transferred to a treatment kettle, and the product is statically layered, the upper layer is mixed acid, and the lower layer is the product perchloromethylmercaptan; then carbon disulfide and hydrochloric acid are added into 1# chlorination reaction kettle, and then the kettle is used as the side reaction kettle, and 2# kettle is used as the main reaction kettle, and chlorine is passed in for chlorination reaction; the two series connection reaction kettles are alternately used to recover carbon disulfide and chlorine, thereby improving product yield, reducing production cost, and overcoming the harm of carbon disulfide leakage to the environment and human health in the prior art.

[0004] The existing device gradually exposes the deficiencies of the technology with use, mainly in the following aspects:

[0005] Firstly, the existing device does not solve the demand of timely heat removal, according to the reaction heat data obtained by using the full-automatic reaction calorimeter, the specific heat release of the reaction is 294.6J / g, and the heat release is large.

[0006] Secondly, the traditional device controls the reaction temperature in a certain range by controlling the feeding rate, and the efficiency is low, and there is certain instability, and if the heat is not removed in time, the selectivity will be reduced.

[0007] From the above, it can be seen that the prior art has obvious inconvenience and defects in actual use, so it is necessary to improve. UTILITY MODEL CONTENTS

[0008] In view of the defects in the prior art, the utility model provides a trickle bed reactor for perchloromethylmercaptan synthesis, which solves the problem of the device in the prior art that the heat is not removed in time, and the problem that the traditional device controls the reaction temperature by controlling the feeding rate, the efficiency is low in a certain range, and there is certain instability, and if the heat is not removed in time, the selectivity will be reduced.

[0009] In order to achieve the above object, the utility model provides the following technical scheme.

[0010] The full chloromethyl mercaptan synthesis trickle bed reactor, including the jar body, the jar body is equipped with a plurality of distributors and fillers from top to bottom,

[0011] The top of the jar body is connected with carbon disulfide inlet pipeline,

[0012] The bottom of the jar body is connected with chlorine inlet pipeline,

[0013] The top of the jar body is also connected with heat exchanger, the outlet end of heat exchanger is connected with carbon disulfide receiving tank, the outlet end of carbon disulfide receiving tank is connected with carbon disulfide inlet pipeline through reflux pipeline.

[0014] As an optimized scheme, the reflux pipeline is connected with material transfer pump.

[0015] As an optimized scheme, the bottom of the jar body is connected with discharge port.

[0016] As an optimized scheme, the outer wall of the jar body is also provided with heat exchange system.

[0017] As an optimized scheme, the discharge port is connected with separation device.

[0018] As an optimized scheme, the heat exchange system includes heat exchange jacket arranged on the outer wall of the jar body.

[0019] As an optimized scheme, the heat exchange jacket is connected with refrigerant inlet and refrigerant outlet.

[0020] As an optimized scheme, the refrigerant inlet is close to the bottom of the heat exchange jacket.

[0021] As an optimized scheme, the refrigerant outlet is close to the top of the heat exchange jacket.

[0022] As an optimized scheme, the refrigerant inlet and the refrigerant outlet are separately arranged on the opposite outer wall of the heat exchange jacket.

[0023] Compared with the prior art, the utility model has the beneficial effects that:

[0024] The trickle bed reactor belongs to gas-liquid-solid three-phase reactor, carbon disulfide is introduced into the reaction section from the top of trickle bed through distributor, chlorine is introduced into the reaction section from the bottom of trickle bed, the reaction section is filled with filler layer, carbon disulfide and chlorine react to generate full chloromethyl mercaptan in the reaction filler section, the reaction is exothermic reaction, the heat released by reaction makes carbon disulfide vaporize, and the vaporization of carbon disulfide plays the effect of heat removal;

[0025] The carbon disulfide vapor is cooled into liquid state by a heat exchanger, and returns to the reaction system, and the heavy phase of the reaction synthesis is discharged through a discharge port at the bottom of the trickle bed and enters a downstream separation process;

[0026] By setting the heat exchange system, on the one hand, the operator is protected from scalding, and on the other hand, the carbon disulfide is ensured to be in an excess state in the reaction system, and the energy consumption of material transfer can be reduced;

[0027] The reaction equipment adopts a trickle bed reactor, the excess carbon disulfide is vaporized to achieve the purpose of heat removal, the gaseous carbon disulfide is returned to the system after being recovered by condensation, and is recycled; and no third component is introduced into the system, which is cleaner;

[0028] The material enters the forced circulation heat exchanger through the bottom of the tank body, is forced to circulate and cooled, heat exchange is strengthened, and the heat exchange effect is maximized. BRIEF DESCRIPTION OF DRAWINGS

[0029] In order to more clearly illustrate the specific embodiments of the present application or the technical solutions in the prior art, the drawings required to be used in the specific embodiments or the prior art description will be briefly introduced below. In all the drawings, similar elements or parts are generally identified by similar reference numerals. In the drawings, the elements or parts are not necessarily drawn according to the actual proportions.

[0030] Figure 1 It is a structural schematic view of the present application.

[0031] In the drawings: 1 - tank body; 2 - carbon disulfide inlet pipeline; 3 - chlorine inlet pipeline; 4 - distributor; 5 - packing; 6 - heat exchange jacket; 7 - coolant outlet; 8 - coolant inlet; 9 - heat exchanger; 10 - carbon disulfide receiving tank; 11 - reflux pipeline; 12 - transfer pump; 13 - discharge port; 14 - forced circulation heat exchanger; 15 - forced circulation pump. DETAILED DESCRIPTION

[0032] The embodiments of the technical solutions of the present application will be described in detail below with reference to the drawings. The following embodiments are only used to more clearly illustrate the technical solutions of the present application, and therefore only serve as examples, and cannot limit the protection scope of the present application.

[0033] As shown in Figure 1 The full chloromethyl mercaptan synthesis trickle bed reactor comprises a tank body 1, a plurality of distributors 4 and packings 5 are arranged side by side in the tank body 1 from top to bottom,

[0034] The top of the tank body 1 is connected with a carbon disulfide inlet pipeline 2,

[0035] The bottom of the tank body 1 is connected with a chlorine inlet pipeline 3,

[0036] The top of the tank 1 is also connected with a heat exchanger 9, the outlet end of the heat exchanger 9 is connected with a carbon disulfide receiving tank 10, the outlet end of the carbon disulfide receiving tank 10 is connected with the carbon disulfide inlet pipeline 2 through a reflux pipeline 11.

[0037] The reflux pipeline 11 is connected with a transfer pump 12.

[0038] The bottom of the tank 1 is connected with a discharge port 13.

[0039] The outer wall of the tank 1 is also provided with a heat exchange system, which is located in the area where the filler is located.

[0040] The discharge port 13 is connected with a separation device.

[0041] The heat exchange system includes a heat exchange jacket 6 arranged on the outer wall of the tank 1.

[0042] Each heat exchange jacket 6 is connected with a refrigerant inlet 8 and a refrigerant outlet 7.

[0043] The refrigerant inlet 8 is close to the bottom of the heat exchange jacket 6.

[0044] The refrigerant outlet 7 is close to the top of the heat exchange jacket 6.

[0045] The refrigerant inlet 8 and the refrigerant outlet 7 are separately arranged on the opposite outer walls of the heat exchange jacket 6.

[0046] The outside of the tank 1 is also connected with a forced circulation heat exchanger 14, the two ends of the forced circulation heat exchanger 14 are correspondingly connected with the bottom and the top of the tank 1, a forced circulation pump 15 is arranged on the pipeline between the forced circulation heat exchanger 14 and the bottom of the tank 1, the material enters the forced circulation heat exchanger through the bottom of the tank 1, and the forced circulation heat exchanger 14 and the tank 1 are connected with the bottom and the top of the tank 1.

[0047] The working principle of the device is as follows:

[0048] The trickle bed reactor belongs to a gas-liquid-solid three-phase reactor, carbon disulfide enters the reaction section from the top of the trickle bed through a distributor, chlorine gas enters the reaction section from the bottom of the trickle bed, the reaction section is filled with a filler layer, carbon disulfide and chlorine gas react to generate perchloromethylthiol in the reaction filler section, the reaction is an exothermic reaction, and the heat released in the reaction causes carbon disulfide to vaporize, thereby achieving the effect of heat removal through the vaporization of carbon disulfide;

[0049] The vaporized carbon disulfide is cooled to a liquid state through the heat exchanger 9 and returns to the reaction system, and the heavy phase synthesized by the reaction is discharged through the discharge port 13 at the bottom of the trickle bed and enters the downstream separation process;

[0050] By arranging the heat exchange system, on the one hand, the heat exchange system can avoid burns and protect operators, and on the other hand, the heat exchange system can ensure that carbon disulfide is in an excess state in the reaction system and can also reduce the energy consumption of material transfer;

[0051] The reaction equipment adopts a trickle bed reactor, excess carbon disulfide is vaporized to achieve the purpose of heat removal, and the gaseous carbon disulfide is returned to the system after being recovered by condensation and recycled; and no third component is introduced into the system, which is cleaner.

[0052] Finally, it should be pointed out that: the above embodiments are only used to illustrate the technical solutions of the utility model, but not to limit them; although the utility model has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: the technical solutions recorded in the foregoing embodiments can still be modified, or part or all of the technical features can be replaced equivalently; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the utility model, and they should be covered in the scope of the claims and the specification of the utility model.

Claims

1. A fluidized bed reactor for the synthesis of perchloromethyl mercaptan, characterized in that: The application relates to a carbon disulfide production device, which comprises a tank body (1), wherein a plurality of distributors (4) and fillers (5) are arranged in parallel from top to bottom in the tank body (1), A carbon disulfide inlet pipeline (2) is connected to the top of the tank body (1), A chlorine inlet pipeline (3) is connected to the bottom of the tank body (1), A heat exchanger (9) is further connected to the top of the tank body (1), the outlet end of the heat exchanger (9) is connected with a carbon disulfide receiving tank (10), and the outlet end of the carbon disulfide receiving tank (10) is connected with the carbon disulfide inlet pipeline (2) through a reflux pipeline (11).

2. The fluidized bed reactor for per-chloromethyl mercaptan synthesis according to claim 1, characterized in that: A material transfer pump (12) is connected to the reflux pipeline (11).

3. The fluidized bed reactor for per-chloromethyl mercaptan synthesis according to claim 1, characterized in that: A discharge port (13) is connected to the bottom of the tank body (1).

4. The fluidized bed reactor for per-chloromethyl mercaptan synthesis according to claim 1, characterized in that: A heat exchange system is further arranged on the outer wall of the tank body (1).

5. The fluidized bed reactor for per-chloromethyl mercaptan synthesis according to claim 3, characterized in that: The discharge port (13) is connected with a separation device.

6. The fluidized bed reactor for per-chloromethyl mercaptan synthesis according to claim 4, characterized in that: The heat exchange system comprises heat exchange jackets (6) arranged on the outer wall of the tank body (1).

7. The fluidized bed reactor for per-chloromethyl mercaptan synthesis according to claim 6, characterized in that: A refrigerant inlet (8) and a refrigerant outlet (7) are connected to each heat exchange jacket (6).

8. The fluidized bed reactor for per-chloromethyl mercaptan synthesis according to claim 7, characterized in that: The refrigerant inlet (8) is close to the bottom of the heat exchange jacket (6), and the refrigerant outlet (7) is close to the top of the heat exchange jacket (6).

9. The fluidized bed reactor for per-chloromethyl mercaptan synthesis according to claim 8, characterized in that: The refrigerant inlet (8) and the refrigerant outlet (7) are arranged on the opposite outer walls of the heat exchange jacket (6).

10. The fluidized bed reactor for per-chloromethyl mercaptan synthesis of claim 1, wherein: A forced circulation heat exchanger (14) is further connected to the outside of the tank body (1), the two ends of the forced circulation heat exchanger (14) are correspondingly connected with the bottom and the top of the tank body (1), and a forced circulation pump (15) is arranged on the pipeline between the forced circulation heat exchanger (14) and the bottom of the tank body (1).

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