Tubular reactor for synthesizing perchloromethyl mercaptan
By using activated carbon packing and external stirring blades in the tubular reactor, the problems of untimely heat transfer and uneven contact in the synthesis of perchloromethanethiol were solved, achieving efficient and safe synthesis of perchloromethanethiol and improving product quality and production efficiency.
Patent Information
- Application Number
- CN202422794750.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-16
- Publication Date
- 2025-11-04
- Estimated Expiration
- 2034-11-16
AI Technical Summary
Untimely heat removal during the synthesis of perchloromethanethiol leads to more byproducts, affects product quality, and poses safety risks. Uneven contact between chlorine and carbon disulfide reduces reaction efficiency.
A tubular reactor is used, with activated carbon packing inside the tubes and external stirring blades. Heat is transferred through a heat exchange medium. Chlorine and carbon disulfide react inside the tubes to produce perchloromethanethiol, and the tail gas is treated by a gas-liquid separator. The stirring blades outside the tubes ensure uniform temperature.
It improves heat transfer efficiency, reduces by-products, enhances reaction efficiency and safety, ensures product quality, and reduces production costs.
Smart Images

Figure CN223505261U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to synthetic device technical field, concretely relates to full chloromethyl mercaptan synthesis uses column pipe type reactor. BACKGROUND
[0002] Full chloromethyl mercaptan is also called trichloro sulfur chloromethane, colorless oily liquid, is the intermediate of pesticide captan, detoxification dan and other fungicides.
[0003] The prior art discloses a patent with publication number CN113480461B, which comprises: carbon disulfide, water is mixed to form a mixed solution, and the mixed solution and chlorine are continuously fed into the reaction tower for reaction to synthesize full chloromethyl mercaptan; the reaction tower is a three-layer feeding tower type reactor; the reaction temperature in the reaction tower is not higher than 35 DEG C. The method can solve the problems of back mixing, multiple by-products, low raw material utilization rate and production efficiency, and low safety in single-kettle full-mixing reaction; continuous production can reduce production equipment, improve reaction conversion rate and selectivity, improve raw material utilization rate, thereby improving production efficiency and yield, reducing production cost, and improving production safety; reaction by-products are recovered by absorption and can be sold as industrial products, improving the comprehensive utilization value of raw materials.
[0004] The existing device gradually exposes the shortcomings of the technology with use, mainly in the following aspects:
[0005] First, in the synthesis process of full chloromethyl mercaptan, heat removal is an important factor limiting its reaction effect, and if heat removal is not timely, not only a large amount of by-products will be produced, affecting product quality, but also there is a certain safety risk.
[0006] Second, the existing synthesis device is limited by structure, and chlorine and carbon disulfide cannot be uniformly contacted in the synthesis device, which reduces the reaction synthesis efficiency.
[0007] From the above, it is obvious that the prior art has inconvenience and defects in actual use, so it is necessary to improve. Utility model content
[0008] In view of the defects in the prior art, the utility model provides a column pipe type reactor for synthesizing full chloromethyl mercaptan, to solve the problem that in the synthesis process of full chloromethyl mercaptan in the prior art, heat removal is an important factor limiting its reaction effect, and if heat removal is not timely, not only a large amount of by-products will be produced, affecting product quality, but also there is a certain safety risk.
[0009] To achieve the above purpose, the utility model provides the following technical scheme.
[0010] The application discloses a column reactor for synthesizing perchloromethyl mercaptan, which comprises a box body, two baffles fixed side by side in the box body from top to bottom, and a plurality of vertical column tubes arranged side by side between the two baffles, the two ends of the column tubes penetrating through the baffles, and the column tubes being rotationally arranged with their axes as the rotation center.
[0011] An activated carbon filler is fixed on the inner wall of each column tube.
[0012] As an optimized scheme, the box body forms a heat transfer area through the area between the two baffles.
[0013] As an optimized scheme, a plurality of mixed flow stirring blades are arranged around the outer wall of the column tube and located in the heat transfer area.
[0014] As an optimized scheme, a heat transfer medium inlet and a heat transfer medium outlet communicating with the heat transfer area are respectively fixed on the opposite side walls of the box body.
[0015] As an optimized scheme, the lower end of the column tube extends to the lower side through the baffle and is fixed with a gear ring, and the adjacent gear rings are engaged.
[0016] As an optimized scheme, a driving machine is fixed at the lower end of the box body, the output shaft of the driving machine extends into the box body and is fixed with a gear engaged with the gear ring.
[0017] As an optimized scheme, a center concave bottom arc flow guide surface is arranged on the inner bottom surface of the box body.
[0018] As an optimized scheme, a center convex top arc flow guide surface is arranged on the top of the box body.
[0019] As an optimized scheme, a material inlet connected with the inner cavity of the box body is fixed on the top of the box body, a gas-liquid mixer is connected to the material inlet, and a chlorine source and a carbon disulfide source are connected to the inlet end of the gas-liquid mixer.
[0020] As an optimized scheme, the height of the heat transfer medium inlet is lower than that of the heat transfer medium outlet.
[0021] As an optimized scheme, a tail gas outlet communicating with the inner cavity of the box body is fixed at the center position of the top of the box body, and a gas-liquid separator is connected to the tail gas outlet.
[0022] As an optimized scheme, a product outlet communicating with the inner cavity of the box body is fixed at the center position of the bottom of the box body.
[0023] As an optimized scheme, the heat transfer medium inlet and the heat transfer medium outlet are separately arranged on the opposite outer walls of the box body.
[0024] Compared with the prior art, the utility model has the advantages of
[0025] Chlorine and carbon bisulfide are mixed by a gas-liquid mixer and then enter the box, and full chloromethyl mercaptan is generated by reaction in the column pipe, a heat removal area is arranged outside the column pipe, heat is removed by a heat exchange medium, and the heat removal efficiency in the synthesis reaction process is ensured.
[0026] The generated full chloromethyl mercaptan product is discharged from the product outlet at the bottom of the equipment, a gas-liquid separator is arranged at the top of the equipment, a small amount of non-condensable liquid is prevented from being discharged by entrainment in the tail gas, and finally the tail gas enters a tail gas treatment system.
[0027] By the activated carbon filler in the column pipe, the falling speed of the material can be reduced, the material can be catalyzed, and the material reaction efficiency can be improved.
[0028] By arranging the mixed flow stirring blades outside the column pipe, the heat exchange medium in the column pipe is stirred during rotation, the temperature of the heat exchange medium in the heat exchange area is uniform, and the problem that the temperature difference between the inlet and the outlet is too large in the traditional technology to affect the material reaction is overcome. BRIEF DESCRIPTION OF DRAWINGS
[0029] In order to more clearly illustrate the specific embodiments of the utility model or the technical solutions in the prior art, the drawings needed 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 scale.
[0030] Figure 1 The structure of the utility model is shown in the figure.
[0031] In the figure, 1 is a box, 2 is a baffle, 3 is a heat removal area, 4 is a column pipe, 5 is a mixed flow stirring blade, 6 is activated carbon filler, 7 is a gear ring, 8 is a driving machine, 9 is a gear, 10 is a tail gas outlet, 11 is a gas-liquid separator, 12 is a material inlet, 13 is a gas-liquid mixer, 14 is a heat exchange medium inlet, 15 is a heat exchange medium outlet, and 16 is a product outlet. DETAILED DESCRIPTION
[0032] The embodiments of the technical solutions of the utility model 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 utility model, and therefore only serve as examples, and cannot limit the protection scope of the utility model.
[0033] As Figure 1The column reactor for synthesizing perchloromethyl mercaptan shown comprises a box 1, two baffles 2 fixed side by side in the box 1 from top to bottom, a plurality of vertical column tubes 4 arranged side by side between the two baffles 2, the two ends of the column tubes 4 penetrating through the baffles 2 respectively, the column tubes 4 being rotationally arranged with their axes as the rotation center,
[0034] An activated carbon filler 6 is fixed on the inner wall of each column tube 4,
[0035] The box 1 forms a heat transfer area 3 through the area between the two baffles 2.
[0036] A plurality of mixed flow stirring blades 5 are arranged around the outer wall of the column tubes 4 in the heat transfer area 3.
[0037] A heat transfer medium inlet 14 and a heat transfer medium outlet 15 are respectively fixed on the opposite side walls of the box 1 and communicate with the heat transfer area 3.
[0038] The lower end of the column tube 4 extends to the lower side through the baffle 2 and is fixed with a gear ring 7, the adjacent gear rings 7 being engaged with each other.
[0039] A driving machine 8 is fixed on the lower end of the box 1, the output shaft of the driving machine 8 extending into the box 1 and being fixed with a gear wheel 9 engaged with the gear ring 7.
[0040] A bottom arc-shaped flow guide surface is arranged on the inner bottom surface of the box 1.
[0041] A top arc-shaped flow guide surface is arranged on the top of the box 1.
[0042] A material inlet 12 connected with the inner cavity of the box 1 is fixed on the top of the box 1, a gas-liquid mixer 13 is connected on the material inlet 12, the inlet end of the gas-liquid mixer 13 being connected with a chlorine source and a carbon disulfide source.
[0043] The height of the heat transfer medium inlet 14 is lower than that of the heat transfer medium outlet 15.
[0044] A tail gas outlet 10 connected with the inner cavity of the box 1 is fixed on the central position of the top of the box 1, a gas-liquid separator 11 is connected on the tail gas outlet 10.
[0045] A product outlet 16 connected with the inner cavity of the box 1 is fixed on the central position of the bottom of the box 1.
[0046] The heat transfer medium inlet 14 and the heat transfer medium outlet 15 are separately arranged on the opposite outer walls of the box 1.
[0047] Mounting holes are arranged on the baffles 2, and sealing rings are arranged between the outer wall of the column tubes 4 and the mounting holes.
[0048] The structure of the gas-liquid mixer 13 and the gas-liquid separator 11 is common and is not described here.
[0049] Compared with the prior art, the utility model has the beneficial effects that:
[0050] Chlorine and carbon disulfide are mixed by gas-liquid mixer 13 and then enter the box 1, and the reaction is carried out inside the column tube 4 to generate perchloro methyl mercaptan, and the heat removal area 3 is arranged outside the column tube 4, and the heat is removed by the heat exchange medium, so that the heat removal efficiency in the synthesis reaction process is ensured;
[0051] The generated perchloro methyl mercaptan product is discharged from the product outlet 16 at the bottom of the equipment, and the gas-liquid separator 11 is arranged at the top of the equipment to prevent a small amount of non-condensable liquid from being entrained in the tail gas and discharged, and finally the tail gas enters the tail gas treatment system;
[0052] By the activated carbon filler inside the column tube, the falling speed of the material can be reduced, and the material can be catalyzed to improve the reaction efficiency of the material;
[0053] By arranging the mixed flow stirring blade 5 outside the column tube 4, the heat exchange medium inside the column tube 4 is stirred during rotation, so that the temperature of the heat exchange medium in the heat exchange area is uniform, and the problem that the temperature difference between the inlet and outlet in the traditional technology is too large to affect the material reaction is overcome.
[0054] Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the utility model, and 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: it can still modify the technical solutions recorded in the foregoing embodiments, or make equivalent replacement to part or all of the technical features; 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 tubular reactor for the synthesis of perchloromethanethiol, characterized in that: The device includes a housing (1), inside which two baffles (2) are fixedly connected side by side from top to bottom. Between the two baffles (2) are several vertically arranged tubes (4), with both ends of the tubes (4) passing through the baffles (2). The tubes (4) are rotatable with their axis as the center of rotation. Activated carbon packing (6) is fixed on the inner wall of each of the tubes (4).
2. The tubular reactor for the synthesis of perchloromethanethiol according to claim 1, characterized in that: The box (1) forms a heat transfer zone (3) between two baffles (2).
3. The tubular reactor for the synthesis of perchloromethanethiol according to claim 2, characterized in that: The outer wall of the tube (4) is surrounded by a number of mixing blades (5) located in the heat transfer zone (3).
4. The tubular reactor for the synthesis of perchloromethanethiol according to claim 3, characterized in that: The heat exchange medium inlet (14) and heat exchange medium outlet (15) that connect to the heat transfer area (3) are respectively fixed to the opposite side walls of the box (1).
5. The tubular reactor for the synthesis of perchloromethanethiol according to claim 4, characterized in that: The lower end of the tube (4) extends through the baffle (2) and is fixed to a toothed ring (7), with adjacent toothed rings (7) meshing with each other.
6. The tubular reactor for the synthesis of perchloromethanethiol according to claim 5, characterized in that: A drive motor (8) is fixedly connected to the lower end of the housing (1). The output shaft of the drive motor (8) extends into the housing (1) and is fixedly connected to a gear (9) that meshes with the gear ring (7).
7. The tubular reactor for the synthesis of perchloromethanethiol according to claim 6, characterized in that: The inner bottom surface of the box (1) is provided with a bottom arc-shaped flow guide surface with a central concave shape, and the top of the box (1) is provided with a top arc-shaped flow guide surface with a central convex shape.
8. The tubular reactor for the synthesis of perchloromethanethiol according to claim 7, characterized in that: The top of the box (1) is fixedly connected to a material inlet (12) that connects to its inner cavity. A gas-liquid mixer (13) is connected to the material inlet (12). The inlet end of the gas-liquid mixer (13) is connected to a chlorine source and a carbon disulfide source.
9. The tubular reactor for the synthesis of perchloromethanethiol according to claim 8, characterized in that: The top center of the box (1) is fixed with an exhaust gas outlet (10) that communicates with its inner cavity, and a gas-liquid separator (11) is connected to the exhaust gas outlet (10).
10. The tubular reactor for the synthesis of perchloromethanethiol according to claim 9, characterized in that: The bottom center of the box (1) is fixed with a product outlet (16) that communicates with its inner cavity.
Citation Information
Patent Citations
Method for continuous synthesis of perchloromethanethiol using a reaction tower
CN113480461B