CN214346485U - Tower type reaction device for continuously synthesizing 2-mercaptobenzothiazole - Google Patents
Tower type reaction device for continuously synthesizing 2-mercaptobenzothiazole Download PDFInfo
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- CN214346485U CN214346485U CN202023181172.3U CN202023181172U CN214346485U CN 214346485 U CN214346485 U CN 214346485U CN 202023181172 U CN202023181172 U CN 202023181172U CN 214346485 U CN214346485 U CN 214346485U
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Abstract
The utility model belongs to the field of chemistry and chemical engineering, in particular to a tower reaction device for continuously synthesizing 2-mercaptobenzothiazole. The device comprises a preheating device, a static mixer, a multistage series-connection packed tower and a gas-liquid separator which are connected in series through pipelines, wherein the preheating device comprises a first preheating device and a second preheating device, and the top of the packed tower is communicated with the gas-liquid separator. The first preheating device and the second preheating device preheat BT and sulfur respectively, the BT and the sulfur enter a static mixer for adiabatic mixing after being preheated, the mixture enters from the bottom of a multistage series packed tower and finally leaves from the top of the tower and enters a gas-liquid separator, and the mixture is separated into tail gas and a crude product of 2-mercaptobenzothiazole through phase separation. The device realizes uniform mixing of BT and sulfur through a static mixer, maintains a liquid-liquid mixing state in a system by using a packed tower, completes high-temperature low-pressure reaction through a mature packed tower technology, continuously synthesizes M, and can solve the problems caused by the current intermittent production.
Description
Technical Field
The utility model belongs to the field of chemistry and chemical engineering, in particular to a tower reaction device for continuously synthesizing 2-mercaptobenzothiazole.
Background
The 2-mercaptobenzothiazole is industrially abbreviated as accelerator M, is a medium-speed and ultra-speed accelerator of natural rubber, is an important vulcanization accelerator, and is an intermediate for synthesizing thiazole and sulfenamide accelerators. The synthesis method of M mainly comprises an o-nitrochlorobenzene method, an aniline method and a benzothiazole method.
The o-nitrochlorobenzene method has complex production process and high production cost;
the aniline method has the advantages of high product quality, high yield, easily available raw materials and low production cost, most companies adopt the aniline method, but a byproduct, namely benzothiazole (hereinafter abbreviated as BT), is generated in the reaction process of the aniline method. In order to utilize the by-products, the BT needs to undergo a secondary reaction, specifically: BT and sulfur are reacted at a certain temperature and pressure to generate M, the reaction is also called a benzothiazole method, the M obtained by the method has high purity, is easy to process, has less solid waste and low safety risk, and the reaction equation is as follows:
BT and sulfur are added into a metering tank to react in a high-pressure reaction kettle. There are currently three major issues to consider:
(1) from the view of a reaction system, an intermittent high-pressure reaction kettle is mainly adopted, the material concentration at different time in the same kettle is different, the BT and sulfur concentration is highest at the beginning, and along with the reaction, the BT and sulfur concentration is gradually reduced, and the M concentration is gradually increased. In the process, whether the stirring can sufficiently mix materials, whether the heat exchange of the jacket of the reaction kettle can be carried out in time, and whether the radial temperature difference exists are main reasons for batch difference of the batch reaction.
(2) From the production operation, BT and sulfur are required to be frequently conveyed in intermittent production, a high-pressure reaction kettle is required to be repeatedly heated and cooled, the pressure is increased and reduced, the production period of a single batch is long, and the production efficiency is low. And conveying equipment is periodic to open and stops, and high-pressure batch autoclave periodic rising and falling temperature, rise and fall and press all can bring the impact to equipment, can bring very big impact to equipment operation maintenance, and the safety risk is big, and is unfavorable for automated control.
(3) From the production product perspective, M produced intermittently has large batch product difference, and the byproduct resin is difficult to control, so that M product with the same quality cannot be stably provided.
Disclosure of Invention
The method aims to solve the problems of low production efficiency, high energy consumption and poor stability of product quality in the prior art of producing the 2-mercaptobenzothiazole by adopting an intermittent high-pressure reaction kettle. The utility model combines the static mixer and the multi-stage packed tower to form a novel tower type continuous reaction device. The device realizes uniform mixing of BT and sulfur through a static mixer, maintains a liquid-liquid mixing state in a system by using a packed tower, completes high-temperature and low-pressure reaction through a mature packed tower technology, and continuously synthesizes M. The M product produced by the device has the advantages of strong stability, high yield, no color difference, low production cost and high production capacity, and can solve the problems caused by the current intermittent production through continuous production.
In order to realize the purpose, the technical scheme of the utility model is that:
a tower type reaction device for continuously synthesizing 2-mercaptobenzothiazole comprises a preheating device, a static mixer, a multistage series packed tower and a gas-liquid separator which are connected in series through pipelines. The preheating device, the static mixer, the multistage serial packed tower and the gas-liquid separator are respectively used for completing the processes of preheating, mixing, reacting and phase separating of raw materials. The preheating device comprises a first preheating device and a second preheating device, a static mixer is arranged at the bottom of the packing tower, and the top of the packing tower is communicated with the gas-liquid separator. The first preheating device and the second preheating device preheat BT and sulfur respectively, the preheated BT and the preheated sulfur enter a static mixer for adiabatic mixing, the mixture enters from the bottom of a multistage series packed tower and finally leaves from the top of the tower, and the reacted material is separated into tail gas and a crude product of 2-mercaptobenzothiazole through phase separation in a gas-liquid separator.
Furthermore, a high-temperature metering pump is further arranged on a feeding pipeline of the preheating device.
Further, the preheating device is a heat exchanger.
Further, the preheated BT and the preheated sulfur enter a static mixer through a three-way pipe fitting to be subjected to heat insulation mixing. The molar ratio of the raw material BT to the sulfur is 1.0: 1.05-5, and the preheating temperature of BT is as follows: 100-170 ℃, and the preheating temperature of the sulfur is as follows: 120-180 ℃.
Further, the static mixer is selected from any one of SV, SK, SX, SH or SL. The static mixer has the function of a mixing unit, so that the BT and sulfur two flows are cut, sheared, rotated and remixed, the directions of the flowing mixer are changed from time to time left and from time to time right, the central flow is pushed to the periphery, and the peripheral flow is pushed to the center, so that a good radial mixing effect is achieved. Meanwhile, the rotation action of the fluid per se also occurs on the joint of the adjacent components, and the perfect radial circulation mixing action enables the materials to be uniformly mixed.
Further, the packed tower is provided withThe tower type reaction equipment of the heat exchange jacket or the heat exchange coil pipe is characterized in that regular packing or random packing is filled in the tower, and the specific surface area of the packing is 20-800 m2/m3The porosity is more than or equal to 0.98, and a pore plate cutting plate can be filled in the tower. The reaction temperature in the multistage series packed tower is controlled at 200-230 ℃, the reaction pressure is 0.3-1 MPa, and the reaction pressure in the multistage series packed tower is controlled by a back pressure valve or a valve group. The retention time of the mixed materials in the multistage series packed tower is 2-4 h.
Further, the gas-liquid separator is connected with a tail gas output pipeline and a 2-mercaptobenzothiazole crude product output pipeline. The temperature of the gas-liquid separator is controlled at 185-195 ℃, the pressure is less than or equal to 0.1MPa, and the retention time of the reaction product in the gas-liquid separator is 20-50 min.
The utility model has the advantages that:
(1) adopt the utility model discloses, carry out the serialization reaction through preheating device, static mixer, multistage series connection packed tower and vapour and liquid separator, the product 2-mercaptobenzothiazole yield that obtains is higher than 98%.
(2) Adopt the utility model discloses react, heat utilization rate is high, and the product of acquisition is stable, process safety.
Drawings
FIG. 1 is a column reaction apparatus for continuously synthesizing 2-mercaptobenzothiazole.
In the drawing, 1 is a high-temperature metering pump, 2 is a preheating device, 201 is a first preheating device, 202 is a second preheating device, 3 is a static mixer, 4 is a packed tower, 5 is a backpressure valve or a valve group, and 6 is a gas-liquid separator.
Detailed Description
The present invention is explained in detail by the following specific embodiments, but the protection scope of the present invention is not limited to the following embodiments, and any person skilled in the art can combine the technical solutions that can be conceived by the common general knowledge in the art on the basis of the present invention, and all belong to the protection scope of the present invention.
EXAMPLE 1 Tower-type reaction apparatus for continuously synthesizing 2-mercaptobenzothiazole
A tower reaction device for continuously synthesizing 2-mercaptobenzothiazole comprises a preheating device 2, a static mixer 3, a multistage series packed tower 4 and a gas-liquid separator 6 which are connected in series through pipelines. The preheating device 2, the static mixer 3, the multistage serial packed tower 4 and the gas-liquid separator 6 are respectively used for completing the processes of preheating, mixing, reacting and phase separating of raw materials. The preheating device 2 comprises a first preheating device 201 and a second preheating device 202, the preheating device 2 is a heat exchanger, and a high-temperature metering pump 1 is further arranged on a feeding pipeline of the heat exchanger.
The heat exchanger comprises a first heat exchanger and a second heat exchanger, BT and sulfur are preheated by a high-temperature metering pump 1 through the first heat exchanger and the second heat exchanger respectively, and the preheated BT and the preheated sulfur enter a static mixer 3 through a tee pipe fitting to be subjected to heat insulation mixing. The mixed material enters from the bottom of a multistage series packed tower 4 and finally leaves from the top of the tower, and the top of the packed tower 4 is communicated with a gas-liquid separator 6. The gas-liquid separator 6 is connected with a tail gas output pipeline and a 2-mercaptobenzothiazole crude product output pipeline, and materials after reaction are separated into tail gas and a 2-mercaptobenzothiazole crude product through phase separation.
The static mixer 3 is selected from: any one of SV, SK, SX, SH or SL.
The multistage series packed tower 4 of the embodiment is a two-stage series packed tower 4, the packed tower 4 is a tower type reaction device with a heat exchange jacket or a heat exchange coil, regular packing, random packing or a pore plate cutting plate is filled in the tower, and the specific surface area of the packing is 20-800 m2/m3The porosity is more than or equal to 0.98.
Example 2 application example 1
The benzothiazole and the sulfur are fed according to the mol ratio of 1.0: 1.15.
The benzothiazole is preheated to 150 ℃ by a first heat exchanger through a high-temperature metering pump at the temperature of 120 ℃, and the sulfur is preheated to 150 ℃ by a second heat exchanger through the high-temperature metering pump at the temperature of 120 ℃. The preheated benzothiazole and the preheated sulfur enter a static mixer (SH type mixing structure, the hydraulic diameter of a channel is 10 mu m) through a three-way pipe fitting and react in a multistage series packed tower (the specific surface area of the packing is 80 m)2/m3A hole, aThe porosity is 0.98), the reaction temperature is 230 ℃, the reaction pressure is 0.3MPa, and the retention time is 4 h. After the hydrogen sulfide gas is stripped and separated by a gas-liquid separator (the temperature of the gas-liquid separator is 195 ℃, the pressure is 0.05MPa, the retention time is 50min), a high-pressure product with the purity of 98 percent of the 2-mercaptobenzothiazole is obtained, and the finished product of the 2-mercaptobenzothiazole is obtained by alkali dissolution, filtration and drying, wherein the initial melting point of the finished product of the 2-mercaptobenzothiazole is 177 ℃.
Example 3 application example 2
The benzothiazole and the sulfur are fed according to the mol ratio of 1.0: 1.2.
The benzothiazole is preheated to 170 ℃ by a first heat exchanger through a high-temperature metering pump at the temperature of 150 ℃, and the sulfur is preheated to 150 ℃ by a second heat exchanger through the high-temperature metering pump at the temperature of 150 ℃. The preheated benzothiazole and the preheated sulfur enter a static mixer (SL type mixing structure, the hydraulic diameter of a channel is 30 mu m) through a three-way pipe fitting and react in a multistage series packed tower (the specific surface area of the packing is 400 m)2/m3Porosity of 0.99), reaction temperature of 225 ℃, reaction pressure of 0.5MPa and retention time of 4 h. After the hydrogen sulfide gas is stripped and separated by a gas-liquid separator (the temperature of the gas-liquid separator is 190 ℃, the pressure is 0.1MPa, the retention time is 30min), a high-pressure product with the purity of 95.3 percent of 2-mercaptobenzothiazole is obtained, and a finished product of 2-mercaptobenzothiazole is obtained by alkali dissolution, filtration and drying, wherein the initial melting point of the finished product of 2-mercaptobenzothiazole is 179 ℃.
Example 4 application example 3
The benzothiazole and the sulfur are fed according to the mol ratio of 1.0: 1.4.
The benzothiazole is preheated to 170 ℃ by a first heat exchanger through a high-temperature metering pump at the temperature of 30 ℃, and the sulfur is preheated to 150 ℃ by a second heat exchanger through a high-temperature metering pump at the temperature of 30 ℃. The preheated benzothiazole and the preheated sulfur enter a static mixer (SV type mixing structure, the hydraulic diameter of a channel is 50 mu m) through a three-way pipe fitting and react in a multistage series packed tower (the specific surface area of the packing is 200 m)2/m3Porosity of 0.98), reaction temperature of 230 ℃, reaction pressure of 0.5MPa and residence time of 3 h. After the hydrogen sulfide gas is stripped and separated by a gas-liquid separator (the temperature of the gas-liquid separator is 190 ℃, the pressure is 0.05MPa, the retention time is 20min)Obtaining a high-pressure product with the purity of the 2-mercaptobenzothiazole of 95 percent, and obtaining the finished product of the 2-mercaptobenzothiazole by alkali dissolution, filtration and drying, wherein the initial melting point of the finished product of the 2-mercaptobenzothiazole is 176 ℃.
Example 5 application example 4
The benzothiazole and the sulfur are fed according to the mol ratio of 1.0: 1.8.
The benzothiazole is preheated to 160 ℃ by a high-temperature metering pump through a first heat exchanger at the temperature of 25 ℃, and the sulfur is preheated to 150 ℃ by a high-temperature metering pump through a second heat exchanger at the temperature of 25 ℃. The preheated benzothiazole and the preheated sulfur enter a static mixer (SX type mixing structure, the hydraulic diameter of a channel is 10 mu m) through a tee pipe fitting and react in a multistage series packed tower (the specific surface area of the packing is 800 m)2/m3The porosity is 0.98), the reaction temperature is 220 ℃, the reaction pressure is 0.4MPa, the residence time is 3.5h, after the gas-liquid separator is used for separating the hydrogen sulfide gas by gas stripping (the gas-liquid separator temperature is 195 ℃, the pressure is 0.05MPa, the residence time is 30min), a high-pressure product with the purity of 2-mercaptobenzothiazole of 97 percent is obtained, the finished product of 2-mercaptobenzothiazole is obtained by alkali dissolution, filtration and drying, and the initial melting point of the finished product of 2-mercaptobenzothiazole is 178 ℃.
Example 6 application example 5
The benzothiazole and the sulfur are fed according to the mol ratio of 1.0: 4.2.
The benzothiazole is preheated to 170 ℃ by a high-temperature metering pump through a first heat exchanger at the temperature of 50 ℃, and the sulfur is preheated to 120 ℃ by a high-temperature metering pump through a second heat exchanger at the temperature of 50 ℃. The preheated benzothiazole and the preheated sulfur enter a static mixer (SK type mixing structure, the hydraulic diameter of a channel is 50 mu m) through a three-way pipe fitting and react in a multistage series packed tower (the specific surface area of the packing is 600 m)2/m3The porosity is 0.98), the reaction temperature is 210 ℃, the reaction pressure is 0.5MPa, the residence time is 3.5h, after the gas-liquid separator is used for separating the hydrogen sulfide gas by gas stripping (the gas-liquid separator temperature is 195 ℃, the pressure is 0.1MPa, the residence time is 30min), a high-pressure product with the purity of 2-mercaptobenzothiazole of 96 percent is obtained, the finished product of 2-mercaptobenzothiazole is obtained by alkali dissolution, filtration and drying, and the initial melting point of the finished product of 2-mercaptobenzothiazole is 178.4 ℃.
The above-mentioned embodiments are merely preferred embodiments of the present invention, and not intended to limit the scope of the present invention, so that equivalent changes or modifications made by the structure, features and principles of the present invention should be included in the claims of the present invention.
Claims (7)
1. The tower type reaction device for continuously synthesizing the 2-mercaptobenzothiazole is characterized by comprising a preheating device (2), a static mixer (3), a multistage packed tower (4) and a gas-liquid separator (6) which are connected in series through pipelines, wherein the preheating device (2) comprises a first preheating device (201) and a second preheating device (202), the first preheating device (201) and the second preheating device (202) preheat BT and sulfur respectively, the static mixer (3) is arranged at the bottom of the packed tower (4), and the top of the packed tower (4) is communicated with the gas-liquid separator (6).
2. The tower reaction device for continuously synthesizing 2-mercaptobenzothiazole according to claim 1, wherein a high temperature metering pump (1) is further arranged on a feeding pipeline of the preheating device (2).
3. The tower reaction device for continuously synthesizing 2-mercaptobenzothiazole according to claim 1, wherein the preheating device (2) is a heat exchanger.
4. The tower reaction device for continuously synthesizing 2-mercaptobenzothiazole according to claim 1, wherein the preheated BT and the preheated sulfur enter the static mixer (3) through a tee pipe for adiabatic mixing.
5. The column reactor for the continuous synthesis of 2-mercaptobenzothiazole according to claim 1, characterized in that the static mixer (3) is selected from any one of SV, SK, SX, SH or SL.
6. The tower type reaction device for continuously synthesizing 2-mercaptobenzothiazole according to claim 1, wherein the packed tower (4) is a tower type reaction device with a heat exchange jacket or a heat exchange coil, and the specific surface area of the packing in the tower is 20-800 m2/m3The porosity is more than or equal to 0.98.
7. The tower type reaction device for continuously synthesizing 2-mercaptobenzothiazole according to claim 1, wherein the gas-liquid separator (6) is connected with a tail gas output pipeline and a 2-mercaptobenzothiazole crude product output pipeline.
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| CN115160255A (en) * | 2022-09-06 | 2022-10-11 | 科迈化工股份有限公司 | Method and system device for continuously producing 2-mercaptobenzothiazole |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115160255A (en) * | 2022-09-06 | 2022-10-11 | 科迈化工股份有限公司 | Method and system device for continuously producing 2-mercaptobenzothiazole |
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