Reaction device for continuous synthesis of 2-mercaptobenzothiazole

A technology of mercaptobenzothiazole and reactor, which is applied in the direction of organic chemistry, can solve problems such as fire, difficulty in controlling the formation of benzothiazole and anilinobenzothiazole, and lack of rapid mixing ability, so as to achieve process safety and product stability Effect

Active Publication Date: 2019-05-28
WILLING NEW MATERIALS TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional pipelines or stirred reaction devices do not have rapid mixing capabilities under high temperature and pressure, so it is difficult to control the formation of benzothiazole and anilinobenzothiazole
Although the use of carbon disulfide solution dissolved in sulfur as a reactant can reduce the system’s requirements for the mixing capacity of the reaction device, it is a very dangerous process in the actual operation process to dissolve sulfur with carbon disulfide, and it is easy to cause fires due to static electricity. Therefore, the invention can quickly and uniformly mix aniline The reaction device for the three raw materials of , carbon disulfide and sulfur is very necessary

Method used

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  • Reaction device for continuous synthesis of 2-mercaptobenzothiazole
  • Reaction device for continuous synthesis of 2-mercaptobenzothiazole

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The molar ratio of aniline, carbon disulfide and sulfur is 1.0:1.1:1.0. At room temperature, it is preheated to 150°C, 40°C, and 180°C respectively through a metering pump and heat exchanger at room temperature, and then enters the micro-mesh dispersing mixer (inner Contains 8 cross-flow shearing screens, the apertures are all 0.5mm, 4 of which are used to disperse sulfur in aniline, and 4 are used to disperse carbon disulfide in aniline), and react in 3-stage series stirred tanks (reaction tank The temperature is 260°C, 250°C and 210°C respectively), the reaction pressure is 8MPa, and the residence time is 1.5h. After hydrogen sulfide is separated by gas stripping (the stripper temperature is 210°C and the pressure is 8MPa), the high-pressure product of 2-mercaptobenzothiazole with a purity of 92% is obtained, and the finished product 2-mercaptobenzothiazole is obtained through alkali-soluble filtration and drying. The melting point is 175°C.

Embodiment 2

[0023] The molar ratio of aniline, carbon disulfide, and sulfur is 1.0:1.2:1.05. They are preheated to 170°C, 40°C, and 150°C through metering pumps and heat exchangers at room temperature, and then enter the micro-mesh dispersing mixer (inner Contains 2 cross-flow shearing screens, the apertures are 2mm, one of which is used to disperse aniline in carbon disulfide, and the other is used to disperse sulfur in carbon disulfide), react in 4-stage series stirred tank (the temperature of the reaction tank 270°C, 260°C, 250°C and 210°C respectively), reaction pressure 8MPa, residence time 2h. After hydrogen sulfide is separated by gas stripping (stripping tower temperature 210°C, pressure 8MPa), the high-pressure product of 2-mercaptobenzothiazole with a purity of 94% is obtained, and the finished product 2-mercaptobenzothiazole is obtained by filtering and drying with alkali. The melting point is 174°C.

Embodiment 3

[0025] The molar ratio of aniline, carbon disulfide, and sulfur is 1.0:1.1:1.1. At room temperature, it is preheated to 200°C, 60°C, and 120°C through a metering pump at room temperature through a heat exchanger, and then enters a micro-channel mixer (a cross-shaped Microchannel structure, each of the three raw materials enters from a branch channel, and the last channel is used as the outlet of the mixed product, the channel hydraulic diameter is 5mm), and the reaction is carried out in a 4-stage series stirred tank (the temperature of the reactor is 270 ° C, 260 ° C, 250 ° C, respectively. ℃ and 210℃), the reaction pressure is 9MPa, and the residence time is 2.3h. After hydrogen sulfide is separated by gas stripping (stripping tower temperature 210°C, pressure 9MPa), the high-pressure product of 2-mercaptobenzothiazole with a purity of 95% is obtained, and the finished product 2-mercaptobenzothiazole is obtained by filtering and drying with alkali. The melting point is 176°C...

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Abstract

The invention discloses a reaction device for continuous synthesis of 2-mercaptobenzothiazole. The reaction device comprises a raw material preheater, a micromixer, multistage reaction kettles and a stripping tower which are connected in series and sequentially complete the preheating, mixing, reacting and phase separating processes of raw materials; the raw materials comprise aniline, carbon disulfide and sulphur which are heated to the respective initial temperatures in the preheating device and then are subjected to insulation mixing in the micromixer, a raw material mixture sequentially enters from the bottom of the multi-stage reaction kettles which are connected in series, leaves from the tops of the multi-stage reaction kettles, and is subjected to multi-stage reaction to generate the 2-mercaptobenzothiazole; and the top of the last-stage reaction kettle communicates with the stripping tower, and the stripping tower is used for separating the reacted materials into tail gas anda 2-mercaptobenzothiazole coarse product. Continuous production can be achieved by using the reaction device, the yield of the 2-mercaptobenzothiazole reaches 92% or above, the resin content is less than 4%, the production efficiency is high, and the product stability is good.

Description

technical field [0001] The invention relates to the technical field of chemistry and chemical engineering, in particular to a continuous synthesis reaction device for rubber vulcanization accelerator 2-mercaptobenzothiazole. Background technique [0002] 2-Mercaptobenzothiazole (also known as Accelerator M) is a medium-speed accelerator for natural rubber. It can be used alone or mixed with other accelerators. It and its derivatives play an important role in the rubber vulcanization process. There are two main synthetic methods of 2-mercaptobenzothiazole: o-nitrochlorobenzene method and aniline method. Due to the high cost of o-nitrochlorobenzene raw materials, the aniline method is the main method for the industrial synthesis of 2-mercaptobenzothiazole. Specifically, the method is to place aniline, carbon disulfide and sulfur under high temperature and high pressure reaction conditions, and at 200°C and a temperature and pressure above 8MPa, the following reaction occurs: ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/72
Inventor 王凯骆广生章娟郭同新
Owner WILLING NEW MATERIALS TECH CO LTD
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