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Tower type microreactor for continuous synthesis of 2-mercaptobenzothiazole

A mercaptobenzothiazole, tower-type technology is applied in the field of tower-type micro-reaction devices of rubber vulcanization accelerator 2-mercaptobenzothiazole, which can solve the problem of short residence time, gas-liquid two-phase mixing, and difficulty in 2-mercaptobenzothiazole. Continuous synthesis of benzothiazole, etc., to achieve the effects of product stability, process safety, and high thermal energy utilization

Active Publication Date: 2019-05-03
WILLING NEW MATERIALS TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, although the microchannel reactor can achieve rapid mixing of reactants, its internal tiny flow channel and extremely short residence time are difficult to implement the continuous synthesis of 2-mercaptobenzothiazole with a reaction time of hours on an industrial scale.
In addition, the output of the microchannel reactor is small. Once the space confinement effect of the microchannel is lost, it is difficult to realize the gas-liquid two-phase mixing in the reaction system.

Method used

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  • Tower type microreactor for continuous synthesis of 2-mercaptobenzothiazole
  • Tower type microreactor for continuous synthesis of 2-mercaptobenzothiazole
  • Tower type microreactor for continuous synthesis of 2-mercaptobenzothiazole

Examples

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Embodiment 1

[0020] 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, 60°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 sieve holes, the hole diameter is 0.5mm, 4 of which are used to disperse liquid sulfur in aniline, and 4 are used to disperse carbon disulfide in aniline) Mix, react in the structured packing tower (the ratio of filler Surface area 100m 2 / m 3 , Porosity 0.93, reaction temperature 280°C, pressure 8MPa, material residence time 1h). After stripping and separating hydrogen sulfide gas (stripping tower temperature 210°C, pressure 8MPa, liquid phase residence time 0.2h), the high-pressure product of 2-mercaptobenzothiazole with a purity of 95% is obtained, and the finished product is obtained by alkali-dissolution filtration and drying 2-Mercaptobenzothiazole has an initial meltin...

Embodiment 2

[0022] The molar ratio of aniline, carbon disulfide and sulfur is 1.0:1.2:1.05. At room temperature, it is preheated to 170°C, 60°C, and 150°C respectively through a metering pump at room temperature through a heat exchanger, and then enters a micro-mesh dispersing mixer (inner Contains 2 cross-flow shear sieve holes, the hole diameter is 2mm, one of which is used to disperse aniline in carbon disulfide, and the other is used to disperse liquid sulfur in carbon disulfide) and mix, react in random packed tower (the specific surface area of ​​the filler 400m 2 / m 3 , porosity 0.95, reaction temperature 280°C, pressure 9MPa, material residence time 1.5h). After stripping and separating hydrogen sulfide gas (stripping tower temperature 210°C, pressure 9MPa, liquid phase residence time 0.5h), a high-pressure product with a purity of 94.3% of 2-mercaptobenzothiazole was obtained, which was filtered and dried by alkali dissolution to obtain the finished product 2-Mercaptobenzothiaz...

Embodiment 3

[0024] The molar ratio of aniline, carbon disulfide, and sulfur is 1.0:1.0:1.2. At room temperature, it is preheated to 200°C, 40°C, and 120°C through a metering pump through a heat exchanger at room temperature, and then enters a microgroove dispersion mixer (contains 2 Transverse cross-flow shear microgrooves, microgroove width 0.5mm, one of which is used to disperse liquid sulfur in aniline, and one is used to disperse carbon disulfide in aniline) mixed, reacted in random packed tower (the specific surface area of ​​the filler 400m 2 / m 3 , Porosity 0.95, reaction temperature 210°C, pressure 8MPa, material residence time 3h). After stripping and separating hydrogen sulfide gas (stripping tower temperature 200°C, pressure 8MPa, liquid phase residence time 1h), the high-pressure product of 2-mercaptobenzothiazole with a purity of 92% was obtained, which was filtered and dried by alkali solution to obtain the finished product 2 -Mercaptobenzothiazole has an initial melting p...

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Abstract

The invention discloses a microreactor for continuous synthesis of 2-mercaptobenzothiazole. The microreactor comprises a raw material preheater, a micromixer, a filling material reaction tower and a stripping tower which are connected in series to successively complete the processes of preheating, mixing, reaction and phase separation of raw materials, wherein the raw materials comprise aniline, carbon disulfide and sulfur, are separately heated to a respective initial temperature in the raw material preheater, and then mixed in the micromixer in a heat-insulation manner; the micromixer is placed at the bottom part of the filling material reaction tower; a raw material mixture enters from the bottom part of the filling material reaction tower for a reaction; and a product leaves from the top part of the filling material reaction tower to enter the stripping tower, and is separated into tail gas and a crude 2-mercaptobenzothiazole product in the stripping tower. By use of the microreactor provided by the invention, continuous production can be realized; the yield of the 2-mercaptobenzothiazole can achieve 95% or above; the content of resin is less than 2%; and high production efficiency and good product quality are achieved.

Description

technical field [0001] The invention relates to the technical field of chemistry and chemical engineering, in particular to a tower-type micro-reaction device for rubber vulcanization accelerator 2-mercaptobenzothiazole. Background technique [0002] 2-Mercaptobenzothiazole, referred to as Accelerator M in the industry, is a medium-speed accelerator for natural rubber. It is not only an important vulcanization accelerator, but also an intermediate for the synthesis of thiazole and sulfenamide accelerators. There are two main synthetic methods of 2-mercaptobenzothiazole: the o-nitrochlorobenzene method and the aniline method. Because the raw material cost of o-nitrochlorobenzene is relatively high, the aniline method is currently the main method for industrially synthesizing 2-mercaptobenzothiazole. method. 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00B01J19/30C07D277/72
Inventor 王凯骆广生章娟郭同新
Owner WILLING NEW MATERIALS TECH CO LTD
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