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Novel process for synthesizing 2-thiol benzothiazole zinc salt by adopting solvent method

A technology of mercaptobenzene and benzothiazole, which is applied in the field of rubber accelerators, can solve the problems of increased waste water treatment costs and comprehensive production costs, and achieves the effects of short production cycles, reduced production costs, and no corrosion of equipment

Pending Publication Date: 2021-04-16
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The cost of wastewater treatment is gradually increasing, environmental protection is becoming stricter, and the overall cost of production is increasing

Method used

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  • Novel process for synthesizing 2-thiol benzothiazole zinc salt by adopting solvent method

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Add 88.13 g (0.5 mol) of 2-mercaptobenzothiazole, 20.7 g (0.26 mol) of zinc oxide, 500 ml of toluene solvent, and 0.5 g of glacial acetic acid as a catalyst into the four-necked reaction flask. Seal it with a rubber stopper, heat it to reflux under normal pressure, and complete the reaction after 3 hours. After filtering and drying, the product ZMBT is obtained as a pale yellow solid. The detected reaction yield was 97.6%, and the initial melting point was 220.8°C.

Embodiment 2

[0019] Add 100 g (0.57 mol) of 2-mercaptobenzothiazole, 23.4 g (0.29 mol) of zinc oxide, 500 ml of ethyl acetate solvent, and 0.5 g of catalyst glacial acetic acid into the four-necked reaction flask, add condensation and reflux to separate water The device is sealed with a rubber stopper, heated to reflux under normal pressure, and the reaction is completed after 3 hours, and the product is obtained as a pale yellow solid ZMBT through filtration and drying processes. The detected reaction yield was 98.1%, and the initial melting point was 222.7°C.

Embodiment 3

[0021] Add 88.13 g (0.5 mol) of 2-mercaptobenzothiazole, 20.7 g (0.26 mol) of zinc oxide, 500 ml of toluene solvent, and 0.5 g of catalyst propionic acid into the four-necked reaction flask, and add a condensation reflux water separation device, Seal it with a rubber stopper, heat it to reflux under normal pressure, and complete the reaction after 3 hours. After filtering and drying, the product ZMBT is obtained as a pale yellow solid. The detected reaction yield was 98.4%, and the initial melting point was 222.5°C.

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Abstract

The invention belongs to the technical field of rubber accelerators, and discloses a new process for synthesizing 2-thiol benzothiazole zinc salt by adopting a solvent method, which comprises the following steps: adding raw materials 2-thiol benzothiazole and zinc oxide into an organic solvent, adding a catalyst, heating under normal pressure to reflux, reacting for 2-3 hours, filtering, and drying to obtain a faint yellow solid. The byproduct of the process is only a small amount of pollution-free water, and compared with the traditional process, no waste salt is generated, the generation of wastewater is reduced, clean production is realized, and the production cost is reduced.

Description

technical field [0001] The invention belongs to the technical field of rubber accelerators, and relates to a new process for synthesizing 2-mercaptobenzothiazole zinc salt by a solvent method. Background technique [0002] The main production method of 2-mercaptobenzothiazole zinc salt at the present stage is: accelerator M (2-mercaptobenzothiazole) is dissolved in sodium hydroxide solution to generate sodium salt, and then zinc sulfate is added dropwise for metathesis reaction, and finally 2-mercaptobenzothiazole zinc salt (ZMBT) is obtained, and the accompanying by-products are a large amount of polluted salt and waste water. The cost of wastewater treatment is gradually increasing, environmental protection is becoming stricter, and the overall cost of production is increasing. Therefore, a new process for the synthesis of clean and environment-friendly 2-mercaptobenzothiazole zinc salt is needed. Contents of the invention [0003] The purpose of the present invention ...

Claims

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Application Information

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IPC IPC(8): C07D277/72
Inventor 丁胜强史宗浩章娟王新杰尹跃宁郭德义王志强郭同新
Owner WILLING NEW MATERIALS TECH CO LTD
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