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Preparation of rubber vulcanization accelerator dibenzothiazyl disulfide

A technology of dibenzothiazole disulfide and rubber vulcanization, applied in organic chemistry and other directions, can solve the problems of non-compliance with the production requirements of national environmental protection policies, high content of 2-mercaptobenzothiazole, and difficult to clean "green" production, etc. Achieve the effects of superior vulcanization performance, white product appearance, and long product shelf life

Active Publication Date: 2009-06-24
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition to discharging harmful gases such as dinitrogen tetroxide, nitrogen monoxide, chlorine, and hydrogen chloride during the production process of this process, what is more serious is that the amount of wastewater per ton of DM has doubled, and the increase in energy consumption has also been very large, making wastewater It is extremely difficult to control and realize "clean" and "green" production, which does not meet the national environmental protection policy and production requirements for energy conservation and emission reduction.
At the same time, the content of free 2-mercaptobenzothiazole in the finished product is relatively high, and the melting point of the product is low, which is difficult to meet the high-end requirements of the domestic and foreign sales markets, and the yield of the product is not high in addition

Method used

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  • Preparation of rubber vulcanization accelerator dibenzothiazyl disulfide

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Effect test

Embodiment 1

[0040] 2-Mercaptobenzothiazole sodium salt (M-Na), hydrogen peroxide, and sulfuric acid are used as raw materials, and the ratio of the oxidizing agent is hydrogen peroxide: sulfuric acid = 1: 1mol;

[0041] The preparation process is: add the mixed mixture of hydrogen peroxide and sulfuric acid dropwise into a reaction kettle containing 2-mercaptobenzothiazole sodium salt (M-Na) at a temperature of 55°C under stirring to carry out oxidation reaction , the oxidation reaction time is 75 minutes; after the oxidant is added dropwise, keep warm for 0.5 hours; after that, measure the pH value of the reaction solution, after the pH value of the reaction solution is stabilized to 6.8, control the temperature at 30°C for solid-liquid separation, The obtained solid is dried, pulverized, sieved and packaged to obtain the finished product dibenzothiazole disulfide (DM), which has an initial melting point of 175°C, a purity of 99.5%, and a product yield of 98%.

Embodiment 2

[0043] Use 2-mercaptobenzothiazole sodium salt (M-Na), hydrogen peroxide, and sulfuric acid as raw materials, wherein the ratio of oxidant is hydrogen peroxide: sulfuric acid = 1.5: 1mol;

[0044]The preparation process is: add the mixed mixture of hydrogen peroxide and sulfuric acid dropwise into a reaction kettle containing 2-mercaptobenzothiazole sodium salt (M-Na) at a temperature of 65°C under stirring to carry out oxidation reaction , the oxidation reaction time is 65 minutes; after the oxidant is added dropwise, keep warm for 0.5 hours; after that, measure the pH value of the reaction solution, after the pH value of the reaction solution is stabilized to 7.3, control the temperature at 30°C for solid-liquid separation, The obtained solid is dried, pulverized, sieved, and packaged to obtain the finished product dibenzothiazole disulfide (DM), which has an initial melting point of 174°C, a purity of 99.8%, and a product yield of 99%.

Embodiment 3

[0046] Use 2-mercaptobenzothiazole sodium salt (M-Na), hydrogen peroxide and sulfuric acid as raw materials, wherein the ratio of oxidant is hydrogen peroxide: sulfuric acid = 2.0: 1mol;

[0047] The preparation process is: add the mixed mixture of hydrogen peroxide and sulfuric acid dropwise into the reaction kettle containing 2-mercaptobenzothiazole sodium salt (M-Na) at a temperature of 61°C under stirring to carry out the oxidation reaction , the oxidation reaction time is 68 minutes; after the oxidant is added dropwise, keep warm for 0.5 hours; after that, measure the pH value of the reaction solution, after the pH value of the reaction solution is stabilized to 7.0, control the temperature at 30°C for solid-liquid separation, The obtained solid is dried, pulverized, sieved and packaged to obtain the finished product dibenzothiazole disulfide (DM), which has an initial melting point of 174.5°C, a purity of 99.7%, and a product yield of 98.5%.

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Abstract

The invention relates to a preparation method of a thiofide (dibenzothiazyl disulfide), wherein, 2-mercaptobenzothiazole sodium salt is taken as a raw material, mixture of hydrogen peroxide and sulfuric acid is taken as an oxidizing agent, and the mol ratio of the hydrogen peroxide to the sulfuric acid is 0.5-2.5:1, and the method comprises the following steps (1) preparation process of the oxidizing agent: evenly mixing the hydrogen peroxide and the sulfuric acid in a container according to the mol ratio; and (2) oxidization process of the product: dropwise adding the mixture of the hydrogen peroxide and the sulfuric acid to a reaction kettle with the 2-mercaptobenzothiazole sodium salt at the temperature of 55 DEG C-65 DEG C while stirring for oxidization reaction for 60-80 minutes, keeping warm for about 0.5 hour after the oxidizing agent is added dropwise; then measuring pH value of the reaction solution, performing solid-liquid separation at the temperature of 30 DEG C when the pH value is stabilized within a range of 6.5-7.5, drying, crushing, screening and packaging the obtained solid to obtain the product. The method can help effectively enhance quality of the product, save energy and lower consumption and reduce 'three wastes' pollution.

Description

technical field [0001] The invention relates to a preparation method of a rubber vulcanization accelerator, in particular to a preparation method of a rubber vulcanization accelerator dibenzothiazole disulfide. Background technique [0002] In recent years, with the rapid development of the domestic automobile industry and communication industry, it has driven the rapid growth of the rubber processing industry and provided unprecedented good opportunities for the development of the rubber additives industry. Rubber vulcanization accelerator dibenzothiazole disulfide (DM) is widely used in the vulcanization process of natural rubber, isoprene rubber, styrene-butadiene rubber, butadiene rubber, EPDM rubber and nitrile rubber. Since the reform and opening up, although the production of rubber accelerator products in my country has been greatly improved, compared with foreign developed countries, there is still a big gap in the inherent quality of products and "green" environmen...

Claims

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Application Information

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IPC IPC(8): C07D277/78C07D277/70C08K5/47C08L21/00
Inventor 郭同新岳法亮王平生徐治松李红喜屈军伟史宗浩
Owner WILLING NEW MATERIALS TECH CO LTD
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