Preparation method of tetrabutylthiuram disulfide used as rubber vulcanization accelerator

A technology of tetrabenzylthiuram disulfide and rubber vulcanization, which is applied in the chemical industry, can solve the problems of no recovery of carbon disulfide, safety problems, and unstable safety, and achieve short vulcanization time, less pollution, and long burning time Effect

Active Publication Date: 2015-02-04
山东斯递尔化工科技有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0007] Chinese patent document CN101462993A also discloses a preparation method of tetrabenzylthiuram disulfide rubber vulcanization accelerator by hydrogen peroxide oxidation method. Although the yield rate of its disclosed product is 96.5%, it has a higher promotion, but pure hydrogen peroxide is used As an oxidant, there are certain safety problems and instability. Using concentrated sulfuric acid to adjust the acidity also has safety problems, and the excessive carbon disulfide is not recovered, which will cause environmental pollution.

Method used

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  • Preparation method of tetrabutylthiuram disulfide used as rubber vulcanization accelerator

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Embodiment 1

[0042] A preparation method of rubber vulcanization accelerator tetrabenzylthiuram disulfide, the steps are as follows:

[0043] (1) Under normal pressure, add dibenzylamine and sodium hydroxide into water, stir and mix evenly, add carbon disulfide dropwise at 23°C, and stir for 0.5h;

[0044] The molar ratio of dibenzylamine, sodium hydroxide and carbon disulfide is 1:1.1:1.35, and the molar volume ratio of dibenzylamine to water is 1:2mol / L;

[0045] (2) The reaction solution obtained in step (1) was left to stand for 0.5h, unreacted carbon disulfide was separated from the bottom, and 10wt% hydrogen peroxide was added dropwise at 58.5°C for oxidation reaction, and the amount added was the total amount of hydrogen peroxide 70% of the total amount of hydrogen peroxide, reacted for 3h, then added dropwise 20wt% hydrogen peroxide, the amount added was 30% of the total amount of hydrogen peroxide, continued the oxidation reaction for 1h, and controlled the rate of addition to 0.8ml...

Embodiment 2

[0068] A kind of preparation method of rubber vulcanization accelerator tetrabenzylthiuram disulfide, step is the same as embodiment 1, and difference is:

[0069] The molar ratio of dibenzylamine, sodium hydroxide and carbon disulfide is 1:1.12:1.15, and other conditions are the same as in Example 1.

[0070] The color of the obtained product is white. After testing, the initial melting point of the product is 132.3° C., the purity of the product is 98.1%, and the yield of the reaction is 95.5%.

Embodiment 3

[0072] A kind of preparation method of rubber vulcanization accelerator tetrabenzylthiuram disulfide, step is the same as embodiment 1, and difference is:

[0073] The molar ratio of hydrogen peroxide to dibenzylamine is 0.8:1, and other conditions are the same as in Example 1.

[0074] The color of the obtained product is white. After testing, the initial melting point of the product is 132.6° C., the purity of the product is 97.9%, and the yield of the reaction is 95.8%.

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Abstract

The invention relates to a preparation method of tetrabutylthiuram disulfide used as a rubber vulcanization accelerator. By virtue of the preparation method, tetrabutylthiuram disulfide is prepared by a two-step process, namely sodium dibenzyl amino sulfonate is prepared from dibenzylamine, carbon disulfide and sodium hydroxide and then oxidized by a hydrogen peroxide oxidant to prepare tetrabutylthiuram disulfide. According to the preparation method, carbon disulfide is excessive, so that dibenzylamine is fully reacted; excessive unreacted carbon disulfide is separated and recycled in time; the production cost is reduced; the pollution to the environment is low; low-concentration hydrogen peroxide with a concentration of 5-20wt% is used as the oxidant and applied to the oxidation reaction; hydrogen peroxide has the characteristics of being low in cost, stable in property, small in pollution, easy to store and transport and high in safety; the cost can be effectively reduced; the pollution to workers in the operation process is alleviated; the safety is improved; meanwhile, the oxidization effect is not reduced.

Description

technical field [0001] The invention relates to a preparation method of tetrabenzylthiuram disulfide, a rubber vulcanization accelerator, and belongs to the technical field of chemical industry. Background technique [0002] Among the rubber vulcanization accelerators, thiurams belong to an important category and have good vulcanization acceleration effects, mainly including thiuram monosulfide, thiuram disulfide and thiuram polysulfide, among which four Methyl thiuram (accelerator TMTD) is the one with the largest output and consumption among thiuram accelerators. In recent years, people have paid more and more attention to the problem that certain accelerators are prone to produce harmful nitrosamines during rubber processing. Studies have shown that N-nitrosamines are produced by the reaction of secondary amines and nitrogen oxides. During the vulcanization process of rubber compounds, vulcanization accelerators based on secondary amines (such as morpholine, diisopropyla...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/32
Inventor 张敏朱嘉震李海存赵新远张平王金才尹传祥
Owner 山东斯递尔化工科技有限公司
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