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Method for preparing zinc dibenzyl dithiocarbamate (ZBDC) thiofide

A technology of zinc dibenzyl dithiocarbamate and rubber vulcanization, applied in organic chemistry and other directions, can solve the problems of product dependence and low initial melting point, and achieve the effects of less environmental pollution, long shelf life and long scorch time

Active Publication Date: 2011-01-26
WILLING NEW MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The production method of the rubber vulcanization accelerator zinc dibenzyl dithiocarbamate (ZBDC) is currently not reported in domestic literature, and most of the products are imported, and the main quality and technical indicators of the reported products have a low initial melting point (178°C)

Method used

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  • Method for preparing zinc dibenzyl dithiocarbamate (ZBDC) thiofide
  • Method for preparing zinc dibenzyl dithiocarbamate (ZBDC) thiofide

Examples

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Embodiment 1

[0028] The raw materials used in this embodiment and their mol ratio are:

[0029] Dibenzylamine: carbon disulfide: sodium hydroxide: anionic surfactant: zinc chloride: sulfuric acid=1: 1.1: 1.08: 0.020: 0.55: 0.008 mol. The specific process is as follows: in the reaction kettle filled with purified water, add a specified amount of dibenzylamine, sodium hydroxide and anionic surfactant in sequence under stirring, wherein the anionic surfactant is sodium dodecylsulfonate, The temperature was lowered to 13°C, and a specified amount of carbon disulfide liquid was started to be added dropwise, and the control time was 6 hours. After the dropwise addition, stir for 0.5°C, control the temperature at 31° C., and add zinc chloride solution dropwise to carry out metathesis reaction. After the reaction, adjust the pH value of the reaction solution to 7 with sulfuric acid, that is, the reaction ends. After stirring for 1.5 hours, solid-liquid separation is carried out, the liquid is di...

Embodiment 2

[0031] The raw materials used in this embodiment and their mol ratio are:

[0032]Dibenzylamine: carbon disulfide: sodium hydroxide: anionic surfactant: zinc chloride: sulfuric acid=1: 1.15: 1.12: 0.022: 0.53: 0.008mol. The specific process is as follows: in the reaction kettle filled with purified water, add a specified amount of dibenzylamine, sodium hydroxide and anionic surfactant in sequence under stirring, wherein the anionic surfactant is sodium dodecylsulfonate, The temperature was lowered to 16°C, and a specified amount of carbon disulfide liquid was started to be added dropwise, and the control time was 6.5 hours. After completion of the dropwise addition, stir for 0.8 hours, control the temperature of 35° C., and add zinc chloride solution dropwise to carry out metathesis reaction. After the reaction was finished, the pH value of the reaction solution was adjusted to 8 with sulfuric acid, that is, the reaction was finished. After stirring for 2 hours, solid-liquid...

Embodiment 3

[0034] The raw materials used in this embodiment and their mol ratio are:

[0035] Dibenzylamine: carbon disulfide: sodium hydroxide: anionic surfactant: zinc chloride: sulfuric acid=1: 1.18: 1.16: 0.025: 0.57: 0.008 mol. The specific process is: into the reaction kettle filled with purified water, add the specified amount of dibenzylamine, sodium hydroxide and anionic surfactant in turn under stirring, wherein the anionic surfactant is regarded as sodium dodecylsulfonate , the temperature was lowered to 18°C, and a specified amount of carbon disulfide liquid was started to be added dropwise, and the control time was 7 hours. After completion of the dropwise addition, stir for 1 hour, control the temperature of 38°C, and add zinc chloride solution dropwise to carry out metathesis reaction. After the reaction, the pH value of the reaction solution was adjusted to 9 with sulfuric acid, and the reaction was completed. After stirring for 1.5 hours, solid-liquid separation is car...

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Abstract

The invention provides a method for preparing zinc dibenzyl dithiocarbamate (ZBDC) thiofide, which comprises that: the raw materials used are dibenzylamine, carbon disulfide, sodium hydroxide and anionic surfactant, wherein the stoichiometric molar ratio of dibenzylamine to carbon disulfide to sodium hydroxide and anionic surfactant to zinc chloride to sulfuric acid is 1:1.05-1.2:1.05-1.2:0.020-0.025:0.53-0.58:0.005-0.015; and the process comprises: adding dibenzylamine, carbon disulfide, sodium hydroxide and anionic surfactant in a given amount into a reaction kettle holding purified water with stirring in turn, lower the temperature by 10 to 20 DEG C totally, dripping carbon disulfide liquid in a given amount within 6 to 7 hours, stirring for 0.5 to 1 hours after the dripping is finished, keeping the temperature at 30 to 38 DEG C constantly, dripping solution of zinc chloride, performing replacement reaction, regulating the pH value of the reaction liquid to 7 to 9 with sulfuric acid after the replacement reaction is finished, finishing the reaction, stirring for 1 to 2 hours, performing solid-liquid separation, discarding liquid and drying, crushing, sieving and packaging the solid. The anionic surfactant is sodium dodecyl sulfate.

Description

technical field [0001] The invention relates to a rubber vulcanization accelerator, especially a production method of the rubber vulcanization accelerator zinc dibenzyl dithiocarbamate. Background technique [0002] In recent years, with the rapid development of the rubber processing industry, the rapid development of the domestic automobile industry and communication industry has driven the rapid growth of the rubber processing industry and provided unprecedented good opportunities for the development of the rubber additives industry. Since my country's accession to the WTO, although the production of rubber accelerator products in China has been greatly improved, compared with foreign developed countries, there is still a big gap in product intrinsic quality and "green" environmental protection technology. In particular, the international community has paid more and more attention to the toxicity of some accelerator products, which are prone to produce harmful substances n...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/16
Inventor 王志强郭同新王平生岳法亮陈合群史宗浩徐治松王飞
Owner WILLING NEW MATERIALS TECH CO LTD
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