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Preparation method of rubber vulcanization accelerator zinc dibenzyl dithiocarbamate

A technology of zinc dibenzyl dithiocarbamate and rubber vulcanization, which is applied in the field of rubber vulcanization accelerators to achieve the effects of reduced reaction cycle, simple operation, and less harsh reaction conditions

Active Publication Date: 2016-03-02
SHANDONG SUNSINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

DE4102337 discloses a kind of preparation method of zinc dibenzyl dithiocarbamate, although this method uses organic solution to drink zinc oxide, got rid of the generation of inorganic salt, but reaction needs 24h, after steaming organic solution, wash product with water, generate a lot of waste water

Method used

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  • Preparation method of rubber vulcanization accelerator zinc dibenzyl dithiocarbamate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The preparation method of rubber vulcanization accelerator zinc dibenzyl dithiocarbamate of the present invention comprises the following steps: in the 500ml four-necked flask equipped with thermometer, stirrer, jacket and temperature control, add 200g dimethylbenzene, 50g dibenzylamine, 0.5g surfactant, 17.4gCS 2 , 8.3gZnO, 6g catalyst, carbon disulfide was added dropwise when the temperature was raised to 25°C, and the reaction was stirred for 6h. Then cool down and filter, add water to azeotropically distill the xylene out of the filtered product, and dry the rest to obtain the product ZBEC. The product yield is 98.1%, the melting point is 183°C, and the zinc content is 10.17%.

[0021] The surfactant is sodium dodecylbenzenesulfonate, an anionic surfactant.

[0022] The catalyst is one of formic acid, acetic acid and propionic acid.

[0023] When the filtered product is added with water and water for azeotropic distillation, the distilled xylene and water can be ...

Embodiment 2

[0025] The preparation method of rubber vulcanization accelerator zinc dibenzyl dithiocarbamate of the present invention comprises the following steps: in the 500ml four-necked flask equipped with thermometer, stirrer, jacket and temperature control, add 240g dimethylbenzene, 50g dibenzylamine, 0.7g surfactant, 21.0gCS 2 , 10gZnO, 4g catalyst, carbon disulfide was added dropwise when the temperature was raised to 40°C, and the reaction was stirred for 5h. Then cool down and filter, add water to azeotropically distill the xylene out of the filtered product, and dry the rest to obtain the product ZBEC. The product yield is 97.9%, the melting point is 183°C, and the zinc content is 10.87%.

[0026] All the other are identical with embodiment 1.

Embodiment 3

[0028] The preparation method of rubber vulcanization accelerator zinc dibenzyl dithiocarbamate of the present invention comprises the following steps: in the 500ml four-necked flask equipped with thermometer, stirrer, jacket and temperature control, add 280g dimethylbenzene, 50g dibenzylamine, 0.8g surfactant, 21.5gCS 2 , 11.9gZnO, 2g catalyst, carbon disulfide was added dropwise when the temperature was raised to 35°C, and the reaction was stirred for 5.5h. Then cool down and filter, add water to azeotropically distill the xylene out of the filtered product, and dry the rest to obtain the product ZBEC. The product yield is 97.8%, the melting point is 183°C, and the zinc content is 10.98%.

[0029] All the other are identical with embodiment 1.

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Abstract

The invention relates to a preparation method of a rubber vulcanization accelerator zinc dibenzyl dithiocarbamate. The method comprises the following steps: adding a solution of dibenzylamine-xylene mixture into a container, and adding a surfactant, a catalyst and zinc oxide; heating to certain temperature, and dropwise adding carbon disulfide into the mixture; stirring and reacting for certain time, and filtering out the product zinc dibenzyl dithiocarbamate from the reaction mixture; adding water into the filtered product for azeotropic distillation with the water to obtain a high-purity product. The method is simple to operate; compared with the traditional preparation method, the reaction conditions are not harsh, the product has high purity, and the solvent is recycled to facilitate environmental protection; more importantly, by adding the catalyst, the reaction time is greatly shortened, and the reaction period is reduced.

Description

(1) Technical field: [0001] The invention belongs to the field of rubber vulcanization accelerators, and relates to a preparation method of the rubber vulcanization accelerator zinc dibenzyl dithiocarbamate. (2) Technical background: [0002] Zinc dibenzyl dithiocarbamate can be abbreviated as: ZBEC, and its structural formula is: [0003] [0004] This product is a very fast super-accelerator, suitable for natural rubber and synthetic rubber. This product is a safe secondary amino dithiocarbamate accelerator. The use of this product does not release carcinogenic nitrous Amine, ZBEC has the longest scorch resistance of all zinc dithiocarbamate accelerators and excellent resistance to early thiolation in latex. Its vulcanization activity temperature is low, and the operation is relatively safe. It can replace ZDBC, ZDEC, PZ, etc., and is an excellent active agent for thiazole accelerators. When using this product, the compounding amount of zinc oxide and sulfur is genera...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C333/16
Inventor 吴艳萍宋晓举薛香菊张凤丽于发涛
Owner SHANDONG SUNSINE CHEM