Synthesis process of tetrabenzylthiuram disulfide

A technology of tetrabenzylthiuram disulfide and carbon disulfide, applied in the direction of organic chemistry, can solve the problems of distillation treatment, limited application fields, high water consumption, etc., and achieve favorable reaction efficiency, high process safety, and improved product quality. Yield effect

Active Publication Date: 2020-04-17
HEBI YUANHAO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that inorganic salt by-products are produced, and the product needs a large amount of water to wash and desalt, and the water consumption is high; the mother liquor still needs further treatment, and the energy consumption is high
Disadvantages: ①The product has a certain solubility in the solvent, which affects the yield; ②The solvent residue in the product limits its application field; ③The solvent still needs to be distilled, and the energy consumption is high
In addition, the dibenzylamine added first in the above method has a side reaction with the generated intermediate product, which competes with the main reaction to affect the yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] At room temperature, to 3m 3 Add 1500kg water in the reactor, start stirring. At 20-30°C, pump 67.1kg of carbon disulfide in sequence, and then slowly add 167.0kg of dibenzylamine. Repeat this feeding 2 times for a total of 3 times, and keep warm for 3 hours. Continue to slowly add 451.0 kg of 10% hydrogen peroxide solution. Gradually raise the temperature to reflux, continue to react for 3h, and the reaction ends. separate. An off-white tetrabenzylthiuram disulfide was obtained. The yield is 99.20%, and the melting point is 130.2°C.

Embodiment 2

[0021] At room temperature, to 2m 3 Add 600kg water in the reactor, start stirring. At 30-40°C, add 23.8kg of carbon disulfide in sequence, and then slowly add 60.0kg of dibenzylamine. Repeat this feeding 1 time, keep warm for 2h. Continue to slowly add 102.4 kg of 10% hydrogen peroxide solution. Gradually raise the temperature to reflux, continue to react for 3h, and the reaction ends. separate. Pale yellow tetrabenzylthiuram disulfide was obtained. The yield is 99.05%, and the melting point is 130.0°C.

Embodiment 3

[0023] At room temperature, to 1m 3 Add 400kg water in the reactor, start stirring. At 30-35°C, add 23.8kg of carbon disulfide and slowly add 60.0kg of dibenzylamine. Keep warm for 3h. Continue to slowly add 56.3 kg of 10% hydrogen peroxide solution. Gradually raise the temperature to reflux, continue the reaction for 2h, and the reaction ends. separate. Pale yellow tetrabenzylthiuram disulfide was obtained. The yield is 99.16%, and the melting point is 130.1°C.

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Abstract

The invention provides a synthesis process of tetrabenzylthiuram disulfide. The synthesis process comprises the following steps: carrying out a mixed reaction on dibenzylamine and carbon disulfide inwater to generate an intermediate product, and carrying out an oxidation reaction on the intermediate product and hydrogen peroxide to prepare tetrabenzylthiuram disulfide. According to the process, water is used as a medium, so operation safety is high, no organic solvent is left in the product, and no inorganic salt by-product is generated; and the competitive reaction of the raw materials and the intermediate is effectively reduced, so product yield is improved.

Description

technical field [0001] The invention relates to the synthesis field of rubber vulcanization accelerators, in particular to a synthesis process of tetrabenzylthiuram disulfide. Background technique [0002] Dithiotetrabenzylthiuram Basic Chemical Information: English Name: [0003] Tetrabenzylthiuram disulfide; English abbreviation: TBzTD; Molecular formula: C 30 h 28 N 2 S 4 ; CAS RN: 10591-85-2. [0004] Among the thiuram rubber vulcanization accelerators, due to their relatively large molecular weight and high thermal stability, when used in the vulcanization system of rubber products, it is difficult to produce nitrosamines during the vulcanization process of the products. A new environment-friendly rubber vulcanization accelerator that is widely used. [0005] At present, the industrial synthesis accelerator TBzTD mainly includes air oxidation method, two-step alkali method, and solvent hydrogen peroxide oxidation method. [0006] (1) Patent CN201310719619.3 discl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C333/32
CPCC07C333/32
Inventor 张智亮李红良常帅军刘俊勇宋志强王艳利
Owner HEBI YUANHAO CHEM CO LTD
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