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Preparation process of post vulcanization agent dihydrated hexa methylene 1.6-disodium dithiosulfate

A technology of disodium dithiosulfate and hexamethylene dihydrate is applied in the fields of synthesis of new post-vulcanization stabilizers, separation and purification of products, and can solve problems such as products that do not meet requirements, achieve easy operation and avoid using , the effect of reducing pollution

Inactive Publication Date: 2006-11-15
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the product needs to be extracted with hot methanol during the purification process, which has certain risks, and if the extraction process is not well controlled, the product may not meet the requirements

Method used

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  • Preparation process of post vulcanization agent dihydrated hexa methylene 1.6-disodium dithiosulfate
  • Preparation process of post vulcanization agent dihydrated hexa methylene 1.6-disodium dithiosulfate

Examples

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Effect test

Embodiment 1

[0016] Weigh 20g of sodium thiosulfate, measure 6mL of dibromohexane into a three-necked flask, add 80mL of 50% ethanol, and react at 60°C to 80°C for 15 to 60min under reflux and stirring conditions.

[0017] After the reaction, add 110mL of 95% ethanol to the reaction solution, reflux at 80°C for 15 minutes and then filter while it is hot. After adding an appropriate amount of tap water to the filtrate, let it cool down gradually, and the product crystallizes out during the cooling process.

[0018] After the obtained product is dried, it becomes the final vulcanizing agent dihydrate hexamethylene 1,6-dithiosulfuric acid disodium salt.

[0019] The result of component analysis of the finished product: the sodium chloride content is less than 0.84%, and the active ingredient content is greater than 97.80%. (The standard used by enterprises is that the sodium chloride content is less than 1%, and the active ingredient content is greater than 95%)

Embodiment 2

[0021] Take 54.6g, 0.35mol of 1,6-dichlorohexane and 163.4g, 0.75mol of sodium thiosulfate and dissolve them in 230mL of water and 230mL of 95% ethanol, and react in the reactor for 6-15min, with the temperature controlled at 90-135 ℃.

[0022] After the reaction, add 900mL of 95% ethanol to the reaction solution, reflux at 80°C for 15 minutes and then filter while it is hot. Then add an appropriate amount of tap water to the filtrate, and then let it cool down gradually. During the cooling process, the product will crystallize.

[0023] After the obtained product is dried, it becomes the final vulcanizing agent dihydrate hexamethylene 1,6-dithiosulfuric acid disodium salt.

[0024] The result of component analysis of the finished product: the sodium chloride content is less than 0.52%, and the active ingredient content is greater than 98.95%.

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Abstract

A process for preparing the bihydrated hexamethylene 1,6-bisodium dithiosulfate used as post-sulfurizing agent includes such steps as putting sodium thiosulfate and dibromohexane or dichlorohexane in reactor, adding alcohol, reflux and stirring while reacting, adding alcohol, reflux, cooling, adding water, filtering and drying.

Description

technical field [0001] The invention relates to the field of organic chemistry, and relates to a synthesis method of a novel post-vulcanization stabilizer and a product separation and purification method. Background technique [0002] As we all know, pure rubber has almost no practical value. In order to make rubber have high elasticity, low plasticity and high strength in a wide temperature range, the degree of crosslinking between rubber molecules must be enhanced to form a network structure, which requires Vulcanize the rubber. The development of anti-reversion agents, which can resist reversion without affecting other properties of vulcanized rubber, and improve the anti-reversion performance of sulfur vulcanized rubber materials, has always been a key issue in improving the simultaneous vulcanization quality and service life of rubber products such as tires. . In recent years, a new type of additive has been used in the rubber industry, which can reduce and (or) elimi...

Claims

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Application Information

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IPC IPC(8): C07C381/02C08K5/41C08L21/00
Inventor 瞿其曙汤晓庆胡效亚刘尹陆晓
Owner YANGZHOU UNIV
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