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Preparation method for organic thiosulfate

A technology of organic thiosulfate and thiosulfate, applied in the direction of organic chemistry, can solve the problems of product yield reduction, inconvenience of industrial production, etc., and achieve the effect of solving acidity, simplifying the production process, and environmental protection of the preparation process

Active Publication Date: 2012-12-12
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this process reduces the pollution to the environment during the production process, the synthesis process can be reproduced according to this process, and the product can be smelled with a foul smell, indicating that there is a by-product thiol compound in the reaction process, which will bring inconvenience to industrial production.
In addition, after the reaction is completed, ethanol is added to continue to reflux, the temperature is lowered to 60-70°C, and then water is added, which will cause a certain amount of dihydrated hexamethylene 1,6-dithiosulfuric acid disodium salt to dissolve in the process. In water, after cooling down, crystallization still cannot be completed, thereby reducing the yield of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]A 200mL four-necked flask equipped with a mechanical stirring device, a thermometer, and a reflux condenser was used as a reaction vessel, and 12.4g of sodium thiosulfate pentahydrate and 0.75g of urea were weighed in the four-necked flask, and 100mL of water was added to dissolve after mechanical stirring. Add 3.9g of 1,6-dichlorohexane while stirring, heat up the above solution, and when the temperature of the reaction solution rises to 102°C, the pH value of the solution is 7. After stirring and reacting for 6 hours under reflux, pour out the solution and add 100mL of ethanol, the solution was left standing at 0°C for 1h, a large amount of solids precipitated, the solid product was filtered out, and dried at 55°C to obtain the disodium hexamethylene 1,6-dithiosulfate dihydrate.

Embodiment 2

[0034] A 200mL four-necked flask equipped with a mechanical stirring device, a thermometer, and a reflux condenser was used as a reaction vessel, and 24.8g of sodium thiosulfate pentahydrate and 5.0g of urea were weighed in the four-necked flask, and 100mL of water was added to dissolve with mechanical stirring. Add 7.8g of 1,6-dichlorohexane while stirring, heat up the above solution, raise the temperature of the reaction solution to 102°C, the pH value of the solution is 9, stir and react under reflux for 5h, pour out the solution and add 200mL Ethanol, after the solution was allowed to stand at 4°C for 3 hours, a large amount of solid precipitated out, the solid product was filtered out, and dried at 45°C to obtain dihydrate hexamethylene 1,6-dithiosulfate disodium salt.

Embodiment 3

[0036] A 200mL four-necked flask equipped with a mechanical stirring device, a thermometer, and a reflux condenser was used as a reaction vessel, and 49.6g of sodium thiosulfate pentahydrate and 6.0g of urea were weighed in the four-necked flask, and 100mL of water was added to dissolve with mechanical stirring. Add 15.5g of 1,6-dichlorohexane while stirring, heat up the above solution, make the temperature of the reaction solution rise to 102°C, the pH of the solution is 9, stir and react under reflux for 6h, pour out the solution and add 150mL of ethanol , put the solution at 10°C for 5h to precipitate a solid, filter out the solid product, and dry it at 55°C to obtain the disodium salt of hexamethylene 1,6-dithiosulfate dihydrate.

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Abstract

The present invention relates to an after-vulcanization stabilizer organic thiosulfate for rubber industry, and especially to a preparation method for an organic thiosulfate. According to the preparation method, urea is subjected to a hydrolysis reaction under a heating condition to generate NH3 to adjust the pH value of the reaction solution to an alkaline state, an organic halogenated alkane and a water-soluble inorganic thiosulfate can be subjected to a complete reaction, and generation of a byproduct thiol compound is inhibited, such that reaction efficiency is effectively improved, the resulting product has high purity, and the preparation process has characteristics of simpleness, easy performing, and low energy consumption.

Description

technical field [0001] The invention relates to a post-vulcanization stabilizer for rubber industry—organic thiosulfate, especially a preparation method of organic thiosulfate. Background technique [0002] Rubber is a chain-like polymer material, adding a vulcanizing agent can produce a cross-linking reaction with it, forming a three-dimensional network structure, making the rubber change from a plastic material to an elastic material, making the rubber highly elastic and flexible in a wide temperature range. Small plasticity, high strength performance. Sulfur vulcanized compounds undergo vulcanization reversion when the vulcanizate is overvulcanized during production or exposed to anaerobic heat aging conditions during use. In addition, the heat generated during use by many compounds is sufficient to cause crosslinking The degradation of the network, in turn, accelerates the generation of heat, so that the product is easily damaged and the service life is shortened, and t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C381/02
CPCC07C381/02
Inventor 董栋赵丽丽甄博鸣
Owner BEIJING RED AVENUE INNOVA
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