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Organic thiosulfuric acid derivative preparation method

A technology of organic thiosulfuric acid and sodium thiosulfate is applied in the field of preparation of organic thiosulfuric acid derivatives to achieve the effects of avoiding post-treatment, developing prospects and reducing pollution

Active Publication Date: 2014-04-09
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Though adopting disclosed preparation method can obtain product---organothiosulfuric acid derivative, because sodium thiosulfate and organic thiosulfuric acid derivative---hexamethylene 1,6-dithiosulfuric acid disodium salt all Soluble in water, insoluble in organic solvents, making it difficult to purify organic thiosulfuric acid derivatives with sodium thiosulfate impurities

Method used

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  • Organic thiosulfuric acid derivative preparation method

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Experimental program
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Effect test

Embodiment 1

[0024] 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 was weighed in the four-necked flask, and 100mL of water was added into the four-necked flask with mechanical stirring to dissolve, and 3.9 g1,6-dichlorohexane, heat up the above solution, and when the temperature of the reaction solution rises to 100°C, slowly add 1% sodium hydroxide solution through a peristaltic pump to adjust the pH value of the reaction solution to 7.5. After stirring and reacting for 6 hours, stop adding the sodium hydroxide solution, add dropwise a 0.05% hydrochloric acid solution to adjust the pH value of the solution to 7, pour out the solution, filter and leave it at 4°C for 3 hours, and a large amount of solids will precipitate out. The solid product was dried at 45°C to obtain the disodium salt of hexamethylene 1,6-dithiosulfate dihydrate.

Embodiment 2

[0026] 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 was weighed in the four-necked flask, and 100mL of water was added into the four-necked flask with mechanical stirring to dissolve, and 7.4 g1,6-dichlorohexane, heat up the above solution, and when the temperature of the reaction solution rises to 90°C, slowly add 1.2% sodium hydroxide solution through a peristaltic pump to adjust the pH value of the reaction solution to 7. After stirring and reacting for 9 hours, stop adding the sodium hydroxide solution, add dropwise a 0.5% hydrochloric acid solution to adjust the pH value of the solution to 6.5, pour the solution out, filter and stand at 0°C for 1 hour, a large amount of solids precipitate out, and filter out The solid product was dried at 55°C to obtain the disodium salt of hexamethylene 1,6-dithiosulfate dihydrate.

Embodiment 3

[0028] A 200mL four-necked flask equipped with a mechanical stirring device, a thermometer and a reflux condenser was used as a reaction vessel, and 52.1g of sodium thiosulfate pentahydrate was weighed in the four-necked flask, and 100mL of water was added to the four-necked flask with mechanical stirring to dissolve, while stirring, 14.8 g1,6-dichlorohexane, heat up the above solution, and when the temperature of the reaction solution rises to 115°C, slowly add 2% sodium hydroxide solution through a peristaltic pump to adjust the pH value of the reaction solution to 9. After stirring and reacting for 6 hours, stop adding the sodium hydroxide solution, add dropwise a 0.1% hydrochloric acid solution to adjust the pH value of the solution to 7, pour the solution out, filter and leave it standing at 5°C for 1 hour, and a large amount of solids precipitate out. The solid product was dried at 45°C to obtain the disodium salt of hexamethylene 1,6-dithiosulfate dihydrate.

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Abstract

The invention provides an organic thiosulfuric acid derivative preparation method. The method specifically includes the steps: synthesizing organic thiosulfuric acid derivative in alkaline aqueous solution, adding acid solution to convert unreacted inorganic thiosulfate into other inorganic salts, filtering, and precipitating the organic thiosulfuric acid derivative from the solution by means of cooling and crystallizing. By the organic thiosulfuric acid derivative prepared by the method, influences of the inorganic thiosulfate in the product can be effectively reduced, so that product purity is improved. In addition, the preparation method is simple, feasible and environment-friendly, no organic solvent is added during preparation, and accordingly environment pollution during production is reduced.

Description

technical field [0001] The invention belongs to the field of organic thiosulfuric acid derivative materials for post-vulcanization stabilizers used in the rubber industry, and in particular relates to a preparation method of organic thiosulfuric acid derivatives. Background technique [0002] Monsanto Corporation of the United States originally developed Duralink HTS (dihydrated hexamethylene 1,6-dithiosulfate disodium salt) in the 1980s to improve the stability of polysulfide crosslinks, but later found that it It also increases operational safety. Duralink HTS contains sulfur atoms and carbon atoms. During vulcanization, HTS inserts a hexamethylene disulfide group in the polysulfide crosslinking bond, and a longer soft and thermally stable alkyl group is embedded in the crosslinking bond structure. The formation of such composite cross-linking bonds can improve the anaerobic aging resistance of the vulcanized rubber, improve the thermal stability of the cross-linking bond...

Claims

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Application Information

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