Preparation method of thiosulfuric acid derivative for rubber industry

A technology of thiosulfuric acid and rubber industry, which is applied in the direction of organic chemistry, can solve the problems of reducing the safety of the production process and the volatilization of organic solvents, and achieve the solution of acidification of the solution, improvement of product purity, and simple and easy preparation process Effect

Active Publication Date: 2013-01-02
BEIJING RED AVENUE INNOVA
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

This method uses irritating volatile organic solvents. During the heating reaction and recycling proce

Method used

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  • Preparation method of thiosulfuric acid derivative for rubber industry

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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 0.42g of sodium bicarbonate and 0.04g of sodium hydroxide were weighed, and 110mL of water was added to prepare sodium bicarbonate with a pH value of 9.6- Sodium hydroxide buffer solution was placed in a reaction vessel, and 13.6g of sodium thiosulfate pentahydrate was weighed and added to the above solution. After mechanical stirring and dissolving, 6.7g of 1,6-dibromohexane was added while stirring, and the temperature was raised and heated. For the above solution, the temperature of the reaction solution was raised to 102°C. After stirring and reacting for 5 hours under reflux, the solution was poured out and 110 mL of ethanol was added, and the solution was left to stand at 4°C for 3 hours. A large amount of solids precipitated, and the solid product was filtered out. After drying, dihydrate hexamethylene 1,6-dithiosulfate diso...

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 0.42g of sodium bicarbonate and 0.04g of sodium hydroxide were weighed, and 110mL of water was added to prepare sodium bicarbonate with a pH value of 9.6- Sodium hydroxide buffer solution was placed in a reaction vessel, and 23.6g of ammonium thiosulfate was weighed and added to the above solution. After mechanical stirring and dissolving, 12.4g of 1,6-dichlorohexane was added while stirring, and the temperature was raised to heat the above solution , raise the temperature of the reaction solution to 80°C, stir and react under reflux for 6h, pour out the solution and add 200mL of ethanol, leave the solution at 0°C for 2h, a large amount of solid precipitates, filter out the solid product, and dry it at 55°C That is, hexamethylene dihydrate 1,6-diammonium thiosulfate was obtained.

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 0.42g of sodium bicarbonate and 0.09g of sodium hydroxide were weighed, and 110mL of water was added to prepare a sodium bicarbonate with a pH value of 10.0- Sodium hydroxide buffer solution was placed in a reaction vessel, and 69.5g of sodium thiosulfate pentahydrate was weighed and added to the above solution. After mechanical stirring and dissolving, 24.1g of 1,6-dichlorohexane was added while stirring, and the temperature was raised and heated. For the above solution, raise the temperature of the reaction solution to 90°C, stir and react under reflux for 9h, then pour out the solution and add 600mL of ethanol, leave the solution at 10°C for 5h, a large amount of solids precipitate, filter out the solid product, 50°C After drying, dihydrate hexamethylene 1,6-dithiosulfate disodium salt is obtained.

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Abstract

The present invention relates to an after-vulcanization stabilizer thiosulfuric acid derivative for rubber industry, especially to a preparation method for a thiosulfuric acid derivative. According to the preparation method, an alkaline buffer solution is adopted to adjust the pH value of a reaction solution to an alkaline state, such that 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

field of invention [0001] The invention belongs to the field of post-vulcanization stabilizer materials used in the rubber industry, and in particular relates to a preparation method of thiosulfuric acid derivatives used in the rubber industry. Background technique [0002] As a new additive for rubber industry, dihydrate hexamethylene 1,6-dithiosulfate disodium salt (Duralink HTS), its unique chemical structure enables it to be used in macromolecular S-S during the vulcanization reaction. Soft hexamethylene groups are embedded between the bonds to form a composite cross-linked structure, which improves the thermal stability of the vulcanizate, so that the traditional vulcanization system containing Duralink HTS can better maintain dynamic properties, such as: tear and fatigue life. [0003] Duralink HTS is a metal sodium salt with an organic aliphatic chain, which is synthesized from organic halogenated hydrocarbons (1,6-dichlorohexane) and sodium thiosulfate. In 1983, U....

Claims

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Application Information

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IPC IPC(8): C07C381/02
Inventor 董栋赵丽丽甄博鸣
Owner BEIJING RED AVENUE INNOVA
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