Preparation method of thiosulfuric acid derivative for rubber industry

A technology of thiosulfuric acid and the rubber industry, which is applied in the field of preparation of thiosulfuric acid derivatives for the rubber industry, 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, The effect of improving safety

Active Publication Date: 2014-07-02
BEIJING RED AVENUE INNOVA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses irritating volatile organic solvents. During the heating reaction and recycling process, the organic solvents are easy to volatilize, thereby reducing the safety of the production process.

Method used

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  • Preparation method of thiosulfuric acid derivative for rubber industry

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Comparison scheme
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 0.42g of sodium bicarbonate and 0.04g of sodium hydroxide were weighed, and 110mL of water was added to prepare a sodium bicarbonate with a pH value of 9.6- Sodium hydroxide buffer solution was placed in a reaction vessel, 13.6g of sodium thiosulfate pentahydrate was weighed, added to the above solution, after mechanical stirring to dissolve, 6.7g of 1,6-dibromohexane was added while stirring, and the temperature was heated. For the above solution, the temperature of the reaction solution was raised to 102 °C, and after stirring the reaction for 5 h under reflux conditions, the solution was poured out and 110 mL of ethanol was added. After drying, hexamethylene dihydrate 1,6-dithiosulfate disodium salt is obtained.

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 a sodium bicarbonate with a pH value of 9.6- Sodium hydroxide buffer solution was placed in a reaction vessel, 23.6g of ammonium thiosulfate was weighed, added to the above solution, after mechanical stirring to dissolve, 12.4g of 1,6-dichlorohexane was added while stirring, and the above solution was heated with temperature , the temperature of the reaction solution was raised to 80 °C, and after stirring the reaction for 6 h under reflux conditions, the solution was poured out and 200 mL of ethanol was added. That is, hexamethylene dihydrate 1,6-dithiosulfate diammonium salt is 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 the reaction vessel, 69.5g of sodium thiosulfate pentahydrate was weighed, added to the above solution, after mechanical stirring to dissolve, 24.1g of 1,6-dichlorohexane was added while stirring, and the temperature was heated. For the above solution, the temperature of the reaction solution was raised to 90 °C, and after the reaction was stirred for 9 h under reflux conditions, the solution was poured out and 600 mL of ethanol was added. After drying, hexamethylene dihydrate 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 particularly relates to a preparation method of a thiosulfuric acid derivative used in the rubber industry. Background technique [0002] As a new type of auxiliary agent for the rubber industry, hexamethylene 1,6-dithiosulfate disodium salt (Duralink HTS), its unique chemical structure enables it to react in the vulcanization reaction of macromolecular S-S 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: tearing and fatigue life. [0003] Duralink HTS is a metal sodium salt with organic aliphatic chain, which is synthesized from organic halogenated hydrocarbon (1,6-dichlorohexane) and sodium thiosulfate. In 1983, U...

Claims

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Application Information

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