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Preparation method of sulfhydryl silane coupling agent

A technology of mercaptosilane coupling agent and chloropropylalkoxysilane, which is applied in the field of preparation of mercaptosilane coupling agent, can solve problems such as agglomeration and increase in rubber viscosity, difficult control of product quality, and high energy consumption in the synthesis process. , to achieve the effect of reducing the viscosity of the rubber, stable quality, and reducing the generation of by-products

Active Publication Date: 2013-01-16
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although Si69 has been used for more than 30 years, Si75 has some advantages over Si69, but they also have many disadvantages in synthesis and use; such as: (1), the synthesis process is complicated, the post-processing is cumbersome, the product quality is difficult to control, and the quality is unstable
(2) The synthesis process consumes a lot of energy and discharges a lot of waste water
(3) The polysulfide bonds of Si69 and Si75 may be broken during use, which may easily cause the rubber to burn and require multiple mixing
(4) The ethanol produced by Si69 and Si75 during use will increase the porosity of the rubber due to its rapid gasification during high temperature mixing
(5) Agglomeration and viscosity increase of rubber are easy to occur during mixing

Method used

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  • Preparation method of sulfhydryl silane coupling agent
  • Preparation method of sulfhydryl silane coupling agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add thiooctanoic acid 647.6g and xylene 1000g in a 5000ml four-necked reaction flask with mechanical stirring, constant pressure dropping funnel and condenser, and drop 3-chloropropyltriethoxy in the constant pressure dropping funnel simultaneously Silane 972.9g. The molar ratio of thiooctanoic acid to 3-chloropropyltriethoxysilane is 1:1, and the amount of xylene added is 50%-100% of the total mass of thiooctanoic acid and 3-chloropropyltriethoxysilane 。 Then start the circulating water vacuum pump, and start the dropwise reaction under mechanical stirring at 400 rpm. The temperature of the reaction system is 80° C., and the dropwise time of 3-chloropropyltriethoxysilane is 4 hours. After the dropwise addition is completed, continue After reacting for 0.5 hours, the hydrogen chloride gas generated by the reaction was absorbed by water, and most of the system reaction had been completed at this time.

[0028] After 0.5 hours, the system was cooled to 40° C., and then 1...

Embodiment 2

[0031] Add thiooctanoic acid 647.6g and xylene 1150g in the 5000ml four-necked reaction flask with mechanical stirring, constant pressure dropping funnel and condenser, drop into 3-chloropropyltriethoxy in the constant pressure dropping funnel simultaneously Silane 972.9g. The molar ratio of thiooctanoic acid to 3-chloropropyltriethoxysilane is 1:1, and the amount of xylene added is 50%-100% of the total mass of thiooctanoic acid and 3-chloropropyltriethoxysilane . Then start the circulating water vacuum pump, and start the dropwise addition reaction under mechanical stirring at 450 rpm. The temperature of the reaction system is 100°C, and the dropwise addition time of 3-chloropropyltriethoxysilane is 3.5 hours. After the dropwise addition is completed, The reaction was continued for 0.5 hour, and the hydrogen chloride gas generated by the reaction was absorbed by water. At this time, the reaction had completed nearly a large part.

[0032] Then the reaction system was coole...

Embodiment 3

[0035] Add thiooctanoic acid 647.6g and xylene 1300g in the 5000ml four-necked reaction flask with mechanical stirring, constant pressure dropping funnel and condenser, drop into 3-chloropropyltriethoxy in the constant pressure dropping funnel simultaneously Silane 972.9g, the molar ratio of thiooctanoic acid to 3-chloropropyltriethoxysilane is 1:1, the amount of xylene added is 50% of the total mass of thioctanoic acid and 3-chloropropyltriethoxysilane %—100%. Then start the circulating water vacuum pump, and start the dropwise addition reaction under mechanical stirring at 400 rpm. The temperature of the reaction system is 135° C., and the dropwise addition time of 3-chloropropyltriethoxysilane is 3 hours. After the dropwise addition is completed, The reaction was continued for 0.5 hour, and the hydrogen chloride gas generated by the reaction was absorbed by water. At this time, the reaction had completed almost a large part.

[0036] Then the reaction system was cooled dow...

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Abstract

The invention relates to a preparation method of a sulfhydryl silane coupling agent, belonging to the field of organic chemistry. According to the invention, the reaction is firstly completed partially under reduced pressure, and a small amount of acid absorbent is added to complete the reaction, thereby reducing the generation of amine hydrochloride and the generation of the byproduct. The sulfhydryl silane coupling agent product prepared by the method has the advantages of high and stable quality, high yield and fewer impurities. The invention does not discharge waste water or pollute the environment, and can easily implement industrial production. The invention solves the problems of complex after-treatment, difficulty in control of product quality, unstable product quality, high energy consumption in the synthetic process, and high waste water discharge amount in the existing complex synthesis technique. The sulfhydryl silane coupling agent prepared by the method can lower the viscosity of rubber, reduce the number of stages of milling, improve the working properties of the rubber, accelerate the dispersion of the reinforcing agent, enhances the dynamic mechanical properties of the rubber and the ageing resistance of the tread rubber, and prolong the storage time of the rubber.

Description

technical field [0001] The invention relates to a preparation method of a mercaptosilane coupling agent, which belongs to the field of organic chemistry. Background technique [0002] At present, the silane coupling agents used in the tire manufacturing industry are almost all sulfur-containing silane coupling agents, of which the most commonly used are bis(triethoxysilylpropyl)tetrasulfide (TESPT) and bis(triethyl Oxysilylpropyl) disulfide (TESPD) two. In 1973, Degussa company first used TESPT as a tackifier, and later used it in tires and found that it can significantly improve the grip of tires. In 1976, when Degussa company first started the industrial production of TESPT in Belgium, it named it Si69. After entering the 1990s, with the rise of green tire technology, this product was quickly used in a large number in the tire industry. [0003] Si69 reacts with white carbon black and other fillers during the rubber mixing process, and forms a coupling bond with the rubb...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 王欣陈圣云刘宇阮少阳胡江华王灿甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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