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Method for preparing mercaptosilicane coupling agent with low VOC (volatile organic compounds) emission

A technology of mercaptosilane coupling agent and chloropropyltrichlorosilane, which is applied in the field of preparation of mercaptosilane coupling agent, can solve the problems of large waste water discharge, scorched rubber material, and increased porosity of rubber, and achieve product High quality, low cost, and the effect of reducing viscosity

Active Publication Date: 2015-04-29
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 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, which is also not conducive to environmental protection
(5) Agglomeration and viscosity increase of rubber are easy to occur during mixing

Method used

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  • Method for preparing mercaptosilicane coupling agent with low VOC (volatile organic compounds) emission
  • Method for preparing mercaptosilicane coupling agent with low VOC (volatile organic compounds) emission

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Drop into 212g of chloropropyltrichlorosilane in a 2000ml four-necked reaction flask with magnetic stirring, constant pressure dropping funnel and low temperature condenser, and drop into 841g of isomeric tridecyl alcohol polyoxyethylene ether in the constant pressure dropping funnel, Start the magnetic stirring, raise the temperature to 130°C, start the circulating water vacuum pump, and start the dropwise addition of isotridecyl alcohol polyoxyethylene ether to carry out the primary esterification reaction. The reaction time is 4 hours, and the hydrogen chloride gas generated by the reaction is absorbed by water. After the isomeric tridecyl alcohol polyoxyethylene ether dropwise reaction is completed, keep the reaction temperature of the system at 130°C, add 46g of ethanol to the constant pressure dropping funnel at the same time, continue to add ethanol dropwise for secondary esterification reaction, and the reaction time for 2 hours. After the reaction, 980 g of iso...

Embodiment 2

[0025] Drop into 212g of chloropropyltrichlorosilane in a 2000ml four-necked reaction flask with magnetic stirring, constant pressure dropping funnel and low temperature condenser, and drop into 841g of isomeric tridecyl alcohol polyoxyethylene ether in the constant pressure dropping funnel, Start the magnetic stirring, raise the temperature to 120°C, start the circulating water vacuum pump, and start the dropwise addition of isotridecyl alcohol polyoxyethylene ether to carry out the primary esterification reaction. The reaction time is 6 hours, and the hydrogen chloride gas generated by the reaction is absorbed by water. After the isomeric tridecyl alcohol polyoxyethylene ether dropwise reaction is completed, keep the reaction temperature of the system at 120°C, add 46g of ethanol to the constant pressure dropping funnel at the same time, continue to add ethanol dropwise to carry out the secondary esterification reaction, and the reaction time for 3 hours. After the reaction,...

Embodiment 3

[0028] Drop into 212g of chloropropyltrichlorosilane in a 2000ml four-necked reaction flask with magnetic stirring, constant pressure dropping funnel and low temperature condenser, and drop into 841g of isomeric tridecyl alcohol polyoxyethylene ether in the constant pressure dropping funnel, Start the magnetic stirring, raise the temperature to 110°C, start the circulating water vacuum pump, and start the dropwise addition of isotridecyl alcohol polyoxyethylene ether to carry out the primary esterification reaction. The reaction time is 8 hours, and the hydrogen chloride gas generated by the reaction is absorbed by water. After the isomeric tridecyl alcohol polyoxyethylene ether dropwise reaction is completed, keep the reaction temperature of the system at 110°C, add 46g of ethanol to the constant pressure dropping funnel at the same time, continue to add ethanol dropwise for secondary esterification reaction, and the reaction time for 4 hours. After the reaction finishes, pro...

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Abstract

The invention relates to a method for preparing a mercaptosilicane coupling agent with low VOC (volatile organic compounds) emission, and belongs to the field of organic chemistry. The method comprises the steps of performing primary esterification on alkyl polyether alcohol and chloropropyl trichlorosilane under reduced pressure at a certain reaction temperature, and continuously removing the generated hydrogen chloride gas so that the esterification reaction is complete; then further adding ethanol for secondary esterification; and performing sulfhydrylation reaction, dissolving anhydrous sodium hydrosulfide into ethanol, and reacting the mixture with newly synthesized chloropropyl trialkoxysilane to obtain the mercaptosilicane coupling agent with low VOC emission. The product prepared by the method has high and stable quality, high yield and few impurities. Through use of the method, wastewater is not discharged, the environment is not polluted and industrialized production is facilitated. The silicon unit of the product only contains 33% of volatile ethoxy groups, so the decrement of VOC can reach over 80%, pollution discharge in the mixing process can be controlled, and the requirement for environment-friendly products can be met.

Description

technical field [0001] The invention relates to a preparation method of a mercaptosilane coupling agent with low VOC emission, belonging to the field of organic chemistry. Background technique [0002] As early as the 1990s, with the improvement of people's requirements for tire performance, the silica-silane filling system was used in the tread rubber of car tires. After mixing with solution-polymerized styrene-butadiene rubber, this filling system can significantly improve the performance of tires. Performance of car tires. Among them, the epoch-making polysulfide functional organosilanes are mainly bis(triethoxysilylpropyl) tetrasulfide (TESPT, Si69) and bis(triethoxysilylpropyl) disulfide (TESPD, Si69) These two are products that, in addition to precipitated silica, can greatly improve wet road grip and reduce rolling resistance. [0003] Although Si69 has been used for more than 30 years, Si75 has some advantages over Si69, but they also have many disadvantages in the...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 王欣甘俊刘宇陈圣云甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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