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Method for preparing mercaptopropyltriethoxysilane through constant-pressure low-temperature aqueous phase

A technology of mercaptopropyltriethoxysilane coupling agent and chloropropyltriethoxysilane, which is applied in the field of preparing high-purity mercaptopropyltriethoxysilane in low-temperature aqueous phase at normal pressure, and can solve the problem of temperature rise, etc. problems, to achieve the effect of reducing production energy consumption, avoiding harsh requirements, and shortening reaction time

Active Publication Date: 2015-09-23
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And one-time addition is easy to make the temperature of the system rise too fast, thus forming a gel

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Install a condenser tube, a mechanical stirrer, and a thermometer in a 500mL four-neck flask and fix it in a water bath heating pot. Put 110g of γ-chloropropyltriethoxysilane into the flask, add 2.4g of 12-crown-4, start stirring, and raise the temperature to 70°C within 30 minutes, and keep it warm for 10 minutes. Add 81g mass fraction of 45% sodium hydrosulfide solution and 16g mass fraction of 50% sodium bisulfite aqueous solution simultaneously in the above solution, and add dropwise in three times, each dripping mass accounts for 1 / 3rd of the total feed liquid mass One, the dropping time is 40 minutes, and the interval between each dropping is 1 hour. After adding all the feed liquids dropwise, increase the stirring speed to continue the reaction. During the reaction, the crude product of the upper organic phase is detected and analyzed by gas chromatography, and the reaction is stopped when the content of γ-chloropropyltriethoxysilane is lower than 1.5%. The feed...

Embodiment 2

[0021] Install a condenser tube, a mechanical stirrer, and a thermometer in a 500mL four-neck flask and fix it in a water bath heating pot. Put 110g of γ-chloropropyltriethoxysilane into the flask, add 2.4g of 18-crown-6, start stirring, and raise the temperature to 70°C within 30 minutes, and keep it warm for 10 minutes. Add 81g mass fraction of 45% sodium hydrosulfide solution and 16g mass fraction of 50% sodium bisulfite aqueous solution simultaneously in the above solution, and add dropwise in three times, each dripping mass accounts for 1 / 3rd of the total feed liquid mass 1. The dropping time is 40 minutes, and the interval between each dropping is 1 hour. After all the feed liquids are added dropwise, increase the stirring speed to continue the reaction. During the reaction, take the crude product of the upper organic phase and use gas chromatography to detect and analyze it. The reaction is stopped when the content of propyltriethoxysilane is lower than 1.5%. The feed ...

Embodiment 3

[0024] Install a condenser tube, a mechanical stirrer, and a thermometer in a 500mL four-neck flask and fix it in a water bath heating pot. Put 110g of γ-chloropropyltriethoxysilane into the flask, add 2.4g of 15-crown-5, start stirring, and raise the temperature to 70°C within 30 minutes, and keep it warm for 10 minutes. Add 81g mass fraction of 45% sodium hydrosulfide solution and 16g mass fraction of 50% sodium bisulfite aqueous solution simultaneously in the above solution, and add dropwise in three times, each dripping mass accounts for 1 / 3rd of the total feed liquid content 1. The dropping time is 40 minutes, and the interval between each dropping is 1 hour. After all the feed liquids are added dropwise, increase the stirring speed to continue the reaction. During the reaction, take the crude product of the upper organic phase and use gas chromatography to detect and analyze it. The reaction is stopped when the content of propyltriethoxysilane is lower than 1.5%. The fe...

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Abstract

The invention relates to a method for preparing mercaptopropyltriethoxysilane through a constant-pressure low-temperature aqueous phase. The invention discloses a preparation method of a gamma-mercaptopropyltriethoxysilane coupling agent. The method is characterized by comprising the following steps of under constant pressure, gamma-chloropropyltriethoxysilane and crown ether are stirred uniformly, a sodium hydrosulfide solution and a pH regulation agent are matched and are added to a mixed solution drop by drop many times, and after the sodium hydrosulfide solution and the pH regulation agent are added drop by drop and when the content of the gamma-chloropropyltriethoxysilane is lower than 1.5%, the reaction is stopped; reaction liquid is cooled and separated so as to obtain crude products, distillation under reduced pressure is performed on the obtained crude products, and condensate of which the gas-phase temperature is higher than or equal to 78 DEG C is collected to be used as finished products. The method disclosed by the invention has the advantages that the technological production is stable, the cost is low, and synthetic products are high in purity, transparent in color and stable in storability.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to the synthesis of a mercaptoalkylsilane coupling agent, in particular to a method for preparing high-purity mercaptopropyltriethoxysilane from an aqueous phase at normal pressure and low temperature. Background technique [0002] γ-mercaptopropyltriethoxysilane, its trade name is KH-580, WD80. Mercaptosilane is a bifunctional coupling agent, which can be filled with resins, elastomers, fibers, metals, minerals and glasses to improve the mechanical and electrical properties of the system. As a class of widely used organosilicon compounds, mercaptoalkoxysilanes are used to treat fillers in the rubber and plastic industries, and their effects are also ideal. Mercaptoalkylsilane can not only be used as a coupling agent in large quantities, but also can develop new silicone resin and rubber products with photocurable properties by utilizing the characteristic of addition reaction betwee...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 王伟方伟陈向前刘继佘慧玲朱晓英刘晓凤来立群
Owner ZHEJIANG XINAN CHEM INDAL GROUP
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