Clean production method of 3-chloropropyltrialkoxysilane

A technology of chloropropyltrialkoxysilane and chloropropyltrichlorosilane, which is applied in the field of 3-chloropropyltrialkoxysilane clean production process and can solve the problem of 3-chloropropyltrialkoxysilane production Problems such as complex process, high recycling cost and complicated equipment can achieve the effect of increasing the rate of esterification reaction, reducing production cost and simplifying equipment

Active Publication Date: 2014-10-08
江西晨光新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the deficiencies of the prior art, to meet the needs of reality, to provide a clean production method for 3-chloropropyltrialkoxysilane, aiming to solve the existing 3-chloropropyltrialkoxysilane production process Technical issues such as complexity, low efficiency, complex equipment, high energy consumption, and high recycling costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0028] Specific embodiment 1: First, add 142.6kg of absolute ethanol into the alcohol storage tank, and after it is gasified to 100°C by a heater at a rate of 15L / min, it is sent to the esterification reaction tower by a booster pump to adjust the ester The temperature in the reaction tower is brought to 100°C, and the vaporized ethanol gas is continuously input to increase the pressure in the esterification reaction tower to 0.15Mpa; after that, 212kg of 3-chloropropyltrichlorosilane is esterified at a rate of 2L / min. The top of the reaction tower is input into it. At this time, the esterification reaction begins. Control the ethanol gas flow rate to keep the pressure in the esterification reaction tower at 0.15Mpa and control the flow rate of 3-chloropropyltrichlorosilane to ensure the esterification The molar ratio of ethanol to 3-chloropropyltrichlorosilane in the reaction tower (alcohol: 3-chloropropyltrichlorosilane) is 3.1; after the feeding is completed, continue the est...

specific Embodiment 2

[0030] Specific embodiment 2, the same as in embodiment 1 will not be stated again, the difference is: after the anhydrous methanol is vaporized, it is heated to 120°C and passed through a booster pump at a rate of 50L / min from the bottom of the esterification reaction tower Input, the temperature of the esterification reaction tower rises to 120°C, after the pressure in the tower reaches 0.2Mpa, 3-chloropropyltrichlorosilane is fed from the top of the esterification reaction tower at a rate of 2.5L / min, and the pressure inside the tower remains 0.2 Mpa, to ensure that the molar ratio of ethanol to 3-chloropropyltrichlorosilane (alcohol: 3-chloropropyltrichlorosilane) in the esterification reaction tower is 10; after the feeding is completed, the esterification will continue for 50 min. The crude esterification reaction product is collected at the bottom of the chemical reaction tower and further subjected to rectification and separation treatment to obtain 3-chloropropyltrimeth...

specific Embodiment 3

[0032] Specific embodiment 3, the same as in embodiment 1 will not be stated again, the difference is: the anhydrous ethanol is heated to 150°C for vaporization, and is fed from the bottom of the esterification reaction tower through a booster pump at a rate of 20L / min. The temperature of the chemical reaction tower was raised to 150°C. After the pressure in the tower reached 0.3Mpa, 3-chloropropyltrichlorosilane was fed from the top of the esterification reaction tower at a rate of 2.5L / min. The pressure in the tower was maintained at 0.2Mpa to ensure The molar ratio of ethanol to 3-chloropropyltrichlorosilane in the esterification reaction tower (alcohol: 3-chloropropyltrichlorosilane) is 5; after the feed is completed, continue the esterification for 80 min, then the esterification reaction tower The crude product of the esterification reaction is collected at the bottom, the ethanol in the crude product is returned to the ethanol gasification line after fractional distillati...

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Abstract

The invention discloses a clean production method of 3-chloropropyltrialkoxysilane, which aims to solve the technical problems of complex procedure, low efficiency, complex equipment, high energy consumption and high recovery cost in the existing 3-chloropropyltrialkoxysilane production. The method comprises the following steps: a. gasifying alcohol, and delivering into an esterification reaction tower via a booster pump; b. controlling the atmospheric pressure in the esterification reaction tower at 0.15-1 Mpa, and keeping the temperature in the esterification reaction tower at 100-200 DEG C; c. delivering 3-chloropropyltrichlorosilane into the esterification reaction tower, and controlling the mole ratio of the alcohol to the 3-chloropropyltrichlorosilane in the esterification reaction tower at 3.1-10; and d. after the esterification reaction is carried out for 50-80 minutes, detecting the 3-chloropropyltrichlorosilane content in the crude product by using a gas phase chromatograph, finishing the reaction when the content is lower than 0.1%, and carrying out rectification separation treatment on the crude product. The method can enhance the esterification reaction rate and reduce the production procedures, thereby avoiding the discharge of hydrogen chloride and being an environment-friendly closed-cycle production technique.

Description

Technical field [0001] The invention relates to a clean production process of 3-chloropropyltrialkoxysilane, in particular to a clean production method of 3-chloropropyltrialkoxysilane. Background technique [0002] 3-chloropropyltrialkoxysilane is an important silane coupling agent, which mainly includes 3-chloropropyltriethoxysilane and 3-chloropropyltrimethoxysilane, and both are also Production of other silane coupling agents (such as 3-aminopropyltrialkoxysilane, 3-mercaptopropyltrialkoxysilane, 3-acryloxypropyltrialkoxysilane, silane coupling agent Si- 69. Important raw material for silane coupling agent Si-75, etc.). At present, the process flow for producing 3-chloropropyltrialkoxysilane is as follows: 1. Hydrogen chloride gas and silicon powder are reacted to prepare trichlorosilane; 2. Trichlorosilane and 3-chloropropene are prepared by hydrosilylation reaction 3-chloropropyltrichlorosilane; 3,3-chloropropyltrichlorosilane and alcohol are esterified to prepare the tar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 丁建峰梁秋鸿葛利伟刘广生刘建华
Owner 江西晨光新材料股份有限公司
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