Method for preparing chloropropyl alkyl alkoxy silicon hydride by passage reaction device

A technology of chloropropylalkylalkoxysilane and channel reaction device, which is applied in the fields of chemical instruments and methods, compounds of group 4/14 elements of the periodic table, organic chemistry, etc., and can solve problems such as unseen large-scale production. Achieve the effect of shortening post-processing working hours, sufficient response, and high output flexibility

Active Publication Date: 2016-06-22
南京曙光新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are few reports on the application of channel reaction devices to the large-scale industrial production of chloropropylalkylalkoxysilanes, at least no real large-scale production has been seen.

Method used

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  • Method for preparing chloropropyl alkyl alkoxy silicon hydride by passage reaction device
  • Method for preparing chloropropyl alkyl alkoxy silicon hydride by passage reaction device
  • Method for preparing chloropropyl alkyl alkoxy silicon hydride by passage reaction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Embodiment 1 prepares 3-chloropropyltriethoxysilane

[0054] The raw material chloropropyltrichlorosilane (content 98.9%) is preheated to 60°C, and absolute ethanol (content 99.6%) is heated into ethanol vapor. The two raw materials enter the channel reaction device with a mass ratio of 212:140 for reaction. Control the flow rate of the reaction flow to 30Kg / h, and the reaction temperature to 120°C. Take the crude product from the collection device for gas chromatography detection, and take a hydrochloric acid sample from the water absorption device to observe the appearance. The test result is that the ethanol content in the crude product is 0.6%, not completely The content of esterified intermediate product is 0.2%, the content of 3-chloropropyltriethoxysilane is 96.9%, and the content of polymer is <0.1%. The hydrochloric acid in the water absorption device is transparent and free of suspended hydrolyzed silane.

Embodiment 2

[0055] Embodiment 2 prepares 3-chloropropyl methyl dimethoxysilane

[0056] The raw material chloropropylmethyldichlorosilane (content 99.2%) is preheated to 50°C, and anhydrous methanol (content 99.8%) is heated into methanol vapor, and the two raw materials enter the channel reaction device with a mass ratio of 191.5:65. Reaction, the flow rate of the reaction flow is controlled to be 30Kg / h, and the reaction temperature is 115°C. The crude product is taken from the collection device for gas chromatography detection, and the hydrochloric acid sample is taken from the water absorption device to observe the appearance. The test results are that the methanol content in the crude product is 0.4%, The content of incompletely esterified intermediate products is 0.2%, the content of 3-chloropropylmethyldimethoxysilane is 98.9%, and the content of polymers is <0.1%. The hydrochloric acid in the water absorption device is transparent and there is no suspended hydrolyzed silane.

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Abstract

The invention aims at providing a method for preparing chloropropyl alkyl alkoxy silicon hydride by a passage reaction device for industrial chloropropyl alkyl alkoxy silicon hydride production, so that chloropropyl chloride-containing silicon hydride and excessive alcohol take esterification reaction in the passage reaction device for preparing the chloropropyl alkyl alkoxy silicon hydride, wherein (1) the structure general formula (a) of the chloropropyl chloride-containing silicon hydride is ClC3H6SiCl<n>R<3-n>, in the formula, R is methyl or ethyl, and n=1, 2 or 3; (2) alcohol is methanol or ethanol, and enters the passage reaction device in a gas phase form; (3) the passage reaction device is at least connected with a posttreatment device and a hydrogen chloride absorption device. The problems of difficulty in regulation of yield and amplification effect and the like of large-sized reaction equipment are solved; the defects caused by the large-sized equipment are weakened or even eliminated.

Description

technical field [0001] The invention relates to a method for preparing chloropropylalkylalkoxysilane by esterification reaction between chloropropyl chlorosilane and alcohol, more specifically a method for preparing chloropropylalkylalkoxysilane by using a channel reaction device. Background technique [0002] The method of preparing chloropropyl alkyl alkoxysilane by esterification reaction of chloropropyl chlorosilane and alcohol is known, such as the reaction of 3-chloropropyl trichlorosilane with ethanol to prepare 3-chloropropyl triethyl Oxysilane, 3-chloropropyltrichlorosilane reacts with methanol to prepare 3-chloropropyltrimethoxysilane, 3-chloropropylmethyldichlorosilane reacts with methanol to prepare 3-chloropropylmethyldimethoxysilane 3-Chloropropylmethyldiethoxysilane is prepared by reacting 3-chloropropylmethyldichlorosilane with ethanol. This type of esterification reaction will produce by-product hydrogen chloride, which will react with raw material alcohol ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/188
Inventor 陶再山李春华
Owner 南京曙光新材料有限公司
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