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Purification method of isocyanate silane coupling agent and isocyanate silane coupling agent

A technology of ester silane coupling agent and purification method, which is applied in the field of isocyanate silane coupling agent products, can solve the problems of affecting the yield of rectification products, more rectification raffinate, and less addition, so as to achieve prominent economic value and reduce Three wastes, strong applicability

Pending Publication Date: 2020-12-11
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the process of rectification and purification of the crude product containing isocyanate silane coupling agent in the prior art, it is unavoidable to bring other active impurity groups, and the double bond addition reaction or polymerization reaction of isocyanate group is prone to occur under the heat of rectification. Cause more rectification raffinate, affect the problem of rectification product yield, the object of the present invention is to provide a kind of purification method of isocyanate silane coupling agent and the isocyanate silane coupling agent product obtained by using the purification method, the purification method It is especially suitable for the purification of isocyanate silane coupling agent prepared by thermal cracking method. The materials added in the purification process are cheap and easy to obtain and the amount of addition is small. The process is simple and hardly increases the manufacturing cost. Bulk polymerization and other side reactions when distillation is heated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Get 500g of crude product containing isocyanatopropylmethyldimethoxysilane, gas chromatography (GC-2014, Shimadzu company) detects that the content of isocyanatopropylmethyldimethoxysilane is 76%, and other impurity components include methanol 3.2%, Methyldimethoxysilylpropylcarbamate 18%. 0.5 g of formyl chloride was added thereto, and stirred to make it uniformly mixed. Then by rectification under reduced pressure, 348g of 90°C-96°C / 15mmHg cuts were collected, and the content of isocyanatopropylmethyldimethoxysilane was detected by gas chromatography (GC-2014, Shimadzu company) to be 97.2%. The rate is 91.6%.

Embodiment 2

[0040] Get 300g of the crude product containing isocyanatopropyl trimethoxysilane, gas chromatography (GC-2014, Shimadzu company) detects that the content of isocyanatopropyl trimethoxysilane is 43.8%, and other impurity components include methanol 2.7%, trimethoxy Methyl silyl propyl carbamate 51.2%. 1.5 g of trifluoropropionyl chloride was added thereto, and stirred to mix uniformly. Then by rectification under reduced pressure, 110 g of 100° C.-110° C. / 15mmHg cuts were collected, and the content of isocyanatopropyl trimethoxysilane detected by gas chromatography (GC-2014, Shimadzu company) was 98.1%, and the rectification yield was 84 %.

Embodiment 3

[0044] Get the crude product 300g containing isocyanatopropyl triethoxysilane, gas chromatography (GC-2014, Shimadzu company) detection isocyanatopropyl triethoxysilane content is 82%, other impurity components include ethanol 0.6%, three Ethoxysilylpropyl Urethane 14.2%. 1 g of ethylsulfonyl chloride was added thereto, and stirred to make the mixture uniform. Then by rectification under reduced pressure, 229g of 120°C-128°C / 15mmHg cuts were collected, and the content of isocyanatopropyl triethoxysilane detected by gas chromatography (GC-2014, Shimadzu company) was 98.6%, and the rectification yield was 93%.

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PUM

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Abstract

The invention discloses a purification method of an isocyanate silane coupling agent and the isocyanate silane coupling agent, alkyl carbonyl chloride or alkyl sulfonyl chloride is added into a crudeproduct containing the isocyanate silane coupling agent in a nitrogen atmosphere, after full mixing, vacuum distillation is carried out, and the isocyanate silane coupling agent is obtained. The method disclosed by the invention has the beneficial effects that the method is suitable for purifying the isocyanate silane coupling agent prepared by adopting a thermal cracking method, the raw materialsare cheap and easy to obtain, the addition amount is small, the process is simple, the manufacturing cost is hardly increased, and side reactions such as bulk polymerization and the like generated when the isocyanate silane coupling agent is rectified and heated can be effectively inhibited.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry, and specifically relates to a method for purifying an isocyanate silane coupling agent and an isocyanate silane coupling agent product obtained by using the purification method. Background technique [0002] Isocyanate silane coupling agent is a special silane coupling agent, which can be widely used in the fields of polymer materials such as adhesives and resin structure improvement of polyurethane materials. or adhesion to metal substrates. According to public information, the current chemical methods for synthesizing isocyanate-containing silane coupling agents mainly include the following: [0003] The phosgene method is used to prepare the isocyanate silane coupling agent, usually using aminoalkylsilane to react with phosgene or triphosgene. As described in US3584024, in organic solvents, such as: benzene, toluene, xylene, chlorobenzene, methylene chloride, chloroform, ether, tet...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C07F7/20
CPCC07F7/1804C07F7/20
Inventor 杨志勇沈鸣张先林曹娜赵亚娟
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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