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Preparation method for 3- isocyanate propyl (trimethylsilanolate) silane

A technology of ester group propyltrialkoxysilane and trimethylsiloxy, which is applied in the field of organic synthesis, can solve problems such as unseen technical routes and reports, and achieve the effect of simple process routes

Inactive Publication Date: 2012-09-12
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing research on the synthesis of isocyanatopropyl tris(trimethylsiloxy)silane products, due to the existence of highly active group isocyanate groups, it is difficult to prepare by traditional methods, and there is no current method in various documents. Technical route report

Method used

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  • Preparation method for 3- isocyanate propyl (trimethylsilanolate) silane
  • Preparation method for 3- isocyanate propyl (trimethylsilanolate) silane
  • Preparation method for 3- isocyanate propyl (trimethylsilanolate) silane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a three-necked flask containing 207.0 g (1.0 mol) of isocyanatopropyl trimethoxysilane and 486.0 g (3.0 mol) of hexamethyldisiloxane, add concentrated sulfuric acid (20.8 g, 3%) and stir to 60~62℃, react at 60~62℃ for 12 hours, then gradually increase the temperature to 120±2℃, and react at a constant temperature of 120±2℃. During the reaction process, the trimethylmethoxysilane is continuously extracted under normal pressure. In order to promote the reaction to the right, improve the reaction efficiency and shorten the reaction time; take a sample after a constant temperature of 120±2°C for 6 hours, and detect it by gas chromatography GC-2014 (Island Feng), when the content of isocyanatopropyltrimethoxysilane in the reaction mixture When the content of isocyanatopropylmethoxy bis(trimethylsiloxy)silane is less than 1% (about 8h), the reaction is over; the reaction mixture is cooled at 30-60°C and the pressure is 2-10KPa Remove residual trimethylmethoxysilane and unr...

Embodiment 2

[0026] In a three-necked flask containing 249.0 g (1.0 mol) of isocyanatopropyl triethoxysilane and 486.0 g (3.0 mol) of hexamethyldisiloxane, add trifluoromethanesulfonic acid (0.735 g, 0.1%) Raise the temperature to 80°C under stirring, and react at 80±2°C for 24 hours, then gradually increase the temperature to 120±2°C, and react at a constant temperature of 120±2°C. Sampling after constant temperature 6h, detect by gas chromatography GC-2014 (Island Feng), when the content of isocyanate propyl triethoxysilane in the reaction mixture is less than 0.2%, and isocyanate propyl ethoxy di( When the content of trimethylsilyl)silane is less than 1% (about 10h), stop the reaction; cool the resulting mixture, and remove the residual trimethylethoxy silicon in the mixture at 60-100°C and a pressure of 10-30KPa and unreacted hexamethyldisiloxane to obtain a mixture containing isocyanatopropyl tris(trimethylsiloxy)silane with a content of 85.7835%, 421.9 g.

[0027] The above mixture ...

Embodiment 3

[0029] In a three-necked flask containing 207.0 g (1.0 mol) of isocyanatopropyl trimethoxysilane and 1620.0 g (10.0 mol) of hexamethyldisiloxane, add trifluoromethanesulfonic acid (18.27 g, 1%) and stir Raise the temperature to 60°C under low temperature, and react at 60-62°C for 8 hours, gradually increase the temperature to 120±2°C, and react at a constant temperature of 120±2°C. Silane; sampling after constant temperature 6h, detected by gas chromatography GC-2014 (Island Feng), when the content of isocyanate propyl trimethylsilane in the reaction mixture is less than 0.2%, and isocyanate propyl methoxy bis (trimethylsilyl) When the silane content is less than 1% (about 10h), stop the reaction, cool the reaction mixture, and remove the residual trimethylethoxy silicon and unreacted Hexamethyldisiloxane, cooled to obtain a mixture containing isocyanatopropyl tris(trimethylsiloxy)silane, content 89.6142wt%, 413.9g.

[0030] The mixture obtained above was subjected to vacuum ...

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Abstract

The invention discloses a preparation method for propyl isocyanate-based motomi (trimethylsilanolate) silane. Preparation steps include using 3- isocyanate propyl alkoxy silane, hexamethyldisiloxane, sulfuric acid or trifluoromethanesulfonic acid as a catalyst; heating, stirring and reacting; extracting generated saturated alkoxy trimethyl silane at the constant pressure in a reaction process; and detecting reaction finished conditions by gas chromatography and obtaining the 3- isocyanate propyl (trimethylsilanolate) silane by means of reduced pressure distillation. The preparation method in the technical scheme has the advantages that a synthesizing process path is simple, raw materials are cheap in price and easy to obtain, are toxic-free and do not cause explosion easily, formed solid and liquid waste residues are basically free of environmental pollution, after rectification purification of the 3- isocyanate propyl (trimethylsilanolate) silane, the purity of the 3- isocyanate propyl (trimethylsilanolate) silane is higher than 95%, and the yield of the 3- isocyanate propyl (trimethylsilanolate) silane is higher than 85%.

Description

technical field [0001] The invention relates to a preparation method of isocyanatopropyl tris(trimethylsiloxy)silane, which belongs to the field of organic synthesis. Background technique [0002] Isocyanatopropyl tri(trimethylsiloxy)silane products are mainly used in the improvement of the resin structure of polyurethane materials, which can effectively improve the adhesion and weather resistance of the resin, and enhance the adhesion to plastic substrates with low surface tension . In the existing research on the synthesis of isocyanatopropyl tris(trimethylsiloxy)silane products, due to the existence of highly active group isocyanate groups, it is difficult to prepare by traditional methods, and there is no current method in various documents. Technical route report. Contents of the invention [0003] The first technical problem to be solved by the present invention is to provide a method for preparing isocyanatopropyl tris(trimethylsiloxy)silane with simple synthetic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 张先林杨志勇沈鸣沈锦良李伟峰张丽亚
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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