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A kind of alkoxy-terminated polysiloxane polymer and preparation method thereof

An alkoxy-terminated and alkoxyhydrosilane technology is applied in the field of alkoxy-terminated polysiloxane polymers and their preparation, and can solve the problems of residual hydroxyalkoxysilane, slow reaction speed, and product end-capping. The problem of low rate, etc., to achieve the effect of fast reaction rate, high end capping rate and good product stability

Active Publication Date: 2022-06-07
HANGZHOU ZHIJIANG SILICONE CHEM +1
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AI Technical Summary

Problems solved by technology

[0004] However, most of the existing preparation methods are based on the reaction of hydroxyl-terminated polysiloxane with methyltrimethoxysilane, methyl orthosilicate and other alkoxy-containing silanes to form alkoxy-terminated polysiloxanes under the catalysis of acids or bases. Silicone oil, the end-capping rate of the product of the above-mentioned preparation method is not high, the reaction speed is slow, and a large number of hydroxyl groups (hydroxyl content greater than 1000ppm) and alkoxysilane residues

Method used

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preparation example Construction

[0027] The invention provides a preparation method of an alkoxy-terminated polysiloxane polymer, comprising the following steps:

[0028] a) Use vinylsilazane and alkoxyhydrosilane, use organic solvent as reaction buffer, inert gas as protective gas, and use metal catalyst to synthesize alkoxy-terminated silazane;

[0029] The general formula of the alkoxy-terminated silazane is:

[0030] R 1 a C 8 H 21 NSi 4 (I);

[0031] In formula (I), R 1 for-OC 2 H 5 or -OCH 3 ; a is an integer from 1 to 3;

[0032] b) The alkoxy-terminated silazane synthesized in step a) and the hydroxyl-terminated polysiloxane are subjected to an aminolysis reaction under the protection of an inert gas to obtain an alkoxy-terminated polysiloxane polymer.

[0033] The present invention firstly adopts vinylsilazane and alkoxyhydrosilane, uses organic solvent as reaction buffer, inert gas as protective gas, and uses metal catalyst to synthesize alkoxy-terminated silazane. In the present invent...

Embodiment 1

[0070] (1) under nitrogen protection, be warming up to 70 ℃, in the 300g toluene mixed liquid of 200g tetramethyldivinyldisilazane and 2.3g triphenylphosphine rhodium chloride catalyst, drip 270g trimethoxysilicon hydrogen alkane, stirred and reacted for 3h to obtain a reaction mixture;

[0071] (2) be warming up to 80 ℃ under nitrogen protection, and the pressure is under-0.09MPa, remove the toluene and excess trimethoxysilane in the reaction mixture that step (1) obtains, obtain reaction product;

[0072] (3) 20 g of the reaction product obtained in step (2) and 2000 g of hydroxyl-terminated silicone oil (HOCH) having a viscosity of 20,000 mPa·s 3 SiO(SiCH 3 O) n SiCH 3 OH, wherein n=900~1500) at 80°C for 3h, to obtain crude product.

[0073] (4) the crude product obtained in step (3) is distilled off under the protection of nitrogen bubbling at 170° C., the pressure is -0.09MPa, and the low molecules are removed to obtain the alkoxy-terminated silicone oil, that is, the...

Embodiment 2

[0075](1) under nitrogen protection, be warming up to 80 ℃, in 330g toluene mixed liquid of 200g tetramethyldivinyldisilazane and 2.9g triphenylphosphine rhodium chloride catalyst, drip 390g triethoxy silicon Hydrogen alkane was stirred for 3h to obtain a reaction mixture;

[0076] (2) be warming up to 95 ℃ under nitrogen protection, and the pressure is under-0.09MPa, remove toluene and excess triethoxysilane in the reaction mixture obtained in step (1), obtain reaction product;

[0077] (3) 16 g of the reaction product obtained in step (2) and 2,000 g of hydroxyl-terminated silicone oil (HOCH) with a viscosity of 80,000 mPa·s 3 SiO(SiCH 3 O) n SiCH 3 OH, wherein n=1600~1870), carry out aminolysis reaction at 80°C for 3h to obtain crude product.

[0078] (4) the crude product obtained in step (3) is distilled off under the protection of nitrogen bubbling at 170° C., the pressure is -0.09MPa, and the low molecules are removed to obtain an alkoxy-terminated silicone oil, tha...

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Abstract

The invention provides a method for preparing an alkoxy-terminated polysiloxane polymer, comprising the following steps: a) using vinylsilazane and alkoxyhydrogensilane, using an organic solvent as a reaction buffer, and using an inert gas As a protective gas, a metal catalyst is used to synthesize an alkoxy-terminated silazane; the general formula of the alkoxy-terminated silazane is: R 1 a C 8 h 21 NSi 4 ; where R 1 for-OC 2 h 5 or-OCH 3 a is an integer of 1 to 3; b) the alkoxy-terminated silazane and hydroxyl-terminated polysiloxane synthesized in step a) are subjected to ammonolysis reaction under the protection of an inert gas to obtain an alkoxy-terminated polysiloxane Silicone polymer. The reaction route of the preparation method is simple, and the alkoxy silicon nitrogen end-capping agent adopts rhodium and nickel catalysts to carry out hydrosilicon addition to produce the alkoxy end-capping agent, which is efficient, stable and non-poisoning, and has good product stability and high end-capping rate. The reaction rate between the silicon nitrogen end-capping agent and the organosilicon hydroxyl polymer is fast, and the end-capping rate is high, which provides a new method for the preparation of the alkoxy end-capped polymer.

Description

technical field [0001] The present invention relates to the technical field of alkoxy-modified polysiloxane, and more particularly, to an alkoxy-terminated polysiloxane polymer and a preparation method thereof. Background technique [0002] Alkoxy-terminated polymers can replace hydroxyl-terminated siloxane polymers. Compared with hydroxyl-terminated polysiloxane polymers, in the production of silicone rubber for condensation systems, it has the advantages of avoiding viscosity peaks in the production process and reducing equipment requirements. The base end-capped polymer-based silicone rubber has the characteristics of long storage life and excellent performance. It has excellent performance in the production of high-performance construction adhesives, industrial electrical and electronic sealing adhesives and other materials. [0003] The alkoxy silicon nitrogen capping agent adopts rhodium and nickel catalysts for hydrosilylation to produce alkoxyl end capping agents wi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/388
CPCC08G77/388
Inventor 常映军汤凯铭郝开强陶小乐何永富
Owner HANGZHOU ZHIJIANG SILICONE CHEM
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