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Preparation method of alkoxy end capping silicone oil

An alkoxy-terminated and alkoxysilane technology, which is applied in the field of preparation of alkoxy-terminated silicone oil, can solve the problems of cumbersome process, poor product storage stability, difficulty in removing hydrogen chloride, etc., and achieves a simple reaction route and stable product. The effect of good performance and high end capping rate

Active Publication Date: 2014-12-24
江苏科幸新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is that the existing preparation method starts from the chlorosilane monomer and the process is cumbersome, and the hydrogen chloride produced by hydrolysis is difficult to remove, resulting in poor storage stability of the product

Method used

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  • Preparation method of alkoxy end capping silicone oil

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0018] The preparation method of alkoxy-terminated silicone oil comprises the following steps:

[0019] a. Under the protection of nitrogen, add a catalyst to the high-viscosity hydroxyl-terminated polydimethylsiloxane and alkoxysilane, raise the temperature to 80-130°C, and react for 1-6 hours;

[0020] b. After the reaction is completed, add a neutralizing agent to neutralize to neutrality;

[0021] c, filter the filtrate, and the filtrate is the crude product of alkoxy-terminated silicone oil;

[0022] d. Distill the crude product at 120-170°C under a pressure of -0.06--0.09 MPa to obtain alkoxy-terminated silicone oil.

[0023] Wherein, in the step a of the preparation method of the above-mentioned alkoxy-terminated silicone oil, the alkoxysilane is tetramethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, vinyltrimethoxysilane Any one of base silane and vinyl triethoxy silane.

[0024] Wherein, in step a of the above method, the viscosity of the high-viscosity...

Embodiment 1

[0035] Put 100 parts of high-viscosity hydroxyl-terminated polydimethylsiloxane and 2 parts of vinyltrimethoxysilane into the reaction kettle, open the nitrogen protection device to feed nitrogen into the reaction kettle, and add 100ppm of potassium siloxane alkoxide catalyst , heated up to 110°C, and reacted for 5 hours. Add a phosphoric acid neutralizing agent in an equimolar ratio to the catalyst, neutralize the product to neutrality, filter the product in a filter device, and place the filtered product in a reaction kettle at -0.09MPa, 150°C Under low boiling conditions, the low boilers were removed by distillation to obtain a colorless, transparent, low-viscosity alkoxy-terminated silicone oil. Product viscosity is 300mPa. s, the refractive index is 1.44.

Embodiment 2～5

[0037] The specific raw materials and operation steps of Examples 2 to 5 are the same as those of Example 1, the difference lies in the ratio of materials, see Table 2 for specific data, and the ratio of materials and output of each embodiment are by weight.

[0038] Table 2

[0039]

[0040]

[0041] According to the data in Table 2, it can be seen that in the formulas of the above examples, the viscosity of the product is directly related to the ratio of the end-capping agent alkoxysilane, and the amount of the catalyst only has an impact on the reaction rate, and has no effect on the final viscosity of the product. Has little effect.

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Abstract

The invention belongs to the field of modified silicone oil, specifically relates to a preparation method of alkoxy end capping silicone oil, and aims at solving the technical problems of the existing preparation that the process is complex because of starting from chlorosilane monomer, hydrogen chloride produced by hydrolyzing is difficult to remove, and therefore, the storage stability of a product is poor. The preparation method of the alkoxy end capping silicone oil comprises the following steps: adding a catalyst to high-viscosity-end hydroxyl polydimethylsiloxane and alkoxy silane under the protection of nitrogen, heating to be 80 to 130 DEG C, and reacting for 1 to 6 hours; b, neutralizing to be neutral after the reaction is done; c, filtering to obtain the filtrate that is the crude alkoxy end capping silicone oil product; d, distilling the crude product under a temperature of 120 to 170 DEG C and at a pressure of -0.06 to -0.09Mpa to obtain the alkoxy end capping silicone oil. According to the preparation method of the alkoxy end capping silicone oil, the reaction line is simple, the alkoxy end capping silicone oil is high in stability and high in end capping rate, and a new method is provided to the preparation of the alkoxy end capping silicone oil.

Description

technical field [0001] The invention belongs to the field of modified silicone oil, in particular to a preparation method of alkoxy-terminated silicone oil. Background technique [0002] Alkoxy silicone oil was first prepared from dimethyldichlorosilane, monomethyltrichlorosilane or trimethylchlorosilane through alcoholysis, hydrolysis, neutralization and other steps. At present, many domestic production and scientific research units are still continuing Use this method to prepare alkoxy-terminated silicone oil products. [0003] The preparation of alkoxy-terminated silicone oils in the prior art has the following problems: 1. The alkoxy-terminated silicone oil products prepared from monomers have relatively high viscosity, are easy to cross-link, and have a wide molecular weight distribution and poor controllability; 2. The prepared raw material is a by-product of organosilicon, the composition is complex, the process is cumbersome, and the applicability is not strong; 3. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/38
Inventor 孙晓泉李争鸣葛强肖维兵朱文英
Owner 江苏科幸新材料有限公司
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