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Borosiloxane and preparation method thereof

A technology of polyborosiloxane and siloxane monomers, which is applied in the field of borosiloxane and its preparation, can solve the problems of low heat resistance temperature, influence on the development of high-tech fields, poor adhesion, etc., and achieves excellent performance. Effect

Active Publication Date: 2013-09-04
上海爱世博有机硅材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is still unable to meet the needs of many high-tech fields, causing the development of some high-tech fields to be seriously affected
In the preparation of existing high-temperature resistant silicone resins disclosed in CN 1962728A, CN 101531761A, and CN 102127389A, the high-temperature resistant silicone resins prepared by CN 102127389A have many disadvantages such as low heat-resistant temperature and poor adhesion at higher operating temperatures.

Method used

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  • Borosiloxane and preparation method thereof
  • Borosiloxane and preparation method thereof
  • Borosiloxane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1. Preparation of hydrolyzate

[0029] a. Weigh 13.6g of ethyl orthosilicate, 28.9g of methyltriethoxysilane, 36.4g of dimethyldiethoxysilane, 18.7g of phenyltriethoxysilane, 12.4g of monomethyltrichlorosilane g, 43.2g of methylethoxydichlorosilane, 34.8g of monophenyltrichlorosilane, and 16.7g of diphenyldichlorosilane were mixed uniformly, placed in a clean container, and set aside.

[0030] b. Weigh 1020g of the hydrolyzing agent into the reaction vessel according to the preparation plan, add 17.9g of boric acid at room temperature, after fully dissolving, keep the temperature at 25~30°C, add the above mixed monomers dropwise while stirring, and carry out the hydrolysis reaction. 4h after the dropwise addition is completed, slowly raise the temperature to T=55~65°C, stir for 1h, let it stand for 45min, separate the lower layer of acid water, and use 2% NaHCO 3 The solution was washed until the pH value of the system was 6.0~7.0. It was washed twice with saturated N...

Embodiment 2

[0038] 1. Preparation of hydrolyzate

[0039] a. Weigh 18.4g of methyltriethoxysilane, 32.4g of dimethyldiethoxysilane, 27.0g of phenyltriethoxysilane, 17.3g of monomethyltrichlorosilane, 17.3g of methylethoxydi 13.2g of chlorosilane, 19.8g of monophenyltrichlorosilane, and 26.7g of diphenyldichlorosilane were mixed uniformly, placed in a clean container, and set aside.

[0040] b. Weigh 1086g of the hydrolyzing agent into the reaction vessel according to the preparation plan, slowly add the above mixed monomers dropwise under the condition of stirring at room temperature, and at the same time slowly inject 14.8g of boron trifluoride gas to carry out the hydrolysis reaction. After 3.5 hours of dropwise addition, slowly raise the temperature to T=55~65°C, stir for 1 hour, let it stand for 45 minutes, separate the lower layer of acidic water, and wash with 2% NaHCO3 solution until the pH value of the system is 6.0~7.0. It was washed twice with saturated NaCl solution to obtain ...

Embodiment 3

[0048] 1. Preparation of hydrolyzate

[0049] a. Weigh 23.3g of dimethyldiethoxysilane, 31.4g of methyltriethoxysilane, 12.8g of monomethyltrichlorosilane, 18.7g of phenyltriethoxysilane, and 18.7g of monomethyltrichlorosilane 25.3g, 12.1g of methylethoxydichlorosilane, 18.0g of monophenyltrichlorosilane, and 28.4g of diphenyldichlorosilane were mixed evenly, placed in a clean container, and set aside.

[0050] b. Weigh 990g of hydrolysis agent into the reaction vessel according to the preparation plan, add 19.2g of boric acid at room temperature, after fully dissolving, keep the temperature at 20°C, add the above mixed monomers dropwise under stirring, and carry out the hydrolysis reaction. After 5.5 hours of dropwise addition, slowly raise the temperature to T=65°C, stir for 1 hour, let it stand for 45 minutes, separate the lower layer of acid water, and use 2% NaHCO 3 The solution was washed until the pH value of the system was 6.0~7.0. It was washed twice with saturated ...

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Abstract

The invention relates to borosiloxane and a preparation method thereof. According to the method, a hydrolysis solvent and a boron compound are mixed proportionally and added to a reactor, the temperature keeps from 10 DEG C to 35 DEG C, and a mixed monomer is slowly dropwise added under the stirring condition for a hydrolysis reaction; the dropwise-adding time is controlled in 3-6 hours, the reactor is slowly heated to the temperature ranging from 55 DEG C to 65 DEG C after the dropwise-adding is finished, a stirring reaction is performed for 1 hour, and still standing is performed; acid water on the lower layer is separated and neutralized to be neutral, a saturated NaCl solution is used for washing, and an oil phase material is obtained; reduced pressure distillation is performed to remove the solvent, a catalyst I is added, the mixture is heated to 110-130 DEG C, and the rearrangement reaction is performed for 3-5 hours; the mixture is heated to 150-160 DEG C, the splitting cyclization reaction is performed for 2-5 hours, the reaction is finished, the mixture is cooled, and a polyborosiloxane prepolymer is obtained; an end-capping reagent and a catalyst II are added to a system and heated to 110-130 DEG C, and react for 2-4 hours; and pressure is reduced to remove a low-boiling-point substance, and a polyborosiloxane resin is obtained. The borosiloxane and the preparation method have the advantages of good temperature resistance, ageing resistance, impact resistance, toughness and low-temperature flexibility, high adhesion and the like.

Description

[technical field] [0001] The invention relates to the technical field of borosiloxane and its preparation method. [Background technique] [0002] With the continuous development of modern industries such as national defense, energy, metallurgy, and petrochemicals, more and more equipment and supporting facilities need to be used at high temperatures. Ordinary high-temperature-resistant resins have poor toughness and durability in high-temperature environments and cannot meet the technical requirements The demand has made people put forward higher requirements for the heat resistance of the resin. Therefore, in many application fields, high temperature resistant resin has received more attention, and some units at home and abroad have also carried out targeted research. [0003] The existing polysiloxane has good high and low temperature resistance and can be widely used in many occasions. However, it is still unable to meet the needs of many high-tech fields, causing the d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/56
Inventor 黄新武王西民刘旭军苗承刚
Owner 上海爱世博有机硅材料有限公司
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