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A kind of preparation method and application of hydrogen-containing polyborosiloxane modified white carbon black

A technology of polyborosiloxane and white carbon black, applied in chemical instruments and methods, dyed organic silicon compound treatment, dyed low-molecular organic compound treatment, etc., can solve the problem of difficult control of polyborosiloxane structure and harsh preparation process , poor product reproducibility and other issues, to achieve excellent hydrophobic and lipophilic properties, uniform dispersion, and not easy to gel

Active Publication Date: 2022-04-19
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention provides a hydrogen-containing polyborosiloxane in order to overcome the defects in the prior art that the structure of polyborosiloxane used to improve the self-adhesiveness of silicone rubber is difficult to control, and at the same time it is easy to gel and solidify, the preparation process is harsh and the product reproducibility is poor. Preparation method and application of borosiloxane modified white carbon black

Method used

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  • A kind of preparation method and application of hydrogen-containing polyborosiloxane modified white carbon black
  • A kind of preparation method and application of hydrogen-containing polyborosiloxane modified white carbon black
  • A kind of preparation method and application of hydrogen-containing polyborosiloxane modified white carbon black

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Experimental program
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Effect test

Embodiment 1

[0035] 1. Preparation of hydrogen-containing polyborosiloxane

[0036] Add 50g water, 10g Me 3 SiOMe, 30g MeHSi(OMe) 2 , 20gMeViSi(OMe) 2 , 15g B(OEt) 3 , 3g of concentrated sulfuric acid and 150g of petroleum ether, stir and mix evenly, heat to 50°C, and react for 6h. Cool to room temperature, separate the lower aqueous layer, and wash the organic layer until neutral. Add 3.5 g of anhydrous sodium sulfate, dry at room temperature for 24 hours, and filter off the desiccant to obtain 190 g of hydrogen-containing polyborosiloxane reaction liquid.

[0037] 2. Preparation of hydrogen-containing polyborosiloxane modified silica

[0038] Under stirring, add 190g of hydrogen-containing polyborosiloxane reaction solution prepared above, 0.01g of chloroplatinic acid-divinyltetramethyldisiloxane complex (platinum mass fraction is 0.02%) to 100g of hydrophilic Water vapor phase method silica (specific surface area is about 300m 2 / g), heat the system to the reflux temperature of p...

Embodiment 2

[0058] 1. Preparation of hydrogen-containing polyborosiloxane

[0059] Add 20g water, 10g Me 3 SiOEt, 10g MeHSi(OMe) 2 , 10gMe 2 Si(OEt) 2 , 10g B(OMe) 3 , 1g of concentrated hydrochloric acid and 100g of toluene, stirred and mixed evenly, heated to 30°C, and reacted for 8h. The lower aqueous layer was separated, and the organic layer was washed with water until neutral. Add 1.2 g of anhydrous magnesium sulfate, dry at room temperature for 12 hours, and filter off the desiccant to obtain 120 g of hydrogen-containing polyborosiloxane reaction liquid.

[0060] 2. Preparation of hydrogen-containing polyborosiloxane modified silica

[0061] Under stirring, 120g hydrogen-containing polyborosiloxane reaction solution, 0.02g chloroplatinic acid isopropanol complex (platinum mass fraction 0.02%) prepared above were added to 100g hydrophilic precipitation method silica (specific surface area about 170m 2 / g), heat the system to the reflux temperature of toluene, react for 5 hou...

Embodiment 3

[0068] 1. Preparation of hydrogen-containing polyborosiloxane

[0069]Add 60g water, 20g Me 3 SiOEt, 50g MeHSi(OEt) 2 , 50gMePhSi(OEt) 2 , 20g B(OBu) 3 , 5g of trifluoromethanesulfonic acid and 200g of xylene, stirred and mixed evenly, heated to 70°C, and reacted for 3h. The lower aqueous layer was separated, and the organic layer was washed with water until neutral. Add 13g of anhydrous calcium chloride, dry at room temperature for 24 hours, and filter off the desiccant to obtain 260g of hydrogen-containing polyborosiloxane reaction liquid.

[0070] 2. Preparation of hydrogen-containing polyborosiloxane modified silica

[0071] Under stirring, 260g of hydrogen-containing polyborosiloxane reaction solution prepared above, 0.05g of chloroplatinic acid tetrahydrofuran complex (platinum mass fraction is 0.02%) was added to 100g of hydrophilic fumed silica (specific surface area approx. 380m 2 / g), heating the system to the reflux temperature of xylene, reacting for 10 h, a...

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Abstract

The invention relates to the technical field of industrial fillers. Aiming at the problem that the structure of polyborosiloxane used to improve the self-adhesiveness of silicone rubber is difficult to control in the prior art, a preparation of hydrogen-containing polyborosiloxane modified white carbon black is disclosed. The method and its application include white carbon black, borate ester, methylhydrodialkoxysilane, methylalkoxysilane, trimethylalkoxysilane, water, acid catalyst, platinum catalyst, organic solvent. Compared with the traditional preparation method of polyborosiloxane, the preparation method of the present invention does not include the process of removing organic solvents, avoids excessive crosslinking of polyborosiloxane, has the advantages of not being easy to gel, good structure and performance reproducibility, etc. ; The surface of the modified white carbon black introduces B-O bonds. After being added to the silicone rubber, it can coordinate with the Si-O bonds of the silicone rubber to improve the self-adhesive properties of the silicone rubber. Compared with traditional boron compound tackifiers, hydrogen-containing polyborosiloxane modified silica is not easy to deliquescence, more uniformly dispersed in silicone rubber, and self-adhesive performance is longer.

Description

technical field [0001] The invention relates to the technical field of industrial fillers, in particular to a hydrogen-containing polyborosiloxane modified silica and its preparation method and its application in self-adhesive silicone rubber, which should belong to the modification of silica and its application in self-adhesive silicone rubber. Application technical field of rubber. Background technique [0002] Silica is widely used in rubber, plastics, coatings, Pharmaceutical and other industries. According to different preparation methods, white carbon black can be divided into two categories: gas phase method and precipitation method. The active silanol and the adsorption of water on the surface of silica make it hydrophilic and oleophobic, easy to agglomerate, difficult to disperse in raw silicone rubber, and has the disadvantages of difficult mixing and easy structuring. For this reason, it is necessary to modify the surface of silica to make the original hydrophi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/06C08K7/26C08G77/56C08L83/07C08K5/14C09C1/30C09C3/08C09C3/12
CPCC08K9/08C08K7/26C08G77/56C08K5/14C09C1/309C09C3/08C09C3/12C09C3/006C08L83/04
Inventor 李美江宋华锋刘美辰
Owner HANGZHOU NORMAL UNIVERSITY
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