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Preparation method for linear polyborosiloxane

A technology of polyborosiloxane and tetramethyldisiloxane, which is applied in the field of preparation of online polyborosiloxane, can solve the problems of long reaction time and high reaction temperature of polyborosiloxane, and achieve the dosage Less, easy to remove, high efficiency effect

Inactive Publication Date: 2017-11-03
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But preparing polyborosiloxane in this way requires higher reaction temperature and longer reaction time

Method used

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  • Preparation method for linear polyborosiloxane
  • Preparation method for linear polyborosiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The three-necked reaction flask is equipped with electromagnetic stirring, a constant pressure dropping funnel and a thermometer. Dissolve 0.01mol (1.2g) of phenylboronic acid and 0.19mol (22.8g) of dimethyldimethoxysilane in 9g of toluene. in the liquid funnel. Put 0.22mol (29.5g) tetramethyldisiloxane, 0.35g tris(pentafluorobenzene) borane and 9g toluene into the three-necked reaction flask, heat to 55°C, complete the reaction of phenylboronic acid and dimethyl The toluene solution of dimethoxysilane was added dropwise, and the reaction was continued for 2 hours after the dropwise addition. Add 3.5g neutral aluminum oxide in solution, stir 30min, adsorption catalyst. Filtrate, and distill off the filtrate toluene and low boilers to obtain polyborosiloxane, which is a transparent viscous liquid.

[0026] 1 H NMR (CDCl 3 ): 0.02, 4.64, 7.38, 7.54ppm

[0027] GPC (toluene as mobile phase, against polystyrene): Mn=49500.

Embodiment 2

[0029] The three-necked reaction flask is equipped with electromagnetic stirring, a constant pressure dropping funnel and a thermometer. Dissolve 0.1mol (12.2g) of phenylboronic acid and 0.12mol (17.8g) of dimethyldiethoxysilane in 16g of tetrahydrofuran, and put it into a constant pressure drop in the liquid funnel. Put 0.18mol (24.1g) of tetramethyldisiloxane, 0.026g of tris(pentafluorophenyl)borane and 11g of tetrahydrofuran into a three-necked reaction flask, heat to 30°C, and complete the reaction of phenylboronic acid and dimethyl in 30 minutes. Diethoxysilane tetrahydrofuran solution was added dropwise, and the reaction was continued for 4.5 hours after the dropwise addition. Add 0.26g of neutral alumina to the solution, stir for 25min, and adsorb the catalyst. Filtrate, distill off the filtrate tetrahydrofuran and low boilers to obtain polyborosiloxane, which is a transparent viscous liquid.

[0030] 1 H NMR (CDCl 3 ): 0.04, 1.05, 3.45, 7.36, 7.52ppm

[0031] GPC ...

Embodiment 3

[0033] The three-necked reaction flask is equipped with electromagnetic stirring, a constant pressure dropping funnel and a thermometer. Dissolve 0.07mol (8.5g) of phenylboronic acid and 0.28mol (37.0g) of methylvinyldimethoxysilane in 19g of toluene, and put in the dropping funnel. Put 0.49mol (65.7g) tetramethyldisiloxane, 0.13g tris(pentafluorophenyl) borane and 26g toluene into the three-necked reaction flask, heat to 45°C, drop phenylboronic acid and toluene in 30 minutes Vinyldimethoxysilane in toluene solution, continue to react for 1.5h after the dropwise addition. Add 1.3g of neutral alumina to the solution, stir for 20min, and adsorb the catalyst. Filtration, toluene and low boilers are evaporated to obtain polyborosiloxane, which is a transparent viscous liquid.

[0034] 1 H NMR (CDCl 3 ): 0.03, 4.54, 5.88, 7.42, 7.61ppm

[0035] GPC (toluene as mobile phase, against polystyrene): Mn=19800.

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Abstract

The invention provides a preparation method for linear polyborosiloxane to overcome problems in the conventional preparation of polyborosiloxane, belonging to the field of chemical and chemical engineering. Specifically, tetramethyldisiloxane, diorganodialkoxysilane and phenylboronic acid are used as raw materials to prepare linear polyborosiloxane by removing hydrogen under the catalysis of tris(pentafluorophenyl)borane. The preparation method provided by the invention is an efficient and green synthetic method.

Description

technical field [0001] The invention relates to the field of chemistry and chemical industry, in particular to a preparation method of linear polyborosiloxane. Background technique [0002] As a new type of organic polymer material in element-modified polysiloxane, polyborosiloxane is a polymer obtained by introducing boron into the siloxane skeleton of polysiloxane. In the main chain of the polymer, Si- There is a p, d conjugated system in the structure of O-B, which is beneficial to improve the thermal stability of the polymer. In addition, the bond energies of B-O bond and Si-O bond are 537.6kJ / mol and 445.2kJ / mol respectively. The addition of B-O bond will make the heat resistance of siloxane better, which is more effective than ordinary organopolysiloxane. Excellent high temperature resistance and adhesive performance, with broader application prospects. [0003] In 1960, Vale first synthesized polyborodimethylsiloxane (PBm) with boric acid and dimethyldichlorosilane....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/22C08G77/08
CPCC08G77/08C08G77/22
Inventor 李美江葛天祥丁洁来国桥
Owner HANGZHOU NORMAL UNIVERSITY