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A kind of preparation method of mixed borosiloxane

A technology of borosiloxane and mixed ring, which is applied in the field of preparation of mixed borosiloxane, which can solve the problems of inapplicability and easy hydrolysis, and achieve the effect of low price, low cost and mild conditions

Active Publication Date: 2018-05-22
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In 1960, Vale first synthesized polyborodimethylsiloxane (PBm) by dehydrochlorination and condensation of boric acid and dimethyldichlorosilane. PBm has good heat resistance, but it is very easy to hydrolyze and cannot be applied (R.L.Vale. J. Chem. Soc, 1960, 2252)

Method used

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  • A kind of preparation method of mixed borosiloxane
  • A kind of preparation method of mixed borosiloxane
  • A kind of preparation method of mixed borosiloxane

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The three-necked reaction flask is equipped with electromagnetic stirring, a constant pressure dropping funnel, and a three-way valve. Under the protection of nitrogen at 20°C, dissolve 0.03mol of phenylboronic acid in 50ml of tetrahydrofuran, put it into the constant pressure dropping funnel, and put it in the three-necked reaction flask. Add 0.15mol dimethyldichlorosilane, drop phenylboronic acid within 30 minutes, continue to react for 5h after the dropwise addition, and then add 0.3mol zinc oxide and 500ml ethyl acetate into the reaction flask under the protection of nitrogen Stir to form a suspension, then transfer the solution after the reaction in the previous step to a constant pressure dropping funnel, drop it into the suspension within 30 minutes, and continue to react for 12 hours after the addition; filter out the insoluble zinc salt, and wash the filtrate with water 100ml After ×2 times, wash 100ml with distilled water ×2 times; dry with anhydrous sodium sul...

Embodiment 2

[0040] The three-neck reaction flask is equipped with electromagnetic stirring, a constant pressure dropping funnel, and a three-way valve. Under the protection of nitrogen at 50°C, dissolve 0.05mol methyl boric acid in 50ml of toluene, put it into the constant pressure dropping funnel, and put it in the three-necked reaction flask. Put in 0.4mol diethyldichlorosilane, add methyl boric acid dropwise within 20 minutes, and continue the reaction for 4 hours after the dropwise addition. Then under the protection of nitrogen, at -10 ° C, first add 0.4 mol of calcium oxide and 500 ml of methyl acetate into the reaction flask and stir to form a suspension, and then transfer the solution after the previous step to the constant pressure dropping funnel. Add it dropwise to the suspension within 20 minutes, and continue to react for 18 hours after the addition; filter off the insoluble calcium salt, wash the filtrate 100ml×2 times with distilled water, and then wash 100ml×2 times with di...

Embodiment 3

[0048] The three-neck reaction flask is equipped with electromagnetic stirring, constant pressure dropping funnel, three-way valve, and electric heating mantle. Under the protection of nitrogen at -20°C, dissolve 0.03mol of phenylboronic acid in 50ml of dichloromethane and put it into the constant pressure dropping funnel. , put 0.09mol diethyldichlorosilane into the three-neck reaction flask, add phenylboronic acid dropwise within 40 minutes, and continue the reaction for 8 hours after the dropwise addition. Then, under the protection of nitrogen at 50°C, first add 0.2mol of copper oxide and 500ml of n-hexane into the reaction flask and stir to form a suspension, then transfer the solution after the reaction in the previous step to a constant pressure dropping funnel, and drop it within 40 minutes. into the suspension, continue to react for 8 hours after the addition; filter off the unreacted copper salt, wash the filtrate 100ml x 2 times with distilled water, then wash 100ml ...

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Abstract

The invention relates to the field of chemistry and chemical engineering, and provides a cheap and efficient borosiloxane intermediate for the preparation of high-performance boron-containing polysiloxane. Under gas protection, drop the mixture of hydrocarbyl boronic acid and organic solvent A into dihydrocarbyl dichlorosilane, stir and react for 3h~8h at a temperature of -20°C~80°C, then add the mixture of organic solvent B and metal oxide , after reacting for 6h~18h, filter, wash with water, evaporate organic solvent A and organic solvent B to obtain mixed borosiloxane. The invention has the advantages of easy-to-obtain raw materials and low cost. The compound can be used to synthesize boron-containing polysiloxanes such as borosilicate rubber, heat-resistant adhesives and heat-resistant coatings, and can be widely used in aerospace, electronics, chemical industry, Machinery and other industries.

Description

technical field [0001] The invention relates to the field of chemical engineering, in particular to a preparation method of mixed borosiloxane. Background technique [0002] With the development of modern science and technology, especially the development of wire and cable, ceramics, aerospace and other industries, people have put forward more and more stringent requirements for the heat resistance of coating rubber. However, the heat resistance of polymers is not ideal at present, and cannot meet the requirements of heat resistance of 400°C or higher. [0003] 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 the B-O bond and the Si-O bond are 537....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21C08G77/56
Inventor 李美江葛天祥来国桥
Owner HANGZHOU NORMAL UNIVERSITY
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