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Method for preparing carborane-siloxane polymer under catalysis of Lewis acid

A Lewis acid, catalytic preparation technology, which is applied in chemical instruments and methods, compounds of Group 4/14 elements of the periodic table, organic chemistry, etc. The effect of easy operation, easy control of reaction conditions and concise process flow

Inactive Publication Date: 2010-11-03
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the cage-type carborane as the main chain structure of the polymer, the molecular stability is high, the steric hindrance is large, and the degree of polymerization is difficult to increase

Method used

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  • Method for preparing carborane-siloxane polymer under catalysis of Lewis acid
  • Method for preparing carborane-siloxane polymer under catalysis of Lewis acid
  • Method for preparing carborane-siloxane polymer under catalysis of Lewis acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: the preparation of two (chloro-dimethylsilyl)-1,7-carborane

[0033] In inert gas N 2 Under protection, 0.72g (5mmol) of 1,2-dicarbo-closed-dodecaborane was dissolved in 30mL of anhydrous diethyl ether, which was clear and transparent. 11 mmol of n-butyllithium was injected into the ether solution of carborane within 5 minutes, and reacted at 0°C for 3 hours under magnetic stirring. The reaction solution was slowly added to 11 mmol of dimethyldichlorosilane at 0° C., and then reacted at room temperature for 12 hours under stirring. The product was filtered to remove lithium chloride, and the filtrate was evaporated to dryness to obtain bis(chloro-dimethylsilyl)-1,2-carborane, which was heated at 350° C. in a quartz tube for 5 hours to obtain a light yellow semi-solid bis( Chloro-dimethylsilyl)-1,7-carborane. 1 H-NMR (CDCl 3 ): δ=0.24ppm (m, 12H, CH 3 ), δ=1.69~2.95ppm (m, 10H, B 10 h 10 ). FTIR: v(3069cm -1 ), C-H; v(2603cm -1 ), B-H; v(1260cm -...

Embodiment 2

[0034] Embodiment 2: the preparation of carborane-siloxane polymer I (shown in formula 1)

[0035]

[0036] Formula 1: Polymer I

[0037] Dissolve 1.66 g (5 mmol) of bis(chloro-dimethylsilyl)-1,7-carborane obtained in Example 1 in 50 mL of tetrahydrofuran, and add 11 mmol of anhydrous methanol dropwise at 65° C., while passing through N 2 Bubble out by-produced HCl. After reacting for 3 hours, bis(methoxy-dimethylsilyl)-1,7-carborane was obtained. Add 3 mg anhydrous FeCl 3 As a catalyst, bis(methoxy-dimethylsilyl)-1,7-carborane was reacted with 11 mmol of dimethyldichlorosilane at 150° C. for 24 hours. Then the low boilers were removed under reduced pressure, and the resulting polycondensation product was washed with acetone until it was washed with NH 4 CNS test until no iron ion, vacuum drying to obtain a rubbery polymer. T g =-35°C, 2.2% weight loss in hot air at 400°C, 15.3% weight loss at 600°C.

Embodiment 3

[0038] Embodiment 3: the preparation of carborane-siloxane polymer II (shown in formula 2)

[0039]

[0040] Formula 2: Polymer II

[0041] in N 2 In an anhydrous and oxygen-free environment under protection, 0.72g (5mmol) of 1,7-dicarbo-closed-dodecaborane was dissolved in 30mL of tetrahydrofuran, and reacted with 11mmol of tert-butyllithium to obtain 1,2-bis Lithium substituted carboranes. It was slowly added into 11 mmol of methylphenyldichlorosilane under stirring in an ice-water bath, and then reacted at room temperature for 20 hours. The reaction product was filtered, and the filtrate was collected. 65℃, through N 2 Under bubbling, 11 mmol of anhydrous methanol was added dropwise to the filtrate and reacted for 5 hours to obtain bis(methoxy-methylphenylsilyl)-1,7-carborane. With 5 mg anhydrous AlCl 3 As a catalyst, bis(methoxy-methylphenylsilyl)-1,7-carborane and equimolar methylphenyldichlorosilane undergo polycondensation, and react at 180°C for 48 hours to ob...

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Abstract

The invention discloses a method for preparing a carborane-siloxane polymer under the catalysis of Lewis acid. The polymer is prepared by reacting closed dicarbadodecaborane (carborane for short), chlorosilane and alkyl lithium serving as raw materials, and an inert solvent serving as a reaction medium under the protection of inert gas in the presence of the Lewis acid serving as a catalyst. The method has the advantages of readily available raw materials, concise process flow, simple and easy operation, and easily controlled reaction conditions. The linear carborane-siloxane polymer is prepared by controlling the molar ratio and feeding sequence of the materials in the presence of the Lewis acid serving as the catalyst. The polymer can be used for preparing a low-temperature vulcanized heat-resisting adhesive and a sealant.

Description

Technical field: [0001] The present invention relates to a process for preparing carborane-siloxane polymers catalyzed by Lewis acids. The method uses dicarbo-closed-dodecaborane (hereinafter referred to as carborane), dichlorosilane, and alkyllithium as raw materials, an inert solvent as a reaction medium, and a Lewis acid as a catalyst, and reacts under the protection of an inert gas. And made. Background technique: [0002] Carborane, carborane, can also be translated as carborane, this type of compound is composed of B, H and C, and its molecular structure is a polyhedron or a part of a polyhedron. Carborane is generally divided into two types in terms of structure: open type and closed type. The open type has nest shape and network shape, and the closed type is cage shape. Carborane currently used in the fields of ceramic fibers and heat-resistant polymer materials is mainly cardecaborane with a cage structure, and its molecular formula is C 2 B 10 h 12 , that is, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/50C08G77/08C07F7/18C07F7/12
Inventor 齐士成李吉明刘煜
Owner BEIJING UNIV OF CHEM TECH
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