High-temperature resistant polymer with main chain containing phenylsilylene-propargyl-benzoxazole ring and preparation method thereof

A technology of benzoxazole ring and silyl methylene, which is applied in the main chain containing silyl methylene-propargyl-benzoxazole ring polymer and its preparation field, which can solve the problem of harsh synthesis reaction conditions and obstacles to development Application, high cost of raw materials, etc., to achieve the effect of low price, increased cross-linking density, and easy access

Inactive Publication Date: 2009-11-18
BEIHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the cost of raw materials for the synthesis of this silicon-containing polymer with acetylene group is high, it is not easy to obtain, and the synthesis reaction conditions are harsh, which hinders its large-scale development and application.

Method used

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  • High-temperature resistant polymer with main chain containing phenylsilylene-propargyl-benzoxazole ring and preparation method thereof
  • High-temperature resistant polymer with main chain containing phenylsilylene-propargyl-benzoxazole ring and preparation method thereof
  • High-temperature resistant polymer with main chain containing phenylsilylene-propargyl-benzoxazole ring and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1: Poly(phenylsilane-4,4'-N,N,N',N'-tetrapropargyl-5-amino-2-(p-aminophenyl)benzoxazole)

[0045] 0.377g (1mmol) N, N, N', N'-tetrapropargyl-5-amino-2-(p-aminobenzene) benzoxazole (propargyl compound of aromatic benzoxazole ring) Add the solution of 2.3ml diethylene glycol dimethyl ether (solvent) into the reaction vessel, gradually add 11.4mg (0.3mmol) lithium aluminum hydride LiAlH under stirring 4 (catalyst) and 0.648g (6mmol) of phenylsilane (silicon hydrogen compound), after being thoroughly mixed, under the protection of an inert gas, the temperature was raised to 120°C, and the reaction was carried out at normal pressure for 24h.

[0046] After the reaction finishes, 2.3ml of toluene and 2.3ml of 1mol / L hydrochloric acid are sequentially added to the reaction vessel at room temperature, fully stirred, liquid-separated, the lower aqueous phase is removed, and 6ml of deionized water is added to the upper organic phase. Separate the liquid, remove the lowe...

Embodiment 2

[0052] Example 2: Poly(phenylsilane-4,4'-N,N,N',N'-tetrapropargyl-1,4-phenylene-di-(5-aminobenzoxazole))

[0053] 1.976g (4mmol) N, N, N', N'-tetrapropargyl-5-amino-2-(p-aminobenzene) benzoxazole (propargyl compound of aromatic benzoxazole ring) Add the solution of 3.77ml diethylene glycol dimethyl ether (solvent) into the reaction vessel, gradually add 19mg (0.5mmol) lithium aluminum hydride LiAlH under stirring 4 (catalyst) and 1.08 g (10 mmol) of phenylsilane (silicon hydrogen compound), after being thoroughly mixed, under the protection of an inert gas, the temperature was raised to 120° C., and the reaction was carried out at normal pressure for 24 hours.

[0054] After the reaction, add 4ml of toluene and 4ml of 1mol / L hydrochloric acid to the reaction vessel in sequence at room temperature, stir fully, separate the liquids, remove the lower aqueous phase, add 15 ml of deionized water to the upper organic phase, and then separate the liquids , remove the lower aqueous...

Embodiment 3

[0057] Example 3: Poly(phenylsilane-4,4'-N,N,N',N'-tetrapropargyl-5-amino-2-(p-aminophenyl)benzoxazole)

[0058] 7.54g (20mmol) N, N, N', N'-tetrapropargyl-5-amino-2-(p-aminobenzene) benzoxazole (propargyl compound of aromatic benzoxazole ring) Add the solution of 30.2ml diethylene glycol dimethyl ether (solvent) into the reaction vessel, gradually add 0.152g (4mmol) lithium aluminum hydride LiAlH under stirring 4 (catalyst) and 8.64g (80mmol) of phenylsilane (silicon hydrogen compound), after being thoroughly mixed, under the protection of an inert gas, the temperature was raised to 120°C, and the reaction was carried out at normal pressure for 30h.

[0059] After the reaction is over, add 30.2ml of toluene and 30.2ml of 1mol / L hydrochloric acid into the reaction vessel in sequence at room temperature, fully stir for 20min, separate the liquids, remove the lower aqueous phase, and add 40ml of deionized water to the upper organic phase , and then separate the liquid, remove...

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Abstract

The invention relates to a polymer with a main chain containing phenylsilylene-propargyl-benzoxazole ring, which has a structural formula shown in the figure, wherein, R has the structural formula shown in the figure. A preparation method of the polymer comprises the following steps: under certain temperature and pressure, propargyl compound and phenylsilylene component, which are dissolved in solvent and contain the benzoxazole ring, are prepared by dehydrogenization coupled reaction in the presence of a catalyst. The molecular weight of the obtained polymer differs according to the mixture ratio of the raw materials, the sorts and the dosage of the solvent as well as the reaction temperature; the range of weight average molecular weight Mw is not specially limited and is measured generally within 850-1,000,000 (based on polystyrene) by gel permeation chromatography, with the preferable range being 1000-50,000. The raw materials of the polymer are easy to prepare, low in price and simple in technique. The high-temperature resistant polymer can be applied to matrix resins of advanced composite materials, high-temperature resistant adhesives and coating as well as precursors for preparing ceramics.

Description

technical field [0001] The invention relates to a high-temperature-resistant polymer, in particular to a main chain containing silicon methylene-propargyl-benzoxazole ring polymer and a preparation method thereof, belonging to the technical field of high-temperature-resistant polymers. Background technique [0002] Poly-p-phenylenebenzobisoxazole (PBO), invented by the aerodynamic development researchers of the U.S. Air Force, has the characteristics of good heat resistance, high modulus and strength, and has now been used industrially. However, PBO is a rigid polymer chain. Compound, poor solubility, can only be dissolved in strong acid, and the processing performance is not good enough; PBO is mainly used in fibers today, but the interface between PBO fiber and resin matrix and resin has poor bonding performance, low interface shear strength, and expensive , limiting its scope of application. Silicon-containing polymers, such as polysiloxanes, polysilazanes, and polysilox...

Claims

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Application Information

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IPC IPC(8): C08G83/00C07F7/08
Inventor 杨光杨智勇
Owner BEIHANG UNIV
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