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Aryne resin containing polysilicone and preparation method thereof

An arylacetylene resin and polysilane technology, applied in the field of polysilane-containing arylacetylene resin and its preparation, can solve the problems of inability to achieve thermal protection effect, high pyrolysis carbon residue rate, low shrinkage rate, etc., and achieve excellent physical and mechanical properties. Performance and heat resistance, low viscosity, good resin processability

Inactive Publication Date: 2008-08-06
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (3) The molecular structure only contains two elements, C and H, and the carbon content is more than 90%, the pyrolysis residual carbon rate is extremely high, and the shrinkage rate is low;
However, if the silicon content of the resin is less than 15%, it is difficult to form a continuous ceramic layer on the surface of the material after pyrolysis at high temperature, and it cannot achieve a good thermal protection effect.

Method used

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  • Aryne resin containing polysilicone and preparation method thereof
  • Aryne resin containing polysilicone and preparation method thereof
  • Aryne resin containing polysilicone and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] (1) Preparation of 1,2-dichlorotetramethyldisilane (III)

[0088] Add anhydrous aluminum trichloride (54g, 410mmol) and dichloromethane (120mL) into a 500mL four-necked flask equipped with a stirring device, a constant pressure funnel, a thermometer and a condenser tube, and then add acetyl chloride (28.7g , 410mmol), about 30min to finish dripping, and stir until a yellow homogeneous solution is formed after the dropwise addition;

[0089] Then the resulting yellow homogeneous solution was added dropwise to a solution of hexamethyldisilane (29.3g, 200mmol) in dichloromethane (80mL) under ice-bath and stirring conditions. In a 500mL four-necked flask with a condenser tube, reflux at 40°C for 12 hours after the dropwise addition;

[0090] Most of the dichloromethane was removed by distillation, and the resulting product was extracted three times with n-hexane. After distillation, 56.53 g of colorless and transparent 1,2-dichlorotetramethyldisilane liquid (III) was obtai...

Embodiment 2

[0102] Preparation of polysilane-containing aryne resin (PSIII-AR-2)

[0103] Add treated magnesium powder (4.36g, 182mmol) and THF (50mL) into a 500mL four-necked flask equipped with a stirring device, a constant pressure funnel, a thermometer, and a condenser, protect it with nitrogen, and slowly add bromine dropwise through a constant pressure funnel. The mixed solution of ethane (18.00g, 165mmol) and THF (50mL) was added dropwise for 1.5h, and then refluxed for 1.5h to obtain a gray-black ethyl Grignard reagent;

[0104] A mixed solution of diethynylbenzene (9.47g, 75mmol) and THF (50mL) was added dropwise under cooling in an ice-water bath, the reaction mixture gradually changed from grayish black to white, the addition was completed within 1h, and then refluxed for 2h;

[0105] Under cooling in a water bath, slowly add a mixed solution of 1,2-dichlorotetramethyldisilane (III) (10.86 g, 60 mmol) and THF (50 mL) through a constant-pressure funnel for about 1 h;

[0106] A...

Embodiment 3

[0113] Preparation of polysilane aryne resin (PSIII-AR-3)

[0114] Add treated magnesium powder (4.36g, 182mmol) and THF (50mL) into a 500mL four-necked flask equipped with a stirring device, a constant pressure funnel, a thermometer, and a condenser, protect it with nitrogen, and slowly add bromine dropwise through a constant pressure funnel. The mixed solution of ethane (18.00g, 165mmol) and THF (50mL) was added dropwise for 1.5h, and then refluxed for 1.5h to obtain a gray-black ethyl Grignard reagent;

[0115] A mixed solution of diethynylbenzene (9.47g, 75mmol) and THF (50mL) was added dropwise under cooling in an ice-water bath, the reaction mixture gradually changed from grayish black to white, the addition was completed within 1h, and then refluxed for 2h;

[0116] Under cooling in a water bath, a mixed solution of 1,2-dichlorotetramethyldisilane (III) (12.22 g, 67.5 mmol) and THF (50 mL) was slowly added through a constant pressure funnel for about 1 h. After the dro...

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Abstract

The invention relates to a polysilane-containing aryne resin represented as right, wherein n is 0-20, x and y are 0-20, R1, R2, R3 and R4 are CH3 and C6H5, or R1 is H, R2, R3 and R4 are CH3 and C6H5, or R1 and R3 are H, R2 and R4 are CH3 and C6H5. The preparation method of polysilane-containing aryne resin uses aryne Grignard reagent to be reacted with terminated chlorine polysilane, while terminated chlorine polysilane is prepared by chlorination process and sodium condensation method. The inventive polysilane-containing aryne resin has better processing character, mechnical character, heat endurance, oxidation resistance and fire-retardancy, which can form ceramic material in high temperature and own better cementation with reinforcing fiber, with wide application in resin substrate and ceramic boving precursor.

Description

【Technical field】 [0001] The invention relates to a novel aryne resin in the technical field of chemistry and chemical engineering, in particular to a polysilane-containing aryne resin and a preparation method thereof. 【Background technique】 [0002] Since the 1950s, the development of high technologies such as aviation, aerospace, navigation, and electronics industry has promoted the research of heat-resistant polymer materials, and many heat-resistant polymers such as polyimide have been applied one after another. Aryne resins are a new type of high temperature resistant thermosetting resins, typically aryl acetylene resins, which are polymerized from ethynyl (usually terminal ethynyl) aromatic compounds. Arylacetylene resin has the following characteristics: [0003] (1) The polymerization process is a polyaddition reaction, and no volatile matter and low molecular weight by-products escape during curing; [0004] (2) After the resin is cured, it usually has a highly cr...

Claims

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Application Information

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IPC IPC(8): C08F138/00C08G77/50
Inventor 黄发荣杜磊尹国光张健黄健翔周燕万里强齐会民
Owner EAST CHINA UNIV OF SCI & TECH
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