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Silica aryne resin containing carborane unit in main chain framework and preparation method thereof

A technology for siloxane and carborane, which is applied in the field of siloxane resin and its preparation, can solve the problems of limiting the number of carborane units, hindering the reaction, high brittleness, etc., and achieves excellent mechanical properties and good processing performance. , the effect of excellent heat resistance and thermo-oxidative stability

Active Publication Date: 2014-10-01
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the high rigidity of the molecular chain of the resin, the brittleness after curing is relatively large; in addition, the rigidity of the silicon-containing aryne resin hinders the reaction with decaborane, which limits the number of carborane units introduced into the same molecular chain

Method used

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  • Silica aryne resin containing carborane unit in main chain framework and preparation method thereof
  • Silica aryne resin containing carborane unit in main chain framework and preparation method thereof
  • Silica aryne resin containing carborane unit in main chain framework and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0054] Preparation of disiloxane-type siloxyaryne resin CB-2-PSOA-10 containing carborane units in the main chain

[0055] 1) Synthesis of 1,3-dichloro-1,1,3,3-tetramethyldisiloxane

[0056] In a 500mL four-neck round bottom flask equipped with a constant pressure funnel, a spherical condenser and a magnetic Teflon stirrer, add PdCl 2 20mg and CCl 4 100mL, protected by nitrogen gas, stirred evenly, and added dropwise 26.8g (0.2mol) of 1,1,3,3-tetramethyldisiloxane CCl at room temperature 4 150mL solution, the dropwise addition time is about 2h, after the dropwise addition is completed, continue to stir at room temperature for 72h. After the reaction was completed, the solvent was removed and distilled under reduced pressure to obtain 32.5 g of a colorless and transparent liquid with a yield of 80.0%.

[0057] 2) Synthesis of disiloxane type siloxyaryne resin (2-PSOA)

[0058] In a 250mL four-necked flask equipped with a stirrer, a reflux condenser, a constant pressure funn...

Embodiment 2

[0065] Preparation of disiloxane-type siloxyaryne resin CB-2-PSOA-40 containing carborane units in the main chain

[0066] Under nitrogen protection, 250 mL of dry toluene, 10 g of 2-PSOA, 4 g of decaborane, and 20 mL of diethyl sulfide were added to a 500 mL flask, and the reactant was magnetically stirred at room temperature for 2 h. Then the solution was heated to 85°C and reacted for 48h. After the reaction was completed, 60 mL of methanol was added (hydrogen gas was generated), allowed to stand overnight, and then refluxed at 65° C. for 12 h. The reaction solution was cooled, washed with water, separated, and the organic phase was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 12.1 g of a tan solid product with a yield of 86.4%. FTIR (KBr, cm -1 ): 3290 (v C-H ,≡C-H), 3062(v C-H , Ar) and (v C-H , cage), 2962 (v C-H , Si-CH 3 ), 2572(v B-H ), 2155(v C≡C ), 1257(v Si-C , Si-CH 3 ), 1048(v Si-O ); 1 H-NMR (C...

Embodiment 3

[0069] Preparation of High Molecular Weight Disiloxane Type Silicone Aryne Resin CB-2u-PSOA-20 Containing Carborane Units in Main Chain Skeleton

[0070] 1) Synthesis of high molecular weight disiloxane type silicone aryne resin (2u-PSOA)

[0071] In a 250mL four-necked flask equipped with a stirrer, a reflux condenser, a constant pressure funnel and a thermometer, nitrogen protection was applied, 6g (0.247mol) of magnesium powder and 50mL of tetrahydrofuran were added, and ethyl bromide was slowly added dropwise at room temperature with a constant pressure funnel The mixed solution of 21.6g (0.198mol) and 50mL tetrahydrofuran was added dropwise for about 1.5h. After the dropwise addition, reflux at 50° C. for 1.5 h, and cool to room temperature. At this time, the reaction solution is gray-black. Weigh a mixed solution of 11.35 g (0.090 mol) of diethynylbenzene and 50 mL of tetrahydrofuran, and slowly add it dropwise into the reaction system under cooling in an ice-water bath...

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Abstract

The invention relates to a silica aryne resin containing carborane unit in main chain framework and a preparation method thereof. The method comprises the following steps: preparing a silica aryne resin from diacetylene-benzene and dihalogenated siloxane by an alkynyl Grignard reagent process, and reacting decaborane with the silica aryne resin under the action of a Lewis base to prepare the silica aryne resin containing carborane unit in main chain framework. The silica aryne resin containing carborane unit in main chain framework is soluble in common organic solvents, and has excellent workability; the resin solidified substance has excellent heat resistance and thermal oxygen stability; and the fiber-reinforced composite material has excellent mechanical properties, and has wide application prospects in the fields of aerospace and the like.

Description

【Technical field】 [0001] The invention relates to the technical field of synthetic resins, in particular to a siloxyaryne resin whose main chain skeleton contains carborane units and a preparation method thereof. 【Background technique】 [0002] Silicon-containing aryne resin is a new type of organic-inorganic hybrid thermosetting resin, which has a highly cross-linked structure after curing. It has excellent heat resistance, excellent electrical properties, mechanical properties and high-temperature ceramic performance, and can be used as a High-temperature materials, wave-transparent materials, ablation-resistant materials, and ceramic precursor materials have broad application prospects. [0003] Since 1994, M.Itoh and others have carried out in-depth research on silicon-containing aryne resins, the most representative of which is MSP resin [M.Itoh, M.Mitsuzuka, et al.Macromolecules, 1994, 27:7917~ 7919.], its structural formula is [-Si(Ph)H-C≡C-C 6 h 4 -C≡C-] n . MSP...

Claims

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Application Information

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IPC IPC(8): C08G77/398C08G77/20C07F7/08C08L83/08C08K7/00C08K7/06
Inventor 黄发荣杜磊姜云鲁加荣汪强李晓杰
Owner EAST CHINA UNIV OF SCI & TECH
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