Sesquialter siloxane polyaryne hybrid resin and preparation method and use thereof

A technology of silsesquioxane and siliaryne, which is applied in the field of silsesquioxane polyaryne hybrid resin and its preparation, can solve problems such as poor mechanical properties of composite materials, and achieve high thermal decomposition temperature and thermal decomposition. Effect of residual rate, good mechanical properties, high thermal or thermal oxidation resistance

Inactive Publication Date: 2008-03-05
EAST CHINA UNIV OF SCI & TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Such as: Luneva et al. have prepared silicon-containing alkyne resins by the reaction of acetylene Grignard reagents and alkyl and aryl silicon halides [L.K.Luneva, A.M.Sladkov, and V.V.Korshak, Vysokomolekulyarnye Soedineniya, Seriya A, 1967, 9 (4) : 910-14.], its heat resistance can reach 450 ℃ ~ 550 ℃; Itoh et al. used magnesium oxide as a catalyst to synthesize a silicon hydrogen aryne resin - MSP resin [a.M.Itoh, M.Mitsuzuka, K.Iwata , K.Inoue.Macromolecules, 1994, 27:7917-7917.b.M.Itoh, K.Inoue, et al., Journal of Materials Science, 2002, 37:3795.], has excellent thermal properties after curing, but due to the material The brittleness and shrinkage during the curing process lead to poor mechanical properties of the composite material; Ohshita et al. successfully synthesized a series of silicon-containing polymers whose side groups are aryne groups by metal lithium method [a.J.Ohshita, A.Yamashita, T. Hiraoka, A. Shimpo, A. Kunai, M. Ishikawa. Macromolecules, 1997, 30: 1540-1549; b. J. Ohshita, A. Shinpo, A. Kunai. Macromolecules, 1999, 32: 5998-6002], the class The polymer has excellent thermal stability, and the weight loss rate at 1000°C is 17%; Buvat et al. have synthesized a phenylacetylene-terminated silicon-hydroaryne resin (called BLJ resin) [Pierrick Buvat., et al., SAMPE Symp. , 2000, 46:134-144], the cured resin did not show glass transition below 450 °C, and the residual rate of decomposition at 1000 °C under argon gas was 80%; Huang Farong et al. also prepared silicon-containing aryne resins with various structures [ [1] Yan Hao, Qi Huimin, Huang Farong, Petrochemical Industry, 2004, 33(9), 880-884; [2] Huang Farong, Du Lei, etc. Chinese Invention Patent, CN1709928, 2005; [3] Fan Wang, et al. , Polymer Bulletin, 2006, 56, 19~26], which greatly improved the process performance, storage stability and mechanical properties of aryne resin

Method used

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  • Sesquialter siloxane polyaryne hybrid resin and preparation method and use thereof
  • Sesquialter siloxane polyaryne hybrid resin and preparation method and use thereof
  • Sesquialter siloxane polyaryne hybrid resin and preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1) Synthesis of octa(tetramethylammonium) silicate

[0040] Add 7.29g of 25% tetramethylammonium hydroxide aqueous solution and 6.61g of methanol into the three-necked flask, and at room temperature under strong stirring, add 4.17g of ethyl orthosilicate dropwise very slowly, and control the dropping within 30 minutes. The vigorous stirring reaction was continued at room temperature for 24h. After the stirring was stopped, it was concentrated to a certain volume and then placed in a refrigerator (4°C) to crystallize. After filtering, washing with acetone, and vacuum drying, 4.41 g of crude octa(tetramethylammonium) silicate was obtained, with a yield of 97%. A 1:1 (volume ratio) mixture of deionized water and methanol can be used for recrystallization to obtain 3.35 g of octa(tetramethylammonium) silicate with a yield of 76%. FT-IR: 3389cm -1 (H 2 O), 3019cm -1 (C-H), 1488cm -1 、1404cm -1 、1397cm -1 、957cm -1 and 948cm -1 (N(CH 3 ) 4 + ), 1013cm -1 (Si-O-S...

Embodiment 2

[0050] Synthesis of POSS-SAR resin (PS-2)

[0051] 0.1g (0.0982mmol) Q 8 m 8 H Add it into a three-necked flask equipped with a stirrer, condenser and constant pressure funnel, add 25mlTHF under nitrogen protection, stir at room temperature for 15min until it is completely dissolved, then add 2.0g (2.67mmol) silicon-containing aryne resin and 3 drops platinum catalyst. The temperature was raised to 70°C for 16h. After the reaction was completed, 5 mg of triphenylphosphine was added, stirred at room temperature for 1 h to inactivate the platinum catalyst, filtered, and the solvent was evaporated under reduced pressure to obtain a resin. FT-IR (KBr): 3295cm -1 (≡CH), 2155cm -1 (C≡C), 1592cm -1 (C=C), 1256cm -1 (Si-C), 1090cm -1 (Si-O-Si). 1 H-NMR (500MHz, CDCl 3 , TMS): 0.1-0.5 (Si-CH 3 ), 3.06(≡CH), 5.5-5.9(CH 2 =CSi[α]), 6.3-7.0 (CH=CHSi[β-trans]), 7.2-7.7 (Ar-H). The resin is a reddish-brown solid with a gel time of 50 minutes at 160°C and is soluble in various ...

Embodiment 3

[0053] Synthesis of POSS-SAR resin (PS-3)

[0054] 0.2g (0.196mmol) Q 8 m 8 H Add it into a three-necked flask equipped with a stirrer, a condenser and a constant pressure funnel, add 25ml of toluene under nitrogen protection, stir at room temperature for 15min until it is completely dissolved, then add 2.0g (2.67mmol) silicon-containing aryne resin and 6 Drops of platinum catalyst. The temperature was raised to 100°C for 24h. After the reaction was completed, 5 mg of triphenylphosphine was added, stirred at room temperature for 1 h to inactivate the platinum catalyst, filtered, and the solvent was evaporated under reduced pressure to obtain a resin. FT-IR (KBr): 3298cm -1 (≡CH), 2155cm -1 (C≡C), 1589cm -1 (C=C), 1256cm -1 (Si-C), 1090cm -1 (Si-O-Si). 1 H-NMR (500MHz, CDCl 3 , TMS): 0.1-0.5 (Si-CH 3 ), 3.07(≡CH), 5.5-5.9(CH 2 =CSi[α]), 6.3-7.0 (CH=CHSi[β-trans]), 7.2-7.7 (Ar-H). The resin is a reddish-brown solid with a gel time of 30 minutes at 160°C and is solu...

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Abstract

The present invention discloses one kind of sesquisiloxane-multiaryne hybrid resin in the structure as shown, its preparation process with octo(dimethyl silicone) sesquisiloxane (Q8M811) and silicon-containing aryne oligomer, and its application in high temperature composite material, such as wave transmitting material, radiation resisting material, etc. The sesquisiloxane-multiaryne hybrid resin has broad application foreground in aviation, space flight, electronics, automobile industry and other fields.

Description

technical field [0001] The invention relates to a silsesquioxane polyaryne hybrid resin and a preparation method thereof, in particular to a silsesquioxane polyaryne silsesquioxane (Q 8 m 8 H ) react with silicon-containing aryne oligomers to obtain an organic-inorganic hybrid resin with excellent processability, heat resistance, mechanical properties and dielectric properties; in addition, the present invention also relates to the polysilsesquioxane Preparation method and application of aryne hybrid resin. Background technique [0002] Polyhedral oligomeric silsesquioxane (POSS for short) is an interesting three-dimensional silicone material connected by silicon and oxygen. The polyhedral structure has a skeleton diameter of 1-3 nm, a molecular weight of more than 1000, and holes in the skeleton. Hexahedral silsesquioxane in cage silsesquioxane is also called T 8 , general formula (RsiO 1.5 ) 8 , its structure is symmetrical, and each face of the hexahedron is compose...

Claims

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Application Information

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IPC IPC(8): C08G77/04C08G77/08B29C70/40
Inventor 黄发荣杜磊周燕杭孝东邓诗峰
Owner EAST CHINA UNIV OF SCI & TECH
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