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Novel alkoxy silane based POSS (polyhedral oligomeric silsesquioxanes) as well as preparation method and application thereof

An alkoxysilyl group, a new type of technology, applied in the direction of silicon organic compounds, can solve the problems of enhancing mechanical properties and thermal properties, and achieve the effect of improving mechanical properties and thermal properties.

Active Publication Date: 2013-09-11
武汉绿凯科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] When POSS is introduced into silicone rubber and silicone resin in a blended manner, due to the small force between the polysiloxane main chain and POSS molecules, POSS molecules tend to aggregate and crystallize themselves, thus failing to achieve enhanced mechanical properties and thermal properties the role of

Method used

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  • Novel alkoxy silane based POSS (polyhedral oligomeric silsesquioxanes) as well as preparation method and application thereof
  • Novel alkoxy silane based POSS (polyhedral oligomeric silsesquioxanes) as well as preparation method and application thereof
  • Novel alkoxy silane based POSS (polyhedral oligomeric silsesquioxanes) as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Anhydrous ether 500g, trimethoxysilane 4.88g (39.5mmol) and H 2 [PtCl 6] (dissolved in isopropanol, concentration 4wt%, take 0.5g) and octavinyl T8-POSS (Vinyl-POSS) 5.00g (7.90mmol, the number of moles of double bonds is 63.20mmol) into a 1000mL three-necked flask , reacted at 35°C for 8h, cooled to 20°C and continued to stir for 15h. After the reaction, add activated carbon, stir at 35°C for 0.5h, filter the obtained black ether solution through silica gel and diatomaceous earth to obtain a clear liquid, concentrate the obtained clear liquid, and obtain 9.78 g of a colorless oily liquid as the obtained product Si 8 o 12 R 1 3 R 3 5 (R 1 = Vinyl, R 3 = trimethoxysilylethyl), yield 98.9%. The NMR characterization results of the product are: 1 HNMR (CDCl 3 ,ppm):δ5.78-6.15(m,H 2 C=CH-,9H),3.55(s,-OCH 3 ,45H),0.66(m,Si-CH 2 ,20H).

[0029] Add commercially available 107# hydroxyl-terminated silicone oil (60.00g) with a viscosity of 80,000 cP into the knead...

Embodiment 2

[0031] Anhydrous tetrahydrofuran (THF) 13g, triethoxysilane 3.90g (32.0mmol) and H 2 [PtCl 6 ] (dissolved in isopropanol, concentration 4wt%, take 0.5g) and tetravinyl tetracyclopentyl T8-POSS (CAS Registry Number: 1228876-88-7) 6.4g (8.00mmol, the number of moles of double bonds 32mmol) into a 100mL three-necked flask, reacted at 65°C for 4h, cooled to 65°C, added activated carbon, stirred at 65°C for 0.5h, filtered the obtained black ether solution through silica gel and diatomaceous earth to obtain a clear liquid, and the obtained clear The solution was concentrated to obtain 10.07 g of a colorless oily liquid, which is the product Si 8 o 12 R 2 4 R 3 4 (R 2 = Cyclopentyl, R 3 = triethoxysilylethyl), yield 97.8%. The NMR characterization results of the product are: 1 HNMR (CDCl 3 ,ppm):δ3.75(m,-OCH 2 CH 3 ,24H),1.4~1.72(m,-C 5 h 9 ,36H),1.36(t,-OCH 2 CH 3 36H),0.61(q,Si-CH 2 ,16H).

[0032] Condensation-type RTV silicone rubber was prepared according to t...

Embodiment 3

[0034] Add 50 g of dichloromethane and 9.50 g of deca(3-(3-methacryloyloxy)propyl)T10-POSS (prepared according to the literature: Dalton Trans., 2010, 39, 3239–32440) into a 250 mL three-necked flask ( 5.0mmol, the mole number of double bonds is 50mmol) and triphenylrhodium chloride catalyst 1.9g (dissolved in THF, concentration 10wt%), after stirring at 40°C for 0.5h, dichloromethane 100mL and dimethyl chloride were added dropwise Add the mixed solution of 0.47g (5.0mmol) silane within 2h, continue to react at 40°C for 4h, add activated carbon after cooling down, stir at 40°C for 0.5h, filter the obtained ether solution through silica gel and diatomaceous earth, Concentrate the resulting clear liquid to obtain 9.86 g of white solid, which is the product Si 10 o 15 R 1 R 3 9 (R 1 =3-(3-methacryloyloxy)propyl, R 3 =(CH 3 ) 2 ClSiCH 2 CH 2 COOC 3 h 6 -), yield 98.9%. The NMR characterization results of the product are: 1 HNMR (CDCl 3 ,ppm): δ6.3~6.4(d,-OCOC(CH 3 ...

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Abstract

The invention discloses novel alkoxy silane based POSS (polyhedral oligomeric silsesquioxanes) as well as a preparation method and application thereof, belonging to the fields of chemical industry and organic polymer materials. The POSS has a general molecular formula of SixOyR1nR2x-m-nR3m, wherein x is 8, 10 or 12, y=1.5x, n=0-(x-1), m=1-x, m+n is less than or equal to x, and m and n are integers. The preparation method comprises the following steps of: taking POSS raw materials, and performing a hydrosilation reaction on the POSS raw materials and hydrogen-containing silane under the action of a hydrosilation catalyst to obtain a target product. According to the preparation method, an alkoxy silane base is introduced into the POSS, and radicals including Si-OH, Si-H, Si-OR and the like in the alkoxy silane base and a polysiloxane system are used for reacting to form a Si-O-Si bond, so that the alkoxy silane based POSS can obviously promote mechanical properties and thermal properties of silicon resin and silicon rubber when added into condensed type silicon resin and room temperature vulcanized silicon rubber.

Description

technical field [0001] The invention relates to a polyhedral oligomeric silsesquioxane (POSS) and a preparation method thereof, in particular to a novel alkoxysilane-based POSS, a preparation method and application thereof, belonging to the fields of chemical engineering and organic polymer materials. Background technique [0002] Polyhedral oligomeric silsesquioxanes (Polyhedral oligomeric silsesquioxanes, referred to as POSS) is a kind of cage-type oligomeric siloxane with a three-dimensional structure. The general molecular formula is: (RSiO 1.5 ) n , n=4, 6, 7, 8, 10, 12, etc., R can be a hydrogen atom, a chlorine atom, an alkyl group, an aryl group, an alkenyl group or the like. In the early 1990s, Lichtenhan and others were committed to preparing copolymer materials containing POSS for making rocket propulsion insulation layers, and POSS aroused people's research interest. In 2003, the American Hybrid Plastics Company began commercial production of various POSS monom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21C08K5/549C08L83/04C08L83/06
Inventor 黄驰易生平张方方黄成
Owner 武汉绿凯科技有限公司
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