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Synthesis method for substituting sesquialter siloxane by non-functional alkyl

A polysilsesquioxane and a synthesis method technology, applied in the direction of silicon organic compounds and the like, can solve the problems of restricting the research, popularization and application of POSS compounds, complicated separation and purification processes, and high synthesis cost, and achieve good product structure unity, The process is simple and easy to implement, and the effect of short reaction time

Inactive Publication Date: 2007-10-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] However, at present, acetone is generally used as a solvent during synthesis, and a single acid or base is used as a catalyst. The reaction cycle is long (at least 3 days, even several months), the separation and purification process is complicated, and the yield is very low.
Therefore, the synthesis cost is high, which limits the research, popularization and application of POSS compounds.

Method used

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  • Synthesis method for substituting sesquialter siloxane by non-functional alkyl
  • Synthesis method for substituting sesquialter siloxane by non-functional alkyl
  • Synthesis method for substituting sesquialter siloxane by non-functional alkyl

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Embodiment 1

[0016] Embodiment 1: the synthesis of the clathrate octapolysilsesquioxane of methyl substitution

[0017] A 500ml three-neck flask was placed in a constant temperature water bath at 80°C, and 90g (5mol) of deionized water, 40ml of acetone, 10ml of acetonitrile, 10ml (about 0.1mol) of triethylamine, and 0.5ml of a mixture of concentrated hydrochloric acid and formic acid with a volume ratio of 1:1 were sequentially Add to the three-necked flask, stir to make it evenly mixed. Then, 178 g (1 mol) of methyltriethoxysilane was added dropwise to the mixed solution, and stirred at 80° C. for 18 h at constant temperature under reflux. The crude product in the form of light yellow powder was obtained by filtration. The crude product was washed three times with 1000 ml of deionized water, then washed with acetone, and dried in vacuum to obtain the final product in the form of white powder with a yield of 86.0%. The molecular structural formula is as follows:

[0018]

Embodiment 2

[0019] Example 2: Synthesis of methyl-substituted cage octapolysilsesquioxane

[0020] Place a 500ml three-neck flask in a water bath with a constant temperature of 50°C, add 180g (10mol) of deionized water, 67ml of acetone, 33ml of acetonitrile, 30ml (about 0.3mol) of trimethylamine, and 5ml of a mixture of concentrated hydrochloric acid and acetic acid with a volume ratio of 1:3. To the three-necked flask, stir to make it evenly mixed. Then 178 g (1 mol) of methyltriethoxysilane was added dropwise to the mixed solution, and stirred under constant temperature at 50° C. for 18 h under reflux. Filter to obtain a light yellow powdery crude product, first wash the crude product with 1000ml deionized water for 3 times, then wash with acetone, and vacuum dry to obtain a white powdery final product. Yield 88.2%.

Embodiment 3

[0021] Embodiment 3: Synthesis of cyclopentyl-substituted clathrate octasilsesquioxane

[0022] Place a 500ml three-neck flask in a constant temperature water bath at 70°C, mix 144g (8mol) of deionized water, 35ml of methyl ethyl ketone, 15ml of butyronitrile, 12ml (about 0.2mol) of trimethylamine, and 2ml of concentrated hydrochloric acid and acetic acid at a volume ratio of 1:2 The solution was added into the three-necked flask in turn, and stirred to make it evenly mixed. Then 232 g (1 mol) of cyclopentyltriethoxysilane was added dropwise to the mixed solution, and stirred under constant temperature at 70° C. for 18 h under reflux. The solvent was removed under vacuum at room temperature to obtain the crude product as light yellow powder. The crude product was first washed with 1000 ml of deionized water for 3 times, then washed with acetone, and vacuum-dried to obtain a white powdery final product with a yield of 85.5%. The molecular structural formula is as follows:

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Abstract

The disclosed high-yield synthesis method for cage octa-silsesquioxanes substituted by non-functional alkyl comprises: with continual stirring at 50-80Deg, dripping the alkyltrialkoxy silane of 1mol into the mixed liquid with 5-10mol deionized water, 50-100ml solvent with ketone and cyanogen, 0.1-0.3ml trialkylamine as structural inhibitor and 0.5-5ml catalyst with strong HCl and organic acid; with constant temperature of 50-80Deg, refluxing and stirring for 18h, and filtering to obtain the coarse product; cleaning by deionized water with mass as 10-20 times to the coarse product then by the acetone; finally, vacuum drying. This invention can speed up hydrolysis and the structural form, and decreases side reaction.

Description

technical field [0001] The invention relates to the synthesis technology of polymers, in particular to a synthesis method of non-functional alkyl substituted cage octapolysilsesquioxane. Background technique [0002] Cage silsesquioxane, also known as polyhedral oligomeric silsesquioxane (POSS), can be used as the precursor of organic-inorganic hybrid materials, additives (crosslinking agent, thermal performance modifier, viscosity adjustment Agents), functional polymers (medical polymers, advanced non-metallic materials, semiconductor materials, optical materials), liquid crystal materials, electroluminescent films and heterogeneous and homogeneous catalysts, etc., have broad application prospects. POSS is an organic-inorganic nano-hybrid structural unit with a special three-dimensional structure, with a three-dimensional size of about 1.5nm and 1-8 organic groups. Its molecular formula can be expressed as (RSiO 1.5 ) 8 , whose chemical composition is between silicon dio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21
Inventor 顾嫒娟梁国正张增平王结良卢婷利
Owner ZHEJIANG UNIV
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