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Synthesis method of multi-amino polyhedral oligomeric silsesquioxanes

A technology of silsesquioxane and a synthesis method, which is applied in the synthesis field of polyamino cage-type silsesquioxane, can solve the problems of restricting the research, popularization and application of POSS compounds, complicated separation and purification process, and high synthesis cost, and achieves Good product structure, simple process and short reaction time

Inactive Publication Date: 2006-07-19
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] However, at present, acetone is generally used as a solvent in synthesis, and inorganic acid or alkali is used as a catalyst. The reaction cycle is long, the separation and purification process is complicated, and the yield is very low, so that the synthesis cost is high, which greatly limits the research and promotion of POSS compounds. and applications

Method used

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  • Synthesis method of multi-amino polyhedral oligomeric silsesquioxanes
  • Synthesis method of multi-amino polyhedral oligomeric silsesquioxanes
  • Synthesis method of multi-amino polyhedral oligomeric silsesquioxanes

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Experimental program
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Effect test

Embodiment 1

[0019] Place a 500ml three-necked flask in a constant temperature water bath at 50°C, first add 90g (5mol) of deionized water, 40ml of ethanol, 10ml of acetonitrile, 10ml (about 0.1mol) of triethylamine and 2ml of tetramethylammonium hydroxide to the three-necked flask in sequence , stirring at medium speed to make it evenly mixed. Then, 221 g (1 mol) of γ-aminopropyltriethoxysilane was added dropwise to the mixed solution, and stirred at reflux at constant temperature for 18 hours at 50°C. 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 92.0%. Its molecular structural formula is as follows:

[0020]

Embodiment 2

[0022] Place a 1000ml three-necked flask in a constant temperature water bath at 80°C, first add 180g (10mol) of deionized water, 80ml of ethanol, 20ml of acetonitrile, 20ml (about 0.2mol) of triethylamine and 5ml of tetraethylammonium hydroxide into the three-necked flask in sequence , stirring at medium speed to make it evenly mixed. Then, 221 g (1 mol) of γ-aminopropyltriethoxysilane was added dropwise to the mixed solution, and stirred at 80° C. for 18 h at constant temperature 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 3 times with 1000 ml of deionized water, then washed with acetone, and vacuum-dried to obtain a white powdery final product. Yield 90.5%.

Embodiment 3

[0024] Put a 1000ml three-necked flask in a constant temperature water bath at 70°C, first add 180g (10mol) of deionized water, 60ml of ethanol, 30ml of propionitrile mixed solvent, 30ml (about 0.3mol) of trimethylamine, and 3ml of tetramethylammonium hydroxide to the three-necked flask in sequence Mix at medium speed to combine evenly. Then, 221 g (1 mol) of γ-aminopropyltriethoxysilane was added dropwise into the mixed solution, and stirred under constant temperature reflux at 70° C. for 18 h. 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 93.0%.

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Abstract

The disclosed high-yield synthesis method for cage polyamino silsesquioxanes comprises: at 50-80Deg, dripping the gamma-aminoprotriethoxy silane of 1mol into the mixed liquid with 5-10mol deionized water, 50-100ml solvent with ethanol and cyanogen, 0.1-0.3ml trialkylamine as structural inhibitor and 2-5ml catalyst with amine compound; at 50-80Deg, refluxing and stirring for 18h, and removing the solvent at normal temperature to obtain the coarse product; cleaning by deionized water with mass as 10-20 times then by the acetone; finally, vacuum drying. This invention can speed up hydrolysis and the structural form, decreases side reaction.

Description

technical field [0001] The present invention relates to the synthesizing technology of polymer, specifically a kind of synthesizing method of polyaminocage silsesquioxane. Background technique [0002] Silsesquioxanes can be used as organic-inorganic hybrid material precursors, additives (crosslinking agents, thermal performance modifiers, viscosity modifiers), functional polymers (medical polymers, advanced non-metallic materials, semiconductor materials, Optical materials), liquid crystal materials, electroluminescent films, heterogeneous and homogeneous catalysts, etc., have broad application prospects. [0003] Polyhedral Oligomeric silsesquioxane (POSS), also known as cage silsesquioxane, is an organic-inorganic nano-hybrid structural unit with a special three-dimensional structure. - 8 reactive organic groups. Its molecular formula can be expressed as (RSiO 1.5 ) 8 , whose composition is between silicon dioxide (SiO 2 ) and silicone resin (R 2 Between SiO), the p...

Claims

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Application Information

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IPC IPC(8): C07F7/21
Inventor 顾媛娟梁国正张增平王结良卢婷利
Owner ZHEJIANG UNIV
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