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Process for preparing hydroxyl polyhedral oligomeric silsesquioxane modified polyurethane

A technology of silsesquioxane and hydroxyl cage type, which is applied in the field of preparation of hydroxyl cage type silsesquioxane modified polyurethane, can solve the problem of limited improvement of thermal stability and the effect of octaphenyl cage type silsesquioxane on the preparation of polyurethane. Polyurethane reinforcement is not very obvious and other problems

Inactive Publication Date: 2012-08-01
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] According to China's "Rubber Industry" magazine (2011, 58: 404-409), polyurethane was modified by cage silsesquioxane, and the research on the performance of modified polyurethane proved that although octavinyl cage Type silsesquioxane has a good reinforcing and toughening effect on polyurethane, but the reinforcing effect of octaphenyl cage silsesquioxane on polyurethane is not obvious. Silosquioxanes physically fill the polyurethane structure with limited improvement in thermal stability

Method used

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  • Process for preparing hydroxyl polyhedral oligomeric silsesquioxane modified polyurethane
  • Process for preparing hydroxyl polyhedral oligomeric silsesquioxane modified polyurethane
  • Process for preparing hydroxyl polyhedral oligomeric silsesquioxane modified polyurethane

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Embodiment 1

[0019] First, dissolve 1.0682g of toluene-2,4-diisocyanate and 12.0000g of polyethylene glycol with a molecular weight of 4000 in 30mL of anhydrous tetrahydrofuran, place them in a reactor under the protection of a nitrogen atmosphere, and drop them under stirring at a temperature of 60°C. Add 0.0035g dibutyltin dilaurate, and react until prepolymer is obtained; then continue to dropwise add 0.1376g dihydroxy-heptaphenyl cage silsesquioxane (2.5% by mole fraction) and 0.1690g 1 A solution prepared by dissolving 4-butanediol in 6 mL of anhydrous tetrahydrofuran until the molar ratio of the total NCO groups and OH groups in the reaction system is 1.2:1, and then continue to react at 60 ° C for 3 h, the The reaction solution was poured into a glass mold uniformly coated with a vegetable oil release agent, and formed into a film in an oven at 80° C. for 48 hours to obtain a polyurethane film modified by hydroxyl cage silsesquioxane.

[0020] In order to compare the advantages of t...

Embodiment 2

[0024] First, dissolve 1.0682g of toluene-2,4-diisocyanate and 12.0000g of polyethylene glycol with a molecular weight of 4000 in 30mL of anhydrous tetrahydrofuran, place them in a reactor under the protection of a nitrogen atmosphere, and add them dropwise at a temperature of 60°C under stirring. 0.0035g dibutyltin dilaurate, react to obtain prepolymer; Continue to add dropwise under stirring by 0.2752g dihydroxyl-heptaphenyl cage silsesquioxane (5.0% molar fraction) and 0.1577g 1, A solution prepared by dissolving 4-butanediol in 6 mL of anhydrous tetrahydrofuran until the molar ratio of the total NCO groups and OH groups in the reaction system is 1.2:1, and then continue to react at 60 ° C for 3 h, the reaction Pour the solution into a glass mold evenly coated with vegetable oil release agent, and form a film in an oven at 80°C for 48 hours to obtain a polyurethane film modified by hydroxyl cage silsesquioxane.

Embodiment 3

[0026]First, dissolve 1.0682g of toluene-2,4-diisocyanate and 12.0000g of polyethylene glycol with a molecular weight of 4000 in 30mL of anhydrous tetrahydrofuran, place them in a reactor under the protection of a nitrogen atmosphere, and drop them under stirring at a temperature of 60°C. Add 0.0035g dibutyltin dilaurate, and react until prepolymer is obtained; then continue to dropwise add 0.4129g dihydroxyl-heptaphenyl cage silsesquioxane (mole fraction 7.5%) and 0.1465g 1 A solution prepared by dissolving 4-butanediol in 6 mL of anhydrous tetrahydrofuran until the molar ratio of the total NCO groups and OH groups in the reaction system is 1.2:1, and then continue to react at 60 ° C for 3 h, the The reaction solution was poured into a glass mold uniformly coated with a vegetable oil release agent, and formed into a film in an oven at 80° C. for 48 hours to obtain a polyurethane film modified by hydroxyl cage silsesquioxane.

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Abstract

The invention discloses a process for preparing hydroxyl polyhedral oligomeric silsesquioxane modified polyurethane, which includes the steps of reacting diisocyanate with polyether diols in the presence of catalyst and under protection of nitrogenous atmosphere to obtain prepolymer, adding 1, 4-butanediol and polyhedral oligomeric silsesquioxane to serve as chain extenders to fully react, and preparing modified polyurethane having good film forming property and heat resistance through chemical bonding modification, so that defects of poor abrasion resistance and heat resistance of traditional polyurethane are overcome. When the content of the hydroxyl polyhedral oligomeric silsesquioxane is increased from 0 to 10%, the glass-transition temperature of the modified polyurethane is increased by 4.7 DEG C, i.e. from -33.5 DEG C to -28.8 DEG C, the melting temperature is increased by 10.2 DEG C, i.e. from 44.3 DEG C to 54.5 DEG C, and the thermal decomposition temperature of the modified polyurethane is respectively increased by 35.5 DEG C and 11.9 DEG C.

Description

technical field [0001] The invention belongs to the technical field of polyurethane preparation technology, and in particular relates to a preparation method of hydroxyl cage silsesquioxane modified polyurethane. Background technique [0002] Taiwan, China "Materials Chemistry and Physics" (Materials Chemistry and Physics, 2009, 117 (1), 91-98 pages) introduces a kind of trans-cyclohexyl-diisobutyl hydroxycage silsesquioxane through Sol-gel technology is used to synthesize polyurethane / hydroxycage silsesquioxane hybrid coatings, and it is proved that hydroxycage silsesquioxane is uniformly dispersed in the polyurethane network through scanning electron microscopy and atomic mechanical microscopy. The successful reaction between the silanol bond of hydroxyl cage silsesquioxane and polyurethane resin was verified by volume gel chromatography, Fourier transform infrared and X-ray crystal diffraction analysis. However, this method does not significantly improve the thermal stab...

Claims

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Application Information

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IPC IPC(8): C08G18/66C08G18/48C08G18/32C08G18/10
Inventor 王文平丁伟良田健
Owner HEFEI UNIV OF TECH
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