Preparation method of isobutyl cage type polysilsesquioxane modified polyurethane

A polysilsesquioxane and isobutyl technology is applied in the preparation field of isobutyl cage polysilsesquioxane modified polyurethane, which can solve the problems of poor dimensional stability, poor thermal stability, production and application of polyurethane materials restrictions, etc.

Inactive Publication Date: 2016-10-12
SICHUAN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to its poor thermal stability, PU in practical applications is extremely vulnerable to the external environment during processing. of The disadvantages of poor shape stability and weak rigidity caused by the impact of the polyurethane material have limited the production and application of polyurethane materials.

Method used

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  • Preparation method of isobutyl cage type polysilsesquioxane modified polyurethane
  • Preparation method of isobutyl cage type polysilsesquioxane modified polyurethane
  • Preparation method of isobutyl cage type polysilsesquioxane modified polyurethane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] First place 1.8g of isobutyl cage polysilsesquioxane in a vacuum oven at a constant temperature of 100°C for 24 hours. After natural cooling in vacuum, dissolve it in 3.7g of 4,4'-diisocyanate In benzene methane, stir in a three-necked flask protected by a nitrogen atmosphere at 40°C until the isobutyl cage polysilsesquioxane is completely dissolved to obtain a prepolymer; 21.2 g of polyether polyols with a molecular weight of 3000 were dissolved in the three-necked bottle, and the stirring was continued for more than 2 hours. Then the transparent viscous liquid obtained is evenly spread on a glass plate, placed in a vacuum oven at 25mmHg, and dried overnight at a constant temperature of 60°C to obtain a polyurethane film modified by isobutyl cage polysilsesquioxane (the content of isobutyl cage polysilsesquioxane is 7wt%).

[0020] In order to compare the performance difference between the isobutyl cage polysilsesquioxane modified polyurethane prepared by the method o...

Embodiment 2

[0023] First place 3g of isobutyl cage polysilsesquioxane in a vacuum oven at a constant temperature of 100°C for 24 hours, and after natural cooling in vacuum, dissolve it in 3.7g of 4,4′-diphenyl diisocyanate In methane, stir in a three-necked flask protected by a nitrogen atmosphere at 40°C until the isobutyl cage polysilsesquioxane is completely dissolved to obtain a prepolymer; then, continue to stir in a nitrogen atmosphere and stir Dissolve 16.6g of polyether polyol with a molecular weight of 3000 in the three-necked bottle, continue to stir for more than 2 hours, spread the obtained transparent viscous liquid evenly on a glass plate, place it in a vacuum oven at 25mmHg, 60°C Dry overnight at constant temperature to obtain isobutyl cage polysilsesquioxane-modified polyurethane (wherein the content of isobutyl cage polysilsesquioxane is 13wt%).

Embodiment 3

[0025] First place 4.4g of trihydroxytriisobutyl cage polysilsesquioxane in a vacuum oven at a constant temperature of 100°C for 24 hours, and then dissolve it in 3.7g of 4,4'-diiso In diphenylmethane cyanate, stir in a three-necked flask protected by a nitrogen atmosphere at 40°C until the isobutyl cage polysilsesquioxane is completely dissolved to obtain a prepolymer; 1. Dissolve 11.5g of polyether polyol with a molecular weight of 3000 in the three-necked bottle under stirring, continue to stir for more than 2 hours, spread the obtained transparent viscous liquid evenly on a glass plate, and place it in a vacuum oven at 25mmHg and dry overnight at a constant temperature of 60°C to obtain isobutyl cage polysilsesquioxane-modified polyurethane (wherein the content of isobutyl cage polysilsesquioxane is 22wt%).

[0026] figure 2 It is the dynamic thermomechanical property spectrum of isobutyl cage polysilsesquioxane modified polyurethane. It can be seen that the glass trans...

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Abstract

The invention discloses a preparation method of isobutyl cage polysilsesquioxane modified polyurethane. First, the isobutyl cage polysilsesquioxane is pretreated in a vacuum oven, and then mixed with xylene Diisocyanate is reacted to prepare prepolymer, and then polyether polyol VORANOL 3010 is added for chain extension reaction, and modified by chemical bonding to prepare nano-organic-inorganic hybrid modified polyurethane. When the content of isobutyl cage polysilsesquioxane increased from 0% to 22%, the glass transition temperature of the modified polyurethane increased from ‑44.3 to ‑13.9°C, an increase of 30.4°C. The mechanical properties have been significantly improved. At the same time, with the increase of isobutyl cage polysilsesquioxane content, some sharp diffraction peaks appeared in the X-ray diffraction pattern of the modified polyurethane. Compared with the X-ray diffraction patterns of pure polyurethane, it can be concluded that the increase of the content of isobutyl cage polysilsesquioxane promotes the formation of crystal clusters and the obvious hard segment-soft segment microphase separation in the modified polyurethane structure Phenomenon, to a certain extent, improve the shaping of modified polyurethane.

Description

technical field [0001] The invention belongs to the technical field of polyurethane preparation technology, and in particular relates to a preparation method of isobutyl cage polysilsesquioxane modified polyurethane. Background technique [0002] In the early 1990s, cage-type silsesquioxane POSS compounds received more and more attention because of the work of two research groups, one was from the Feher group at the University of California, and the other was from Lichtenhan in the United States. team. The former has designed a variety of methods for the synthesis and modification of the well-defined Si / O structure. For example, the catalytic hydrogenation of aryl groups on POSS provides efficient aliphatic silsesquioxanes. These new silsesquioxanes are compared with POSS with aryl group has greater solubility in common organic solvents. The latter did a completely different job. Lichtenhan's group synthesized a series of POSS compounds, all of which have corresponding fun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08G18/10C08G18/61C08G18/48
Inventor 不公告发明人
Owner SICHUAN NORMAL UNIVERSITY
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