Two-step synthetic method of polyurethane modulus gradient material

A technology of gradient modulus and polyurethane, applied in the field of two-step synthesis of polyurethane modulus gradient materials

Active Publication Date: 2015-01-28
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The above three shortcomings are inevit

Method used

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  • Two-step synthetic method of polyurethane modulus gradient material

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Experimental program
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Effect test

Embodiment 1

[0022] Add 200g (0.2mol) of polyoxypropylene glycol (PPG 1000) into a 1000mL three-neck flask, attach a thermometer and a reflux condenser, and dehydrate under reduced pressure at 105°C and a vacuum of 0.1MPa. After 2 hours of dehydration, the temperature began to drop. When the temperature was lower than 70°C, 200 g of acetone and 56 g (0.32 mol) of toluene diisocyanate (TDI) were added, and refluxed for 2.5 hours to obtain a polyurethane prepolymer. Continue to add the TDI of 25.6g (the 10wt% of polyurethane prepolymer) in reaction system, add the N of 2.1g again, the bisphenol A diglycidyl ether of N-dimethyl benzyl amine and 2.1g (catalyst consumption is 1.5 wt%), after reacting at 60°C for 10min, the solution was poured into a polytetrafluoroethylene mold, acetone volatilized and then bulk polymerized. ester-isocyanate), yield 96.8%.

Embodiment 2

[0024] Add 200g (0.2mol) of polyoxypropylene glycol (PPG 1000) into a 1000mL three-neck flask, attach a thermometer and a reflux condenser, and dehydrate under reduced pressure at 105°C and a vacuum of 0.1MPa. After dehydration for 2 hours, the temperature began to drop. When the temperature was lower than 70°C, 200 g of acetone and 59 g (0.34 mol) of toluene diisocyanate (TDI) were added, and refluxed for 3 hours to obtain a polyurethane prepolymer. Continue to add the TDI of 25.9g (the 10wt% of polyurethane prepolymer) in reaction system, add the N of 2.1g again, the bisphenol A diglycidyl ether of N-dimethyl benzyl amine and 2.1g (catalyst consumption is 1.5 wt%), after reacting at 60°C for 10min, the solution was poured into a polytetrafluoroethylene mold, acetone volatilized and then bulk polymerized, the heating conditions were 80°C / 2h+100°C / 2h+120°C / 2h, and finally 273g of poly(ammonia ester-isocyanate), yield 94.3%.

Embodiment 3

[0026] Add 200g (0.2mol) of polyoxypropylene glycol (PPG 1000) into a 1000mL three-neck flask, attach a thermometer and a reflux condenser, and dehydrate under reduced pressure at 105°C and a vacuum of 0.1MPa. After 2 hours of dehydration, the temperature began to drop. When the temperature was lower than 70°C, 200 g of acetone and 62 g (0.36 mol) of toluene diisocyanate (TDI) were added, and refluxed for 4 hours to obtain a polyurethane prepolymer. In the reaction system, continue to add the TDI of 26.2g (10wt% of polyurethane prepolymer), add the N of N, N-dimethyl benzyl amine and the bisphenol A diglycidyl ether of 2.2g again (catalyst consumption is 1.5 wt%), after reacting at 60°C for 10min, the solution was poured into a polytetrafluoroethylene mold, acetone volatilized and then bulk polymerized. ester-isocyanate), yield 97.2%.

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Abstract

The invention provides a two-step synthetic method of a polyurethane modulus gradient material. The method is as below: first, using low molecular weight polyether glycol and aromatic diisocyanate as raw materials to synthesize an isocyanate terminated polyurethane prepolymer; and second, mixing the product with aromatic diisocyanate in different molar ratios, and then conducting ring trimerization reaction in the solvent under body condition, so as to finally obtain the polyurethane modulus gradient material. The synthetic method has the advantages that the first step has reaction stability and stable and controllable product quality, and the second step reaction system has low viscosity and even mixing, and is conducive to forming process of the material, and materials with different elastic modulus can be obtained by adjusting the molar ratio of the reactants. Different from the traditional polyurethane, the polyurethane modulus gradient material does not have obvious glass transition region, and shows gradual decrease of the elastic modulus with the increase of temperature.

Description

technical field [0001] The invention relates to a two-step synthesis method of a polyurethane modulus gradient material. The method takes polyether diol and aromatic diisocyanate as the main raw materials, first reacts in a solvent to obtain an isocyanate-terminated polyurethane prepolymer, and then further performs cyclotrimerization reaction with aromatic diisocyanate under the action of a catalyst to obtain Polyurethane modulus gradient material with three-dimensional crosslinked structure of isocyanate three-membered ring and flexible linking chain. Test its tensile properties at room temperature and high temperature. Background technique [0002] "Functional Gradient Material" is proposed to reduce the interface thermal stress of ceramic / metal composite high-temperature resistant materials. The basic principle is to select two or more materials with different properties and change the microscopic elements of the two materials in a stepwise manner. (such as composition...

Claims

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Application Information

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IPC IPC(8): C08G18/48C08G18/10C08G18/18
CPCC08G18/10C08G18/4825C08G18/7614
Inventor 江盛玲张孝阿齐士成吕亚非
Owner BEIJING UNIV OF CHEM TECH
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