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A Two-step Synthesis Method of Polyurethane Modulus Gradient Material

A technology of gradient modulus and polyurethane, which is applied in the field of two-step synthesis of polyurethane modulus gradient materials, can solve the problems of non-overlapping functional areas, unfavorable high-performance engineering materials, temperature sensitivity, etc.

Active Publication Date: 2017-01-04
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

First, the rubber material must have high elasticity in the rubber state, but its damping performance has a maximum value in the glass transition region. When an elastic material is required to have high elasticity and high damping performance at the same time, the traditional rubber material appears to be functional. Second, in the glass transition region, the elastic modulus of traditional rubber materials changes greatly with temperature changes, showing a high degree of temperature sensitivity, which is extremely unfavorable for high-performance engineering materials; Third, the glass transition region is usually only 20-30°C, and the material required to have damping properties is often in the temperature range of 60°C or even wider
[0004] The above three shortcomings are inevitable problems of traditional polymer materials

Method used

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  • A Two-step Synthesis Method of Polyurethane Modulus Gradient Material

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Experimental program
Comparison scheme
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 synthesis method of a polyurethane modulus gradient material. In the first step, the isocyanate-terminated polyurethane prepolymer is synthesized from low molecular weight polyether diol and aromatic diisocyanate; in the second step, the above product is mixed with aromatic diisocyanate in different molar ratios, and then neutralized in a solvent The cyclotrimerization reaction is carried out in the bulk state, and finally the polyurethane modulus gradient material is obtained. The advantages of this synthesis method are: the first step has good reaction stability, and the product quality is stable and controllable; the second step reaction system has low viscosity and uniform mixing, which is beneficial to the molding process of the material, and by adjusting the molar ratio of the reactants, it can be obtained. Materials with different moduli of elasticity. Unlike traditional polyurethane materials, polyurethane materials with gradient modulus have no obvious glass transition region, and their elastic modulus shows a gradual decrease 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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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/48C08G18/10C08G18/18
Inventor 江盛玲张孝阿齐士成吕亚非
Owner BEIJING UNIV OF CHEM TECH