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Method for preparing biodegradable aliphatic thermoplastic poly(ester urethane) and its elastomer by non-isocyanate method

A non-isocyanate method and biodegradable technology, which is applied in the field of non-isocyanate method to prepare biodegradable aliphatic thermoplastic poly(ester urethane) and its elastomers, can solve the problem that it is not suitable for TPU materials, and it is difficult to meet the requirements of plastics or elastomers. , low glass transition temperature, etc.

Active Publication Date: 2018-03-30
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although linear polyurethane can be obtained by the reaction of two-membered ring carbonate and diamine, the structure contains a large number of hydroxyl groups, which is a random structure, and the glass transition temperature is often low, so it is not suitable for TPU materials in the usual sense. Difficult to meet requirements for use as a plastic or elastomer

Method used

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  • Method for preparing biodegradable aliphatic thermoplastic poly(ester urethane) and its elastomer by non-isocyanate method
  • Method for preparing biodegradable aliphatic thermoplastic poly(ester urethane) and its elastomer by non-isocyanate method
  • Method for preparing biodegradable aliphatic thermoplastic poly(ester urethane) and its elastomer by non-isocyanate method

Examples

Experimental program
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Embodiment 1

[0026] 1) Preparation of hydroxyl-terminated polybutylene adipate oligomer (PrePBA): 36.38 parts by weight of adipic acid, 33.75 parts of 1,4-butanediol, 0.14 parts of phosphorous acid, 0.14 parts of After stannous chloride was reacted at 150°C for 1 hour, the temperature was gradually raised to 200°C. When the amount of water evaporated reached the theoretical value, the water pump was used to gradually reduce the pressure for 4 hours, and then the oil pump was used to reduce the pressure to 1-5mmHg for 3 hours. A polybutylene adipate prepolymer PrePBA having an acid value of 1.91 mgKOH / g and a hydroxyl value of 68.54 mgKOH / g was obtained.

[0027] 2) Synthesis of diurethane diol prepolymer: Weigh 20 parts of hexamethylene diurethane diol monomer and 0.04 part of stannous chloride in parts by weight, melt and polycondense under reduced pressure with a water pump at 170°C for 1 hour, and then use The oil pump was decompressed to a vacuum degree of 1 to 5 mmHg and reacted for 1...

Embodiment 2

[0030] 1) Synthesis of hexamethylenediurethanediol prepolymer: Weigh 20 parts of hexamethylenediurethanediol monomer and 0.04 part of stannous chloride in parts by weight, react under reduced pressure with a water pump at 170°C for 1 hour, and then use The oil pump was decompressed to a vacuum degree of 1 to 5 mmHg and reacted for 2.3 hours to obtain a hexamethylene diurethane diol prepolymer with a hydroxyl value of 55.60 mgKOH / g.

[0031] 2) Take by weight 6.33 parts and 0.012 parts of stannous chloride of 6.33 parts of hexamethylenediurethane diol prepolymer prepared in 5 parts of PrePBA prepared in embodiment 1 step 1), embodiment 2 step 1), in At 170°C, use an oil pump to depressurize to 1-5mmHg and react until the viscosity of the polymer no longer increases. The number average molecular weight of the obtained poly(ester urethane) is 17900, and the melting point is T m It is 94.21°C, its tensile strength is 14.52MPa, its elongation at break is 629.35%, its rebound rate a...

Embodiment 3

[0033] 1) Synthesis of diurethane diol prepolymer: Weigh 20 parts of hexamethylene diurethane diol monomer and 0.04 part of stannous chloride in parts by weight, react under reduced pressure with a water pump at 170°C for 1 hour, and then use an oil pump to Reduce the pressure to a vacuum degree of 1-5 mmHg and react for 7.2 hours to obtain a hexamethylene diurethane diol prepolymer with a hydroxyl value of 37.69 mgKOH / g.

[0034] 2) Take by weight 5 parts of PrePBA prepared in embodiment 1 step 1) and 9.34 parts of hexamethylene diurethane diol prepolymer prepared in embodiment 3 step 1), 0.012 part of stannous chloride at 170 ℃ with an oil pump to depressurize to 1-5mmHg and react until the viscosity of the polymer no longer increases. The number-average molecular weight of the obtained poly(ester urethane) is 17300, and the melting point is T mIt is 113.23°C. Its tensile strength is 18.81MPa, its elongation at break is 450.04%, its rebound rate is 67.12% when stretched at ...

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Abstract

The invention relates to a method for preparing biodegradable aliphatic thermoplastic poly (ester urethane) and elastomer thereof through a non-isocyanate method, and belongs to the technical field of polyurethane. Firstly, melt phase polycondensation is conducted on aliphatic dibasic acids and superfluous dihydric alcohols to prepare polyester oligomer with terminal hydroxyl groups, then further polycondensation is conducted on prepolymer prepared by self polymerization of diurethaneglycol and the polyester oligomer with the terminal hydroxyl groups, and the biodegradable aliphatic thermoplastic poly (ester urethane) and the elastomer thereof can be obtained. The method for preparing the biodegradable aliphatic thermoplastic poly (ester urethane) and the elastomer thereof through the non-isocyanate method has the advantages of being easy and simple to operate, free from pollution, green and environmentally friendly; the obtained thermoplastic poly (ester urethane) is easy to crystallize, structural adjustment and control are convenient, and comparatively high melting point, good thermal performance and mechanical performance are achieved.

Description

technical field [0001] The invention relates to a method for preparing biodegradable aliphatic thermoplastic poly(ester urethane) and its elastomer by a non-isocyanate method. First, aliphatic dibasic acid and dibasic alcohol are reacted to synthesize a hydroxyl-terminated polyester oligomer. Then it reacts with diurethane diol oligomer to synthesize biodegradable aliphatic thermoplastic poly(ester urethane) and elastomer, and the number average molecular weight of the obtained polymer reaches 35900, which belongs to the technical field of polyurethane. technical background [0002] Thermoplastic polyurethane (TPU) is an important class of polymer materials with good strength, toughness and wear resistance, and is widely used. TPU is currently mainly synthesized by reacting diisocyanate with low molecular weight polyester or polyether diol, small molecule diol, and diamine chain extender. However, isocyanate is poisonous, and its preparation raw material is highly toxic pho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/78C08G18/42C08G18/10
CPCC08G18/10C08G18/4238C08G18/7843C08G2230/00C08G18/42
Inventor 赵京波李越张军营杨万泰
Owner BEIJING UNIV OF CHEM TECH
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