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Two-step feeding synthesis method of high-performance polyetherester elastomer

A polyether ester elastomer, high-performance technology, applied in the field of two-step feeding synthesis method of high-performance polyether ester elastomer, can solve the problems of limited improvement of material mechanical properties, reduce production costs, and make the synthesis process easy to operate , Reduce the effect of thermal degradation side reactions

Active Publication Date: 2016-06-08
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005]The existing preparation processes of these polyether ester elastomers have failed to fully realize the effective control of the molecular structure of polyether ester elastomers, which is very important for the improvement of the mechanical properties of materials. limited

Method used

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  • Two-step feeding synthesis method of high-performance polyetherester elastomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Example 1 Add 194.0g of terephthalic acid, 158.0g of butanediol and 0.097g of tetrabutyl titanate into a 1L reactor, react at 220°C for 4h under the protection of nitrogen, then raise the temperature to 240°C, and react for 1h under a vacuum of less than 60Pa . The temperature of the system was lowered to 180°C, nitrogen protection was introduced, and 367.0 g of polytetrahydrofuran (the average number of repeating units in the soft segment was 12.0) with a molecular weight of 1,000 g / mol, 0.097 g of tetrabutyl titanate and antioxidant 1010 were added. 0.485g. The system was slowly heated up to 230°C under the protection of nitrogen, then reacted under 1,000Pa vacuum for 1h, then raised the system temperature to 250°C, and reacted under less than 60Pa vacuum for 6h to obtain a polyether ester elastomer product. The samples were dried under water cooling and cutting into pellets. GPC test results show product molecular weight M n The PDI is 29,000g / mol, and the PDI ...

Embodiment 2

[0052] Example 2 Add 271.0g of terephthalic acid, 135.0g of butanediol and 0.1355g of isopropyl titanate into a 1L reactor, react at 220°C for 4h under the protection of nitrogen, then raise the temperature to 240°C, and react for 1h under a vacuum of less than 60Pa . The temperature of the system was lowered to 180°C, nitrogen protection was introduced, and 131.0 g of polytetrahydrofuran with a molecular weight of 1,000 g / mol (the average number of repeating units in the soft segment was 12.0), 0.1355 g of isopropyl titanate and 1098 antioxidant were added as 0.678g. The system was slowly heated up to 230°C under the protection of nitrogen, then reacted under 1,000Pa vacuum for 1h, then raised the system temperature to 250°C, and reacted under less than 60Pa vacuum for 6h to obtain a polyether ester elastomer product. The samples were cooled under water and pelletized and then vacuum-dried. GPC test shows product molecular weight M n 27,000g / mol, PDI 2.0; DSC test resul...

Embodiment 3

[0053] Example 3 Add 176.0g of terephthalic acid, 135.0g of butanediol and 0.088g of isopropyl titanate into a 1L reaction kettle, react at 220°C for 4h under the protection of nitrogen, then raise the temperature to 240°C, and react for 1h under a vacuum of less than 60Pa . The temperature of the system was lowered to 180°C, nitrogen protection was introduced, 87.0 g of polytetrahydrofuran (the average number of repeating units in the soft segment was 22.7), 0.088 g of isopropyl titanate and antioxidant 1010 were added. 0.44g. The system was slowly heated up to 230°C under the protection of nitrogen, and then reacted under a vacuum of about 1,000Pa for 1h, then the temperature of the system was raised to 250°C, and reacted under a vacuum of less than 60Pa for 6h to obtain a polyetherester elastomer product. The samples were cooled under water and pelletized and dried in vacuum. GPC test shows product molecular weight M n It is 28,000g / mol, and the PDI is 1.5; DSC result...

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Abstract

The invention discloses a two-step feeding synthesis method of high-performance polyether ester elastomer, which comprises: mixing and reacting diacid, glycol and a catalyst to obtain a polyester hard segment, and combining the polyester hard segment with polyether The polyol, antioxidant and catalyst are reacted to obtain the high-performance polyether ester elastomer. The invention has the advantages of simple process, easy operation, good controllability, safety and environmental protection, and low cost. The side reaction of thermal degradation caused by long-term reaction at high temperature, thus obtaining a polyether ester elastomer with high molecular weight, controllable molecular weight of polyester hard segment and polyether soft segment, and excellent performance.

Description

technical field [0001] The invention relates to a synthesis method of a polyether ester elastomer, in particular to a two-step feeding synthesis method of a high-performance polyether ester elastomer. Background technique [0002] Polyetherester elastomer is a kind of material with both rubber elasticity and plastic thermoplasticity. At room temperature, the material shows excellent rubber elasticity; at high temperature, the material can be heated and melted, showing a processability similar to that of plastic. This excellent performance comes from the unique block structure in its molecular chain. Among them, the hard segment is a polyester segment with crystallinity and high melting point, and the soft segment is an amorphous polyether segment with a low glass transition temperature. The ratio of hard and soft segments in the material structure determines the hardness, physical mechanical properties and thermal properties of the material. Increasing the proportion of h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/672C08G63/78C08K5/134C08K5/526
Inventor 张俊午刘斐王静刚那海宁朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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