Two-step feeding synthesis method of high-performance poly(ether ester) elastomer

A polyetherester elastomer and high-performance technology, which is applied in the field of two-step feeding synthesis method of high-performance polyetherester elastomer, can solve the problems of limited improvement of material mechanical properties, and achieve lower production costs and better controllability. , the effect of reducing requirements

Active Publication Date: 2015-02-25
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 poly(ether ester) elastomer

Examples

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Comparison scheme
Effect test

Embodiment 1

[0052] 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, 367.0 g of polytetrahydrofuran with a molecular weight of 1,000 g / mol was added (the average number of repeating units in the soft segment was 12.0), 0.097 g of tetrabutyl titanate and antioxidant 1010 were 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 i...

Embodiment 2

[0053] 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, then vacuum-dried. GPC test shows product molecular weight M n 27,000g / mol, PDI 2.0; DSC test results...

Embodiment 3

[0054] 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 a high-performance poly(ether ester) elastomer. The two-step feeding synthesis method comprises the following steps: mixing dicarboxylic acid, dihydric alcohol and a catalyst, and reacting, so as to obtain a polyester hard segment; enabling the polyester hard segment to react with polyether polyol, an antioxidant and a catalyst to obtain the high-performance poly(ether ester) elastomer. The two-step feeding synthesis method is simple in process, easy to operate, good in controllability, safe, environmentally friendly, and low in cost; the inhibiting effect on esterification reaction in polyester hard segment synthesis caused by the polyether polyol is avoided; the side reaction of thermal degradation caused by long-term reaction of the polyether polyol at relatively high temperature is reduced; and therefore, the poly(ether ester) elastomer with high molecular weight, controllable molecular weight of the polyester hard segment and the polyether soft segment and excellent performance is obtained.

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 Applications(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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