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Method for preparing poly(2-methyl butylene succinate) with high molecular weight (HMW)

A technology of butylene methyl succinate and methyl succinic acid is applied in the field of preparation of high-molecular-weight polybutylene 2-methyl succinate, which can solve the problems such as the inability to reduce the environmental load, and achieves the The effect of excellent physical and mechanical properties and biodegradability

Inactive Publication Date: 2013-09-25
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For the situation that the high molecular weight aliphatic polyester produced in the prior art still cannot reduce the environmental load, the purpose of the present invention is to provide a kind of preparation method of high molecular weight polybutylene 2-methylsuccinate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1,4-butanediol and 2-methylsuccinic acid are placed in a 250ml flask with a molar ratio of 1:1, and the catalyst tetrabutyl titanate is added in an amount equal to the molar amount of 2-methylsuccinic acid 10% of. Connect the water separator, thermometer and stirrer, raise the temperature to 110°C under the protection of nitrogen and stir vigorously. When no more water is generated in the water separator, the esterification reaction ends. Then the temperature was raised to 180° C., and the pressure was reduced to 30 Pa to carry out the polycondensation reaction, and the reaction time was 3 hours. After cooling, add the chain extender malonic anhydride to the reaction device, the amount of which is 10% of the molar amount of 2-methylsuccinic acid, and react at 150°C and 50Pa for 5 hours to obtain poly-2-methyl Butylene glycol succinate.

[0018] Adopt gel chromatography to detect the molecular weight of gained polybutylene 2-methylsuccinate, its weight-average molecula...

Embodiment 2

[0020] 1,4-butanediol and 2-methylsuccinic acid are placed in a 250ml flask with a molar ratio of 3:1, and the catalyst p-toluenesulfonic acid is added in an amount of 2-methylsuccinic acid molar weight 10%. Connect the water separator, thermometer and stirrer, raise the temperature to 170°C under the protection of nitrogen and stir vigorously. When no more water is generated in the water separator, the esterification reaction ends. Then the temperature was raised to 180° C., and the pressure was reduced to 30 Pa to carry out the polycondensation reaction, and the reaction time was 3 hours. After cooling, add chain extender phthalic anhydride to the reaction device, the amount added is 10% of the molar amount of 2-methylsuccinic acid, and react at 150°C and 50Pa for 5 hours to obtain poly-2- Butylene Methyl Succinate.

[0021] Adopt gel chromatography to detect the molecular weight of gained polybutylene 2-methylsuccinate, its weight-average molecular weight M w 15.6×10 4 ...

Embodiment 3

[0023] 1,4-butanediol and 2-methylsuccinic acid are placed in a 250ml flask with a molar ratio of 2:1, and the catalyst tetrabutyl titanate is added in an amount equal to the molar amount of 2-methylsuccinic acid 10% of. Connect the water separator, thermometer and stirrer, raise the temperature to 150°C under the protection of nitrogen and stir vigorously. When no more water is generated in the water separator, the esterification reaction ends. Then the temperature was raised to 230° C., and the pressure was reduced to 30 Pa to carry out the polycondensation reaction, and the reaction time was 3 hours. After cooling, add chain extender succinic anhydride to the reaction device, the amount added is 10% of the molar amount of 2-methylsuccinic acid, and react at 150°C and 50Pa for 5 hours to obtain poly-2-methyl Butylene glycol succinate.

[0024] Adopt gel chromatography to detect the molecular weight of gained polybutylene 2-methylsuccinate, its weight-average molecular weig...

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Abstract

The invention provides a method for preparing poly(2-methyl butylene succinate) with high molecular weight (HMW). The method comprises the following steps: heating 2-methyl succinic acid, butanediol and a catalyst to 110-170 DEG C in the presence of nitrogen to carry out esterification under normal pressure so as to obtain a polyester prepolymer; reducing the pressure of the polyester prepolymer and raising the temperature to 180-230 DEG C to carry out polycondensation so as to obtain poly(2-methyl butylene succinate); and finally adding a chain extender to carry out chain extension to obtain the poly(2-methyl butylene succinate) with HMW. The method has the following advantages and positive effects: in the presence of methyl, the regularity of the main polymer chain is reduced and the symmetry of the chain is destroyed, thus changing the crystallization property of the polymer and then adjusting the biodegradability of the polymer; and the obtained 2-methyl polyester succinate is expected to have good biodegradability, thus really realizing biological recycling of limited resources.

Description

technical field [0001] The invention belongs to the field of polymer materials, and relates to a method for preparing polyester by polycondensation, in particular to a method for preparing high molecular weight polybutylene 2-methylsuccinate. Background technique [0002] With the increasing application fields of polymer materials and the concern of human beings on environmental issues, the problem of "white pollution" caused by refractory polymer materials to the environment needs to be solved. Replacing the currently widely used non-degradable plastics with biodegradable polymer materials is an effective way to solve the problem of "white pollution". [0003] Biodegradable polymer materials have attracted widespread attention because they can be decomposed by microorganisms in the natural environment and then returned to nature. Among the currently researched biodegradable polymers, aliphatic polyesters have been deeply studied in the fields of biomedicine, pharmaceutical...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/16C08G63/181C08G63/685C08G63/78
Inventor 高传慧王传兴谢清伟武玉民许军
Owner QINGDAO UNIV OF SCI & TECH
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