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Method for preparing aliphatic polyoxalate

A polyoxalate and aliphatic technology, which is applied in the field of preparation of high molecular weight polyoxalate, can solve the problems of high cost, difficulty in improving the molecular weight, etc., and achieve the effects of increasing yield, reducing dependence, and facilitating programming

Active Publication Date: 2012-10-10
南通药享科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In order to solve the defects of the prior art, such as the decomposition phenomenon of polyoxalate in the synthesis process, difficulty in increasing the molecular weight, and high cost of the process, the present invention focuses on solving the decomposition problem in the preparation process of polyoxalate, through low-temperature melt polymerization, and high vacuum solid state polycondensation to obtain high molecular weight polyoxalate

Method used

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  • Method for preparing aliphatic polyoxalate
  • Method for preparing aliphatic polyoxalate
  • Method for preparing aliphatic polyoxalate

Examples

Experimental program
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Effect test

Embodiment 1

[0059] Take 200g of dimethyl oxalate, 136g of ethylene glycol, add 0.03% stannous chloride, 0.2‰ stabilizer polyphosphoric acid, mix well, and add to a 1L multifunctional polyester reactor. Heat the reaction, keep the internal temperature at 150°C, strengthen it at 400kPa, react for 3 hours, and fractionally distill methanol to reach about 95% of the theoretical amount. Start vacuuming, keep at 150°C with an absolute pressure of 40kPa for 1h, at 160°C with an absolute pressure of 15kPa for 1h, and at a temperature of 180°C with an absolute pressure of 100Pa for 3 hours. The material was discharged and vacuum-dried for 12 hours, the yield was 83.45%, and the product was a white solid. Take the above dry product, put it into a 250ml round bottom flask, and react for 40h at 125°C with an absolute pressure below 100Pa. The final product was obtained with a yield of 99.77%.

[0060] The infrared spectrogram of the polyethylene oxalate prepared in the present embodiment one. Depe...

Embodiment 2

[0068] Take 200g of dimethyl oxalate and 136g of ethylene glycol, add 0.03% antimony trioxide and 0.2‰ stabilizer polyphosphoric acid, mix well, and add to a 1L multifunctional polyester reactor. Heat the reaction, keep the internal temperature at 180°C, and the pressure at 600kPa, react for 2 hours, and fractionally distill methanol to reach about 95% of the theoretical amount. Start vacuuming, keep at 150°C with an absolute pressure of 40kPa for 1h, at 160°C with an absolute pressure of 15kPa for 1h, and at a temperature of 180°C with an absolute pressure of 100Pa for 3 hours. The material was discharged and vacuum-dried for 12 hours, the yield was 66.32%, and the product was a white solid. Take the above dry product, put it into a 250ml round bottom flask, and react for 55h at 100°C with an absolute pressure below 100Pa. The final product was obtained with a yield of 99.32%.

Embodiment 3

[0070] Take 200g of dimethyl oxalate, 136g of ethylene glycol, add 0.25% zinc acetate, 0.2‰ stabilizer polyphosphoric acid, mix well, and add to a 1L multifunctional polyester reactor. Heat the reaction, keep the internal temperature at 120°C, and the pressure at 200kPa, react for 6 hours, fractionally distill methanol to reach about 95% of the theoretical amount. Start vacuuming, keep at 150°C with a vacuum degree of 40kPa for 1h, at 160°C with an absolute pressure of 20kPa for 1h, and at a temperature of 180°C with an absolute pressure of 100Pa for 3 hours. The material was discharged and vacuum-dried for 12 hours, and the yield was 78.63%. Take the above dry product, put it into a 250ml round bottom flask, and react for 50h at 125°C with an absolute pressure below 100Pa. Just get the final product, the yield is 99.87%, and the product is a white solid.

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Abstract

The invention relates to a method for preparing aliphatic polyoxalate. The method includes the following steps of A, placing R1OOCCOOR2, dihydric alcohol, a catalytic agent and a stabilizing agent in a reaction device, under the nitrogen protection, increasing the temperature to 120 DEG C to 180 DEG C until reactants are completely melted, stirring the reactants at a constant temperature and maintaining an absolute pressure of the reaction at 200kPa to 600kPa to react for 2 to 6 hours; B, vacuumizing, maintaining an internal temperature at 150 DEG C to 155 DEG C and the absolute pressure at 30kPa to 40kPa for 1 to 2 hours, maintaining for 1 to 2 hours at the internal temperature of 160 DEG C to 165 DEG C and the absolute pressure of 5kPa to 15kPa, maintaining for 1 to 4 hours at the internal temperature of 180 DEG C to 200 DEG C and the absolute pressure below 100 Pa, discharging materials and performing vacuum drying; and C, smashing solids, and performing a solid phase polycondensation at the temperature of 100 DEG C to 125 DEG C and the absolute pressure below 100 Pa for 30 to 55 hours. According to the method for preparing the aliphatic polyoxalate, the decomposition problem of oxalate or oxalic ester is solved, and the molecular weight and viscosity of the obtained polyoxalate are high.

Description

technical field [0001] The invention relates to a preparation method of high molecular weight polyoxalate, which belongs to the technical field of polymer materials. Background technique [0002] Traditional polyesters generally come from non-renewable petroleum resources and are difficult to degrade, causing white pollution. Therefore, the development of non-petroleum-based renewable and degradable plastics to replace traditional plastics is of great significance to the sustainable development of resources and the environment and environmental protection. [0003] Aliphatic polyester has good biodegradability, and generally degrades into carbon dioxide and water in the environment, so it is a hot spot in the research of modern polyester plastics. The main problems of current aliphatic biodegradable materials are mechanical properties and cost issues. Common degradable polyesters include polylactic acid (PLA), polyglycolic acid (PGA), polyhydroxyalkanoate (PHA), poly(ε-cap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/16C08G63/78
Inventor 崔爱军田俊凯蒋卫华李静陈群何明阳
Owner 南通药享科技有限公司
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