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Synthesizing method of high-molecular-weight poly(butylene adipate-co-terephthalate)

A technology of butylene phthalate and polyadipic acid, which is applied in the field of synthesis of high molecular weight polybutylene terephthalate adipate, can solve the problem of low molecular quality, poor product performance, and mixed materials. Non-uniformity and other problems, to achieve uniform molecular chain structure, high elongation at break, and meet the needs of blown film

Active Publication Date: 2016-01-13
BEIJING CHEM IND RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, through literature research and previous experimental results, we learned that the synthesis of PBAT based on the existing technology, on the one hand, the molecular weight can only reach about 4,500, and by changing the catalyst system, the highest molecular weight can only reach about 30,000, which needs to be obtained by melting polycondensation-solid phase The synthesis of high molecular weight PBAT can only be realized by the combination of viscosity increasing technology
It can be seen that the solid phase polycondensation in the post-modification stage requires high-temperature melting, which can easily lead to partial degradation, and the molecular weight of the product in the early synthesis stage is not easy to control, which has a greater impact on the later modification and affects product quality; post-modification adds fillers Or chain extender, easy to cause uneven mixing, complex operation, resulting in low overall molecular quality; Poor performance, can not meet the requirements of use

Method used

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  • Synthesizing method of high-molecular-weight poly(butylene adipate-co-terephthalate)
  • Synthesizing method of high-molecular-weight poly(butylene adipate-co-terephthalate)

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Esterification stage: 1314g of adipic acid (AA) and 1050g of 1,4-butanediol (BDO) are added respectively in 10 liters of polycondensation reactors, start to heat slowly, after stirring, add sorbitol of 8g as The chain extender of this reaction, continue to heat up and keep at 150-160 ℃ to carry out normal pressure esterification dehydration reaction, react for 1.5 hours, the water yield reaches 80% of the theoretical value, and its acid value is measured at the same time. 7.8mg / g, that is is the end point of the reaction;

[0021] Secondary esterification stage: add the terephthalic acid (PTA) of 1494g and the 1,4-butanediol (BDO) of 1400g after esterification finishes, stir for a while, add 11.25g titanium-magnesium composite catalyst, and slowly be warming up to The normal dehydration reaction was carried out at 210°C for 2 hours, and the total amount of distilled by-products in the two stages of the reaction reached the sum of the theoretical amount of water and meth...

Embodiment 2

[0024] Esterification stage: Add 1314g of adipic acid (AA) and 920g of 1,4-butanediol (BDO) into a 10-liter polycondensation reactor respectively, start to heat slowly, and add 18g of glycerol after stirring evenly As a chain extender for this reaction, continue to heat up and keep it at 150-160°C for normal pressure esterification dehydration reaction, react for 2 hours, the water output reaches 80% of the theoretical value, and its acid value is measured at the same time. 5.3mg / g, is the end point of the reaction;

[0025] Transesterification stage: add dimethyl terephthalate (DMT) of 1746g and 1,4-butanediol (BDO) of 1400g after the esterification reaction finishes, stir for a while, add 0.38g tetra-n-butyl titanate, and Slowly raise the temperature to 210°C for normal dehydration reaction for 2.25 hours, the total amount of distilled by-products in the two stages of reaction reaches the total amount of theoretical water and methanol, which is the reaction end point of this...

Embodiment 3

[0028] Esterification stage: 1314g of adipic acid (AA) and 920g of 1,4-butanediol (BDO) were added respectively in 10 liters of polycondensation reactor, began to slowly heat, after stirring evenly, 15g of pentaerythritol was added as this The reaction chain extender, continue to heat up and keep at 150-160 ℃ to carry out normal pressure esterification dehydration reaction, react for 2.2 hours, the water yield reaches 80% of the theoretical value, and its acid value is measured at the same time 2.6mg / g, which is end point of reaction;

[0029] Transesterification stage: add dimethyl terephthalate (DMT) of 1746g and 1,4-butanediol (BDO) of 1400g after the esterification reaction finishes, stir for a while, add 0.38g tetra-n-butyl titanate, and Slowly raise the temperature to 210°C for normal dehydration reaction for 2.5 hours, the total amount of distilled by-products in the two stages of reaction reaches the total amount of theoretical water and methanol, which is the end poin...

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Abstract

The invention relates to a synthesizing method of high-molecular-weight poly(butylene adipate-co-terephthalate). According to the invention, polyol is added as a chain extender, and the high-molecular-weight poly(butylene adipate-co-terephthalate) (PBAT) is directly synthesized with a melt condensation process. According to the invention, polyol is directly added in a synthesis stage, and high-molecular-weight PBAT can be synthesized. With the method, molecular weight controllable synthesis can be realized, the molecular weight is uniform, and molecular chain structure is uniform. Also, the added polyol is easy to obtain. The addition amount is low, and product performance is not influenced. Through the control over the process and the optimization of reaction auxiliary agents, the reaction time is greatly shortened. The synthesized product has good color, good mechanical performances, and high elongation at break, such that the requirements of film blowing can be satisfied.

Description

technical field [0001] The invention relates to the field of biodegradable plastics, in particular to a high-molecular-weight polyhexene diethylene glycol used for film-blown degradable plastic products such as fast food boxes, food and beverage packaging boxes, agricultural mulch films, supermarket shopping bags, cosmetic outer packaging, and medical supplies. Synthetic method of acid butylene terephthalate (PBAT). Background technique [0002] Aliphatic-aromatic copolyesters (CPEs) are biodegradable polyesters, which not only have the biodegradable properties of aliphatic polyesters, but also combine the excellent mechanical properties and physical properties of aromatic polyesters. It has been a hot topic of research since the 1980s. Biodegradable plastics are mainly used in packaging, fiber, agriculture, injection molding and other fields. Some environmentalists pointed out that my country consumes about 6 billion fast food boxes and 5 billion instant noodle bowls every...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/85
Inventor 钱志国尹继磊钱毅朱朗晖孙洁郭雪山竺朝山孙玉增马月博冯步学刘威王利新廖险峰王海强曹亮唐帅曹金波胡永宁杨传忠
Owner BEIJING CHEM IND RES INST
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