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Biodegradable aliphatic-aromatic block mixed polyester preparation method

A mixed polyester, biodegradable technology, applied in the field of preparation of biodegradable aliphatic-aromatic block mixed polyester, can solve the problems of aggravation, incomplete reaction, low reactivity of terephthalic acid, etc.

Inactive Publication Date: 2014-06-25
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wang Xiaohui et al. (Petrochemical Industry, 2010, 39(11), 1273) used terephthalic acid (PTA), 1,4-butanediol and adipic acid as raw materials to synthesize polyhexamethylene terephthalate by direct esterification. Diacid-butanediol copolyester, the process of this method is simple, but the polycondensation temperature is relatively high, about 270-275 ° C, and the high temperature side reaction will be intensified in the later stage of the polymerization reaction; at the same time, the reactivity of terephthalic acid is low, and the reaction incomplete

Method used

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  • Biodegradable aliphatic-aromatic block mixed polyester preparation method
  • Biodegradable aliphatic-aromatic block mixed polyester preparation method
  • Biodegradable aliphatic-aromatic block mixed polyester preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0035] 1) Preparation of aliphatic-aromatic block mixed polyester prepolymer: take by weight 20 parts of dimethyl terephthalate, 29.69 parts of 1,4-butanediol, 0.10 part of stannous chloride , 0.10 parts of phosphorous acid, 0.14 parts of tetrabutyl titanate, after reacting at 160°C for 4 hours, gradually raise the temperature to 200°C, when the amount of methanol evaporated reaches the theoretical value, gradually raise the temperature to 240°C to remove excess unreacted 1, 4-butanediol; then lower the temperature to 180°C, add 16.56 parts of adipic acid, continue the reaction for 4 hours, then gradually raise the temperature to 200°C; finally use a decompression device, first use a water pump to depressurize gradually for 3 hours, and then use an oil pump Reduce the pressure to 2mmHg and react for 2 hours to obtain a polyterephthalic acid-adipate-butylene glycol ester prepolymer with an intrinsic viscosity of 0.36dL / g, an acid value of 118.83mgKOH / g, and a hydroxyl value of 3...

Embodiment 2

[0038] 1) Preparation of PrePBAT prepolymer: Weigh 20 parts of dimethyl terephthalate, 29.69 parts of 1,4-butanediol, 0.10 part of stannous chloride, 0.10 part of phosphorous acid, 0.14 part of titanium in parts by weight After reacting at 160°C for 4 hours, gradually raise the temperature to 200°C. When the amount of methanol evaporated reaches the theoretical value, gradually raise the temperature to 240°C to remove excess unreacted 1,4-butanediol; then cool down to 180°C, add 13.55 parts of adipic acid, continue to react for 4 hours, then gradually raise the temperature to 200°C; finally use a water pump to gradually reduce the pressure for 3 hours, and then use an oil pump to reduce the pressure to 2mmHg and react for 2 hours to obtain an intrinsic viscosity of 0.35dL / g, a PrePBAT prepolymer with an acid value of 107.65 mgKOH / g and a hydroxyl value of 22.95 mgKOH / g.

[0039] 2) Weigh 6.15 parts of PrePBAT prepared in step 1), 1.07 parts of 1,4-phenyl-bis(2-oxazoline), 0.0...

Embodiment 3

[0041] 1) Preparation of PrePBAT prepolymer: Weigh 20 parts of dimethyl terephthalate, 29.69 parts of 1,4-butanediol, 0.10 part of stannous chloride, 0.10 part of phosphorous acid, 0.14 part of titanium in parts by weight Under the protection of a nitrogen atmosphere, react at 160°C for 4 hours, then gradually raise the temperature to 200°C, and when the amount of methanol evaporated reaches the theoretical value, gradually raise the temperature to 240°C to remove excess unreacted 1,4- Butanediol; then lower the temperature to 180°C, add 10.54 parts of adipic acid, continue the reaction for 4 hours, then gradually raise the temperature to 200°C; finally use a water pump to gradually reduce the pressure for 3 hours, and then use an oil pump to reduce the pressure to 2mmHg for 2 hours. A PrePBAT prepolymer having an intrinsic viscosity of 0.42 dL / g, an acid value of 71.35 mgKOH / g, and a hydroxyl value of 2.78 mgKOH / g was obtained.

[0042] 2) Weigh 5.44g parts of PrePBAT prepare...

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Abstract

The invention relates to a biodegradable aliphatic-aromatic block mixed polyester preparation method, and belongs to the technical field of mixed polyesters. The preparation method comprises that: dimethyl terephthalate and excess aliphatic diol are subjected to ester exchange to obtain a poly terephthalate diester oligomer having terminal hydroxyl, the poly terephthalate diester oligomer having the terminal hydroxyl reacts with an aliphatic dicarboxylic acid to obtain an aliphatic-aromatic block mixed polyester prepolymer, and chain extenders such as diacyl di-lactam and bisoxazoline are adopted to carry out chain extension to prepare the biodegradable aliphatic-aromatic block mixed polyester with the 30 DEG C intrinsic viscosity of 0.48-0.78 dL / g. According to the method, the polymerization temperature is moderate and is 180-240 DEG C so as to avoid side reaction intensifying at the later stage of the high temperature reaction, and the obtained polymer has characteristics of high melting point, excellent thermal stability and excellent mechanical property.

Description

technical field [0001] The invention relates to a preparation method of biodegradable aliphatic-aromatic block mixed polyester, which adopts dimethyl terephthalate (DMT) and aliphatic dihydric alcohol to react to synthesize polyterephthalate with terminal hydroxyl Ester oligomer, then react with dibasic acid to synthesize aliphatic-aromatic block mixed polyester prepolymer, and then extend the chain to prepare biodegradable aliphatic-aromatic with intrinsic viscosity of 0.48~0.78dL / g at room temperature 30°C The method for block mixed polyester belongs to the technical field of mixed polyester. technical background [0002] Aliphatic-aromatic copolyester is a kind of material with good performance. It not only has the flexibility and biodegradability of aliphatic polyester but also has the rigidity of aromatic polyester, and has excellent processing performance. Therefore, aliphatic-aromatic copolyesters have good application prospects. Ma Yiping et al. (Plastics, 2010, 39...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/685C08G63/183
Inventor 赵京波关浩杨万泰
Owner BEIJING UNIV OF CHEM TECH
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