Biodegradable copolyester and preparation method thereof

A biodegradable and copolyester technology is applied in the field of aliphatic/aromatic copolyester and its preparation, which can solve the problems of poor biodegradability of aromatic polyesters and the use of non-degradable materials, and achieves low esterification reaction temperature and high synthesis efficiency. The effect of shortening the reaction time and increasing the reaction speed

Active Publication Date: 2011-08-03
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, aromatic polyester has poor biodegradability and cannot be used alone as a degradable material

Method used

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  • Biodegradable copolyester and preparation method thereof
  • Biodegradable copolyester and preparation method thereof
  • Biodegradable copolyester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 820g of purified terephthalic acid (PTA), 180g of adipic acid (AA), 525g of 1,4-butanediol (1,4- BD) and 40g ethylene glycol (EG), 0.2g tetrabutyl titanate (equivalent to 200ppm of the total weight of PTA and AA), 0.6g antimony acetate (equivalent to 600ppm of the total weight of PTA and AA). Maintain normal pressure in the kettle and stir at a constant speed. When the temperature in the reaction kettle rises to 150°C, water will start to come out. Continue to raise the temperature and control the inner temperature of the reaction kettle to not exceed 220°C. When the amount of water is produced, the esterification reaction ends. Continue to add 0.05g trimethyl phosphate (50ppm equivalent to the total weight of PTA and AA) in the kettle, vacuumize, make the pressure in the polymerization kettle be reduced to below 150Pa in 60 minutes, react under this pressure for 85 minutes, react The final temperature is controlled at 280°C, and then the reaction system is returne...

Embodiment 2

[0025] In a 5L stainless steel reaction kettle equipped with nitrogen inlet, condensate outlet and stirrer, 630g of purified terephthalic acid (PTA), 370g of adipic acid (AA), 549g of 1,4-butanediol (1,4- BD) and 94g ethylene glycol (EG), 0.2g tetrapropyl titanate or tetraisopropyl titanate (equivalent to 200ppm of the total weight of PTA and AA) and 0.3g antimony trioxide (equivalent to the total weight of PTA and AA 300ppm by weight). Maintain normal pressure in the kettle and stir at a constant speed. When the temperature in the reaction kettle rises to 150°C, water will start to come out. Continue to raise the temperature and control the inner temperature of the reaction kettle to not exceed 220°C. When the amount of water is produced, the esterification reaction ends. Continue to add 0.3g tetrapropyl titanate (equivalent to 300ppm of the total weight of PTA and AA), 0.1g antimony trioxide (equivalent to 100ppm of the total weight of PTA and AA) and 0.15g triethyl phospha...

Embodiment 3

[0027]In a 5L stainless steel reaction kettle equipped with nitrogen inlet, condensate outlet and stirrer, add 333g of purified terephthalic acid (PTA), 468g of adipic acid (AA), 322g of 1,4-butanediol (1,4- BD) and 40 g of ethylene glycol (EG), 0.3 g of tetramethyl titanate (corresponding to 300 ppm of the total weight of PTA and AA) and 0.3 g of antimony ethylene glycol (corresponding to 300 ppm of the total weight of PTA and AA). Maintain normal pressure in the kettle and stir at a constant speed. When the temperature in the reaction kettle rises to 150°C, water will start to come out. Continue to raise the temperature and control the inner temperature of the reaction kettle to not exceed 220°C. When the amount of water is produced, the esterification reaction ends. Continue to add 0.5g tetramethyl titanate (equivalent to 500ppm of the total weight of PTA and AA) and 0.2g triphenyl phosphate or triphenyl phosphite (equivalent to 200ppm of the total weight of PTA and AA) in ...

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Abstract

The invention relates to biodegradable copolyester and a preparation method thereof. The preparation method comprises the following steps of: undergoing an esterification reaction on pure terephthalic acid, hexanedioic acid, 1,4-butylene glycol and ethylene glycol under normal pressure at the temperature of between 150 DEG C and 220 DEG C, wherein the molar ratio of the pure terephthalic acid to the hexanedioic acid is (3:7)-(8:2), the molar ratio of the ethylene glycol to the 1,4-butylene glycol is (1:9)-(9:1), and the ratio of the total mole number of the pure terephthalic acid and the hexanedioic acid to the total mole number of the ethylene glycol and the 1,4-butylene glycol is 1:(1.0-1.8); and undergoing condensation polymerization under the pressure of between 10 Pa and 150 Pa to obtain the copolyester, wherein the dosage of a titanium compound is 200-1,200 ppm relative to the total weight of terephthalic acid and the hexanedioic acid, the dosage of an antimony compound is 100-600 ppm relative to the total weight of the terephthalic acid and the hexanedioic acid, and the dosage of a phosphorous compound is 50-400 ppm relative to the total weight of the terephthalic acid and the hexanedioic acid. The biodegradable copolyester has the advantages of low raw material price, reaction at low temperature and under low pressure and high inherent viscosity.

Description

Technical field: [0001] The present invention relates to a kind of biodegradable aliphatic / aromatic copolyester and preparation method thereof, more specifically relate to aromatic dicarboxylic acid, aliphatic dicarboxylic acid and aliphatic dibasic alcohol direct esterification and Preparation of biodegradable aliphatic / aromatic copolyesters by copolycondensation and process for their preparation. Background technique: [0002] Aliphatic polyester is a fully biodegradable polymer that can be decomposed into carbon dioxide, water and mineralized inorganic salts of the elements it contains and new biomass under the action of microorganisms. At present, many varieties have entered mass production or industrial production. However, the high cost of the material and high product prices have become bottlenecks restricting the further development of aliphatic polyesters. Thermoplastic aromatic polyester has stable thermal properties, excellent mechanical properties, easy process...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/86C08G63/85C08G63/183
Inventor 史君王晓慧陈颖李连斌付志峰李振忠吴佩华胡亚文邹妍温国防刘智全刘冬李彦钧
Owner PETROCHINA CO LTD
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