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Preparation method of high molecular weight copolyester with high gas barrier

A gas barrier, high molecular weight technology, applied in the field of materials, can solve the problems of fast crystallization rate of PBT, slow PX construction, difficult to obtain transparent products, etc., to achieve the effect of improving transparency, excellent gas barrier performance, and high molecular weight

Inactive Publication Date: 2019-09-13
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the fusing point of PBT is at 225 ℃~235 ℃, and synthesis and processing temperature are all higher; The crystallization rate of PBT is very fast, and it is difficult to obtain transparent goods; PX), PX is heavily dependent on petrochemical resources. Affected by many factors, the pace of PX construction in my country is slow, and half of the consumption depends on imports

Method used

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  • Preparation method of high molecular weight copolyester with high gas barrier
  • Preparation method of high molecular weight copolyester with high gas barrier
  • Preparation method of high molecular weight copolyester with high gas barrier

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] Add dimethyl terephthalate, dimethyl 2,5-furandicarboxylate, 1,4-butanediol, and anhydrous cobalt acetate into the reaction kettle in a molar ratio of 0.85:0.15:1.6:0.0015, and vacuumize 1. Replace with nitrogen for three times, then gradually raise the temperature to 200°C, and react for 0.5h. Then add 2,5-dimethyl furandicarboxylate and dimethyl terephthalate with a total molar weight of 0.5% antimony acetate, 0.2% triphenyl phosphate, and 0.2% antioxidant 1010, and slowly evacuate to 200Pa ~2000Pa, heat up to 210°C for 1.0h pre-condensation. Then the temperature was raised to 235° C., the vacuum was lowered to below 100 Pa, and the reaction was carried out for 4.0 hours to obtain a high molecular weight and high gas barrier bio-based copolyester.

[0069] The intrinsic viscosity of the high molecular weight and high gas barrier bio-based copolyester obtained in this example is 1.20dL / g, the melting point is 204°C, there is no cold crystallization peak, the melting e...

Embodiment 2

[0071] Add dimethyl terephthalate, dimethyl 2,5-furandicarboxylate, 1,4-butanediol, and anhydrous cobalt acetate into the reaction kettle in a molar ratio of 0.70:0.30:1.8:0.001, and vacuumize 1. Replace with nitrogen for three times, then gradually raise the temperature to 180°C, and react for 3.0 hours. Then add 2,5-dimethyl furandicarboxylate and dimethyl terephthalate with a total molar weight of 0.3% antimony trioxide, 0.2% triphenyl phosphate, and 0.2% antioxidant 1010, and slowly vacuumize To 150Pa ~ 2000Pa, the temperature is raised to 195 ℃ for 1.0h pre-condensation. Then, the temperature was raised to 230° C., the vacuum was evacuated to below 40 Pa, and the reaction was carried out for 4.0 hours to obtain a high molecular weight and high gas barrier bio-based copolyester.

[0072] The intrinsic viscosity of the high molecular weight and high gas barrier bio-based copolyester obtained in this example is 1.05dL / g, the melting point is 179°C, the cold crystallization ...

Embodiment 3

[0074] Add dimethyl terephthalate, dimethyl 2,5-furandicarboxylate, 1,4-butanediol, and anhydrous manganese acetate into the reaction kettle in a molar ratio of 0.55:0.45:1.8:0.0012, and vacuumize 1. Replace with nitrogen for three times, then gradually raise the temperature to 190°C, and react for 2.5 hours. Then add 2,5-dimethyl furandicarboxylate and dimethyl terephthalate with a total molar mass of 0.25% antimony trioxide, 0.15% triphenyl phosphate, 0.15% antioxidant 1010, and slowly vacuumize To 100Pa ~ 2000Pa, the temperature is raised to 210 ℃ for 0.5h pre-condensation. Then the temperature was raised to 230° C., the vacuum was lowered to below 50 Pa, and the reaction was carried out for 3.0 hours to obtain a high molecular weight and high gas barrier bio-based copolyester.

[0075] The intrinsic viscosity of the high molecular weight and high gas barrier bio-based copolyester obtained in this example is 0.96dL / g, the melting point is 148°C, the cold crystallization en...

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Abstract

The invention discloses a preparation method of high molecular weight copolyester with high gas barrier, comprising the following steps: raw materials including ingredients (a), (b) and (c) are subjected to a reaction I in the presence of a catalyst I, and then a reaction II is carried out in the presence of a catalyst II to prepare the high molecular weight copolyester with high gas barrier. In the raw materials, (a) is a compound as shown in a formula I, (b) is a compound as shown in a formula II, and (c) is fatty alcohol with its chemical formula as shown in the specification, wherein n isan integer of 2-10. The reaction I comprises an esterification reaction and / or a transesterification reaction; the catalyst I comprises an esterification reaction catalyst and / or a transesterificationreaction catalyst; the reaction II comprises a condensation polymerization reaction; and the catalyst II comprises a condensation polymerization catalyst. In the formula I or the formula II, R1 and R2 are separately selected from H and C1-C8 alkyl.

Description

technical field [0001] The present application relates to the field of material technology, in particular, to a preparation method of high molecular weight and high gas barrier bio-based copolyester. Background technique [0002] Polybutylene terephthalate (PBT) is an important thermoplastic engineering plastic, which has the characteristics of high temperature resistance, humidity resistance, good electrical insulation performance, oil resistance, chemical corrosion resistance, fast molding, etc., and the price is moderate, so it can be widely used Used in electronic appliances, automobiles, industrial parts and other fields. But the fusing point of PBT is at 225 ℃~235 ℃, and synthesis and processing temperature are all higher; The crystallization rate of PBT is very fast, and it is difficult to obtain transparent goods; PX), PX is heavily dependent on petrochemical resources. Affected by many factors, the pace of PX construction in my country is slow, and half of the consu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/672C08G63/183C08G63/86
CPCC08G63/183C08G63/672C08G63/866
Inventor 王静刚刘小青张小琴慎昂朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI