Preparation method of degradable PET-based copolyester

A technology of copolyester and glycolic acid copolyester, which is applied in the field of preparation of degradable PET-based copolyester, can solve the problems of slow degradation rate of copolyester, poor thermal stability, complicated preparation process, etc., and achieve simple and easy operation line, improve thermal stability, good thermal stability effect

Active Publication Date: 2022-04-08
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned polymerization process uses a two-step method to prepare PET-based copolyesters. The preparation process is complicated, which is not conducive to industrial scale-up production, and the degradation rate of copolyesters is slow, and the thermal stability is poor, so the scope of application is limited.

Method used

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  • Preparation method of degradable PET-based copolyester
  • Preparation method of degradable PET-based copolyester
  • Preparation method of degradable PET-based copolyester

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preparation example Construction

[0029] Introduce rapidly degradable PGA in PET molecular chain, obtain terephthalic acid-ethylene glycol-glycolic acid copolyester P (ET-co-GA), its preparation method comprises the steps:

[0030] 1. One-step melt polycondensation

[0031]Add dimethyl terephthalate, ethylene glycol, glycolic acid, catalyst and stabilizer to the reactor, wherein the molar ratio of ethylene glycol to dimethyl terephthalate is 1-2, glycolic acid and terephthalic acid The molar ratio of dimethyl diformate is 0-0.5; raise the temperature twice under an inert atmosphere, first raise the temperature to 150-190°C, pressurize to 0-0.02MPa, react for 1-3h, then raise the temperature to 200-230°C, React for 1 to 5 hours, carry out the transesterification / esterification reaction, the heating time of the transesterification can be determined according to the discharged small molecules; after the discharge of water or methanol exceeds 80% of the theoretical value, the temperature is raised twice under vacu...

Embodiment 1

[0043] One-step melt polycondensation to obtain P(ET-co-GA-5), x / 1-x=5mol%.

[0044] 500g dimethyl terephthalate, 223.9g ethylene glycol, 9.8g glycolic acid, antimony trioxide of 0.04% of total monomer mass, anhydrous zinc acetate of 0.0175% of total monomer mass and 0.07% of total monomer mass Add tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]pentaerythritol ester into a 2.5L stainless steel polycondensation reactor (Yangzhou Pulit Co., Ltd.), fully replace the reactor with nitrogen In the air, heat the reactor to 160°C, pressurize to 0.01MPa, react for 1h, heat up to 210°C and continue the reaction until the methanol discharge is 40% of the theoretical value, continue to heat up to 230°C, and react for 3h; until methanol After the discharge volume is 80% of the theoretical value, first raise the temperature to 250°C under vacuum, reduce the pressure to 0.066MPa, react for 0.5h, then raise the temperature to 260°C, reduce the pressure to 40Pa, react for 1h, carry o...

Embodiment 2

[0046] One-step melt polycondensation to obtain P(ET-co-GA-10), x / 1-x=10mol%.

[0047] 500g dimethyl terephthalate, 223.9g ethylene glycol, 19.6g glycolic acid, antimony trioxide of 0.04% of total monomer mass, anhydrous zinc acetate of 0.0175% of total monomer mass and 0.07% of total monomer mass Add tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]pentaerythritol ester into a 2.5L stainless steel polycondensation reactor (Yangzhou Pulit Co., Ltd.), fully replace the reactor with nitrogen In the air, heat the reactor to 160°C, pressurize to 0.01MPa, react for 1h, heat up to 210°C and continue the reaction until the methanol discharge is 40% of the theoretical value, continue to heat up to 230°C, and react for 3h; until methanol After the discharge volume is 80% of the theoretical value, first raise the temperature to 250°C under vacuum, reduce the pressure to 0.066MPa, react for 0.5h, then raise the temperature to 260°C, reduce the pressure to 40Pa, react for 1h, carr...

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Abstract

The invention relates to the technical field of polyester preparation, and discloses a preparation method of degradable PET-based copolyester, the degradable PET-based copolyester is terephthalic acid-ethylene glycol-glycollic acid copolyester, and the preparation method comprises the following steps: adding dimethyl terephthalate, ethylene glycol, glycollic acid, a catalyst and a stabilizer into a reactor; heating is performed twice in an inert atmosphere, the temperature is firstly increased to 150-190 DEG C, then the temperature is increased to 200-230 DEG C, and transesterification / esterification reaction is performed; and discharging water or methanol, heating twice in vacuum, firstly heating to 230-250 DEG C, then heating to 250-265 DEG C, and carrying out melt polycondensation reaction to obtain the terephthalic acid-ethylene glycol-glycolic acid copolyester. The heat stability and the intrinsic viscosity are improved by introducing the rapidly degradable PGA and adopting one-step melt polycondensation, and the intrinsic viscosity can be greater than 1.20 dL / g by further combining a solid phase polycondensation process.

Description

technical field [0001] The invention relates to the technical field of polyester preparation, in particular to a preparation method of degradable PET-based copolyester. Background technique [0002] Polyethylene terephthalate (PET) has good mechanical properties, thermal properties and permeability, and has been widely used in the fields of fibers, films, polyester bottles, etc. It is one of the most widely used traditional petroleum-based polymers one. Because PET materials are chemically inert and not easily degraded, it takes decades for their hydrolytic degradation, so they will exist in the natural environment for a long time, bringing serious pollution problems to the ecological environment. Although infrastructure exists around the world to collect and sort PET products, typically only 20% to 30% of PET is recycled, mainly through physical methods, resulting in poor performance recycled products that end up in landfills or be burned. Therefore, realizing the degrad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/60C08G63/78C08G63/80
CPCY02W90/10
Inventor 潘鹏举项望凯郑映刘园园
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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