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A kind of preparation method of polyterephthalic acid isophthalic acid adipate/butylene glycol copolyester

A technology of polyterephthalic acid isophthalic acid and butanediol copolyester, which is applied in the field of preparation of biodegradable polymers, can solve the problems of low light transmittance, inability to meet the needs of use, poor whiteness, etc., and achieve High whiteness, excellent mechanical properties, and high intrinsic viscosity

Active Publication Date: 2016-12-07
KINGFA SCI & TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the light transmittance of this product is low and the whiteness is poor, which still cannot meet its use requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 24.8kg of terephthalic acid, 2.48kg of isophthalic acid, 19.4kg of adipic acid and 40kg of 1,4-butanediol into the reaction kettle, and perform esterification reaction at 160-240°C under an inert gas atmosphere. , when the temperature rises to 230°C, add 30g of tetrabutyl titanate (equivalent to 0.5‰ in the total weight of the product) to remove by-product water and generate adipate / butylene terephthalate isophthalate , when the total esterification rate reaches more than 95%, the esterification reaction ends; continue to add the compound of 24g phosphorous acid and triphenyl phosphate, and the weight ratio of the two is 2:1, (equivalent to the total weight of the product 0.4‰); then depressurize the reactor continuously to a high vacuum of 10-200Pa within 100 minutes. During this process, the by-product 1,4-butanediol is continuously distilled out. The vacuum polycondensation time is 1.5h, and then the reactor is returned to normal pressure with an inert gas to obt...

Embodiment 2

[0029] Add 24.8kg of terephthalic acid, 1.24kg of isophthalic acid, 19.4kg of adipic acid and 40kg of 1,4-butanediol into the reaction kettle, and perform esterification reaction at a temperature of 160-240°C under an inert gas atmosphere. , when the temperature rises to 230°C, add 30g of tetrapropyl titanate (equivalent to 0.05% of the total weight of the product) to remove by-product water and generate adipate / butylene terephthalate isophthalate , when the total esterification rate reaches more than 95%, the esterification reaction ends; continue to add 30g of tetrapropyl titanate (equivalent to 0.05% in the total product weight) and 30g of phosphorous acid and trimethyl phosphate compound, The weight ratio between the two is 1:2, (equivalent to 0.05% of the total weight of the product); then the reactor is continuously decompressed to a high vacuum of 10-200Pa within 100 minutes, and the by-product 1 is continuously distilled during this process. , 4-butanediol, the final r...

Embodiment 3

[0031] Add 24.8kg of terephthalic acid, 0.496kg of isophthalic acid, 19.4kg of adipic acid and 40kg of 1,4-butanediol into the reaction kettle, and perform esterification reaction at a temperature of 160-240°C under an inert gas atmosphere. , when the temperature rises to 230°C, add 54g of tetraisopropyl titanate (equivalent to 0.9‰ in the total weight of the product) to remove by-product water and generate terephthalic acid isophthalic acid adipate / butanediol ester, when the total esterification rate reaches more than 95%, the esterification reaction ends; continue to add the compound of 48g phosphoric acid and diethyl phosphite, and the weight ratio of the two is 1:1, (equivalent to the total product 0.8‰ of the weight); then the reactor was continuously decompressed to a high vacuum of 10-200Pa within 100 minutes. During this process, the by-product 1,4-butanediol was continuously distilled out. The high vacuum polycondensation time is 2 hours, and then the reactor is retur...

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Abstract

The invention discloses a preparation method of poly-terephthalic acid isophthalic acid adipic acid / butanediol copolyester, comprising the following steps: performing esterification reaction on terephthalic acid, isophthalic acid, adipic acid and 1,4-butanediol at the temperature of 160-240 DEG C, performing polycondensation in a high vacuum of 10-200Pa to obtain a polymer, wherein the molar ratio of terephthalic acid to adipic acid is 1:1 to 2:1, the molar ratio of terephthalic acid to isophthalic acid is 1:0.005 to 1:0.15, the molar ratio of the sum of mole numbers of terephthalic acid, isophthalic acid and adipic acid to 1,4-butanediol is 1:(1.2-2.5); and the added amount of a titanium compound is on the basis that the titanium compound accounts for 0.05%-0.3% of the total weight of the product, and the added amount of a phosphorus compound is on the basis that the phosphorus compound accounts for 0.01%-0.5% of the total weight of the product. The copolyester obtained according to the invention has the advantages of high transparency, intrinsic viscosity and whiteness, excellent mechanical property, good stability and the like, and can be applied to membrane materials, packaging materials and the like.

Description

technical field [0001] The invention relates to a preparation method of a biodegradable polymer, in particular to a preparation method of polyterephthalic acid isophthalic acid adipate / butylene glycol copolyester. Background technique [0002] Biodegradable copolyesters are a class of aliphatic copolyesters or aliphatic / aromatic copolyesters that are fully biodegradable. Mainly including polybutylene succinate (PBS), poly(butylene adipate co-butylene terephthalate) (PBAT), and poly(butylene succinate co-p-hexyl Butylene Glycol Dioxide) (PBSA). It is used as a packaging material in engineering, and is involved in daily necessities, medical and agricultural applications. Compared with other degradable materials, it has lower cost and stable mechanical properties. However, when this kind of material is used as a film material, there are defects such as low light transmittance, low whiteness, and poor mechanical properties, which seriously affect the performance. [0003] CN2...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08G63/85
Inventor 唐美军苑仁旭徐依斌蔡彤旻曾祥斌
Owner KINGFA SCI & TECH CO LTD