1, 4; 3, 6-diglycidyl hexanehexol modified PET polyester and semi-continuous preparation method thereof

A modified technology of hexanehexanol, which is applied in the field of 1 and 4, and can solve the problems of low conversion rate, low catalyst dosage and low reactivity

Active Publication Date: 2021-05-28
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method utilizes the good solubility of esterified monomers to monomers and the synergistic effect between transesterification catalysts and polycondensation catalysts to overcome the problems of low reactivity, low conversion rate and high production cost of bio-based monomers. The dosage is extremely low, avoiding the complex catalyst separation process and the problem of metal residues in the polymer, and the semi-continuous method is more conducive to the realization of industrial production

Method used

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  • 1, 4; 3, 6-diglycidyl hexanehexol modified PET polyester and semi-continuous preparation method thereof
  • 1, 4; 3, 6-diglycidyl hexanehexol modified PET polyester and semi-continuous preparation method thereof
  • 1, 4; 3, 6-diglycidyl hexanehexol modified PET polyester and semi-continuous preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1 Semi-continuous method efficiently prepares high heat-resistant high-performance (terephthalic acid-isosorbide-ethylene glycol-1,4-cyclohexanedimethanol) copolyester

[0046] (1) Under the protection of nitrogen atmosphere, in the first esterification kettle, add 24.9kg (150mol) terephthalic acid, 18.6kg (300mol) ethylene glycol (the molar ratio of terephthalic acid and ethylene glycol is 1 : 2), pressurized to 300kPa, stirred and reacted at 240° C. for 3 hours, and distilled out the by-product water produced by the reaction. After the by-product water is all evaporated, the reaction is complete, and the esterified product of terephthalic acid and ethylene glycol is obtained; 2 / 3 of the esterified product is discharged into the second esterification kettle, and 16.6kg (100mol) of terephthalic acid and 12.4kg (200mol) ethylene glycol mixture is fed into the first esterification kettle at a speed of 10kg / min to continue the esterification reaction with the re...

Embodiment 2

[0051] Example 2 Semi-continuous method for efficiently preparing high heat-resistant high-performance (terephthalic acid-isosorbide-ethylene glycol-1,3-cyclohexanedimethanol) copolyester

[0052] (1) Under the protection of nitrogen atmosphere, in the first esterification kettle, add 24.9kg (150mol) terephthalic acid, 23.25kg (375mol) ethylene glycol (the mol ratio of terephthalic acid and ethylene glycol is 1 : 2.5), pressurized to 300kPa, stirred and reacted at 245°C for 4 hours, and distilled out the by-product water produced by the reaction. After the by-product water is all evaporated, the reaction is complete, and the esterified product of terephthalic acid and ethylene glycol is obtained; 2 / 3 of the esterified product is discharged into the second esterification kettle, and 16.6kg (100mol) of terephthalic acid and 15.5kg (250mol) of ethylene glycol mixture was fed into the first esterification kettle at a rate of 10kg / min to continue the esterification reaction with th...

Embodiment 3

[0056] Example 3 Semi-continuous method efficiently prepares high heat-resistant high-performance (terephthalic acid-isosorbide-ethylene glycol-1,4-cyclohexanediol) copolyester

[0057] (1) Under the protection of nitrogen atmosphere, in the first esterification kettle, add 24.9kg (150mol) terephthalic acid, 13.95kg (225mol) ethylene glycol (the molar ratio of terephthalic acid and ethylene glycol is 1 : 1.5), pressurized to 280kPa, stirred and reacted at 250°C for 3.5 hours, and distilled off the by-product water produced by the reaction. After the by-product water is all evaporated, the reaction is complete, and the esterified product of terephthalic acid and ethylene glycol is obtained; 2 / 3 of the esterified product is discharged into the second esterification kettle, and 16.6kg (100mol) of terephthalic acid and 9.3kg (150mol) of ethylene glycol mixture was fed into the first esterification kettle at a rate of 10kg / min to continue the esterification reaction with the remain...

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Abstract

The invention discloses a 1,4; 3, 6-diglycidyl hexanehexol modified PET polyester and a semi-continuous preparation method thereof, and monomers of the modified PET polyester comprise (a) terephthalic acid, (b) ethylene glycol, and (c) 1, 4; 3, 6-dihexanediol or mixtures thereof, and (d) aliphatic and / or alicyclic dihydric alcohol. The method comprises the following steps: preparing a certain amount of terephthalic acid glycol ester in a first esterification kettle, then continuously adding mixed terephthalic acid and glycol slurry into the first esterification kettle at a certain flow rate for reaction, and intermittently discharging reaction products into a second esterification kettle, and adding the modified monomer / ester exchange catalyst into the second esterification kettle for esterification / ester exchange reaction to obtain a prepolymer, discharging all the prepolymer into a polycondensation kettle, adding a polycondensation catalyst, and carrying out melt polycondensation to obtain a final polymer. The method provided by the invention overcomes the problems of low reaction activity, low conversion rate and high production cost of bio-based monomers, avoids the problem of metal residues, and is beneficial to realization of industrial production.

Description

technical field [0001] The invention belongs to the field of macromolecular materials, and in particular relates to a 1,4;3,6-dihydroxyhexylhexyl alcohol-modified PET polyester and a semi-continuous preparation method thereof, in particular to a semi-continuous method for preparing high-efficiency and high-conversion Performance 1,4; 3,6-Di-Hexyl-Hexyl Alcohol Modification of PET Copolyester. Background technique [0002] Polyethylene terephthalate (PET) has the advantages of good strength and toughness, non-toxic, weak acid and organic solvent resistance, so it is widely used in packaging materials, beverage bottles and textile and clothing products and other fields. However, the problems of overcapacity and low added value also limit the development of PET. Differentiation and functional modification have become a new direction for the development of PET. The heat resistance of PET is poor, and it will cause severe deformation and greatly reduce the performance when used ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/42C08G63/85C08G63/86C08G63/87
CPCC08G63/42C08G63/866C08G63/85C08G63/87
Inventor 刘佳健李春成孟现明张栋
Owner INST OF CHEM CHINESE ACAD OF SCI
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