Preparation method for 1, 6-hexanediol modified polyester for hot shrink films

A heat-shrinkable film and hexylene glycol technology, applied in the field of polyethylene terephthalate 1, can solve the problem of reducing the transparency of the copolymer

Active Publication Date: 2014-04-02
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Titanium catalysts often produce copolymers with a yellow color, and antimony and cobalt catalysts are often reduced to metals, so that the copolymers often have a gray appearance and greatly reduce transparency. Only proper selection of catalysts can obtain copolymers with good properties. However, due to The synergistic effect of some combination of catalysts, the choice is not obvious

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 996 grams of purified terephthalic acid (PTA), 99 grams of 1,6-hexanediol (HD), and 421ml of ethylene glycol in a 5L stainless steel reaction kettle equipped with nitrogen inlet, condensate outlet, stirrer and temperature indicator (EG) and 200ppm zinc acetate, 100ppm cobalt acetate, and 100ppm germanium acetate compound catalyst, then pressurize to 0.25MPa-0.3MPa with nitrogen, keep constant pressure, and the temperature in the reaction kettle rises to 240°C. When the amount of by-product water distilled out reaches the theoretical water output, the pressure in the kettle returns to normal pressure, and then 300ppm tetrabutyl titanate is added to the kettle, and the pressure in the polymerization kettle is reduced to within 20-30 minutes by vacuuming. 50-100Pa, react under this pressure for 60 minutes, the reaction is controlled at 275-285 ° C, and then the reaction system is returned to normal pressure with nitrogen, and the polymer melt is cast into pellets to obt...

Embodiment 2

[0030] Add 996 grams of purified terephthalic acid (PTA), 199 grams of 1,6-hexanediol (HD), 387ml of ethylene glycol and 100ppm germanium oxide, 100ppm cobalt acetate, 100ppm zinc acetate compound catalyst, then pressurize to 0.25MPa-0.3MPa with nitrogen, keep constant pressure, the temperature inside the reactor rises to 240°C, and the by-product water is distilled out of the reactor When the amount reaches the theoretical water output, the pressure in the kettle returns to normal pressure, and then 300ppm tetrabutyl titanate is added to the kettle, and the pressure in the polymerization kettle is reduced to 50-100Pa within 20-30 minutes by vacuuming. React under pressure for 60 minutes, the reaction is controlled at 275-285 ° C, and then the reaction system is returned to normal pressure with nitrogen, and the polymer melt is cast into pellets to obtain a colorless and transparent product. Its intrinsic viscosity is 0.55-0.75dL / g, and its melting point is 160°C-230°C.

Embodiment 3

[0032] Add 996 grams of purified terephthalic acid (PTA), 199 grams of 1,6-hexanediol (HD), and 374ml of ethylene glycol in a 5L stainless steel reaction kettle equipped with nitrogen inlet, condensate outlet, stirrer and temperature indicator. Alcohol and 100ppm of cobalt nitrate, 100ppm of germanium oxide, 200ppm of zinc acetate compound catalyst, then pressurize with nitrogen to 0.25MPa-0.3MPa, keep constant pressure, the temperature in the reactor rises to 240°C, and wait for the reactor to distill When the amount of by-product water reaches the theoretical water output, the pressure in the kettle returns to normal pressure, then add 400ppm tetrabutyl titanate into the kettle, and vacuumize the pressure in the polymerization kettle to drop to 50-100Pa within 20-30 minutes , react under this pressure for 60 minutes, the reaction is controlled at 275-285 ° C, and then the reaction system is returned to normal pressure with nitrogen, and the polymer melt is cast into pellets t...

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PUM

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Abstract

The invention relates to a preparation method for 1, 6-hexanediol modified polyester for hot shrink films. 1, 6-hexanediol, pure terephthalic acid and hexanediol are synthesized into polyethylene terephthalate 1, 6-hexanediol copolyester under catalysis of a compound catalyst by esterification and polycondensation reaction; the molar ratio of the hexanediol and the 1, 6-hexanediol is 40:60-90:10; the mole number ratio of the sum of the mole numbers of the pure terephthalic acid, the hexanediol and the 1, 6-hexanediol is 1:1.0-1.8; the catalyst is a composite catalyst of titanium compound, antimony compound, cobalt compound and germanium compound; and the melting point of the copolymer is 160-230 DEG C, the intrinsic viscosity is 0.55-0.75 d L / g, and the breaking elongation is larger than 100 %. The 1, 6-hexanediol modified polyester overcomes the defects of poor color and adhesion easiness, bending performance and tensile performance are improved, the melting point is reduced, post-processing performance is improved, and the 1, 6-hexanediol modified polyester can be used to process hot shrink films.

Description

technical field [0001] The invention relates to the preparation of polyethylene terephthalate by direct esterification and co-condensation reaction of purified terephthalic acid (PTA), ethylene glycol (EG) and 1,6-hexanediol under the catalysis of a compound catalyst 1,6-hexanediol ester method. Background technique [0002] Ordinary polyester (PET) and various modified ordinary polyesters have been widely used in various fields of people's daily life as engineering materials, and they can be made into fibers, beverage bottles, films and other materials. These polymers are prepared through two processes: esterification or transesterification of terephthalic acid or its esterified products with aliphatic dihydric alcohols. Usually the esterification process occurs under high pressure conditions, and the transesterification process occurs in normal conditions. Under pressure; vacuum polycondensation of esterification or transesterification products. Since the direct esterifi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08G63/85C08G63/83C08G63/82C08L67/02
Inventor 史君夏秀丽陈颖张培华张野马城华于春江吴传祥刘元胜杨旭
Owner PETROCHINA CO LTD
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