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Production method of low acetaldehyde titanium system polyester

A technology of titanium-based polyester and a production method is applied in the production field of low-acetaldehyde titanium-based polyester, and can solve the problems of high residual acetaldehyde and slow solid-phase polymerization of polyester.

Active Publication Date: 2015-05-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is the problem that the solid-phase polymerization speed of polyester prepared by titanium-based catalyst is relatively slow and the residual amount of acetaldehyde is relatively high in the past, and a new production method of low-acetaldehyde titanium-based polyester is provided

Method used

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  • Production method of low acetaldehyde titanium system polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Preparation of Catalyst A

[0039] Add 12.4 grams (0.2 moles) of ethylene glycol into a reactor equipped with a stirrer, a condenser and a thermometer, slowly drop 28.4 grams (0.1 moles) of tetraisopropyl titanate into the reactor, and precipitate a white precipitate. After reacting at 70°C for 2 hours, the product was centrifuged, and the residue was washed with distilled water three times, and the product was vacuum-dried at 70°C to obtain a white powder.

[0040] Place the dried white powdery substance in a reactor with a stirrer, a condenser and a thermometer, add 50 grams of ethylene glycol, 32 grams of 25% aqueous sodium hydroxide solution (0.2 mol), 18 grams of lactic acid (0.2 moles), 28 grams (0.2 moles) of trimethyl phosphate, and 73.2 grams (0.4 moles) of zinc acetate were reacted for 2 hours at a reaction temperature of 150° C. to obtain a nearly colorless homogeneous liquid, which was Catalyst A.

[0041] Preparation of polyester

[0042] 600 grams of ter...

Embodiment 2

[0048] Preparation of polyester

[0049] 600 grams of terephthalic acid, 316 grams of ethylene glycol and catalyst A (based on the amount of polyester produced, the weight of titanium atoms is 2.5ppm), mixed to form a slurry, added to the polymerization tank for esterification , The esterification temperature is 230-255°C, the pressure is 0.25MPa, and the water generated by the reaction is discharged through the rectification device. Return to normal pressure after the esterification, add potassium acetate 6 × 10 -3 g (6×10 -5 mol), zinc acetate 1.6×10 -2 g (8×10 -5 mol), vacuumize and decompress until the system pressure is lower than 130Pa, and at the same time, the reaction temperature gradually rises to 280°C. When the system reaction reaches 150min, the reaction is stopped, and the reaction product is continuously extruded from the bottom of the polymerization kettle in a strip shape, cooled and cut. grain.

[0050] Solid State Polymerization of Polyester

[0051] P...

Embodiment 3

[0055] Preparation of Catalyst B

[0056] Add 12.4 grams (0.2 moles) of ethylene glycol into a reactor equipped with a stirrer, a condenser and a thermometer, slowly drop 28.4 grams (0.1 moles) of tetraisopropyl titanate into the reactor, and precipitate a white precipitate. After reacting at 70°C for 2 hours, the product was centrifuged, and the residue was washed with distilled water three times, and the product was vacuum-dried at 70°C to obtain a white powder.

[0057] Place the dried white powdery substance in a reactor with a stirrer, a condenser and a thermometer, add 50 grams of ethylene glycol, 32 grams of 25% aqueous sodium hydroxide solution (0.2 moles), citric acid monohydrate 63 g (0.3 mole), 28 g (0.2 mole) of trimethyl phosphate, and 42.6 g (0.3 mole) of magnesium acetate were reacted at a reaction temperature of 150° C. for 2 hours to obtain a nearly colorless homogeneous liquid, which was catalyst B.

[0058] Preparation of polyester

[0059] 600 grams of te...

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Abstract

The invention relates to a production method of a low acetaldehyde titanium system polyester, and mainly solves the problems of low speed of solid-phase polymerization and high acetaldehyde residual of the polyester produced by the titanium system catalyst in the prior art. According to the invention, titanium system catalyst is used for the preparation of polyester; after esterification reaction, alkali metal carboxylate salt compound G and at least a metal compound H selected from the group consisting of IIA, IB, IIB, VIIB and VIII in the elements periodic table are added; and then melt phase polycondensation products are subjected to a solid-phase polymerization under appropriate temperature and pressure conditions, so as to further obtain polyester with high molecular weight and viscosity. The technical scheme well solves the above problems, and can be used in the industrial production of polyester.

Description

technical field [0001] The invention relates to a production method of low-acetaldehyde titanium series polyester. Background technique [0002] Polyethylene terephthalate is an important industrial raw material. Due to its excellent chemical and physical properties, it is widely used in fibers, films, sheets, bottles and other materials. It has excellent mechanical strength, chemical stability, gas barrier properties, aroma retention, hygiene, etc., is cheap and light in weight, and is especially suitable for manufacturing beverage containers that require thermal sterilization and filling. The container can be manufactured by injection molding a bottomed tubular preform, reheating to soften it, and stretch blow molding. At this time, the blow mold is heated to heat-set the bottle, and the molecular chains are aligned by stretching, and the crystals are fixed to improve the gas barrier property of the bottle. [0003] At present, the polyester catalysts with more industria...

Claims

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Application Information

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IPC IPC(8): C08G63/86C08G63/85C08G63/83C08G63/82C08G63/80C08G63/183
Inventor 宋歌关震宇张俊章瑛虹周文乐
Owner CHINA PETROLEUM & CHEM CORP
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