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High-activity catalyst and its application in synthesizing polyester

A catalyst and compound technology, applied in the field of high-activity titanium-based catalysts, can solve the problems of easy hydrolysis of titanate and low catalytic activity

Inactive Publication Date: 2004-09-01
济南齐鲁化纤集团有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] JP 2000-143789 uses easily hydrolyzed titanate and magnesium acetate as catalysts, which is more active than using titanate alone, but there is still the problem of easy hydrolysis of titanate, and the catalytic activity (calculated as Ti) is still low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 2.5-liter stainless steel reactor, add 996 grams of terephthalic acid, 465 grams of ethylene glycol and 0.04 grams of titanium glycol, wherein the titanium content in titanium glycol is 26.1%. At 2.0-3.0kg / cm 2 Carry out esterification under the pressure of G, and discharge the water generated by the reaction through the rectification device. When the temperature rises to 255-260°C, the reaction time is about 133min. When it drops to normal pressure, continue to heat up to 260°C. Distillate is discharged, vacuumize and depressurize to 20000Pa, and reduce the pressure to 300Pa within 60min, raise the temperature to 265-280℃, further reduce the pressure to below 50-60Pa, control the temperature within 275-300℃, when When the polymer viscosity reaches 0.68dl / g, the total polycondensation time is about 140min, and the synthesized polyester is slightly light yellow and transparent, and becomes colorless and transparent within 10 hours under sunlight.

Embodiment 2

[0028] In a 2.5-liter stainless steel reactor, add 996 grams of terephthalic acid, 465 grams of ethylene glycol at 2.0-3.0kg / cm 2 Carry out esterification under G pressure, and discharge the water generated by the reaction through a rectification device. When the temperature rises to 255-260°C, the reaction time is about 148min. Content is 26.1%) into 10g of ethylene glycol, after mechanical stirring or ultrasonic dispersion, add to the reaction kettle and wash with ethylene glycol, continue to heat up to 260 ° C, at this time no more distillate is discharged, vacuumize and depressurize to 20,000Pa, and reduce the pressure to 300Pa within 60min, increase the temperature to 265-280°C, further reduce the pressure to below 50-60Pa, and keep the temperature within 275-300°C. When the polymer viscosity reaches 0.68dl / g, the total The polycondensation time is about 134min, and the synthesized polyester is slightly light yellow and transparent, and becomes colorless and transparent w...

Embodiment 3

[0030] In a 2.5-liter stainless steel reactor, add 996 grams of terephthalic acid, 520 grams of ethylene glycol, 0.04 grams of titanium glycolate (titanium content is 26.1%) and 0.1 grams of crystalline sodium acetate, at 2.0-3.0kg / cm 2Carry out esterification under the pressure of G, and discharge the water generated by the reaction through the rectification device. When the temperature rises to 255-260°C, the reaction time is about 128min. When it drops to normal pressure, continue to heat up to 260°C. Distillate is discharged, vacuumize and depressurize to 20000Pa, and reduce the pressure to 300Pa within 60min, raise the temperature to 265-280℃, further reduce the pressure to below 50-60Pa, the temperature is within 275-300℃, when the polymerization When the viscosity of the product reaches 0.68dl / g, the total polycondensation time is about 137min, and the synthesized polyester is colorless and transparent.

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Abstract

A high-activity catalyst for both esterification and polycondensation contains anti-hydrolytic high-activity glycol titanium, the acetate, carbonate or oxalate of (1-4)-valence metal ions, and at least one of alkoxyl compound, organic acid and phosphorous compound. Its advantages are high activity, short reaction period, and no environmental pollution. Its resultant polyester has high photochemical performance and whiteness.

Description

technical field [0001] The invention relates to a polyester catalyst, in particular to a highly active titanium series catalyst used in the production of polyester prepared by the esterification and condensation reaction of aromatic dibasic acid and aliphatic dibasic alcohol. Background technique [0002] Among the polyesters reacted by dibasic acids and diols, PET (abbreviation for polyethylene terephthalate) is a polymer with excellent comprehensive properties. At present, the world's total output has exceeded 20 million tons. And it is still increasing at a rate of more than 7% per year. PET is generally synthesized by direct esterification or transesterification of terephthalic acid or dimethyl terephthalate and ethylene glycol to form ethylene terephthalate, and then further polycondensation in the presence of a catalyst. As PET polycondensation catalysts, antimony compounds, germanium compounds and easily hydrolyzed titanium compounds are gen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/82
Inventor 曹善文张伟红
Owner 济南齐鲁化纤集团有限责任公司
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