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Method for titanium glycolate catalyzed synthesis of modified copolyester slice

A titanium glycol catalyzed, titanium ethylene glycol technology is applied in the field of titanium glycol catalyzed synthesis of modified copolyester chips, which can solve the problems of increased polyester production costs, high equipment requirements, and expensive prices, and achieve Increased polycondensation reaction speed, high intrinsic viscosity, and easy industrialization

Inactive Publication Date: 2016-10-12
JIANGSU JINGHONG NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN1033772673A discloses a method for synthesizing PET polyester chips with a titanium-based catalyst, wherein the production process of the titanium-based catalyst will produce toxic hydrogen chloride gas, which requires tail gas treatment, which requires high equipment and is not conducive to mass production
Patent No. 200510127804.9 discloses a method for catalytically synthesizing modified copolyester with titanium ethylene glycol, but this method uses expensive cocatalysts such as germanium oxide, which increases the cost of polyester production
CN103772685A provides a method for synthesizing titanium-based catalysts, but the preparation process is relatively complicated, which is not conducive to mass production, and the prepared polyester has a yellowish hue

Method used

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  • Method for titanium glycolate catalyzed synthesis of modified copolyester slice
  • Method for titanium glycolate catalyzed synthesis of modified copolyester slice
  • Method for titanium glycolate catalyzed synthesis of modified copolyester slice

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add terephthalic acid, glycol, titanium glycolate and cobalt compound into the beating kettle according to the ingredient list, beat into a slurry, and then import it into the reaction kettle through a delivery pump, and carry out the esterification under 0.2Mpa nitrogen pressure at 255°C. reaction, the esterification stirring speed is 30rpm. After 150 min of reaction, 4.2 kg of esterification water was collected, and the esterification reaction was completed.

[0035] Using nitrogen pressure, the above-mentioned esterification reaction product is pressed into the polycondensation kettle. According to the ingredients list, add ethylene glycol, blue dye (R=1, R1=1), red dye with R as methyl, and trimethyl phosphate into the polycondensation tank at 265°C and 40rpm stirring , vacuumize the polycondensation kettle continuously, within 40 minutes, control the pressure inside the kettle to 200 Pa, then within 30 minutes, control the pressure inside the kettle to 50 Pa, cont...

Embodiment 2

[0037] Put terephthalic acid, ethylene glycol, 1,4-cyclohexanedimethanol, ethylene glycol titanium, and cobalt nitrate into the beating kettle according to the ingredient list, and after making slurry, add it to the reaction kettle via a delivery pump. The esterification reaction was carried out at 235° C. under a nitrogen pressure of 0.3 Mpa, and the stirring speed of the esterification was 30 rpm. After 140 min of reaction, 3.9 kg of esterification water was collected, and the esterification reaction was completed.

[0038] Using nitrogen pressure, the above-mentioned esterification reaction product is pressed into the polycondensation kettle. According to the ingredients list, add ethylene glycol, (R=2, R1=3) blue dye, R is ethyl red dye, and triphenyl phosphate into the polycondensation tank, and stir at 260 ° C and 40 rpm , vacuumize the polycondensation kettle continuously, within 30 minutes, control the pressure inside the kettle to 500 Pa, then within 40 minutes, cont...

Embodiment 3

[0040] Put terephthalic acid, ethylene glycol, isosorbide, ethylene glycol titanium, and cobalt acetate tetrahydrate into the beating kettle according to the ingredient list, and put it into the reaction kettle through a delivery pump after making a slurry. The esterification reaction was carried out at 258° C., and the stirring speed of the esterification was 30 rpm. After reacting for 180 min, 4.2 kg of esterification water was collected, and the esterification reaction was completed.

[0041] Using nitrogen pressure, the above-mentioned esterification reaction product is pressed into the polycondensation kettle. Add ethylene glycol, (R=3, R1=1) blue dye, red dye whose R is methoxy, and triethyl phosphate to the polycondensation tank according to the ingredients list, and stir at 265°C and 40rpm , vacuumize the polycondensation kettle continuously, within 30 minutes, control the pressure inside the kettle to 400 Pa, then within 40 minutes, control the pressure inside the ke...

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Abstract

The invention discloses a method for titanium glycolate catalyzed synthesis of a modified copolyester slice. The method includes: subjecting terephthalic acid and diol in a mole ratio of 1:1.2-2.0, a titanium glycolate catalyst and a cobalt compound to esterification, subjecting the esterification product to polycondensation with blue dye, red dye, an organic compound stabilizer of phosphorus and a small amount of ethylene glycol, then utilizing nitrogen to extrude a melt, and performing casting strip dicing to obtain a modified copolyester slice, wherein the titanium glycolate catalyst is obtained by under the protection of nitrogen, mixing tetrabutyl titanate with ethylene glycol to form a clarified solution, performing heating to 160DEG C, carrying out reaction for 9h, distilling off and collecting the reaction generated n-butanol, cooling the reaction solution to room temperature, conducting filtering and collecting solid, washing the solid with acetone repeatedly, and carrying out drying. The method accelerates the polymerization reaction, and the synthesis process of titanium glycolate does not generate hydrogen chloride or other toxic gases, the process is simple and is convenient for industrialization, and the prepared copolyester slice has neutral tone.

Description

technical field [0001] The invention belongs to the field of preparation of modified copolyester, in particular to a method for catalytically synthesizing modified copolyester chips with titanium ethylene glycol. Background technique [0002] Modified copolyester refers to the copolymerization modification of polyethylene terephthalate (PET) by the third monomer, so that the regularity of PET macromolecules is broken, and non-crystalline or low-crystallinity polyester is prepared. Copolyester. Modified copolyesters are mainly used in markets such as plates, sheets, high-performance heat-shrinkable films, and bottles. Copolyester heat shrinkable film has excellent shrinkage and printing properties, and can replace traditional heat shrinkable film raw material polyvinyl chloride (PVC). With the increasing tide of environmental protection at home and abroad, the demand for copolyester heat shrinkable film will undoubtedly increase. Rapid growth. [0003] Antimony (Sb) cataly...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/85
Inventor 吴培龙
Owner JIANGSU JINGHONG NEW MATERIAL TECH
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