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Titanium-series polyester catalyst and method thereof for producing copolyester

A technology for titanium-based polyesters and catalysts, applied in the field of titanium-based polyester catalysts and the production of copolyesters using said catalysts, can solve problems such as high equipment requirements, yellowing of polyester products, and complicated preparation processes, and achieve reduction of side effects. Effects of reaction, enhanced solubility, and high intrinsic viscosity

Active Publication Date: 2017-12-26
JIANGSU JINGHONG NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For germanium-based catalysts, due to the scarcity of germanium resources in nature, germanium-based catalysts are expensive and rarely used in polyester production
For a long time, titanium-based catalysts have become the most researched type of polyester catalysts due to their high catalytic activity and safety and environmental protection. However, titanium-based catalysts also have disadvantages such as poor stability and yellowing of polyester products.
[0004] CN103539928A discloses a production method of a titanium-based polyester catalyst, but its preparation process is relatively complicated, and is only used in the synthesis of PET; CN103709383 provides a titanium-based catalyst, using nano-silica as a carrier, and ethylene glycol Titanium is used as a catalytic active center, but the polyester chip b value prepared by it is relatively large; CN1962720B provides a method for preparing a titanium-based catalyst, but the preparation process requires vacuum distillation, which requires high equipment, and the catalyst is only used in Production of PET

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The preparation of titanium series polyester catalyst A:

[0025] Add 56.8 g (0.2 mol) of tetraisopropyl titanate and 124 g (2 mol) of ethylene glycol into a reaction kettle equipped with a distillation device, mix well and stir for 5 minutes. Heating to 120°C under the protection of nitrogen produced a white solid. After reacting for 9 h, a total of 47.8 g of isopropanol was distilled out. Add 28 grams (0.2 moles) of trimethyl phosphate, heat to 180° C. and react for 5 hours, and finally obtain milky white titanium-based polyester catalyst A.

[0026] Preparation of copolyester:

[0027] 20 kg of terephthalic acid, 7.47 kg of ethylene glycol and 3.76 kg of neopentyl glycol were made into a slurry and put into a reaction kettle for esterification at a temperature of 250°C and a pressure of 0.15 MPa. The water generated by the reaction was discharged through a rectification device. The esterification time was 180 min. After the esterification was completed, catalyst A ...

Embodiment 2

[0029] The preparation of titanium series polyester catalyst B:

[0030] Add 68 g (0.2 mol) of tetrabutyl titanate and 124 g (2 mol) of ethylene glycol into a reactor equipped with a distillation device, mix well and stir for 5 minutes. Heating to 160°C under the protection of nitrogen produced a white solid. After reacting for 9 h, a total of 58 g of n-butanol was distilled out. Then add 72.8 g (0.4 mol) of triethyl phosphate, heat to 180° C. and react for 5 hours, and finally obtain milky white titanium-based polyester catalyst B.

[0031] Preparation of copolyester:

[0032] 20 kg of terephthalic acid, 7.47 kg of ethylene glycol, and 8.67 kg of 1,4-cyclohexanedimethanol were made into a slurry and put into a reaction kettle for esterification reaction. The esterification temperature was 260°C and the pressure was 0.45Mpa. The water generated by the reaction was discharged through a rectification device. The esterification time was 140 min. After the esterification was com...

Embodiment 3

[0034] Preparation of Titanium-based Polyester Catalyst C

[0035] Add 46 g (0.2 mol) of tetraethyl titanate and 248 g (4 mol) of ethylene glycol into a reaction kettle equipped with a distillation device, mix well and stir for 5 minutes. Heated to 90°C under the protection of nitrogen to produce a white solid. After reacting for 9 h, 36 g of ethanol was distilled out. Then add 326 g (1 mole) of triphenyl phosphate, heat to 160° C. and react for 10 hours to finally obtain milky white titanium-based polyester catalyst C.

[0036] Preparation of copolyester

[0037] Put 20 kilograms of terephthalic acid, 7.8 kilograms of ethylene glycol, 5 kilograms of 1,4-cyclohexanedimethanol and 2.8 kilograms of isosorbide into a slurry and put them into the reaction kettle for esterification reaction. The esterification temperature is 245 ℃, the pressure is 0.35Mpa. The water generated by the reaction was discharged through a rectification device. The esterification time was 160 min. Afte...

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Abstract

The invention discloses a titanium-series polyester catalyst and a method thereof for producing copolyester. The catalyst is obtained by the reaction of titanate, ethylene glycol and phosphoric acid ester. A copolyester chip is produced by using the catalyst, and the intrinsic viscosity of the chip is 0.75 to 0.81dl / g, the b value is between 1 and 3.5. The copolyester product provided by the invention is characterized in that the copolyester product has the advantages of neutral color, high intrinsic viscosity and good transparency, and can be widely applied to the markets of plates, sheets, high-performance heat shrinkable films, bottles and the like.

Description

technical field [0001] The invention relates to a titanium series polyester catalyst and a method for producing copolyester by using the catalyst. Background technique [0002] Copolyester refers to the modification of polyethylene terephthalate (PET) with modified diols. After these modified diols are introduced into the PET macromolecular chain, the original structure of PET can be made It is changed to reduce the crystallization ability of PET and improve the flexibility of macromolecular chains. The modified copolyester has the characteristics of high transparency, good toughness and good heat shrinkability. It can be widely used in fields such as sheets, cosmetic bottles, heat shrinkable films, etc., and has a good market prospect. [0003] Generally, the commonly used catalysts for copolyester synthesis are: antimony, germanium, titanium, etc., among which antimony is a heavy metal catalyst, which has safety problems. In the production of food containers that are rel...

Claims

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Application Information

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IPC IPC(8): C08G63/85C08G63/87C08G63/183C08G63/199C08G63/42
CPCC08G63/183C08G63/199C08G63/42C08G63/85C08G63/87
Inventor 吴培龙吴迪陆银秋
Owner JIANGSU JINGHONG NEW MATERIAL TECH
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