Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Antimony/ titanium composite catalyst and application thereof in method for preparing polyethylene glycol terephthalate (PET) copolyesters

A technology of composite catalyst and titanium catalyst, which is applied in the field of highly active antimony/titanium composite catalyst, can solve the problems of large amount of antimony-based catalysts, decreased thermal stability of polyester, and easy graying of products, so as to prevent graying of products, Good heat stability and low dosage

Active Publication Date: 2014-06-11
MATRIX GUANGZHOU CHEM CORP
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the amount of antimony-based catalysts in the prior art is large, and the products are prone to graying; the titanium-based catalysts are likely to cause yellowing of the products and reduce the thermal stability of polyester

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Slowly add butyl titanate to ethylene glycol at 70°C, the molar concentration of butyl titanate is 1.0mol / L, stir until the mixture is uniform, and raise the temperature to 190°C under the condition of continuously feeding nitrogen, and continue Stir for 12 hours, add antimony acetate, stir evenly, store at 50°C until use, and name it Catalyst A.

[0020] Add 3880g of dimethyl terephthalate, 2400g of ethylene glycol, 310g of polyethylene glycol 8000, and catalyst A (based on the amount of polymer produced, the amount of titanium used is 15ppm, and the amount of antimony used is 150ppm) into the reactor, Under the protection of nitrogen, keep the temperature in the reactor at 180°C, react for 100 minutes, then add 300ppm of triphenyl phosphite, 50ppm of di(tetradecyl)thiodipropionate, raise the temperature to 270°C, and gradually establish a vacuum, at 45 Reduce the pressure in the reactor to 60Pa within 1 minute, react for 1.5 hours, fill with nitrogen to break the vacu...

Embodiment 2

[0023] Slowly add isopropyl titanate to ethylene glycol at 70°C, the molar concentration of butyl titanate is 2.0mol / L, stir until the mixture is uniform, and raise the temperature to 190°C under the condition of continuously feeding nitrogen. Stirring was continued for 12 hours. Add antimony trioxide, stir evenly and store at 50°C until use. Named Catalyst B.

[0024] Add 3880g of dimethyl terephthalate, 2400g of ethylene glycol, 155g of polytetrahydrofuran 2000, and catalyst B (based on the amount of polymer produced, the amount of titanium is 35ppm, and the amount of antimony is 100ppm) into the reactor, under nitrogen protection The temperature in the reactor was maintained at 180° C., and the reaction was carried out for 80 minutes. Then add triphenyl phosphate 300ppm, di(dodecyl) thiodipropionate 50ppm, heat up to 270 o C, and gradually establish a vacuum, reduce the pressure in the reactor to 60Pa in 45 minutes, and react for 1.5 hours. Nitrogen is filled to break t...

Embodiment 3

[0027] Slowly add isopropyl titanate to ethylene glycol at 70°C, the molar concentration of butyl titanate is 1.5mol / L, stir until the mixture is uniform, and raise the temperature to 190°C under the condition of continuously feeding nitrogen. Stirring was continued for 12 hours. Add antimony ethylene glycol, stir well and store at 50°C until use. Named Catalyst C.

[0028] Add 3880g of dimethyl terephthalate, 2400g of ethylene glycol, 246g of polyethylene glycol 2000, catalyst C (based on the amount of polymer produced, the amount of titanium used is 50ppm, and the amount of antimony is 70ppm), added to the reactor, Under the protection of nitrogen, the temperature in the reactor was maintained at 180° C., and the reaction was carried out for 80 minutes. Then add 150ppm of trimethyl phosphate and 20ppm of di(tridecyl)thiodipropionate, raise the temperature to 270°C, and gradually establish a vacuum, reduce the pressure in the reactor to 60Pa within 45 minutes, and react for...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
melting pointaaaaaaaaaa
crystallization temperatureaaaaaaaaaa
melting pointaaaaaaaaaa
Login to View More

Abstract

The invention discloses a high-activity antimony / titanium composite catalyst, which contains the following components: 1 antimony catalysts, 2 titanium catalysts, 3 first catalyst promoters and 4 second catalyst promoters, wherein the antimony catalysts are oxides and salts of antimony, the titanium catalysts are titanates, the first catalyst promoters are phosphoric acids, phosphorous acids and alkyl groups and / or polyaryl ethers of the phosphorous acids, and the second catalyst promoters are benzothiodiazoles. The antimony / titanium composite catalyst can be used in a method for preparing polyethylene glycol terephthalate (PET) copolyesters, which includes the following steps: 1 mixing and adding the antimony / titanium catalyst, the first catalyst promoters, the second catalyst promoters and binary acids into a reaction system, 2 leading the terephthalic acids, esters of the terephthalic acids and excess ethylene glycol to together perform an esterification reaction at temperature of 240-260 DEG C, at pressure of 0.2-0.4MPa and with reaction time of 1-2 hours, and 3 adding copolymerization glycol monomers for a polycondensation reaction to obtain the copolyesters. The antimony / titanium composite catalyst and the application thereof in the method for preparing the PET copolyesters have the advantages that the catalyst can activate the antimony series catalyst and shortens polycondensation time, and the problem of decreasing of polyester heat stability due to the fact that the antimony series catalyst is apt to yellow products is solved.

Description

technical field [0001] The invention relates to a high-activity antimony / titanium composite catalyst, and also relates to the application of the high-activity antimony / titanium composite catalyst in PET copolyester. Background technique [0002] Antimony trioxide or antimony acetate are generally used as catalysts in polyester production. Although the properties of the polyester products prepared by them, such as viscosity and color, can meet the requirements of general-purpose polyesters, there are still some shortcomings: 1. During the polycondensation process, Sb 3+ It is reduced to metal antimony, which makes the product gray; 2. The amount of antimony catalyst added is relatively large, generally 150~300ppm. Germanium-based catalysts have good stability, cause fewer side reactions in the reaction, and the obtained polyester has a good hue, but due to the lack of resources, the price is expensive; titanium-based catalysts have high activity, but titanium-based catalysts ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/86C08G63/183C08G63/672
Inventor 赵巍蔡彤旻曾祥斌徐依斌苑仁旭焦建钟宇科
Owner MATRIX GUANGZHOU CHEM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com