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High-activity titanium complex catalyst, preparation method and application thereof in copolyester synthesis

A composite catalyst and high-activity technology, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., to achieve high activity, improve reaction efficiency, eliminate potential hazards and protect the environment Effects of Pollution Problems

Active Publication Date: 2013-01-16
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Although the titanium-based catalysts invented by existing patents have high catalytic activity, they still need to be further improved in terms of product thermal stability, product appearance and the cost of the catalyst itself.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Slowly add tetraisopropyl titanate into 1,4-butanediol, the molar concentration of tetraisopropyl titanate in the mixed solution is 1.0mol / L, stir until the mixture is uniform, and the temperature is React at 190°C for 12 hours, and continuously feed high-purity nitrogen to remove volatile small molecules, and cool to room temperature to obtain a butanediol solution of nano-titanium dioxide particles.

[0034] Add a certain amount of n-butyl titanate (TBOT) and potassium tripolyphosphate (PTPP) to the above-mentioned butanediol solution of nano-titanium dioxide to form n-butyl titanate (TBOT), nano-titanium dioxide (TiO 2 ), a mixture of potassium tripolyphosphate (PTPP), whose composition is TBOT / TiO 2 / PTPP=0.2 / 0.1 / 0.1, named catalyst A.

[0035] 16.1kg of 1,4 butanediol, 10.4kg of dimethyl terephthalate, 85.6g of trimethylolpropane, and catalyst A (based on the amount of polymer produced, the amount of titanium is 50ppm) are added to the reactor , under the protect...

Embodiment 2

[0039] Slowly add tetraisopropyl titanate into 1,4-butanediol, the molar concentration of tetraisopropyl titanate in the mixed solution is 1.0 mol / L, stir until the mixture is uniform, at a temperature of 200°C The reaction was carried out for 8 hours under the same conditions, and high-purity nitrogen gas was continuously fed in order to remove volatile small molecules, and cooled to room temperature to obtain a butanediol solution of nano-titanium dioxide particles.

[0040] Add a certain amount of n-butyl titanate (TBOT) and sodium tripolyphosphate (STPP) to the above-mentioned butanediol solution of nano-titanium dioxide to form n-butyl titanate (TBOT), nano-titanium dioxide (TiO 2 ), a mixture of sodium tripolyphosphate (STPP), whose composition is TBOT / TiO 2 / STPP=0.2 / 0.1 / 0.1, named Catalyst B.

[0041] Add 60 g of 1,4-butanediol and 35 g of dimethyl terephthalate into the flask, under nitrogen protection, heat up to 170° C., add catalyst B (based on the amount of polym...

Embodiment 3

[0045] Slowly add tetraisopropyl titanate to 1,4-butanediol, the molar concentration of tetraisopropyl titanate in the mixed solution is 1.5mol / L, stir until the mixture is uniform, and at a temperature of 190 The reaction was carried out under the condition of ℃ for 10 hours, and high-purity nitrogen gas was constantly fed in order to remove volatile small molecules, and cooled to room temperature to obtain a butanediol solution of nano-titanium dioxide particles.

[0046] A certain amount of tetraisopropyl titanate (TPT) and sodium dihydrogen phosphate (SDP) are added to the butanediol solution of the above-mentioned nano-titanium dioxide to form tetraisopropyl titanate (TPT), nano-titanium dioxide (TiO 2 ), a mixture of sodium dihydrogen phosphate (SDP), whose composition is TPT / TiO 2 / SDP=0.2 / 0.1 / 0.1, named catalyst C.

[0047] 54g 1,4 butanediol, 30g dimethyl terephthalate, 5g dimethyl isophthalate are added in the flask, under the protection of nitrogen, the temperature...

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Abstract

The invention discloses a high-activity titanium complex catalyst, a preparation method and application thereof in copolyester synthesis. The high-activity titanium complex catalyst comprises a main catalyst, a first cocatalyst and a second cocatalyst, wherein the main catalyst is titanate, the first cocatalyst is nanometer titanium dioxide, and the second cocatalyst is phosphate of IA, IIA or IIIA group metals; and the molar ratio of the nanometer titanium dioxide to the main catalyst is 0-3:1, and the molar ratio of phosphorus atoms in the phosphate to the main catalyst is 0-3:1. The titanium complex catalyst has high activity, and can improve the efficiency of esterification and polycondensation reactions during the catalytic synthesis of polyester; the titanium complex catalyst does not contain heavy metals, and can eliminate the potential hazard of heavy metal catalysts on human health and environmental pollution problem; and the polyester produced by the titanium complex catalyst has better appearance.

Description

Background technique [0001] In the polycondensation process of polyester, more than 90% use antimony (Sb) catalysts, which are composed of antimony acetate and antimony trioxide (Sb) 2 o 3 ) and other compositions, the effective concentration of Sb is about 150-300ppm. Antimony (Sb) catalysts can be used for almost all grades of polyesters because of their ease of use, low price, and high catalytic activity. Despite the excellent performance of antimony catalysts, recent scientific research has found that antimony elements are harmful to human health and environmental pollution, and the latest European and Chinese mainland laws have clearly limited the content of antimony, and require low antimony content for textiles , and the products are distinguished by eco-friendly textiles and the "ECO" label and the unofficial "OEKO" label, especially for sportswear and intimate clothing that use polyester fibers, which have been marked with "antimony-free" or "heavy metal-free" The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/26C08G63/85
Inventor 苑仁旭徐依斌焦建曾祥斌夏世勇袁志敏
Owner KINGFA SCI & TECH CO LTD
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