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Titanium catalyst and preparation method and application thereof

A titanium catalyst and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problems of unsuitable polymerization reaction catalysts, difficulty in obtaining high viscosity and low activity and other problems, to achieve the effect of improving catalytic activity, short esterification reaction and polymerization reaction time, and high catalytic activity

Inactive Publication Date: 2013-01-16
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Butyl titanate or isopropyl titanate has high catalytic activity for esterification reaction, however, they are easy to hydrolyze, because a large amount of water is generated in the late stage of esterification reaction, so they are not suitable as catalysts for polymerization reaction
The above three antimony compounds have higher activity for the polymerization of PET, but have lower activity for the polymerization of 1,3-trimethylene terephthalate (also known as PTT). They are used as catalysts for the polymerization of PTT , it is difficult to obtain high-viscosity PTT, and low-viscosity PTT cannot be spun

Method used

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  • Titanium catalyst and preparation method and application thereof
  • Titanium catalyst and preparation method and application thereof
  • Titanium catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 18.38 grams of α-glycolic acid (Sinopharm Chemical Reagent Co., Ltd., chemically pure), put it into a 250-ml round-bottomed single-necked flask, measure 60 mL of tetrahydrofuran and pour it into the flask, magnetically stir to dissolve α-glycolic acid, and heat up to At 60°C (oil bath temperature, the same below), add 40.84g of butyl titanate (Tianjin Fuchen Chemical Reagent Factory, chemically pure) dropwise with a constant pressure dropping funnel, a large amount of white precipitates are produced, and the dropwise addition is completed in 1 hour. Heat up to tetrahydrofuran reflux, continue to stir and react for 2.5 hours, cool to room temperature, carefully filter with suction, wash with a small amount of absolute ethanol several times, drain, dry in a blast oven at 70°C for several hours, and weigh 22.57g , the yield was 96%.

Embodiment 2

[0025] Put 91.46 grams of α-glycolic acid (Shanghai Aladdin Reagent Factory, purity 99.5%) into a 1000mL three-necked flask, then pour 150mL of absolute ethanol (analytical grade), stir magnetically, heat up to 65°C, and wait for α-glycolic acid After it was completely dissolved, 204.17 g of butyl titanate (Tianjin Fuchen Chemical Reagent Factory, chemically pure) was added dropwise through a constant-pressure dropping funnel. A large amount of white precipitates were produced, and the addition was completed in about 1 hour. Continue to stir and react at this temperature for 2.5 hours, cool to room temperature, carefully suction filter, wash 3 times with a small amount of absolute ethanol, drain, dry in a blast oven at 70°C for several hours, and weigh 106.26 grams. The yield is 90%.

Embodiment 3

[0027] Weigh 91.30 grams of α-glycolic acid (Shanghai Aladdin Reagent Factory, purity 99.5%) in a 1000mL three-necked flask, then pour 150mL of absolute ethanol (analytical grade), and stir magnetically. After the α-glycolic acid is completely dissolved, Add 204.04 g of butyl titanate (Tianjin Fuchen Chemical Reagent Factory, chemically pure) dropwise at room temperature, and finish the dropwise addition in 3 hours. Only when more butyl titanate is added dropwise will white precipitate occur. Continue to stir and react for 2 hours at room temperature , carefully suction filtered, washed 3 times with a small amount of absolute ethanol, drained, dried in a blast oven at 90°C for 5 hours, and weighed to obtain 104.48 grams of titanium α-hydroxyacetate, with a yield of 89%.

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Abstract

The invention discloses a titanium catalyst and a preparation method and application thereof. The titanium catalyst is alpha-titanium glycolate with a structural formula as shown in Formula I. The alpha-titanium glycolate catalyst is synthesized through transesterification of alpha-hydroxy acetic acid and titanium butoxide. The structure of the alpha-titanium glycolate of the invention is verified by linked determination of hydrogen spectrum of nuclear magnetic resonance (1HNMR) and high-performance liquid chromatography-electrospray ionization mass spectrometry (HPLC-ESI / MS). When the catalyst of the invention is used for synthesizing polyester, the rates of esterification and polymerization are high, the reaction time is short, the intrinsic viscosity of the obtained polyester is high, and the polyester is conducive to spinning. Moreover, the catalyst of the invention has high reactivity and good stability, and can not be easily hydrolyzed, thereby improving the catalytic activity of the organic titanium.

Description

technical field [0001] The invention relates to a titanium catalyst, in particular to a titanium catalyst used for preparing polyester and a preparation method thereof. Background technique [0002] The catalyst used in the esterification reaction of synthetic polyethylene terephthalate (also known as PET) is usually butyl titanate or isopropyl titanate, and antimony compounds such as antimony trioxide, antimony acetate or antimony glycol. Butyl titanate or isopropyl titanate has high catalytic activity for esterification reaction, however, they are easy to hydrolyze, because a large amount of water is generated in the late stage of esterification reaction, so they are not suitable as catalysts for polymerization reaction. The above three antimony compounds have higher activity for the polymerization of PET, but have lower activity for the polymerization of 1,3-trimethylene terephthalate (also known as PTT). They are used as catalysts for the polymerization of PTT , It is ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C08G63/85C08G63/183
Inventor 王拴紧孟跃中刘坚肖敏
Owner SUN YAT SEN UNIV
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