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Polyester polycondensation catalyst, preparation method and application thereof

A polycondensation catalyst and polyester technology, which are applied to the polyester polycondensation catalyst and the fields of preparation and application thereof, can solve the problems of polluting the environment, yellowing of the product, increase in cost, etc., and achieve the effects of high catalytic efficiency, lower dosage and lower usage.

Active Publication Date: 2009-10-28
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the common problem of these catalysts is that the product is yellow, and toner needs to be added, which increases the cost and has the risk of polluting the environment.

Method used

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  • Polyester polycondensation catalyst, preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1, preparation polyester polycondensation catalyst

[0024] Take 5mL concentrated hydrochloric acid, 10mL ethanol, mix with 19.6g tetraethyl orthosilicate (TEOS) at room temperature, stir for 1 hour to obtain the product A SiO 2 Sol.

[0025] Mix 2.5g of titanium tetrachloride with 10mL of concentrated hydrochloric acid at room temperature and stir for 1 hour at room temperature to obtain the product B TiO 2 Sol.

[0026] The product A SiO 2 Sol and product B TiO 2 The sols were mixed and stirred at 50°C for 12 hours to obtain the product CTiO 2 / SiO 2 Sol.

[0027] At room temperature, the product C TiO 2 / SiO 2 The sol was reacted with 3g of 1,2 dimethyl-3-N-hexadecylimidazolium bromide in 30g of water, and after stirring for 8 hours, the supernatant was centrifuged and washed with AgNO 3 Br was not detected - , and vacuum-dried the obtained precipitate at 80° C. to obtain a polyester polycondensation catalyst numbered D, as shown in Table 2.

[...

Embodiment 2

[0029] Embodiment 2, preparation polyester polycondensation catalyst

[0030] Take 5mL concentrated hydrochloric acid, 10mL ethanol, mix with 19.6g tetraethyl orthosilicate (TEOS) at room temperature, stir for 1 hour to obtain the product A SiO 2 Sol.

[0031] Take 2.5g titanium tetrachloride and mix with 10mL concentrated hydrochloric acid, stir at room temperature for 1 hour to obtain the product B TiO 2 Sol.

[0032] The product A SiO 2 Sol and product B TiO 2 The sols were mixed and stirred at 50°C for 12 hours to obtain the product CTiO 2 / SiO 2 Sol.

[0033] At room temperature, the product C TiO 2 / SiO 2 The sol was reacted with 1g of polyvinylpyrrolidone (PVP) in 20g of ethylene glycol, stirred for 24 hours, washed twice with ethylene glycol, and the resulting precipitate was vacuum-dried at 120°C to obtain a polyester polycondensation catalyst numbered G, such as Table 3 shows.

[0034] Using the same preparation method and conditions as above, only 1g of po...

Embodiment 3

[0039] Embodiment 3, preparation polyester polycondensation catalyst

[0040] Take 5mL concentrated hydrochloric acid, 10mL ethanol, mix with 19.6g tetraethyl orthosilicate (TEOS) at room temperature, and stir for 1 hour to obtain the product A SiO 2 Sol.

[0041] Take 2.5g titanium tetrachloride and mix with 10mL concentrated hydrochloric acid, stir at room temperature for 1 hour to obtain the product B TiO 2 Sol.

[0042] The product A SiO 2 Sol and product B TiO 2 The sols were mixed and stirred at 50°C for 12 hours to obtain the product CTiO 2 / SiO 2 Sol.

[0043] At room temperature, the product C TiO 2 / SiO 2 The sol was added to 30 g of water and ethanol with a weight ratio of 1:9 to react with 3 g of hexadecyl triphenylphosphine. After stirring for 8 hours, the supernatant was centrifuged and washed with AgNO 3 Br was not detected - , and vacuum-dried the obtained precipitate at 80° C. to obtain the polyester polycondensation catalyst numbered J provided by t...

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Abstract

The invention discloses a polyester polycondensation catalyst, a preparation method and application thereof. The preparation method comprises the following steps that: 1) a titanium-containing compound is hydrolyzed in water and / or an alcoholic solution to obtain a TiO2 sol, a silicon-containing compound is hydrolyzed in the water and / or the alcoholic solution to obtain a SiO2 sol, and the two sols are mixed evenly to obtain a TiO2 / SiO2 sol; and 2) the TiO2 / SiO2 sol and a nitrogen-containing or phosphorus-containing compound react to obtain a target product. The method for preparing the polyester polycondensation catalyst has simple and convenient process, is easy to operate, regulates and controls the activity of a catalytic center Ti through the coordination effect of the nitrogen-containing or phosphorus-containing compound with high thermal stability, remarkably reduces the using amount of the Ti, and fully inhibits the catalysis effect of the catalyst on a condensation side reaction and the thermal degradation of polyester. The catalyst does not need to add a toner during the use, has high catalytic efficiency, and can be used for catalyzing the polymerization of aromatic and aliphatic polyesters; and the using amount of the catalyst is greatly reduced and is about 0.0003 to 0.05 percent of the theoretical yield of the polyesters.

Description

technical field [0001] The invention relates to a polyester polycondensation catalyst, a preparation method and application thereof. Background technique [0002] Polyester is a very important material, which is widely used in packaging, transportation, textile, construction and other fields closely related to people's daily life. Today, my country has become the world's second largest producer of polyester. In 2006, my country's polyester output was 8.12 million tons, and it is expected to exceed 19 million tons in 2010. In the production of polyester, polyester polycondensation catalyst is essential. At present, the commonly used polyester polycondensation catalysts mainly include antimony series and titanium series. The antimony-based polycondensation catalyst has high activity and a small catalytic effect on thermal degradation of PET, and the obtained polyester material has good color and performance. However, the fatal disadvantage of antimony-based catalysts is th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/82
Inventor 殷明李春成管国虎张栋肖耀南袁学培
Owner INST OF CHEM CHINESE ACAD OF SCI
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