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Polyester polycondensation catalyst, preparation method thereof and application thereof

A polycondensation catalyst and catalyst technology are applied in the field of preparation of polyester polycondensation catalysts, which can solve the problems of limited range of performance improvement of nano-composite materials, reduced thermal stability of PET, and it is difficult to completely peel off sheets, etc. Good gas barrier properties, shortened polymerization time, and high polycondensation activity

Active Publication Date: 2011-09-07
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, layered silicate such as montmorillonite has a strong ionic bond between the sheets. Due to the relatively weak polarity of the polyester, the compatibility with the clay is poor, and the clay is in the polyester. It is difficult to achieve complete peeling between the sheets, and it is easy to form large-scale agglomerations, resulting in limited improvement in the performance of polyester / clay nanocomposites
Moreover, the synthesis and processing of PET have to experience high temperatures of nearly 300°C, which often lead to the decomposition of organic cations, thereby inducing the decomposition of PET and reducing the thermal stability of PET.

Method used

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  • Polyester polycondensation catalyst, preparation method thereof and application thereof
  • Polyester polycondensation catalyst, preparation method thereof and application thereof

Examples

Experimental program
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Effect test

Embodiment 1-2

[0025] 6g of Na-montmorillonite was dispersed in 600g of water and stirred for 5 hours. Slowly add 6.6ml TiCl to 95.7ml HCL solution 4 , and stirred for 5 hours. 5.1 ml of the above solution was added dropwise into the suspension of montmorillonite, and the stirring was continued for 5 hours for ion exchange. After the ion exchange is completed, the montmorillonite is repeatedly centrifuged and washed with water until the pH of the centrifuged supernatant is 7 and washed with a drop of AgNO 3 Can not detect Cl - . The obtained titanium-based montmorillonite was dried at 110° C. for 5 hours, calcined at 250° C. for 2 hours, and passed through a 300-mesh sieve to obtain PET polycondensation catalyst A. Take 1.5g of catalyst A, 0.94g of cetyltriphenylphosphine, and 60g of water, and react at 80°C for 3 hours. The reaction product was repeatedly centrifuged and washed until the supernatant was washed with a drop of AgNO 3 Br was not detected - . The product was dried at 11...

Embodiment 3-5

[0027] 20g of Na-montmorillonite was dispersed in 300g of ethylene glycol and stirred for 5 hours. Slowly add 2.2ml TiCl in 300ml ethylene glycol solution 4 , and stirred for 5 hours. Take 30ml of the above solution and add it dropwise into the suspension of montmorillonite, and continue to stir for 5 hours to carry out ion exchange. After the ion exchange is completed, the montmorillonite is repeatedly centrifuged and washed with ethylene glycol until the pH of the centrifuged supernatant is 7 and washed with a drop of AgNO 3 Can not detect Cl - . The obtained titanium-based montmorillonite was dried at 110° C. for 5 hours, and calcined at 250° C. for 2 hours to obtain PET polycondensation catalyst C. Take 1.5 g of catalyst C, 0.8 g of hexadecyl pyridinium bromide, and 60 g of water, and react at 80° C. for 3 hours. The reaction product was repeatedly centrifuged and washed until the supernatant was washed with a drop of AgNO 3 Br was not detected - . Dry the product ...

Embodiment 6-7

[0029] 6g of Na-montmorillonite was dispersed in 600g of water and stirred for 5 hours. Slowly add 2.2ml TiCl in 300ml ethylene glycol solution 4, and stirred for 5 hours. 18ml of the above solution was added dropwise to the suspension of montmorillonite, and the stirring was continued for 5 hours for ion exchange. After the ion exchange is completed, the montmorillonite is repeatedly centrifuged and washed with water until the pH of the centrifuged supernatant is 7 and washed with a drop of AgNO 3 Can not detect Cl - . The obtained titanium-based montmorillonite was dried at 110° C. for 5 hours, calcined at 250° C. for 2 hours, and passed through a 300-mesh sieve to obtain PET polycondensation catalyst F. Catalyst F1.5g, calcined at 400°C for 4h, added polyvinyl alcohol 1.2g, water 60g, reacted at 80°C for 3 hours. The reaction product was repeatedly centrifuged and washed until the supernatant was washed with a drop of AgNO 3 Br was not detected - . Dry the product a...

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Abstract

The invention relates to a polyester polycondensation catalyst, a preparation method thereof and application thereof. The method comprises the steps that: dispersing clay into dissolvant, performing iron exchanging with Ti ion-containing solution, removing the dissolvant, and calcinating under high temperature, wherein the usage amount of the Ti ion is 0.05-1mmol / g of clay; suspending the clay inclay dissolvant for processing organic chemical processing agent or surface processing agent, wherein the usage amount of the organic chemical processing agent is 0.1-1mmol / g of clay; the catalyst isused for the in-situ preparation of p-phenyl dicarboxylic acid gylcol ester or copolymer thereof and clay nanometer composite material; the adding amount of the catalyst is 0.1-10% of the weight of final polymerized p-phenyl dicarboxylic acid gylcol ester and clay nanometer composite material; and the Ti-based clay has high catalytic polycondensation, can shorten polymerization time, and is environment-friendly. The prepared PET and clay nanometer composite material has even clay dispersibility, and better material mechanical property and gas isolation performance.

Description

technical field [0001] The invention relates to a preparation method of a polyester polycondensation catalyst, which can prepare polyethylene terephthalate (PET) and clay nanocomposite materials in situ, and is nontoxic to the environment and human body. Background technique [0002] Polyester polycondensation catalyst is an essential raw material for the production of PET. At present, more than 90% of PET devices in the world use antimony-based catalysts, such as antimony trioxide and antimony acetate. The advantages of antimony-based catalysts are high catalytic activity, relatively low thermal degradation of PET, and excellent comprehensive performance. However, the fatal disadvantage of antimony-based catalysts is that antimony is carcinogenic, and antimony-containing ethylene glycol must be burned in a special furnace, or must be treated as dangerous goods, resulting in increased production costs. In addition, antimony can also be leached out during fiber dyeing, caus...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/82C08L67/02C08K9/00
Inventor 殷明李春成祖凤华管国虎张栋乔明肖耀南
Owner PETROCHINA CO LTD
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