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Special optical polyester synthesis catalyst and preparation method and application thereof

A catalyst and co-catalyst technology, which is applied in the field of special catalysts for optical polyester synthesis, can solve problems such as unsatisfactory polycondensation activity, and achieve the effects of easier control of product quality stability, improved environmental friendliness, and reduced usage

Active Publication Date: 2016-08-17
HARBIN INST OF TECH WUXI RES INST OF NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN101117432B discloses a polyester / AlOOH nanocomposite material and its preparation method and the use of the composite material as a flame retardant material. In the process, ethylene glycol sol with nano-AlOOH is added, and polyester / AlOOH nanocomposites are prepared through esterification and polycondensation reactions. Unfortunately, when γ-AlOOH is used alone, the polycondensation activity is not ideal, and it can only be used as a filler in polyester composites. Among the materials, it cannot be used alone as a catalyst in the synthesis of polyester, and there is no report on the use of γ-AlOOH as a polyester polycondensation catalyst.

Method used

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  • Special optical polyester synthesis catalyst and preparation method and application thereof
  • Special optical polyester synthesis catalyst and preparation method and application thereof
  • Special optical polyester synthesis catalyst and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] Heat, stir and hydrolyze 2 g of basic aluminum acetate in 0.02 g of sodium acetate in deionized water (100 mL in volume) at 100°C for 2 hours, then cool and stand for 0.5 hours to discard the precipitate to obtain γ-AlOOH hydrogel;

[0076] Add 100mL of ethylene glycol to the obtained γ-AlOOH hydrogel, distill off water at 70°C under reduced pressure, and obtain a γ-AlOOH-ethylene glycol dispersion after filtration, the measured concentration is 0.0193g / mL;

[0077] Measure 50ml of γ-AlOOH-ethylene glycol dispersion, add ethylene glycol antimony (2.4125g) with a mass ratio of 10:4 to γ-AlOOH, stir well and filter to obtain a special catalyst for optical polyester synthesis (total mass Concentration 0.067 g / mL);

[0078] Use 1.2mL of this catalyst to catalyze terephthalic acid (200g) and ethylene glycol to synthesize polyethylene terephthalate (direct esterification method, alkyd ratio 1.3) in a polyester synthesis kettle, and the esterification temperature is 265 °C, t...

Embodiment 2

[0080] Heat, stir and hydrolyze 2 g of basic aluminum acetate in 0.08 g of sodium acetate in deionized water (volume 100 mL) at 90°C for 3 hours, then cool and stand for 0.5 hours to discard the precipitate to obtain γ-AlOOH hydrogel;

[0081] Add 100mL of ethylene glycol to the obtained γ-AlOOH hydrogel, distill off water at 80°C under reduced pressure, and obtain a γ-AlOOH-ethylene glycol dispersion after filtration, the measured concentration is 0.0197g / mL;

[0082] Measure 50ml of γ-AlOOH-ethylene glycol dispersion, add antimony acetate (2.4625g) with a mass ratio of γ-AlOOH of 10:4, stir well and filter to prepare a special catalyst for optical polyester synthesis (total mass concentration 0.068 g / mL);

[0083] Use 1.17mL of this catalyst to catalyze terephthalic acid (200g) and ethylene glycol to synthesize polyethylene terephthalate (direct esterification method, alkyd ratio 1.3) in a polyester synthesis kettle, and the esterification temperature is 265 °C, the end poi...

Embodiment 3

[0085] Heat and stir 2 g of basic aluminum acetate under the action of 0.1 g of sodium acetate in deionized water (volume 100 mL) at 100 ° C for 2 hours for hydrolysis, then cool and stand for 1 hour to discard the precipitate to obtain γ-AlOOH hydrogel;

[0086] Add 100mL of ethylene glycol to the obtained γ-AlOOH hydrogel, distill off water at 80°C under reduced pressure, and obtain a γ-AlOOH-ethylene glycol dispersion after filtration, the measured concentration is 0.0195g / mL;

[0087] Measure 50ml of γ-AlOOH-ethylene glycol dispersion, add ethylene glycol antimony (4.875g) with a mass ratio of 5:1 to γ-AlOOH, stir well and filter to prepare a special catalyst for optical polyester synthesis (total mass Concentration 0.117g / mL);

[0088] Use 0.52mL of this catalyst to catalyze terephthalic acid (200g) and ethylene glycol to synthesize polyethylene terephthalate (direct esterification method, alkyd ratio 1.3) in a polyester synthesis kettle, and the esterification temperatur...

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Abstract

The invention discloses a special optical polyester synthesis catalyst. The special optical polyester synthesis catalyst is formed by gamma-A100H and a catalyst promoter by mass of 1:10-9:10 and is a combination of one or multiple of ethylene glycol antimony, antimonous oxide, antimony acetate, tetrabutyl titanate and germanium dioxide. The invention further discloses a preparation method and application of the catalyst. Polyester synthesized by the obtained special optical polyester synthesis catalyst is good in optical performance, low in diethylene glycol and carboxyl-terminated content and applicable to manufacture of optical polyester films.

Description

technical field [0001] The invention relates to the technical field of optical polyester synthesis, in particular to a special catalyst for optical polyester synthesis, its preparation method and application. Background technique [0002] Optical polyester film represented by BOPET is the basic raw material for various optical functional films, optical tapes, optical labels and other high-end products used in the production of liquid crystal displays, and has very strict production technology requirements. In the traditional polyester synthesis process for optical BOPET, a single antimony-based catalyst is generally used. Although the catalyst has excellent catalytic efficiency, the antimony-based catalyst is easily reduced to simple antimony during the reaction process, making the product grayish in color. Optical performance degrades. [0003] In addition, although titanium-based, zirconium-based, aluminum-based and tin-based catalysts have been widely studied and tried t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/84C08G63/86C08G63/85C08G63/183
CPCC08G63/183C08G63/84C08G63/85C08G63/866
Inventor 白永平张福臣黄玉东刘丽姜波李卫东席丹殷晓芬
Owner HARBIN INST OF TECH WUXI RES INST OF NEW MATERIALS
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