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Preparation method of poly terephthalic acid-2,3-butylene terephthalate

A technology of polyterephthalic acid and terephthalic acid, which is applied in the synthesis of polyester and the field of polyterephthalic acid-2, can solve problems such as the preparation process that has not been introduced in detail, and achieve rich product types and excellent performance. Effect

Inactive Publication Date: 2012-05-16
SHANGHAI JUYOU CHEM ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Recently, the patent CN101525414A applied by Toray Fiber Research Institute (China) Co., Ltd., a branch of Toray Corporation of Japan in China, introduced poly(2,3-butylene terephthalate) products, but did not introduce its preparation in detail craft
However, there are very few studies on this in China, and there are few such patents and literature reports.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 332g (2mol) of terephthalic acid and 234g (2.6mol) of 2,3-butanediol into the reactor, and add 3.396g of tetrabutyl titanate at a gauge pressure of 0.5MPa and a temperature of 220°C , the by-product water is removed, and when the esterification rate reaches 98%, the esterification is terminated; 0.1132g of ethylene glycol antimony is added, and the temperature is raised to 275°C, and the pre-condensation reaction is carried out under the condition of a vacuum of 0.1kPa. The pre-condensation time After 60 minutes, the by-products were removed; then the final polycondensation reaction was carried out under high vacuum, the vacuum degree was 50 Pa, and the reaction time was 180 minutes to obtain poly(2,3-butylene terephthalate) macromolecular compounds, which were tested by the national standard of polyester Method (GB / T-14190-1993) measures its intrinsic viscosity as (IV) 0.60dl / g.

Embodiment 2

[0025] Add 298.8g (1.8mol) of terephthalic acid and 243g (2.7mol) of 2,3-butanediol into the reactor, and add 2.167g of tetratitanate at a gauge pressure of 0.3MPa and a temperature of 210°C Butyl ester, by-product water, when the esterification rate reaches 97%, end the esterification; add 1.0836g ethylene glycol antimony and 0.3612g trimethyl phosphate, and raise the temperature to 285 ° C, under the condition of a vacuum of 0.15kPa , carry out pre-condensation reaction, the pre-condensation time is 80min, and the by-product is removed; then the final polycondensation reaction is carried out under high vacuum, the vacuum degree is 40Pa, and the reaction time is 200min to obtain poly-2,3-butylene terephthalate. Molecular compound, its intrinsic viscosity measured by polyester national standard test method (GB / T-14190-1993) is (IV) 0.64dl / g.

Embodiment 3

[0027] Add 388g (2mol) of dimethyl terephthalate and 360g (4mol) of 2,3-butanediol into the reactor, and add 3.74g of tetratitanate at a gauge pressure of 0.1MPa and a temperature of 180°C Butyl ester, the by-product water is removed, and when the esterification rate reaches 98.5%, the esterification is terminated; 2.244g of antimony trioxide is added, and the temperature is raised to 280°C, and the vacuum is 0.12kPa, and the pre-condensation reaction is carried out. The polycondensation time is 30 minutes, and the by-products are removed; then the final polycondensation reaction is carried out under high vacuum, the vacuum degree is 30 Pa, and the reaction time is 160 minutes to obtain poly(2,3-butylene terephthalate) macromolecular compounds. Standard test method (GB / T-14190-1993) measures its intrinsic viscosity as (IV) 0.72dl / g.

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PUM

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Abstract

The invention discloses a preparation method of poly terephthalic acid-2,3-butylene terephthalate. The invention is characterized by being realized through the following method: preparing an esterification compound terephthalic acid-2,3-butylene terephthalate by an esterification reaction or an ester interchange reaction between terephthalic acid or a derivative thereof and 2,3-butylene glycol; preparing poly terephthalic acid-2,3-butylene terephthalate macromolecular compound by a condensation polymerization reaction. The 2,3-butylene glycol can be prepared by a biological method or a chemical method. The polyester product prepared by the invention has high characteristic viscosity, is prepared by a simple method, enriches product variety of differentiation polyester family and provides guarantee for structural adjustment and upgrading of polyester industry of our country.

Description

technical field [0001] The invention relates to a method for synthesizing polyester, belonging to the technical field of polymer material synthesis, in particular to a method for preparing poly-2,3-butylene terephthalate. Background technique [0002] Polyester is widely used in fiber, resin, film and other fields due to its good mechanical properties and molding processability. It is one of the most important and largest synthetic materials in the world. [0003] With the improvement of people's living standards, more and more attention has been paid to resources and living environment. Since the synthetic raw materials of polyester are almost all derived from non-renewable resource petroleum, it is an urgent problem to be solved to develop materials that can use renewable raw materials and be environmentally friendly. [0004] Especially the rapid development of my country's polyester industry, in 2010, my country's polyester production reached more than 29 million tons, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/87C08G63/86C08G63/85
Inventor 汪少朋韩冰甘胜华
Owner SHANGHAI JUYOU CHEM ENG
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