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Method for preparing copolyester

A copolyester and esterification technology, which is applied in the field of copolyester preparation, can solve the problems of blocking production equipment pipelines, difficult control and adjustment, and decreased catalyst activity.

Active Publication Date: 2015-02-11
SHINKONG SYNTHETIC FIBERS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Those who use titanium alcohol salts, such as U.S. Patent No. 5,681,918 and No. 5,744,571, have the disadvantages of being sensitive to moisture and easily hydrolyzed, resulting in a decrease in catalyst activity and prolonging the polymerization time. In addition, it may also be reduced to the form of inorganic particles and affect Transparency, even blockage of production equipment pipelines, resulting in the need to suspend operation of production equipment for cleaning
[0004] Those who use inorganic titanium oxides, such as U.S. Patent No. 6,559,272, have the disadvantage that the solubility of inorganic titanium oxides in the reaction system is insufficient. Oxides can also cause turbidity to increase, thereby affecting the transparency of ester particles. Therefore, the production conditions of using inorganic titanium oxide as a catalyst are not easy to control and adjust

Method used

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  • Method for preparing copolyester
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preparation example Construction

[0030] The preparation method of the copolyester of the present invention includes two steps. The first step is an esterification step. The reaction temperature ranges from 230 to 260°C, the preferred range is between 240 to 260°C, and the optimal range is between Between 245~255℃. The esterification step can adopt normal pressure or pressurized mode, and the optimum pressure range for pressurized esterification is 0.1~3.0Kg / cm 2 . The esterification reaction time is controlled within 100-360 minutes, preferably 270-360 minutes. Since the esterification rate is affected by factors such as temperature, pressure, and alkyd ratio, it must be adjusted according to actual conditions.

[0031] The second stage is the polymerization step, the reaction temperature range is between 260-290°C, the preferred range is between 265-285°C, and the optimal range is between 270-280°C. The polymerization step must be performed under vacuum with a vacuum degree of 0.1-10 torr to remove by-products...

Embodiment 2

[0048] Take 255 g of terephthalic acid, 97.6 g of ethylene glycol, and 184.4 g of 1,4 cyclohexanedimethanol, and carry out the first stage esterification step in the reactor. The temperature of the esterification step was raised to 250°C, and the esterification was carried out for 5.5 hours under normal pressure. After the esterification step is completed, 5.1 mg of phosphoric acid, 60 mg of cobalt acetate, and 120 mg of titanium-phosphorus co-catalyst are added sequentially, and then the second stage polymerization step is performed. Gradually vacuumize and reduce pressure to 1torr, the upper limit of the reaction temperature is 280℃, and the reaction time is when the stirrer reaches 100rpm / torque=8 as the end of polymerization.

Embodiment 3

[0050] The preparation method of Example 2 differs from Example 2 in that the amount of phosphoric acid added is 15 mg, and the rest are the same.

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Abstract

The invention discloses a method for preparing copolyester, comprising the steps: using 100 mol% at least one dibasic acid and 100-150 mol% at least one dihydric alcohol as monomer materials, and obtaining oligomer after esterification reaction; and conducting polymerization reaction for the oligomer with a titanium phosphorus common catalytic agent so as to obtain the copolyester. Therefore, the prepared copolyester has characteristics of good hue, improved brightness and stable production.

Description

Technical field [0001] The invention discloses a method for preparing a copolyester containing at least one dibasic acid and at least one dihydric alcohol by using a titanium-phosphorus co-catalyst with good hydrolysis resistance and rapid reaction. Background technique [0002] Polymethyl terephthalate (hereinafter referred to as PET) has become a commonly used plastic widely used in human life since its first patent was published in 1941. Its excellent physical properties enable its applications to cover man-made fibers, PET bottles, and films. , Film, engineering plastics, etc. In common technology, various forms of dibasic acid or glycol monomers are often added to modify PET to improve its processability or impart special properties. This is commonly known as PET copolyester. Traditionally, PET or PET copolyesters are polymerized using antimony catalysts, but the hue of ester particles prepared using antimony catalysts is dark, which cannot meet the requirements of applicat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/85
Inventor 赖重光沈淑贞黄柏豪陈丰官
Owner SHINKONG SYNTHETIC FIBERS
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