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Preparation methods of high-viscosity polytrimethylene terephthalate and copolyester thereof

A kind of technology of polytrimethylene terephthalate, trimethylene phthalate

Inactive Publication Date: 2016-06-01
ZHANGJIAGANG GLORY CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many researches on this technology at home and abroad, but there are few high-viscosity PTT polymers in actual industrial production.
Foreign polymerization technology is mainly a high-temperature three-pot process. The external circulation esterification tank has a high alkyd molar ratio, difficult to control esterification, high energy consumption, and many by-products. During the pre-shrinking process, the reactor needs to rely on dihydric alcohol Steam is used to provide power and energy consumption is high. Due to the sensitivity of PTT products to heat, the color and hue of the obtained products have a great influence. However, no matter the long process in China, the process takes a long time. In order to obtain high-viscosity PTT polymers, there are many sets of equipment and catalysts. High consumption, especially with the continuous expansion of the application field of PTT products, a single PTT polyester cannot meet the demand, and it needs to be copolymerized and modified, so the above-mentioned domestic and foreign reaction processes are limited

Method used

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  • Preparation methods of high-viscosity polytrimethylene terephthalate and copolyester thereof
  • Preparation methods of high-viscosity polytrimethylene terephthalate and copolyester thereof

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preparation example Construction

[0030] On the one hand, the invention provides a kind of preparation method of high-viscosity polytrimethylene terephthalate, figure 1 A schematic flow chart of the preparation method is shown. Such as figure 1 Shown, this preparation method comprises the steps:

[0031] Mixing step: prepare a slurry made of terephthalic acid and 1,3-propanediol at 40-60°C under normal pressure;

[0032] Primary esterification step: the slurry is continuously transported to the first esterification tank for primary esterification to obtain the first esterified product;

[0033] Secondary esterification step: transporting the first esterified product into a second esterification tank for secondary esterification to obtain a second esterified product;

[0034] Pre-condensation step: the second esterified product is continuously transported into a pre-condensation tank for polycondensation, and small molecules are removed to obtain a polytrimethylene terephthalate prepolymer;

[0035] Final p...

Embodiment 1

[0046] Prepare terephthalic acid and 1,3-propanediol in a molar ratio of 1:1.4 to form a slurry, and then continuously send it to the first esterification tank at a flow rate of 475kg / h for an esterification reaction at an absolute pressure of 140kPa At a temperature of 240° C., 0.1 kg / h of tetrabutyl titanate was continuously added and kept for 2 hours to obtain the first esterified product. Then the first esterification product enters the second esterification tank for secondary esterification reaction, and stays for 1 hour at an absolute pressure of 80 kPa and a temperature of 250° C. to obtain the second esterification product. Then the second esterified product is continuously sent into the pre-condensation tank for polycondensation reaction, and 0.1kg / h tetrabutyl titanate is added at the same time, and the temperature is raised to 260°C, and the vacuum degree is 2kPa, and the by-product is released for 30 minutes. obtained prepolymer. Finally, the prepolymer enters the...

Embodiment 2

[0048] Add 350kg / h terephthalic acid, 350kg / h succinic acid and 800kg / h 1,3-propanediol into the slurry tank continuously to make a slurry, and then continuously send it to the first esterification tank for an esterification reaction , at an absolute pressure of 60kPa and a temperature of 240°C, add 0.4kg / h tetrabutyl titanate, stay for 4h, remove by-product water, and obtain the first esterified product. Then the first esterified product enters the second esterification tank for the second esterification reaction. Under the absolute pressure of 40kPa and the temperature of 240°C, it stays for 2 hours to remove by-product water to obtain the second esterified product. Then the second esterified product enters the pre-condensation tank for polycondensation reaction, and at the same time, 0.1kg / h tetrabutyl titanate is added, and the temperature is raised to 260°C, and the vacuum degree is 3kPa, and it stays for 120min to remove by-products and obtain pre-polymerization things. ...

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Abstract

The invention discloses a preparation method of high-viscosity polytrimethylene terephthalate. The preparation method of high-viscosity polytrimethylene terephthalate comprises the following steps: mixing: preparing polyterephthalic acid and 1,3-propanediol into a slurry under atmospheric pressure; primary esterification: continuously delivering the slurry into a first esterification kettle, and carrying out primary esterification reaction to obtain a first esterification product; secondary esterification: delivering the first esterification product into a second esterification kettle, and carrying out secondary esterification reaction to obtain a second esterification product; pre-polycondensation: continuously delivering the second esterification product into a pre-polycondensation kettle, and carrying out polycondensation to remove small molecules, thereby obtaining a polytrimethylene terephthalate prepolymer; and final polycondensation: continuously delivering the polytrimethylene terephthalate prepolymer into a final polycondensation kettle, and carrying out condensation polymerization to remove small molecules, thereby obtaining the polytrimethylene terephthalate high polymer. The invention also discloses a preparation method of the high-viscosity polytrimethylene terephthalate copolyester. The products have the advantages of high inherent viscosity and high quality.

Description

technical field [0001] The invention relates to the technical field of polymer material synthesis, in particular to a preparation method of high-viscosity polytrimethylene terephthalate (PTT) and its copolyester. Background technique [0002] Polytrimethylene terephthalate (PTT) is a new type of thermoplastic polyester with broad development prospects successfully developed in the 1990s, and polyethylene terephthalate (PET) and polybutylene terephthalate Esters (PBT) are the same polymer series as high molecular aromatics. However, it has better processing performance, electrical performance, mechanical performance and dimensional stability than PET and PBT. PTT maintains the excellent wrinkle resistance and chemical resistance of PET, and at the same time has the softness of nylon and the bulkiness of acrylic fiber due to its unique spiral structure. Its good comprehensive properties have been rapidly developed and applied in carpets, textile fibers, monofilaments, films ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/78
CPCC08G63/183C08G63/78
Inventor 张怀立韩冰
Owner ZHANGJIAGANG GLORY CHEM IND CO LTD
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