Composite catalyst and preparation method of polytrimethylene terephthalate

A technology of polytrimethylene terephthalate and terephthalic acid, which is applied in the chemical industry, can solve the problems that the intrinsic viscosity cannot be satisfied, is not suitable for industrial application, and the reaction is difficult to control, and can reduce the coordination and complexing ability, Non-toxic price, fast response effect

Active Publication Date: 2018-12-14
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Tin-based catalysts have high catalytic activity, but tin-based catalysts have strong neurotoxicity, strong irritation to eyes and skin, are also harmful to the environment, and are likely to cause water pollution; although antimony-based catalysts are cheap, their activity is low, and Antimony-based catalysts often contain arsenic, which makes them more toxic; rare earth catalysts have higher activity, but are expensive and not suitable for industrial applications
Titanium-based catalysts have high catalytic activity, are non-toxic, and are cheap, but because of their high catalytic activity, the reaction is difficult to control, resulting in yellowing of the product, and it is difficult to achieve a satisfactory intrinsic viscosity.

Method used

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  • Composite catalyst and preparation method of polytrimethylene terephthalate
  • Composite catalyst and preparation method of polytrimethylene terephthalate
  • Composite catalyst and preparation method of polytrimethylene terephthalate

Examples

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Comparison scheme
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Embodiment approach

[0038] image 3 It shows the experimental equipment and corresponding process flow for preparing polytrimethylene terephthalate with terephthalic acid and 1,3-propanediol as raw materials. The reactor 1 is equipped with a stirrer 28, and the reactor is provided with a feeding hopper 2 , the measured material is sent into the reactor through the feeding hopper, and the entire reaction process of beating, esterification and polycondensation (initial polycondensation and final polycondensation) is completed in the reactor, and an agitator drive motor 10 is arranged above the reactor. Drive the agitator to work according to the process needs. In a preferred embodiment, the end point of the polycondensation reaction can be judged by the electric current of the stirrer driving motor. This judgment method is simple, convenient and effective, and is convenient for automatic control. The bearing part of the agitator should be provided with a shaft seal and equipped with a shaft seal s...

Embodiment 1

[0054]Embodiment 1: first utilize high-purity nitrogen to displace reactor 2 times, under the protection of high-purity nitrogen, drop into terephthalic acid 2492g (15mol), 1,3-propanediol 1484g (19.5mol), and add composite catalyst tetra-titanate Butyl ester / bis(2,4-di-tert-butylphenyl)pentaerythritol diphosphite, the amount of n-butyl titanate is 2000ppm, the amount of bis(2,4-di-tert-butylphenyl)pentaerythritol diphosphite is 2200ppm. Elevate the temperature to carry out the esterification reaction, the temperature is 235°C, and the pressure is 200kPa. Esterification water is distilled out at the same time. After the theoretical amount of esterification water is removed, the temperature is raised to 250°C, and the absolute pressure is slowly reduced to about 2kPa, and enters the pre-condensation stage for about 30 minutes. After the pre-polycondensation is completed, further vacuumize and enter the final polycondensation stage. The temperature is kept at 250°C, and the pre...

Embodiment 2

[0055] Example 2: First, use high-purity nitrogen to replace the reactor for 2 times, under the protection of high-purity nitrogen, put in 2492g (15mol) of terephthalic acid, 1712g (22.5mol) of 1,3-propanediol, and add the composite catalyst tetra-titanate Butyl ester / bis(2,4,6-tri-tert-butylphenyl)pentaerythritol diphosphite, the amount of n-tetrabutyl titanate is 1500ppm, bis(2,4,6-tri-tert-butylphenyl)pentaerythritol diphosphite Phosphite consumption is 2000ppm. Elevate the temperature to carry out the esterification reaction, the temperature is 235°C, and the pressure is 200kPa. Esterification water is distilled out at the same time. After the theoretical amount of esterification water is removed, the temperature is raised to 250°C, and the absolute pressure is slowly reduced to about 2kPa, and enters the pre-condensation stage for about 30 minutes. After the pre-polycondensation is completed, further vacuumize and enter the final polycondensation stage. The temperature i...

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Abstract

The invention relates to a composite catalyst suitable for preparation of polytrimethylene terephthalate, and a method for preparing polytrimethylene terephthalate by adopting the composite catalyst. The composite catalyst comprises tetra-n-butyl titanate and phosphite according to a preferable mass ratio of 0.6-1.15. Polytrimethylene terephthalate is prepared from terephthalic acid and 1,3-propylene glycol through an esterification reaction and a condensation polymerization reaction with the composite catalyst as a catalyst. Phosphate is added to the catalyst, so the catalysis activity of tetra-n-butyl titanate on the degradation reaction of PTT (polytrimethylene terephthalate) is effectively reduced, and the catalysis selectivity is improved; the composite catalyst used in the preparation of the PTT has the advantages of small amount, low cost, fast reaction speed, mild reaction conditions, and controllable reaction; and the characteristic viscosity of the PTT reaches 0.85-1.07dL / g, and the PTT is white in color.

Description

technical field [0001] The invention relates to a composite catalyst suitable for preparing polytrimethylene terephthalate, and also relates to a preparation method of polytrimethylene terephthalate using the composite catalyst, which belongs to the technical field of chemical industry. Background technique [0002] Polytrimethylene terephthalate (PTT) is a relatively new semi-crystalline thermoplastic polyester with unique properties compared to polyethylene terephthalate and polybutylene terephthalate. The helical structure has excellent performance, and has the softness of nylon, the bulkiness of acrylic fiber and the stain resistance of polyester, plus its inherent elasticity, moderate glass transition temperature and good processing performance. The excellent properties of the fiber are integrated into one. At present, it has become one of the most popular new polymer materials in the world. It is not only used in the field of synthetic fibers, but also develops rapidl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/183C08G63/85C08G63/87
Inventor 周华堂顾爱军许贤文吕陈秋朱文祥周雪松张宇航陈久波李春成
Owner BC P INC CHINA NAT PETROLEUM CORP
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