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Preparation method for antimony-free polyester for bottles

A technology for bottles and polyester, applied in the field of preparation of polyethylene terephthalate (PET) materials, which can solve the problems of antimony element precipitation, high acetaldehyde content, obvious side reactions, etc., to reduce production capacity Consumption, shorten the process flow, save the effect of solid phase polycondensation

Active Publication Date: 2014-09-03
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] On the other hand, antimony (Sb)-based catalysts are usually used in the polycondensation process of PET, and a small amount of antimony element will be precipitated in the process of making containers to store food and beverages, which poses a threat to human health
Titanium-based catalysts are the most promising environmentally friendly catalysts to replace antimony-based catalysts. A lot of research work has been done at home and abroad, but the application effect and promotion are still not ideal. The main reason is that titanium-based catalysts have higher catalytic activity and catalytic selectivity. Poor, side reactions are obvious, and the melt color is yellowish. The current research and development work is mainly focused on the improvement of the titanium-based catalyst itself, and there is no report on solving the yellowish color of the titanium-based catalyst polyester from the transformation of the polycondensation reactor.
[0004] Due to the one-step melt polycondensation method to prepare PET high-viscosity melt, it is easy to produce problems such as yellowish hue and high acetaldehyde content, and titanium-based catalysts will aggravate the yellowish hue and high acetaldehyde content of PET high-viscosity melt due to high catalytic activity and poor selectivity. Therefore, it is generally believed that the one-step melt polycondensation method cannot use titanium-based catalysts to prepare PET high-viscosity melts.

Method used

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  • Preparation method for antimony-free polyester for bottles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The molar ratio of PTA to EG is 1:1.3, add 2.0% IPA and 0.8% DEG by weight of PTA, add Ti-Mg catalyst equivalent to 10 ppm of PTA weight in terms of titanium element, and 1.8 ppm of blue toner, Carry out esterification reaction, the temperature of the esterification reaction is 240~250°C, the relative pressure is 0~0.2MPa, the by-product water is released, and ethylene terephthalate (BHET) and its oligomers are generated; when the esterification conversion rate reaches After 97%, vacuumize for polycondensation, add 9ppm of phosphoric acid in terms of phosphorus and 30ppm of antioxidant 1010, polycondensation temperature 255~265℃, absolute pressure 0.1~20kPa; when the intrinsic viscosity reaches about 0.35dL / g, the PET base The melt is distributed to the upper ends of the vertically downward falling film tubes in the liquid phase thickening reactor, and then slides down by gravity to form a film on the outer wall of the tube for polycondensation reaction. The falling film...

Embodiment 2

[0028] The ratio of raw materials and esterification are the same as in Example 1; when the conversion rate of esterification reaches 97%, vacuumize for polycondensation, the polycondensation temperature is 250~260°C, and the absolute pressure is 0.1~20kPa; when the intrinsic viscosity reaches about 0.25dL / g, The PET basic melt is transported to the first liquid phase thickening reactor for falling film reaction. The falling film reaction temperature is 255~265°C, the absolute pressure is 50~200Pa, and the PET basic melt flow rate of each falling film tube is 20kg / hour. The intrinsic viscosity of the melt discharged from the first liquid phase thickening reactor is about 0.50dL / g, and then transported to the second liquid phase thickening reactor for falling film reaction. The falling film reaction temperature is 255~265°C and the absolute pressure is 25~ 150Pa, the basic melt flow rate of PET in each falling film tube is 15kg / hour, and the melt will converge to the bottom of t...

Embodiment 3

[0030] The catalyst was changed to C-94 (Acordis product of Germany), and the addition amount was equivalent to 10 ppm of PTA weight in terms of titanium element, and the rest were the same as in Example 1.

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Abstract

The invention discloses a preparation method for antimony-free polyethylene glycol terephthalate (PET) for bottles. An esterification, fusion polycondensation and liquid-phase viscosity-increasing one-step method is used for preparing the PET resin for bottles, and the PET resin has the characteristic viscosity of 0.70-1.00 dL / g. A polycondensation catalyst is a titanium-serial catalyst. The PET resin for bottles is high in safety to human body, solid-phase polycondensation and other processes are saved, equipment investment is reduced, the process flow is shortened, and production energy consumption is reduced.

Description

technical field [0001] The invention belongs to the technical field of polyester production for bottles, and in particular relates to a preparation method of heavy metal antimony-free polyethylene terephthalate (PET) material. Background technique [0002] Polyester, especially polyethylene terephthalate (PET), is widely used in the field of food packaging because of its excellent physical and mechanical properties, low price, and recyclable recycling. At present, the preparation of PET resin for bottles generally adopts a two-step method, that is, through esterification and melt polycondensation (generally including pre-condensation and final polycondensation) to obtain a PET resin with an intrinsic viscosity of 0.60~0.65dL / g, and then through solidification. Phase polycondensation (temperature 180-230°C) produces PET resin for bottles with an intrinsic viscosity of 0.70-0.90 dL / g. Another function of solid-state polycondensation is to reduce the acetaldehyde content in PET...

Claims

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Application Information

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IPC IPC(8): C08G63/183C08G63/85
Inventor 陈文兴张先明王秀华
Owner ZHEJIANG SCI-TECH UNIV
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