Batch polycondensation method and rotating disc reactor therefor

A reactor and polycondensation technology, applied in the field of discontinuous polycondensation and its agitated reactors, can solve problems such as limiting polycondensation efficiency

Inactive Publication Date: 2006-02-01
LURGI ZIMMER GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Disadvantages of these known stirred autoclaves, for example, in the PET batch production process are:
[0017] - limits polycondensation efficiency to a maximum of 7 batches per day, and

Method used

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  • Batch polycondensation method and rotating disc reactor therefor
  • Batch polycondensation method and rotating disc reactor therefor
  • Batch polycondensation method and rotating disc reactor therefor

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0119] Starting from 212 kg of terephthalic acid (TPA) and 90 kg of ethylene glycol (EG), about 245 kg of PET is regularly produced as a melt in a typical plant in a discontinuous esterification and polycondensation process, and processed to obtain pellets, deduction of 2 to a starting loss of 2.5%.

[0120]Precondensation and polycondensation were done in the presence of 180 ppm Sb and 10 ppm P, which had been supplied to the process as antimony triacetate in ethanol solution or as phosphoric acid.

[0121] The temperature and pressure of the precondensation ended at 276°C and 60 mbar; prepolymer sampling showed a TPA conversion of 98.6% and an intrinsic viscosity IV in the range of 0.165 to 0.17 dl / g.

[0122] Within about 15 minutes, the prepolymer was transferred by means of nitrogen pressure into an agitated annular disk autoclave type B according to Table 2. After the previous batch had been granulated and the discharge valve closed, the autoclave was provided to accept ...

example 2

[0137] Similar to the plant in Example 1, in a typical plant starting from 180 kg of terephthalic acid (TPA) and 107 kg of 1,3-propanediol (PDO), approximately 222 kg of polypropylene terephthalate is produced intermittently as a melt (PTT), 85 ppm titanium was added in the form of butyl titanate, and granulation was performed with a yield of about 95%.

[0138] By means of esterification, the precondensation was carried out at a final temperature of 256° C. and a final pressure of 50 mbar. The precondensate showed a TPA conversion of about 99.9% and an intrinsic viscosity IV = about 0.17 dl / g.

[0139] Using speed control and pumping similar to Example 2 for external recirculation of the product, the polycondensation was completed at a vacuum of about 1.0 mbar after 60 minutes and a final vacuum of 0.5 mbar after about 150 minutes. Heating at a temperature of 254°C with constant HTM. The polycondensation was terminated after about 156 minutes, the product temperature rose t...

example 3

[0143] In the esterification transfer and polycondensation process of a typical plant, 250 kg of dimethyl terephthalate (DMT) and 151 kg of 1,4-butanediol (BDO) and 45 ppm Ti as tetraisopropyl titanate were used. 283 kg of polybutylene terephthalate (PBT) were produced and pelletized.

[0144] The precondensation was terminated at 236° C. with a vacuum of 80 mbar. For further polycondensation, the precondensate was supplied to a stirred reactor type A according to Table 2 and polycondensed to a DMT conversion of 99.5% and a solution viscosity IV=0.16 dl / g.

[0145] The main reaction parameters are:

[0146] - polycondensation time is 170 minutes,

[0147] - a constant rotation speed of 6.7 rpm for about 100 minutes, a linear decrease in rotation speed from 6.7 to 1.2 rpm in another hour, and a constant rotation speed of 1.0 rpm thereafter,

[0148] - a vacuum of 1.5 mbar after 60 minutes and a final vacuum of 1.2 mbar after about 150 minutes,

[0149] - product temperature...

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Abstract

The invention relates to a method for the batch production of granules made of polycondensation polymers by pre-condensating an oligomer at 5 to 400 mbar and by means of subsequent polycondensation in a rotating disc reactor and subsequent granulation. In the area of the discharge connection piece, the dragging surface density ranges between 1 and 8m<2> per m<3> in the reactor chamber and is steadily increased at an increasing distance from the discharge area. There is a viscosity gradient within the reactor and between the area that is the remotest from the discharge connection piece and the zone of the discharge connection piece. Thermal reduction of the polymer melt draining off from the reactor is compensated during granulation. The rotating disc reactor comprising a horizontal and longitudinal axis has approximately the form of a simple or double truncated cone. The reactor has rotatable, vertical product dragging surfaces and stationary strippers therebetween.

Description

technical field [0001] The present invention relates to a process for the discontinuous production of granules from polycondensates having a kinetic viscosity in the range of about 100 to 1600 Pa·s at the relevant polycondensation temperature, preheated at a pressure of 5 to 400 mbar (absolute) in any autoclave Polycondensation of a low-molecular oligomer followed by condensation of a precondensate in a stirred reactor having a horizontal axis and a vertical product delivery surface, as well as a discharge port, a vapor port, at least one filling port and at least A recirculation port followed by granulation of the polycondensate. [0002] The invention also relates to a stirred reactor having a horizontal axis and a vertical product delivery surface, as well as at least one filling port, at least one recirculation port, a vapor port, a discharge port and means for heating the reactor The precondensate is polycondensed discontinuously to obtain a polycondensate having a dynam...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/18C08G63/78C08G85/00B01F7/00C08F2/00
CPCB01J2219/00779B01J19/18C08G63/78B01J2219/1943B01J2219/00765B01J2219/1946B01J2219/00094C08G63/785B01J2219/182B01F7/0045B01J2219/00168B01F27/115
Inventor 弗里茨·威廉费迪南德·芬克尔戴
Owner LURGI ZIMMER GMBH
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