Quaternary ammonium salt catalyst, application thereof and isosorbide modified polyester

A technology of modified polyester and quaternary ammonium salt, which is applied in the field of chemical preparation, can solve problems such as easy deposition of hydrolyzed products to block pipelines, inconvenient production, and reduced catalytic efficiency, so as to reduce the probability of side reactions in the system, reduce the loss of raw materials, and reduce the Effect of polycondensation reaction temperature

Active Publication Date: 2020-06-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, bismuth-based catalysts and tin-based catalysts have certain defects. Due to their own characteristics, bismuth-based catalysts and tin-based catalysts can easily interact with water generated in the reaction system to form hydrolyzed products, which not only reduces catalytic efficiency, but also easily deposits and clogs the hydrolyzed products. pipelines, causing inconvenience to production

Method used

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  • Quaternary ammonium salt catalyst, application thereof and isosorbide modified polyester
  • Quaternary ammonium salt catalyst, application thereof and isosorbide modified polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The preparation of embodiment 1 quaternary ammonium salt catalyst

[0039] Catalyst A Preparation

[0040] The preparation of described catalyst A can operate according to the following steps:

[0041] First, add 82.8 g of octyltrimethylammonium chloride and 200 mL of absolute ethanol into a 500 mL three-necked flask and stir evenly. 31.5gBiCl 3 with 13.1gTiCl 4 (BiCl 3 with TiCl 4 The molar ratio is about 2:1) was dissolved in 10mL of ethanol, and dropped into the three-necked flask under stirring conditions. After no gas is released, it is aged at room temperature for 12 hours. A solution of Catalyst A in ethanol was obtained by filtration.

[0042] Catalyst B preparation

[0043] Catalyst B was prepared in the same way as Catalyst A except that the BiCl 3 with SnCl 4 The molar ratio is about 1:1.

[0044] Catalyst C preparation

[0045] Catalyst C was prepared in the same way as Catalyst A except that the BiCl 3 with SnCl 4 The molar ratio is about 1:2....

Embodiment 2

[0052] The preparation of embodiment 2 isosorbide modified polyester

[0053] Preparation of polyester sample 1#

[0054] In 1L polyester reactor, add 168.13g terephthalic acid, 67.65g ethylene glycol and 16.08g isosorbide (the molar ratio of terephthalic acid and isosorbide and ethylene glycol total molar weight 1:1.2, ethylene glycol Alcohol to isosorbide molar ratio 10:1) and 0.1mL ethanol solution of catalyst A (ie solution 1#), replaced with inert gas three times. Heat and stir under normal pressure, raise the temperature to 180°C, carry out esterification reaction, fractionate the by-product water in time, after 2 hours, quickly raise the temperature to 210°C, carry out polycondensation reaction under 5mmHg vacuum degree, and obtain isosorbide after 60 minutes The modified polyester is referred to as polyester sample 1#.

[0055] Prepare polyester samples 2#~6#, the preparation method of polyester samples 2#~6# is carried out according to the preparation method of poly...

Embodiment 3

[0057] Embodiment 3 intrinsic viscosity (IV) measurement

[0058] Dissolve polyester samples 1# to 10# in o-chlorophenol (OCP) at 150°C, respectively. The polymer concentration was adjusted to 0.12%. The measurement was performed at 35° C. in a thermostatic bath using an Ubbelohde viscometer.

[0059] The test results are shown in Table 1, Table 2 and Table 3.

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PUM

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Abstract

The invention discloses a quaternary ammonium salt catalyst, which is prepared by the following steps: adding metal chloride into a solution containing quaternary ammonium salt, aging, and filtering to obtain a solution containing the quaternary ammonium salt catalyst. The metal complex modified quaternary ammonium salt designed and synthesized by the invention can effectively shorten the esterification reaction time, reduce the polycondensation reaction temperature, reduce the raw material loss and reduce the system side reaction occurrence probability in the preparation process of modified polyester. The isosorbide modified polyester prepared by utilizing the catalyst is good in heat resistance, high in intrinsic viscosity and excellent in chromaticity, and an efficient way is provided for efficient preparation of the modified polyester.

Description

technical field [0001] The application relates to a quaternary ammonium salt catalyst and its application and isosorbide-modified polyester, belonging to the field of chemical preparation. Background technique [0002] Polyester refers to a polymer compound containing a large number of ester bonds on the main chain of a macromolecule, which is produced by direct esterification or transesterification of a dibasic (or polybasic) acid (or its ester) and a dibasic (or polybasic) alcohol. According to dibasic acid and dibasic alcohol, various polyesters can be synthesized. [0003] Catalyst is an important part of polyester production process, and the research on catalyst has always been one of the important contents of polyester industrial technology development. Foreign scholars have conducted in-depth research on the mechanism of polycondensation reaction, the catalytic effect of metal catalysts, the types of catalysts, and have never stopped exploring new catalysts. There a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/87C08G63/85C08G63/672C08G63/78
CPCC08G63/672C08G63/78C08G63/85C08G63/87
Inventor 郑玺徐杰高进孙颖杜文强石松苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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