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Preparation method of PTT-based (polytrimethylene terephthalate-based) low-melting-point copolyester

A low melting point, copolyester technology, applied in the field of polyester preparation, can solve the problems of copolycondensation catalysis and thermal degradation control, low thermal stability of the melt, low intrinsic viscosity of the product, etc., and achieve excellent thermal stability and The effect of hue, easy control of reaction process, and high intrinsic viscosity

Active Publication Date: 2019-04-05
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The present invention proposes a method for preparing PTT-based low-melting copolyesters, which can solve the problem of low intrinsic viscosity and low melting point of the product due to the difficulty of co-polycondensation catalysis and thermal degradation control in the current preparation process of PTT-based low-melting copolyesters. Problems of low bulk thermal stability and poor spinnability when combined with conventional PET

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] At first carry out the preparation of the 1,3-propanediol solution of titanium series catalyst I and titanium series catalyst II, it comprises the steps:

[0049] a) Add sodium hydroxide to 1,3-propanediol, control the temperature at 105°C, and keep stirring until the system is a uniform and clear solution. The molar ratio of sodium hydroxide to 1,3-propanediol is 1:50.

[0050] b) Add cobalt acetate to 1,3-propanediol, control the temperature at 130°C, and keep stirring until the system is a uniform and clear dark purple solution, and the molar ratio of cobalt acetate to 1,3-propanediol is 1:50.

[0051] c) Add tetra-n-butyl titanate to the clear solution prepared in step a) under the condition of dry nitrogen protection, the molar ratio of tetra-n-butyl titanate to sodium hydroxide contained in the clear solution is 1: 1.02, and the reaction is controlled The temperature is 130°C, and the stirring speed is 1500 rpm. During the reaction, 1,3-propanediol is refluxed, an...

Embodiment 2

[0075] At first carry out the preparation of the 1,3-propanediol solution of titanium series catalyst I and titanium series catalyst II, it comprises the steps:

[0076] a) Add potassium hydroxide to 1,3-propanediol, control the temperature at 120°C, and keep stirring until the system is a uniform and clear solution. The molar ratio of potassium hydroxide to 1,3-propanediol is 1:30.

[0077] b) Add cobalt acetate to 1,3-propanediol, control the temperature at 150°C, and keep stirring until the system is a uniform and clear deep purple solution, and the molar ratio of cobalt acetate to 1,3-propanediol is 1:30.

[0078] c) Add tetraisopropyl titanate to the clarified solution prepared in step a) under the condition of dry nitrogen protection, the molar ratio of tetraisopropyl titanate to potassium hydroxide contained in the clarified solution is 1: 1.03, and the reaction is controlled The temperature is 120°C, the stirring speed is 1500 rpm, during the reaction, 1,3-propanediol ...

Embodiment 3

[0102] At first carry out the preparation of the 1,3-propanediol solution of titanium series catalyst I and titanium series catalyst II, it comprises the steps:

[0103] a) Add sodium hydroxide to 1,3-propanediol, control the temperature at 115°C, and keep stirring until the system is a uniform and clear solution. The molar ratio of sodium hydroxide to 1,3-propanediol is 1:60.

[0104] b) Add cobalt acetate to 1,3-propanediol, control the temperature at 135°C, and keep stirring until the system is a uniform and clear deep purple solution, and the molar ratio of cobalt acetate to 1,3-propanediol is 1:60.

[0105] c) Add tetraisopropyl titanate to the clarified solution prepared in step a) under the condition of dry nitrogen protection, the molar ratio of tetraisopropyl titanate to sodium hydroxide contained in the clarified solution is 1: 1.03, and the reaction is controlled The temperature is 120°C, the stirring speed is 1500 rpm, during the reaction, 1,3-propanediol is reflux...

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Abstract

The invention provides a preparation method of a PTT-based (polytrimethylene terephthalate-based) low-melting-point copolyester. The PTT-based low-melting-point copolyester is prepared by subjecting terephthalic acid, 1,3-propanediol, 1,6-adipic acid, a diol solution of a titanium-containing catalyst and a stabilizer to esterification before copolycondensation. The catalyst with double-titanium diol titanium structure is synthesized through unique design and has good stability and diol solubility; the catalyst may efficiently catalyze esterification and copolycondensation, is highly adaptive to copolycondensation catalysis under different ratios, and helps evidently solve the problem that an existing titanium-containing catalyst can accelerate thermal degradation of the copolyester. The finished product prepared via the preparation method of the PTT-based low-melting-point copolyester has a melting point of 110.7-209.3 DEG C and high characteristic viscosity (0.975-1.312 dl / g), is wellcombine-spinnable with conventional PET (polyethylene terephthalate), and has good color and good melt thermal stability.

Description

technical field [0001] The invention relates to the technical field of polyester preparation, in particular to a preparation method of PTT-based low-melting copolyester. Background technique [0002] Low-melting point copolyester is an important raw material for the production of hot-melt adhesive fibers and hot-melt adhesives, and is widely used in the fields of textiles, clothing, medicine and health. Low-melting point copolyesters have various molecular structures, generally based on common aromatic polyesters PET (polyethylene phthalate), PBT (polybutylene phthalate), PTT (polytrimethylene phthalate) Based on the structural monomer, asymmetric bifunctional structure (such as: isophthalic acid, 2-methyl-1,3-propanediol, etc.) or long linear and functional group structure (such as: 1,6 - adipic acid, polyethylene glycol, etc.) to prepare. Among them, compared with PET-based or PBT-based low-melting-point copolyesters, PTT-based low-melting-point copolyesters have a struc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/78C08G63/85
CPCC08G63/183C08G63/78C08G63/85
Inventor 王少博王华平岳献阳黄鑫王明环于保康刘守作
Owner ZHONGYUAN ENGINEERING COLLEGE
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