Polyester with low oligomer content and preparation method of polyester

An oligomer and content technology, applied in the field of polymer materials, can solve the problems of reducing the oligomer content in polyester, dyeing uniformity interference, etc., to reduce the oligomer content, low oligomer content, quality high effect

Active Publication Date: 2019-02-22
DONGHUA UNIV
View PDF8 Cites 14 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A method like this adds additional processing procedures, and is not suitable for polyester products such as fibers, because it is difficult for surfactants to stably shield the oligomers inside the product during the process of fabric dyeing and finishing
The patent US7208456A aimed at the problem of oligomer deposition in the fiber dyeing process, developed a composition of nonionic surfactant and anionic surfactant, and prevented the oligomer from being dispersed in the dyeing bath by realizing stable dispersion of the oligomer Crystal deposition on the surface of the fiber avoids its interference to the uniformity of dyeing, but none of the above methods can reduce the content of oligomers in polyester from the source

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Polyester with low oligomer content and preparation method of polyester
  • Polyester with low oligomer content and preparation method of polyester
  • Polyester with low oligomer content and preparation method of polyester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A preparation method of polyester with low oligomer content, the steps are as follows:

[0049] (1) Add dimethyl terephthalate (291g), 1,4-butanediol (189g) and tetrabutyl titanate (0.7g) into a 2L polymerization reactor, and use vacuum / nitrogen circulation for 3 times as much as possible It is possible to exclude the residual air in the reaction kettle, and apply a slow nitrogen flow to the reaction system, then heat to 125°C to distill the by-product methanol, and gradually raise the temperature to 190°C to maintain the esterification reaction until the amount of methanol evaporated reaches 95% of the theoretical value;

[0050] (2) Vacuumize the reaction system to implement the first-stage polycondensation reaction, the vacuum degree is 1KPa, the set reaction temperature is 220°C, and the reaction time is 0.5h;

[0051] (3) Apply a high vacuum to the reaction system (vacuum degree is 90Pa), and increase the reaction temperature to 260°C to carry out the second stage ...

Embodiment 2

[0062] A preparation method of polyester with low oligomer content, the preparation steps are basically the same as in Example 1, the difference is that in step (5), chain extender hexamethylene diisocyanate (15g) is added to carry out chain extension reaction .

[0063] The intrinsic viscosity and oligomer content of the finally obtained polyester are shown in Table 1.

Embodiment 3

[0065] A preparation method of polyester with low oligomer content, the steps are as follows:

[0066] (1) Add dimethyl terephthalate (310.7g), 1,4-butanediol (259.5g), tetrabutyl titanate (3.3g) and antioxidant 1010 (6.0g) into a 2L polymerization reactor ), use vacuum / nitrogen circulation 3 times to remove residual air in the reactor as much as possible, and apply a slow nitrogen flow to the reaction system, then heat to 125°C to distill out the by-product methanol, and gradually raise the temperature to 190°C to maintain the esterification reaction until the methanol Evaporated amount reaches 95% of theoretical value;

[0067] (2) Vacuumize the reaction system to implement the first-stage polycondensation reaction, the vacuum degree is 1KPa, the set reaction temperature is 220°C, and the reaction time is 0.5h;

[0068] (3) Apply a high vacuum to the reaction system (vacuum degree is 90Pa), and increase the reaction temperature to 260°C to carry out the second stage polycon...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a polyester with low oligomer content and a preparation method of the polyester. The method comprises the following steps: carrying out an esterification reaction and a first-stage condensation polymerization reaction on M and dihydric alcohol in the presence of a catalyst A; carrying out a second-stage condensation polymerization reaction; adding a catalyst B and carryingout a third-stage condensation polymerization reaction; and finally, adding a chain extender for carrying out a chain extension reaction, thereby obtaining the polyester with low oligomer content, wherein M is dicarboxylic acid or binary alkyl carboxylate; the catalyst A is a titanium catalyst, an antimony catalyst or metal acetate, the catalyst B is more than one of aluminum isopropoxide, dibutyl tin oxide, monobutyltin oxide, stannous octoate and stannous 2-ethyl caproate, and the oligomer content in the prepared polyester is less than 1.5wt%. The method disclosed by the invention is simplein operation, and the prepared product is low in oligomer content and has excellent popularization value.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and relates to a polyester with low oligomer content and a preparation method thereof. Background technique [0002] Polyester, including aromatic polyester, semi-aromatic polyester and aliphatic polyester, is an extremely important polymer material. Due to different chemical structures, different types of polyesters have different excellent properties, so polyesters can be used in the production of various products such as fibers, engineering plastics and films. [0003] Cyclic oligomers may be produced during the production and processing of polyester, such as chip drying, spinning and dyeing. The content and types of cyclic oligomers contained in different polyester products are slightly different. Among them, cyclic oligomers in ethylene terephthalate (PET) account for about 2 to 3.2 wt%, and cyclic trimers account for the largest proportion, accounting for about 75 wt% of the tot...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C08G63/183C08G63/78
CPCC08G63/183C08G63/78
Inventor 乌婧王华平吉鹏陈敬樱王晶晶祁捷斐
Owner DONGHUA UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap