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A kind of polyester with low oligomer content and preparation method thereof

A technology of oligomer content, applied in the field of polymer materials, can solve the problems of reducing oligomer content in polyester, dyeing uniformity interference, etc., to achieve low oligomer content, low oligomer content, good The effect of applying the foreground

Active Publication Date: 2020-04-17
DONGHUA UNIV
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  • 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
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  • A kind of polyester with low oligomer content and preparation method thereof
  • A kind of polyester with low oligomer content and preparation method thereof
  • A kind of polyester with low oligomer content and preparation method thereof

Examples

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Effect test

Embodiment 1

[0048] A method for preparing 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 3 times to complete It is possible to eliminate the residual air in the reactor and apply a slow nitrogen flow to the reaction system, then heat to 125°C to distill out the by-product methanol, and gradually increase the temperature to 190°C to maintain the esterification reaction until the amount of methanol evaporated reaches 95% of the theoretical value;

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

[0051] (3) Apply high vacuum to the reaction system (vacuum is 90Pa), and increase the reaction temperature to 260°C for the second-stage polycondensation reaction, ...

Embodiment 2

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

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

Embodiment 3

[0065] A method for preparing 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 the vacuum / nitrogen cycle 3 times to remove the residual air in the reactor as much as possible, apply a slow nitrogen flow to the reaction system, then heat to 125°C to distill out the by-product methanol, and gradually increase the temperature to 190°C to maintain the esterification reaction until methanol The steam output reaches 95% of the theoretical value;

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

[0068] (3) Apply high vacuum to the reaction system (vacuum is 90Pa), and increase the reaction temperature to 260°C for the second-stage polycondensation react...

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
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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 includes aromatic polyester, semi-aromatic polyester and aliphatic polyester, and is an extremely important polymer material. Due to the difference in chemical structure, different types of polyester have different excellent properties, so polyester can be used to produce fibers, engineering plastics and films and other products. [0003] Cyclic oligomers may be produced during polyester production and processing, 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%, of which cyclic trimers account for the largest proportion, accounting for about 75 wt% of the total oligomers; The...

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
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Application Information

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Patent Type & Authority Patents(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
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