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Full biodegrade copolyester fibers and preparation method thereof

A copolyester and all-biological technology, applied in the direction of single-component copolyester artificial filaments, etc., can solve problems such as insufficient esterification rate, inability to meet spinning processing requirements, and low molecular weight of products

Active Publication Date: 2020-05-05
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to solve the problems in the prior art that when IXDML is used to prepare biodegradable copolyesters, it is difficult to realize multi-component effective copolymerization, the thermal degradation is serious, and the molecular weight of the polymerization product is low, which cannot meet the requirements of spinning processing. Fully biodegradable copolyester based on IXDML and its preparation method, and then prepared into fibers
The present invention realizes multi-component high-efficiency copolymerization by adjusting and controlling the process conditions of comonomer esterification or transesterification reaction, and simultaneously effectively solves the severe thermal degradation of IXDML at high temperature and the reaction between fatty diols and fatty dibasic acids or aromatic dibasic carboxylic acids. Low temperature and insufficient esterification rate make the product molecular weight not high

Method used

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  • Full biodegrade copolyester fibers and preparation method thereof
  • Full biodegrade copolyester fibers and preparation method thereof
  • Full biodegrade copolyester fibers and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0044] A preparation method of fully biodegradable copolyester fibers, the steps are as follows:

[0045] (1) The first stage reaction: using 1,4-butanediol, terephthalic acid and adipic acid as raw materials, adding phosphoric acid and antioxidant 1010 at the same time, under the temperature of 190°C and under the action of tetrabutyl titanate Esterification for 2 hours, followed by prepolymerization for 0.5 hours at a pressure of 0.05 mbar and a temperature of 200° C., wherein the ratio of the molar weight of 1,4-butanediol to the sum of the molar weights of terephthalic acid and adipic acid is 1.1: 1. The ratio of the molar weight of tetrabutyl titanate to the sum of the molar weights of terephthalic acid and adipic acid is 50ppm, and the addition amounts of phosphoric acid and antioxidant 1010 are 1,4-butanediol and terephthalic acid respectively 0.1% and 0.2% of the sum of mass of adipic acid;

[0046] (2) Second-stage reaction: take the first-stage product, IIDML and adip...

Embodiment 2

[0062] A preparation method of fully biodegradable copolyester fibers, the steps are as follows:

[0063] (1) The first stage reaction: using 1,4-butanediol, terephthalic acid and adipic acid as raw materials, adding phosphoric acid and antioxidant 1010 at the same time, under the temperature of 210°C and under the action of tetrabutyl titanate Esterification for 2 hours, followed by prepolymerization for 0.5 hours at a pressure of 0.05 mbar and a temperature of 230° C., wherein the ratio of the molar weight of 1,4-butanediol to the sum of the molar weights of terephthalic acid and adipic acid is 1.5: 1. The ratio of the molar weight of tetrabutyl titanate to the sum of the molar weights of terephthalic acid and adipic acid is 2000ppm, and the addition amounts of phosphoric acid and antioxidant 1010 are 1,4-butanediol and terephthalic acid respectively 0.1% and 0.2% of the sum of mass of adipic acid;

[0064] (2) The second-stage reaction: using the first-stage product, IIDML...

Embodiment 3

[0071] A preparation method of fully biodegradable copolyester fibers is basically the same as in Example 2, except that 2,4-pentanediol is added in step (2) instead of 1,4-butanediol, The molar amount of IIDML in step (2) accounts for 50% of the sum of the molar amounts of 2,4-pentanediol in step (2) and IIDML in step (2).

[0072] The intrinsic viscosity of the fully biodegradable copolyester that finally makes is 0.60dL / g, and the number-average molecular weight is 16,800g / mol, and the molar weight of IIDML accounts for the 1,4-butanediol, 4-butanediol, 2 in the step (2), the ratio of the molar weight sum of 4-pentanediol and IIDML accounts for the 1,4-butanediol in the step (1), the 2 in the step (2) when the molar weight of IIDML accounts for the proportion ratio of feeding. , the ratio of the sum of the moles of 4-pentanediol and IIDML is lower than 0%;

[0073](4) Melt-spinning the fully biodegradable copolyester prepared in step (3) to obtain fully biodegradable copol...

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Abstract

The invention relates to full biodegrade copolyester fibers and a preparation method thereof. The preparation method comprises the steps of: firstly, performing a first-stage reaction under the high-temperature condition and under the action of a first catalyst by using A1, B1 and B2 as raw materials; then performing a second-stage reaction under the low-temperature condition and under the actionof a second catalyst by using a first-stage product, IXDML, A2 and B3 as raw materials; then performing a polycondensation reaction to prepare full biodegrade copolyester; and finally, preparing the full biodegrade copolyester fibers by a melt spinning forming method, wherein the prepared fibers has a moisture regain which is greater than or equal to 3.3% and a surface contact angle which is smaller than or equal to 67 degrees, and have a good thermodynamic property. The invention solves problems that the IXDML is seriously degraded and a polymerization product is low in molecular weight and cannot meet the spinning requirement; and the prepared fibers are good in moisture absorption, excellent in degradation property and high in mechanical strength, can be applied to the fields of home textiles, clothing, a portable medical material and the like, and has good application prospect.

Description

technical field [0001] The invention belongs to the field of fiber preparation, and relates to a fully biodegradable copolyester fiber and a preparation method thereof, in particular to a fully biodegradable copolyester fiber based on IXDML and a preparation method thereof. Background technique [0002] China is a big textile country in the world. The amount of waste textiles exceeds 20 million tons every year, but the recycling rate is less than 10%, resulting in serious waste of resources and solid waste pollution. In particular, polyester fiber (mainly PET-based polyester fiber), which accounts for nearly 70% of textile raw materials, has an annual output of nearly 40 million tons in 2015. Polyethylene terephthalate (PET) used in the manufacture of polyester fibers has a high glass transition temperature (~70-80°C), high crystallinity and hydrophobicity due to the high specific gravity of rigid terephthalic acid monomers . The moisture regain of PET is only 0.4% under t...

Claims

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Application Information

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IPC IPC(8): D01F6/84C08G63/42C08G63/83C08G63/85C08G63/86
CPCC08G63/42C08G63/83C08G63/85C08G63/866D01F6/84
Inventor 乌婧王华平林一鸣陈咏陈烨
Owner DONGHUA UNIV
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