CN110791850A - High-strength pulp-free polylactic acid multifilament and preparation method thereof - Google Patents

High-strength pulp-free polylactic acid multifilament and preparation method thereof Download PDF

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Publication number
CN110791850A
CN110791850A CN201911197380.1A CN201911197380A CN110791850A CN 110791850 A CN110791850 A CN 110791850A CN 201911197380 A CN201911197380 A CN 201911197380A CN 110791850 A CN110791850 A CN 110791850A
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China
Prior art keywords
pla
multifilament
free
layer
core layer
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CN201911197380.1A
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Chinese (zh)
Inventor
刘庆生
邓炳耀
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Jiangnan University
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Jiangnan University
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    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02GCRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
    • D02G3/00Yarns or threads, e.g. fancy yarns; Processes or apparatus for the production thereof, not otherwise provided for
    • D02G3/02Yarns or threads characterised by the material or by the materials from which they are made
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/28Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30Conjugate filaments; Spinnerette packs therefor
    • D01D5/34Core-skin structure; Spinnerette packs therefor
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • DTEXTILES; PAPER
    • D02YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
    • D02JFINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
    • D02J13/00Heating or cooling the yarn, thread, cord, rope, or the like, not specific to any one of the processes provided for in this subclass
    • DTEXTILES; PAPER
    • D10INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10BINDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/04Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
    • D10B2331/041Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET] derived from hydroxy-carboxylic acids, e.g. lactones

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Multicomponent Fibers (AREA)

Abstract

The invention discloses a high-strength pulp-free polylactic acid (PLA) multifilament and a preparation method thereof, wherein the high-strength pulp-free PLA multifilament consists of 24-288 PLA monofilaments, each PLA monofilament has a sheath-core structure, the sheath layer is low-melting-point PLA, the core layer is high-melting-point PLA, and the mass ratio of the sheath layer to the core layer is 5: 90-50: 50; the preparation method of the high-strength pulp-free PLA multifilament comprises the following steps: drying the raw materials of the skin layer and the core layer, respectively adding the dried raw materials into a hopper corresponding to a composite spinning machine, and performing melt spinning, side-blowing cooling, oiling and winding to obtain the PLA nascent multifilament with the skin-core structure; the high-strength pulp-free monofilament is prepared by stretching and heat setting the nascent multifilament, the setting temperature is higher than the melting point of the skin layer and lower than the melting point of the core layer during heat setting, and the high strength and pulp-free of the multifilament are realized through the bonding effect of the skin layer. The prepared high-strength non-sizing multifilament can be used in the fields of clothing textiles, decorative textiles and industrial textiles.

Description

High-strength pulp-free polylactic acid multifilament and preparation method thereof
Technical Field
The invention relates to the field of fibers, in particular to a high-strength pulp-free polylactic acid multifilament and a preparation method thereof.
Background
The textile industry is the national economy pillar industry, important civil industry and the industry with obvious international competitive advantages in China, and is also an important component of strategy emerging industry and an important carrier of national culture inheritance, however, the development of the textile industry has the problems of resource shortage and environmental pollution, for example, the raw materials of synthetic fibers mainly come from petroleum, the petroleum is non-renewable resources, the problem of resource exhaustion is faced after 50 years, most of petroleum-based synthetic fibers are not biodegradable and can generate environmental pollution, in addition, the multifilaments need to be sized in the warp preparation process, desizing is needed in dyeing and finishing, and sizing and desizing can generate the problems of environmental pollution and resource consumption. Polylactic acid (PLA) is renewable and biodegradable, can be used as a raw material of synthetic fibers, and can be specially designed and processed to realize pulp-free fiber structures so as to solve the problems of environmental pollution and resource shortage.
Disclosure of Invention
The invention aims to develop a high-strength non-sizing polylactic acid multifilament aiming at the problems of environmental and resource consumption caused by petroleum-derived raw materials of synthetic fibers and sizing and desizing, and provides a preparation method thereof.
The high-strength pulp-free polylactic acid PLA multifilament comprises the following raw materials:
(1) the high-strength pulp-free PLA multifilament consists of 24-288 PLA monofilaments, and the linear density of the multifilament is 50-1000D;
(2) the PLA monofilament has a skin-core structure, the core layer is made of PLA with D-LA content of 0-10 mol%, and the viscosity average molecular weight is 5.0 × 104~1.0×106(ii) a The core layer can also be stereocomplex polylactic acid sc-PLA, wherein the sc-PLA is a mixture of levorotatory polylactic acid PLLA and dextrorotatory polylactic acid PDLA, and the weight ratio of the PLLA to the PDLA is 1: 1, viscosity average molecular weight of PLLA and PDLA is 5.0X 104~1.0×106
(3) When the core layer is PLA fiber with the D-LA content of 0-10 mol%, the cortex layer is PLA with the D-LA content of 10-50 mol% of a D-LA structural unit, and the viscosity average molecular weight is 3.0 multiplied by 104~1.0×106(ii) a When the core layer is sc-PLA fiber, the skin layer is PLA with the D-LA content of 0-100%, and the viscosity average molecular weight is 3.0 multiplied by 104~1.0×106
(4) The mass ratio of the skin layer to the core layer is 5: 90-50: 50;
(5) the melting point of the single filament skin layer in the high-strength pulp-free PLA multifilament is lower than that of the core layer, and the multifilament is bonded together by virtue of the molten skin layer.
The preparation method of the high-strength pulp-free polylactic acid PLA multifilament comprises the following steps:
(1) respectively drying the PLA raw materials of the skin layer and the core layer in a vacuum oven for 8-48 h at the drying temperature of 50-105 ℃;
(2) adding PLA raw materials corresponding to a skin layer and a core layer into a hopper corresponding to a composite spinning machine, and preparing PLA nascent multifilaments with a skin-core structure through melt spinning, side blowing cooling, oiling and winding, wherein the melt extrusion temperature of the skin layer is 130-220 ℃, the melt extrusion temperature of the core layer is 180-250 ℃, the spinning speed is 500-3000 m/min, and the composite ratio is 5: 90-50: 50;
(3) and (2) stretching and heat setting the nascent fiber to prepare the high-strength pulp-free PLA multifilament, wherein the stretching multiple is 2-15 times, the stretching temperature is 65-120 ℃, the heat setting temperature is 80-210 ℃, when the cortex is amorphous PLA, the heat setting temperature is higher than the softening temperature of the cortex PLA, and when the cortex is crystalline PLA, the heat setting temperature is higher than the melting point of the PLA.
Has the advantages that:
(1) the high-strength pulp-free PLA multifilament is completely prepared from PLA, and has renewable resources and biodegradability.
(2) The preparation process of the high-strength pulp-free PLA multifilament is simple, no additional working procedure is added, the heat setting temperature is between the skin layer and the core layer during heat setting, the skin layers of the fibers are bonded together, the cohesive force between the fibers is increased, the pulp-free effect is realized, and the strength of the multifilament can be improved.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are only for illustrating the present invention and do not limit the scope of the present invention. Further, it should be understood that various changes and modifications to the present invention may be effected by those skilled in the art after reading the teachings herein, and such equivalents are intended to fall within the scope of the appended claims.
Example 1
(1) Firstly, stereocomplex polylactic acid (sc-PLA) and PLA with the D-LA content of 2mol percent are dried and pre-crystallized in a vacuum oven at 105 ℃ for 24 hours for standby, and the viscosity average molecular weights of PLLA and PDLA in the sc-PLA are respectively 1.8 multiplied by 105And 2.0X 105The viscosity average molecular weight of PLA was 2.2X 10, respectively5
(2) Adding PLA raw materials corresponding to a skin layer and a core layer into a hopper corresponding to a composite spinning machine, and preparing PLA nascent multifilament with a skin-core structure by melt spinning, side air blowing cooling, oiling and winding, wherein the melt extrusion temperature of the skin layer is 210 ℃, the melt extrusion temperature of the core layer is 230 ℃, the spinning speed is 1500m/min, and the composite spinning ratio is 10: 90, respectively;
(3) stretching and heat setting the nascent fiber to obtain high-strength pulp-free PLA multifilament, wherein the stretching multiple is 7.2 times, the stretching temperature is 100 ℃, and the heat setting temperature is 190 ℃; the obtained high-strength pulp-free PLA multifilament has the specification of 150D/48f, the strength of 5.6cN/dtex and the elongation at break of 18 percent.
Example 2
(1) Firstly, levorotatory polylactic acid PLLA (D-LA content is 0) and PLA with D-LA content of 10 mol% are dried in a vacuum oven at 80 ℃ for 24 hours for standby application, and the viscosity average molecular weights of the PLLA and the PLA are respectively 1.8 multiplied by 105And 1.5X 105
(2) Adding PLA raw materials corresponding to a skin layer and a core layer into a hopper corresponding to a composite spinning machine, and preparing PLA nascent multifilament with a skin-core structure by melt spinning, side air blowing cooling, oiling and winding, wherein the melt extrusion temperature of the skin layer is 180 ℃, the melt extrusion temperature of the core layer is 230 ℃, the spinning speed is 1500m/min, and the composite spinning ratio is 10: 90, respectively;
(3) stretching and heat setting the nascent fiber to obtain high-strength pulp-free PLA multifilament, wherein the stretching multiple is 8.5 times, the stretching temperature is 90 ℃, and the heat setting temperature is 140 ℃; the obtained high-strength pulp-free PLA multifilament has the specification of 150D/48f, the strength of 5.0cN/dtex and the elongation at break of 20 percent.
Example 3
(1) Firstly, levorotatory polylactic acid PLLA (D-LA content is 0) and PLA with D-LA content of 10 mol% are dried in a vacuum oven at 85 ℃ for 48 hours for standby application, and the viscosity average molecular weights of the PLLA and the PLA are respectively 1.8 multiplied by 105And 1.5X 105
(2) Adding PLA raw materials corresponding to a skin layer and a core layer into a hopper corresponding to a composite spinning machine, and preparing PLA nascent multifilament with a skin-core structure by melt spinning, side air blowing cooling, oiling and winding, wherein the melt extrusion temperature of the skin layer is 180 ℃, the melt extrusion temperature of the core layer is 230 ℃, the spinning speed is 1500m/min, and the composite spinning ratio is 20: 80;
(3) stretching and heat setting the nascent fiber to obtain high-strength pulp-free PLA multifilament, wherein the stretching multiple is 6.8 times, the stretching temperature is 85 ℃, and the heat setting temperature is 140 ℃; the obtained high-strength pulp-free PLA multifilament has the specification of 200D/48f, the strength of 4.2cN/dtex and the elongation at break of 23 percent.
Example 4
(1) Firstly, stereo-complex polylactic acid (sc-PLA) and levorotatory polylactic acid PLLA (D-LA content is 0) are dried in a vacuum oven at 90 ℃ for 24 hours for later use, and the viscosity average molecular weight of the PLLA and the viscosity average molecular weight of the PDLA in the sc-PLA are respectively 1.8 multiplied by 105And 2.0X 105The viscosity average molecular weight of PLA was 2.2X 10, respectively5
(2) Adding PLA raw materials corresponding to a skin layer and a core layer into a hopper corresponding to a composite spinning machine, and preparing PLA nascent multifilament with a skin-core structure by melt spinning, side air blowing cooling, oiling and winding, wherein the melt extrusion temperature of the skin layer is 220 ℃, the melt extrusion temperature of the core layer is 230 ℃, the spinning speed is 2000m/min, and the composite spinning ratio is 10: 90, respectively;
(3) stretching and heat setting the nascent fiber to obtain high-strength pulp-free PLA multifilament, wherein the stretching multiple is 8.8 times, the stretching temperature is 110 ℃, and the heat setting temperature is 185 ℃; the obtained high-strength pulp-free PLA multifilament has the specification of 150D/48f, the strength of 6.3cN/dtex and the elongation at break of 12 percent.

Claims (2)

1. A high-strength pulp-free polylactic acid (PLA) multifilament comprises the following raw materials:
(1) the high-strength pulp-free PLA multifilament consists of 24-288 PLA monofilaments, and the linear density of the multifilament is 50-1000D;
(2) the PLA monofilament has a skin-core structure, the core layer is made of PLA with D-LA content of 0-10 mol%, and the viscosity average molecular weight is 5.0 × 104~1.0×106(ii) a The core layer can also be stereocomplex polylactic acid sc-PLA, wherein the sc-PLA is a mixture of levorotatory polylactic acid PLLA and dextrorotatory polylactic acid PDLA, and the weight ratio of the PLLA to the PDLA is 1: 1, viscosity average molecular weight of PLLA and PDLA is 5.0X 104~1.0×106
(3) When the core layer is PLA fiber with the D-LA content of 0-10 mol%, the cortex layer is PLA with the D-LA content of 10-50 mol% of a D-LA structural unit, and the viscosity average molecular weight is 3.0 multiplied by 104~1.0×106(ii) a When the core layer is sc-PLA fiber, the skin layer is PLA with the D-LA content of 0-100%, and the viscosity average molecular weight is 3.0 multiplied by 104~1.0×106
(4) The mass ratio of the skin layer to the core layer is 5: 90-50: 50;
(5) the melting point of the single filament skin layer in the high-strength pulp-free PLA multifilament is lower than that of the core layer, and the multifilament is bonded together by virtue of the molten skin layer.
2. The method for preparing high-strength pulp-free polylactic acid (PLA) multifilament according to claim 1, comprising the steps of:
(1) respectively drying the PLA raw materials of the skin layer and the core layer in a vacuum oven for 8-48 h at the drying temperature of 50-105 ℃;
(2) adding PLA raw materials corresponding to a skin layer and a core layer into a hopper corresponding to a composite spinning machine, and preparing PLA nascent multifilaments with a skin-core structure through melt spinning, side blowing cooling, oiling and winding, wherein the melt extrusion temperature of the skin layer is 130-220 ℃, the melt extrusion temperature of the core layer is 180-250 ℃, the spinning speed is 500-3000 m/min, and the composite ratio is 5: 90-50: 50;
(3) and (2) stretching and heat setting the nascent fiber to prepare the high-strength pulp-free PLA multifilament, wherein the stretching multiple is 2-15 times, the stretching temperature is 65-120 ℃, the heat setting temperature is 80-210 ℃, when the cortex is amorphous PLA, the heat setting temperature is higher than the softening temperature of the cortex PLA, and when the cortex is crystalline PLA, the heat setting temperature is higher than the melting point of the PLA.
CN201911197380.1A 2019-11-29 2019-11-29 High-strength pulp-free polylactic acid multifilament and preparation method thereof Pending CN110791850A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024060501A1 (en) * 2022-09-23 2024-03-28 云南中烟工业有限责任公司 Preparation method for knife-hitting-preventing polylactic acid fiber filter stick

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KR20130112464A (en) * 2012-04-04 2013-10-14 현대자동차주식회사 Sheath-core all-in-one poly lactic acid fiber and a fabrication process thereof
CN105133082A (en) * 2015-07-24 2015-12-09 北京普利玛科技有限责任公司 Low-melting-point sheath-core-type polylactic acid composite fiber and preparation method thereof
CN106637500A (en) * 2016-11-08 2017-05-10 江南大学 High-heat-resistance skin-core structural polylactic acid fiber and preparation method thereof
CN106637523A (en) * 2016-11-08 2017-05-10 江南大学 Preparation method of porous polylactic acid fiber
CN106671545A (en) * 2016-11-08 2017-05-17 江南大学 High-fiber volume content polylactic acid homopolymer composite material and preparation method thereof
CN107475808A (en) * 2016-06-14 2017-12-15 中国石化仪征化纤有限责任公司 A kind of preparation method of low melting point skin-core structure polylactic acid short-fiber

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20130112464A (en) * 2012-04-04 2013-10-14 현대자동차주식회사 Sheath-core all-in-one poly lactic acid fiber and a fabrication process thereof
CN103074716A (en) * 2013-02-07 2013-05-01 中国烟草总公司郑州烟草研究院 Sheath-core polylactic acid tobacco tow and filter stick and preparation method thereof
CN105133082A (en) * 2015-07-24 2015-12-09 北京普利玛科技有限责任公司 Low-melting-point sheath-core-type polylactic acid composite fiber and preparation method thereof
CN107475808A (en) * 2016-06-14 2017-12-15 中国石化仪征化纤有限责任公司 A kind of preparation method of low melting point skin-core structure polylactic acid short-fiber
CN106637500A (en) * 2016-11-08 2017-05-10 江南大学 High-heat-resistance skin-core structural polylactic acid fiber and preparation method thereof
CN106637523A (en) * 2016-11-08 2017-05-10 江南大学 Preparation method of porous polylactic acid fiber
CN106671545A (en) * 2016-11-08 2017-05-17 江南大学 High-fiber volume content polylactic acid homopolymer composite material and preparation method thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2024060501A1 (en) * 2022-09-23 2024-03-28 云南中烟工业有限责任公司 Preparation method for knife-hitting-preventing polylactic acid fiber filter stick

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