CN108193317A - A kind of hollow acid fiber by polylactic of high-melting-point and preparation method thereof - Google Patents

A kind of hollow acid fiber by polylactic of high-melting-point and preparation method thereof Download PDF

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Publication number
CN108193317A
CN108193317A CN201711458041.5A CN201711458041A CN108193317A CN 108193317 A CN108193317 A CN 108193317A CN 201711458041 A CN201711458041 A CN 201711458041A CN 108193317 A CN108193317 A CN 108193317A
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China
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polylactic
melting
point
hollow
acid fiber
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Inventor
陆育明
冯忠耀
李东华
刘萍
朱亚宏
陈辉华
顾惠琴
杨卫忠
杨成
李忠
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SHANGHAI DEFULUN CHEMICAL FIBER CO Ltd
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SHANGHAI DEFULUN CHEMICAL FIBER CO Ltd
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Priority to CN201711458041.5A priority Critical patent/CN108193317A/en
Publication of CN108193317A publication Critical patent/CN108193317A/en
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    • 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
    • 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
    • D01D5/12Stretch-spinning methods
    • 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
    • D01D5/24Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
    • 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
    • D01D5/253Formation of filaments, threads, or the like with a non-circular cross section; 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
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/04Pigments
    • 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
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties

Abstract

The present invention relates to technical field of fibre production, specifically a kind of hollow acid fiber by polylactic of high-melting-point and preparation method thereof, the polylactic acid fiber with high melting point is process by high-melting-point polylactic acid master batch and two kinds of configuration polylactic acid slices by hollow profile spinning.The invention has the advantages that:Not only the shortcomings that prior art needs the acid fiber by polylactic faced the dye for carrying out poststaining to acid fiber by polylactic dark difficult had been overcome, but also has overcome the shortcomings that fabric wearability that polylactic acid fabric poststaining and flatiron are brought reduces.With the pure spinning of the hollow acid fiber by polylactic of high-melting-point of the present invention or it is blended made of clothes there is high color fastness, warming, fluffy, good permeability, rich in gloss, good hand touch, moisture conducting and sweat absorbing, resistance to ultraviolet and biodegradable.

Description

A kind of hollow acid fiber by polylactic of high-melting-point and preparation method thereof
Technical field
The present invention relates to technical field of fibre production, specifically, being a kind of hollow acid fiber by polylactic of high-melting-point and its system Preparation Method.
Background technology
Synthetic fibers polyester, nylon, polypropylene, acrylic be using petrochemicals as Material synthesis, physics and Chemical property is stablized, but the problem of there is using rear waste that can not decompose, it was reported that cotton in Xinjiang growing area is China The region of fouling membrane most serious, the Plastic-film pollution problem increasingly aggravated affects the yield and quality of crops, also, oil is Non-renewable resources, along with the loss of petrochemical material, in order to realize sustainable development, it is former that field of textiles needs new replacement Material, particularly environment amenable polymer can be applied to the more agricultural mulching of people's requirement and non-returnable container material Material, hygienic material.Polylactic acid (PLA) is exactly an outstanding representative, and material acid may be from the renewable sources of energy such as corn, sweet tea Dish etc., PLA belong to linear aliphatic race thermoplastic polyester, and this molecular structure means it with good biocompatibility and can Degradation property under conditions of certain temperature, pH value and moisture, can be decomposed into water and carbon dioxide.The U.S. NatureWorks companies are the leaders of global PLA fiber developments and production, and PLA fibers are mainly used for disposable products, account for The 60%~70% of NatureWorks companies total sales volume.Other weaving Frontier, Inc such as U.S. DuPont, Unifi, Fiber The companies such as Innovation, Parkdale, Interface, Japanese Supreme Being people, clock spinning, Kuraray have also grasped the key of PLA exploitations Technology, and relevant PLA textiles are developed, in the forward position of PLA exploitations, China is at present also in passive imitation situation.
PLA fibers compare from petroleum-based PET fiber, have penetrability is good, elastic recovery is high, the combustion heat is small, Burning fuming is few, ultra-violet resistance is good, refractive index is low, rich in gloss, good and biodegradable etc. the outstanding advantages of fabric feeling.But Also there are some defects, such as linear aliphatic race thermoplastic poly ester structure so that its hydrolysis resistance is poor for PLA fibers, thus dyes More adverse effect can be generated to fiber, reduce wearability, acid fiber by polylactic fusing point is low, heat resistance with postfinishing process Difference, greatly reduces the occasion used, and the scale for fundamentally limiting acid fiber by polylactic uses.
Chinese patent literature CN101805941A (application number 201010145777.9) discloses a kind of high-melting-point polylactic acid The preparation method of fiber, including:(1) poly (l-lactic acid) (PLLA) is sliced and is dried in vacuo with poly- D-ALPHA-Hydroxypropionic acid (PDLA) slice; (2) dry PLLA slices with PDLA slices by weight 20: 80~80: 20 are mixed, adds and account for PLA slice total weights The nucleating agent of 0.01wt%~5wt% be sufficiently mixed uniformly;(3) mixed material is subjected to melt blending, blend melt warp Spinneret spray, by quenching, oil after be wound into as-spun fibre;(4) as-spun fibre is carried out to 3~12 times of hot-drawn It stretches;(5) fiber stretched is imported in heat-setting box and carries out tensioned thermal finalization, acid fiber by polylactic fusing point obtained is 209 DEG C, there is heat-resist, good mechanical performance, fully biodegradable, solve acid fiber by polylactic to a certain extent The dyeing of fabric and flatiron problem, but does not solve the problems, such as fundamentally also the dark difficulty of polylactic acid fiber fabric dye and The problem of poststaining and flatiron cause polylactic acid fabric wearability to reduce, therefore, original liquid coloring prepare high-melting-point polylactic acid fibre Dimension is basic settling mode.
Acid fiber by polylactic is also needed in some use occasions with warmth retention property in terms of applied to textile garment and home textile use With gas permeability dual function, profiled polylactic acid fiber is processed into using profile spinneret in production, will further be widened The application of acid fiber by polylactic assigns the good warmth retention property of fiber and bulkiness.
2007 London College of Fashion of UK Polymer Showcase disclose follow-up in order to cancel Staining procedure, avoid potentially hydrolyze, degradation, U.S. DyeCatTMCompany develops suitable chromophore and is loaded into catalyst In structure, apply the polymerization stage in PLA, a direct step has made coloured PLA polymer, and develop black PLA polyester with And it is generally necessary to high dyestuff loads some colors being difficult to realize.Do not grasping the current of PLA core key production technologies also, The country is still difficult to realize the so big leap of amplitude.
Chinese patent literature CN106894103A (application number 201710137990.7) discloses a kind of acid fiber by polylactic and spins Preceding original liquid coloring solvent carrier type color masterbatch, raw material composition:Solvent carrier 40-89.5%, dyestuff or pigment 10-60% and dispersion Agent 0.5-5%.A few class solvent carriers in selected polylactic acid dedicated solvent carrier model color masterbatch have good compatible with polylactic acid Property, by adding online, utilization rate improves, and actually faces many difficulties, requires the technology for the personnel that match colors height, corresponding raw Production equipment is also required to be transformed, and the operation of pigment residual is complex during variety renovation, is not the mode of production of mainstream in the market.
Chinese patent literature CN106633693A (application number 201611143792.3) discloses a kind of acid fiber by polylactic and spins Preceding original liquid coloring Masterbatch, it is composed of the following components by weight:The modified PET polyester that 40~95 parts of fusing points are 180 DEG C, 0~50 part of pigment A or dyestuff a, 0~25 part of pigment B or dyestuff b, 0~15 part of pigment C or dyestuff c, 0~10 part of pigment D or dye Material d, 0.3~1.0 part of thermostabilization auxiliary agent, 0~2.5 part of dispersing aid, 0~2.5 part of rheology modifier add in color masterbatch in spinning Grain can obtain the acid fiber by polylactic of 3 grades of water resistance color fastness or more, 4 grades of light shine color fastness or more.
More than two literature research carrier be solvent carrier, 180 DEG C of modified PET polyester, be required for considering and poly- breast The consistency problem of acid slice, experimental study process is all complex cumbersome, is developed according to the applicant's acid fiber by polylactic over the years Experience, carrier selection polylactic acid slice, without considering consistency problem.
Invention content
It has done a large amount of research work early period of the invention to coloured acid fiber by polylactic, two kinds of configuration polylactic acid slices is selected to make For carrier, it is proposed that thus a kind of hollow acid fiber by polylactic of high-melting-point and preparation method thereof, the present invention generate.
The first aspect of the present invention, provides a kind of preparation method of the hollow acid fiber by polylactic of high-melting-point, and the high-melting-point gathers Acid fiber is process by high-melting-point polylactic acid master batch and two kinds of configuration polylactic acid slices by hollow profile spinning, including with Lower step:
A, the preparation of high-melting-point polylactic acid master batch:
Carrier poly (l-lactic acid) (PLLA) slice and poly- D-ALPHA-Hydroxypropionic acid (PDLA) slice are ground into powder, with environmentally friendly colorant and auxiliary Material is uniformly mixed, blended drying, and is melted through screw extruding, squeezed out, cool down, tie rod, pelletizing and dry high-melting-point is made gathering Lactic acid master batch;
B, the preparation of the hollow acid fiber by polylactic of high-melting-point:
After high-melting-point polylactic acid master batch, PLLA slices and PDLA slices, nucleating agent are dried on LHV431 type spinning-drawing machines Spinning carries out drawing-off spinning on LHV903 joint drafting machines, through drying, hollow profile spinning, winding, molding, boundling, leads It stretches, thermal finalization, curling, obtain the hollow acid fiber by polylactic of high-melting-point after cut-out.
Preferably, in the step A, the weight of carrier PLLA slices and PDLA slices powder, environmentally friendly colorant and auxiliary material Percentage is:Carrier PLLA is sliced and PDLA is sliced powder 65~85%, environmentally friendly colorant 5~20%, auxiliary material 10~30%.It is described Environmentally friendly colorant proportioning be preferably 5~15wt%, more preferable 8~12wt%.
Preferably, in the step A, the carrier PLLA slices and PDLA coupon weights ratio are 1:1.
Preferably, in the step A, carrier PLLA, PDLA slice powder size is 100nm~300nm.Through examination It tests, powder of the size in the range of 100nm~300nm and the compatibility of environmentally friendly colorant and auxiliary material are good, are not susceptible to reunite, preferably , powder size is 140nm~220nm.
Preferably, in the step A, the environmental protection colorant is selected from C.I. Pigment whites 6, C.I. face white 18:1、12、C.I Paratonere 101, C.I pigment red 4s 9:1st, C.I paratoneres 68, C.I pigment yellows 32, C.I. pigment yellows 16, C.I. pigment blacks 11, C.I. pigment black 15, C.I. solvent yellow 19s, C.I. pigment oranges 24, C.I pigment violet 3s, C.I. pigment blue 1s 0, phthalocyanine blue b, C.I. face Material basket 29, C.I pigment blue 1s 7:1st, in C.I naphthol greens 8, sun-proof emerald green color lake, environmentally-friecarbon carbon black FR8150, environmentally-friecarbon carbon black FR5200 One or more kinds of mixtures.
Preferably, in the step A, the auxiliary material is 40~60wt% polyethylene waxes and 40~60wt% nano-sized carbons The mixture of sour calcium.
Carrier PLLA is sliced and PDLA slice powder melt viscosities are high, and the poor compatibility with surface of pigments needs to add in auxiliary For material to reduce carrier viscosity, realization is compatible with pigment, meanwhile, it is easier to penetrate into pigment agglomerate internal void, in weakening Poly- power, make pigment agglomerate outside plus scissors power under the action of be easier open, newborn particle can also obtain rapidly soak and Protection, so as to promote the dispersion of pigment in original liquid coloring master batch.
Preferably, in the step B, high-melting-point polylactic acid master batch, PLLA slices and PDLA slices, the weight of nucleating agent Percentage is:High-melting-point polylactic acid master batch 5~12%, PLLA slices and PDLA are sliced 85~94%, nucleating agent 1~3%.
Preferably, in the step B, the PLLA slices and PDLA coupon weights ratio are 1:1
Preferably, in the step B, the nucleating agent is by aluminum benzoate, hydrated magnesium silicate and silica according to weight Amount is than being 2:1:1 mixes.
Studied through applicant, by aluminum benzoate, hydrated magnesium silicate and silica according to weight ratio be 2:1:1 mixes Nucleating agent can be effectively improved the crystal habit of polylactic acid, promote the formation of polylactic acid stereoscopic composite (sc-PLA) crystal, And effectively inhibit the generation of poly- D-ALPHA-Hydroxypropionic acid crystal and poly (l-lactic acid) crystal, meanwhile, poly- D-ALPHA-Hydroxypropionic acid crystal and poly (l-lactic acid) crystal energy It is enough to be converted into polylactic acid stereoscopic composite (sc-PLA) crystal at a lower temperature, so as to which acid fiber by polylactic be made to keep more satisfactory Mechanical property.
Preferably, in the step B, spinning technology parameter is:High-melting-point polylactic acid master batch, polylactic acid slice drying temperature Degree:116~120 DEG C, dry 16h, spinning pump is 780~1000g/min (preferably 816g/min) for amount, and spinning temperature is 240~280 DEG C (preferably 250~270 DEG C), spinning speed are 980~1100m/min (preferably 1020m/min), and drafting multiple is 3.1~3.6 times (preferably 3.35 times), 160~170 DEG C of heat setting temperature (preferably 165 DEG C).
Preferably, in the step B, in the hollow shape of profile spinneret selection circle, cross-shaped hollow shape, the hollow shapes of four T One kind, 1700 hole of spinneret hole count.
The professional standard that polylactic acid short-fiber test is formulated according to Shanghai Defulun Chemical Fiber Co., Ltd.:《The short fibre of polylactic acid Dimension》FZ/T 52041-2015.After tested, fibre technology index, fracture strength:>=3.70cN/dtex, elongation at break:30~ 60%, line density deviation ratio:± 8.0%, length variation rate:± 8.0%, crispation number:10 ± 2.5/25mm, crimp percent:10 ± 2.5%, 150 DEG C of dry-hot shrinkages:≤ 6.0%, regain:>=0.5%, line density:1.5~2.1dtex, biological decomposition Rate:>=60%, fusing point:210 DEG C, limit oxygen index:LOI:24~26%, fastness to soaping:>=4 grades, degree of hollowness:15~ 18%.
The second aspect of the present invention provides a kind of high-melting-point hollow acid fiber by polylactic, the hollow polylactic acid of the high-melting-point Fiber is prepared by as above any preparation method.
The invention has the advantages that:
1. it carries out melting hollow profile using PLLA slices and PDLA pieces, nucleating agent and high-melting-point polylactic acid master batch blending to spin The hollow acid fiber by polylactic of high-melting-point is prepared in silk, and uses the processing method of original liquid coloring, and fiber melt is high, bulkiness is good, Both the shortcomings that prior art needs the acid fiber by polylactic faced the dye for carrying out poststaining to acid fiber by polylactic dark difficult had been overcome, Polylactic acid fabric poststaining is overcome again and presses the shortcomings that fabric wearability brought reduces.
2. by aluminum benzoate, hydrated magnesium silicate and silica according to weight ratio be 2:1:The 1 nucleating agent energy mixed The crystal habit of polylactic acid is enough effectively improved, promotes the formation of polylactic acid stereoscopic composite (sc-PLA) crystal, and is effectively inhibited The generation of poly- D-ALPHA-Hydroxypropionic acid crystal and poly (l-lactic acid) crystal, meanwhile, poly- D-ALPHA-Hydroxypropionic acid crystal and poly (l-lactic acid) crystal can be relatively low At a temperature of be converted into polylactic acid stereoscopic composite (sc-PLA) crystal, so as to which acid fiber by polylactic be made to keep comparatively ideal mechanical property Energy.
3. the carrier that PLLA slices and PDLA slices is selected to be synthesized as master batch, efficiently solves the prior art using PET The problem of polyester cannot be compatible with polylactic acid slice, and be conducive to improve the fusing point of original liquid coloring acid fiber by polylactic, scheme is simple It is easy.
4. the hollow acid fiber by polylactic of high-melting-point derives from the renewable resources such as the cornstarch being easy to get, substitute non-renewable Fossil resource can be degraded into carbon dioxide and water, and final back to nature has the characteristics that low-carbon, environmental protection, can be fundamentally Solve the environmental problems such as " white pollution ", " greenhouse effects ".
It is 5. high, warming, fluffy, saturating with color fastness with the pure spinning of the hollow acid fiber by polylactic of high-melting-point or blended manufactured clothes Gas is good, rich in gloss, good hand touch, moisture conducting and sweat absorbing, it is resistance to ultraviolet and biodegradable the advantages that.
Specific embodiment
It elaborates with reference to embodiment to specific embodiment provided by the invention.
The preparation of the hollow acid fiber by polylactic of the red high-melting-point of embodiment 1
A, the preparation of red high-melting-point polylactic acid master batch:
Carrier PLLA slices and PDLA slices are ground into size as 100nm~300nm powders respectively, with environmentally friendly colorant Mixture (the 60wt% of C.I paratoneres 68 and auxiliary material polyethylene wax and nano-calcium carbonate:It 40wt%) is uniformly mixed, weight percent Than for:PLLA is sliced powder 32.5%, PDLA slice powders 32.5%, environmentally friendly colorant 5%, auxiliary material 30%.Blended drying, and Melt, squeeze out through screw extruding, cooling down, tie rod, pelletizing and drying original liquid coloring red high-melting-point polylactic acid master batch is made.
B, the preparation of the hollow acid fiber by polylactic of red high-melting-point:
Red high-melting-point polylactic acid master batch, PLLA slices, PDLA slices and nucleating agent are spun after drying in LHV431 types Spinning on silk machine carries out drawing-off spinning on LHV903 joint drafting machines, and weight percent is:Original liquid coloring red high-melting-point gathers Lactic acid master batch 12%, PLLA are sliced 42.5%, PDLA slices 42.5%, nucleating agent aluminum benzoate 1.5%, hydrated magnesium silicate 0.75%, silica 0.75%, through drying, the hollow spinning of circle, winding, molding, boundling, drawing-off, thermal finalization, curling, cut-out After obtain the hollow acid fiber by polylactic of red high-melting-point.
117 DEG C of high-melting-point polylactic acid master batch, PLLA slices, PDLA slices and nucleating agent drying temperature, dry 16h, spinning Metering pump is for amount 780g/min, 245~280 DEG C, spinning speed 980m/min of spinning temperature, 3.1 times of drafting multiple, thermal finalization temperature 160 DEG C of degree.
After tested, fibre technology index, fracture strength:3.8cN/dtex, elongation at break:42.6%, line density deviation Rate:3.2%, length variation rate:1.9%, crispation number:6/25mm, crimp percent:5.8%, 150 DEG C of dry-hot shrinkages:3.2%, Regain:0.6%, line density:2.1dtex, biological decomposition rate:92%, fusing point:208 DEG C, limit oxygen index LOI:24%, it is resistance to WASHING COLOR FASTNESS:4-5 grades, degree of hollowness:18%.
The preparation of the 2 hollow polylactic acid fiber with high melting point of blue of embodiment
A, the preparation of blue high-melting-point polylactic acid master batch:
Carrier PLLA slices and PDLA slices are ground into size as 100nm~300nm powders respectively, with environmentally friendly colorant C.I. mixture (the 50wt% of pigment blue 10 and auxiliary material polyethylene wax and nano-calcium carbonate:It 50wt%) is uniformly mixed, weight hundred Point ratio is:Carrier PLLA is sliced powder 37.5%, PDLA slice powders 37.5%, environmentally friendly colorant 8%, auxiliary material 17%.It is blended It is dry, and melt through screw extruding, squeeze out, cool down, tie rod, pelletizing and dry original liquid coloring blue high-melting-point polylactic acid mother being made Grain.
B, the preparation of the hollow acid fiber by polylactic of blue high-melting-point:
Blue high-melting-point polylactic acid master batch, PLLA slices, PDLA slices and nucleating agent are spun after drying in LHV431 types Spinning on silk machine carries out drawing-off spinning on LHV903 joint drafting machines, and weight percent is:Blue high-melting-point polylactic acid master batch 9%, PLLA are sliced 45%, PDLA slices 45%, nucleating agent aluminum benzoate 0.5%, hydrated magnesium silicate 0.25%, silica 0.25%, obtain blue Gao Rong after drying, cross-shaped hollow spinning, winding, molding, boundling, drawing-off, thermal finalization, curling, cut-out Point acid fiber by polylactic.
116 DEG C of blue high-melting-point polylactic acid master batch, PLLA slices, PDLA slices and nucleating agent drying temperature, dry 16h, Spinning pump is for amount 1000g/min, 250~270 DEG C, spinning speed 1100m/min of spinning temperature, 3.5 times of drafting multiple, warm 165 DEG C of setting temperature.
After tested, fibre technology index, fracture strength:4.2cN/dtex, elongation at break:36.3%, line density deviation Rate:1.6%, length variation rate:1.2%, crispation number:9.3/25mm, crimp percent:10.2%, 150 DEG C of dry-hot shrinkages: 4.6%, regain:0.6%, line density:1.5dtex, biological decomposition rate:94%, fusing point:209 DEG C, limit oxygen index LOI: 25%, fastness to soaping:4-5 grades, degree of hollowness:15%.
The preparation of the hollow polylactic acid fiber with high melting point of 3 yellow of embodiment
A, the preparation of yellow high-melting-point polylactic acid master batch:
Carrier PLLA slices and PDLA slices are ground into size as 100nm~300nm powders respectively, with environmentally friendly colorant Mixture (the 40wt% of C.I pigment yellows 16 and auxiliary material polyethylene wax and nano-calcium carbonate:It 60wt%) is uniformly mixed, weight percent Than for:Carrier PLLA is sliced 40%, PDLA slices 40%, environmentally friendly colorant 10%, auxiliary material 10%.Blended drying, and through screw rod Original liquid coloring yellow high-melting-point polylactic acid master batch is made in extrusion molten, extrusion, cooling, tie rod, pelletizing and drying.
B, the preparation of the hollow acid fiber by polylactic of yellow high-melting-point:
Original liquid coloring yellow high-melting-point polylactic acid master batch, PLLA slices, PDLA slices and nucleating agent are existed after drying Spinning on LHV431 type spinning-drawing machines carries out drawing-off spinning on LHV903 joint drafting machines, and weight percent is:Original liquid coloring is yellow Color high-melting-point polylactic acid master batch 5%, PLLA are sliced 46.5%, PDLA slices 46.5%, and nucleating agent aluminum benzoate 1% is hydrated silicon Sour magnesium 0.5%, silica 0.5% through drying, the hollow spinning of four T, winding, molding, boundling, drawing-off, thermal finalization, are crimped, are cut It has no progeny to obtain original liquid coloring yellow polylactic acid fiber with high melting point.
120 DEG C of yellow high-melting-point polylactic acid master batch, PLLA slices, PDLA slices and nucleating agent drying temperature, dry 16h, Spinning pump supplies amount as 816g/min, 250~270 DEG C, spinning speed 1020m/min of spinning temperature, 3.35 times of drafting multiple, 170 DEG C of heat setting temperature.
After tested, fibre technology index, fracture strength:3.9cN/dtex, elongation at break:42.4%, line density deviation Rate:1.2%, length variation rate:5.4%, crispation number:10.2/25mm, crimp percent:11.6%, 150 DEG C of dry-hot shrinkages: 3.9%, regain:0.6%, line density:1.7dtex, biological decomposition rate:92%, fusing point:212 DEG C, limit oxygen index LOI: 25%, fastness to soaping:4-5 grades, degree of hollowness:16%.
The preparation of the red hollow acid fiber by polylactic A of comparative example 1
Change the carrier PLLA slices in the step A of embodiment 1 and PDLA into PLLA slices, other raw materials, weight ratio are same Embodiment 1.
After tested, fibre technology index, fracture strength:3.5cN/dtex, elongation at break:35.5%, line density deviation Rate:4.5%, length variation rate:3.6%, crispation number:6.8/25mm, crimp percent:5.9%, 150 DEG C of dry-hot shrinkages: 6.7%, regain:0.5%, line density:2.1dtex, biological decomposition rate:92%, fusing point:200 DEG C, limit oxygen index LOI: 24%, fastness to soaping:4-5 grades, degree of hollowness:13%, fusing point is less than 1 product of embodiment.
The preparation of the 2 hollow acid fiber by polylactic of blue of comparative example
Change the carrier PLLA slices and PDLA of embodiment 2 into PLLA slices, other raw materials, weight ratio are the same as embodiment 2.
After tested, fibre technology index, fracture strength:3.4cN/dtex, elongation at break:41.6%, line density deviation Rate:0.8%, length variation rate:0.9%, crispation number:10.6/25mm, crimp percent:10.5%, 130 DEG C of dry-hot shrinkages: 4.0%, regain:0.5%, line density:1.5dtex, biological decomposition rate:92%, fusing point:175 DEG C, limit oxygen index LOI: 26%, fastness to soaping:4-5 grades, degree of hollowness:12%, fusing point is less than 2 product of embodiment.
The preparation of the high acid fiber by polylactic of 3 yellow of comparative example
The spinning spinneret of embodiment 3 is changed to circular solids, with embodiment 3, production technology is same for other raw materials, weight ratio Embodiment 3.
After tested, fibre technology index, fracture strength:4.7cN/dtex, elongation at break:46.6%, line density deviation Rate:1.9%, length variation rate:5.0%, crispation number:10.8/25mm, crimp percent:12.1%, 150 DEG C of dry-hot shrinkages: 3.9%, regain:0.6%, line density:1.7dtex, biological decomposition rate:92%, fusing point:212 DEG C, limit oxygen index LOI: 25%, fastness to soaping:4-5 grades, the bulkiness of fiber is than the difference of embodiment 3.
The preparation of the red hollow acid fiber by polylactic B of comparative example 4
Raw material proportioning in the step A of embodiment 1 is changed to:PLLA is sliced powder 32.5%, PDLA slice powders 52.5%, environmentally friendly colorant 5%, auxiliary material 10%, remaining production technology is the same as embodiment 1.
After tested, the fibre technology index that prepared by comparative example 4 is fracture strength:3.8cN/dtex, elongation at break: 42.8%, line density deviation ratio:9.2%, length variation rate:3.3%, crispation number:5.4/25mm, crimp percent:5.1%, 150 DEG C dry-hot shrinkage:5.7%, regain:0.5%, line density:2.1dtex, biological decomposition rate:92%, fusing point:186 DEG C, pole Limited oxygen index LOI:24%, fastness to soaping:4-5 grades, degree of hollowness:15%, fusing point is less than 1 product of embodiment.
The preparation of the red hollow acid fiber by polylactic C of comparative example 5
Raw material proportioning in the step B of embodiment 1 is changed to:Red high-melting-point polylactic acid master batch 12%, PLLA slices 22.5%, PDLA slice 62.5%, nucleating agent aluminum benzoate 1.5%, hydrated magnesium silicate 0.75%, silica 0.75%, Remaining years production. art is the same as embodiment 1.
After tested, the fibre technology index that prepared by comparative example 5 is fracture strength:3.8cN/dtex, elongation at break: 42.5%, line density deviation ratio:8.4%, length variation rate:2.3%, crispation number:6.6/25mm, crimp percent:5.7%, 150 DEG C dry-hot shrinkage:6.9%, regain:0.4%, line density:2.1dtex, biological decomposition rate:93%, fusing point:180 DEG C, pole Limited oxygen index LOI:24%, fastness to soaping:4-5 grades, degree of hollowness:15%, fusing point is less than 1 product of embodiment.
The preparation of the red hollow acid fiber by polylactic D of comparative example 6
By the auxiliary material polyethylene wax in the step A of embodiment 1 and the mixture of nano-calcium carbonate change into polyethylene wax (not plus Nano-calcium carbonate), other raw materials, weight ratio and production technology are the same as embodiment 1.
In step A prepares red master batch, when polylactic acid powder is mixed with environmental protection colorant and auxiliary material, dispersion effect compared with Difference occurs part and reunites, and master batch prepares difficult.
Occurs spinning moulding difficulty in step B, the quality and technical index of product is unstable.
The preparation of the hollow acid fiber by polylactic A of 7 yellow of comparative example
Raw material in the step A of embodiment 3 is not added with auxiliary material, other raw materials, weight ratio production technology are same
Embodiment 3.
During step A prepares yellow masterbatch, when polylactic acid powder is with environmentally friendly coloring material for mixing, dispersion effect is poor, occurs Reunite, master batch prepares difficult.
Occurs spinning moulding difficulty in step B, the quality and technical index of product is unstable.
The preparation of the hollow acid fiber by polylactic B of 8 yellow of comparative example
Raw material proportioning in the step A of embodiment 3 is changed to:Yellow high-melting-point polylactic acid master batch 5%, PLLA slices 46.5%, PDLA slice 46.5%, nucleating agent aluminum benzoate 1%, hydrated magnesium silicate 0.2%, silica 0.8%, Qi Tasheng Production. art is the same as embodiment 3.
After tested, the fibre technology index that prepared by comparative example 8 is fracture strength:3.7cN/dtex, elongation at break: 42.6%, line density deviation ratio:8.5%, length variation rate:3.8%, crispation number:6.7/25mm, crimp percent:6.9%, 150 DEG C dry-hot shrinkage:7.2%, regain:0.4%, line density:1.7dtex, biological decomposition rate:93%, fusing point:194 DEG C, pole Limited oxygen index LOI:24%, fastness to soaping:4-5 grades, degree of hollowness:14%, fusing point is less than 3 product of embodiment.
The preferred embodiment of the invention is illustrated above, but the invention be not limited to it is described Embodiment, those skilled in the art can also make various equivalent under the premise of without prejudice to the invention spirit Modification or replacement, these equivalent modifications or replacement are all contained in the application claim limited range.

Claims (9)

1. a kind of preparation method of the hollow acid fiber by polylactic of high-melting-point, which is characterized in that include the following steps:
A, the preparation of high-melting-point polylactic acid master batch:
Carrier PLLA slices and PDLA slices are ground into powder, are uniformly mixed with environmentally friendly colorant and auxiliary material, blended drying, and Melt, squeeze out through screw extruding, cooling down, tie rod, pelletizing and drying high-melting-point polylactic acid master batch is made;Wherein, carrier PLLA is cut Piece and PDLA slices powder, environmentally friendly colorant and auxiliary material weight percent be:Carrier PLLA be sliced and PDLA slice powder 65~ 85%, environmentally friendly colorant 5~20%, auxiliary material 10~30%;The auxiliary material is 40~60wt% polyethylene waxes and 40~60wt% The mixture of nano-calcium carbonate;
B, the preparation of the hollow acid fiber by polylactic of high-melting-point:
The spinning on LHV431 type spinning-drawing machines after high-melting-point polylactic acid master batch, PLLA slices and PDLA slices, nucleating agent are dried, Drawing-off spinning is carried out on LHV903 joint drafting machines, it is fixed through drying, hollow profile spinning, winding, molding, boundling, drawing-off, heat The hollow acid fiber by polylactic of high-melting-point is obtained after type, curling, cut-out;Wherein, high-melting-point polylactic acid master batch, PLLA slices and PDLA are cut Piece, nucleating agent weight percent be:High-melting-point polylactic acid master batch 5~12%, PLLA slices and PDLA are sliced 85~94%, into Core agent 1~3%.
2. the preparation method of the hollow acid fiber by polylactic of high-melting-point according to claim 1, which is characterized in that the step In A, the carrier PLLA slices and PDLA coupon weights ratio are 1:1.
3. the preparation method of the hollow acid fiber by polylactic of high-melting-point according to claim 1, which is characterized in that the step In A, carrier PLLA, PDLA slice powder size is 100nm~300nm.
4. the preparation method of the hollow acid fiber by polylactic of high-melting-point according to claim 1, which is characterized in that the step In A, the environmental protection colorant is selected from C.I. Pigment whites 6, C.I. face white 18:1st, 12, C.I paratoneres 101, C.I pigment red 4s 9:1、 C.I paratoneres 68, C.I pigment yellows 32, C.I. pigment yellows 16, C.I. pigment blacks 11, C.I. pigment blacks 15, C.I. solvent yellow 19s, C.I. pigment orange 24, C.I pigment violet 3s, C.I. pigment blue 1s 0, phthalocyanine blue b, C.I. pigment blues 29, C.I pigment blue 1s 7:1st, C.I face Expect the mixture in one or more of green 8, sun-proof emerald green color lake, environmentally-friecarbon carbon black FR8150, environmentally-friecarbon carbon black FR5200.
5. the preparation method of the hollow acid fiber by polylactic of high-melting-point according to claim 1, which is characterized in that the step In B, the PLLA slices and PDLA coupon weights ratio are 1:1.
6. the preparation method of the hollow acid fiber by polylactic of high-melting-point according to claim 1, which is characterized in that the step In B, the nucleating agent is 2 according to weight ratio by aluminum benzoate, hydrated magnesium silicate and silica:1:1 mixes.
7. the preparation method of the hollow acid fiber by polylactic of high-melting-point according to claim 1, which is characterized in that the step In B, spinning technology parameter is:High-melting-point polylactic acid master batch, polylactic acid slice drying temperature:116~120 DEG C, dry 16h is spun Thread metering pump is 780~1000g/min for amount, and spinning temperature is 240~280 DEG C, and spinning speed is 980~1100m/min, is led It is 3.1~3.6 times to stretch multiple, 160~170 DEG C of heat setting temperature.
8. the preparation method of the hollow acid fiber by polylactic of high-melting-point according to claim 1, which is characterized in that the step In B, one kind in the hollow shape of profile spinneret selection circle, cross-shaped hollow shape, the hollow shapes of four T, 1700 hole of spinneret hole count.
9. a kind of hollow acid fiber by polylactic of high-melting-point, which is characterized in that the hollow acid fiber by polylactic of the high-melting-point will by right Any preparation methods of 1-8 is asked to be prepared.
CN201711458041.5A 2017-12-28 2017-12-28 A kind of hollow acid fiber by polylactic of high-melting-point and preparation method thereof Pending CN108193317A (en)

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Application publication date: 20180622