CN108166096A - A kind of original liquid coloring flame-proof polylactic acid fiber and preparation method thereof - Google Patents
A kind of original liquid coloring flame-proof polylactic acid fiber and preparation method thereof Download PDFInfo
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- CN108166096A CN108166096A CN201711461646.XA CN201711461646A CN108166096A CN 108166096 A CN108166096 A CN 108166096A CN 201711461646 A CN201711461646 A CN 201711461646A CN 108166096 A CN108166096 A CN 108166096A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/04—Pigments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
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- Artificial Filaments (AREA)
Abstract
The invention discloses a kind of original liquid coloring flame-proof polylactic acid fibers and preparation method thereof, and the method includes the steps the preparations of A, original liquid coloring flame-proof polylactic acid master batch：65~82wt% polylactic acid powder, 5~15wt% environmental protection colorant, fire retardant 5~10% and 5~15wt% auxiliary materials are uniformly mixed, original liquid coloring flame-proof polylactic acid master batch is made through screw extruder extruding pelletization after drying；B, the preparation of original liquid coloring flame-proof polylactic acid fiber：5~12wt% original liquid coloring flame-proof polylactic acid master batches and 88~95wt% polylactic acid slices are subjected to spinning and drawing-off obtains original liquid coloring flame-proof polylactic acid fiber.Colorant and fire retardant are uniformly dispersed in the original liquid coloring flame-proof polylactic acid master batch, applicable fiber system, and original liquid coloring flame-proof polylactic acid master batch is used as raw material, it can solve the problems, such as that prior art color masterbatch carrier cannot be compatible with polylactic acid slice, while the fiber prepared has preferable wearability and flame retardant property.
Description
Technical field
The invention belongs to technical field of fibre production, and in particular to a kind of original liquid coloring flame-proof polylactic acid fiber and its 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 with postfinishing process.
UK Polymer Showcase 2007London College of Fashion disclose subsequent in order to cancel
Staining procedure avoids potentially hydrolyzing, degrade.U.S. DyeCatTMCompany develops suitable chromophore and is loaded into catalyst knot
On structure, apply the polymerization stage in PLA, a direct step has made coloured PLA polymer, and develop black PLA polyester and
It is generally necessary to high dyestuff loads some colors being difficult to realize.In current, the state for not grasping PLA core key production technologies also
Inside still it is difficult to realize the so big leap of amplitude.
Chinese patent 201710137990.7 discloses original liquid coloring solvent carrier type color before a kind of acid fiber by polylactic is spun
Mother, raw material composition：Solvent carrier 40-89.5%, dyestuff or pigment 10-60% and dispersant 0.5-5%.Selected polylactic acid is special
There is excellent compatibility with a few class solvent carriers in solvent carrier type color masterbatch and polylactic acid, by adding online, utilization rate carries
Height actually faces many difficulties, requires height to the technology for the personnel that match colors, corresponding production equipment is also required to be transformed, product
The operation of pigment residual is complex when kind is replaced, and is not the mode of production of mainstream in the market.
Chinese patent 201611143792.3 discloses original liquid coloring Masterbatch before a kind of acid fiber by polylactic is spun, by weight
Part meter is composed of the following components：40~95 parts of fusing points are 180 DEG C of modified PET polyester, 0~50 part of pigment A or dyestuff a, 0~25
Part pigment B or dyestuff b, 0~15 part of pigment C or dyestuff c, 0~10 part of pigment D or dyestuff d, 0.3~1.0 part of thermostabilization auxiliary agent, 0
~2.5 parts of dispersing aiies, 0~2.5 part of rheology modifier, Masterbatch is added in spinning, can obtain 3 grades of water resistance color fastness
Above, the acid fiber by polylactic of 4 grades of light shine color fastness or more.
More than 2 research carriers for solvent carrier, 180 DEG C of modified PET polyester, be required for consider and polylactic acid slice
Consistency problem, experimental study process is all complex cumbersome.
In addition, Chinese patent 201310087582.7 discloses a kind of preparation method of halogen-free flame-retardant polylactic acid fiber, packet
It includes：(1) polylactic acid slice and fire retardant are mixed, under the conditions of 180~220 DEG C, melt blending, cooling granulation obtains fire-retardant
Polylactic acid master batch；(2) polylactic acid slice and synergist are mixed, under the conditions of 190~220 DEG C, melt blending, cooling granulation,
Obtain collaboration polylactic acid master batch；(3) it by polylactic acid slice, flame-proof polylactic acid master batch, collaboration polylactic acid master batch, dispersant, mixes,
Carry out spinning, obtain as-spun fibre, then by as-spun fibre using drawing-off post-processing to get halogen-free flame-retardant polylactic acid fiber.
The PLA Composite Fiber material spinning moulding arrived is good, and fiber quality is excellent；Fire retardant used is halogen-free flame retardants, uses and fires
It is safe and non-toxic during burning, belong to environmentally protective fiber；It has higher requirements available for clothes, interior trim, home textile etc. to flame retardant property
Field, wide market.
Chinese patent 201610619302.6 discloses a kind of preparation method of flame-proof polylactic acid fabric lining：(1) it presses
Row parts by weight are equipped with raw material, then add in high-speed mixer and are uniformly dispersed to obtain polydactyl acid mixed raw material：PLA gathers breast
It is 65-89 parts sour；PBS0.2 parts；0.2 part of tourmaline powder；0.8-1 parts of montmorillonite；1 part of stachyose；0.2-04 parts of chitosan；Neatly
0.3-0.5 parts of stone；0.8 part of mica powder；0.3 part of silicon carbide；(2) above-mentioned mixed uniformly polydactyl acid mixed raw material is passed through
Double screw extruder melt blending squeezes out obtained polydactyl acid master batch, and is dried in vacuo, and mixture passes through on melt spinning machine
Round spinneret orifice spinning obtains modified polylactic acid fiber；(3) above-mentioned acid fiber by polylactic is woven into inflaming retarding fabric.
The acid fiber by polylactic prepared in above-mentioned two pieces patent has flame retardant property, but is the failure to colour, and color is single.It is and former
Liquid colours acid fiber by polylactic in terms of applied to textile garment and home textile, is also needed in some use occasions with flame retarding function,
The application range that the exploitation of original liquid coloring flame-proof polylactic acid fiber will further widen acid fiber by polylactic.
Invention content
Therefore, for the prior art in the preparation of PLA fibers, color masterbatch carrier is asked with technology of the polylactic acid there are compatibility
Topic, the present invention select carrier of the polylactic acid slice as color masterbatch, it is proposed that a kind of original liquid coloring flame-proof polylactic acid fiber and its system
Preparation Method avoids solvent carrier or modified PET polyester and the consistency problem of polylactic acid slice, while promotes the anti-flammability of fiber
Energy.
In the preparation method of original liquid coloring flame-proof polylactic acid fiber provided by the invention, original liquid coloring flame-proof polylactic acid is used
Master batch and polylactic acid slice prepare original liquid coloring flame-proof polylactic acid fiber by spinning processing.It the described method comprises the following steps：
A, the preparation of original liquid coloring flame-proof polylactic acid master batch：
By 65~82wt% polylactic acid powder, 5~15wt% environmental protection colorant, fire retardant 5~10% and 5~15wt% auxiliary materials
It is uniformly mixed, original liquid coloring flame-proof polylactic acid master batch is made through screw extruder extruding pelletization after drying；The auxiliary material is poly-
The mixture of ethylene waxes and nano-calcium carbonate；
B, the preparation of original liquid coloring flame-proof polylactic acid fiber：
5~12wt% original liquid coloring flame-proof polylactic acid master batches and 88~95wt% polylactic acid slices are subjected to spinning and drawing-off
Obtain original liquid coloring flame-proof polylactic acid fiber.
When step A prepares original liquid coloring flame-proof polylactic acid master batch, using polylactic acid as carrier, but polylactic acid melt viscosity
Height, the poor compatibility with colorant surface, the addition of auxiliary material polyethylene wax and nano-calcium carbonate can reduce carrier viscosity, realize poly-
Lactic acid melt is compatible with colorant, meanwhile, auxiliary material is easier to penetrate into colorant aggregate internal void, weakens cohesive force, makes color
Dough aggressiveness is being easier to open outside plus under the action of scissors power, and newborn particle also rapidly can be soaked and be protected, so as to
Promote the dispersion of colorant in original liquid coloring master batch.The addition of the fire retardant can effectively provide the flame retardant property of obtained fiber.
In step A, the polylactic acid powder size is 100nm~300nm, can be made by polylactic acid slice is ground.
Through experiment, powder of the size in the range of 100nm~300nm and the compatibility of environmentally friendly colorant, fire retardant and auxiliary material are good, are not easy to send out
It is raw to reunite, it is preferred that powder size is 140nm~220nm.
Preferably, in step A, the environmentally friendly colorant is selected from C.I. Pigment whites 6, C.I. Pigment whites, C.I. face white 18：1、
12nd, C.I. paratoneres 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
Black 11, C.I. pigment blacks 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. pigment blue 29, C.I pigment blue 1s 7：1st, C.I naphthol greens 8, sun-proof emerald green color lake, environmentally-friecarbon carbon black FR8150 and environmentally-friecarbon carbon black
One or more of FR5200 mixtures.
Further, in step A, environmentally friendly colorant proportioning preferably 8~12wt%.
Preferably, in step A, the fire retardant is trichlorine pyrophosphate and the mixture of pentaerythrite.
Fire retardant mechanism is：Trichlorine pyrophosphate can decomposite ammonia and polyphosphoric acid at high temperature, then polyphosphoric acid meeting
Phosphoric acid is reduced into, forms acid film layer barrier air, addition pentaerythrite can promote polylactic acid system to generate foam layer of charcoal, improve
Flame retardant effect.
Further, the fire retardant is 70~80wt% trichlorines pyrophosphate and 20~30wt% pentaerythrites
Mixture.
Preferably, in step A, the auxiliary material is 40~60wt% polyethylene waxes and 40~60wt% nano-calcium carbonates
Mixture.
Preferably, in step A, extruding pelletization refers specifically to：Polylactic acid slice powder, environmentally friendly colorant, fire retardant and auxiliary material mix
Through drying after closing uniformly, and hindered through screw extruder extrusion molten, extrusion, cooling, tie rod, pelletizing and the dry original liquid coloring that is made
Fire polylactic acid master batch.
Preferably, in step B, spinning and drawing-off refer specifically to：Original liquid coloring flame-proof polylactic acid master batch and polylactic acid slice according to
It is secondary that original liquid coloring flame-proof polylactic acid fibre is obtained after drying, spinning, winding, molding, boundling, drawing-off, thermal finalization, curling, cut-out
Dimension.
Preferably, in step B, one in spinning spinneret selection circle, the hollow shape of circle, cross-shaped hollow shape, the hollow shapes of four T
Kind, 1700 hole of spinneret hole count.
Preferably, in step B, the technological parameter of spinning and drawing-off is：Original liquid coloring flame-proof polylactic acid master batch, polylactic acid are cut
116~120 DEG C of piece drying temperature, the preferred 16h of 12~20h of drying time, spinning pump are (excellent for 780~1000g/min for amount
Select 820g/min), spinning temperature is 225~260 DEG C (preferably 240~260 DEG C), and spinning speed is (excellent for 980~1100m/min
Select 1020m/min), drafting multiple is 3.1~3.6 times (preferably 3.35 times).
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, the fibre technology index that prepared by the method for the invention, fracture strength：≥3.40cN/
Dtex, elongation at break：45 ± 6.0%, line density deviation ratio：± 8.0%, length variation rate：± 8.0%, crispation number：10±
2.5/25mm, crimp percent：10 ± 2.5%, 130 DEG C of dry-hot shrinkages：≤ 5.0%, regain：>=0.5%, line density：1.5
~2.1dtex, biological decomposition rate：>=60%, fusing point：173~176 DEG C, limit oxygen index：LOI：29-33%, resistance to color jail of soaping
Degree：>=4 grades.
The positive effect of the present invention is：
1. the present invention prepares the original liquid coloring flame-proof polylactic acid master batch, by the use for allocating environmentally friendly colorant and fire retardant
Amount, using the mixture of polyethylene wax and nano-calcium carbonate as auxiliary material, polyethylene wax and nano-calcium carbonate are used cooperatively, Ke Yiyou
Effect reduces the viscosity of carrier polylactic acid, realizes that polylactic acid melt is compatible with colorant, meanwhile, the auxiliary material is easier to penetrate into colorant
In aggregate internal void, weaken cohesive force, colorant aggregate is made to be easier to open outside plus under the action of scissors power, newborn grain
Son also rapidly can be soaked and be protected, so as to promote the dispersion of colorant in original liquid coloring master batch.The original liquid coloring is fire-retardant
In polylactic acid master batch colorant be uniformly dispersed, good fluidity, long flow path, fusing point it is high, applicable fiber system.
It is Raw material processing into original liquid coloring flame-proof polylactic acid that 2. the present invention, which uses the original liquid coloring flame-proof polylactic acid master batch,
Fiber, avoids spinning after stain and postfinishing process to it at the defects of can fundamentally overcoming polylactic acid hydrolysis-resisting energy force difference
The adverse effect of generation improves the wearability of acid fiber by polylactic and expands application range, simultaneous selection polylactic acid powder
As Masterbatch synthesis carrier, efficiently solve the prior art using PET polyester as color masterbatch carrier when and polylactic acid slice
Cannot be compatible the problem of, scheme is simple and practicable.
3. the present invention selects the mixture of trichlorine pyrophosphate and pentaerythrite as fire retardant, the auxiliary material is similary
Trichlorine pyrophosphate and pentaerythrite can be made to be dispersed in polylactic acid carrier, and existed based on trichlorine pyrophosphate
Ammonia and polyphosphoric acid can be decomposited under high temperature, then polyphosphoric acid can be reduced into phosphoric acid, form acid film layer barrier air, add season
Penta tetrol can promote polylactic acid system to generate foam layer of charcoal, improve flame retardant effect.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail, it should be understood that these embodiments are merely to illustrate this hair
Bright rather than the limitation present invention application range.
Fibre technology index test foundation prepared by following embodiment and comparative example is the limited public affairs of Shanghai De Fulun chemical fibres
Take charge of the professional standard formulated：《Polylactic acid short-fiber》FZ/T 52041-2015.
The preparation of 1 original liquid coloring white flame-proof polylactic acid fiber of embodiment
A, the preparation of original liquid coloring flame-proof polylactic acid master batch：
Carrier polylactic acid slice is ground into size as 100nm~300nm powders, with environmentally friendly colorant (C.I. face white 18：
1), fire retardant and auxiliary material (mixture of 40wt% polyethylene waxes and 60wt% nano-calcium carbonates) are uniformly mixed, weight percent
For：Carrier polylactic acid slice powder 65%, environmentally friendly colorant 10%, trichlorine pyrophosphate 7.5%, pentaerythrite 2.5% are auxiliary
Material 15%.Then it dries, and melts, squeezes out through screw extruding, cooling down, tie rod, pelletizing and dry the resistance of original liquid coloring white being made
Fire polylactic acid master batch.
B, the preparation of original liquid coloring white flame-proof polylactic acid fiber：
By after original liquid coloring white flame-proof polylactic acid master batch, polylactic acid slice drying in LHV431 types spinning-drawing machine (Shanghai the
Two textile machinery Machine Co., Ltd) on spinning, LHV903 combine drafting machine (the limited public affairs of Shanghai the second textile machine share
Department) on carry out drawing-off spinning, weight percent is：Original liquid coloring white flame-proof polylactic acid master batch 10%, polylactic acid slice 90%,
Original liquid coloring white is obtained after drying, the spinning of circle hollow profile, winding, molding, boundling, drawing-off, thermal finalization, curling, cut-out
Flame-proof polylactic acid fiber.
Original liquid coloring white flame-proof polylactic acid master batch, 117 DEG C of polylactic acid slice drying temperature, dry 16h, spinning pump
For measuring 780g/min, 240~260 DEG C, spinning speed 980m/min of spinning temperature, 3.1 times of drafting multiple.
After tested, fibre technology index, fracture strength：3.4cN/dtex, elongation at break：40.5%, line density deviation
Rate：2.8%, length variation rate：1.5%, crispation number：9.5/25mm, crimp percent：9.4%, 130 DEG C of dry-hot shrinkages：
4.6%, regain：0.6%, line density：1.5dtex, biological decomposition rate：90%, fusing point：176 DEG C, limit oxygen index LOI：
30%, fastness to soaping：4-5 grades, degree of hollowness：14%.
The preparation of 2 original liquid coloring blue flame-proof polylactic acid fiber of embodiment
A, the preparation of original liquid coloring blue flame-proof polylactic acid master batch：
Carrier polylactic acid slice is ground into size as 100nm~300nm powders, with environmentally friendly colorant (C.I. pigment blues
10), fire retardant and auxiliary material (mixture of 50wt% polyethylene waxes and 50wt% nano-calcium carbonates) are uniformly mixed, weight percent
For：Carrier polylactic acid slice powder 82%, environmentally friendly colorant 5%, trichlorine pyrophosphate 5.25%, pentaerythrite 1.75%,
Auxiliary material 5%.Then it dries, and melts, squeezes out through screw extruding, cooling down, tie rod, pelletizing and dry the resistance of original liquid coloring blue being made
Fire polylactic acid master batch.
B, the preparation of original liquid coloring blue flame-proof polylactic acid fiber：
The spinning on LHV431 type spinning-drawing machines after original liquid coloring blue flame-proof polylactic acid master batch, polylactic acid slice are dried,
Drawing-off spinning is carried out on LHV903 joint drafting machines, weight percent is：Original liquid coloring blue polylactic acid master batch 8%, poly- breast
Acid slice 92% obtains original after drying, round spinneret spinning, winding, molding, boundling, drawing-off, thermal finalization, curling, cut-out
Liquid colored blue flame-proof polylactic acid fiber.
Original liquid coloring blue flame-proof polylactic acid master batch, 116 DEG C of polylactic acid slice drying temperature, dry 16h, spinning pump
For measuring 1000g/min, 225~240 DEG C, spinning speed 1100m/min of spinning temperature, 3.6 times of drafting multiple.
After tested, fibre technology index, fracture strength：3.6cN/dtex, elongation at break：39.7%, line density deviation
Rate：2.3%, length variation rate：0.6%, crispation number：11.2/25mm, crimp percent：9.5%, 130 DEG C of dry-hot shrinkages：
3.1%, regain：0.5%, line density：2.1dtex, biological decomposition rate：91%, fusing point：175 DEG C, limit oxygen index LOI：
30%, fastness to soaping：4-5 grades.
The preparation of 3 original liquid coloring Green Flammability acid fiber by polylactic of embodiment
A, the preparation of original liquid coloring Green Flammability polylactic acid master batch：
Carrier polylactic acid slice is ground into size as 100nm~300nm powders, with environmentally friendly colorant (C.I naphthol greens 8),
Fire retardant and auxiliary material (mixture of 60wt% polyethylene waxes and 40wt% nano-calcium carbonates) are uniformly mixed, and weight percent is：
Carrier polylactic acid slice powder 74%, environmentally friendly colorant 8%, trichlorine pyrophosphate 7.5%, pentaerythrite 2.5%, auxiliary material
8%.Then it dries, and melts, squeezes out through screw extruding, cooling down, tie rod, pelletizing and dry original liquid coloring Green Flammability is made gathering
Lactic acid master batch.
B, the preparation of original liquid coloring Green Flammability acid fiber by polylactic：
The spinning on LHV431 type spinning-drawing machines after original liquid coloring green polylactic acid master batch, polylactic acid slice are dried,
Drawing-off spinning is carried out on LHV903 joint drafting machines, weight percent is：Original liquid coloring green polylactic acid master batch 5%, polylactic acid
Slice 95%, original is obtained after drying, four T hollow profiles spinning, winding, molding, boundling, drawing-off, thermal finalization, curling, cut-out
The green acid fiber by polylactic of liquid coloring.
Original liquid coloring Green Flammability polylactic acid master batch, 120 DEG C of polylactic acid slice drying temperature, dry 16h, spinning pump
For measuring as 816g/min, 240~260 DEG C, spinning speed 1020m/min of spinning temperature, 3.35 times of drafting multiple.
After tested, fibre technology index, fracture strength：3.6cN/dtex, elongation at break：42.4%, line density deviation
Rate：3.7%, length variation rate：2.9%, crispation number：11.6/25mm, crimp percent：11.3%, 130 DEG C of dry-hot shrinkages：
3.7%, regain：0.7%, line density：1.7dtex, biological decomposition rate：90%, fusing point：175 DEG C, limit oxygen index LOI：
32%, fastness to soaping：4-5 grades, degree of hollowness：15%.
In above-described embodiment 1~3, step A is prepared in original liquid coloring flame-proof polylactic acid master batch, and colorant and fire retardant dispersion are equal
Even, good fluidity, long flow path, fusing point are high, applicable fiber system.And original liquid coloring flame-proof polylactic acid master batch is used to add for raw material
Work is into original liquid coloring flame-proof polylactic acid fiber, the defects of can fundamentally overcoming polylactic acid hydrolysis-resisting energy force difference, avoids spinning
The adverse effect that silk after stain and postfinishing process generate it improves the wearability of acid fiber by polylactic and expands using model
It encloses.Moreover, also effectively controlling the influence of addition original excellent performance to acid fiber by polylactic of fire retardant, substantially increase simultaneously
The flame retardant property of fiber, limit oxygen index LOI reach 30~32%, belong to nonflammable material.Simultaneous selection polylactic acid powder is as color
The carrier of master batch synthesis, efficiently solving cannot phase with polylactic acid slice when the prior art uses PET polyester as color masterbatch carrier
The problem of appearance, scheme are simple and practicable.
The preparation of the red flame-proof polylactic acid fiber of comparative example 1
Change the carrier polylactic acid slice in the step A of embodiment 1 into 180 DEG C of modified PETs, other raw materials, weight ratio are same
Embodiment 1, production technology is the same as embodiment 1.When master batch prepares mixing, part reunion has occurred, dispersion effect is poor, spinning moulding
It is more difficult.
After tested, fibre technology index, fracture strength：2.2cN/dtex, elongation at break：31.5%, line density deviation
Rate：9.8%, length variation rate：6.9%, crispation number：9.2/25mm, crimp percent：9.3%, 130 DEG C of dry-hot shrinkages：
6.8%, regain：0.4%, line density：1.5dtex, biological decomposition rate：52%, fusing point：170 DEG C, limit oxygen index LOI：
27%, fastness to soaping：3 grades.Although there is certain anti-flammability but significantly lower than 1 product of embodiment, other indices
Not as good as 1 product of embodiment.
The preparation of 2 original liquid coloring blue acid fiber by polylactic of comparative example
Fire retardant is not added with, other raw materials, weight ratio are with embodiment 2, and production technology is the same as embodiment 2.
After tested, fibre technology index, fracture strength：3.9cN/dtex, elongation at break：44.6%, line density deviation
Rate：0.8%, length variation rate：0.9%, crispation number：10.2/25mm, crimp percent：10.54%, 130 DEG C of dry-hot shrinkages：
4.0%, regain：0.5%, line density：2.1dtex, biological decomposition rate：96%, fusing point：175 DEG C, limit oxygen index LOI：
26%, fastness to soaping：4-5 grades, flame-retardant fiber is poor, limit oxygen index LOI：26%, belong to combustible material.
The preparation of 3 original liquid coloring white flame-proof polylactic acid fiber A of comparative example
Raw material proportioning in the step A of embodiment 1 is changed to：Carrier polylactic acid slice powder 50%, environmentally friendly colorant：
10%, trichlorine pyrophosphate 7.5%, pentaerythrite 2.5%, auxiliary material：25%, remaining production technology is the same as embodiment 1.
Dispersibility is poor when step A blendings make master batch, and part occurs and reunites, master batch prepares difficult.
Occurs spinning moulding difficulty in step B, blocking the situations such as spinneret causes technical target of the product to differ greatly.
After tested, the fibre technology index that prepared by comparative example 3 is fracture strength：2.6cN/dtex, elongation at break：
17.2%, line density deviation ratio：23.5%, length variation rate：5.9%, crispation number：5.3/25mm, crimp percent：5.1%,
130 DEG C of dry-hot shrinkages：8.3%, regain：0.3%, line density：1.5dtex, biological decomposition rate：75%, fusing point：175 DEG C,
Limit oxygen index LOI：27%, fastness to soaping：3 grades.Indices are not as good as 1 product of embodiment, and production is difficult, unit consumption
It is high.
The preparation of 4 original liquid coloring white flame-proof polylactic acid fiber B of comparative example
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 master batch, when polylactic acid powder is mixed with environmentally friendly colorant and auxiliary material, dispersion effect is poor,
Part occurs to reunite, master batch prepares difficult.
Occurs spinning moulding difficulty in step B, the quality and technical index of product is unstable.
After tested, the fibre technology index that prepared by comparative example 4 is fracture strength：2.8cN/dtex, elongation at break：
24.3%, line density deviation ratio：7.2%, length variation rate：8.4%, crispation number：6.6/25mm, crimp percent：7.8%, 130
DEG C dry-hot shrinkage：6.4%, regain：0.3%, line density：1.5dtex, biological decomposition rate：89%, fusing point：175 DEG C, pole
Limited oxygen index LOI：29%, fastness to soaping：3 grades.Indices are not as good as 1 product of embodiment.
The preparation of 5 original liquid coloring green acid fiber by polylactic A of comparative example
Auxiliary material is not added with, other raw materials, weight ratio are the same as embodiment 3.
In step A prepares green master batch, when polylactic acid powder is with environmentally friendly coloring material for mixing, reunite serious, master batch system
Standby failure.
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 be equal 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 (10)
1. a kind of preparation method of original liquid coloring flame-proof polylactic acid fiber, which is characterized in that include the following steps：
A, the preparation of original liquid coloring flame-proof polylactic acid master batch：
65~82wt% polylactic acid powder, 5~15wt% environmental protection colorant, fire retardant 5~10% and 5~15wt% auxiliary materials are mixed
Uniformly, original liquid coloring flame-proof polylactic acid master batch is made through screw extruder extruding pelletization after drying；The auxiliary material is polyethylene
The mixture of wax and nano-calcium carbonate；
B, the preparation of original liquid coloring flame-proof polylactic acid fiber：
5~12wt% original liquid coloring flame-proof polylactic acid master batches and 88~95wt% polylactic acid slices are subjected to spinning and drawing-off obtains
Original liquid coloring flame-proof polylactic acid fiber.
2. the method as described in claim 1, which is characterized in that in step A, the polylactic acid powder is ground by polylactic acid slice
It grinds, size is 100nm~300nm, preferably 140nm~220nm.
3. the method as described in claim 1, which is characterized in that in step A, the environmentally friendly colorant be selected from C.I. Pigment whites 6,
C.I. Pigment white, C.I. face white 18：1st, 12, C.I. paratoneres 101, C.I. pigment red 4s 9：1st, C.I paratoneres 68, C.I pigment yellows
32nd, C.I. pigment yellows 16, C.I. pigment blacks 11, C.I. pigment blacks 15, C.I. solvent yellow 19s, C.I. pigment oranges 24, C.I. pigment
Purple 3, C.I. pigment blue 1s 0, phthalocyanine blue b, C.I. pigment blues 29, C.I pigment blue 1s 7：1st, C.I naphthol greens 8, sun-proof emerald green color lake,
One or more of environmentally-friecarbon carbon black FR8150 and environmentally-friecarbon carbon black FR5200 mixture.
4. the method as described in claim 1, which is characterized in that in step A, the fire retardant is trichlorine pyrophosphate
With the mixture of pentaerythrite.
5. method as claimed in claim 4, which is characterized in that in step A, the fire retardant is 70~80wt% trichlorine cyanogen
The mixture of amine pyrophosphate and 20~30wt% pentaerythrites.
6. the method as described in claim 1, which is characterized in that in step A, the auxiliary material is 40~60wt% polyethylene waxes
With the mixture of 40~60wt% nano-calcium carbonates.
7. the method as described in claim 1, which is characterized in that in step A, extruding pelletization refers specifically to：Polylactic acid slice powder,
Environmentally friendly colorant, fire retardant and auxiliary material be uniformly mixed after through drying, and through screw extruder extrusion molten, extrusion, cooling, tie rod,
Original liquid coloring flame-proof polylactic acid master batch is made in pelletizing and drying.
8. the method as described in claim 1, which is characterized in that in step B, spinning and drawing-off refer specifically to：Original liquid coloring is fire-retardant
Polylactic acid master batch and polylactic acid slice are successively after drying, spinning, winding, molding, boundling, drawing-off, thermal finalization, curling, cut-out
Obtain original liquid coloring flame-proof polylactic acid fiber.
9. method as claimed in claim 8, which is characterized in that in step B, the technological parameter of spinning and drawing-off is：Stoste
116~120 DEG C, 12~20h of drying time of color flame-proof polylactic acid master batch, polylactic acid slice drying temperature, spinning pump is for amount
For 780~1000g/min, spinning temperature is 225~260 DEG C, and spinning speed is 980~1100m/min, drafting multiple 3.1
~3.6 times.
10. the original liquid coloring flame-proof polylactic acid fiber prepared by claim 1~9 any one of them method.
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| CN112553707A (en) * | 2020-11-13 | 2021-03-26 | 浙江汇隆新材料股份有限公司 | Preparation method of flame-retardant colored functional environment-friendly fiber |
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| CN112553707A (en) * | 2020-11-13 | 2021-03-26 | 浙江汇隆新材料股份有限公司 | Preparation method of flame-retardant colored functional environment-friendly fiber |
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Application publication date: 20180615 |