CN108315836A - A kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber - Google Patents
A kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber Download PDFInfo
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- CN108315836A CN108315836A CN201810212814.XA CN201810212814A CN108315836A CN 108315836 A CN108315836 A CN 108315836A CN 201810212814 A CN201810212814 A CN 201810212814A CN 108315836 A CN108315836 A CN 108315836A
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- pigment
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- original liquid
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- 239000000835 fiber Substances 0.000 title claims abstract description 81
- 229920000728 polyester Polymers 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000004040 coloring Methods 0.000 title claims abstract description 24
- 239000007788 liquid Substances 0.000 title claims abstract description 21
- 239000000049 pigment Substances 0.000 claims abstract description 40
- 239000004595 color masterbatch Substances 0.000 claims abstract description 26
- 238000009998 heat setting Methods 0.000 claims abstract description 15
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000004806 packaging method and process Methods 0.000 claims abstract description 8
- 230000032050 esterification Effects 0.000 claims abstract description 3
- 238000005886 esterification reaction Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 37
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 35
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 28
- 238000002788 crimping Methods 0.000 claims description 14
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 238000009987 spinning Methods 0.000 claims description 12
- 239000003381 stabilizer Substances 0.000 claims description 11
- 230000009471 action Effects 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000012805 post-processing Methods 0.000 claims description 7
- 238000007493 shaping process Methods 0.000 claims description 7
- 230000003068 static effect Effects 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 239000000908 ammonium hydroxide Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000012982 microporous membrane Substances 0.000 claims description 6
- 150000008301 phosphite esters Chemical class 0.000 claims description 6
- 239000004576 sand Substances 0.000 claims description 6
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- JVLRYPRBKSMEBF-UHFFFAOYSA-K diacetyloxystibanyl acetate Chemical compound [Sb+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JVLRYPRBKSMEBF-UHFFFAOYSA-K 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 4
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- XVBXJBGOQQLLAO-UHFFFAOYSA-J [Ti+4].C=C.OCC([O-])=O.OCC([O-])=O.OCC([O-])=O.OCC([O-])=O Chemical compound [Ti+4].C=C.OCC([O-])=O.OCC([O-])=O.OCC([O-])=O.OCC([O-])=O XVBXJBGOQQLLAO-UHFFFAOYSA-J 0.000 claims description 3
- 229910052787 antimony Inorganic materials 0.000 claims description 3
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N nitrous oxide Inorganic materials [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims 2
- 206010011224 Cough Diseases 0.000 claims 1
- 150000005125 dioxazines Chemical class 0.000 claims 1
- QKQGPTWJARHPJQ-UHFFFAOYSA-N pyrazolo[3,4-h]quinolin-2-one Chemical class C1=C2N=NC=C2C2=NC(=O)C=CC2=C1 QKQGPTWJARHPJQ-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000012209 synthetic fiber Substances 0.000 abstract description 2
- 229920002994 synthetic fiber Polymers 0.000 abstract description 2
- 238000002074 melt spinning Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 238000004043 dyeing Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- 238000010924 continuous production Methods 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 238000013459 approach Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical class C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 238000010186 staining Methods 0.000 description 2
- UXYHZIYEDDINQH-UHFFFAOYSA-N C1=CNC2=C3C=NN=C3C=CC2=C1 Chemical compound C1=CNC2=C3C=NN=C3C=CC2=C1 UXYHZIYEDDINQH-UHFFFAOYSA-N 0.000 description 1
- 238000012356 Product development Methods 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 150000004885 piperazines Chemical class 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- -1 quinoline ketone Chemical class 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
Abstract
The invention belongs to synthetic fibers field of production, and in particular to the production technology of polyester fiber, the method that especially a kind of original liquid coloring prepares high color fastness differential polyester staple fiber.This method mainly includes the following steps：（1）The preparation of color master-batch；（2）Raw material is uniformly mixed esterification；（3）Temperature is increased, polycondensation obtains polyester fondant；（4）Melt spinning obtains as-spun fibre；（5）As-spun fibre is through drawing-off, nervous thermal finalization, curling, relaxation heat setting；（6）Tow cut-out, packaging.The method that a kind of original liquid coloring provided by the invention prepares high color fastness differential polyester staple fiber, the color master-batch thermal stability and compatibility of preparation are preferable, and the binding force of pigment and polyester is stronger at high temperature, the height of the color fastness of fiber；This method operability is strong, and rational technology is of low cost, and production efficiency is high, environment friendly and pollution-free, it can be achieved that industrialized production.
Description
Technical field
The invention belongs to synthetic fibers field of production, and in particular to the production technology of polyester fiber, it is especially a kind of
The method that original liquid coloring prepares high color fastness differential polyester staple fiber.
Background technology
In recent years, as the improvement of people's living standards, people increase the demand of high-quality colour fabric year by year.Though
So by development for many years, China rapidly becomes the first in the world experimental branch line big country, but is mainly expanded with normal polyester yield
Based on, routinize, unification it is serious, there are wretched insufficiency, differentiation of product rates in terms of product development and technological innovation
Well below developed country.Therefore the colorful polyester fiber for finding suitable method continuous production high quality is significant, helps
In the differential level for improving PET industry.
Polyester fiber is with ethylene glycol using terephthalic acid (TPA) and its derivative by a kind of purposes obtained by polycondensation reaction
Extensive chemical fibre, the fibrous fracture intensity and elasticity modulus are high, and thermal finalization is excellent, and heat resistance and light resistance are good, are synthesis
One of kind with fastest developing speed in fiber.Polyester fiber molecules align is regular, and closely, crystallinity and the degree of orientation are high, and lack
Stainable group, therefore, polyster fibre dyeing is more difficult, and polyster fibre dyeing equipment requirement is high, invests more, three-protection design
The problems such as trouble, has become the key technical problem of its development of puzzlement.
For polyester textile, the color method used at present mainly has two major classes：First, using traditional weaving
Technique is by polyester fiber (spinning) woven fabric, and using the colouring method of high temperature, high pressure or adding carrier, what is generated in dyeing course has
Color sewage disposal difficulty is big, of high cost, if direct emission can cause serious environmental pollution.Second is that before being spun using polyester fiber
(stoste) colours, and original liquid coloring is added colorant progress spinning and is directly prepared into colouredization i.e. in the spinning solution of chemical fibre
The method for learning fiber.The technology prepare colored fibre color aberration is small, light fastness is high, it is often more important that downstream is omitted
Chemical fibers dyeing link meets the demand for development of current energy-saving and emission-reduction, be solve that some molecules aligns are regular, crystallinity is high and
Lack the important means that can be contaminated the difficult dyeing chemistry fibre staining of group, reduce dyeing pollution, improve color fastness, reduce cost,
With good development prospect.But existing polymerization process colouring is mainly used for the high-volume serialization of conventional black silk
Production, the disadvantage is that：Single varieties can not carry out the high-volume continuous production of multi-color system.Because polymerization process colouring
Key, which is to select to mix with the good suitable pigment of polyester compatibility and dispersant, evenly dispersed has mill base material.Polyester is poly-
It closes and spinning generally carries out at a high temperature of 280-290 DEG C, it is desirable that pigment energy high temperature resistant, and the knot of pigment and polyester at high temperature
Resultant force is stronger.And the prior art can not also solve the evenly dispersed of multi-color system pigment and the consistency problem with polyester.
Invention content
For overcome the deficiencies in the prior art, it is an object of the invention to：There is provided one kind can make pigment uniform in the polyester
Dispersion, high temperature resistant, can carrying out the original liquid coloring of the high-volume continuous production of multi-color system, to prepare the differential terylene of high color fastness short
The method of fiber.
In order to achieve the object of the present invention, the present invention adopts the following technical scheme that：
A kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber, this approach includes the following steps:
(1) preparation of color master-batch：(a) it is 25-35%'s to take cetyl trimethylammonium bromide to be scattered in mass fraction
In ethanol water, mass fraction 1-3%, then ammonium hydroxide is added thereto, adjusting pH value is 10-11, in the item of magnetic agitation
Under part 1-2h is stirred in 25 DEG C；(b) it is 1 to weigh mass ratio：1 ethyl orthosilicate and pigment are added to the reaction solution of step (a)
In, mass fraction 1-3% reacts 5-8h；(c) reaction solution of step (b) is placed in sand mill, adds solution gross mass
The Silane coupling agent KH550 of 1-5% be ground 3-5h, then after filtering with microporous membrane, washing is placed in 85-90
It is dried in DEG C air dry oven, obtains required color master-batch；
(2) 1-6% color master-batch, 40-50% ethylene glycol are added in reaction kettle, are stirred at being 50-60 DEG C in temperature
1-2h；
(3) by 50-60% terephthalic acid (TPA)s, 0.1-0.5% catalyst, be added in the reaction kettle of step (2) and carry out ester
Change reaction, control system temperature reacts 2-3h at 230-255 DEG C；
(4) 0.5-1.5% stabilizers are added, then vacuumize, quickly increase temperature to 260-280 DEG C of progress polycondensation, contracting
Poly- reaction 3-5h, the inherent viscosity of final polyester fondant in 0.55-0.68dL/g, the vacuum degree control of reaction kettle 70Pa with
It is interior；
(5) polyester fondant is pumped to secondary filter through melt, and filtered melt is set the static mixing in pipeline
Enter spinning manifold after device, in the triangles through the cooling as-spun fibre for obtaining condition of high vacuum degree under the action of empty spinneret；
(6) as-spun fibre carries out post-processing after balance, carries out drawing-off, nervous thermal finalization successively；
(7) fiber after drawn enters in crimping machine, in crimper formed high density crispation number fiber, after pass through
Reciprocal trolley, which is sent into J-shaped case, to be arranged, and the fiber arranged, which enters in loosening heat setting machine, to be carried out shaping；
(8) tow cut-out, packaging.
Further, pigment described above is carbon black, azo pigment, triarylmethane compound pigment, phthalocyanine pigment, bis- Evil
Piperazine class pigment, quinophthalone class pigment, nitrogen methine class pigment, nitro and nitrous base class pigment, condensed ring ketone pigment, pyrazolo quinoline
One kind in quinoline ketone pigment, pyroles pigment or indoline-like pigment.
Further, the grain size of color master-batch described above is 50-500nm.
Further, catalyst described above is titanium ethylene glycolate, tetraethyl titanate, metatitanic acid orthocarbonate, antimony glycol, three vinegar
One or more of sour antimony.
Further, stabilizer described above is phosphoric acid and phosphite ester 1-3 in mass ratio：The compound of 1 composition.
Further, the level-one oil bath drawing temperature described in above-mentioned steps (6) is 65-75 DEG C, and second steam drawing temperature is
100-130 DEG C, nervous heat setting temperature is 180-220 DEG C, and whole drafting multiple is at 3.5-4.5 times.
Further, the temperature of the crimping machine described in above-mentioned steps (7) is 80-120 DEG C, and main pressure is 150-180kPa, back pressure
For 175-200kPa, 110 DEG C -125 DEG C of setting temperature, setting time 0.5-1h.
The present invention has following advantageous effect：
(1) method that a kind of original liquid coloring provided by the invention prepares high color fastness differential polyester staple fiber, the present invention
The color master-batch of preparation can by coating dye in silicon dioxide microsphere, not only can ensure hot stage dyestuff not
It will appear decomposition and distillation, greatly improve the high high-temp stability of organic pigment；And the color master-batch and resin of 50-500nm
Melt has preferable compatibility, ensure that the stability of spinning, avoid being directly added into pigment and the agglomeration traits that occur.
(2) method that a kind of original liquid coloring provided by the invention prepares high color fastness differential polyester staple fiber, the present invention
Color master-batch carrier silicas, surface be rich in hydroxyl, on the one hand improve compatibility, on the other hand in polyester polymerization process
In, esterification can occur with part material terephthalic acid (TPA) so that the binding force of pigment and polyester is stronger at high temperature, from
And prepare the polyester fiber of high color fastness.
(3) method that a kind of original liquid coloring provided by the invention prepares high color fastness differential polyester staple fiber, the present invention
The stabiliser compositions of selection are conducive to the stability of system during raising polyester condensation, avoid the degradation of polyester under high temperature,
Improve the intensity of polyester fiber.
(4) method that a kind of original liquid coloring provided by the invention prepares high color fastness differential polyester staple fiber, it is operable
Property strong, rational technology, of low cost, production efficiency is high, environment friendly and pollution-free, it can be achieved that industrialized production.
Description of the drawings
Fig. 1 is the process flow chart for a kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber.
Specific implementation mode
Presently in connection with embodiment, the present invention is described in further detail.
Embodiment 1
A kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber, this approach includes the following steps:
(1) preparation of color master-batch：(a) cetyl trimethylammonium bromide is taken to be scattered in the ethyl alcohol that mass fraction is 25%
In aqueous solution, mass fraction 1%, then ammonium hydroxide is added thereto, it is 10 to adjust pH value, in 25 DEG C under conditions of magnetic agitation
Stir 2h；(b) it is 1 to weigh mass ratio：1 ethyl orthosilicate and quinophthalone class pigment is added in the reaction solution of step (a), matter
It is 1% to measure score, reacts 8h；(c) reaction solution of step (b) is placed in sand mill, adds 1% silicon of solution gross mass
Alkane coupling agent KH550 is ground 3h, and then after filtering with microporous membrane, washing is placed in 85 DEG C of air dry ovens and dries
It is dry, obtain the required color master-batch that grain size is 50nm；
(2) 1% color master-batch, 50% ethylene glycol are added in reaction kettle, 1h is stirred at being 60 DEG C in temperature；
(3) by 50% terephthalic acid (TPA), 0.1% titanium ethylene glycolate, be added in the reaction kettle of step (2) be esterified it is anti-
It answers, control system temperature reacts 3h at 230 DEG C；
(4) 0.5% phosphoric acid and phosphite ester in mass ratio 1 is added：1 composition stabilizer, then vacuumizes, quickly increases temperature
Degree is to 260 DEG C of progress polycondensations, and polycondensation reaction 3h, the inherent viscosity of final polyester fondant is in 0.55dL/g, the vacuum degree of reaction kettle
Control is within 70Pa；
(5) polyester fondant is pumped to secondary filter through melt, and filtered melt is set the static mixing in pipeline
Enter spinning manifold after device, in the triangles through the cooling as-spun fibre for obtaining condition of high vacuum degree under the action of empty spinneret；
(6) as-spun fibre carries out post-processing after balance, carries out drawing-off, nervous thermal finalization, wherein level-one oil bath successively
Drawing temperature is 65 DEG C, and second steam drawing temperature is 100 DEG C, and nervous heat setting temperature is 180 DEG C, and whole drafting multiple exists
3.5 again；
(7) fiber after drawn enters in crimping machine, in crimper formed high density crispation number fiber, after pass through
Reciprocal trolley, which is sent into J-shaped case, to be arranged, and the fiber arranged, which enters in loosening heat setting machine, to be carried out shaping, wherein crimping machine
Temperature be 80 DEG C, it is main pressure be 150kPa, back pressure 175kPa, 110 DEG C DEG C of setting temperature, setting time 0.5h；
(8) tow cut-out, packaging.
Embodiment 2
(1) preparation of color master-batch：(a) cetyl trimethylammonium bromide is taken to be scattered in the ethyl alcohol that mass fraction is 30%
In aqueous solution, mass fraction 2%, then ammonium hydroxide is added thereto, it is 11 to adjust pH value, in 25 DEG C under conditions of magnetic agitation
Stir 1.5h；(b) it is 1 to weigh mass ratio：1 ethyl orthosilicate and condensed ring ketone pigment is added in the reaction solution of step (a),
Mass fraction is 2%, reacts 5-8h；(c) reaction solution of step (b) is placed in sand mill, adds the 3% of solution gross mass
Silane coupling agent KH550 be ground 4h, then after filtering with microporous membrane, washing, be placed in 88 DEG C of air dry ovens
Middle drying obtains the required color master-batch that grain size is 300nm；
(2) 3% color master-batch, 40% ethylene glycol are added in reaction kettle, 1-2h is stirred at being 50-60 DEG C in temperature；
(3) by 60% terephthalic acid (TPA), 0.1-0.5% tetraethyl titanates, be added in the reaction kettle of step (2) and carry out ester
Change reaction, control system temperature reacts 2.5h at 240 DEG C；
(4) 1% phosphoric acid and phosphite ester in mass ratio 2 is added：1 composition stabilizer stabilizer, then vacuumizes, quickly rises
High-temperature is to 270 DEG C of progress polycondensations, polycondensation reaction 4h, the inherent viscosity of final polyester fondant in 0.62dL/g, reaction kettle it is true
Reciprocal of duty cycle controls within 70Pa；
(5) polyester fondant is pumped to secondary filter through melt, and filtered melt is set the static mixing in pipeline
Enter spinning manifold after device, in the triangles through the cooling as-spun fibre for obtaining condition of high vacuum degree under the action of empty spinneret；
(6) as-spun fibre carries out post-processing after balance, carries out drawing-off, nervous thermal finalization, wherein level-one oil bath successively
Drawing temperature is 70 DEG C, and second steam drawing temperature is 120 DEG C, and nervous heat setting temperature is 200 DEG C, and whole drafting multiple is 4
Times；
(7) fiber after drawn enters in crimping machine, in crimper formed high density crispation number fiber, after pass through
Reciprocal trolley, which is sent into J-shaped case, to be arranged, and the fiber arranged, which enters in loosening heat setting machine, to be carried out shaping, wherein crimping machine
Temperature be 100 DEG C, it is main pressure be 165kPa, back pressure 190kPa, 120 DEG C DEG C of setting temperature, setting time 1h；
(8) tow cut-out, packaging.
Embodiment 3
(1) preparation of color master-batch：(a) cetyl trimethylammonium bromide is taken to be scattered in the ethyl alcohol that mass fraction is 35%
In aqueous solution, mass fraction 3%, then ammonium hydroxide is added thereto, it is 11 to adjust pH value, in 25 DEG C under conditions of magnetic agitation
Stir 1h；(b) it is 1 to weigh mass ratio：1 ethyl orthosilicate and phthalocyanine pigment is added in the reaction solution of step (a), quality
Score is 3%, reacts 5h；(c) reaction solution of step (b) is placed in sand mill, adds 5% silane of solution gross mass
Coupling agent KH550 is ground 3h, and then after filtering with microporous membrane, washing is placed in 90 DEG C of air dry ovens and dries,
Obtain the required color master-batch that grain size is 500nm；
(2) 6% color master-batch, 45% ethylene glycol are added in reaction kettle, 1h is stirred at being 60 DEG C in temperature；
(3) by 55% terephthalic acid (TPA), 0.5% antimony triacetate, be added in the reaction kettle of step (2) be esterified it is anti-
It answers, control system temperature reacts 2h at 255 DEG C；
(4) 1.5% phosphoric acid and phosphite ester in mass ratio 3 is added：The stabilizer of 1 composition, then vacuumizes, and quickly increases
Temperature is to 280 DEG C of progress polycondensations, and polycondensation reaction 3h, the inherent viscosity of final polyester fondant is in 0.68dL/g, the vacuum of reaction kettle
Degree control is within 70Pa；
(5) polyester fondant is pumped to secondary filter through melt, and filtered melt is set the static mixing in pipeline
Enter spinning manifold after device, in the triangles through the cooling as-spun fibre for obtaining condition of high vacuum degree under the action of empty spinneret；
(6) as-spun fibre carries out post-processing after balance, carries out drawing-off, nervous thermal finalization, wherein level-one oil bath successively
Drawing temperature is 75 DEG C, and second steam drawing temperature is 130 DEG C, and nervous heat setting temperature is 220 DEG C, and whole drafting multiple exists
4.5 again；
(7) fiber after drawn enters in crimping machine, in crimper formed high density crispation number fiber, after pass through
Reciprocal trolley, which is sent into J-shaped case, to be arranged, and the fiber arranged, which enters in loosening heat setting machine, to be carried out shaping, wherein crimping machine
Temperature be 120 DEG C, it is main pressure be 180kPa, back pressure 200kPa, 125 DEG C DEG C of setting temperature, setting time 1h；
(8) tow cut-out, packaging.
Comparative example 1 is compared with embodiment 3
(1) phthalocyanine pigment, 45% ethylene glycol are added in reaction kettle, 1h is stirred at being 60 DEG C in temperature；
(2) by 55% terephthalic acid (TPA), 0.5% antimony triacetate, be added in the reaction kettle of step (2) be esterified it is anti-
It answers, control system temperature reacts 2h at 255 DEG C；
(3) 1.5% phosphoric acid and phosphite ester in mass ratio 3 is added：The stabilizer of 1 composition, then vacuumizes, and quickly increases
Temperature is to 280 DEG C of progress polycondensations, and polycondensation reaction 3h, the inherent viscosity of final polyester fondant is in 0.68dL/g, the vacuum of reaction kettle
Degree control is within 70Pa；
(4) polyester fondant is pumped to secondary filter through melt, and filtered melt is set the static mixing in pipeline
Enter spinning manifold after device, in the triangles through the cooling as-spun fibre for obtaining condition of high vacuum degree under the action of empty spinneret；
(5) as-spun fibre carries out post-processing after balance, carries out drawing-off, nervous thermal finalization, wherein level-one oil bath successively
Drawing temperature is 75 DEG C, and second steam drawing temperature is 130 DEG C, and nervous heat setting temperature is 220 DEG C, and whole drafting multiple exists
4.5 again；
(6) fiber after drawn enters in crimping machine, in crimper formed high density crispation number fiber, after pass through
Reciprocal trolley, which is sent into J-shaped case, to be arranged, and the fiber arranged, which enters in loosening heat setting machine, to be carried out shaping, wherein crimping machine
Temperature be 120 DEG C, it is main pressure be 180kPa, back pressure 200kPa, 125 DEG C DEG C of setting temperature, setting time 1h；
(7) tow cut-out, packaging.
Comparative example 2 is compared with embodiment 3
(1) preparation of color master-batch：(a) cetyl trimethylammonium bromide is taken to be scattered in the ethyl alcohol that mass fraction is 35%
In aqueous solution, mass fraction 3%, then ammonium hydroxide is added thereto, it is 11 to adjust pH value, in 25 DEG C under conditions of magnetic agitation
Stir 1h；(b) it is 1 to weigh mass ratio：1 ethyl orthosilicate and phthalocyanine pigment is added in the reaction solution of step (a), quality
Score is 3%, reacts 5h；(c) reaction solution of step (b) is placed in sand mill, adds 5% silane of solution gross mass
Coupling agent KH550 is ground 3h, and then after filtering with microporous membrane, washing is placed in 90 DEG C of air dry ovens and dries,
Obtain the required color master-batch that grain size is 500nm；
(2) 6% color master-batch, 45% ethylene glycol are added in reaction kettle, 1h is stirred at being 60 DEG C in temperature；
(3) by 55% terephthalic acid (TPA), 0.5% antimony triacetate, be added in the reaction kettle of step (2) be esterified it is anti-
It answers, control system temperature reacts 2h at 255 DEG C；
(4) it vacuumizes, quickly increases temperature to 280 DEG C of progress polycondensations, the characteristic of polycondensation reaction 3h, final polyester fondant are viscous
Degree is in 0.68dL/g, and the vacuum degree control of reaction kettle is within 70Pa；
(5) polyester fondant is pumped to secondary filter through melt, and filtered melt is set the static mixing in pipeline
Enter spinning manifold after device, in the triangles through the cooling as-spun fibre for obtaining condition of high vacuum degree under the action of empty spinneret；
(6) as-spun fibre carries out post-processing after balance, carries out drawing-off, nervous thermal finalization, wherein level-one oil bath successively
Drawing temperature is 75 DEG C, and second steam drawing temperature is 130 DEG C, and nervous heat setting temperature is 220 DEG C, and whole drafting multiple exists
4.5 again；
(7) fiber after drawn enters in crimping machine, in crimper formed high density crispation number fiber, after pass through
Reciprocal trolley, which is sent into J-shaped case, to be arranged, and the fiber arranged, which enters in loosening heat setting machine, to be carried out shaping, wherein crimping machine
Temperature be 120 DEG C, it is main pressure be 180kPa, back pressure 200kPa, 125 DEG C DEG C of setting temperature, setting time 1h；
(8) tow cut-out, packaging.
Product testing such as table 1：
Table 1
As it can be seen from table 1 polyester fiber prepared by color master-batch and stabilizer that embodiment 1-3 is added, fiber it is strong
Degree is high, and color fastness to washing (discoloration, staining) reaches 4-5 grades, and color fastness to light can reach 7 grades, the whole color fastness of polyester fiber
It is higher, and directly polyester system is added in pigment by comparative example 1, fiber color fastness obtained is poor, and comparative example 2 is steady due to not being added
Determine agent, the intensity of polyester fiber declines.
It is enlightenment with above-mentioned desirable embodiment according to the present invention, through the above description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the contents of the specification, it is necessary to determine its technical scope according to right.
Claims (7)
1. a kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber, it is characterised in that:This method include with
Lower step:
（1）The preparation of color master-batch：（a）Cetyl trimethylammonium bromide is taken to be scattered in the ethanol water that mass fraction is 25-35%
In solution, mass fraction 1-3%, then ammonium hydroxide is added thereto, adjusting pH value is 10-11, in 25 under conditions of magnetic agitation
DEG C stirring 1-2h；（b）It is 1 to weigh mass ratio：1 ethyl orthosilicate and pigment is added to step（a）Reaction solution in, quality point
Number is 1-3%, reaction 5-8 h；（c）By step（b）Reaction solution be placed in sand mill, add the 1-5%'s of solution gross mass
Silane coupling agent KH550 is ground 3-5h, and then after filtering with microporous membrane, it is dry to be placed in 85-90 DEG C of air blast for washing
It is dried in dry case, obtains required color master-batch；
（2）1-6% color master-batch, 40-50% ethylene glycol are added in reaction kettle, 1-2h is stirred at being 50-60 DEG C in temperature；
（3）By 50-60% terephthalic acid (TPA)s, 0.1-0.5% catalyst, it is added to step（2）Reaction kettle in carry out esterification,
Control system temperature reacts 2-3h at 230-255 DEG C；
（4）0.5-1.5% stabilizers are added, then vacuumize, quickly increase temperature to 260-280 DEG C of progress polycondensation, polycondensation reaction
3-5h, the inherent viscosity of final polyester fondant is in 0.55-0.68dL/g, and the vacuum degree control of reaction kettle is within 70Pa；
（5）Polyester fondant is pumped to secondary filter through melt, filtered melt be set pipeline static mixer it
Enter spinning manifold afterwards, in the triangles through the cooling as-spun fibre for obtaining condition of high vacuum degree under the action of empty spinneret；
（6）As-spun fibre carries out post-processing after balance, carries out drawing-off, nervous thermal finalization successively；
（7）Fiber after drawn enters in crimping machine, and the fiber of high density crispation number is formed in crimper, after through reciprocal
Trolley is sent into J shape casees and is arranged, and the fiber arranged, which enters in loosening heat setting machine, to be carried out shaping；
（8）Tow cut-out, packaging.
2. a kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber as described in claim 1, feature
It is:The pigment is carbon black, azo pigment, triarylmethane compound pigment, phthalocyanine pigment, dioxazines pigment, quinoline phthalein
Ketone pigment, nitrogen methine class pigment, nitro and nitrous base class pigment, condensed ring ketone pigment, pyrazolo quinolinones pigment, pyrrole
Cough up one kind in class pigment or indoline-like pigment.
3. a kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber as described in claim 1, feature
It is:The grain size of the color master-batch is 50-500nm.
4. a kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber as described in claim 1, feature
It is:The catalyst is one kind in titanium ethylene glycolate, tetraethyl titanate, metatitanic acid orthocarbonate, antimony glycol, antimony triacetate
Or it is several.
5. a kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber as described in claim 1, feature
It is:The stabilizer is phosphoric acid and phosphite ester 1-3 in mass ratio：The compound of 1 composition.
6. a kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber as described in claim 1, feature
It is:Step（6）The level-one oil bath drawing temperature is 65-75 DEG C, and second steam drawing temperature is 100-130 DEG C, tightly
It is 180-220 DEG C to open heat setting temperature, and whole drafting multiple is at 3.5-4.5 times.
7. a kind of method that original liquid coloring prepares high color fastness differential polyester staple fiber as described in claim 1, feature
It is:Step（7）The temperature of the crimping machine be 80-120 DEG C, it is main pressure be 150-180kPa, back pressure 175-200kPa,
110 DEG C -125 DEG C of setting temperature, setting time 0.5-1h.
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| CN110777446A (en) * | 2019-11-25 | 2020-02-11 | 杭州奔马化纤纺丝有限公司 | Preparation process of non-dyed regenerated polyester staple fiber |
| CN110886031A (en) * | 2019-12-06 | 2020-03-17 | 江苏垶恒复合材料有限公司 | Preparation method of high-color-fastness stock solution coloring regenerated polyester fiber |
| CN111270335A (en) * | 2019-11-18 | 2020-06-12 | 厦门翔鹭化纤股份有限公司 | Antibacterial polyester fiber and preparation method thereof |
| CN115717278A (en) * | 2022-10-24 | 2023-02-28 | 桐乡市励志特种纤维股份有限公司 | Stock solution coloring regenerated triangular special-shaped polyester long fiber and preparation method thereof |
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Application publication date: 20180724 |