CN109706546A - A kind of graphene sea-island fibre and its manufacturing method - Google Patents
A kind of graphene sea-island fibre and its manufacturing method Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 191
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 187
- 239000000835 fiber Substances 0.000 title claims abstract description 101
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 229920000728 polyester Polymers 0.000 claims abstract description 73
- 239000002243 precursor Substances 0.000 claims abstract description 26
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 19
- 230000008569 process Effects 0.000 claims abstract description 14
- 238000005520 cutting process Methods 0.000 claims abstract description 10
- 238000009998 heat setting Methods 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 57
- 238000002360 preparation method Methods 0.000 claims description 36
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 23
- 239000002028 Biomass Substances 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 21
- 238000002844 melting Methods 0.000 claims description 17
- 230000008018 melting Effects 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 239000004744 fabric Substances 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 16
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- 238000009987 spinning Methods 0.000 claims description 13
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- 238000003756 stirring Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 238000006068 polycondensation reaction Methods 0.000 claims description 8
- 238000004804 winding Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 6
- -1 polyethylene terephthalate Polymers 0.000 claims description 6
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 5
- 229920002415 Pluronic P-123 Polymers 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 230000008676 import Effects 0.000 claims description 5
- 238000004513 sizing Methods 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 150000001336 alkenes Chemical class 0.000 claims description 4
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims description 4
- 229910001388 sodium aluminate Inorganic materials 0.000 claims description 4
- 239000004575 stone Substances 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 2
- HQPMKSGTIOYHJT-UHFFFAOYSA-N ethane-1,2-diol;propane-1,2-diol Chemical compound OCCO.CC(O)CO HQPMKSGTIOYHJT-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 229920001993 poloxamer 188 Polymers 0.000 claims description 2
- 229920001992 poloxamer 407 Polymers 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 238000007730 finishing process Methods 0.000 claims 2
- 235000008331 Pinus X rigitaeda Nutrition 0.000 claims 1
- 235000011613 Pinus brutia Nutrition 0.000 claims 1
- 241000018646 Pinus brutia Species 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 229940071125 manganese acetate Drugs 0.000 claims 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 16
- 239000003921 oil Substances 0.000 abstract description 14
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- 239000004753 textile Substances 0.000 abstract description 9
- 231100000252 nontoxic Toxicity 0.000 abstract description 4
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- 239000010410 layer Substances 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- 239000010902 straw Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
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- VQWQYXBWRCCZGX-UHFFFAOYSA-N acetic acid;manganese Chemical compound [Mn].CC(O)=O.CC(O)=O VQWQYXBWRCCZGX-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
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- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
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- 239000002932 luster Substances 0.000 description 2
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- 241000609240 Ambelania acida Species 0.000 description 1
- 208000019901 Anxiety disease Diseases 0.000 description 1
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- 229920000742 Cotton Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 244000046109 Sorghum vulgare var. nervosum Species 0.000 description 1
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- Artificial Filaments (AREA)
Abstract
A kind of graphene sea-island fibre and its manufacturing method include the following steps: that graphene master batch is made by fat polymerization by graphene functional material, are blended later with PET, melt obtained graphene island component；By graphene island component and soluble polyester sea component melt blending, graphene island precursor is obtained, then through boundling, drawing-off, nervous thermal finalization crimps, oils, relaxation heat setting, graphene sea-island fibre is made in the processes such as cutting.Graphene sea-island fibre of the invention can reduce material surface resistivity, and the electrostatic charge of generation can be released rapidly, while assign material surface certain lubricity, further decrease coefficient of friction, to inhibit and reduce the generation of electrostatic charge；Biocompatibility is good, is a kind of nontoxic, green, efficient function textile, has far infrared, antibacterial bacteriostatic, the anti-static function of graphene fiber concurrently.
Description
Technical field
The invention belongs to synthetic fibers production technical fields, and in particular to a kind of graphene sea-island fibre and its manufacturer
Method.
Background technique
With economy, the development of social life, requirement of the people to multifunctional textile product is increasingly improved, especially nontoxic,
Green, antibacterial bacteriostatic, antistatic, has the function of unique metallic luster, is lasting etc. without chemical dyeing and finishing, natural in color far infrared
Textile it is in great demand.It is island-in-sea type composite fiber fabrics feel soft, smooth, it can be made into highly dense property, hygroscopicity, water repellent
Property, and have the fabric of unique aesthetics and fashionable dress style；Island-in-sea type composite fiber monofilament linear density is small, pulp freeness
Greatly, spreadability, bulkiness, warming and high adsorption, make fabric have extremely strong dust absorption, soil release performance and filterability；Island
Gap is more and close between composite fibre, has excellent waterproof and breathable performance, and heat-insulation warm keeping is made good use of.Island-in-sea type composite fiber is ultra-fine,
Fiber is more soft, and fabric is made, and can produce the core sucting action of capillary, so that fabric is adsorbed more juicy, and can be by these water
Divide and move to fabric surface, makes its evaporation, increase the comfort of dress.Therefore, sea-island fibre has general fibre incomparable
The advantages of, the textile of many high-performance and high added value can be made, such as utilize the shrinkage of high-shrinkage filament, can be made into close
Spend bigger, the higher fabric of water pressure resistance.Though this kind fabric density is very high, quality is slim and graceful, and drapability is good, and the soft feel of color is soft
It is soft and plentiful, appearance Yong Hua and it is warm, while being able to maintain comparable penetrability and gas permeability, wear very comfortable.
Graphene is a kind of New Type of Carbon nanometer light material, has unique monoatomic layer two dimensional crystal structure, Gao Bibiao
Area, high intensity, conductivity, thermal conductivity, screening effect ideal high to the absorption efficiency of each lightlike line.Graphene is known as
The magical material of 21 century " change ", gradually mature perfect with graphene application field related process, mobile phone screen is any
Bending, electric car momentary charge, computer screen thin transparent such as blank sheet of paper these mysterious things will come true.2015
November 30, Chinese industrial and informationization portion, National Development and Reform Commission, the Department of Science and Technology print and distribute " about quickening graphene re-invent industry
Several opinions of development ", proposition forms perfect graphene industrial system to the year two thousand twenty, realizes grapheme material standardization, is
Columnization and cost effective.Grapheme material equally causes extensive concern in terms of functions of textile fabrics exploitation, in the poly- of textile fabric
Fiber mechanics, electric property can be significantly improved by adding a small amount of graphene in conjunction or spinning process.It is used to prepare the graphite of fiber
Olefinic functionality material can be obtained by different preparation methods, such as mechanical stripping method, CVD method, chemistry redox method, intercalation stripping
Method, biomass resource hydrothermal carbonization etc., can have certain impurity elements, carbon in the graphene that prior art preparation obtains
Other allotropes or the non-single layer of the number of plies even graphene-structured (such as 3 layers, 5 layers, 10 layers, 20 layers etc.) of multilayer.Biology
Matter graphene is with agricultural wastes such as cornstalk, corncob, kaoliang stalk, megasse, bagasse, furfural dregs, xylose residue, wood
What the raw materials such as bits, cotton stalk were prepared by biomass resource hydrothermal carbonization mode.
Chinese patent CN106702530A discloses a kind of sea-island fibre, and the sea-island fibre is by by graphene and nanometer function
Can particle and the first island component it is pre-dispersed after be made nano functional master batch, then with the second island component after evenly mixing with extra large component one
It rises and carries out blend melt spinning, the sea-island fibre with specific function effect is made.The patent points out that sea-island fibre itself is opposite
Relatively thin (﹤ 0.05D), fiber mechanical performance itself is poor, causes the mechanical performance of fabric finished product and fuzz balls performance poor, and receives
The addition of rice functional particles certainly will more influence the mechanical performance of fiber.Therefore the patent is while being added nano functional particle
Graphene is added, the addition of graphene can improve the mechanical performance of sea-island fibre.It can be seen that the graphene of the patent be intended only as it is auxiliary
Material is helped, the purpose of addition is merely to make functional fibre obtain better mechanical performance.So far, have no that graphene is special
It is used to prepare the relevant report for washing sea-island fibre.
Summary of the invention
The purpose of the present invention is to provide a kind of graphene sea-island fibre and its manufacturing method, which can reduce material
Expect surface resistivity, the electrostatic charge of generation is released rapidly, while assigning material surface certain lubricity, further decrease and rub
Coefficient is wiped, to inhibit and reduce the generation of electrostatic charge；Biocompatibility is good, is a kind of nontoxic, green, efficient function spinning
Fabric has far infrared, antibacterial bacteriostatic, the anti-static function of graphene fiber concurrently.
In order to achieve the above objectives, the technical scheme is that
The present invention by graphene functional material by fat polymerization be made graphene master batch, later with PET polyester blend,
It melts and graphene polyester island component is made；By graphene polyester island component and soluble polyester sea component melt blending, stone is obtained
Black alkene island precursor, then through boundling, drawing-off, nervous thermal finalization, crimp, oil, graphite is made in relaxation heat setting, the processes such as cutting
Alkene sea-island fibre.
Specifically, a kind of manufacturing method of graphene sea-island fibre provided by the invention comprising following steps:
Step S1: the preparation of graphene master batch: by weight percentage by 30%~65% graphene powder, 10%~
25% dispersing agent and 15%~30% surfactant mixing, it is agitated, dispersion, be made graphene slurries；Again by graphite
Alkene slurries are blended to obtain mixed liquor with p-phthalic acid (PTA), ethylene glycol (EG), add catalyst sodium aluminate or acetic acid
Manganese stirs evenly, and imports in reaction kettle and carries out esterification, and the additional amount of the catalyst is the 0.5~2% of mixed liquor weight；
Mixture after esterification is imported in polycondensation vessel and carries out polycondensation reaction, using preshrunk, final minification, Cast Strip, cooling, granulation, drying,
Graphene master batch is made；
Step S2: the preparation of graphene polyester: by the polyethylene terephthalate (PET) after graphene master batch and drying
It is blended, stirs evenly, graphene polyester is made in screw extruder melting；
Step S3: the preparation of graphene island precursor: the soluble polyester of drying process, graphene polyester are separately dried
Pass through screw extruder melting extrusion afterwards；By after melting extrusion soluble polyester fondant and graphene polyester fondant pass through respectively respectively
From after pipeline, metering pump-metered, it is delivered to spinning manifold respectively, into same fabric of island-in-sea type composite spinneret pack, by island
Respective runner and filtration system in type composite spinneret pack, by soluble polyester fondant and graphene polyester fondant through spinneret
Hole sprays after converging from spinneret orifice, then cooling through air-flow forced, and winding is made using graphene polyester as island component, soluble poly
Ester is the graphene island precursor of sea component；
Step S4: the preparation of graphene sea-island fibre: graphene island precursor prepared by step S3 through boundling, drawing-off,
Nervous thermal finalization, crimp, oil, graphene sea-island fibre is made in relaxation heat setting, the processes such as cutting.
Further, in step S1, the graphene powder particle size is 55nm~90nm.Through testing, partial size exists
The compatibility of graphene powder and polyester powder within the scope of 55nm~90nm is good, is not susceptible to reunite, preferred graphene
Diameter of particle is 75nm~88nm.
Also, the graphene powder functional material includes biomass graphene and abiotic matter graphene in step S1.Institute
Stating biomass graphene is prepared in such a way that biomass straw is by biomass resource hydrothermal carbonization, in this way
Biomass graphene obtained has graphene two-dimensional slice structure, far-infrared functional enhancing.The abiotic matter graphene is
Commercial goods, need to only meet graphene powder partial size is 55nm~90nm.
Preferably, in step S1, the weight percent of the graphene powder, dispersing agent and surfactant is distinguished
Are as follows: graphene powder: 30~65%, dispersing agent: 10~25%, surfactant: 10~30%.
It is furthermore preferred that in step S1, the weight percent of the graphene powder, dispersing agent and surfactant are as follows:
60%:25%:15%.
It is furthermore preferred that the weight percent of the graphene powder, dispersing agent and surfactant is distinguished in step S1
Are as follows: 65%:25%:15%.
It is furthermore preferred that the weight percent of the graphene powder, dispersing agent and surfactant is distinguished in step S1
Are as follows: 45%:28%:27%.
Further, in step S1, the surfactant is in ether alcohol sulfate, sucrose ester, alkylolamides
It is a kind of.
In step S1, the dispersing agent is Pluronic P123, in Pluronic F68, Pluronic F127
It is a kind of.All contain hydrophilic chain in the molecular structure of these three dispersing agents, make it have water solubility, also has with graphene by hydrophobic
The connected hydrophobic part of effect.
In step S1, the graphene slurries, p-phthalic acid (PTA), ethylene glycol (EG) weight percent are as follows:
10%~20%:40%~70%:10%~30%.Due to adding graphene ingredient in PTA, it is equivalent to and has been mixed into " impurity ".
In order to make " impurity " to homogenize, graphene slurries, p-phthalic acid (PTA), the weight percent of ethylene glycol (EG) three are non-
Chang Guanjian.
Preferably, the graphene slurries, p-phthalic acid's polyester PTA, ethylene glycol EG weight percent are as follows:
15%:65%:20%.
Preferably, the graphene slurries, p-phthalic acid's polyester PTA, ethylene glycol EG weight percent are as follows:
18%:61%:21%.
In step S2, the graphene master batch is respectively 15%~25% with PET weight percent after drying:
75%~85%.Preferably 18%:82% or 22%:78%.
In step S3, the soluble polyester is one or more of COPET, PVA, PS, PE.Preferably, described
Soluble polyester uses alkali solubility COPET, and basic solvent can be sodium hydroxide or potassium hydroxide solution.
Preferably, in step S3, the fabric of island-in-sea type composite spinneret pack is the spray that sea-island fibre is prepared for melt spinning
Silk component, the composite spinneret pack fitted together by muti-piece distribution plate, filter screen, spinneret, headgear etc., the needle tubing containing " 37 " island
Arrangement, usual island number is 16,36,37,51,64,88, the island 98, Ye You number be more than 100 or even 1000.To reach stable company
Continuous island structure, needle tubing rounded uniform equidistant radial arrangement in island therein, it is ensured that do not separate, protect between island in forming process
Hold monofilament form, while island component adhesion in forming process, i.e., it is good between monofilament lagoon island and island to separate.One of it is preferred that
Island number be 37；It is preferred that two island number be 51.
In step S3, the proportional region that the present invention controls the island Hai Yu is 25:75~35:65, is needed when spinning sea-island fibre
The variation of fiber roundness caused by grout leaking is controlled, the easier grout leaking of the smaller melt of extra large ratio is on the contrary then be not easy grout leaking.
Preferably, in step S3, the filtration system sets two-stage, complementation filtering, and filter sizes precision is 35 mesh~115
Mesh, filter sizes precision are preferably 60 mesh~100 mesh, and filtered bath component is made to reach hyperfine energy continuous production water
It is flat.
In step S3, before spinneret converges, it is described solubility polyester fondant (sea component) temperature control 270 DEG C~
295 DEG C (preferably 275 DEG C~280 DEG C), graphene polyester fondant (island component) temperature is controlled at 270 DEG C~290 DEG C (preferably
275℃)。
In step S4, the drawing-off includes level-one drawing-off, second level drawing-off, and 2.80~3.30 times of drawing-off general times；Level-one is led
It stretches for oil bath drawing-off, oil bath temperature is 75 DEG C~80 DEG C；Second level drawing-off is superheated steam drawing-off, and superheat steam temperature is 110 DEG C
~140 DEG C, preferably 130 DEG C.
In step S4, it is described anxiety thermal finalization be carry out 18 roller sizings, preceding 8 roller heating temperatures be 160 DEG C~165 DEG C,
Lead to cooling water in 10 rollers afterwards to cool down to tow.
In step S4, the relaxation heat setting is 100 DEG C~110 DEG C baking oven relaxation heat settings, leading when relaxation heat setting
Maximum speed is stretched no more than 120m/min.
The present invention also provides a kind of graphene sea-island fibre, the graphene sea-island fibre is prepared by above-mentioned manufacturing method
It obtains.
In the present invention as the graphene polyester of island component in the molten state apparent viscosity with as the solvable of sea component
Property polyester (COPET, PVA, PS or PE) in the molten state apparent viscosity it is close, avoid the generation of melt buckling phenomenon, benefit
In spinning.
The functional tests such as antibacterial, the far infrared performance of graphene sea-island fibre prepared by the present invention use Shanghai De Fulunization
The group norms that fine Co., Ltd participates and draw: T/CCFA01031-2017 " graphene modified dacron staple fiber ", after tested: full
Sufficient far infrared transmissivity >=0.88, Far-infrared spoke shine temperature rise >=2.8 DEG C, Escherichia coli bacteriostasis rate >=75%, Staphylococcus aureus
Bacterium bacteriostasis rate >=75%, Candida albicans bacteriostasis rate >=70%.The test results such as anti-microbial property also meet Shanghai De Fulun simultaneously
Chemical fibre Co., Ltd takes the lead the professional standard of formulation: FZ/T 52035-2014 " antibacterial dacron staple fiber " and GB/T 20944.3-
2008 " the evaluation third portions of antibacterial textile performance: succusion ", the strain of bacteriostasis rate refers to staphylococcus aureus (ATCC
6538), Escherichia coli (ATCC 8739).
After tested, graphene sea-island fibre performance prepared by the present invention meets following index: the breaking strength of fiber: >=
2.0cn/dtex, elongation at break: M1 ± 10.0%, crispation number: M2 ± 4.0/25mm, crimp percent: M3 ± 4.0%, 180 DEG C
Dry-hot shrinkage :≤10.0%, line density: 3.0dtex~5.56dtex.
The present invention is slim and graceful in high-tech sea-island fibre quality, and drapability is good, and color is soft, soft plentiful, appearance harmony
It is magnificent warm, on the basis of moisture-penetrable ventilated, develop the graphene for having antibacterial, antistatic, uvioresistant and far infrared multiple functions concurrently
Sea-island fibre, the graphene sea-island fibre have far infrared, antibacterial bacteriostatic, the anti-static function of graphene fiber, also have only
Special metallic luster, without chemical dyeing and finishing, natural in color is lasting, has expanded the kind and application of sea-island fibre, and new category meets new
Function and new demand.
Beneficial effects of the present invention:
1. existing islands-in-sea bicomponent fibre is using PET or PA as island component, sea component mostly uses greatly PS or PE, then
With the organic solvents such as benzene, toluene remove sea component, but bring in this way environmental pollution, it is inflammable and explosive the problems such as.Of the invention can
Dissolubility polyester preferably uses alkali solubility COPET, efficiently solves the above problem.
2. graphene is used to prepare by the present invention washs sea-island fibre, without functions such as additional addition mineral powder/metal powders
Material can have function far infrared radiation function, far infrared transmissivity >=0.88 at normal temperature, and Far-infrared spoke shines temperature rise >=1.7
℃.So the fiber can automatically adjust under blood heat, draw human peripheral and the radiation energy of itself, generate to people
The beneficial far infrared of body improves microcirculation so that the histiocytic vigor of exciting human, boosts metabolism, and improves immune
Power acts on body-care to reach.The preferred biomass graphene preparation of the present invention, biomass graphene is with biomass straw
Cellulose is raw material in stalk, not only has graphene two-dimensional slice structure, also has enhancing far infrared performance.
3. the nutrient that bacterium has been cut off in the presence of graphene in graphene sea-island fibre provided by the invention supports base, together
Shi Liyong graphene has the performance of high-specific surface area, so, which has absorption peculiar smell, antibacterial suppression
The functions such as bacterium, bacteriostasis rate reach 99% or more.
4. graphene sea-island fibre provided by the invention can reduce material surface resistivity, the electrostatic charge of generation is let out rapidly
Dew, while assigning material surface certain lubricity, coefficient of friction is reduced, to inhibit and reduce the generation of electrostatic charge.
5. graphene sea-island fibre provided by the invention has good biocompatibility, without containing also not generating to human body
Harmful chemical substance and ingredient are a kind of nontoxic, green, efficient function textiles.
Specific embodiment
It elaborates below with reference to embodiment to specific embodiment provided by the invention.
Embodiment 1
The preparation of S1, graphene master batch: 60% 80nm is provided with biomass straw by biomass by weight percentage
Biomass graphene powder that source hydrothermal carbonization mode is prepared, 25% dispersing agent Pluronic P123 and 15% table
Face activating agent ether alcohol sulfate mixing, agitated, dispersion, is made graphene slurries；Again with 15% graphene slurries and 65% essence
Terephthalic acid (TPA) PTA, 20% ethylene glycol EG are blended to obtain mixed liquor, add catalyst sodium aluminate and stir evenly, and import reaction
Esterification is carried out in kettle, the additional amount of the catalyst is the 1% of mixed liquor weight；Mixture after esterification is imported into polycondensation
Polycondensation reaction is carried out in kettle, and using preshrunk, final minification, Cast Strip, cooling, granulation, drying, graphene master batch is made.
The preparation of S2, graphene polyester island component: 18% graphene master batch and 82% PET after drying are total to
It is mixed, it stirs evenly, graphene polyester island component is made in screw extruder melting；
The preparation of S3, graphene island precursor: by soluble polyester sea component COPET, the graphene polyester of drying process
Island group lease making is after respectively system is dry, the melting extrusion in respective screw extruder, and enters through respective pipeline, metering pump same
One spinning pack, then filtered through respective runner, 80 mesh of filtration system, then soluble polyester sea component melt and graphene are poly-
Ester island component melt sprays after spinneret hole converges from spinneret orifice, cooling through air-flow forced, and graphene island is made in winding
Precursor；Wherein, in 30:70, sea component temperature is controlled at 275 DEG C for sea, the control of island ratio；Island component temperature is controlled at 275 DEG C.
The preparation of S4, graphene sea-island fibre: graphene island precursor is through boundling；Drawing-off: level-one drawing-off oil bath temperature is
75 DEG C, second level drawing-off be 130 DEG C of superheated steam drawing-offs, 3.0 times of drawing-off general times；Nervous thermal finalization: preceding 8 rollers add in 18 rollers
Hot temperature is 160 DEG C, leads to cooling water in rear 10 rollers to tow cooling；Humidification, curling, oils, and 100 DEG C of baking oven relaxation heat are fixed
Type, drawing-off maximum speed 110m/min；Graphene sea-island fibre is made in the processes such as cutting.
After tested, the breaking strength of graphene sea-island fibre manufactured in the present embodiment: >=2.0cn/dtex, crispation number M2 ±
4.0/25mm, crimp percent M3 ± 4.0%, 180 DEG C of dry-hot shrinkage≤10.0%, line density 3.0dtex~5.56dtex, suppression
Bacterium rate 99%, elongation at break 26.9%, draw ratio 4.6, crystallinity 38%, far infrared normal emittance 0.88, far infrared
2.8 DEG C of temperature rise of irradiation, fiber have far infrared, antibacterial bacteriostatic, the anti-static function of graphene fiber.
Embodiment 2
The preparation of S1, graphene master batch: 65% 80nm is provided with biomass straw by biomass by weight percentage
Biomass graphene powder that source hydrothermal carbonization mode is prepared, 15% dispersing agent Pluronic P123 and 20% table
Face activating agent ether alcohol sulfate mixing, agitated, dispersion, is made graphene slurries；Again with 18% graphene slurries and 61% essence
Terephthalic acid (TPA) PTA, 21% ethylene glycol EG are blended to obtain mixed liquor, add catalyst acetic acid manganese and stir evenly, and import reaction
Esterification is carried out in kettle, the additional amount of the catalyst is the 0.5% of mixed liquor weight；Mixture after esterification is imported into contracting
Polycondensation reaction is carried out in poly- kettle, and using preshrunk, final minification, Cast Strip, cooling, granulation, drying, graphene master batch is made.
The preparation of S2, graphene polyester island component: 22% graphene master batch and 78% PET after drying are total to
It is mixed, it stirs evenly, graphene polyester island component is made in screw extruder melting；
The preparation of S3, graphene island precursor: by soluble polyester sea component COPET, the graphene polyester of drying process
Island group lease making is after respectively system is dry, the melting extrusion in respective screw extruder, and enters through respective pipeline, metering pump same
One spinning pack, then through respective runner, filtration system, then soluble polyester sea component melt and graphene polyester island component are molten
Body sprays after spinneret hole converges from spinneret orifice, cooling through air-flow forced, and graphene island precursor is made in winding；Wherein,
Ratio control in island is controlled in 30:70, sea component temperature at 275 DEG C；Island component temperature is controlled at 275 DEG C.
The preparation of S4, graphene sea-island fibre: graphene island precursor is through boundling；Drawing-off: level-one drawing-off oil bath temperature is
80 DEG C, second level drawing-off be 130 DEG C of superheated steam drawing-offs, 2.8 times of drawing-off general times；Nervous thermal finalization: preceding 8 rollers add in 18 rollers
Hot temperature is 165 DEG C, leads to cooling water in rear 10 rollers to tow cooling；Humidification, curling, oils, and 110 DEG C of baking oven relaxation heat are fixed
Type, drawing-off maximum speed 120m/min；Graphene sea-island fibre is made in the processes such as cutting.
After tested, the breaking strength of graphene sea-island fibre two: >=2.0cn/dtex, crispation number M2 ± 4.0/25mm,
Crimp percent M3 ± 4.0%, 180 DEG C of dry-hot shrinkage≤10.0%, line density 3.0dtex~5.56dtex, bacteriostasis rate 98%,
Elongation at break 26.5%, draw ratio 4.4, crystallinity 37.5%, far infrared normal emittance 0.89, Far-infrared spoke shine temperature rise
2.6 DEG C, fiber has far infrared, antibacterial bacteriostatic, the anti-static function of graphene fiber.
The preparation of 3 graphene sea-island fibre three of embodiment
The preparation of S1, graphene master batch: 45% 80nm is provided with biomass straw by biomass by weight percentage
Biomass graphene powder that source hydrothermal carbonization mode is prepared, 28% dispersing agent Pluronic P123 and 27% table
Face activating agent ether alcohol sulfate mixing, agitated, dispersion, is made graphene slurries；Again with 15% graphene slurries and 65% essence
Terephthalic acid (TPA) PTA, 20% ethylene glycol EG are blended to obtain mixed liquor, add catalyst sodium aluminate and stir evenly, and import reaction
Esterification is carried out in kettle, the additional amount of the catalyst is the 1.8% of mixed liquor weight；Mixture after esterification is imported into contracting
Polycondensation reaction is carried out in poly- kettle, and using preshrunk, final minification, Cast Strip, cooling, granulation, drying, graphene master batch is made.
The preparation of S2, graphene polyester island component: 18% graphene master batch and 82% PET after drying are total to
It is mixed, it stirs evenly, graphene polyester island component is made in screw extruder melting；
The preparation of S3, graphene island precursor: by soluble polyester sea component COPET, the graphene polyester of drying process
Island group lease making is after respectively system is dry, the melting extrusion in respective screw extruder, and enters through respective pipeline, metering pump same
One spinning pack, then through respective runner, filtration system, then soluble polyester sea component melt and graphene polyester island component are molten
Body sprays after spinneret hole converges from spinneret orifice, and graphene island precursor is made in, winding cooling through air-flow forced；Wherein,
Wherein, ratio control in island is controlled in 30:70, sea component temperature at 275 DEG C；Island component temperature is controlled at 275 DEG C.
The preparation of S4, graphene sea-island fibre: graphene island precursor is through boundling；Drawing-off: level-one drawing-off oil bath temperature is
75 DEG C, second level drawing-off be 130 DEG C of superheated steam drawing-offs, 3.0 times of drawing-off general times；Nervous thermal finalization: preceding 8 rollers add in 18 rollers
Hot temperature is 165 DEG C, leads to cooling water in rear 10 rollers to tow cooling；Humidification, curling, oils, and 110 DEG C of baking oven relaxation heat are fixed
Type, drawing-off maximum speed 110m/min；Graphene sea-island fibre is made in the processes such as cutting.
After tested, the breaking strength of graphene sea-island fibre three: >=2.0cn/dtex, crispation number M2 ± 4.0/25mm,
Crimp percent M3 ± 4.0%, 180 DEG C of dry-hot shrinkage≤10.0%, line density 3.0dtex~5.56dtex, bacteriostasis rate 98%,
Elongation at break 26.4%, draw ratio 4.4, crystallinity 37.42%, far infrared normal emittance 0.88, Far-infrared spoke is according to temperature
2.47 DEG C are risen, fiber has far infrared, antibacterial bacteriostatic, the anti-static function of graphene fiber.
Comparative example 1
Be not added with graphene, production technology similar to embodiment 1, specifically:
The preparation of S1, polyester island component: with PET slice through drying, polyester island component is made in screw extruder melting；
The preparation of S2, island precursor: respectively by the soluble polyester sea component COPET of drying process, polyester island group lease making
After system is dry, the melting extrusion in respective screw extruder, and enter same spinning pack through respective pipeline, metering pump,
Again through respective runner, filtration system, then soluble polyester sea component melt and polyester island component melt converge through spinneret hole
Afterwards, it is sprayed from spinneret orifice, island precursor is made in, winding cooling through air-flow forced；Wherein, the temperature control in sea, island component exists
275 ℃。
S3, the preparation for washing sea-island fibre: island precursor oils through boundling, drawing-off, nervous thermal finalization, curling, relaxation heat
Sizing, the processes such as cutting, which are made, washs sea-island fibre.
After tested, the breaking strength of sea-island fibre one is washed: >=2.0cn/dtex, crispation number M2 ± 4.0/25mm, volume
Curvature M3 ± 4.0%, 180 DEG C of dry-hot shrinkage≤10.0%, line density 3.0dtex~5.56dtex, elongation at break
28.3%, draw ratio 5.6, crystallinity 39.2%.Compared with embodiment 1,1 fibre strength of comparative example is slightly higher, but does not have stone
Far infrared, antibacterial bacteriostatic, the anti-static function of black alkene fiber.
Comparative example 2
Be not added with graphene, production technology similar to embodiment 2, specifically:
The preparation of S1, polyester island component: with PET slice through drying, polyester island component is made in screw extruder melting；
The preparation of S2, island precursor: respectively by the soluble polyester sea component COPET of drying process, polyester island group lease making
After system is dry, the melting extrusion in respective screw extruder, and enter same spinning pack through respective pipeline, metering pump,
Again through respective runner, filtration system, then soluble polyester sea component melt and polyester island component melt converge through spinneret hole
Afterwards, it is sprayed from spinneret orifice, cooling through air-flow forced, island precursor is made in winding；Wherein, the temperature control in sea, island component exists
275 ℃。
S3, the preparation for washing sea-island fibre: island precursor oils through boundling, drawing-off, nervous thermal finalization, curling, relaxation heat
Sizing, the processes such as cutting, which are made, washs sea-island fibre.
After tested, the breaking strength of sea-island fibre two is washed: >=2.0cn/dtex, crispation number M2 ± 4.0/25mm, volume
Curvature M3 ± 4.0%, 180 DEG C of dry-hot shrinkage≤10.0%, line density 3.0dtex~5.56dtex, elongation at break
28.5%, draw ratio 5.61, crystallinity 39.7%.Embodiment 2 is compared, 2 fibre strength of comparative example is also slightly higher, but does not also have
There are far infrared, antibacterial bacteriostatic, the anti-static function of graphene fiber.
Comparative example 3
Be not added with graphene, production technology similar to embodiment 3, specifically:
The preparation of S1, polyester island component: with PET slice through drying, polyester island component is made in screw extruder melting；
The preparation of S2, island precursor: respectively by the soluble polyester sea component COPET of drying process, polyester island group lease making
After system is dry, the melting extrusion in respective screw extruder, and enter same spinning pack through respective pipeline, metering pump,
Again through respective runner, filtration system, then soluble polyester sea component melt and polyester island component melt converge through spinneret hole
Afterwards, it is sprayed from spinneret orifice, cooling through air-flow forced, island precursor is made in winding；Wherein, the temperature control in sea, island component exists
275 ℃。
S3, the preparation for washing sea-island fibre: island precursor oils through boundling, drawing-off, nervous thermal finalization, curling, relaxation heat
Sizing, the processes such as cutting, which are made, washs sea-island fibre.
After tested, this comparative example washs the breaking strength of sea-island fibre: >=2.0cn/dtex, and crispation number M2 ± 4.0/
25mm, crimp percent M3 ± 4.0%, 180 DEG C of dry-hot shrinkage≤10.0%, line density 3.0dtex~5.56dtex, fracture are stretched
Long rate 27.5%, draw ratio 5.65, crystallinity 39.8%.Embodiment 3 is compared, 3 fibre strength of comparative example is equally slightly higher, together
Sample does not have far infrared, antibacterial bacteriostatic, the anti-static function of graphene fiber yet.
Comparative example 4
The weight percent of biomass graphene powder, dispersing agent, surfactant in the preparation process of graphene master batch
Are as follows: 25%:45%:30%, graphene slurries, p-phthalic acid, ethylene glycol weight percent are as follows: 5%:70%:25%,
Other are the same as embodiment 1.
After tested, the breaking strength of this comparative example sea-island fibre: >=2.0cn/dtex, crispation number M2 ± 4.0/25mm,
Crimp percent M3 ± 4.0%, 180 DEG C of dry-hot shrinkage≤10.0%, line density 3.0dtex~5.56dtex, bacteriostasis rate 50%,
Elongation at break 27.5%, draw ratio 5.0, crystallinity 38.5%, far infrared normal emittance 0.50, Far-infrared spoke shine temperature rise
1.5 DEG C, fiber far infrared, antibacterial bacteriostatic, anti-static function are weaker, are not enough to meet textile product standard index.
Comparative example 5
The weight percent of biomass graphene powder, dispersing agent, surfactant in the preparation process of graphene master batch
Are as follows: 70%:15%:15%, graphene slurries, p-phthalic acid, ethylene glycol weight percent are as follows: 30%:40%:
30%, other are the same as embodiment 1.
After tested, breaking strength < 1.0cn/dtex of this comparative example sea-island fibre, crispation number M2 ± 4.0/25mm, volume
Curvature M3 ± 4.0%, 180 DEG C of dry-hot shrinkage≤10.0%, line density 3.0dtex~5.56dtex, bacteriostasis rate 99% break
Elongation 24% is split, draw ratio 3, crystallinity 36%, far infrared normal emittance 0.88, Far-infrared spoke is according to 3.0 DEG C of temperature rise, fibre
Dimension is more crisp, is easily broken.
The preferred embodiment of the present invention has been described in detail above, but the invention be not limited to it is described
Embodiment, those skilled in the art can also make various equivalent on the premise of not violating the inventive spirit of the present invention
Variation or replacement, these equivalent variation or replacement are all included in the scope defined by the claims of the present application.
Claims (12)
1. a kind of manufacturing method of graphene sea-island fibre, includes the following steps:
Step S1: the preparation of graphene master batch: by weight percentage by 30%~65% graphene powder, 10%~25%
Dispersing agent and 15%~30% surfactant mixing, it is agitated, dispersion, be made graphene slurries；Again by graphene slurries
With p-phthalic acid, ethylene glycol by weight percentage: 10%~20%:40%~70%:10%~30%, which is blended, to be mixed
Liquid is closed, catalyst sodium aluminate is added or manganese acetate stirs evenly, imports in reaction kettle and carries out esterification, the catalyst
Additional amount is the 0.5~2% of mixed liquor weight；Mixture after esterification is imported in polycondensation vessel and carries out polycondensation reaction, using
Graphene master batch is made in preshrunk, final minification, Cast Strip, cooling, granulation, drying；
Step S2: the preparation of graphene polyester: graphene master batch is blended with the polyethylene terephthalate after drying, is stirred
Uniformly, screw extruder melts, and graphene polyester is made；
Step S3: the preparation of graphene island precursor: lead to after the soluble polyester of drying process, graphene polyester are separately dried
Cross screw extruder melting extrusion；By after melting extrusion soluble polyester fondant and graphene polyester fondant respectively managed respectively
After road, metering pump-metered, it is delivered to spinning manifold respectively, it is multiple by fabric of island-in-sea type into same fabric of island-in-sea type composite spinneret pack
Respective runner and filtration system in spinning pack are closed, soluble polyester fondant and graphene polyester fondant are converged through spinneret hole
It is sprayed after conjunction from spinneret orifice, then cooling through air-flow forced, winding, it is obtained to be by island component, soluble polyester of graphene polyester
The graphene island precursor of sea component；
Step S4: the preparation of graphene sea-island fibre: graphene island precursor prepared by step S3 is made through finishing process
Graphene sea-island fibre, the finishing process include boundling, drawing-off, nervous thermal finalization, crimp, oil, relaxation heat setting, cutting
Disconnected process.
2. the manufacturing method of graphene sea-island fibre according to claim 1, which is characterized in that in step S1, the stone
Black alkene powder is biomass graphene or abiotic matter graphene.
3. the manufacturing method of graphene sea-island fibre according to claim 1 or 2, which is characterized in that described in step S1
Graphene powder particle size be 55nm~90nm.
4. the manufacturing method of graphene sea-island fibre according to claim 1, which is characterized in that described in step S1
Surfactant is selected from one of ether alcohol sulfate, sucrose ester, alkylolamides.
5. the manufacturing method of graphene sea-island fibre according to claim 1, which is characterized in that described in step S1
Dispersing agent is one of Pluronic P123, Pluronic F68, Pluronic F127.
6. the manufacturing method of graphene sea-island fibre according to claim 1, which is characterized in that described in step S2
Graphene master batch and polyethylene terephthalate weight percent after drying be respectively 15%~25%:75%~
85%.
7. the manufacturing method of graphene sea-island fibre according to claim 1, which is characterized in that described in step S3
Soluble polyester is one or more of COPET, PVA, PS, PE.
8. the manufacturing method of graphene sea-island fibre according to claim 1, which is characterized in that in step S3, in spinneret
Before converging at plate, the solubility polyester melt temperature control is at 270 DEG C~295 DEG C, the graphene polyester fondant temperature control
System is at 270 DEG C~290 DEG C.
9. the manufacturing method of graphene sea-island fibre according to claim 1, which is characterized in that described to lead in step S4
It stretches including level-one drawing-off, second level drawing-off, 2.80~3.30 times of drawing-off general times；Level-one drawing-off is oil bath drawing-off, and oil bath temperature is
75 DEG C~80 DEG C；Second level drawing-off is superheated steam drawing-off, and superheat steam temperature is 110 DEG C~140 DEG C.
10. the manufacturing method of graphene sea-island fibre according to claim 1, which is characterized in that described tight in step S4
It opens thermal finalization and carries out 18 roller sizings, preceding 8 roller heating temperatures are 160 DEG C~165 DEG C, lead to cooling water in rear 10 rollers to tow drop
Temperature.
11. the manufacturing method of graphene sea-island fibre according to claim 1, which is characterized in that in step S4, the pine
Controlled at 100 DEG C~110 DEG C in relaxation heat setting process, draft speed is no more than 120m/min.
12. by the graphene sea-island fibre of the described in any item manufacturing method preparations of claim 1-11.
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