CN106884210B - A kind of graphene tencel composite fibre and preparation method thereof - Google Patents

A kind of graphene tencel composite fibre and preparation method thereof Download PDF

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Publication number
CN106884210B
CN106884210B CN201710138437.5A CN201710138437A CN106884210B CN 106884210 B CN106884210 B CN 106884210B CN 201710138437 A CN201710138437 A CN 201710138437A CN 106884210 B CN106884210 B CN 106884210B
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graphene
tencel
solution
graphene oxide
composite fibre
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CN106884210A (en
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张炜栋
黄旭
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Changzhou Zhuosheng Textile Co ltd
Shenzhen Pengbo Information Technology Co ltd
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Nantong Textile Vocational Technology College
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/09Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • D01F1/103Agents inhibiting growth of microorganisms
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/73Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
    • D06M11/74Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/55Epoxy resins
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic

Abstract

The invention discloses a kind of graphene tencel composite fibres and preparation method thereof, the graphene tencel composite fibre is to be mixed using graphene oxide solution with cellulose pulp addition NMMO (N-methyl morpholine-N oxide) and water, dissolution, filtering, pass through dry spray wet processing spinning, then be prepared by silk thread with the arrangement of graphene oxide finishing fluid.The tencel composite fibre contains graphene, using following steps: spinning solution preparation, spinning, yarn graphene arrange.Yarn obtained in the present invention is capable of the good characteristic of abundant soft tencel and graphene, and the superior physical properties such as hygroscopicity, dyeability, comfort, high intensity with tencel also increase graphene flexibility, electric conductivity and antibiotic property, are that ideal takes fiber.No pollution to the environment in preparation process production process, fiber product waste can natural degradation, environment will not be damaged, be easily formed recyclable regenerative resource.

Description

A kind of graphene tencel composite fibre and preparation method thereof
Technical field
The invention belongs to new textile material field, it is related to a kind of graphene tencel composite fibre and preparation method thereof.
Background technique
Graphene is a kind of New Type of Carbon nanometer light material, has unique monoatomic layer two dimensional crystal structure.Due to it The functions such as intensity, excellent electric conductivity, thermal conductivity and the translucency and excellent antibacterial, UV resistance, far infrared of superelevation.
Tencel fiber produces a kind of Fresh fats through solvent spinning process using wood pulp as raw material.Have cotton comfort, terylene it is strong Degree, unique sense of touch of the luxurious aesthetic feeling of wool fabric and silk and the soft pendant that hangs down, under dry state, great toughness.Under wet condition, Wet strength outclass the cellulose fibre of cotton.Natural material, environmentally friendly manufacturing process are environmentally protective.
Up to the present, while there is superpower, excellent electric conductivity, thermal conductivity, UV resistance, far infrared, excellent antibacterial and suitable There is not been reported for the research of the functional composite fiber for comfortably taking environmental protection in direct contact with the skin and preparation method, therefore opens Sending out to have both the environmental protection of graphene and tencel fiber advantage a kind of, to take fiber very necessary.
Summary of the invention
Goal of the invention: the object of the present invention is to provide a kind of graphene tencel composite fibres and preparation method thereof, by graphite Alkene is introduced into tencel fiber, and the functional characteristic of graphene is embodied on tencel fiber, makes functional excellent tencel Fiber assigns the functions such as good conduction, thermal conductivity, antibiotic property, UV resistance, far infrared, further increases tencel fiber mechanical property Energy.
Technical solution: to solve the above problems, the technical scheme is that a kind of graphene tencel composite fibre graphite Alkene tencel composite fibre, the graphene tencel composite fibre are that NMMO is added using graphene oxide solution and cellulose pulp (N-methyl morpholine-N oxide) and water through mixing, dissolution, filtering, by dry spray wet processing spinning, then by silk thread with The arrangement of graphene oxide finishing fluid is prepared.
A kind of preparation method of the graphene tencel composite fibre according to, comprising the following steps:
Step 1: graphene oxide NMMOH is prepared2O solution: mass fraction 10-30% graphene oxide solution is added Enter to the NMMO aqueous solution that mass fraction is 70-80% and 3-5h is mixed, 1-2h is handled in ultrasonic wave, by being evaporated under reduced pressure to Graphene oxide NMMOH2O solution;
Step 2: dissolution, filtering spinning mixed solution: in graphene oxide NMMOH2The degree of polymerization is added in O solution Wood pulp, the antibacterial agent, antioxidant of 600-1000 crushing dissolve 3-5h in 100 DEG C of mixings, handle 1-2h in ultrasonic wave, 15-20h is vacuumized at 70-80 DEG C, graphene oxide and wood pulp cellulose weight ratio are 1:20-1:80;
Step 3: it prepares graphene tencel composite fibre: by dissolution, filtered spinning mixed solution, screw rod is added and squeezes Press through spinning, the postprocessing working procedures such as washes, oils, dries and obtain fiber;Wherein, 90-130 DEG C of screw extruder temperature, spray Filament plate aperture is 10-60 μm, 400-600 μm of hole capillary pipe length, jet stretch ratio 2.60-3.00, gas length 50-200mm, Coagulating bath NMMO concentration of aqueous solution is 10-30%, coagulating bath length 1.5-2.5m, 10-16 DEG C of coagulation bath temperature, spinning speed 50-80m/min。
As optimization: antibacterial agent in the step 2 are as follows: AEM5700-A nano silver inorganic antimicrobial agent, antibacterial mildew inhibitor BM- 2, organosilicon quaternary ammonium salt HM98-3, poly hexamethylene adipamide carbamyl inferior amine salt hydrochlorate, poly- methylene hydrochloric acid PHMB.
As optimization: antioxidant in the step 2 are as follows: propyl gallate, antioxidant AO-60, antioxidant 2112, SANBO-103R graphite antioxidant, antioxidant T501.
A kind for the treatment of process for the fiber that the preparation method of the graphene tencel composite fibre according to is prepared, it is described Graphene tencel composite fibre is prepared by compound (1) silk thread and the arrangement of graphene oxide finishing fluid;Concrete operations are as follows:
Step 1: graphene polyurethane solutions are prepared: mass fraction 10-30% graphene oxide solution, 3-12% is even Connection agent is added to the resin solution that mass fraction is 60-70% and 3-5h is mixed, and handles 1-2h in ultrasonic wave, is steamed by decompression Evaporate to obtain graphene oxide resin solution;
Step 2: prepare graphene tencel composite fibre: graphene oxide finishing fluid arranges yarn, by above-mentioned graphene tree Graphene tencel long filament is prepared coated on above-mentioned in lipoprotein solution, and the graphene tencel infiltrates in graphene resin solution, 80-120 pick-up is dried, 80-90 DEG C of drying, 140-160 DEG C bakes, the graphene tencel fiber that must be put in order.
As optimization: the step 1 coupling agent are as follows: aluminate coupling agent DL-411, titanate coupling agent SD-109, boron Sour rouge coupling agent.
As optimization: resin solution in the step 2 are as follows: acrylic resin HK-1029, epoxy resin E-44, polyurethane HKR-329。
The utility model has the advantages that advantage of the invention is as follows:
1, yarn obtained in the present invention is capable of the good characteristic of abundant soft tencel and graphene, the moisture absorption with tencel Property, the superior physical properties such as dyeability, comfort, high intensity, also increase graphene flexibility, electric conductivity and antibiotic property, be reason Want to take fiber.No pollution to the environment in preparation process production process, fiber product waste can natural degradation, will not be to environment It damages, is easily formed recyclable regenerative resource.
2, the graphene tencel composite fibre produced in the present invention: dry breaking strength is 2.19cN/dtex, wet disconnected Resistance to spalling is 1.13cN/dtex, and initial modulus 22.6, elongation at break 10.7%, volume conductance is 3.9 × 10-6S/ Cm, fiber thermal decomposition temperature are 350 DEG C.
Specific embodiment
The present invention will be described in detail combined with specific embodiments below.
Specific embodiment one:
A kind of graphene tencel composite fibre graphene tencel composite fibre, the graphene tencel composite fibre are to utilize Graphene oxide solution and cellulose pulp are added NMMO (N-methyl morpholine-N oxide) and water is mixed, dissolution, filtering, By dry spray wet processing spinning, then be prepared by silk thread and the arrangement of graphene oxide finishing fluid.
A kind of preparation method of the graphene tencel composite fibre according to, comprising the following steps:
Step 1: graphene oxide NMMOH is prepared2O solution: 10% graphene oxide solution of mass fraction is added to 3h is mixed in the NMMO aqueous solution that mass fraction is 70%, 1h is handled in ultrasonic wave, by being evaporated under reduced pressure to graphene oxide NMMO·H2O solution.
Step 2: dissolution, filtering spinning mixed solution: in graphene oxide NMMOH2The degree of polymerization 600 is added in O solution Wood pulp, antibacterial agent, the antioxidant of crushing dissolve 3h in 100 DEG C of mixings, handle 1h in ultrasonic wave, take out at 70 DEG C true Empty 15h, graphene oxide and wood pulp cellulose weight ratio are 1:20.
Antibacterial agent are as follows: AEM5700-A nano silver inorganic antimicrobial agent, antibacterial mildew inhibitor BM-2.
Antioxidant are as follows: propyl gallate, antioxidant AO-60.
Step 3: it prepares graphene tencel composite fibre: by dissolution, filtered spinning mixed solution, screw rod is added and squeezes Press through spinning, the postprocessing working procedures such as washes, oils, dries and obtain fiber;Wherein, 90 DEG C of screw extruder temperature, spinneret Aperture be 10 μm, 400 μm of hole capillary pipe length, jet stretch ratio 2.60, gas length 50mm, coagulating bath NMMO concentration of aqueous solution It is 10%, coagulating bath length 1.5m, 10 DEG C of coagulation bath temperature, spinning speed 50m/min.
A kind for the treatment of process for the fiber that the preparation method of the graphene tencel composite fibre according to is prepared, it is described Graphene tencel composite fibre is prepared by compound (1) silk thread and the arrangement of graphene oxide finishing fluid;Concrete operations are as follows:
Step 1: graphene polyurethane solutions are prepared: 10% graphene oxide solution of mass fraction, 3% coupling agent is added Enter to the resin solution that mass fraction is 60% and 3h is mixed, 1h is handled in ultrasonic wave, by being evaporated under reduced pressure to graphite oxide Olefine resin solution;Coupling agent are as follows: aluminate coupling agent DL-411.
Step 2: prepare graphene tencel composite fibre: graphene oxide finishing fluid arranges yarn, by above-mentioned graphene tree Graphene tencel long filament is prepared coated on above-mentioned in lipoprotein solution, and the graphene tencel infiltrates in graphene resin solution, 80 pick-ups are dried, 80 DEG C of drying, 140 DEG C bake, the graphene tencel fiber that must be put in order.Resin solution are as follows: acrylic acid tree Rouge HK-1029.
Specific embodiment two:
A kind of graphene tencel composite fibre graphene tencel composite fibre, the graphene tencel composite fibre are to utilize Graphene oxide solution and cellulose pulp are added NMMO (N-methyl morpholine-N oxide) and water is mixed, dissolution, filtering, By dry spray wet processing spinning, then be prepared by silk thread and the arrangement of graphene oxide finishing fluid.
A kind of preparation method of the graphene tencel composite fibre according to, comprising the following steps:
Step 1: graphene oxide NMMOH is prepared2O solution: 30% graphene oxide solution of mass fraction is added to 5h is mixed in the NMMO aqueous solution that mass fraction is 80%, 2h is handled in ultrasonic wave, by being evaporated under reduced pressure to graphene oxide NMMO·H2O solution.
Step 2: dissolution, filtering spinning mixed solution: in graphene oxide NMMOH2The degree of polymerization is added in O solution Wood pulp, the antibacterial agent, antioxidant of 600-1000 crushing dissolve 5h in 100 DEG C of mixings, 2h are handled in ultrasonic wave, in 80 20h is vacuumized at DEG C, graphene oxide and wood pulp cellulose weight ratio are 1:80.
Antibacterial agent are as follows: organosilicon quaternary ammonium salt HM98-3, poly hexamethylene adipamide carbamyl inferior amine salt hydrochlorate.
Antioxidant are as follows: antioxidant 2112, SANBO-103R graphite antioxidant.
Step 3: it prepares graphene tencel composite fibre: by dissolution, filtered spinning mixed solution, screw rod is added and squeezes Press through spinning, the postprocessing working procedures such as washes, oils, dries and obtain fiber;Wherein, 130 DEG C of screw extruder temperature, spinneret Panel aperture be 60 μm, 600 μm of hole capillary pipe length, jet stretch ratio 3.00, gas length 200mm, coagulating bath NMMO aqueous solution Concentration is 30%, coagulating bath length 2.5m, 16 DEG C of coagulation bath temperature, spinning speed 80m/min.
A kind for the treatment of process for the fiber that the preparation method of the graphene tencel composite fibre according to is prepared, it is described Graphene tencel composite fibre is prepared by compound (1) silk thread and the arrangement of graphene oxide finishing fluid;Concrete operations are as follows:
Step 1: graphene polyurethane solutions are prepared: 30% graphene oxide solution of mass fraction, 12% coupling agent is added Enter to the resin solution that mass fraction is 70% and 5h is mixed, 2h is handled in ultrasonic wave, by being evaporated under reduced pressure to graphite oxide Olefine resin solution;Coupling agent are as follows: titanate coupling agent SD-109.
Step 2: prepare graphene tencel composite fibre: graphene oxide finishing fluid arranges yarn, by above-mentioned graphene tree Graphene tencel long filament is prepared coated on above-mentioned in lipoprotein solution, and the graphene tencel infiltrates in graphene resin solution, 120 pick-ups are dried, 90 DEG C of drying, 160 DEG C bake, the graphene tencel fiber that must be put in order.Resin solution are as follows: epoxy resin E-44。
Specific embodiment three:
A kind of graphene tencel composite fibre graphene tencel composite fibre, the graphene tencel composite fibre are to utilize Graphene oxide solution and cellulose pulp are added NMMO (N-methyl morpholine-N oxide) and water is mixed, dissolution, filtering, By dry spray wet processing spinning, then be prepared by silk thread and the arrangement of graphene oxide finishing fluid.
A kind of preparation method of the graphene tencel composite fibre according to, comprising the following steps:
Step 1: graphene oxide NMMOH is prepared2O solution: 20% graphene oxide solution of mass fraction is added to 4h is mixed in the NMMO aqueous solution that mass fraction is 70-80%, 1.4h is handled in ultrasonic wave, by being evaporated under reduced pressure to oxidation stone Black alkene NMMOH2O solution.
Step 2: dissolution, filtering spinning mixed solution: in graphene oxide NMMOH2The degree of polymerization 800 is added in O solution Wood pulp, antibacterial agent, the antioxidant of crushing dissolve 4h in 100 DEG C of mixings, handle 1.6h in ultrasonic wave, take out at 76 DEG C Vacuum 17h, graphene oxide and wood pulp cellulose weight ratio are 1:50.
Antibacterial agent are as follows: poly hexamethylene adipamide carbamyl inferior amine salt hydrochlorate, poly- methylene hydrochloric acid PHMB.
Antioxidant are as follows: SANBO-103R graphite antioxidant, antioxidant T501.
Step 3: it prepares graphene tencel composite fibre: by dissolution, filtered spinning mixed solution, screw rod is added and squeezes Press through spinning, the postprocessing working procedures such as washes, oils, dries and obtain fiber;Wherein, 110 DEG C of screw extruder temperature, spinneret Panel aperture be 40 μm, 500 μm of hole capillary pipe length, jet stretch ratio 2.80, gas length 130mm, coagulating bath NMMO aqueous solution Concentration is 20%, coagulating bath length 1.7m, 14 DEG C of coagulation bath temperature, spinning speed 70m/min.
A kind for the treatment of process for the fiber that the preparation method of the graphene tencel composite fibre according to is prepared, it is described Graphene tencel composite fibre is prepared by compound (1) silk thread and the arrangement of graphene oxide finishing fluid;Concrete operations are as follows:
Step 1: graphene polyurethane solutions are prepared: 20% graphene oxide solution of mass fraction, 8% coupling agent is added Enter to the resin solution that mass fraction is 66% and 4h is mixed, 1.6h is handled in ultrasonic wave, by being evaporated under reduced pressure to oxidation stone Black olefine resin solution;Coupling agent are as follows: boric acid rouge coupling agent.
Step 2: prepare graphene tencel composite fibre: graphene oxide finishing fluid arranges yarn, by above-mentioned graphene tree Graphene tencel long filament is prepared coated on above-mentioned in lipoprotein solution, and the graphene tencel infiltrates in graphene resin solution, 110 pick-ups are dried, 87 DEG C of drying, 150 DEG C bake, the graphene tencel fiber that must be put in order.Resin solution are as follows: polyurethane HKR-329。
The present invention is not limited to above-mentioned preferred forms, anyone can show that other are various under the inspiration of the present invention The product of form, however, make any variation in its shape or structure, it is all that there is skill identical or similar to the present application Art scheme, is within the scope of the present invention.

Claims (3)

1. a kind of preparation method of graphene tencel composite fibre, it is characterised in that: the graphene tencel composite fibre is benefit It is mixed with graphene oxide solution with cellulose pulp addition NMMO (N-methyl morpholine-N oxide) and water, dissolution, mistake Filter forms compound (1) silk thread by dry spray wet processing spinning, then is arranged and prepared by compound (1) silk thread and graphene oxide finishing fluid Made of;Wherein:
The preparation method of the compound (1) silk thread the following steps are included:
Step 1: graphene oxide NMMOH is prepared2O solution: mass fraction 10-30% graphene oxide solution is added to matter It measures the NMMO aqueous solution that score is 70-80% and 3-5h is mixed, 1-2h is handled in ultrasonic wave, by being evaporated under reduced pressure to oxidation stone Black alkene NMMOH2O solution;
Step 2: dissolution, filtering spinning mixed solution: in graphene oxide NMMOH2Degree of polymerization 600-1000 is added in O solution Wood pulp, antibacterial agent, the antioxidant of crushing dissolve 3-5h in 100 DEG C of mixings, 1-2h are handled in ultrasonic wave, in 70-80 DEG C Under vacuumize 15-20h, graphene oxide and wood pulp cellulose weight ratio are 1:20-1:80;
Step 3: it prepares compound (1) silk thread: by dissolution, filtered spinning mixed solution, screw extruder is added, through spinning, water It washes, oil, drying postprocessing working procedures and obtain fiber;Wherein, 90-130 DEG C of screw extruder temperature, the hole diameter of spinneret are 10-60 μ M, 400-600 μm of hole capillary pipe length, jet stretch ratio 2.60-3.00, gas length 50-200mm, coagulating bath NMMO aqueous solution Concentration is 10-30%, coagulating bath length 1.5-2.5m, 10-16 DEG C of coagulation bath temperature, spinning speed 50-80m/min;
The graphene tencel composite fibre is to arrange the specific behaviour being prepared by compound (1) silk thread and graphene oxide finishing fluid Make as follows:
Step 1: graphene polyurethane solutions are prepared: by mass fraction 10-30% graphene oxide solution, 3-12% coupling agent It is added to the resin solution that mass fraction is 60-70% and 3-5h is mixed, 1-2h is handled in ultrasonic wave, by being evaporated under reduced pressure to Graphene oxide resin solution;The coupling agent are as follows: aluminate coupling agent DL-411, titanate coupling agent SD-109, boric acid rouge Coupling agent;
Step 2: processing graphene tencel composite fibre: graphene oxide finishing fluid arranges yarn, and above-mentioned graphite olefine resin is molten Liquid is coated on the above-mentioned compound (1) silk thread being prepared, and the compound (1) silk thread infiltrates in graphene resin solution, dries 80- 120 pick-ups, 80-90 DEG C of drying, 140-160 DEG C bakes, the graphene tencel fiber that must be put in order.
2. the preparation method of graphene tencel composite fibre according to claim 1, it is characterised in that: in the step 2 Antibacterial agent are as follows: AEM5700-A nano silver inorganic antimicrobial agent, antibacterial mildew inhibitor BM-2, organosilicon quaternary ammonium salt HM98-3, poly hexamethylene adipamide Carbamyl inferior amine salt hydrochlorate, poly- methylene hydrochloric acid PHMB.
3. the preparation method of graphene tencel composite fibre according to claim 1, it is characterised in that: in the step 2 Antioxidant are as follows: propyl gallate, antioxidant AO-60, antioxidant 2112, SANBO-103R graphite antioxidant, antioxidant T501.
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CN104674362B (en) * 2015-03-11 2016-09-07 苏州欧尔迪威地暖科技有限公司 A kind of preparation method of fibroin/graphene conductive fiber
CN105506765B (en) * 2015-11-20 2018-08-03 济南圣泉集团股份有限公司 A kind of functional regenerated cellulose fibre and its preparation method and application

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