CN115247285A - Preparation method of carbon quantum dot acrylic fiber with far infrared performance and acrylic fiber - Google Patents
Preparation method of carbon quantum dot acrylic fiber with far infrared performance and acrylic fiber Download PDFInfo
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- CN115247285A CN115247285A CN202110453398.4A CN202110453398A CN115247285A CN 115247285 A CN115247285 A CN 115247285A CN 202110453398 A CN202110453398 A CN 202110453398A CN 115247285 A CN115247285 A CN 115247285A
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 254
- 229920002972 Acrylic fiber Polymers 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 155
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 126
- 229910001868 water Inorganic materials 0.000 claims abstract description 116
- 239000000835 fiber Substances 0.000 claims abstract description 115
- 238000009987 spinning Methods 0.000 claims abstract description 64
- 238000000034 method Methods 0.000 claims abstract description 28
- 238000007334 copolymerization reaction Methods 0.000 claims abstract description 20
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 230000008569 process Effects 0.000 claims abstract description 7
- 238000007493 shaping process Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 190
- 239000007864 aqueous solution Substances 0.000 claims description 43
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 32
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical group CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 23
- 239000003960 organic solvent Substances 0.000 claims description 9
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 61
- 229910002804 graphite Inorganic materials 0.000 description 27
- 239000010439 graphite Substances 0.000 description 27
- 229940113088 dimethylacetamide Drugs 0.000 description 25
- 229920000642 polymer Polymers 0.000 description 25
- 230000002378 acidificating effect Effects 0.000 description 24
- 229920002239 polyacrylonitrile Polymers 0.000 description 23
- 238000002156 mixing Methods 0.000 description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 12
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 12
- 239000012528 membrane Substances 0.000 description 12
- 239000000843 powder Substances 0.000 description 12
- 238000000926 separation method Methods 0.000 description 12
- 238000004513 sizing Methods 0.000 description 12
- 239000000178 monomer Substances 0.000 description 11
- 230000001105 regulatory effect Effects 0.000 description 11
- 239000012153 distilled water Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 10
- 230000036541 health Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000001112 coagulating effect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- YIWGJFPJRAEKMK-UHFFFAOYSA-N 1-(2H-benzotriazol-5-yl)-3-methyl-8-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carbonyl]-1,3,8-triazaspiro[4.5]decane-2,4-dione Chemical compound CN1C(=O)N(c2ccc3n[nH]nc3c2)C2(CCN(CC2)C(=O)c2cnc(NCc3cccc(OC(F)(F)F)c3)nc2)C1=O YIWGJFPJRAEKMK-UHFFFAOYSA-N 0.000 description 1
- ZRPAUEVGEGEPFQ-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]pyrazol-1-yl]-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethanone Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C=1C=NN(C=1)CC(=O)N1CC2=C(CC1)NN=N2 ZRPAUEVGEGEPFQ-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- -1 but not limited to Chemical compound 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000012921 fluorescence analysis Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- RAYLUPYCGGKXQO-UHFFFAOYSA-N n,n-dimethylacetamide;hydrate Chemical compound O.CN(C)C(C)=O RAYLUPYCGGKXQO-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000008041 oiling agent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000000554 physical therapy Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 229910000165 zinc phosphate Inorganic materials 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 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
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/54—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polymers of unsaturated nitriles
-
- 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating 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
- D06M11/73—Treating 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
- D06M11/74—Treating 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
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention discloses a preparation method of carbon quantum dot acrylic fiber with far infrared performance and acrylic fiber, wherein the preparation method comprises the following steps: step 1, forming a spinning solution after copolymerization reaction of acrylonitrile and a comonomer; step 2, heating the spinning solution and extruding the spinning solution from a spinneret plate to form nascent fibers; step 3, washing the nascent fiber, drafting, oiling, drying and shaping to form acrylic fiber; adding a carbon quantum dot solution in the copolymerization reaction process in the step 1; or, adding a carbon quantum dot solution into the spinning solution in the step 1 or the step 2; or, adding a carbon quantum dot solution in the water washing process of the step 3. According to the invention, the carbon quantum dot solution is added in the preparation process of the acrylic fiber, so that the carbon quantum dots are dispersed on the prepared acrylic fiber, the far infrared performance and the mechanical property of the acrylic fiber are improved, and the acrylic fiber has good health-care and antibacterial effects and can be widely applied to the fields of medical treatment, sanitation and the like.
Description
Technical Field
The invention belongs to the technical field of fibers, and particularly relates to a preparation method of carbon quantum dot acrylic fibers with far infrared performance and the acrylic fibers.
Background
The acrylic fiber has excellent mothproof property and good fluffy feeling and comfortable feeling, has the hand feeling similar to wool, and has the wearing comfort and air permeability which are more in line with the requirements of people. Therefore, the method has strong development advantages in the application fields of textile products such as gloves, cushions, sweaters, scarves, quilts and the like.
With the improvement of the life quality of people, the demand of functional acrylic fiber products is rapidly improved. Wherein, the far infrared acrylic fiber is a novel functional fiber with the functions of absorbing and emitting far infrared electromagnetic waves. The acrylic fiber compounded with the nano inorganic far infrared health-care component can emit high and far infrared electromagnetic waves with wavelengths corresponding to the absorption of human body radiation, is a good far infrared radiation material for human body health care, and has the functions of ultraviolet resistance, sterilization, peculiar smell elimination and the like. The far infrared acrylic fiber can effectively improve human microcirculation, improve oxygen supply of tissues, activate tissue cells, improve metabolism, prevent aging, enhance immune system and the like.
At present, the main preparation method of far infrared functional acrylic fiber is as follows: the far infrared fiber is prepared by blending ceramic particles with far infrared radiation function and conventional polymers and carrying out melt spinning. Because the ceramic particles with far infrared radiation function have poor compatibility with the conventional polymer, the far infrared performance of the prepared acrylic fiber is relatively poor, and the preparation process is single and cannot meet the diversified production requirements.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to solve the technical problem of poor far infrared performance of the existing acrylic fiber, and provides the preparation method of the carbon quantum dot acrylic fiber with the far infrared performance and the acrylic fiber, so that the far infrared performance of the acrylic fiber is good, and the obtained acrylic fiber also has good heat preservation, health care and antibacterial performance.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of carbon quantum dot acrylic fiber with far infrared performance comprises the following steps:
step 1, carrying out copolymerization reaction on acrylonitrile and a comonomer to form a spinning solution;
step 2, heating the spinning solution and extruding the spinning solution from a spinneret plate to form nascent fibers;
step 3, washing the nascent fiber, drafting, oiling, drying and shaping to form acrylic fiber;
adding a carbon quantum dot solution in the copolymerization reaction process in the step 1;
and/or adding a carbon quantum dot solution into the spinning solution in the step 1 or the step 2;
and/or adding a carbon quantum dot solution in the water washing process of the step 3.
Wherein, the carbon quantum dot solution added in the step 1 and the step 2 is a carbon quantum dot organic solution; and 3, adding a carbon quantum dot solution into the mixture to obtain a carbon quantum dot aqueous solution.
The organic solvent in the carbon quantum dot organic solution is the same as the organic solvent in the spinning solution;
preferably, the organic solvent is dimethylacetamide.
In the invention, the organic solvent in the carbon quantum dot organic solution is the same as the organic solvent in the spinning solution, so that the compatibility of the carbon quantum dot solution and the spinning solution is improved, and the carbon quantum dots can be uniformly dispersed in the spinning solution.
The carbon quantum dot water solution is added in the washing process, so that the carbon quantum dots are uniformly dispersed in water in the washing tank, and the carbon quantum dots can be uniformly distributed on the fiber after washing.
In the present invention, step 1 comprises: mixing acrylonitrile and a comonomer, carrying out aqueous phase suspension polymerization reaction, and processing after the reaction is finished to obtain a polyacrylonitrile powdery polymer;
the comonomer is a variety of monomers that can be polymerized with acrylonitrile including, but not limited to, vinyl acetate.
Dissolving polyacrylonitrile powder polymer in a solvent such as dimethylacetamide at 80-90 ℃, filtering, and adding a retarder to obtain a spinning stock solution;
or, adding retarder into solvent such as dimethylacetamide, mixing, and adding polyacrylonitrile powder polymer at 80-90 deg.C to obtain spinning solution.
Wherein, the retarder comprises one or a mixture of more than two of water, sodium borate, zinc sulfate and phosphate.
The step 2 comprises the following steps: extruding the spinning solution from a spinneret plate under the pressure of 0.7-0.9 MPa and the temperature of 80-97 ℃, and solidifying and forming in a coagulating bath solution to obtain nascent fiber;
the coagulating bath solution is dimethyl acetamide water solution.
The step 3 comprises the following steps:
a. washing and drafting the obtained nascent fiber, wherein the drafting temperature is controlled to be 65-99 ℃, and the drafting multiple is controlled to be 3.5-5.5 times;
c. oiling: adding a tow oiling agent to the tows after washing and drafting;
d. drying;
e. curling: introducing the dried tows into a steaming box through a tension frame, after the temperature reaches a certain value, feeding the tows into a crimping machine to form tows, and loading the tows for preparation for shaping;
f. shaping: and (3) packaging the crimped tows by using a tow trolley, feeding the tows into a sizing pot, performing sizing through the processes of vacuumizing, introducing steam and emptying, and finally taking the tows out of the pot to obtain the acrylic fibers.
Further, the temperature of water washing in the step 3 is 30-95 ℃;
further, the temperature of the water washing in step 3 is 40 to 90 ℃.
Furthermore, the washing pressure in the step 3 is 0-1MPa (gauge pressure), and the washing time is 2-30min.
Further, in step 3, the nascent fiber is subjected to multiple water washes, and a carbon quantum dot solution is added in at least one water wash of the multiple water washes;
preferably, the nascent fiber is subjected to at least first water washing, second water washing and third water washing in sequence, and the carbon quantum dot solution is added in the first water washing and the second water washing.
Or the nascent fiber is subjected to at least first water washing, second water washing, third water washing and fourth water washing in sequence, and the carbon quantum dot solution is added in the first water washing and the third water washing.
Or the nascent fiber is subjected to at least first water washing, second water washing, third water washing and fourth water washing in sequence, and the carbon quantum dot solution is added in the first water washing, the second water washing and the third water washing.
Further, the mass ratio of the carbon quantum dot solution to the nascent fiber is 0.1-15.
Further, the mass ratio of the carbon quantum dot solution to the nascent fiber is 1-5.
The concentration of carbon quantum dots in the carbon quantum dot solution is 0.1-10000 × 10 6 Per ml;
preferably, the concentration of carbon quantum dots in the carbon quantum dot solutionIs 1-100 x 10 6 One per ml.
Further, the carbon quantum dots with the particle size of 2-10nm in the carbon quantum dot solution account for 60-100% of the total carbon quantum dots in the carbon quantum dot solution.
Further, in the carbon quantum dot solution, the carbon quantum dots with the particle size of 2-10nm account for 80-100% of the total carbon quantum dots in the carbon quantum dot solution.
The invention also provides acrylic fiber which is provided with carbon quantum dots;
preferably, the density of the carbon quantum dots on the acrylic fiber is 0.01-1000 x 10 4 Per cm 2 ；
Preferably, the density of the carbon quantum dots on the acrylic fiber is 1-100 x 10 4 Per cm 2 ；
Preferably, the carbon quantum dots with the particle size of 2-10nm on the acrylic fiber account for 80-100% of the total carbon quantum dots on the acrylic fiber;
preferably, the carbon quantum dots with the particle size of 2-10nm on the acrylic fiber account for 60-100% of the total carbon quantum dots on the acrylic fiber carbon;
preferably, the compound is prepared by the preparation method.
According to the invention, the carbon quantum dots are dispersed in the tows of the acrylic fibers, or dispersed among the tows of the acrylic fibers, or dispersed and adsorbed on the tows of the acrylic fibers by the preparation method.
The acrylic fiber is provided with the carbon quantum dots, so that the far infrared performance of the fiber can be effectively improved, the acrylic fiber is widely applied to the fields of health, sanitation and the like, and has good antibacterial and health-care performances; in addition, the mechanical property of the acrylic fiber can be improved.
In the invention, the carbon quantum dot aqueous solution is prepared by adopting the following method:
in the acid solution, a positive electrode and a negative electrode of a direct current power supply are respectively connected with a graphite source, the voltage of the direct current power supply is regulated, and electrochemical reaction is carried out to obtain the carbon quantum dot acidic aqueous solution. And separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device to obtain a carbon quantum dot primary aqueous solution. The carbon quantum dot primary aqueous solution can be formed into a carbon quantum dot aqueous solution by optionally adding water.
In the invention, the carbon quantum dot organic solution is prepared by adopting the following method:
in the acid solution, the positive electrode and the negative electrode of a direct current power supply are respectively connected with a graphite source, the voltage of the direct current power supply is adjusted, and electrochemical reaction is carried out to obtain the carbon quantum dot acidic aqueous solution. And separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device to obtain a carbon quantum dot primary aqueous solution. Freeze drying the primary water solution of the carbon quantum dots to obtain carbon quantum dot powder; and then mixing the carbon quantum dot powder in an organic solvent, and performing ultrasonic dispersion to obtain a carbon quantum dot organic solution.
The graphite source may be a graphite rod or a graphite flake.
Preferably, the purity of the graphite source is more than 99% of carbon content, and the ash content is less than 1%;
preferably, the purity of the graphite source is more than 99.9% of carbon content, and the ash content is less than 0.1%.
The voltage of the direct current power supply is 0.1-60V, the time is 1-15 days, the temperature is 0-80 ℃, and the pressure is 0-1MPa.
The carbon quantum dot solution with different particle sizes can be obtained by changing the conditions such as the using amount of the acid solution, the voltage of a direct current power supply, the electrolysis time and the like.
Preferably, the acid solution is selected from at least one of phosphoric acid, sulfuric acid and hydrochloric acid.
The acrylic fiber can be used for manufacturing non-woven fabrics or woven fabrics and applied to the sanitary and cosmetic fields of physical therapy clothes, underwear, blankets, bedding, tents, facial masks, wet tissues and the like.
After adopting the technical scheme, compared with the prior art, the invention has the following beneficial effects:
the acrylic fiber provided by the invention has the carbon quantum dots, so that the far infrared performance and the mechanical property of the acrylic fiber are effectively improved, and the acrylic fiber has better health-care and antibacterial functions and can be widely applied to the fields of medical treatment, health care and the like.
In addition, the carbon quantum dot aqueous solution is added in the primary fiber washing process, so that the carbon quantum dots are uniformly dispersed on the acrylic fiber, the preparation process is simple, and the washing solution mixed with the carbon quantum dot aqueous solution after washing can be recycled.
The invention can also increase the effective adding amount of the carbon quantum dots in the acrylic fiber by adding the carbon quantum dot solution in the copolymerization reaction process of the acrylonitrile and the comonomer (such as vinyl acetate), so that the carbon quantum dots are uniformly dispersed in the acrylic fiber, and the far infrared performance and the strength of the acrylic fiber are effectively improved.
The invention can also directly add the carbon quantum dot solution into the spinning solution, has simple adding mode, provides various choices for preparing the acrylic fiber with far infrared performance and meets the diversified production requirements.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments are described clearly and completely below, and the following embodiments are used for illustrating the present invention and are not used for limiting the scope of the present invention.
Example 1:
step 1, mixing two monomers of acrylonitrile and vinyl acetate, carrying out copolymerization reaction to obtain a polyacrylonitrile powder polymer, and dissolving the polyacrylonitrile powder polymer in dimethylacetamide to obtain a spinning solution;
step 2, heating the spinning solution, extruding the spinning solution from a spinneret plate, and solidifying and forming the spinning solution in a dimethylacetamide aqueous solution to obtain nascent fibers;
and 3, adding 1000L of distilled water and 500ml of concentrated sulfuric acid (98 wt%) into a water tank at normal temperature and normal pressure, respectively connecting a positive electrode and a negative electrode of a direct current power supply with two ends of a graphite rod, vertically placing the graphite rod into the water tank, regulating the voltage to 20V, timing, and stirring for 5 days to obtain the electrolyzed carbon quantum dot acidic aqueous solution.
Step 4, separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device with the model of US2K to obtain a carbon quantum dot solution;
step 5, sequentially carrying out primary water washing, secondary water washing, tertiary water washing and quaternary water washing on the nascent fiber; in the second washing process, adding the carbon quantum dot solution into water to wash the nascent fiber;
wherein the mass ratio of the carbon quantum dot solution to the nascent fiber is 3.5:1;
the concentration of the carbon quantum dots in the carbon quantum dot solution is 10 x 10 6 And each ml, wherein the carbon quantum dots with the particle size of 2-10nm in the carbon quantum dot solution account for 90% of the total carbon quantum dots in the carbon quantum dot solution.
In the second washing process, the temperature is 60 ℃, the pressure is 0.1MPa (gauge pressure), and the time is 15min; the temperature of the first washing, the third washing and the fourth washing is 70 ℃, the pressure is 0MPa (gauge pressure), and the time is 5min.
Step 6: after the washing, the fiber tows are formed by drafting, and the acrylic fiber is prepared by oiling, drying and sizing the fiber tows.
Example 2:
step 1, mixing two monomers of acrylonitrile and vinyl acetate, carrying out copolymerization reaction to obtain a polyacrylonitrile powdery polymer, and dissolving the polyacrylonitrile powdery polymer in dimethylacetamide to obtain a spinning solution;
step 2, heating the spinning solution, extruding the spinning solution from a spinneret plate, and solidifying and forming the spinning solution in a dimethylacetamide aqueous solution to obtain nascent fiber;
and 3, adding 1000L of distilled water and 200ml of concentrated sulfuric acid (98 wt%) into a water tank at normal temperature and normal pressure, respectively connecting a positive electrode and a negative electrode of a direct current power supply with two ends of a graphite rod, vertically placing the graphite rod into the water tank, regulating the voltage to 40V, timing, and stirring for 5 days to obtain the electrolyzed carbon quantum dot acidic aqueous solution.
Step 4, separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device with the model of US2K to obtain a carbon quantum dot solution;
step 5, sequentially carrying out primary water washing, secondary water washing, tertiary water washing and quaternary water washing on the nascent fiber; in the second washing process, adding the carbon quantum dot solution into water to wash the nascent fiber;
wherein the mass ratio of the carbon quantum dot solution to the nascent fiber is 5:1;
the concentration of carbon quantum dots in the carbon quantum dot solution is 0.1 x 10 6 And each ml, wherein the carbon quantum dots with the particle size of 2-10nm in the carbon quantum dot solution account for 100% of the total carbon quantum dots in the carbon quantum dot solution.
In the second water washing process, the temperature is 90 ℃, the pressure is 0MPa, and the time is 2min; the temperature of the first washing, the third washing and the fourth washing is 70 ℃, the pressure is 0MPa, and the time is 5min.
And 6: after the washing, the fiber tows are formed by drafting, and the acrylic fiber is prepared by oiling, drying and sizing the fiber tows.
Example 3:
step 1, mixing two monomers of acrylonitrile and vinyl acetate, carrying out copolymerization reaction to obtain a polyacrylonitrile powder polymer, and dissolving the polyacrylonitrile powder polymer in dimethylacetamide to obtain a spinning solution;
step 2, heating the spinning solution, extruding the spinning solution from a spinneret plate, and solidifying and forming the spinning solution in a dimethylacetamide aqueous solution to obtain nascent fiber;
and 3, adding 1000L of distilled water and 1500ml of concentrated sulfuric acid (98 wt%) into a water tank at normal temperature and normal pressure, respectively connecting a positive electrode and a negative electrode of a direct current power supply with two ends of a graphite rod, vertically placing the graphite rod into the water tank, regulating the voltage to 20V, timing, and stirring for 5 days to obtain the electrolyzed carbon quantum dot acidic aqueous solution.
Step 4, separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device with the model of US2K to obtain a carbon quantum dot solution;
step 5, sequentially carrying out primary water washing, secondary water washing, tertiary water washing and quaternary water washing on the nascent fiber; in the second washing process, adding the carbon quantum dot solution into water to wash the nascent fiber;
wherein the mass ratio of the carbon quantum dot solution to the nascent fiber is 1:1;
the concentration of the carbon quantum dots in the carbon quantum dot solution is 100 x 10 6 Carbon quantum dots with particle size of 2-10nm in carbon quantum dot solution/ml80% of the total carbon quantum dots in the carbon quantum dot solution.
In the second washing process, the temperature is 40 ℃, the pressure is 0.2MPa, and the time is 30min; the temperature of the first washing, the third washing and the fourth washing is 70 ℃, the pressure is 0MPa, and the time is 5min.
Step 6: after the washing, the fiber tows are formed by drafting, and the acrylic fiber is prepared by oiling, drying and sizing the fiber tows.
Example 4:
step 1, mixing two monomers of acrylonitrile and vinyl acetate, carrying out copolymerization reaction to obtain a polyacrylonitrile powdery polymer, and dissolving the polyacrylonitrile powdery polymer in dimethylacetamide to obtain a spinning solution;
step 2, heating the spinning solution, extruding the spinning solution from a spinneret plate, and solidifying and forming the spinning solution in a dimethylacetamide aqueous solution to obtain nascent fiber;
and 3, adding 1000L of distilled water and 1500ml of concentrated sulfuric acid (98 wt%) into a water tank at normal temperature and normal pressure, respectively connecting a positive electrode and a negative electrode of a direct current power supply with two ends of a graphite rod, vertically placing the graphite rod into the water tank, regulating the voltage to 50V, timing, and stirring for 5 days to obtain the electrolyzed carbon quantum dot acidic aqueous solution.
Step 4, separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device with the model of US2K to obtain a carbon quantum dot solution;
step 5, sequentially carrying out primary water washing, secondary water washing, tertiary water washing and quaternary water washing on the nascent fiber; in the second washing process, adding the carbon quantum dot solution into water to wash the nascent fiber;
wherein the mass ratio of the carbon quantum dot solution to the nascent fiber is 3.5:1;
the concentration of the carbon quantum dots in the carbon quantum dot solution is 1000 x 10 6 And each ml, wherein the carbon quantum dots with the particle size of 2-10nm in the carbon quantum dot solution account for 90% of the total carbon quantum dots in the carbon quantum dot solution.
In the second washing process, the temperature is 30 ℃, the pressure is 0.5MPa, and the time is 15min; the temperature of the first washing, the third washing and the fourth washing is 70 ℃, the pressure is 0MPa, and the time is 5min.
And 6: after the washing, the fiber tows are formed by drafting, and the acrylic fiber is prepared by oiling, drying and sizing the fiber tows.
Example 5:
step 1, mixing two monomers of acrylonitrile and vinyl acetate, carrying out copolymerization reaction to obtain a polyacrylonitrile powder polymer, and dissolving the polyacrylonitrile powder polymer in dimethylacetamide to obtain a spinning solution;
step 2, heating the spinning solution, extruding the spinning solution from a spinneret plate, and solidifying and forming the spinning solution in a dimethylacetamide aqueous solution to obtain nascent fibers;
and 3, adding 1000L of distilled water and 200ml of concentrated sulfuric acid (98 wt%) into a water tank at normal temperature and normal pressure, respectively connecting a positive electrode and a negative electrode of a direct current power supply with two ends of a graphite rod, vertically placing the graphite rod into the water tank, regulating the voltage to 60V, timing, and stirring for 5 days to obtain the electrolyzed carbon quantum dot acidic aqueous solution.
Step 4, separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device with the model of US2K to obtain a carbon quantum dot solution;
step 5, sequentially carrying out primary water washing, secondary water washing, tertiary water washing and quaternary water washing on the nascent fiber; in the second washing process, adding the carbon quantum dot solution into water to wash the nascent fiber;
wherein the mass ratio of the carbon quantum dot solution to the nascent fiber is 3.5:1;
the concentration of carbon quantum dots in the carbon quantum dot solution is 0.1 x 10 6 And each ml, wherein the carbon quantum dots with the particle size of 2-10nm in the carbon quantum dot solution account for 90% of the total carbon quantum dots in the carbon quantum dot solution.
In the second water washing process, the temperature is 95 ℃, the pressure is 0.5MPa, and the time is 17min; the temperature of the first washing, the third washing and the fourth washing is 70 ℃, the pressure is 0MPa, and the time is 5min.
And 6: after the washing, the fiber tows are formed by drafting, and the acrylic fiber is prepared by oiling, drying and sizing the fiber tows.
Example 6:
step 1, mixing two monomers of acrylonitrile and vinyl acetate, carrying out copolymerization reaction to obtain a polyacrylonitrile powder polymer, and dissolving the polyacrylonitrile powder polymer in dimethylacetamide to obtain a spinning solution;
step 2, heating the spinning solution, extruding the spinning solution from a spinneret plate, and solidifying and forming the spinning solution in a dimethylacetamide aqueous solution to obtain nascent fibers;
and 3, adding 1000L of distilled water and 200ml of concentrated sulfuric acid (98 wt%) into a water tank at normal temperature and normal pressure, respectively connecting a positive electrode and a negative electrode of a direct current power supply with two ends of a graphite rod, vertically placing the graphite rod into the water tank, regulating the voltage to 60V, timing, and stirring for 5 days to obtain the electrolyzed carbon quantum dot acidic aqueous solution.
Step 4, separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device with the model of US2K to obtain a carbon quantum dot solution;
step 5, sequentially carrying out primary water washing, secondary water washing, tertiary water washing and quaternary water washing on the nascent fiber; in the second washing process, adding the carbon quantum dot solution into water to wash the nascent fiber;
wherein the mass ratio of the carbon quantum dot solution to the nascent fiber is 15:1;
the concentration of carbon quantum dots in the carbon quantum dot solution is 0.1 x 10 6 And each ml, wherein the carbon quantum dots with the particle size of 2-10nm in the carbon quantum dot solution account for 90% of the total carbon quantum dots in the carbon quantum dot solution.
In the second water washing process, the temperature is 50 ℃, the pressure is 1MPa, and the time is 20min; the temperature of the first washing, the third washing and the fourth washing is 70 ℃, the pressure is 0MPa, and the time is 5min.
Step 6: after washing, drafting to form fiber tows, and oiling, drying and sizing the fiber tows to obtain the acrylic fibers.
Example 7:
step 1, mixing two monomers of acrylonitrile and vinyl acetate, carrying out copolymerization reaction to obtain a polyacrylonitrile powdery polymer, and dissolving the polyacrylonitrile powdery polymer in dimethylacetamide to obtain a spinning solution;
step 2, heating the spinning solution, extruding the spinning solution from a spinneret plate, and solidifying and forming the spinning solution in a dimethylacetamide aqueous solution to obtain nascent fibers;
and 3, adding 1000L of distilled water and 200ml of concentrated sulfuric acid (98 wt%) into a water tank at normal temperature and normal pressure, respectively connecting a positive electrode and a negative electrode of a direct current power supply with two ends of a graphite rod, vertically placing the graphite rod into the water tank, regulating the voltage to 60V, timing, and stirring for 5 days to obtain the electrolyzed carbon quantum dot acidic aqueous solution.
Step 4, separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device with the model of US2K to obtain a carbon quantum dot solution;
step 5, sequentially carrying out primary water washing, secondary water washing, tertiary water washing and quaternary water washing on the nascent fiber; in the second washing process, adding the carbon quantum dot solution into water to wash the nascent fiber;
wherein the mass ratio of the carbon quantum dot solution to the nascent fiber is 0.1:1;
the concentration of the carbon quantum dots in the carbon quantum dot solution is 0.1 x 10 6 And each ml, wherein the carbon quantum dots with the particle size of 2-10nm in the carbon quantum dot solution account for 90% of the total carbon quantum dots in the carbon quantum dot solution.
In the second water washing process, the temperature is 50 ℃, the pressure is 1MPa, and the time is 20min; the temperature of the first washing, the third washing and the fourth washing is 70 ℃, the pressure is 0MPa, and the time is 5min.
And 6: after washing, drafting to form fiber tows, and oiling, drying and sizing the fiber tows to obtain the acrylic fibers.
Example 8:
step 1, mixing two monomers of acrylonitrile and vinyl acetate, carrying out copolymerization reaction to obtain a polyacrylonitrile powdery polymer, and dissolving the polyacrylonitrile powdery polymer in dimethylacetamide to obtain a spinning solution;
step 2, heating the spinning solution, extruding the spinning solution from a spinneret plate, and solidifying and forming the spinning solution in a dimethylacetamide aqueous solution to obtain nascent fiber;
and 3, adding 1000L of distilled water and 300ml of concentrated sulfuric acid (98 wt%) into a water tank at normal temperature and normal pressure, respectively connecting a positive electrode and a negative electrode of a direct current power supply with two ends of a graphite rod, vertically placing the graphite rod into the water tank, regulating the voltage to 15V, timing, and stirring for 15 days to obtain the electrolyzed carbon quantum dot acidic aqueous solution.
Step 4, separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device with the model of US2K to obtain a carbon quantum dot solution;
wherein the carbon quantum dots with the particle size of 2-10nm in the carbon quantum dot solution account for 60% of the total carbon quantum dots in the carbon quantum dot solution, and the concentration of the carbon quantum dots is 20 x 10 5 Per ml;
step 5, sequentially carrying out primary water washing, secondary water washing, tertiary water washing and quaternary water washing on the nascent fiber; in the second washing process, adding the carbon quantum dot solution into water to wash the nascent fiber;
wherein the mass ratio of the carbon quantum dot solution to the nascent fiber is 0.1:1;
in the second water washing process, the temperature is 50 ℃, the pressure is 1MPa, and the time is 20min; the temperature of the first washing, the third washing and the fourth washing is 70 ℃, the pressure is 0MPa, and the time is 5min.
Step 6: after the washing, the fiber tows are formed by drafting, and the acrylic fiber is prepared by oiling, drying and sizing the fiber tows.
Example 9:
step 1, mixing two monomers of acrylonitrile and vinyl acetate, carrying out copolymerization reaction to obtain a polyacrylonitrile powdery polymer, and dissolving the polyacrylonitrile powdery polymer in dimethylacetamide to obtain a spinning solution;
step 2, heating the spinning solution, extruding the spinning solution from a spinneret plate, and solidifying and forming the spinning solution in a dimethylacetamide aqueous solution to obtain nascent fibers;
and 3, adding 1000L of distilled water and 50ml of concentrated sulfuric acid (98 wt%) into a water tank at normal temperature and normal pressure, respectively connecting a positive electrode and a negative electrode of a direct current power supply with two ends of a graphite rod, vertically placing the graphite rod into the water tank, regulating the voltage to 20V, timing, and stirring for 5 days to obtain the electrolyzed carbon quantum dot acidic aqueous solution.
Step 4, separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device with the model of US2K to obtain a carbon quantum dot solution;
wherein, the carbon quantum dots with the grain diameter of 2-10nm in the carbon quantum dot solution account for 70 percent of the total carbon quantum dots in the carbon quantum dot solution, and the concentration of the carbon quantum dots is 0.1 per ml.
Step 5, sequentially carrying out primary water washing, secondary water washing, tertiary water washing and quaternary water washing on the nascent fiber; in the second washing process, adding the carbon quantum dot solution into water to wash the nascent fiber;
wherein the mass ratio of the carbon quantum dot solution to the nascent fiber is 0.1:1;
in the second water washing process, the temperature is 50 ℃, the pressure is 1MPa, and the time is 20min; the temperature of the first washing, the third washing and the fourth washing is 70 ℃, the pressure is 0MPa, and the time is 5min.
Step 6: after washing, drafting to form fiber tows, and oiling, drying and sizing the fiber tows to obtain the acrylic fibers.
Example 10:
step 1, mixing two monomers of acrylonitrile and vinyl acetate, carrying out copolymerization reaction to obtain a polyacrylonitrile powdery polymer, and dissolving the polyacrylonitrile powdery polymer in dimethylacetamide to obtain a spinning solution;
step 2, heating the spinning solution, extruding the spinning solution from a spinneret plate, and solidifying and forming the spinning solution in a dimethylacetamide aqueous solution to obtain nascent fiber;
and 3, adding 1000L of distilled water and 80ml of concentrated sulfuric acid (98 wt%) into a water tank at normal temperature and normal pressure, respectively connecting a positive electrode and a negative electrode of a direct current power supply with two ends of a graphite rod, vertically placing the graphite rod into the water tank, regulating the voltage to 20V, timing, and stirring for 3 days to obtain the electrolyzed carbon quantum dot acidic aqueous solution. .
Step 4, separating the carbon quantum dot acidic aqueous solution by adopting a membrane separation device with the model of US2K to obtain a carbon quantum dot solution;
wherein, the carbon quantum dots with the grain diameter of 2-10nm in the carbon quantum dot solution account for 70% of the total carbon quantum dots in the carbon quantum dot solution, and the concentration of the carbon quantum dots is 1/ml.
Step 5, sequentially carrying out primary water washing, secondary water washing, tertiary water washing and quaternary water washing on the nascent fiber; in the second washing process, adding the carbon quantum dot solution into water to wash the nascent fiber;
wherein the mass ratio of the carbon quantum dot solution to the nascent fiber is 0.1:1;
in the second washing process, the temperature is 50 ℃, the pressure is 1MPa, and the time is 20min; the temperature of the first washing, the third washing and the fourth washing is 70 ℃, the pressure is 0MPa, and the time is 5min.
Step 6: after washing, drafting to form fiber tows, and oiling, drying and sizing the fiber tows to obtain the acrylic fibers.
Comparative example 1:
the comparative example differs from example 1 only in that: the carbon quantum dots with the particle size of 2-10nm in the carbon quantum dot solution account for 60% of the total carbon quantum dots in the carbon quantum dot solution.
Comparative example 2:
the comparative example only differs from example 1 in that: no carbon quantum dot solution is added in the primary fiber washing process.
Comparative example 3:
the comparative example differs from example 1 only in that: replacing the carbon quantum dot solution with graphene aqueous dispersion.
Comparative example 4:
the comparative example only differs from example 1 in that: replacing the carbon quantum dot solution with an active carbon water dispersion liquid.
Comparative example 5:
the comparative example differs from example 1 only in that: in the second washing, the temperature was 70 ℃.
Comparative example 6:
the comparative example differs from example 1 only in that: in the second washing, the temperature was 80 ℃.
Comparative example 7:
the comparative example differs from example 1 only in that: in the second washing, the temperature was 90 ℃.
Comparative example 8:
the comparative example differs from example 1 only in that: the mass ratio of the carbon quantum dot solution to the nascent fiber is 1.
Comparative example 9:
the comparative example only differs from example 1 in that: the mass ratio of the carbon quantum dot solution to the nascent fiber is 2.
Comparative example 10:
the comparative example differs from example 1 only in that: the mass ratio of the carbon quantum dot solution to the nascent fiber is 3.
Comparative example 11:
the comparative example differs from example 1 only in that: the mass ratio of the carbon quantum dot solution to the nascent fiber is 5.
Comparative example 12:
the comparative example only differs from example 1 in that: adding dimethyl acetamide solution with equal carbon quantum dot concentration in the copolymerization reaction process of the step 1.
Comparative example 13:
the comparative example differs from example 1 only in that: adding a dimethylacetamide solution with equal carbon quantum dot concentration into the spinning solution obtained in the step 1.
Comparative example 14:
the comparative example differs from example 1 only in that: the concentration of the carbon quantum dots in the carbon quantum dot solution is 100 x 10 6 One per ml.
Comparative example 15:
the comparative example differs from example 1 only in that: the concentration of the carbon quantum dots in the carbon quantum dot solution is 1000 x 10 6 One per ml.
Comparative example 16:
the comparative example only differs from example 1 in that: the concentration of the carbon quantum dots in the carbon quantum dot solution is 10000 × 10 6 One per ml.
The invention measures the particle size of the carbon quantum dots, and the measuring method comprises the following steps: the measurement was carried out by a transmission electron microscope (JEOL, japan Electron JEOL Ltd.), under the following conditions: accelerating voltage of 10kV, preparing a sample by adopting a suspension method, putting the carbon quantum dot solution into a 2mL glass bottle, dispersing by using absolute ethyl alcohol, uniformly oscillating, dripping the sample on a sample copper net with the diameter of 3mm by using a dropper, putting the sample into a sample injector after drying, inserting the sample into a corresponding position of an electron microscope, observing, and randomly taking 100 particles for carrying out particle size statistics.
The invention measures the density of carbon quantum dots on fiber, and the measuring method comprises the following steps: the concentration of the carbon quantum dots is determined by fluorescence analysis, and the content of the carbon quantum dots is calculated by an external standard method.
The invention tests the far infrared performance of the acrylic fiber according to GB/T130127-2013.
The far infrared performance, the elongation at break and the fiber strength of the acrylic fibers obtained in example 1 and comparative examples 1 to 4 are measured, and the measurement results are shown in the following table 1:
table 1:
| group of | Density of carbon quantum dots on fiber/10 4 Per cm 2 | Far infrared performance/%) | Elongation at break/% | Fiber strength cN/dtex |
| Example 1 | 9 | 93 | 46 | 2.89 |
| Comparative example 1 | 0.4 | 92 | 41 | 2.38 |
| Comparative example 2 | / | 79 | 43 | 2.25 |
| Comparative example 3 | / | 80 | 42 | 2.37 |
| Comparative example 4 | / | 82 | 39 | 2.13 |
As can be seen from the above table, the far infrared performance of the acrylic fiber prepared in example 1 is better than that of the acrylic fiber prepared in comparative example 1. And the elongation at break and fiber strength of the acrylic fiber prepared in example 1 were higher than those of comparative example 1. Therefore, the higher the proportion of the carbon quantum dots with the particle size of 2-10nm in the carbon quantum dot solution to the total carbon quantum dots in the carbon quantum dot solution is, the better the far infrared performance and the mechanical performance of the obtained acrylic fiber are.
In addition, the far infrared performance corresponding to the acrylic fiber prepared in the embodiment 1 is far higher than that of the fiber corresponding to the comparative examples 2-4, the requirement of the standard GB/T130127-2013 on far infrared performance of the textile is met, and the acrylic fiber can be used as far infrared health care functional fabric in the fields of underwear, blankets, bedding, tents and the like. Meanwhile, the breaking elongation and the fiber strength of the acrylic fiber prepared in the embodiment 1 are higher than those of the fibers prepared in the comparative examples 2 and 4, which shows that the mechanical property of the acrylic fiber can be effectively improved by adding the carbon quantum dot solution in the fiber washing process.
The far infrared performance, the elongation at break and the fiber strength of the acrylic fibers obtained in example 1 and comparative examples 5 to 7 were measured, and the measurement results are shown in the following table 2:
table 2:
| group of | Second Water washing temperature (. Degree. C.) | Far infrared performance/%) | Elongation at break/% | Fiber strength cN/dtex |
| Example 1 | 60 | 93 | 46 | 2.89 |
| Comparative example 5 | 70 | 91 | 43 | 2.64 |
| Comparative example 6 | 80 | 90 | 43 | 2.41 |
| Comparative example 7 | 90 | 88 | 41 | 2.36 |
As is apparent from Table 2, the far infrared properties, elongation at break and fiber strength of the acrylic fibers obtained in example 1 were higher than those of the acrylic fibers obtained in comparative examples 5, 6 and 7. It is understood from this that if the washing temperature is too high, it is not favorable to improve the far infrared performance, elongation at break and fiber strength of the acrylic fiber.
The far infrared performance, the elongation at break and the fiber strength of the acrylic fibers obtained in example 1, comparative example 8 to comparative example 11 were measured, and the results are shown in the following table 3:
table 3:
| group of | Carbon quantum dot solution and nascent fiberIn mass ratio of | Far infrared performance/%) | Elongation at break/% | Fiber strength cN/dtex |
| Example 1 | 3.5：1 | 93 | 46 | 2.89 |
| Comparative example 8 | 1:1 | 90 | 41 | 2.52 |
| Comparative example 9 | 2:1 | 91 | 45 | 2.81 |
| Comparative example 10 | 3:1 | 93 | 45 | 2.85 |
| Comparative example 11 | 5:1 | 94 | 44 | 2.36 |
It can be known from table 3 that the larger the mass ratio of the carbon quantum dot solution to the nascent fiber is, the higher the far infrared performance and the fiber strength of the obtained acrylic fiber are, which is beneficial to improving the quality of the acrylic fiber. In addition, the mass ratio of the carbon quantum dot solution to the nascent fiber is increased to a certain extent, so that the strength and the elongation at break of the fiber can be effectively improved, and the mechanical property of the fiber is improved.
The far infrared performance, the elongation at break and the fiber strength of the acrylic fibers obtained in example 1, comparative example 12 and comparative example 13 were measured, and the results are shown in the following table 4:
table 4:
| group of | Far infrared performance/%) | Elongation at break/% | Fiber strength cN/dtex |
| Example 1 | 93 | 46 | 2.89 |
| Comparative example 12 | 90 | 48 | 2.91 |
| Comparative example 13 | 92 | 49 | 2.96 |
As can be seen from the above table, the addition of the carbon quantum dot solution during the water washing process is better in far infrared performance than the addition of the carbon quantum dot solution in the copolymerization reaction and the spinning solution. The carbon quantum dot solution is added in the spinning solution or the copolymerization reaction process, and compared with the carbon quantum dot solution added in the water washing process, the acrylic fiber has higher breaking elongation and fiber strength and better mechanical property.
The present invention also performs the far infrared performance, elongation at break and fiber strength measurements on the acrylic fibers obtained in example 1, comparative example 14 to comparative example 16, and the results are shown in the following table 5:
table 5:
| group of | Concentration of carbon Quantum dots (one/ml) | Far infrared Property (%) | Elongation at Break (%) | Fiber Strength (cN/dtex) |
| Example 1 | 10*10 6 | 93 | 46 | 2.89 |
| Comparative example 14 | 100*10 6 | 94 | 51 | 2.97 |
| Comparative example 15 | 1000*10 6 | 94 | 53 | 2.99 |
| Comparative example 16 | 10000*10 6 | 91 | 43 | 2.65 |
As can be seen from table 5, the elongation at break and the fiber strength of the acrylic fiber are both improved with the increase of the concentration of the carbon quantum dots within a certain range, i.e., the increase of the concentration of the carbon quantum dots is beneficial to improving the mechanical properties of the acrylic fiber.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of carbon quantum dot acrylic fiber with far infrared performance comprises the following steps:
step 1, forming a spinning solution after copolymerization reaction of acrylonitrile and a comonomer;
step 2, heating the spinning solution and extruding the spinning solution from a spinneret plate to form nascent fibers;
step 3, washing the nascent fiber, drafting, oiling, drying and shaping to form acrylic fiber;
the method is characterized in that: adding a carbon quantum dot solution in the copolymerization reaction process in the step 1;
and/or adding a carbon quantum dot solution into the spinning solution in the step 1 or the step 2;
and/or adding a carbon quantum dot solution in the water washing process of the step 3.
2. The method for preparing carbon quantum dot acrylic fiber with far infrared performance as claimed in claim 1, wherein the method comprises the following steps: the concentration of the carbon quantum dots in the carbon quantum dot solution is 0.1-10000 x 10 6 Per ml, preferably 1-100 x 10 6 One per ml.
3. The method for preparing carbon quantum dot acrylic fiber with far infrared performance as claimed in claim 1 or 2, characterized in that: in the carbon quantum dot solution, carbon quantum dots with the particle size of 2-10nm account for 60-100%, preferably 80-100% of the total carbon quantum dots.
4. The method for preparing carbon quantum dot acrylic fiber with far infrared performance as claimed in any one of claims 1-3, wherein the method comprises the following steps: the carbon quantum dot solution added in the step 1 and the step 2 is a carbon quantum dot organic solution.
5. The method for preparing carbon quantum dot acrylic fiber with far infrared performance as claimed in claim 4, characterized in that: the organic solvent in the carbon quantum dot organic solution is the same as the organic solvent in the spinning solution;
preferably, the organic solvent is dimethylacetamide.
6. The method for preparing carbon quantum dot acrylic fiber with far infrared performance as claimed in any one of claims 1-5, wherein the method comprises the following steps: the carbon quantum dot solution added in the step 3 is a carbon quantum dot aqueous solution.
7. The method for preparing carbon quantum dot acrylic fiber with far infrared performance as claimed in any one of claims 1-6, wherein the method comprises the following steps: in the step 3, the washing temperature is 30-95 ℃, the washing pressure is 0-1Mpa, and the washing time is 2-30min;
preferably, the temperature of the water washing is 40-90 ℃.
8. The method for preparing carbon quantum dot acrylic fiber with far infrared performance as claimed in any one of claims 1 to 7, wherein the method comprises the following steps: in the step 3, the nascent fiber is washed for multiple times, and a carbon quantum dot solution is added into at least one of the multiple times of washing;
preferably, the nascent fiber is subjected to at least first water washing, second water washing and third water washing in sequence, and the carbon quantum dot solution is added in the first water washing and the second water washing.
9. The method for preparing carbon quantum dot acrylic fiber with far infrared performance as claimed in any one of claims 1-8, wherein the method comprises the following steps: the mass ratio of the carbon quantum dot solution to the primary fiber is 0.1-15, preferably 1-5.
10. An acrylic fiber is characterized in that: the acrylic fiber is provided with carbon quantum dots;
preferably, the density of the carbon quantum dots on the acrylic fiber is 0.01-1000 x 10 4 Per cm 2 ；
Preferably, the density of the carbon quantum dots on the acrylic fiber is 1-100 x 10 4 Per cm 2 ；
Preferably, the carbon quantum dots with the particle size of 2-10nm on the acrylic fiber account for 80-100% of the total carbon quantum dots on the acrylic fiber;
preferably, the carbon quantum dots with the particle size of 2-10nm on the acrylic fiber account for 60-100% of the total carbon quantum dots on the acrylic fiber carbon;
preferably, the fiber strength of the acrylic fiber is 2.36-2.99cN/dtex;
preferably, the preparation method is adopted in any one of the preparation methods of the claims 1-9.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102944538A (en) * | 2012-08-06 | 2013-02-27 | 中国科学院新疆理化技术研究所 | Preparation method and use of fluorescent carbon quantum dot/polyacrylonitrile nanofiber membrane |
| CN106435802A (en) * | 2016-09-29 | 2017-02-22 | 宁波中新腈纶有限公司 | Acrylic fibers with peanut-shaped cross section and production method thereof |
| CN112127000A (en) * | 2020-09-04 | 2020-12-25 | 河北艾科瑞纤维有限公司 | Far infrared acrylic fiber and preparation method thereof |
| CN112663330A (en) * | 2019-12-24 | 2021-04-16 | 中科量子(广州)新材料有限公司 | Fiber, non-woven fabric, mask cloth and mask containing nano graphene and preparation method |
-
2021
- 2021-04-26 CN CN202110453398.4A patent/CN115247285B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102944538A (en) * | 2012-08-06 | 2013-02-27 | 中国科学院新疆理化技术研究所 | Preparation method and use of fluorescent carbon quantum dot/polyacrylonitrile nanofiber membrane |
| CN106435802A (en) * | 2016-09-29 | 2017-02-22 | 宁波中新腈纶有限公司 | Acrylic fibers with peanut-shaped cross section and production method thereof |
| CN112663330A (en) * | 2019-12-24 | 2021-04-16 | 中科量子(广州)新材料有限公司 | Fiber, non-woven fabric, mask cloth and mask containing nano graphene and preparation method |
| CN112127000A (en) * | 2020-09-04 | 2020-12-25 | 河北艾科瑞纤维有限公司 | Far infrared acrylic fiber and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| BANAFSHEH SAFAEI: "Synthesis and Properties of Photoluminescent Carbon Quantum Dot/Polyacrylonitrile Composite Nanofibers", SMART SCIENCE, pages 1 - 8 * |
| ZHENG LIU: "Lyotropic Liquid Crystal of Polyacrylonitrile-Grafted Graphene Oxide and Its Assembled Continuous Strong Nacre-Mimetic Fibers", MACROMOLECULES, no. 46, pages 6931 * |
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