CN114622329A - Nano antibacterial sea-island fiber fabric and manufacturing method thereof - Google Patents
Nano antibacterial sea-island fiber fabric and manufacturing method thereof Download PDFInfo
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- CN114622329A CN114622329A CN202210238321.XA CN202210238321A CN114622329A CN 114622329 A CN114622329 A CN 114622329A CN 202210238321 A CN202210238321 A CN 202210238321A CN 114622329 A CN114622329 A CN 114622329A
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 86
- 239000000835 fiber Substances 0.000 title claims abstract description 71
- 239000004744 fabric Substances 0.000 title claims abstract description 60
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 19
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 80
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 55
- 239000002114 nanocomposite Substances 0.000 claims abstract description 50
- 239000002078 nanoshell Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 5
- 238000009941 weaving Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 33
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 30
- 239000004246 zinc acetate Substances 0.000 claims description 30
- 229910002804 graphite Inorganic materials 0.000 claims description 27
- 239000010439 graphite Substances 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 22
- 238000002156 mixing Methods 0.000 claims description 20
- 238000009210 therapy by ultrasound Methods 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229940011182 cobalt acetate Drugs 0.000 claims description 13
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000009987 spinning Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229920000728 polyester Polymers 0.000 claims description 8
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 7
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- 229910017052 cobalt Inorganic materials 0.000 claims description 6
- 239000010941 cobalt Substances 0.000 claims description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 6
- -1 polyethylene Polymers 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 229910052725 zinc Inorganic materials 0.000 claims description 6
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920002223 polystyrene Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 239000004753 textile Substances 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 239000011787 zinc oxide Substances 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 12
- 239000002105 nanoparticle Substances 0.000 description 10
- 229910001429 cobalt ion Inorganic materials 0.000 description 6
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 6
- 238000002604 ultrasonography Methods 0.000 description 5
- 239000000155 melt Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 241000191967 Staphylococcus aureus Species 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 241000588724 Escherichia coli Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000003385 bacteriostatic effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000222122 Candida albicans Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229940095731 candida albicans Drugs 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000012510 hollow fiber Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
- D03D15/292—Conjugate, i.e. bi- or multicomponent, fibres or filaments
-
- 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
- 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
- D01F1/103—Agents inhibiting growth of microorganisms
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/50—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the properties of the yarns or threads
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04B—KNITTING
- D04B1/00—Weft knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
- D04B1/14—Other fabrics or articles characterised primarily by the use of particular thread materials
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04B—KNITTING
- D04B21/00—Warp knitting processes for the production of fabrics or articles not dependent on the use of particular machines; Fabrics or articles defined by such processes
-
- 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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic System
Abstract
The invention belongs to the technical field of textile fabrics, and particularly discloses a nano antibacterial sea-island fiber fabric and a manufacturing method thereof, wherein the fabric comprises the following raw materials: the composite material comprises an island component, a sea component, nano shell powder and a zinc oxide @ graphene nanocomposite, wherein the mass of the zinc oxide @ graphene nanocomposite is 5-8% of that of the island component, and the mass of the nano shell powder is 3-5% of that of the island component. The manufacturing method of the fabric comprises the following steps: (1) preparing a zinc oxide @ graphene nanocomposite; (2) preparing island phase functional master batches; (3) preparing nano antibacterial sea-island precursor; (4) preparing nano antibacterial sea-island fibers; (5) preparing nano antibacterial sea-island fiber yarns; (6) and (6) weaving. The invention not only reduces the consumption of nano materials, but also improves the mechanical property of the fabric, and the fabric is soft and comfortable to use.
Description
Technical Field
The invention relates to the technical field of textile fabrics, in particular to a nano antibacterial sea-island fiber fabric and a manufacturing method thereof.
Background
The sea-island fiber is a bi-component fiber with a sea and island (continuous phase is sea, disperse phase is island) structure prepared by blending spinning or composite spinning two thermodynamics incompatible high polymers according to a certain proportion. Sea-island fiber can be dissolved to remove sea component to obtain superfine fiber, and sea-island component is removed to obtain porous hollow fiber with honeycomb structure.
The sea-island fiber has small monofilament linear density and large specific surface area, and the fabric woven by the sea-island fiber has soft and smooth hand feeling and obvious comfort, so that the fabric with high tightness, hygroscopicity, water repellency, unique aesthetic property and fashion style can be prepared from the sea-island fiber.
With the development of socio-economic, the sea-island fiber fabric is required to have higher requirements, and it is desired that the sea-island fiber fabric has the above-mentioned advantages and also has antibacterial properties so as to inhibit the growth of bacteria during the use of the fabric, thereby improving the hygiene and safety of the use of the fabric. At present, it has been tried to add nanoparticles having antibacterial effect such as nano silica, nano silver/copper powder, nano zinc oxide, etc. to sea-island fiber to make sea-island fiber having antibacterial effect, but since the particle size of the nanoparticles is small, agglomeration is easily generated in the sea-island fiber to affect the antibacterial effect of the sea-island fiber, it is necessary to add a larger amount of nanoparticles to make the sea-island fiber have better antibacterial effect. However, the more the amount of the added nanoparticles is, the more the mechanical properties of the sea-island fiber are affected, and the higher the cost is, so that there is a need for a sea-island fiber having a good antibacterial effect and a small amount of nanoparticles added.
Disclosure of Invention
In view of the above-mentioned disadvantages of the prior art, the present invention aims to provide a nano antibacterial sea-island fiber fabric and a manufacturing method thereof, which are used for solving the problem of excessive decrease of mechanical properties of the sea-island fiber caused by excessive addition of nano particles in the prior art.
In order to achieve the above objects and other related objects, the present invention provides a nano antibacterial sea-island fiber fabric, comprising the following raw materials: the composite material comprises an island component, a sea component, nano shell powder and a zinc oxide @ graphene nanocomposite, wherein the mass of the zinc oxide @ graphene nanocomposite is 5-8% of that of the island component, and the mass of the nano shell powder is 3-5% of that of the island component.
The invention also provides a manufacturing method of the nano antibacterial sea-island fiber fabric, which comprises the following steps:
s1, preparing the zinc oxide @ graphene nanocomposite: adding graphite oxide into ethylene glycol, performing ultrasonic treatment to obtain graphite oxide dispersion liquid, adding zinc acetate into ethylene glycol, performing ultrasonic treatment to obtain zinc acetate solution, adding the zinc acetate solution into the graphite oxide dispersion liquid, uniformly stirring, adding alkali liquor to adjust the pH value to 8.5-9, stirring for 30-40 min, adding hydrazine hydrate, performing hydrothermal reaction at 155-165 ℃ for more than 24h, performing suction filtration, taking a filter cake, washing, performing vacuum drying at 60-65 ℃ for 12-13 h, and grinding for later use;
s2, preparing island phase functional master batches: mixing the island component, the nano shell powder and the zinc oxide @ graphene nano composite material in the step S1, and then carrying out melt blending under the action of ultrasonic waves and microwaves to prepare an island phase functional master batch;
s3, preparing the nano antibacterial sea-island precursor: mixing the sea component with the island phase functional master batch in the step S2, and then carrying out melt blending spinning to obtain nano antibacterial sea island precursor;
s4, preparing the nano antibacterial sea-island fiber: the nano antibacterial sea-island protofilament in the step S3 is subjected to the procedures of oiling, stretching, curling, drying and cutting to obtain the nano antibacterial sea-island fiber;
s5, preparing the nano antibacterial sea-island fiber yarn: spinning the nano antibacterial sea-island fiber obtained in the step S5 to obtain a nano antibacterial sea-island fiber yarn;
s6, preparing raw cloth: and (4) weaving the nano antibacterial sea-island fiber yarn in the step S5 to obtain the original cloth.
Optionally, the particle sizes of the nano shell powder and the zinc oxide @ graphene nano composite material are both 20-100 nm.
Optionally, the mass ratio of the island phase functional master batch to the sea component is 3: 2-2.5.
Optionally, the island component is selected from one of polyester, polyamide and polyacrylonitrile, and the sea component is selected from one of water-soluble polyester, polyethylene, polypropylene, polyvinyl alcohol, polystyrene and acrylate copolymer.
Optionally, the method for manufacturing the nano antibacterial sea-island fiber fabric further comprises the following steps:
s7, after finishing: taking a sodium hydroxide solution with the concentration of 9-11 g/L as a finishing liquid, soaking the original cloth in the step S6 into the finishing liquid at 40-50 ℃, heating to 85-90 ℃, keeping the temperature for 15-20 min, heating to 105-115 ℃, and keeping the temperature for 30-45 min; then, cleaning with hot water at the temperature of 75-80 ℃ for 15-20 min, and adding glacial acetic acid for neutralization to enable the pH value of the cleaning solution to reach 6-7; and then drying the mixture at 105-110 ℃ to constant weight.
Optionally, in step S1, when adding zinc acetate to ethylene glycol, adding cobalt acetate at the same time, performing ultrasonic treatment to obtain a zinc acetate/cobalt acetate mixed solution, adding the zinc acetate/cobalt acetate mixed solution to the graphite oxide dispersion, and stirring uniformly.
Optionally, in step S1, the molar ratio of zinc to cobalt is 1: 0.005-0.009.
Optionally, the mass ratio of the graphite oxide to the zinc acetate is 2.5-3.5: 1000.
Optionally, in step S2, the mass of the zinc oxide @ graphene nanocomposite is 5-7% of the mass of the island component.
Optionally, in step S1, the mass ratio of the graphite oxide to the hydrazine hydrate is 10: 7-10.
Optionally, in step S2, the ultrasonic power is 150-170W, the microwave power is 120-200W, and the duration of the microwave is 25-30S.
Optionally, in step S1, when the graphite oxide is subjected to ultrasound in ethylene glycol, the ultrasonic power is 350 to 400W, and the duration of the ultrasound is 1.5 to 2 hours.
Optionally, in step S1, when the zinc acetate is subjected to ultrasound in ethylene glycol, the ultrasonic power is 300-360W, and the duration of the ultrasound is 10-30 min.
As described above, the nano antibacterial sea-island fiber fabric and the manufacturing method thereof of the present invention have the following beneficial effects:
1. according to the invention, the zinc oxide @ graphene nanocomposite is adopted to replace single nano-particles with antibacterial functions such as nano-zinc oxide, and the antibacterial performance of the zinc oxide @ graphene nanocomposite is superior to that of nano-zinc oxide. The nano zinc oxide has small particle size, is easy to agglomerate, and has influenced antibacterial performance, the graphene has a unique planar network structure and a huge specific surface area, and oxygen-containing functional groups rich on the surface provide crystal sites for the growth of nano zinc oxide particles, so that the nano zinc oxide can be uniformly distributed on the surface of the graphene, the agglomeration of the nano zinc oxide is prevented, the nano zinc oxide maintains higher surface activity, and the antibacterial performance of the nano zinc oxide is improved; secondly, the graphene provides a good interface for bacteria adsorption, and the bacteria are adsorbed on the zinc oxide @ graphene nanocomposite, so that the nano zinc oxide can conveniently play an antibacterial role. Therefore, on the premise that the fabric has the same antibacterial property, the addition amount of the zinc oxide @ graphene nanocomposite is obviously less than that of the nano zinc oxide, so that the problem that the mechanical properties of the sea-island fibers are excessively reduced due to excessive addition of the nano particles is solved.
2. According to the invention, the unique planar network structure of graphene in the zinc oxide @ graphene nanocomposite and substances in island components can form a composite structure, so that the mechanical properties of the sea-island fibers are improved. Moreover, the nano shell powder is a natural organic-inorganic hybrid material, has a unique crossed layered structure, and has fracture toughness and strength which are incomparable with common calcium carbonate, so that the mechanical property of the sea-island fiber is further improved by adding the nano shell powder.
3. In the invention, in the process of preparing the zinc oxide @ graphene nanocomposite, the cobalt acetate is added, so that the zinc oxide @ graphene nanocomposite doped with cobalt ions is obtained, and the cobalt ions can improve the antibacterial property of the nano zinc oxide in the visible light range, thereby further reducing the addition of the zinc oxide @ graphene nanocomposite.
4. According to the invention, ultrasonic waves and microwaves are jointly used for acting on the melting and blending process of the island component, the nano shell powder and the zinc oxide @ graphene nanocomposite, the ultrasonic waves can enable particles to be dispersed more uniformly in a medium, and the microwaves can enable the zinc oxide @ graphene nanocomposite to generate high-energy high heat to overcome van der Waals force between graphene sheets, so that the zinc oxide @ graphene nanocomposite is dispersed more uniformly. Therefore, the nano shell powder and zinc oxide @ graphene nanocomposite can be uniformly dispersed in the island component, and the mechanical property of the sea-island fiber is further improved.
5. The fabric disclosed by the invention is soft in hand feeling, comfortable to use and good in antibacterial function.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The invention provides a method for manufacturing a nano antibacterial sea-island fiber fabric, which comprises the following steps:
s1, preparing the zinc oxide @ graphene nanocomposite: adding graphite oxide into ethylene glycol, performing ultrasonic treatment to obtain graphite oxide dispersion liquid, adding zinc acetate into the ethylene glycol, performing ultrasonic treatment to obtain a zinc acetate solution, adding the zinc acetate solution into the graphite oxide dispersion liquid, uniformly stirring, adding alkali liquor to adjust the pH value to 8.5-9, stirring for 30-40 min, adding hydrazine hydrate, performing hydrothermal reaction at 155-165 ℃ for more than 24h, performing suction filtration, taking a filter cake, washing, performing vacuum drying at 60-65 ℃ for 12-13 h, and grinding for later use.
The graphite oxide is prepared from graphite powder as a raw material by a Hummers method, and the preparation of the graphite oxide by the Hummers method belongs to the technology known by persons skilled in the art and is not described herein again. The mass ratio of the graphite oxide to the zinc acetate is 2.5-3.5: 1000; the mass ratio of the graphite oxide to the hydrazine hydrate is 10: 7-10; when graphite oxide is subjected to ultrasonic treatment in ethylene glycol, the ultrasonic power is 350-400W, and the ultrasonic treatment time is 1.5-2 h; when zinc acetate is subjected to ultrasonic treatment in ethylene glycol, the ultrasonic power is 300-360W, and the ultrasonic treatment time is 10-30 min; the particle size of the zinc oxide @ graphene nanocomposite is 20-100 nm.
S2, preparing island phase functional master batches: and (4) mixing the island component, the nano shell powder and the zinc oxide @ graphene nano composite material obtained in the step S1, and then carrying out melt blending under the action of ultrasonic waves and microwaves, wherein the melt blending temperature is 270-275 ℃, so as to obtain the island phase functional master batch.
Wherein the island component is selected from one of polyester, polyamide and polyacrylonitrile; the mass of the zinc oxide @ graphene nano composite material is 5-8% of that of the island component, the mass of the nano shell powder is 3-5% of that of the island component, and the particle size of the nano shell powder is 20-100 nm; the power of the ultrasonic wave is 150-170W, the power of the microwave is 120-200W, and the duration of the microwave is 25-30 s.
S3, preparing the nano antibacterial sea-island precursor: and (4) mixing the sea component with the island phase functional master batch in the step S2, and then carrying out melt blending spinning, wherein the melt blending temperature reaches 272-285 ℃, so as to obtain the nano antibacterial sea island precursor.
Wherein the sea component is selected from one of water-soluble polyester, polyethylene, polypropylene, polyvinyl alcohol, polystyrene and acrylate copolymer; the mass ratio of the island phase functional master batch to the sea component is 3: 2-2.5.
S4, preparing the nano antibacterial sea-island fiber: and (4) oiling, stretching, curling, drying and cutting the nano antibacterial sea-island protofilament in the step (S3) to obtain the nano antibacterial sea-island fiber.
S5, preparing the nano antibacterial sea-island fiber yarn: the nano antibacterial sea-island fiber obtained in step S5 is subjected to a spinning step to obtain a nano antibacterial sea-island fiber yarn.
S6, preparing raw cloth: and (4) weaving the nano antibacterial sea-island fiber yarn in the step S5 to obtain the original cloth.
S7, after finishing: taking a sodium hydroxide solution with the concentration of 9-11 g/L as a finishing liquid, soaking the original cloth in the step S6 into the finishing liquid at 40-50 ℃, heating to 85-90 ℃, keeping the temperature for 15-20 min, heating to 105-115 ℃, and keeping the temperature for 30-45 min; then, cleaning with hot water at the temperature of 75-80 ℃ for 15-20 min, and adding glacial acetic acid for neutralization to enable the pH value of the cleaning solution to reach 6-7; and then drying the mixture at 105-110 ℃ to constant weight.
In another embodiment provided by the present invention, in step S1, when adding zinc acetate into ethylene glycol, adding cobalt acetate at the same time, performing ultrasound to obtain a zinc acetate/cobalt acetate mixed solution, adding the zinc acetate/cobalt acetate mixed solution into the graphite oxide dispersion, stirring uniformly, and obtaining the zinc oxide @ graphene nanocomposite doped with cobalt ions according to the preparation method of the zinc oxide @ graphene nanocomposite. Wherein the molar ratio of the zinc to the cobalt is 1: 0.005-0.009. In step S2, the mass of the zinc oxide @ graphene nanocomposite is 5-7% of the mass of the island component.
The invention also provides the nano antibacterial sea-island fiber fabric prepared by the preparation method.
The present invention will be described in detail with reference to the following specific examples. It should also be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention, and that numerous insubstantial modifications and adaptations of the invention described above will occur to those skilled in the art. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
A manufacturing method of a nano antibacterial sea-island fiber fabric comprises the following steps:
s1, preparing the zinc oxide @ graphene nanocomposite: adding 30mg of graphite oxide into 20mL of ethylene glycol, and carrying out ultrasonic treatment to obtain a graphite oxide dispersion liquid, wherein the ultrasonic power is 400W, and the ultrasonic treatment time is 2 h. Adding 10g of zinc acetate into 30mL of ethylene glycol, and carrying out ultrasonic treatment to obtain a zinc acetate solution, wherein the ultrasonic power is 360W, and the ultrasonic treatment time is 10 min. And then, adding a zinc acetate solution into the graphite oxide dispersion liquid, uniformly stirring, adding a sodium hydroxide solution to adjust the pH value to 9, stirring for 30min, adding 21mg of hydrazine hydrate, carrying out hydrothermal reaction at 160 ℃ for 24h, carrying out suction filtration after the reaction is finished, taking a filter cake, washing with deionized water and ethanol, carrying out vacuum drying at 60 ℃ for 12h, and grinding for later use. The particle size of the obtained zinc oxide @ graphene nanocomposite is 20-100 nm.
S2, preparing island phase functional master batches: drying the PET master batch (island component) at 120 ℃ until the water content of the PET master batch is below 0.4%, and simultaneously drying the nano shell powder (with the particle size of 20-100 nm) at 80 ℃ for 2 h. And then, mixing the PET master batch, the nano shell powder and the zinc oxide @ graphene nano composite material obtained in the step S1, extruding the mixture by a double-screw extruder (the melt blending temperature of the double-screw extruder reaches about 270 ℃), cooling and granulating to obtain the island-phase functional master batch. The double-screw extruder is positioned in an ultrasonic field and a microwave field, the ultrasonic power of the ultrasonic field is 150W, the microwave power is 200W, and the microwave duration is 25 s. The mass of the zinc oxide @ graphene nano composite material is 5% of that of the PET master batch, and the mass of the nano shell powder is 3% of that of the PET master batch.
S3, preparing the nano antibacterial sea-island precursor: and (2) drying the water-soluble polyester (sea component) at 120 ℃ for 5h, and then carrying out melt blending spinning on the island phase functional master batch in the step S2 and the water-soluble polyester on a double-screw extruder according to the mass ratio of 3:2 (the melt blending temperature of the double-screw extruder reaches about 280 ℃) to obtain the nano antibacterial sea-island precursor.
S4, preparing the nano antibacterial sea-island fiber: and (4) oiling, stretching, curling, drying and cutting the nano antibacterial sea-island protofilament in the step (S3) to obtain the nano antibacterial sea-island fiber.
S5, preparing the nano antibacterial sea-island fiber yarn: the nano antibacterial sea-island fiber obtained in step S5 is subjected to a spinning step to obtain a nano antibacterial sea-island fiber yarn.
S6, preparing raw cloth: the nano antibacterial sea-island fiber yarn in step S5 is subjected to a weaving process to obtain a raw cloth.
S7, post-finishing: taking a sodium hydroxide solution with the concentration of 10g/L as a finishing liquid, soaking the original cloth in the step S6 into the finishing liquid at 45 ℃, heating to 85 ℃, keeping the temperature for 15min, heating to 110 ℃, and keeping the temperature for 35 min; then, cleaning with hot water at the temperature of 75 ℃ for 20min, and adding glacial acetic acid for neutralization to enable the pH value of the cleaning solution to reach 6-7; and then drying at 110 ℃ to constant weight to obtain the nano antibacterial sea-island fiber fabric.
Example 2
The present embodiment is different from embodiment 1 in that: in this example, the mass of the zinc oxide @ graphene nanocomposite is 8% of the mass of the island component.
Example 3
The present embodiment is different from embodiment 1 in that: in this example, the mass of the zinc oxide @ graphene nanocomposite is 7% of the mass of the island component.
Example 4
The present embodiment is different from embodiment 1 in that: in this example, the mass of the nano shell powder was 5% of the mass of the island component.
Example 5
The present embodiment is different from embodiment 1 in that: in step S1 of this embodiment, when zinc acetate is added into ethylene glycol, cobalt acetate is simultaneously added, a zinc acetate/cobalt acetate mixed solution is obtained by ultrasonic processing, and the zinc acetate/cobalt acetate mixed solution is added into the graphite oxide dispersion liquid and stirred uniformly, so as to obtain the zinc oxide @ graphene nanocomposite doped with cobalt ions. Wherein the molar ratio of the zinc to the cobalt is 1: 0.007.
Example 6
The present embodiment is different from embodiment 5 in that: in this example, the mass of the zinc oxide @ graphene nanocomposite is 7% of the mass of the island component.
Example 7
This embodiment is different from embodiment 5 in that: the molar ratio of zinc to cobalt was 1: 0.009.
Example 8
This embodiment is different from embodiment 5 in that: the molar ratio of zinc to cobalt was 1: 0.005.
Comparative example 1
This comparative example differs from example 1 in that: in step S2 of this comparative example, ultrasonic waves and microwaves were not used.
Comparative example 2
This comparative example differs from example 1 in that: in the comparative example, the zinc oxide @ graphene nanocomposite material is replaced by the same amount of nano zinc oxide.
Examples of the experiments
Evaluation of antibacterial properties of textiles according to "GB/T20994.3-2008, section 3: the oscillation method is used for carrying out antibacterial property tests on the fabrics of the embodiments 1-8 and the comparative examples 1-2, the washing method of a color fastness to washing tester is adopted, and the antibacterial rate of the fabric after 20 times of washing is tested, and the results are shown in table 1.
The fabrics of examples 1-8 and comparative examples 1-2 were subjected to a breaking strength test according to "GB/T3923.1-2013 tensile properties of textile fabrics", and the results are shown in Table 1.
TABLE 1 fracture Strength and bacteriostatic Table of each example and comparative example
(note: the bacteriostasis rate to staphylococcus aureus and colibacillus is more than or equal to 70 percent, or the bacteriostasis rate to candida albicans is more than or equal to 60 percent, and the sample has antibacterial effect)
As can be seen from table 1, the breaking strength and the bacteriostatic ratio of example 1 are respectively higher than those of comparative example 1, which shows that the dispersibility of the zinc oxide @ graphene nanocomposite and the nano shell powder can be improved by ultrasonic waves and microwaves, and further the mechanical properties of the fabric can be improved.
The fracture strength of example 1 is higher than that of comparative example 2, which shows that the mechanical property of the fabric can be improved by the zinc oxide @ graphene nanocomposite material compared with nano zinc oxide. The bacteriostasis rate of the embodiment 1 is higher than that of the comparative example 2, which shows that the antibacterial effect of the zinc oxide @ graphene nano composite material is superior to that of nano zinc oxide. Therefore, on the premise that the fabric achieves the same antibacterial effect, the zinc oxide @ graphene nanocomposite is less in addition amount and lower in cost.
Example 1 compares with example 5, and example 3 compares with example 6, it is easy to find that the bacteriostasis rate of example 5 is higher than that of example 1, and even the bacteriostasis rates of example 5 to staphylococcus aureus and escherichia coli are respectively higher than that of example 3 to staphylococcus aureus and escherichia coli; the bacteriostasis rate of example 6 is higher than that of example 3, and even the bacteriostasis rate of example 6 is higher than that of example 2. Therefore, the antibacterial effect of the zinc oxide @ graphene nanocomposite doped with cobalt ions is superior to that of the zinc oxide @ graphene nanocomposite not doped with cobalt ions.
In conclusion, the zinc oxide @ graphene nanocomposite is adopted to replace single nano zinc oxide and other nano particles with antibacterial functions, and when the fabric achieves the same antibacterial effect, the addition amount of the nano materials is reduced, so that the problem that the mechanical properties of the sea-island fibers are excessively reduced due to excessive addition of the nano particles is solved, the mechanical properties of the fabric are improved, and the cost is reduced. In addition, the mode of combined action of ultrasonic waves and microwaves is adopted, so that the dispersion uniformity of the nano material in the island components is improved, and the antibacterial property and the mechanical property of the fabric are further improved. Moreover, the fabric disclosed by the invention is soft in hand feeling and comfortable to use.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. The nano antibacterial sea-island fiber fabric is characterized by comprising the following raw materials: the composite material comprises an island component, a sea component, nano shell powder and a zinc oxide @ graphene nanocomposite, wherein the mass of the zinc oxide @ graphene nanocomposite is 5-8% of that of the island component, and the mass of the nano shell powder is 3-5% of that of the island component.
2. The nano antibacterial sea-island fiber fabric according to claim 1, wherein: the particle size of the nano shell powder and the particle size of the zinc oxide @ graphene nano composite material are both 20-100 nm;
and/or the mass ratio of the island phase functional master batch to the sea component is 3: 2-2.5;
and/or the island component is selected from one of polyester, polyamide and polyacrylonitrile, and the sea component is selected from one of water-soluble polyester, polyethylene, polypropylene, polyvinyl alcohol, polystyrene and acrylate copolymer.
3. The method for manufacturing the nano antibacterial sea-island fiber fabric according to claim 1 or 2, which comprises the following steps:
s1, preparing the zinc oxide @ graphene nanocomposite: adding graphite oxide into ethylene glycol, performing ultrasonic treatment to obtain graphite oxide dispersion liquid, adding zinc acetate into ethylene glycol, performing ultrasonic treatment to obtain zinc acetate solution, adding the zinc acetate solution into the graphite oxide dispersion liquid, uniformly stirring, adding alkali liquor to adjust the pH value to 8.5-9, stirring for 30-40 min, adding hydrazine hydrate, performing hydrothermal reaction at 155-165 ℃ for more than 24h, performing suction filtration, taking a filter cake, washing, performing vacuum drying at 60-65 ℃ for 12-13 h, and grinding for later use;
s2, preparing island phase functional master batches: mixing the island component, the nano shell powder and the zinc oxide @ graphene nano composite material in the step S1, and then carrying out melt blending under the action of ultrasonic waves and microwaves to prepare an island phase functional master batch;
s3, preparing the nano antibacterial sea-island precursor: mixing the sea component with the island phase functional master batches obtained in the step S2, and then carrying out melt blending spinning to obtain nano antibacterial sea island precursor;
s4, preparing the nano antibacterial sea-island fiber: the nano antibacterial sea-island protofilament in the step S3 is oiled, stretched, curled, dried and cut to obtain the nano antibacterial sea-island fiber;
s5, preparing the nano antibacterial sea-island fiber yarn: spinning the nano antibacterial sea-island fiber obtained in the step S5 to obtain a nano antibacterial sea-island fiber yarn;
s6, preparing raw cloth: and (4) weaving the nano antibacterial sea-island fiber yarn in the step S5 to obtain the original cloth.
4. The method for manufacturing the nano antibacterial sea-island fiber fabric according to claim 3, further comprising the following steps:
s7, after finishing: taking a sodium hydroxide solution with the concentration of 9-11 g/L as a finishing liquid, soaking the original cloth in the step S6 into the finishing liquid at 40-50 ℃, heating to 85-90 ℃, keeping the temperature for 15-20 min, heating to 105-115 ℃, and keeping the temperature for 30-45 min; then, cleaning with hot water at the temperature of 75-80 ℃ for 15-20 min, and adding glacial acetic acid for neutralization to enable the pH value of the cleaning solution to reach 6-7; and then drying the mixture at 105-110 ℃ to constant weight.
5. The method for manufacturing a nano antibacterial sea-island fiber fabric according to claim 3 or 4, wherein the method comprises the following steps: in step S1, when adding zinc acetate to ethylene glycol, adding cobalt acetate at the same time, performing ultrasonic processing to obtain a zinc acetate/cobalt acetate mixed solution, adding the zinc acetate/cobalt acetate mixed solution to the graphite oxide dispersion, and stirring uniformly.
6. The method for manufacturing the nano antibacterial sea-island fiber fabric according to claim 5, is characterized in that: in step S1, the molar ratio of zinc to cobalt is 1: 0.005-0.009;
and/or the mass ratio of the graphite oxide to the zinc acetate is 2.5-3.5: 1000.
7. The method for manufacturing the nano antibacterial sea-island fiber fabric according to claim 6, is characterized in that: in step S2, the mass of the zinc oxide @ graphene nanocomposite is 5-7% of the mass of the island component.
8. The method for manufacturing the nano antibacterial sea-island fiber fabric according to claim 3, wherein the method comprises the following steps: in step S1, the mass ratio of the graphite oxide to the hydrazine hydrate is 10: 7-10.
9. The method for manufacturing a nano antibacterial sea-island fiber fabric according to claim 3, 6 or 7, wherein: in step S2, the power of the ultrasonic wave is 150-170W, the power of the microwave is 120-200W, and the duration of the microwave is 25-30S.
10. The method for manufacturing the nano antibacterial sea-island fiber fabric according to claim 3, wherein the method comprises the following steps: in step S1, when graphite oxide is subjected to ultrasonic treatment in ethylene glycol, the ultrasonic power is 350-400W, and the ultrasonic treatment time is 1.5-2 h;
and/or in step S1, when the zinc acetate is subjected to ultrasonic treatment in the ethylene glycol, the ultrasonic power is 300-360W, and the ultrasonic treatment time is 10-30 min.
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