CN109126881B - Photocatalyst-loaded micro-nano composite fiber material and preparation method thereof - Google Patents
Photocatalyst-loaded micro-nano composite fiber material and preparation method thereof Download PDFInfo
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- CN109126881B CN109126881B CN201810998005.6A CN201810998005A CN109126881B CN 109126881 B CN109126881 B CN 109126881B CN 201810998005 A CN201810998005 A CN 201810998005A CN 109126881 B CN109126881 B CN 109126881B
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 58
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 55
- 239000002657 fibrous material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000835 fiber Substances 0.000 claims abstract description 66
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 61
- 229920000767 polyaniline Polymers 0.000 claims abstract description 29
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 24
- 239000002121 nanofiber Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000002166 wet spinning Methods 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 8
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000002243 precursor Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 40
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 38
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 238000009987 spinning Methods 0.000 claims description 20
- 239000011259 mixed solution Substances 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229910001868 water Inorganic materials 0.000 claims description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 10
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000011282 treatment Methods 0.000 claims description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000004642 Polyimide Substances 0.000 claims description 7
- 229920001721 polyimide Polymers 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910000161 silver phosphate Inorganic materials 0.000 claims description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 5
- 239000004065 semiconductor Substances 0.000 claims description 5
- 239000004020 conductor Substances 0.000 claims description 3
- 230000000379 polymerizing effect Effects 0.000 claims description 3
- 238000004381 surface treatment Methods 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 2
- 230000001112 coagulating effect Effects 0.000 claims description 2
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 2
- 239000011162 core material Substances 0.000 claims description 2
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229920001197 polyacetylene Polymers 0.000 claims description 2
- 229920000128 polypyrrole Polymers 0.000 claims description 2
- 229920000123 polythiophene Polymers 0.000 claims description 2
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 claims description 2
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 2
- 239000011550 stock solution Substances 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 7
- 239000003344 environmental pollutant Substances 0.000 abstract description 5
- 231100000719 pollutant Toxicity 0.000 abstract description 5
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 238000006116 polymerization reaction Methods 0.000 abstract description 3
- 230000000593 degrading effect Effects 0.000 abstract 1
- 230000004298 light response Effects 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 description 14
- 239000010410 layer Substances 0.000 description 12
- 229920001410 Microfiber Polymers 0.000 description 7
- 239000003658 microfiber Substances 0.000 description 7
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 7
- 229940043267 rhodamine b Drugs 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 238000001000 micrograph Methods 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 4
- 229920001940 conductive polymer Polymers 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- VLDPXPPHXDGHEW-UHFFFAOYSA-N 1-chloro-2-dichlorophosphoryloxybenzene Chemical compound ClC1=CC=CC=C1OP(Cl)(Cl)=O VLDPXPPHXDGHEW-UHFFFAOYSA-N 0.000 description 1
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 1
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000013305 flexible fiber Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011490 mineral wool Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000008262 pumice Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
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- B01J35/39—
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- B01J35/58—
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- B01J35/61—
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- 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
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/14—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated alcohols, e.g. polyvinyl alcohol, or of their acetals or ketals
-
- 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
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/18—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
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- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
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- 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
- D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/22—Halides of elements of Groups 5 or 15 of the Periodic System
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/61—Polyamines polyimines
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- 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
- D06M2101/24—Polymers or copolymers of alkenylalcohols or esters thereof; Polymers or copolymers of alkenylethers, acetals or ketones
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- D—TEXTILES; PAPER
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- 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
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- D—TEXTILES; PAPER
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- 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
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention discloses a photocatalyst-loaded micro-nano composite fiber material and a preparation method thereof. Preparing polyacrylonitrile micron fibers by adopting a wet spinning process, growing a layer of conductive high molecular polymer polyaniline on the surfaces of the polyacrylonitrile micron fibers through in-situ polymerization, and covering a layer of polyacrylonitrile nano fibers containing photocatalyst precursors on the surfaces of the polyacrylonitrile micron fibers through an electrostatic spinning process to form the micro-nano composite fiber material with visible light response photocatalysis capability. The photocatalyst-loaded micro-nano composite fiber material provided by the invention has the advantages of large specific surface area, strong adsorbability to pollutants, capability of degrading pollutants under visible light and the like. Meanwhile, the photocatalyst composite fiber provided by the invention solves the problems that the powder photocatalyst is difficult to recover, the strength of the flexible photocatalyst carrier is poor, the flexible photocatalyst carrier cannot be woven and the like, and widens the application field of materials.
Description
Technical Field
The invention relates to a functional composite material, in particular to a photocatalyst-loaded micro-nano composite fiber material and a preparation method thereof, and belongs to the technical field of composite material photocatalysis.
Background
With the development of the economic change and the continuous increase of the population, the problems of global environmental pollution and the increase of the demand of energy supply are highlighted. According to statistics, about 300-400 million tons of pollutants including sewage containing heavy metals exceeding the standard, toxic solvents and other wastes are discharged to global water areas every year by factories, so that serious environmental pollution is caused, and sustainable development becomes a road which must be selected by modern society. On one hand, solar energy is used as a renewable energy source, has the characteristics of rich resources, cleanness and low price, can be used freely without transportation, has no pollution to the environment, and is the basis for realizing the sustainable development of the human society. On the other hand, a novel and green photocatalysis technology relates to the fields of semiconductor physics, catalytic chemistry, nanotechnology and the like, and has application prospects in the aspects of important problems facing human beings such as energy, environment, health and the like. The emerging technology can directly use sunlight as a light source to sensitize a catalyst and drive an oxidation-reduction reaction, thereby achieving the purposes of sewage treatment, air purification and cleaning sterilization.
The powdery photocatalyst has the problems of difficult recovery, easy secondary pollution and the like, and in order to overcome the defects, the method for loading the semiconductor photocatalyst on a recyclable carrier is a new method. Commonly used photocatalyst carriers are alumina, silica gel, pumice and diatomaceous earth, but these carriers are rigid materials and cannot adapt to the application environment requiring shape change. Therefore, the fiber carrier with flexibility attracts attention, such as glass fiber disclosed in the Chinese patent application CN1943849A, cellulose fiber disclosed in the patent application CN105536878A, and slag wool fiber disclosed in the patent application CN 105251540A. The carrier has the defects of small specific surface area, poor pollutant adsorption capacity and the like.
Disclosure of Invention
Aiming at the defects of the existing photocatalyst flexible fiber carrier, the invention provides a photocatalyst-loaded micro-nano composite fiber material with large specific surface area and strong pollutant adsorption performance and a preparation method thereof.
In order to achieve the aim, the invention adopts the technical scheme that a preparation method of a photocatalyst-loaded micro-nano composite fiber material is provided, and comprises the following steps:
(1) preparing 10-20% spinning stock solution by mass, spinning by adopting a wet spinning process after defoaming treatment, and preparing micrometer fibers with the diameters of 50-100 micrometers through thermal stretching treatment;
(2) in-situ polymerizing the conductive high molecular polymer on the surface of the micron fiber to obtain a conductive fiber;
(3) adding a photocatalyst or a photocatalyst precursor into an electrostatic spinning solution to prepare an electrostatic spinning solution, using the conductive fiber prepared in the step (2) as a receiver, and covering a layer of photocatalyst-loaded nanofiber with the thickness of 5-10 microns on the surface of the conductive fiber by adopting an electrostatic spinning process under the conditions that the flow rate is 0.5-1.2 mL/h, the voltage is 8-15 kv, and the receiving distance is 10-25 cm to obtain the photocatalyst-loaded micro-nano composite fiber material.
One preferred embodiment of the present invention is: the wet spinning solution comprises polyacrylonitrile/N, N-dimethylformamide solution, polyimide/dimethyl sulfoxide solution and polyvinyl alcohol/water solution; the coagulating bath adopted by the wet spinning process is one of a mixed solution of N, N-dimethylformamide and water, a mixed solution of methanol and water and methanol.
The conductive high molecular polymer comprises polyaniline, polypyrrole, polythiophene and polyacetylene; the preparation process of the conductive fiber in the step (2) comprises the following steps: mixing ammonium persulfate and aniline according to a molar ratio of (2-6): 4, adding polyvinylpyrrolidone with the mass concentration of 2-5% and hydrochloric acid with the concentration of 0.5-2 mol/L to prepare a reaction solution, placing the micron fibers in the reaction solution, and reacting for 1-3 hours at the temperature of 0-10 ℃.
The electrostatic spinning solution comprises one of polyacrylonitrile/N, N-dimethylformamide solution, polyvinyl alcohol/water solution and polyvinylpyrrolidone/N, N-dimethylformamide solution.
The photocatalyst comprises BiOI and Cu2O、BiOBr、Bi2WO6、TiO2、g-C3N4、Ag3PO4、AgCl、AgBr、AgI。
The technical scheme of the invention is further optimized as follows: and (4) carrying out surface treatment on the micro-nano composite fiber material loaded with the photocatalyst obtained in the step (3) to obtain a composite fiber material with a nano-scale heterogeneous semiconductor material or a conductive material as a shell layer.
According to the photocatalyst-loaded micro-nano composite fiber material prepared by the invention, the proportion of the photocatalyst in the micro-nano composite fiber is 1.0-5.0% by mass.
The technical scheme of the invention also comprises a photocatalyst-loaded micro-nano composite fiber material, which takes micron fibers with the diameter of 50-100 mu m as core materials, and a conductive high polymer is polymerized on the surfaces of the micron fibers, and a layer of photocatalyst-loaded nano fibers with the thickness of 5-10 mu m is covered on the surfaces of the micron fibers.
Compared with the prior art, the invention has the following advantages:
1. according to the photocatalyst-loaded micro-nano composite fiber material provided by the invention, the strength is provided by taking the micro-fibers prepared by wet spinning as a core layer, and the nano-fibers prepared by electrostatic spinning as a skin layer are taken as a photocatalyst carrier; the conductive polymer is polymerized on the surface of the micron fiber and is used as a receiver of electrostatic spinning, the micron-nano fiber is perfectly combined, and the polymer is easy to recover after the photocatalytic reaction is finished, so that secondary pollution is avoided. The micro-nano composite fiber material can be continuously produced, and is a novel material with photocatalytic performance.
2. The micro-nano composite fiber material loaded with the photocatalyst not only provides a carrier for the photocatalyst, but also develops a composite photocatalyst, namely, the photocatalyst is combined on the surface of the nano fiber loaded with the photocatalyst or a substance beneficial to improving the photocatalytic activity.
3. The micro-nano composite fiber provided by the invention has good flexibility, can be simply woven to be made into fiber cloth, and expands the application range.
Drawings
FIG. 1 is a comparison graph of X-ray diffraction curves of polyacrylonitrile micro-fibers, polyacrylonitrile/polyaniline conductive fibers and polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide micro-nano composite fibers provided by the embodiment of the invention;
fig. 2 is a scanning electron microscope image of polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide micro-nano composite fiber provided by an embodiment of the present invention, in which, (a) is a scanning electron microscope image of a cross section of the micro-nano composite fiber, and (b) is a scanning electron microscope image of a certain local surface of the micro-nano composite fiber;
FIG. 3 is a comparison graph of ultraviolet absorption spectra of a rhodamine B aqueous solution carrying a polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide micro-nano composite fiber material provided by the embodiment of the invention at different times under visible light irradiation.
Detailed Description
The technical scheme of the invention is further explained by combining the drawings and the embodiment.
Example 1
The embodiment provides a preparation method of a photocatalyst-loaded micro-nano composite fiber material, which comprises the following steps:
preparing polyacrylonitrile micron fibers: 10 g of polyacrylonitrile, 40 mL of dimethyl sulfoxide and 0.8 mL of water were poured into a three-necked flask, and stirred at room temperature to sufficiently swell. Then heating and stirring the mixture for 3 hours at 40 ℃ to fully dissolve the polyacrylonitrile, and placing the mixture into a vacuum drying oven at 60 ℃ for vacuum-pumping and defoaming treatment. Taking the spinning solution, preparing polyacrylonitrile micron fiber by a wet spinning device,the spinning process comprises the following steps: spinning temperature: 40 ℃; pressure: 0.2 MPa; spinning hole inner diameter: 0.5 mm; coagulation bath: mixed solution of N, N-dimethylformamide and water (Vol)DMF: VolH2O= 3: 1). Finally, the hot stretching treatment is carried out at 150 ℃.
In-situ polymerization of conductive polymer polyaniline on the surface of polyacrylonitrile micron fiber: putting polyacrylonitrile micron fiber with a certain length into a mixed solution of aniline (1.86 g), polyvinylpyrrolidone (2.08 g) and 40 mL of hydrochloric acid, adding a mixed solution of ammonium persulfate (2.28 g) and 20 mL of hydrochloric acid after 30 min, and reacting for 3h at 0 ℃.
Preparing an electrostatic spinning solution: 0.5g of polyacrylonitrile was dissolved in 6 mL of N, N-dimethylformamide solution. And (3) taking polyacrylonitrile micron fibers with surfaces covered with a layer of polyaniline as receivers on an electrostatic spinning receiving device, carrying out electrostatic spinning under the spinning conditions of the flow rate of 0.06 mL/h, the voltage of 15 kv and the distance of 15 cm, and obtaining the polyacrylonitrile/polyaniline/polyacrylonitrile micro-nano composite fibers on the receiving device.
And taking down the polyacrylonitrile/polyaniline/polyacrylonitrile micro-nano composite fiber prepared on the electrostatic spinning receiving device, soaking the polyacrylonitrile/polyaniline/polyacrylonitrile micro-nano composite fiber in 0.5 mM bismuth nitrate solution for 30 min, and then dropwise adding 0.5 mM potassium iodide solution into the solution. Then transferring the mixed solution into a Teflon reaction kettle for hydrothermal reaction, wherein the reaction conditions are as follows: and obtaining the polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide micro-nano composite fiber at the temperature of 100 ℃ for 10 hours.
Soaking polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide micro-nano composite fibers prepared by electrostatic spinning in 0.5 mM bismuth nitrate solution for 30 min, and then dropwise adding 0.25 mM ammonium tungstate aqueous solution into the solution. Then transferring the mixed solution into a Teflon reaction kettle for hydrothermal reaction, wherein the reaction conditions are as follows: and (4) obtaining the micro-nano composite fiber material loaded with the photocatalyst at 150 ℃ for 18 h.
Referring to the attached figure 1, a graph comparing X-ray diffraction curves of polyacrylonitrile micro-fibers, polyacrylonitrile/polyaniline micro-fibers and polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide micro-nano composite fibers prepared in the embodiment is shown; as can be seen from fig. 1: the broad peak appearing at 2 θ =16 ° is a characteristic peak of polyacrylonitrile; as polyaniline is in an amorphous state, a characteristic peak of the polyaniline is not detected; the test result of the polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide sample comprises a characteristic peak of polyacrylonitrile and a characteristic peak matched with a standard PDF card (PDF #73-2062) of bismuth oxyiodide, which indicates that the polyacrylonitrile fiber is loaded with bismuth oxyiodide crystals.
Fig. 2 is a scanning electron microscope image of polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide micro-nano composite fiber provided in this embodiment, in which (a) is a scanning electron microscope image of a cross section of the micro-nano composite fiber, and (b) is a scanning electron microscope image of a local surface of the micro-nano composite fiber; according to the graph (a), a nanofiber layer covers the surface of the micron fiber, and the polyacrylonitrile micro-nano composite fiber is successfully prepared; the loading condition of the polyacrylonitrile nanofiber surface can be seen from the graph (b): the flaky bismuth oxyiodide crystal grows along the nano-fiber, and has the advantages of large specific surface area, uniform distribution and no agglomeration.
FIG. 3 is a comparison graph of ultraviolet-visible light absorption spectra of a pure rhodamine B aqueous solution and the rhodamine B aqueous solution loaded with the polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide micro-nano composite fiber material provided by the embodiment of the invention after visible light irradiation. Therefore, the concentration of rhodamine B is obviously reduced after an adsorption equilibrium experiment (illumination for 0 hour), which shows that the polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide micro-nano composite fiber has excellent adsorption capacity, and the large specific surface area is benefited; compared with a pure rhodamine B aqueous solution, the rhodamine B aqueous solution loaded with the polyacrylonitrile/polyaniline/polyacrylonitrile/bismuth oxyiodide micro-nano composite fiber gradually weakens the absorption peak intensity after being irradiated by visible light at different time, and the blue shift (the dye molecular structure is destroyed) occurs at the peak position, which indicates that the dye rhodamine B is continuously photodegraded.
Example 2
Preparing polyimide micron fibers: 3.204 g of 4, 4' -diaminodiphenyl ether and 0.433 g of p-phenylenediamine were poured into a three-necked flask, and the flask was placed in an ice-water bath (0 ℃ C.) and purged with nitrogen for 2 hours. 4.450 g of pyromellitic dianhydride were then added to the three-necked flask at three equal intervals of half an hour. To react for 2 hoursAfter that time, 1.021 g of acetic anhydride and 0.791 g of pyridine were slowly added dropwise. After reacting for 2 hours, the mixed solution is subjected to vacuum-pumping defoaming treatment in a vacuum drying oven at 60 ℃ to be used as spinning solution. Preparing the polyimide fiber from the spinning solution by a self-made wet spinning device, wherein the spinning process comprises the following steps: spinning temperature: 50 ℃; pressure: 0.2 MPa; spinning hole inner diameter: 0.5 mm; coagulation bath: mixed solution of methanol and water (Vol)methanol:VolH2O=7: 3). Finally, the hot stretching treatment is carried out at 300 ℃.
In-situ polymerization of conductive polymer polyaniline on the surface of the polyimide micron fiber: putting polyimide micron fibers with a certain length into a mixed solution of aniline (1.86 g), polyvinylpyrrolidone (2.08 g) and 40 mL of hydrochloric acid, adding a mixed solution of ammonium persulfate (2.28 g) and 20 mL of hydrochloric acid after 30 min, and reacting for 3h at 0 ℃.
Preparing an electrostatic spinning solution: 0.5g of polyacrylonitrile and 0.5g of silver nitrate were dissolved in 6 mL of N, N-dimethylformamide solution. The polyimide microfiber with a polyaniline layer covered on the surface is used as a receiver on an electrostatic spinning receiving device, and electrostatic spinning is carried out under the spinning conditions of the flow rate of 0.06 mL/h, the voltage of 15 kv and the distance of 15 cm.
Drying the micro-nano composite fiber subjected to electrostatic spinning in a blast oven (in dark place) at 40 ℃ for 1h, wherein Ag is generated in the process of solvent volatilization+The surface of polyacrylonitrile nano-fiber is taken, and then the polyacrylonitrile nano-fiber is soaked in a mixed solution of disodium hydrogen phosphate (2.8 g), polyvinylpyrrolidone (1.1 g) and 100 mL of deionized water for 30 min, and Ag is generated on the surface of the polyacrylonitrile nano-fiber through ion exchange reaction3PO4And (3) granules.
Ag3PO4Is a photocatalyst having excellent properties, but has photo-corrosiveness, so Ag is supported on the photocatalyst3PO4The surface of the micro-nano composite fiber is coated with a layer of polyaniline, so that on one hand, Ag can be coated3PO4The protection is prevented from photo-corrosion, and on the other hand, the coated polyaniline can improve the migration of photo-generated electrons, thereby improving the photocatalytic performance.
Load to be obtained in this exampleThe micro-nano composite fiber material of the photocatalyst is subjected to surface treatment to form (e) capable of promoting photogeneration of electron-hole pairs--h+) The nano-scale shell layer, such as the shell layer, containing nano-scale heterogeneous semiconductor materials or conductive materials, thereby improving the photocatalytic activity of the fiber material. The specific method comprises the following steps:
example 3
Preparing polyvinyl alcohol micron fibers: pouring 10 g of PVA, 39 mL of dimethyl sulfoxide and 13 mL of water into a three-neck flask, continuously stirring for 4 h at 90 ℃ until the PVA is completely dissolved to obtain a uniform and transparent PVA solution, and then standing for 2 h for defoaming. Preparing the polyvinyl alcohol fiber from the spinning solution by a self-made wet spinning device, wherein the spinning process comprises the following steps: spinning temperature: 50 ℃; pressure: 0.2 MPa; spinning hole inner diameter: 0.5 mm; coagulation bath: methanol. Finally, the hot stretching treatment at 200 ℃ is carried out.
In-situ polymerizing conductive polymer polyaniline on the surface of polyvinyl alcohol micron fiber: polyvinyl alcohol microfiber with a certain length is put into a mixed solution of aniline (1.86 g), polyvinylpyrrolidone (2.08 g) and 40 mL hydrochloric acid, a mixed solution of ammonium persulfate (2.28 g) and 20 mL hydrochloric acid is added after 30 minutes, and the reaction is carried out at 0 ℃ for 3 hours.
Preparing an electrostatic spinning solution: 0.5g of polyacrylonitrile and 0.5g of silver nitrate were dissolved in 6 mL of N, N-dimethylformamide solution. The polyvinyl alcohol microfiber with the surface covered with a layer of polyaniline is used as a receiving device for electrostatic spinning, and electrostatic spinning is carried out under the spinning conditions of the flow rate of 0.06 mL/h, the voltage of 15 kv and the distance of 15 cm.
Drying the micro-nano composite fiber subjected to electrostatic spinning in a blast oven (in dark place) at 40 ℃ for 1h, wherein Ag is generated in the process of solvent volatilization+The surface of polyacrylonitrile nano-fiber is taken, and then the polyacrylonitrile nano-fiber is soaked in a mixed solution of disodium hydrogen phosphate (2.8 g), polyvinylpyrrolidone (1.1 g) and 100 mL of deionized water for 30 min, and Ag is generated on the surface of the polyacrylonitrile nano-fiber through ion exchange reaction3PO4And (3) granules.
Ag3PO4Is an excellent photocatalyst, but has photo-corrosiveness, so the photocatalyst is used in the field of photocatalystLoaded with Ag3PO4The surface of the micro-nano composite fiber is coated with a layer of titanium dioxide sol to form a protective layer to inhibit Ag3PO4The photo-corrosiveness of the fiber material is improved at the same time.
Claims (10)
1. A preparation method of a photocatalyst-loaded micro-nano composite fiber material is characterized by comprising the following steps:
(1) preparing 10-20% spinning stock solution by mass, spinning by adopting a wet spinning process after defoaming treatment, and preparing micrometer fibers with the diameters of 50-100 micrometers through thermal stretching treatment;
(2) in-situ polymerizing the conductive high molecular polymer on the surface of the micron fiber to obtain a conductive fiber;
(3) adding a photocatalyst or a photocatalyst precursor into an electrostatic spinning solution to prepare an electrostatic spinning solution, using the conductive fiber prepared in the step (2) as a receiver, and covering a layer of photocatalyst-loaded nanofiber with the thickness of 5-10 microns on the surface of the conductive fiber by adopting an electrostatic spinning process under the conditions that the flow rate is 0.5-1.2 mL/h, the voltage is 8-15 kv, and the receiving distance is 10-25 cm to obtain the photocatalyst-loaded micro-nano composite fiber material.
2. The preparation method of the photocatalyst-loaded micro-nano composite fiber material according to claim 1, characterized by comprising the following steps: the wet spinning solution comprises polyacrylonitrile/N, N-dimethylformamide solution, polyimide/dimethyl sulfoxide solution and polyvinyl alcohol/water solution.
3. The preparation method of the photocatalyst-loaded micro-nano composite fiber material according to claim 1, characterized by comprising the following steps: the coagulating bath adopted by the wet spinning process is one of a mixed solution of N, N-dimethylformamide and water, a mixed solution of methanol and water and methanol.
4. The preparation method of the photocatalyst-loaded micro-nano composite fiber material according to claim 1, characterized by comprising the following steps: the conductive high molecular polymer comprises polyaniline, polypyrrole, polythiophene and polyacetylene.
5. The preparation method of the photocatalyst-loaded micro-nano composite fiber material according to claim 1, characterized by comprising the following steps: the preparation process of the conductive fiber in the step (2) comprises the following steps: mixing ammonium persulfate and aniline according to a molar ratio of (2-6): 4, adding polyvinylpyrrolidone with the mass concentration of 2-5% and hydrochloric acid with the concentration of 0.5-2 mol/L to prepare a reaction solution, placing the micron fibers in the reaction solution, and reacting for 1-3 hours at the temperature of 0-10 ℃.
6. The preparation method of the photocatalyst-loaded micro-nano composite fiber material according to claim 1, characterized by comprising the following steps: the electrostatic spinning solution comprises one of polyacrylonitrile/N, N-dimethylformamide solution, polyvinyl alcohol/water solution and polyvinylpyrrolidone/N, N-dimethylformamide solution.
7. The preparation method of the photocatalyst-loaded micro-nano composite fiber material according to claim 1, characterized by comprising the following steps: the photocatalyst comprises BiOI and Cu2O、BiOBr、Bi2WO6、TiO2、g-C3N4、Ag3PO4、AgCl、AgBr、AgI。
8. The preparation method of the photocatalyst-loaded micro-nano composite fiber material according to claim 1, characterized by comprising the following steps: and (4) carrying out surface treatment on the micro-nano composite fiber material loaded with the photocatalyst obtained in the step (3) to obtain a composite fiber material with a nano-scale heterogeneous semiconductor material or a conductive material as a shell layer.
9. The preparation method of the photocatalyst-loaded micro-nano composite fiber material according to claim 1 or 8, characterized by comprising the following steps: the proportion of the photocatalyst in the micro-nano composite fiber is 1.0-5.0% by mass.
10. A photocatalyst-loaded micro-nano composite fiber material is characterized in that: the preparation method takes micron fibers with the diameter of 50-100 microns as core materials, conductive high polymer is polymerized on the surfaces of the micron fibers, and a layer of nano fibers which are 5-10 microns thick and are loaded with a photocatalyst is covered on the surfaces of the micron fibers.
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