CN106552674A - Aerogel carried nickel-phosphorus alloy catalysis material of a kind of nanofiber and preparation method thereof - Google Patents
Aerogel carried nickel-phosphorus alloy catalysis material of a kind of nanofiber and preparation method thereof Download PDFInfo
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- CN106552674A CN106552674A CN201610861020.7A CN201610861020A CN106552674A CN 106552674 A CN106552674 A CN 106552674A CN 201610861020 A CN201610861020 A CN 201610861020A CN 106552674 A CN106552674 A CN 106552674A
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- nanofiber
- nickel
- solution
- phosphorus alloy
- catalysis material
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- 239000002121 nanofiber Substances 0.000 title claims abstract description 154
- 239000000463 material Substances 0.000 title claims abstract description 64
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 51
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 239000004964 aerogel Substances 0.000 title claims abstract description 46
- 229910001096 P alloy Inorganic materials 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000835 fiber Substances 0.000 claims abstract description 47
- 239000011230 binding agent Substances 0.000 claims abstract description 29
- 239000000725 suspension Substances 0.000 claims abstract description 29
- 229920001169 thermoplastic Polymers 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 claims abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 108
- 239000000243 solution Substances 0.000 claims description 86
- 229910052759 nickel Inorganic materials 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 38
- 239000002131 composite material Substances 0.000 claims description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims description 20
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 17
- 239000004952 Polyamide Substances 0.000 claims description 17
- 238000010521 absorption reaction Methods 0.000 claims description 17
- 239000012528 membrane Substances 0.000 claims description 17
- 229920002647 polyamide Polymers 0.000 claims description 17
- 230000003213 activating effect Effects 0.000 claims description 16
- 230000001235 sensitizing effect Effects 0.000 claims description 16
- 229920001661 Chitosan Polymers 0.000 claims description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 14
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 14
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 12
- 230000004913 activation Effects 0.000 claims description 12
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 10
- 229960003638 dopamine Drugs 0.000 claims description 10
- PIBWKRNGBLPSSY-UHFFFAOYSA-L palladium(II) chloride Chemical compound Cl[Pd]Cl PIBWKRNGBLPSSY-UHFFFAOYSA-L 0.000 claims description 10
- 206010070834 Sensitisation Diseases 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- -1 polypropylene Polymers 0.000 claims description 9
- 230000008313 sensitization Effects 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 239000003643 water by type Substances 0.000 claims description 7
- 241000209094 Oryza Species 0.000 claims description 6
- 235000007164 Oryza sativa Nutrition 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 239000004310 lactic acid Substances 0.000 claims description 6
- 235000014655 lactic acid Nutrition 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002074 melt spinning Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910001453 nickel ion Inorganic materials 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- JYVLIDXNZAXMDK-UHFFFAOYSA-N pentan-2-ol Chemical compound CCCC(C)O JYVLIDXNZAXMDK-UHFFFAOYSA-N 0.000 claims description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 6
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 6
- 235000009566 rice Nutrition 0.000 claims description 6
- 239000001632 sodium acetate Substances 0.000 claims description 6
- 235000017281 sodium acetate Nutrition 0.000 claims description 6
- 235000011150 stannous chloride Nutrition 0.000 claims description 6
- CTENFNNZBMHDDG-UHFFFAOYSA-N Dopamine hydrochloride Chemical compound Cl.NCCC1=CC=C(O)C(O)=C1 CTENFNNZBMHDDG-UHFFFAOYSA-N 0.000 claims description 5
- 229960001149 dopamine hydrochloride Drugs 0.000 claims description 5
- 239000000284 extract Substances 0.000 claims description 5
- 239000001509 sodium citrate Substances 0.000 claims description 5
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 5
- 238000009987 spinning Methods 0.000 claims description 5
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 4
- 239000007853 buffer solution Substances 0.000 claims description 4
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 239000002070 nanowire Substances 0.000 claims description 3
- 229910052698 phosphorus Inorganic materials 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- GPRLSGONYQIRFK-MNYXATJNSA-N triton Chemical compound [3H+] GPRLSGONYQIRFK-MNYXATJNSA-N 0.000 claims description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 claims description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 2
- 239000004743 Polypropylene Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000004945 emulsification Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- 239000008187 granular material Substances 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229920001690 polydopamine Polymers 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 2
- QKNYBSVHEMOAJP-UHFFFAOYSA-N 2-amino-2-(hydroxymethyl)propane-1,3-diol;hydron;chloride Chemical compound Cl.OCC(N)(CO)CO QKNYBSVHEMOAJP-UHFFFAOYSA-N 0.000 claims 1
- KGZLFTWMCMEEJR-UHFFFAOYSA-N heptane;hydrochloride Chemical compound Cl.CCCCCCC KGZLFTWMCMEEJR-UHFFFAOYSA-N 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- 229920002215 polytrimethylene terephthalate Polymers 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 230000003197 catalytic effect Effects 0.000 abstract description 11
- 238000000151 deposition Methods 0.000 abstract description 4
- 230000008021 deposition Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 238000005234 chemical deposition Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 13
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 8
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 8
- 239000001119 stannous chloride Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- UGZICOVULPINFH-UHFFFAOYSA-N acetic acid;butanoic acid Chemical compound CC(O)=O.CCCC(O)=O UGZICOVULPINFH-UHFFFAOYSA-N 0.000 description 5
- 238000000605 extraction Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- MSXVEPNJUHWQHW-UHFFFAOYSA-N 2-methylbutan-2-ol Chemical compound CCC(C)(C)O MSXVEPNJUHWQHW-UHFFFAOYSA-N 0.000 description 4
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 description 4
- 229910002666 PdCl2 Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- NQXGLOVMOABDLI-UHFFFAOYSA-N sodium oxido(oxo)phosphanium Chemical compound [Na+].[O-][PH+]=O NQXGLOVMOABDLI-UHFFFAOYSA-N 0.000 description 4
- 239000004416 thermosoftening plastic Substances 0.000 description 4
- 229910000990 Ni alloy Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 229920001038 ethylene copolymer Polymers 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229920001707 polybutylene terephthalate Polymers 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- WGYFACNYUJGZQO-UHFFFAOYSA-N aminomethanetriol Chemical compound NC(O)(O)O WGYFACNYUJGZQO-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 229920001727 cellulose butyrate Polymers 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009432 framing Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000013462 industrial intermediate Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- NQMRYBIKMRVZLB-UHFFFAOYSA-N methylamine hydrochloride Chemical compound [Cl-].[NH3+]C NQMRYBIKMRVZLB-UHFFFAOYSA-N 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 125000000636 p-nitrophenyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)[N+]([O-])=O 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B01J35/23—
-
- 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
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/063—Polymers comprising a characteristic microstructure
-
- 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
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- B01J35/396—
Abstract
The invention discloses aerogel carried nickel-phosphorus alloy catalysis material of a kind of nanofiber and preparation method thereof, belongs to nano-functional material field.The catalysis material that the present invention is provided is made up of the nickel-phosphorus alloy nano-particle that Nanofiber Network skeleton and bag are attached to Nanofiber Network skeleton surface, and Nanofiber Network skeleton is made up of with the binding agent for being attached to nanofiber surface nanofiber.The preparation method of the present invention includes, it is separated initially with melt blending, disperses suspension modified and cryodesiccated method to prepare thermoplastic polymer nanofiber's fiber aeroge, then with thermoplastic polymer nanofiber's fiber aeroge as carrier, by the method for chemical deposition by nickel phosphorus nanoparticle deposition in the fiber surface of constitutionally stable aerogel material, the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber is prepared.The preparation method process of the present invention is simple, it is easy to accomplish large-scale production, and the catalysis material for preparing has high specific surface area, porosity and preferable catalytic effect.
Description
Technical field
The invention belongs to nano-functional material field, specifically belongs to a kind of aerogel carried nickel-phosphorus alloy of nanofiber and urges
Change material and preparation method thereof.
Background technology
Trade effluent becomes the important factor of restriction socio-economic development at this stage.Pollutant nitrobenzene compounds
Be a class be important industrial chemicals or intermediate while and be one of main organic pollution in environment, but p-nitrophenyl
The Reduction Body p-aminophenol of phenol is a kind of common pharmacy, the intermediate of chemical industry, realizes turning waste into wealth, and meaning is notable.Nickel alloy
It is a kind of cheap and widely used catalyst, it is obvious to the catalytic effect of the pollutant of paranitrophenol etc.Catalyst
Including unsupported catalyst, another kind of is loaded catalyst, carrier mainly natural ore species used, adsorbent class,
Ceramic-like and organic etc..Nanofiber is a kind of superfine fibre, with specific surface area is big, draw ratio big, is had after film forming
Little aperture and big porosity, after being especially prepared into aeroge, the overall specific surface area and porosity of material will
It is obviously improved, as carrier, prepared loaded catalyst will show very high catalysis activity.
Chinese invention patent application (application publication number：CN105148996A, applies for publication date：2015-12-16) disclose
A kind of Membrane catalysis nickel nano fibrous membrane and preparation method thereof.The method prepares thermoplastic poly by the method for scatter coated
Compound micro/nano fibrous membrane material, then deposits nickel alloy material in membrane material surfaces externally and internally by the method for chemical plating, is prepared into
To the nickel micro/nano fibrous membrane material for pollutant catalytic decomposition.Advantage is that method is simply efficient, it is easy to volume production, catalysis material after
The high-specific surface area feature of micro/nano fibrous membrane material is held, catalytic performance is excellent, flexible easy processing is easily isolated in application process
With realization recycling.Have the disadvantage that the specific surface area and porosity of prepared thermoplastic polymer nanofiber's fibrous membrane is limited, should
The catalytic performance of loading type nickel-based catalysis material need further to be lifted.
The content of the invention
To solve above-mentioned technical problem, the invention provides a kind of aerogel carried nickel-phosphorus alloy catalysis material of nanofiber
And preparation method thereof.The present invention with thermoplastic polymer nanofiber's fiber aeroge as carrier, by the method for chemical deposition by nickel
In the fiber surface of constitutionally stable aerogel material, carrier has high specific surface area and porosity to nanoparticle deposition,
Improve the catalytic effect of catalyst.
For achieving the above object, the invention discloses a kind of aerogel carried nickel-phosphorus alloy catalysis material of nanofiber, urges
Change material to be made up of the nickel-phosphorus alloy nano-particle that Nanofiber Network skeleton and bag are attached to Nanofiber Network skeleton surface, institute
State Nanofiber Network skeleton to be made up of with the binding agent for being attached to nanofiber surface nanofiber, the nanofiber is by warm
Thermoplastic polymer is constituted.
Further, the Nanofiber Network skeleton with the mass percent of nickel-phosphorus alloy nano-particle is：50～
75%：25～50%, the nanofiber with the mass percent of binding agent is：50～80%：20～50%.
Yet further, in the nickel-phosphorus alloy nano-particle, the atom number percentage ratio of nickel and phosphorus is：50～80%：20
～50%, and the particle diameter of nickel-phosphorus alloy nano-particle is 1～50nm.
Further, described adhesive is the one kind in polyvinyl alcohol, shitosan or poly-dopamine；The thermoplastic poly
Compound is polyvinyl alcohol-ethylene copolymer, polypropylene, polyamide, polyethylene terephthalate, poly terephthalic acid the third two
One kind in alcohol ester, polybutylene terephthalate (PBT) or polyurethane.
Present invention also offers a kind of preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber, including with
Lower step：
1) prepare composite fibre：Thermoplastic polymer is uniformly mixed with acetylbutyrylcellulose, Jing double screw extruders
Extrusion, pelletize, prepare thermoplastic polymer/acetylbutyrylcellulose composite, continue thermoplastic polymer/acetate butyrate
Cellulose composite material Jing melt spinning machines carry out drawing-off, spinning, obtain composite fibre；
2) prepare nanofiber suspension：By the step 1) composite fibre for preparing is placed in acetone and flows back, extraction
Normal temperature drying is carried out after taking out acetylbutyrylcellulose, thermoplastic polymer nanofiber's fiber is prepared, then by thermoplastic poly
Compound nanofiber is scattered in mixed solution of the organic solvent with water by the concentration of 1～10g/L, is prepared finely dispersed
Nanofiber suspension；
3) prepare binder solution：During binder solution is poly-vinyl alcohol solution, chitosan solution or dopamine solution
One kind, the poly-vinyl alcohol solution are that polyvinyl alcohol is dissolved in the water to prepare；The chitosan solution is by shitosan
Powder is dispersed in water and prepares；The dopamine solution is that Dopamine Hydrochloride powder is scattered in trishydroxymethylaminomethane
The buffer solution of hydrochlorate is prepared；
4) prepare nanofiber aeroge：By the step 3) binder solution and the step 2 that prepare) receiving of preparing
Rice fibrous suspension mix homogeneously, prepares nanofiber mixing suspension, nanofiber mixing suspension is placed in container
In template, lyophilization in freezer dryer is then placed in again, nanofiber aeroge is prepared；
5) configure the bath of nickel nano fibrous membrane sensitizing solution, activating solution and nickel；
6) prepare the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber：By the step 4) the nanofiber gas for preparing
Gel immerses the step 5) in the nickel nano fibrous membrane sensitizing solution for preparing vibration absorption obtain the nanofiber aeroge being sensitized,
Continue will the nanofiber aeroge of sensitization immerse the step 5) in the activating solution for preparing, vibration absorption obtains the nanometer for activating
The nanofiber aeroge of activation is immersed oscillating reactionss in nickel bath, then deionized water and ethanol rinse by fiber aeroge,
Dry again, that is, prepare the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber.
Further, the step 5) in,
Configuration nickel nano fibrous membrane sensitizing solution：10g stannous chlorides are taken, mass concentration is 38% 30ml hydrochloric acid solutions, plus
Enter in 1L deionized waters；
Configuration activating solution：0.25g Palladous chloride .s are taken, mass concentration is 38% 20ml hydrochloric acid solutions, is added to 1L deionizations
In water；
Configuration nickel bath：In nickel bath, the molar concentration of bivalent nickel ion is 0.07～0.12mol/L, the matter of sodium hypophosphite
Amount concentration is 16～40g/L, and the mass concentration of sodium acetate is 15～20g/L, and the mass concentration of triton x-100 is 5～10mg/
The mass concentration of L or Tween 80 is 5～10mg/L, and the mass concentration of sodium citrate is 8～10g/L, and the mass concentration of lactic acid is
10～12g/L, the acid-base value of the nickel bath is pH=4.5～5.0.
Yet further, the step 6) in, by the step 4) the nanofiber aeroge for preparing immerses the step
5) in the nano fibrous membrane sensitizing solution for preparing, it is ensured that bath raio is 30：1, the taking-up after vibration 1～5min of absorption at 15～25 DEG C,
Obtain the nanofiber aeroge being sensitized, continue will the nanofiber aeroge of sensitization immerse the step 5) activating solution for preparing
In, it is ensured that bath raio is 30：1, then deionized water cleaning is being taken out after vibration 1～5min of absorption at 15～25 DEG C, is being lived
The nanofiber aeroge of change；To react in the nanofiber aeroge immersion nickel bath of activation, it is ensured that bath raio is 10：1, Ran Hou
Take out after 10～20min of oscillating reactionss under constant temperature, respectively deionized water and ethanol rinse 3 times, finally dry at 50 DEG C, i.e.,
Prepare the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber.
Further, the step 4) in, by the step 3) binder solution and the step 2 that prepare) prepare
Nanofiber suspension according to volume ratio be 2～5：10 mix homogeneously, prepare nanometer in the presence of emulsification pretreatment machine
Fiber mixing suspension, nanofiber mixing suspension is placed in container template, and in being subsequently placed in freezer dryer, freezing is dry
Dry, cryogenic temperature is 20 DEG C of 80 DEG C～﹣ of ﹣, and cooling time is 4～6h, and drying time is 24～72h, prepares nanofiber
Aeroge.
Further, the step 3) in,
The preparation process of the poly-vinyl alcohol solution is：Polyvinyl alcohol is dissolved in the water, is sufficiently stirred for, obtain quality dense
Spend the poly (vinyl alcohol) binder solution for 1.0～2.0%；
The preparation process of the chitosan solution is：It is 50% by mass percent：50% Chitosan powder and acetic acid
Mixing, is then added in 25～50 times that quality is Chitosan powder quality of water, is uniformly dispersed, prepares mass concentration
For 1.0～2.0% chitosan solution；
The preparation process of the dopamine solution is：Dopamine Hydrochloride powder is dispersed in into the trihydroxy methyl ammonia of pH=8.5
In the buffer solution of methylmethane hydrochlorate, it is sufficiently stirred for, prepares the dopamine solution that mass concentration is 0.2～2.0%.
Further, the step 1) in, the mass percent of thermoplastic polymer and acetylbutyrylcellulose is 5～
40%：60～95%；The step 2) in, a diameter of 50～350nm of thermoplastic polymer nanofiber's fiber, the organic solvent
For the one kind in the tert-butyl alcohol, tert-pentyl alcohol or sec-amyl alcohol, and the volume ratio of organic solvent and water is 1～3：1.
Beneficial effects of the present invention：
1. the thermoplastic polymer nanofiber's fiber aeroge in the present invention is separated, is disperseed suspension modified using melt blending
And cryodesiccated method, process is simple, energy-conserving and environment-protective, it is easy to accomplish large-scale production；On the other hand, resulting aeroge
Stability Analysis of Structures after thermoplastic nanofibers' fiber solvent resistant and binding agent are crosslinked in material, so that this method is compared obtained by other methods
Aerogel material has excellent physics and steady chemical structure, is more widely applied.
2. the load-type nickel phosphorus catalyst of the present invention is with thermoplastic polymer nanofiber's fiber aeroge as carrier, by chemistry
By nickel phosphorus nanoparticle deposition in the fiber surface of constitutionally stable aerogel material, carrier has high ratio to the method for deposition
Surface area and porosity, make the catalyst have very high catalytic effect, so as to not only solve the made non-loading type of traditional method
Catalyst and reactant, the separation problem of product that nickel phosphorus catalyst brings, it is to avoid that what is brought in sewage disposal is secondary
Pollute, and greatly improve the catalytic efficiency of the made load-type nickel phosphorus catalyst (film catalyst) of existing method and be difficult to be lifted
Problem.
3. the method that the nickel nano fibrous membrane of the present invention adopts whole liquid phase synthesis, it is easy to control the growth of nickel dam, changes
The consistency of the thickness, the size of coating granule and coating of nanometer nickel coating；It is easy to by changing reducing agent in nickel bath simultaneously
Phosphorus element content in concentration optimization coating, optimizes the electronic structure of nickel alloy, further lifts the catalytic of nickel nano fibrous membrane
Energy.
Specific embodiment
In order to preferably explain the present invention, the main contents of the present invention are further elucidated below in conjunction with specific embodiment, but
Present disclosure is not limited solely to following examples.
Embodiment 1
This enforcement discloses a kind of preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber, including following
Step：
1) prepare composite fibre：Will be the polyvinyl alcohol-ethylene copolymer (PVA-co-PE) of 1kg fine with the acetate butyrate of 4kg
Dimension plain (CAB) is uniformly mixed, and carries out extruding, pelletize in the double screw extruder that processing temperature is 170 DEG C, obtains PVA-
Co-PE/CAB composites；
2) prepare nanofiber suspension：PVA-co-PE/CAB composite Jing melt spinning machines are carried out into drawing-off, is spun
Silk, obtains composite fibre；Composite fibre is flowed back in 60 DEG C of acetone 72h extraction acetylbutyrylcelluloses, will extract acetic acid
Composite fibre after cellulose butyrate carries out normal temperature drying, prepares the PVA-co-PE Nanowires that average diameter is 200nm
Dimension；0.5gPVA-co-PE nanofiber dispersions are taken in the mixed solution of the tert-butyl alcohol of the water and 30ml of 20ml, is sufficiently stirred for point
Dissipate and obtain nanofiber suspension；
3) prepare binder solution：0.1g polyvinyl alcohol is taken, is stirred at 80 DEG C and is completely dissolved in the water of 10ml, prepared
Obtain the poly (vinyl alcohol) binder solution that mass concentration is 1%；
4) prepare nanofiber aeroge：By the step 3) the poly (vinyl alcohol) binder solution for preparing is added to the step
In the rapid nanofiber suspension for 2) preparing, mix homogeneously is placed in container template, freezes 6h at -30 DEG C, is dried 36h, i.e.,
PVA-co-PE nanofiber aeroges are obtained；
5) configure sensitizing solution：Take 10g stannous chloride (SnCl2), mass concentration is 38% 30ml hydrochloric acid solutions, is added to
In 1L deionized waters；
Configuration activating solution：Take 0.25g Palladous chloride. (PdCl2), mass concentration is 38% 20ml hydrochloric acid solutions, is added to 1L
In deionized water；
Configuration nickel bath：Bivalent nickel ion (Ni in the nickel bath2+) concentration be 0.07mol/L, sodium hypophosphite (NaH2PO2)
Concentration be 16g/L, sodium acetate (CH3COONa concentration) is 18g/L, and the concentration of triton x-100 is 10mg/L, citric acid
The concentration of sodium is 8g/L, and the concentration of lactic acid is 10g/L, and the acid-base value of the nickel bath is pH=4.6；
6) prepare the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber：By the step 4) PVA-co-PE for preparing
Nanofiber aeroge immerses the step 5) in the sensitizing solution that configures, it is ensured that bath raio is 30：1,3 points of the vibration absorption at 20 DEG C
Take out after clock, obtain the nanofiber aeroge being sensitized, then the nanofiber aeroge of sensitization is immersed into the step 5) configuration
Activating solution in, it is ensured that bath raio is 30：1, then deionized water cleaning is taken out after absorption being vibrated at 20 DEG C 2 minutes, is obtained
The nanofiber aeroge of activation；The nanofiber aeroge of activation is finally immersed in 50 DEG C of the step 5) nickel bath in
Reaction, it is ensured that bath raio is 10：1, then oscillating reactionss were taken out after 15 minutes at a constant temperature, respectively deionized water and ethanol rinse
3 times, finally dry at 50 DEG C, obtain the aerogel carried Ni of PVA-co-PE nanofibers2P catalysis materials.
The aerogel carried Ni of PVA-co-PE nanofibers in the present embodiment2The performance parameter of P catalysis materials is shown in Table 1.
Embodiment 2
This enforcement discloses a kind of preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber, including following
Step：
1) prepare composite fibre：The acetylbutyrylcellulose (CAB) of the polyamide (PA) and 3kg that take 2kg is uniformly mixed
Close, carry out extruding in the double screw extruder that processing temperature is 170 DEG C, pelletize, obtain PA/CAB composites；
2) prepare nanofiber suspension：PA/CAB composite Jing melt spinning machines are carried out into drawing-off, spinning is answered
Condensating fiber；Composite fibre is flowed back 72 hours in 60 DEG C of acetone and extracts acetylbutyrylcellulose, will be extraction acetate butyrate fine
Composite fibre after dimension element carries out normal temperature drying, prepares the PA nanofibers that average diameter is 200nm；Take 0.5gPA nanometers
In the mixed solution of the tert-pentyl alcohol of the water and 25ml that are scattered in 25ml of fiber, it is sufficiently stirred for dispersion and obtains nanofiber suspension
Liquid；
3) prepare binder solution：0.4g Chitosan powders are taken, stirring under 0.4g acetic acid room temperature is completely dissolved in 20ml's
In water, the shitosan binder solution that mass concentration is 2% is prepared；
4) prepare nanofiber aeroge：By the step 3) the shitosan binder solution for preparing is added to the step
2) in the nanofiber suspension for preparing, mix homogeneously is placed in container template, is freezed 4 hours at -50 DEG C, is dried 24 little
When, you can obtain PA nanofiber aeroges；
5) configure sensitizing solution：Take 10g stannous chloride (SnCl2), mass concentration is 38% 30ml hydrochloric acid solutions, is added to
In 1L deionized waters；
Configuration activating solution：Take 0.25g Palladous chloride. (PdCl2), mass concentration is 38% 20ml hydrochloric acid solutions, is added to 1L
In deionized water；
Configuration nickel bath：Bivalent nickel ion (Ni in the nickel bath2+) concentration be 0.12mol/L, sodium hypophosphite (NaH2PO2)
Concentration be 40g/L, sodium acetate (CH3COONa concentration) is 20g/L, and the concentration of Tween 80 is 8mg/L, sodium citrate it is dense
Spend for 8g/L, the concentration of lactic acid is 12g/L, the acid-base value of the nickel bath is pH=4.5；
6) prepare the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber：By the step 4) the PA nanofibers that prepare
Aeroge immerses the step 5) in the sensitizing solution that configures, it is ensured that bath raio is 30：1, take after vibrating absorption 3 minutes at 20 DEG C
Go out, obtain the nanofiber aeroge being sensitized, then the nanofiber aeroge of sensitization is immersed into the step 5) activation that configures
In liquid, it is ensured that bath raio is 30：1, then deionized water cleaning is taken out after absorption being vibrated at 20 DEG C 2 minutes, obtains what is activated
Nanofiber aeroge；The nanofiber aeroge of activation is finally immersed in 50 DEG C of the step 5) nickel bath in react,
Ensure that bath raio is 10：1, then take out after oscillating reactionss 15 minutes at a constant temperature, respectively deionized water and ethanol rinse 3 times,
It is last to dry at 50 DEG C, obtain the aerogel carried Ni of PA nanofibers3P catalysis materials.
The aerogel carried Ni of PA nanofibers in the present embodiment3The performance parameter of P catalysis materials is shown in Table 1.
Embodiment 3
This enforcement discloses a kind of preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber, including following
Step：
1) prepare composite fibre：Take the polyethylene terephthalate (PET) of 1kg and the acetylbutyrylcellulose of 5kg
(CAB) uniformly mixed, carry out extruding in the double screw extruder that processing temperature is 170 DEG C, pelletize, obtained PA/CAB multiple
Condensation material；
2) prepare nanofiber suspension：PA/CAB composite Jing melt spinning machines are carried out into drawing-off, spinning is answered
Condensating fiber；Composite fibre is flowed back 72 hours in 60 DEG C of acetone and extracts acetylbutyrylcellulose, will be extraction acetate butyrate fine
Composite fibre after dimension element carries out normal temperature drying, prepares the PET nanofibers that average diameter is 100nm；Take 0.5gPET to receive
In the mixed solution of the sec-amyl alcohol of the water and 35ml that are scattered in 15ml of rice fiber, it is sufficiently stirred for dispersion and obtains nanofiber suspension
Liquid；
3) prepare binder solution：Take the three hydroxyl first that stirring under 0.1g Dopamine Hydrochloride powder room temperature is completely dissolved in 10ml
In base aminomethane hydrochloride, the dopamine binder solution that mass concentration is 1% is prepared；
4) prepare nanofiber aeroge：By the step 3) the dopamine binder solution for preparing is added to the step
2) in the nanofiber suspension for preparing, mix homogeneously is placed in container template, is freezed 6 hours at -20 DEG C, is dried 72 little
When, you can obtain PET nanofiber aeroges；
5) configure sensitizing solution：Take 10g stannous chloride (SnCl2), mass concentration is 38% 30ml hydrochloric acid solutions, is added to
In 1L deionized waters；
Configuration activating solution：Take 0.25g Palladous chloride. (PdCl2), mass concentration is 38% 20ml hydrochloric acid solutions, is added to 1L
In deionized water；
Configuration nickel bath：Bivalent nickel ion (Ni in the nickel bath2+) concentration be 0.10mol/L, sodium hypophosphite (NaH2PO2)
Concentration be 30g/L, sodium acetate (CH3COONa concentration) is 18g/L, and the concentration of Tween 80 is 7mg/L, sodium citrate it is dense
Spend for 8g/L, the concentration of lactic acid is 11g/L, the acid-base value of the nickel bath is pH=4.7；
6) prepare the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber：By the step 4) the PA nanofibers that prepare
Aeroge immerses the step 5) in the sensitizing solution that configures, it is ensured that bath raio is 30：1, take after vibrating absorption 3 minutes at 20 DEG C
Go out, obtain the nanofiber aeroge being sensitized, then the nanofiber aeroge of sensitization is immersed into the step 5) activation that configures
In liquid, it is ensured that bath raio is 30：1, then deionized water cleaning is taken out after absorption being vibrated at 20 DEG C 2 minutes, obtains what is activated
Nanofiber aeroge；The nanofiber aeroge of activation is finally immersed in 50 DEG C of the step 5) nickel bath in react,
Ensure that bath raio is 10：1, then take out after oscillating reactionss 15 minutes at a constant temperature, respectively deionized water and ethanol rinse 3 times,
It is last to dry at 50 DEG C, obtain the aerogel carried Ni of PA nanofibers2P5Catalysis material.
Embodiment 4
This enforcement discloses a kind of preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber, including following
Step：
1) prepare composite fibre：Take the polyvinyl alcohol-ethylene copolymer (PVA-co-PE) of 1kg and the acetate butyrate of 4.5kg
Cellulose (CAB) is uniformly mixed, and carries out extruding, pelletize in the double screw extruder that processing temperature is 170 DEG C, is obtained
PVA-co-PE/CAB composites；
2) prepare nanofiber suspension：PA/CAB composite Jing melt spinning machines are carried out into drawing-off, spinning is answered
Condensating fiber；Composite fibre is flowed back 72 hours in 60 DEG C of acetone and extracts acetylbutyrylcellulose, will be extraction acetate butyrate fine
Composite fibre after dimension element carries out normal temperature drying, prepares the PVA-co-PE nanofibers that average diameter is 100nm；Take
In the mixed solution of the tert-butyl alcohol of the water and 30ml that are scattered in 20ml of 0.5g PVA-co-PE nanofibers, dispersion is sufficiently stirred for
Obtain nanofiber suspension；
3) prepare binder solution：0.2g polyvinyl alcohol is taken, is stirred at 80 DEG C and is completely dissolved in the water of 10ml, prepared
Obtain the poly (vinyl alcohol) binder solution that mass concentration is 2%；
4) prepare nanofiber aeroge：By the step 3) the poly (vinyl alcohol) binder solution for preparing is added to the step
In the rapid nanofiber suspension for 2) preparing, mix homogeneously is placed in container template, is freezed 7 hours at -80 DEG C, is dried 36
Hour, you can obtain PVA-co-PE nanofiber aeroges；
5) configure sensitizing solution：Take 10g stannous chloride (SnCl2), mass concentration is 38% 30ml hydrochloric acid solutions, is added to
In 1L deionized waters；
Configuration activating solution：Take 0.25g Palladous chloride. (PdCl2), mass concentration is 38% 20ml hydrochloric acid solutions, is added to 1L
In deionized water；
Configuration nickel bath：Bivalent nickel ion (Ni in the nickel bath2+) concentration be 0.12mol/L, sodium hypophosphite (NaH2PO2)
Concentration be 30g/L, sodium acetate (CH3COONa concentration) is 19g/L, and the concentration of TritonX X is 100 8mg/L, sodium citrate
Concentration be 10g/L, the concentration of lactic acid is 11g/L, and the acid-base value of the nickel bath is pH=5.0；
6) prepare the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber：By the step 4) the PA nanofibers that prepare
Aeroge immerses the step 5) in the sensitizing solution that configures, it is ensured that bath raio is 30：1, take after vibrating absorption 3 minutes at 20 DEG C
Go out, obtain the nanofiber aeroge being sensitized, then the nanofiber aeroge of sensitization is immersed into the step 5) activation that configures
In liquid, it is ensured that bath raio is 30：1, then deionized water cleaning is taken out after absorption being vibrated at 20 DEG C 2 minutes, obtains what is activated
Nanofiber aeroge；The nanofiber aeroge of activation is finally immersed in 50 DEG C of the step 5) nickel bath in react,
Ensure that bath raio is 10：1, then take out after oscillating reactionss 15 minutes at a constant temperature, respectively deionized water and ethanol rinse 3 times,
It is last to dry at 50 DEG C, obtain the aerogel carried Ni of PVA-co-PE nanofibers3P catalysis materials.
The aerogel carried Ni of PVA-co-PE nanofibers in the present embodiment3The performance parameter of P catalysis materials is shown in Table 1.
In order to the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber for illustrating present invention preparation has preferable performance,
It is further explained with reference to relevant comparative's example.
With reference to table 1, comparative example 1 and the respectively Chinese invention patent application of comparative example 2：Embodiment in CN105148996A
1 and embodiment 4.In embodiments of the invention 1-4 and comparative example, the catalytic performance test process of catalysis material is as follows：By 3mg's
Catalysis material is placed in containing 3mL, adsorbs 20min, then in the quartz colorimetric utensil of paranitrophenol (PNP) aqueous solution of 0.5mM
0.3ml, the sodium borohydride aqueous solution of 1M are injected in this cuvette, test mixing solution is to the absorption intensity of ultraviolet light with the time
Variation tendency, catalysis material is calculated to the catalysis of paranitrophenol reduction reaction speed by the light intensity for contrasting different time
Rate.The experimental result of embodiments of the invention and comparative example such as table 1.
The porosity and catalytic performance of 1 embodiment of table and comparative example
Understand that with reference to table 1 the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber prepared by the present invention is received due to having
Rice network of fibers framing structure, porosity are higher, and nickel catalyst carried with Nanofiber Network skeleton as carrier, are deposited on
The fiber surface of constitutionally stable aerogel material, makes the catalyst have very high catalytic effect.
Claims (10)
1. the aerogel carried nickel-phosphorus alloy catalysis material of a kind of nanofiber, it is characterised in that：Catalysis material is by nanometer fiber net
Network skeleton and bag are attached to the nickel-phosphorus alloy nano-particle composition on Nanofiber Network skeleton surface, the Nanofiber Network skeleton
It is made up of nanofiber and the binding agent for being attached to nanofiber surface, the nanofiber is made up of thermoplastic polymer.
2. the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber according to claim 1, it is characterised in that：It is described to receive
Rice network of fibers skeleton with the mass percent of nickel-phosphorus alloy nano-particle be：50～75%：25～50%, the nanofiber
Mass percent with binding agent is：50～80%：20～50%.
3. the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber according to claim 1 and 2, it is characterised in that：Institute
The atom number percentage ratio for stating nickel and phosphorus in nickel-phosphorus alloy nano-particle is：50～80%：20～50%, and nickel-phosphorus alloy nanometer
The particle diameter of granule is 1～50nm.
4. the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber according to claim 1 and 2, it is characterised in that：Institute
Binding agent is stated for the one kind in polyvinyl alcohol, shitosan or poly-dopamine；The thermoplastic polymer is common for polyvinyl alcohol-ethylene
Polymers, polypropylene, polyamide, polyethylene terephthalate, PTT, poly terephthalic acid fourth two
One kind in alcohol ester or polyurethane.
5. the preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of a kind of nanofiber, it is characterised in that：Including following step
Suddenly：
1) prepare composite fibre：Thermoplastic polymer is uniformly mixed with acetylbutyrylcellulose, Jing double screw extruders extrusion,
Pelletize, prepares thermoplastic polymer/acetylbutyrylcellulose composite, continues thermoplastic polymer/acetate butyrate fiber
Plain composite Jing melt spinning machines carry out drawing-off, spinning, obtain composite fibre；
2) prepare nanofiber suspension：By the step 1) composite fibre for preparing is placed in acetone and flows back, extract
Normal temperature drying is carried out after acetylbutyrylcellulose, thermoplastic polymer nanofiber's fiber is prepared, then by thermoplastic polymer
Nanofiber is scattered in mixed solution of the organic solvent with water by the concentration of 1～10g/L, prepares finely dispersed nanometer
Fibrous suspension；
3) prepare binder solution：Binder solution is the one kind in poly-vinyl alcohol solution, chitosan solution or dopamine solution,
The poly-vinyl alcohol solution is that polyvinyl alcohol is dissolved in the water to prepare；The chitosan solution is by Chitosan powder point
Dissipate and prepare in water；The dopamine solution is that Dopamine Hydrochloride powder is scattered in Tri(Hydroxymethyl) Amino Methane Hydrochloride
Buffer solution prepare；
4) prepare nanofiber aeroge：By the step 3) binder solution and the step 2 that prepare) Nanowire for preparing
Dimension suspension mix homogeneously, prepares nanofiber mixing suspension, nanofiber mixing suspension is placed in container template
In, lyophilization in freezer dryer is then placed in again, prepares nanofiber aeroge；
5) configure the bath of nickel nano fibrous membrane sensitizing solution, activating solution and nickel；
6) prepare the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber：By the step 4) the nanofiber aeroge for preparing
Immerse the step 5) in the nickel nano fibrous membrane sensitizing solution for preparing vibration absorption obtain the nanofiber aeroge being sensitized, continue
The nanofiber aeroge of sensitization is immersed into the step 5) in the activating solution for preparing, vibration absorption obtains the nanofiber for activating
The nanofiber aeroge of activation is immersed oscillating reactionss in nickel bath, then deionized water and ethanol rinse, then is dried by aeroge
It is dry, that is, prepare the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber.
6. the preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber according to claim 5, its feature
It is：The step 5) in,
Configuration nickel nano fibrous membrane sensitizing solution：10g stannous chlorides are taken, mass concentration is 38% 30ml hydrochloric acid solutions, is added to
In 1L deionized waters；
Configuration activating solution：0.25g Palladous chloride .s are taken, mass concentration is 38% 20ml hydrochloric acid solutions, is added in 1L deionized waters；
Configuration nickel bath：In nickel bath, the molar concentration of bivalent nickel ion is 0.07～0.12mol/L, and the quality of sodium hypophosphite is dense
Spend for 16～40g/L, the mass concentration of sodium acetate is 15～20g/L, the mass concentration of triton x-100 be 5～10mg/L or
The mass concentration of Tween 80 is 5～10mg/L, and the mass concentration of sodium citrate is 8～10g/L, the mass concentration of lactic acid is 10～
12g/L, the acid-base value of the nickel bath is pH=4.5～5.0.
7. the preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber according to claim 5 or 6, which is special
Levy and be：The step 6) in, by the step 4) the nanofiber aeroge for preparing immerses the step 5) nanometer for preparing
In fibrous membrane sensitizing solution, it is ensured that bath raio is 30：1, taking out after vibration 1～5min of absorption at 15～25 DEG C, obtaining receiving for sensitization
Rice fiber aeroge, continue will the nanofiber aeroge of sensitization immerse the step 5) in the activating solution for preparing, it is ensured that bath raio
For 30：1, then deionized water cleaning is being taken out after vibration 1～5min of absorption at 15～25 DEG C, is obtaining the Nanowire for activating
Dimension aeroge；To react in the nanofiber aeroge immersion nickel bath of activation, it is ensured that bath raio is 10：1, then vibrate at a constant temperature
Take out after 10～20min of reaction, respectively deionized water and ethanol rinse 3 times, finally dry at 50 DEG C, that is, prepare and receive
The aerogel carried nickel-phosphorus alloy catalysis material of rice fiber.
8. the preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber according to claim 5, its feature
It is：The step 4) in, by the step 3) binder solution and the step 2 that prepare) nanofiber for preparing suspends
Liquid is 2～5 according to volume ratio：10 mix homogeneously, prepare nanofiber mixing suspension in the presence of emulsification pretreatment machine,
Nanofiber mixing suspension is placed in container template, lyophilization in freezer dryer is subsequently placed in, cryogenic temperature is ﹣ 80
DEG C～20 DEG C of ﹣, cooling time is 4～6h, and drying time is 24～72h, prepares nanofiber aeroge.
9. the preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber according to claim 5, its feature
It is：The step 3) in,
The preparation process of the poly-vinyl alcohol solution is：Polyvinyl alcohol is dissolved in the water, is sufficiently stirred for, obtaining mass concentration is
1.0～2.0% poly (vinyl alcohol) binder solution；
The preparation process of the chitosan solution is：It is 50% by mass percent：50% Chitosan powder is mixed with acetic acid,
Be then added in 25～50 times that quality is Chitosan powder quality of water, be uniformly dispersed, mass concentration is prepared for 1.0
～2.0% chitosan solution；
The preparation process of the dopamine solution is：Dopamine Hydrochloride powder is dispersed in into the trihydroxy methyl amino first of pH=8.5
In the buffer solution of heptane hydrochloride salt, it is sufficiently stirred for, prepares the dopamine solution that mass concentration is 0.2～2.0%.
10. the preparation method of the aerogel carried nickel-phosphorus alloy catalysis material of nanofiber according to claim 5, its feature
It is：The step 1) in, thermoplastic polymer is 5～40% with the mass percent of acetylbutyrylcellulose：60～95%；
The step 2) in, a diameter of 50～350nm of thermoplastic polymer nanofiber's fiber, the organic solvent are the tert-butyl alcohol, uncle penta
One kind in alcohol or sec-amyl alcohol, and the volume ratio of organic solvent and water is 1～3：1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109834791A (en) * | 2017-11-25 | 2019-06-04 | 徐州顺平生物科技有限公司 | A kind of enhanced water resistance nano modification timber |
| CN110327900A (en) * | 2019-07-08 | 2019-10-15 | 武汉纺织大学 | A kind of nanofiber hollow out ball sponge material and preparation method thereof |
| CN112281491A (en) * | 2020-10-30 | 2021-01-29 | 齐鲁工业大学 | Preparation and application of plant fiber-based reinforced carbon fiber network |
| CN115646063A (en) * | 2022-09-27 | 2023-01-31 | 美埃(南京)电子设备有限公司 | Anti-cracking micro-static filter element material and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285920A (en) * | 2013-05-27 | 2013-09-11 | 东华大学 | Three-dimensional fiber-based aerogel catalyst carrier and preparation method thereof |
| CN104674383A (en) * | 2015-02-12 | 2015-06-03 | 中国科学院城市环境研究所 | Carbon nano fiber aerogel electrostatic spinning construction method |
| CN105148996A (en) * | 2015-09-26 | 2015-12-16 | 佛山市维晨科技有限公司 | Nickel nanofiber membrane for membrane catalysis and preparation method of nickel nanofiber membrane |
| CN105543995A (en) * | 2015-12-18 | 2016-05-04 | 山东大学 | A polyacrylonitrile organic aerogel fiber material, a preparing method thereof and applications of the material |
-
2016
- 2016-09-28 CN CN201610861020.7A patent/CN106552674B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103285920A (en) * | 2013-05-27 | 2013-09-11 | 东华大学 | Three-dimensional fiber-based aerogel catalyst carrier and preparation method thereof |
| CN104674383A (en) * | 2015-02-12 | 2015-06-03 | 中国科学院城市环境研究所 | Carbon nano fiber aerogel electrostatic spinning construction method |
| CN105148996A (en) * | 2015-09-26 | 2015-12-16 | 佛山市维晨科技有限公司 | Nickel nanofiber membrane for membrane catalysis and preparation method of nickel nanofiber membrane |
| CN105543995A (en) * | 2015-12-18 | 2016-05-04 | 山东大学 | A polyacrylonitrile organic aerogel fiber material, a preparing method thereof and applications of the material |
Non-Patent Citations (1)
| Title |
|---|
| WEI-JIANG WANG ET AL.: "Amorphous NiP/SiO2 aerogel: Its preparation, its high thermal stability and its activity during the selective hydrogenation of cyclopentadiene to cyclopentene", 《APPLIED CATALYSIS A：GENERAL》 * |
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| CN110327900A (en) * | 2019-07-08 | 2019-10-15 | 武汉纺织大学 | A kind of nanofiber hollow out ball sponge material and preparation method thereof |
| WO2021004458A1 (en) * | 2019-07-08 | 2021-01-14 | 武汉纺织大学 | Ion exchange-type nanofiber skeleton three-dimensional separation material having controllable structure, and preparation method for same |
| CN112281491A (en) * | 2020-10-30 | 2021-01-29 | 齐鲁工业大学 | Preparation and application of plant fiber-based reinforced carbon fiber network |
| CN112281491B (en) * | 2020-10-30 | 2022-07-22 | 齐鲁工业大学 | Preparation and application of plant fiber-based reinforced carbon fiber network |
| CN115646063A (en) * | 2022-09-27 | 2023-01-31 | 美埃(南京)电子设备有限公司 | Anti-cracking micro-static filter element material and preparation method thereof |
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