CN105688914A - Method for preparing recyclable nickel nanowire-cuprous oxide multiplex photo-catalyst - Google Patents
Method for preparing recyclable nickel nanowire-cuprous oxide multiplex photo-catalyst Download PDFInfo
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- CN105688914A CN105688914A CN201610035714.5A CN201610035714A CN105688914A CN 105688914 A CN105688914 A CN 105688914A CN 201610035714 A CN201610035714 A CN 201610035714A CN 105688914 A CN105688914 A CN 105688914A
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- nano wire
- copper oxide
- oxide composite
- nickel nano
- red copper
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 92
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 27
- 229940112669 cuprous oxide Drugs 0.000 title abstract 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 17
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- 238000001291 vacuum drying Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 33
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- 239000002131 composite material Substances 0.000 claims description 29
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 230000001476 alcoholic effect Effects 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- 239000000975 dye Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 6
- 229940012189 methyl orange Drugs 0.000 claims description 6
- 150000002815 nickel Chemical class 0.000 claims description 6
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical group O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 230000001376 precipitating effect Effects 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 4
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 4
- 239000008103 glucose Substances 0.000 claims description 4
- HKOOXMFOFWEVGF-UHFFFAOYSA-N phenylhydrazine Chemical compound NNC1=CC=CC=C1 HKOOXMFOFWEVGF-UHFFFAOYSA-N 0.000 claims description 4
- 229940067157 phenylhydrazine Drugs 0.000 claims description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 3
- MPVDXIMFBOLMNW-ISLYRVAYSA-N 7-hydroxy-8-[(E)-phenyldiazenyl]naphthalene-1,3-disulfonic acid Chemical compound OC1=CC=C2C=C(S(O)(=O)=O)C=C(S(O)(=O)=O)C2=C1\N=N\C1=CC=CC=C1 MPVDXIMFBOLMNW-ISLYRVAYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- IQFVPQOLBLOTPF-HKXUKFGYSA-L congo red Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(/N=N/C3=CC=C(C=C3)C3=CC=C(C=C3)/N=N/C3=C(C4=CC=CC=C4C(=C3)S([O-])(=O)=O)N)=CC(S([O-])(=O)=O)=C21 IQFVPQOLBLOTPF-HKXUKFGYSA-L 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 2
- 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 claims description 2
- 229940043267 rhodamine b Drugs 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000005389 magnetism Effects 0.000 abstract 1
- 238000010907 mechanical stirring Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 150000003839 salts Chemical class 0.000 abstract 1
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- JTTXECQCCPZGII-UHFFFAOYSA-M sodium;ethane-1,2-diol;hydroxide Chemical compound [OH-].[Na+].OCCO JTTXECQCCPZGII-UHFFFAOYSA-M 0.000 description 4
- 239000000725 suspension Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000003911 water pollution Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- LBJNMUFDOHXDFG-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu].[Cu] LBJNMUFDOHXDFG-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000001089 mineralizing effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 230000002186 photoactivation Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 238000003900 soil pollution Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- B01J35/33—
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a method for preparing a recyclable nickel nanowire-cuprous oxide multiplex photo-catalyst. The method comprises the following steps of: firstly preparing nickel nanowires modified by polyvinylpyrrolidone; then performing ultrasonic dispersion on the nickel nanowires in an alcohol solvent of cupric salt; and adding a reducing agent under a mechanical stirring condition, and performing centrifugal treatment and vacuum drying, thereby obtaining the nickel nanowire-cuprous oxide multiplex photo-catalyst. The method is simple in process, low in cost, mild in condition and beneficial to large-scale industrial production; the nickel nanowire-cuprous oxide multiplex photo-catalyst prepared by the method is high in catalytic efficiency, has particle magnetism, is easy to recycle and reusable, and is capable of avoiding secondary pollution.
Description
Technical field
The preparation method that the present invention relates to a kind of nano particle photocatalyst, is specifically related to a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst。
Background technology
In recent years, environmental problem receives much concern。Water pollution, soil pollution, the health of the atmospheric pollution serious threat mankind and ecological balance。Wherein, water pollution is mainly derived from and produces and the waste water from dyestuff of discharge, agricultural chemicals waste water, surface active agent wastewater etc. in life process。Due to waste water from dyestuff there is complex chemical composition, be difficult to biochemical degradation, the feature such as content of organics is high, toxicity is big, be therefore one of industrial wastewater that difficulty of governance is bigger。
The appearance of nanotechnology and develop the process for waste water from dyestuff rapidly and provide new approach。Utilizing metal semiconductor oxide nano-particles photocatalytic degradation of dye waste water is a kind of novel Pollutant Treatment technology。Photoactivation agent processes sewage, has an advantage in that: catalytic reaction condition simple (normal temperature and pressure), energy consumption is low, it is fast, easy and simple to handle to degrade, and the broad spectrum activity of organic pollutant degradation is high。At present, most popular semiconductor light-catalyst is titanium dioxide (TiO2), this photocatalyst can by thorough for most organic pollutants mineralizing and degrading。But TiO2Greater band gap (Eg ≈ 3.2eV), its catalytic performance is only capable of the ultraviolet excitation of occupied solar energy 5%。Therefore, people focus on the semiconductor catalyst that research and development are excitation source with visible ray (accounting for the 45% of solar energy) more。Wherein, Red copper oxide (Cu2O) being widely used as environmentally friendly direct band gap P-type semiconductor, its energy gap is about 2.07eV, available most visible ray。
Although big quantity research shows that nano particle photocatalyst has the features such as specific surface area is big, the active height of catalysis, chemical reaction are fast, but is faced with recovery difficulty in actual applications, recycling rate of waterused is low, secondary pollution problems。In recent years, reclaiming of nano particle photocatalyst separates and improves emphasis and the difficult point that its catalysis activity under visible light is photocatalysis field research。
Therefore, those skilled in the art is devoted to the preparation method of developing a kind of efficient recyclable photocatalyst。
Summary of the invention
The technical problem to be solved is: overcome above-mentioned the deficiencies in the prior art, it is proposed to a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst。
For achieving the above object, the invention provides a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst, it is adsorbed on the copper ion of nickel nanowire surface by in-situ reducing, and obtains recyclable nickel nano wire-Red copper oxide composite solids through centrifugal and vacuum drying treatment。Concrete technical scheme is as follows:
A kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst, comprises the following steps:
Step 1, is dissolved in the ethylene glycol solution of polyvinylpyrrolidone by soluble nickel salt, obtains the first reaction solution；Sodium hydroxide is dissolved in ethylene glycol, obtains the second reaction solution；Under stirring condition, the first reaction solution is joined formation the 3rd reaction solution in the second reaction solution；3rd reaction solution add the first reducing agent and stirs, obtaining the 4th reaction solution；4th reaction solution prepares polyvinyl pyrrolidon modified nickel nano wire by water-bath under the influence of a magnetic field；
Step 2, by polyvinyl pyrrolidon modified nickel nano wire ultrasonic disperse in the alcoholic solution of mantoquita, obtains reaction dispersion liquid；Then, under mechanical agitation, in reaction dispersion liquid, drip the second reducing agent, obtain compound precursor；
Step 3, is centrifuged compound precursor processing, and uses deionized water washing and precipitating after first time is centrifugal；Centrifugal three times again, precipitate with washes of absolute alcohol after being centrifuged every time；Finally precipitation vacuum drying can be obtained nickel nano wire-Red copper oxide composite solids。
Preferably, in step 1, soluble nickel salt is Nickel dichloride hexahydrate, and in the first reaction solution, the concentration of soluble nickel salt is 0.005～0.04mol/L。
Preferably, in step 1, in the ethylene glycol solution of polyvinylpyrrolidone, the mass fraction of polyvinylpyrrolidone is 1～4%, and the molecular weight of polyvinylpyrrolidone is 10000～55000。
Preferably, in step 1, in the second reaction solution, the concentration of sodium hydroxide is 0.05～1.0mol/L。
Preferably, in step 1, the intensity in magnetic field is 0.2～1T；The temperature of water-bath is 50～100 DEG C, and the time of water-bath is 0.5～2h。
Preferably, in step 2, in the alcoholic solution of mantoquita, solvent is the one among methanol, ethanol or propanol, and mantoquita is the one among copper sulfate, copper nitrate, copper acetate or copper chloride, and in the alcoholic solution of mantoquita, the concentration of mantoquita is 0.01～0.1mol/L。
Preferably, in step 2, the ultrasonic disperse time is 0.25～1h, and the mechanical agitation time is 0.5～2h。
Preferably, in step 3, centrifugal rotational speed is 500～3000rpm, and vacuum drying temperature is 30～60 DEG C。
Preferably, the first reducing agent is the one among hydrazine hydrate, phenylhydrazine, azanol, sodium borohydride, ammonia or glucose；Second reducing agent is the one among hydrazine hydrate, phenylhydrazine, azanol, sodium borohydride, ammonia or glucose。
In a series of detailed description of the invention of the present invention, the nickel Nanowire Quality being dispersed in the alcoholic solution of mantoquita is 5～20mg, the addition of the first reducing agent is 5～20mL, and the addition of the second reducing agent is 50～150 μ L, and the volume of the alcoholic solution of mantoquita is 40～150mL。
Nickel nano wire-Red copper oxide composite photo-catalyst prepared by above method can be used for the photocatalytic degradation of organic dyestuff, and organic dyestuff is the one among methyl orange, methyl blue, rhodamine B, Congo red or orange G。
Compared with prior art, there is advantages that cost is low, be suitable for industrialized production, prepared nickel nano wire-Red copper oxide composite photo-catalyst has magnetic, is easily recycled, it is to avoid cause secondary pollution in actual water pollution processes。
Hereinafter the technique effect of the design of the present invention, instantiation and generation is described further, to be fully understood from the present invention。There is provided these descriptive purposes to be only that and help explain the present invention, should not be taken to limit the scope of the claims of the present invention。
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of nickel nanometer powder；
Fig. 2 is the scanning electron microscope (SEM) photograph of nickel nano wire-Red copper oxide composite powder；
Fig. 3 is the X-ray powder diffraction figure of nickel nano wire-Red copper oxide composite powder；
Fig. 4 is the hysteresis curve figure of nickel nano wire-Red copper oxide composite powder；
Fig. 5 is the ultraviolet visible absorption spectra figure of nickel nano wire-Red copper oxide complex and nickel nanometer solution；
Fig. 6 is the visible absorption spectrogram of nickel nano wire-Red copper oxide complex photocatalysis methyl orange。
Detailed description of the invention
Below in conjunction with accompanying drawing, embodiments of the invention being elaborated, the present embodiment is carried out under premised on technical solution of the present invention, gives detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment。
Embodiment 1
Step 1,0.5g Nickel dichloride hexahydrate is dissolved in the ethylene glycol solution of polyvinylpyrrolidone (molecular weight 55000) of 100mL mass fraction 4%, under stirring condition, nickel chloride solution is poured in the sodium hydroxide ethylene glycol solution of 100ml (0.5mol/L), the hydrazine hydrate of 15ml mass fraction 85% is added in mixed liquor, after solution turned blue, reaction is transferred in water-bath, when 0.5T externally-applied magnetic field, water-bath 80 DEG C reaction 1h, question response terminate after by product cleaning, obtain nickel nano wire；
Step 2, take 5mg nickel nano wire ultrasonic disperse (0.05mol/L) in the alcoholic solution of 50ml copper nitrate in step 1, under mechanical agitation, in dispersion liquid, drip the hydrazine hydrate solution of 100 μ L mass fractions 35%, after continuing stirring 1h, obtain compound precursor；
Step 3, is centrifuged gained presoma in step 2 with the rotating speed of 2000rpm, is poured off suspension after first time is centrifugal, use deionized water washing and precipitating, centrifugal 3 times again, with washes of absolute alcohol precipitate after being centrifuged every time, precipitation vacuum drying can be obtained nickel nano wire-Red copper oxide composite solids。
Embodiment 2
Step 1,0.5g Nickel dichloride hexahydrate is dissolved in the ethylene glycol solution of polyvinylpyrrolidone (molecular weight 55000) of 100mL mass fraction 2%, under stirring condition, nickel chloride solution is poured in the sodium hydroxide ethylene glycol solution of 100ml (0.5mol/L), the ammonia of 20ml mass fraction 25% is added in mixed liquor, after solution turned blue, reaction is transferred in water-bath, when 0.5T externally-applied magnetic field, water-bath 80 DEG C reaction 1h, question response terminate after by product cleaning, obtain nickel nano wire；
Step 2, take 5mg nickel nano wire ultrasonic disperse (0.05mol/L) in the alcoholic solution of 50ml copper nitrate in step 1, under mechanical agitation, in dispersion liquid, drip the ammonia spirit of 120 μ L mass fractions 25%, after continuing stirring 1h, obtain compound precursor；
Step 3, is centrifuged gained presoma in step 2 with the rotating speed of 1500rpm, is poured off suspension after first time is centrifugal, use deionized water washing and precipitating, centrifugal 3 times again, with washes of absolute alcohol precipitate after being centrifuged every time, precipitation vacuum drying can be obtained nickel nano wire-Red copper oxide composite solids。
Embodiment 3
Step 1,0.5g Nickel dichloride hexahydrate is dissolved in the ethylene glycol solution of polyvinylpyrrolidone (molecular weight 55000) of 100mL mass fraction 2%, under stirring condition, nickel chloride solution is poured in the sodium hydroxide ethylene glycol solution of 100ml (0.5mol/L), the azanol of 10ml mass fraction 50% is added in mixed liquor, after solution turned blue, reaction is transferred in water-bath, when 1T externally-applied magnetic field, water-bath 60 DEG C reaction 1h, question response terminate after by product cleaning, obtain nickel nano wire；
Step 2, take 5mg nickel nano wire ultrasonic disperse (0.05mol/L) in the alcoholic solution of 50ml copper sulfate in step 1, under mechanical agitation, in dispersion liquid, drip the hydroxylamine solution of 60 μ L mass fractions 50%, after continuing stirring 1h, obtain compound precursor；
Step 3, is centrifuged gained presoma in step 2 with the rotating speed of 2000rpm, is poured off suspension after first time is centrifugal, use deionized water washing and precipitating, centrifugal 3 times again, with washes of absolute alcohol precipitate after being centrifuged every time, precipitation vacuum drying can be obtained nickel nano wire-Red copper oxide composite solids。
Embodiment 4
Step 1,0.3g Nickel dichloride hexahydrate is dissolved in the ethylene glycol solution of polyvinylpyrrolidone (molecular weight 55000) of 100mL mass fraction 2%, under stirring condition, nickel chloride solution is poured in the sodium hydroxide ethylene glycol solution of 100ml (0.5mol/L), the hydrazine hydrate of 15ml mass fraction 85% is added in mixed liquor, after solution turned blue, reaction is transferred in water-bath, when 1T externally-applied magnetic field, water-bath 75 DEG C reaction 0.5h, question response terminate after by product cleaning, obtain nickel nano wire；
Step 2, take 5mg nickel nano wire ultrasonic disperse (0.03mol/L) in the alcoholic solution of 50ml copper nitrate in step 1, under mechanical agitation, in dispersion liquid, drip the hydrazine hydrate solution of 100 μ L mass fractions 35%, after continuing stirring 1h, obtain compound precursor；
Step 3, is centrifuged gained presoma in step 2 with the rotating speed of 2000rpm, is poured off suspension after first time is centrifugal, use deionized water washing and precipitating, centrifugal 3 times again, with washes of absolute alcohol precipitate after being centrifuged every time, precipitation vacuum drying can be obtained nickel nano wire-Red copper oxide composite solids。
Embodiment 5
With the nickel nano wire-Red copper oxide complex of embodiment 1 preparation for photocatalyst, catalysis methyl orange dye。Using the photochemical reactor of the luxuriant and rich with fragrance Lay production of Beijing pool as catalysis light source, wherein the power of xenon lamp is 300W, grows up in 420nm with radiation light-wave after optical filter elimination ultraviolet light。With the 464nm maximum absorption wavelength being methyl orange solution, survey its absorbance。The photocatalytic activity of sample=(A0-At)/A0× 100%。Wherein A0For the initial concentration of methyl orange, AtConcentration for different catalysis time condition Methyl Oranges。After catalysis 80min, nickel nano wire-Red copper oxide composite photo-catalyst to the degradation rate of methyl orange up to 93.8%。
The preferred embodiment of the present invention described in detail above。Should be appreciated that those of ordinary skill in the art just can make many modifications and variations according to the design of the present invention without creative work。Therefore, all technical staff in the art, all should in the protection domain being defined in the patent claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment。
Claims (10)
1. the method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst, it is characterised in that comprise the following steps:
Step 1, is dissolved in the ethylene glycol solution of polyvinylpyrrolidone by soluble nickel salt, obtains the first reaction solution；Sodium hydroxide is dissolved in ethylene glycol, obtains the second reaction solution；Under stirring condition, described first reaction solution is joined formation the 3rd reaction solution in described second reaction solution；Described 3rd reaction solution add the first reducing agent and stirs, obtaining the 4th reaction solution；Described 4th reaction solution prepares polyvinyl pyrrolidon modified nickel nano wire by water-bath under the influence of a magnetic field；
Step 2, by described polyvinyl pyrrolidon modified nickel nano wire ultrasonic disperse in the alcoholic solution of mantoquita, obtains reaction dispersion liquid；Then, under mechanical agitation, in described reaction dispersion liquid, drip the second reducing agent, obtain compound precursor；
Step 3, is centrifuged described compound precursor processing, and uses deionized water washing and precipitating after first time is centrifugal；Centrifugal three times again, precipitate with washes of absolute alcohol after being centrifuged every time；Finally precipitation vacuum drying can be obtained nickel nano wire-Red copper oxide composite solids。
2. a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst according to claim 1, it is characterized in that, in step 1, described soluble nickel salt is Nickel dichloride hexahydrate, and described in described first reaction solution, the concentration of soluble nickel salt is 0.005～0.04mol/L。
3. a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst according to claim 1, it is characterized in that, in step 1, the mass fraction of polyvinylpyrrolidone described in the ethylene glycol solution of described polyvinylpyrrolidone is 1～4%, and the molecular weight of described polyvinylpyrrolidone is 10000～55000。
4. a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst according to claim 1, it is characterised in that in step 1, described in described second reaction solution, the concentration of sodium hydroxide is 0.05～1.0mol/L。
5. a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst according to claim 1, it is characterised in that in step 1, the intensity in described magnetic field is 0.2～1T；The temperature of described water-bath is 50～100 DEG C, and the time of described water-bath is 0.5～2h。
6. a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst according to claim 1, it is characterized in that, in step 2, in the alcoholic solution of described mantoquita, solvent is the one among methanol, ethanol or propanol, described mantoquita is the one among copper sulfate, copper nitrate, copper acetate or copper chloride, and the concentration of mantoquita described in the alcoholic solution of described mantoquita is 0.01～0.1mol/L。
7. a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst according to claim 1, it is characterised in that in step 2, the described ultrasonic disperse time is 0.25～1h, and the described mechanical agitation time is 0.5～2h。
8. a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst according to claim 1, it is characterised in that in step 3, described centrifugal rotational speed is 500～3000rpm, and described vacuum drying temperature is 30～60 DEG C。
9. a kind of method preparing recyclable nickel nano wire-Red copper oxide composite photo-catalyst according to claim 1, it is characterised in that described first reducing agent is the one among hydrazine hydrate, phenylhydrazine, azanol, sodium borohydride, ammonia or glucose；Described second reducing agent is the one among hydrazine hydrate, phenylhydrazine, azanol, sodium borohydride, ammonia or glucose。
10. nickel nano wire-Red copper oxide composite photo-catalyst application in photocatalytic degradation that preparation method according to any one of claim 1-9 prepares, it is characterized in that, described nickel nano wire-Red copper oxide composite photo-catalyst is for the photocatalytic degradation of organic dyestuff, and described organic dyestuff is the one among methyl orange, methyl blue, rhodamine B, Congo red or orange G。
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| CN106519086A (en) * | 2016-11-03 | 2017-03-22 | 哈尔滨工业大学 | Polyvinyl pyrrolidine imine high-molecular compound, and preparation method and applications thereof |
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