CN109589999A - A kind of dyestuff waste liquid processing preparation method of NiO/BiOBr composite photo-catalyst - Google Patents
A kind of dyestuff waste liquid processing preparation method of NiO/BiOBr composite photo-catalyst Download PDFInfo
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- CN109589999A CN109589999A CN201910030612.8A CN201910030612A CN109589999A CN 109589999 A CN109589999 A CN 109589999A CN 201910030612 A CN201910030612 A CN 201910030612A CN 109589999 A CN109589999 A CN 109589999A
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- 239000007788 liquid Substances 0.000 title claims abstract description 39
- 239000000975 dye Substances 0.000 title claims abstract description 35
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 34
- 239000002699 waste material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000012545 processing Methods 0.000 title description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 37
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 229910000480 nickel oxide Inorganic materials 0.000 claims abstract description 15
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 13
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 59
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 36
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000013049 sediment Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 4
- 238000010189 synthetic method Methods 0.000 claims description 4
- 229910052794 bromium Inorganic materials 0.000 claims description 3
- 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 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 125000001246 bromo group Chemical group Br* 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 2
- 229910052797 bismuth Inorganic materials 0.000 claims 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims 1
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- 229910052759 nickel Inorganic materials 0.000 claims 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 150000001875 compounds Chemical class 0.000 abstract description 7
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 230000004298 light response Effects 0.000 abstract description 2
- 239000012779 reinforcing material Substances 0.000 abstract description 2
- 239000011858 nanopowder Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 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 description 6
- 238000000034 method Methods 0.000 description 6
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- AOPCKOPZYFFEDA-UHFFFAOYSA-N nickel(2+);dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O AOPCKOPZYFFEDA-UHFFFAOYSA-N 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- 229910002651 NO3 Inorganic materials 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 3
- 238000006303 photolysis reaction Methods 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000008235 industrial water Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002894 chemical waste Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
Abstract
The present invention relates to a kind of preparation methods of dyestuff waste liquid catalysts for treating, it is to be dispersed in nano-nickel oxide in bismuth nitrate alcoholic solution to obtain solution A, solution A and solution B Hybrid Heating are reacted, heating, which recycles reaction product after reaction and carries out removal of impurities, handles obtained NiO/BiOBr composite photo-catalyst, and the solution B is aqueous sodium bromide.NiO/BiOBr composite photo-catalyst be BiOBr nanometer sheet the granular NiO of area load it is nanocrystalline.The size of BiOBr nanometer sheet is 100~300nm, and NiO nanocrystalline size is 20~50nm.Above-mentioned technical proposal, the NiO of ultraviolet light response and visible light-responded two kinds of semiconductors of BiOBr are carried out compound, on the one hand the utilization rate of sunlight can be greatly improved, on the other hand photogenerated charge separative efficiency can also be greatly improved, to the Photocatalytic activity of effective reinforcing material, the ability repaired to environment is improved.
Description
Technical field
The present invention relates to chemical waste liquid process fields, and in particular to a kind of dyestuff waste liquid processing NiO/BiOBr complex light
The preparation method of catalyst.
Background technique
In recent years, it is short to cause the energy to the excessive exploitation and use of coal, oil and natural gas non-renewable resources by the mankind
It lacks continuous worsening with environment.In the past few decades, industry and textile industry are as important industry drive economic development, largely
Industrial wastewater and water-soluble dye waste liquid are discharged into rivers, cause serious injury to people's lives industrial water.To solve the energy
It is main idea with environmental crisis, each state all is sparing no effort to seek alternative green energy resource and develop to improve the pollution-free of environment
Technology.
Photocatalysis technology provides the technological approaches of green for alleviating energy crisis and solution this two hang-up of environmental pollution.
However, the development and application of the technology are but by the restriction of catalysis material, the existing generally existing solar energy of catalysis material
The bottleneck problem of low two urgent need to resolve low with quantum efficiency of utilization rate.By semiconductor and other materials it is compound be improve semiconductor
One of photocatalytic activity and the effective means of efficiency.There are a large amount of contact surface and interface between two kinds of compound materials, make
Material after compound also shows many synergistic effects other than the various performances with every kind of monomer, significantly improves half
The performance of conductor.
BiOX (X=Cl, Br, I) is conducive to electrons and holes with its unique electronic structure and layered crystal structure
Separation and migration, indirect transition mode restrained effectively the compound of light induced electron and hole, be beneficial to improve photochemical catalyst
Quantum efficiency.Nevertheless, still in application process, nevertheless suffering from the restriction of some key scientific problems.Wherein, BiOBr
Forbidden bandwidth in 2.7eV or so, although have it is visible light-responded, it is limited to the absorption of visible light, in addition, for monomer
BiOBr, the recombination probability of electrons and holes is still very big, needs further to make great efforts to improve quantum efficiency.
Nickel oxide is typical transition metal oxide, is a kind of direct wide band gap semiconducter.With regard to as photochemical catalyst
For, forbidden bandwidth at room temperature is 3.6 ~ 4.0eV, can only absorb the photon of UV light region, but ultraviolet light only accounts for sunlight
4% energy is greatly limited the effective use of solar energy.
Summary of the invention
The present invention provides a kind of NiO/BiOBr composite photo-catalyst.
A kind of NiO/BiOBr composite photo-catalyst, it is characterised in that: the granular NiO of the area load of BiOBr nanometer sheet
It is nanocrystalline.Specifically, the size of BiOBr nanometer sheet is 100~300nm, NiO nanocrystalline size is 20~50nm.
The present invention also provides a kind of processing methods of dyestuff waste liquid, including operate as follows:
Catalyst is added in dyestuff waste liquid and carries out dark adsorption treatment, photodissociation processing is carried out after dark adsorption treatment；The catalysis
Agent is NiO/BiOBr composite photo-catalyst, and rhodamine and/or Congo red is contained in the dyestuff waste liquid.
The time of dark adsorption treatment is 1.8~2.2h.
Photodissociation processing light source used is xenon source, and the power of specific xenon source is the nm of 300W, λ >=400.
The mass ratio of pollutant is 1:0.12~0.14 in the additional amount and dyestuff waste liquid of catalyst, and the quality of pollutant is
Rhodamine and Congo red quality sum, 45~60min of time of photodissociation processing.
The present invention also provides a kind of preparation methods of dyestuff waste liquid catalysts for treating, including operate as follows:
Nano-nickel oxide is dispersed in bismuth nitrate alcoholic solution and obtains solution A, solution A and solution B Hybrid Heating are reacted, heating
Reaction product is recycled after reaction and carries out removal of impurities and handles obtained NiO/BiOBr composite photo-catalyst, and the solution B is bromine
Change sodium water solution.
Specific scheme are as follows:
Bismuth nitrate alcoholic solution is dissolved in prepare in ethylene glycol by five nitric hydrate bismuths and be obtained.
Solution A and the reaction of solution B Hybrid Heating are operated using water-bath synthetic method.
Nano-nickel oxide is that nickel nitrate aqueous solution and the reaction of aqueous sodium carbonate Hybrid Heating are made.
Nickel nitrate aqueous solution and aqueous sodium carbonate pass through water-bath synthetic method preparing nano nickel oxide.
Solution A and solution B Hybrid Heating recycle reaction product by the way of filtering after reaction, and reaction product is washed
It washs completely, is then dried and grinds obtained NiO/BiOBr composite photo-catalyst.
Solution A, solution B are that the progress of 1:1.5~2.5 Hybrid Heating is reacted with the molar ratio of sodium bromide according to bismuth nitrate, molten
Dispersed in liquid A according to every 1mmol bismuth nitrate addition 0.05~0.2g nano-nickel oxide.
Nickel nitrate aqueous solution, aqueous sodium carbonate are that 1:1.8~2.2 are mixed according to the molar ratio of nickel nitrate, sodium carbonate
Close heating reaction.
Bismuth nitrate alcoholic solution is dissolved in prepare in 20ml ethylene glycol by every five nitric hydrate bismuth of 1mmol and be obtained.
Stirring and dissolving in ethylene glycol first is added in five nitric hydrate bismuths, is then added nano-nickel oxide, ultrasonic disperse 20~
40 minutes, obtained solution A；Sodium bromide is dissolved in deionized water again and obtains solution B；Solution B is added in solution A, magnetic force stirs
It mixes 15~25 minutes, is subsequently placed in 90 DEG C of thermostat water baths, react 2 hours, after reaction, cooled to room temperature is taken out
Filter recycling reaction product sequentially washs reaction product, is dried, grinding obtained NiO/BiOBr composite photo-catalyst.
Nickelous nitrate hexahydrate is dissolved in deionized water, is then added aqueous sodium carbonate, 15~25 points of magnetic agitation
Clock；Above-mentioned mixed liquor is placed in water-bath, 90 DEG C are reacted 1~3 hour, and cooled to room temperature, filters recycling after reaction
Reaction product is then sequentially washed, dries to obtain nickeliferous sediment, nickeliferous sediment is put into resistance furnace, and heat treatment 1 is small
When to get nano-nickel oxide.
Above-mentioned technical proposal, the NiO of ultraviolet light response and visible light-responded two kinds of semiconductors progress of BiOBr is compound,
On the one hand the utilization rate of sunlight can be greatly improved, photogenerated charge separative efficiency on the other hand can also be greatly improved, thus
The Photocatalytic activity of effective reinforcing material, improves the ability repaired to environment.
In addition, above-mentioned preparation method, does not need using toxic solvent, environment protecting and power-saving；Raw material is easy to get, is low in cost,
Production line is short, is suitable for industrialized production.Catalysis material, optics, in terms of have huge application prospect.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) figure of NiO/BiOBr composite photo-catalyst produced by the present invention.
Fig. 2 is scanning electron microscope (SEM) photo of NiO/BiOBr composite photo-catalyst produced by the present invention.
Fig. 3 be NiO/BiOBr composite photo-catalyst produced by the present invention and pure BiOBr and pure NiO rhodamine B degradation,
The effect contrast figure of Congo red mixed dyestuff waste liquid.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments specific
It is bright.It should be appreciated that following text is only used to describe one or more of specific embodiments of the invention, not to the present invention
The protection scope specifically requested carries out considered critical.
Unless otherwise instructed, used drug and reagent are commercially available by commercial sources.
Embodiment 1
Weigh 2mmol Nickelous nitrate hexahydrate (Ni (NO3)2·6H2O it) is dissolved in 30mL deionized water, 30mL is then added and contains
4mmol sodium carbonate (Na2CO3) aqueous solution, magnetic agitation 20 minutes；Above-mentioned reaction solution is placed in water-bath, temperature 90 is set
DEG C, it reacts 2 hours, cooled to room temperature, filters, wash, is dry that nickeliferous sediment, sediment are put into resistance furnace,
400 DEG C of setting is heat-treated 1 hour, obtains NiO nano powder；Weigh five nitric hydrate bismuth (Bi (NO of 1mmol3)3·5H2O), it is added
Then stirring and dissolving in 20mL ethylene glycol is added the NiO nano powder of 0.1g, ultrasonic disperse 30 minutes, obtains solution A；It weighs
2.0mmol sodium bromide (NaBr) is added 40mL deionized water, dissolves to obtain solution B；Solution B is added in solution A, magnetic force stirs
It mixes 20 minutes, is subsequently placed in 90 DEG C of thermostat water baths, react 2 hours；After reaction, cooled to room temperature is filtered, is washed
It washs, dry, grinding to get the NiO/BiOBr composite photo-catalyst of organic dyestuff is mixed to a kind of degradation.
Map detection is carried out to NiO/BiOBr composite photo-catalyst obtained above, as a result as shown in Figure 1, 2.Referring to attached
X-ray diffraction (XRD) map of NiO/BiOBr composite photo-catalyst is made for embodiment 1,37.25 in figure in Fig. 1o、43.27oWith
62.86oThree peak indexs that place occurs are the diffraction maximum of (111) of cubic phase nickel oxide, (200) and (220) three crystal faces, with
The standard diffraction peak of JCPDS card (47-1049) nickel oxide is consistent.Remaining spectral line peak position and JCPDS card (09- in figure
0393) standard diffraction peak of BiOBr corresponds.Show that prepared product is NiO/BiOBr compound.
Referring to attached drawing 2, the scanning electron microscope (SEM) that NiO/BiOBr composite photo-catalyst is made for embodiment 1 is shone
Piece, it is seen that nano-sheet substrate is BiOBr, and the size of nanometer sheet is 100~300 nm, and 20~50 nm are granular
NiO is nanocrystalline to be closely supported on the surface of BiOBr nanometer sheet.
Embodiment 2
50ml dyestuff waste liquid is taken, the concentration of rhodamine B is 20mg/L in dyestuff waste liquid, Congo red concentration is 90mg/L, to dye
Expect the NiO/BiOBr composite photo-catalyst that 40mg is added in waste liquid, dark adsorption treatment reaches adsorption-desorption balance for 2 hours；
Then above-mentioned solution being placed under xenon source (nm of 300W, λ >=400) vertical irradiation, illumination period is every at regular intervals,
It is sampled, is centrifuged, take its supernatant, detect absorbance with ultraviolet-visible spectrophotometer, record data.
50ml dyestuff waste liquid is taken, the concentration of rhodamine B is 20mg/L in dyestuff waste liquid, Congo red concentration is 90mg/L,
The NiO catalyst of 40mg is added into dyestuff waste liquid, dark adsorption treatment reaches adsorption-desorption balance for 2 hours；It then will be upper
It states solution and is placed under xenon source (nm of 300W, λ >=400) vertical irradiation, illumination period is taken per at regular intervals
Sample, centrifugation take its supernatant, detect absorbance with ultraviolet-visible spectrophotometer, record data.
50ml dyestuff waste liquid is taken, the concentration of rhodamine B is 20mg/L in dyestuff waste liquid, Congo red concentration is 90mg/L,
The BiOBr catalyst of 40mg is added into dyestuff waste liquid, dark adsorption treatment reaches adsorption-desorption balance for 2 hours；Then will
Above-mentioned solution is placed under xenon source (nm of 300W, λ >=400) vertical irradiation, and illumination period is carried out per at regular intervals
Sampling, centrifugation, take its supernatant, detect absorbance with ultraviolet-visible spectrophotometer, record data.
As a result as shown in figure 3, NiO/BiOBr composite photo-catalyst is made to two kinds of mixing dyes in waste water from dyestuff in embodiment 1
The decolorization of material will be significantly stronger than pure BiOBr and pure NiO, have superior photocatalysis performance.
Embodiment 3
Weigh 2mmol Nickelous nitrate hexahydrate (Ni (NO3)2·6H2O it) is dissolved in 30mL deionized water, 30mL is then added and contains
4mmol sodium carbonate (Na2CO3) aqueous solution, magnetic agitation 15 minutes；Above-mentioned reaction solution is placed in water-bath, temperature 90 is set
DEG C, it reacts 2.5 hours, cooled to room temperature, filters, wash, is dry that nickeliferous sediment, sediment are put into resistance furnace
In, it is arranged 450 DEG C, is heat-treated 1 hour, obtains NiO nano powder；Weigh five nitric hydrate bismuth (Bi (NO of 1mmol3)3·5H2O),
Stirring and dissolving in 20mL ethylene glycol is added, the NiO nano powder of 0.2g is then added, ultrasonic disperse 35 minutes, obtains solution A；It weighs
2.5mmol sodium bromide (NaBr) is added 40mL deionized water, dissolves to obtain solution B；Solution B is added in solution A, magnetic force stirs
It mixes 25 minutes, is subsequently placed in 90 DEG C of thermostat water baths, react 2 hours；After reaction, cooled to room temperature is filtered, is washed
It washs, dry, grinding to get NiO/BiOBr composite photo-catalyst is arrived.
It is detected through XRD, SEM, the map and micro-structure diagram of NiO/BiOBr composite photo-catalyst made from the present embodiment are equal
It is consistent with embodiment 1.Using the identical method of embodiment 2 to the present embodiment be made NiO/BiOBr composite photo-catalyst with
NiO catalyst, BiOBr catalyst catalytic performance be compared, be as a result consistent with embodiment 2, NiO/BiOBr complex light
The photocatalysis performance of catalyst is substantially better than NiO catalyst, BiOBr catalyst.
Embodiment 4
Weigh 2mmol Nickelous nitrate hexahydrate (Ni (NO3)2·6H2O it) is dissolved in 30mL deionized water, 30mL is then added and contains
4mmol sodium carbonate (Na2CO3) aqueous solution, magnetic agitation 25 minutes；Above-mentioned reaction solution is placed in water-bath, temperature 90 is set
DEG C, it reacts 3 hours, cooled to room temperature, filters, wash, is dry that nickeliferous sediment, sediment are put into resistance furnace,
350 DEG C of setting is heat-treated 1 hour, obtains NiO nano powder；Weigh five nitric hydrate bismuth (Bi (NO of 1mmol3)3·5H2O), it is added
Then stirring and dissolving in 20mL ethylene glycol is added the NiO nano powder of 0.15g, ultrasonic disperse 25 minutes, obtains solution A；It weighs
2.0mmol sodium bromide (NaBr) is added 40mL deionized water, dissolves to obtain solution B；Solution B is added in solution A, magnetic force stirs
It mixes 25 minutes, is subsequently placed in 90 DEG C of thermostat water baths, react 2 hours；After reaction, cooled to room temperature is filtered, is washed
It washs, dry, grinding to get NiO/BiOBr composite photo-catalyst is arrived.
It is detected through XRD, SEM, the map and micro-structure diagram of NiO/BiOBr composite photo-catalyst made from the present embodiment are equal
It is consistent with embodiment 1.Using the identical method of embodiment 2 to the present embodiment be made NiO/BiOBr composite photo-catalyst with
NiO catalyst, BiOBr catalyst catalytic performance be compared, be as a result consistent with embodiment 2, NiO/BiOBr complex light
The photocatalysis performance of catalyst is substantially better than NiO catalyst, BiOBr catalyst.
Embodiment 5
Weigh 2mmol Nickelous nitrate hexahydrate (Ni (NO3)2·6H2O it) is dissolved in 30mL deionized water, 30mL is then added and contains
4mmol sodium carbonate (Na2CO3) aqueous solution, magnetic agitation 20 minutes；Above-mentioned reaction solution is placed in water-bath, temperature 90 is set
DEG C, it reacts 2 hours, cooled to room temperature, filters, wash, is dry that nickeliferous sediment, sediment are put into resistance furnace,
500 DEG C of setting is heat-treated 1 hour, obtains NiO nano powder；Weigh five nitric hydrate bismuth (Bi (NO of 1mmol3)3·5H2O), it is added
Then stirring and dissolving in 20mL ethylene glycol is added the NiO nano powder of 0.08g, ultrasonic disperse 20 minutes, obtains solution A；It weighs
1.5mmol sodium bromide (NaBr) is added 40mL deionized water, dissolves to obtain solution B；Solution B is added in solution A, magnetic force stirs
It mixes 20 minutes, is subsequently placed in 90 DEG C of thermostat water baths, react 2 hours；After reaction, cooled to room temperature is filtered, is washed
It washs, dry, grinding to get NiO/BiOBr composite photo-catalyst is arrived.
It is detected through XRD, SEM, the map and micro-structure diagram of NiO/BiOBr composite photo-catalyst made from the present embodiment are equal
It is consistent with embodiment 1.Using the identical method of embodiment 2 to the present embodiment be made NiO/BiOBr composite photo-catalyst with
NiO catalyst, BiOBr catalyst catalytic performance be compared, be as a result consistent with embodiment 2, NiO/BiOBr complex light
The photocatalysis performance of catalyst is substantially better than NiO catalyst, BiOBr catalyst.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered
It is considered as protection scope of the present invention.Structure, device and the operating method for not specifically describing and illustrating in the present invention, such as nothing
It illustrates and limits, implemented according to the conventional means of this field.
Claims (14)
1. a kind of preparation method of dyestuff waste liquid catalysts for treating, including operate as follows:
Nano-nickel oxide is dispersed in bismuth nitrate alcoholic solution and obtains solution A, solution A and solution B Hybrid Heating are reacted, heating
Reaction product is recycled after reaction and carries out removal of impurities and handles obtained NiO/BiOBr composite photo-catalyst, and the solution B is bromine
Change sodium water solution.
2. the preparation method of dyestuff waste liquid catalysts for treating according to claim 1, it is characterised in that: NiO/BiOBr
Composite photo-catalyst is that the granular NiO of area load of BiOBr nanometer sheet is nanocrystalline.
3. the preparation method of dyestuff waste liquid catalysts for treating according to claim 2, it is characterised in that: BiOBr nanometers
The size of piece is 100~300nm, and NiO nanocrystalline size is 20~50nm.
4. the preparation method of dyestuff waste liquid catalysts for treating according to claim 1, it is characterised in that: bismuth nitrate alcohol is molten
Liquid is dissolved in prepare in ethylene glycol by five nitric hydrate bismuths and be obtained.
5. the preparation method of dyestuff waste liquid catalysts for treating according to claim 1, it is characterised in that: solution A and molten
The reaction of liquid B Hybrid Heating is operated using water-bath synthetic method.
6. the preparation method of dyestuff waste liquid catalysts for treating according to claim 1, it is characterised in that: nano-nickel oxide
It is made for nickel nitrate aqueous solution and the reaction of aqueous sodium carbonate Hybrid Heating.
7. the preparation method of dyestuff waste liquid catalysts for treating according to claim 6, it is characterised in that: nickel nitrate is water-soluble
Liquid and aqueous sodium carbonate pass through water-bath synthetic method preparing nano nickel oxide.
8. the preparation method of dyestuff waste liquid catalysts for treating according to claim 1, it is characterised in that: solution A and molten
Liquid B Hybrid Heating recycles reaction product by the way of filtering after reaction, then reaction product washes clean is done
NiO/BiOBr composite photo-catalyst is made in dry and grinding.
9. the preparation method of dyestuff waste liquid catalysts for treating according to claim 1, it is characterised in that: solution A, solution
B is that the progress of 1:1.5~2.5 Hybrid Heating is reacted with the molar ratio of sodium bromide according to bismuth nitrate, according to every 1mmol nitre in solution A
Sour bismuth addition 0.05~0.2g nano-nickel oxide is dispersed.
10. the preparation method of dyestuff waste liquid catalysts for treating according to claim 6, it is characterised in that: nickel nitrate water
Solution, aqueous sodium carbonate are that 1:1.8~2.2 carries out Hybrid Heating reaction according to the molar ratio of nickel nitrate, sodium carbonate.
11. the preparation method of dyestuff waste liquid catalysts for treating according to claim 4, it is characterised in that: bismuth nitrate alcohol
Solution is dissolved in prepare in 20ml ethylene glycol by every five nitric hydrate bismuth of 1mmol and be obtained.
12. the preparation method of dyestuff waste liquid catalysts for treating according to claim 1, it is characterised in that: first by five water
It closes bismuth nitrate and stirring and dissolving in ethylene glycol is added, be then added nano-nickel oxide, ultrasonic disperse 20~40 minutes, obtained solution A；
Sodium bromide is dissolved in deionized water again and obtains solution B；Solution B is added in solution A, magnetic agitation 15~25 minutes, then
It is placed in 90 DEG C of thermostat water baths, reacts 2 hours, after reaction, cooled to room temperature filters recycling reaction product, according to
Ordered pair reaction product is washed, is dried, grinding obtained NiO/BiOBr composite photo-catalyst.
13. the preparation method of dyestuff waste liquid catalysts for treating according to claim 10, it is characterised in that: by six hydrations
Nickel nitrate is dissolved in deionized water, is then added aqueous sodium carbonate, and magnetic agitation 15~25 minutes；Above-mentioned mixed liquor is set
In water-bath, 90 DEG C are reacted 1~3 hour, and cooled to room temperature, filters recycling reaction product, then sequentially after reaction
It washed, dry to obtain nickeliferous sediment, nickeliferous sediment is put into resistance furnace, be heat-treated 1 hour to get nano oxidized
Nickel.
14. a kind of NiO/BiOBr composite photo-catalyst, it is characterised in that: NiO/BiOBr composite photo-catalyst is BiOBr nanometers
The granular NiO of the area load of piece is nanocrystalline.
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