CN109174152A - A kind of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst and preparation method thereof - Google Patents
A kind of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst and preparation method thereof Download PDFInfo
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- CN109174152A CN109174152A CN201811025756.6A CN201811025756A CN109174152A CN 109174152 A CN109174152 A CN 109174152A CN 201811025756 A CN201811025756 A CN 201811025756A CN 109174152 A CN109174152 A CN 109174152A
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- 239000011777 magnesium Substances 0.000 title claims abstract description 46
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052749 magnesium Inorganic materials 0.000 title claims abstract description 20
- 239000003054 catalyst Substances 0.000 title claims abstract description 18
- -1 calcium niobium oxygen nitrogen Chemical compound 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 27
- 230000008569 process Effects 0.000 claims abstract description 11
- 239000003426 co-catalyst Substances 0.000 claims abstract description 10
- 239000004480 active ingredient Substances 0.000 claims abstract description 7
- 238000000975 co-precipitation Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 55
- 238000001354 calcination Methods 0.000 claims description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 15
- ZHJGWYRLJUCMRT-UHFFFAOYSA-N 5-[6-[(4-methylpiperazin-1-yl)methyl]benzimidazol-1-yl]-3-[1-[2-(trifluoromethyl)phenyl]ethoxy]thiophene-2-carboxamide Chemical compound C=1C=CC=C(C(F)(F)F)C=1C(C)OC(=C(S1)C(N)=O)C=C1N(C1=C2)C=NC1=CC=C2CN1CCN(C)CC1 ZHJGWYRLJUCMRT-UHFFFAOYSA-N 0.000 claims description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic acid anhydride Natural products CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims description 12
- UPXYJUPSYMBDCO-UHFFFAOYSA-L magnesium;diacetate;hydrate Chemical compound O.[Mg+2].CC([O-])=O.CC([O-])=O UPXYJUPSYMBDCO-UHFFFAOYSA-L 0.000 claims description 12
- 239000012702 metal oxide precursor Substances 0.000 claims description 11
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 claims description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 108010029541 Laccase Proteins 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229910021529 ammonia Inorganic materials 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 8
- 229910000428 cobalt oxide Inorganic materials 0.000 claims description 8
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 7
- 239000002105 nanoparticle Substances 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000084 colloidal system Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000004176 ammonification Methods 0.000 claims description 4
- 239000001103 potassium chloride Substances 0.000 claims description 4
- 235000011164 potassium chloride Nutrition 0.000 claims description 4
- 229960004543 anhydrous citric acid Drugs 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 claims description 2
- 229960004756 ethanol Drugs 0.000 claims 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims 1
- 150000004706 metal oxides Chemical class 0.000 claims 1
- 150000002927 oxygen compounds Chemical class 0.000 claims 1
- 230000001568 sexual effect Effects 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 75
- 230000001699 photocatalysis Effects 0.000 abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 12
- 230000015556 catabolic process Effects 0.000 abstract description 12
- 238000006731 degradation reaction Methods 0.000 abstract description 12
- 239000001257 hydrogen Substances 0.000 abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000000354 decomposition reaction Methods 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 description 10
- 239000010955 niobium Substances 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 230000008859 change Effects 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 229910017052 cobalt Inorganic materials 0.000 description 3
- 239000010941 cobalt Substances 0.000 description 3
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 2
- 239000011654 magnesium acetate Substances 0.000 description 2
- 235000011285 magnesium acetate Nutrition 0.000 description 2
- 229940069446 magnesium acetate Drugs 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 201000004624 Dermatitis Diseases 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Classifications
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J27/24—Nitrogen compounds
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention relates to a kind of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst and preparation method thereof, photocatalyst catalyst includes active ingredient and co-catalyst, and the molecular formula of the active ingredient is CaNb1‑ xMgxO2+yN1‑y, wherein 0≤x, y≤1, synthetic method have: sol-gal process, PC method, coprecipitation, molte-salt synthesis, the above method can obtain CaNb1‑xMgxO2+yN1‑yPure phase sample, and the difference of the amount with magnesium doping, its visible absorption CaNb continuously adjustable at 550 nanometers to 600 nanometers, prepared1‑xMgxO2+yN1‑yAfter supporting suitable co-catalyst, excellent photocatalytic hydrogen production by water decomposition and degradation of formaldehyde performance are shown.
Description
Technical field
The invention belongs to nano-photocatalyst material technical fields, and in particular to a kind of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalysis
Agent and preparation method thereof.
Background technique
With the high speed development of global economy, human society is higher and higher to the desirability of the energy, and is used as energy now
The fossil fuel of source main body will be depleted in centuries, and the toxic and harmful gas discharged after its burning can bring greenhouse to imitate
It answers, the serious environmental problem such as acid rain, haze.In order to solve the energy crisis got worse and environmental problem, exploitation finds one
Kind new green energy is just particularly important.
Solar energy is a kind of inexhaustible, nexhaustible renewable and clean energy resource, it is reported that: the sun can also be held
Afterflame is burnt 5,000,000,000 years, and one hour energy for arriving at earth surface just can satisfy mankind's energy demand in 1 year.However, the sun
Energy energy density is low, is easy to receive the influence such as region, weather and day-night change and make it using there are unstability and interval
The shortcomings that property, utilization rate is caused to substantially reduce.Nowadays, there are three types of the principal modes for developing solar energy: (1) it is converted into thermal energy,
Such as common solar cooker, water heater；(2) it is converted into electric energy, such as present photovoltaic power generation；(3) it is converted into chemical energy, as light is urged
Change water decomposition hydrogen manufacturing, photocatalysis fixed nitrogen etc..Hydrogen is a kind of ideal clean energy resource, and the heat for release of burning is high, combustion
Burning product is water, without any pollution.Therefore, solar energy photocatalytic water decomposition hydrogen manufacturing (H is carried out using photocatalyst2O→H2+O2)
It is a kind of ideal energy conversion exploitation mode, chemical energy can be converted by dispersion, discontinuous solar energy
(H2) stored utilization.
Photocatalyst not only can have good performance in solar energy water decomposing hydrogen-production, also have in terms of degradable organic pollutant
Huge application value.Now, indoor hardware fitting and furniture more or less all can the pernicious gases such as release formaldehyde, especially
In closed space environment, formaldehyde pollution is especially huge to human injury.According to relevant regulations, indoor formaldehyde content cannot surpass
Cross 0.08mg/m3, the formaldehyde of high concentration can cause eye, throat discomfort, uncomfortable in chest, asthma, dermatitis etc., or even there are also carcinogenic wind
Danger.In order to solve the problems, such as formaldehyde pollution, many purification methods of degrading are suggested, such as microbial degradation method, plant purification, chemistry
Reaction method, physisorphtion, nano photo catalyzed oxidation etc..Compared to other methods, nano photo catalyzed oxidation is because of its safety, height
Effect, energy consumption are small and become the hot spot of the area research.
Chinese patent CN 106390740A discloses a kind of formaldehyde degradation by photocatalytic oxidation process film, by nanoscale catalysis material
TiO2It is added to automobile film in a certain way, building film, in household film hard conating, ensure that the original performance of product, neither change
Become hardness, the scratch resistance performance of former film hard conating, transmitance etc., and increase the function of degradation of formaldehyde, wherein TiO2It is a kind of normal
The photocatalyst material seen, but TiO2Ultraviolet light is only responded, photocatalysis efficiency not high to light utilization efficiency visible in sunlight
It is lower.Another common photocatalyst CdS (The Journal of Physical Chemistry C, 115 (2011)
11466-11473) then because material stability itself is bad, easily generation self-corrosion, and dirt easily is caused to environment containing toxic metals
Dye, so nor ideal.
Summary of the invention
The purpose of the present invention is to solve the above-mentioned problems and provides a kind of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst
And preparation method thereof.
The purpose of the present invention is achieved through the following technical solutions:
A kind of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst, including active ingredient and co-catalyst, the active ingredient
Molecular formula is CaNb1-xMgxO2+yN1-y, wherein 0≤x, y≤1.
Further, the co-catalyst is selected from one of cobalt oxide, Platinum Nanoparticles or nano silver or a variety of.
Further, the photocatalyst catalyst loading laccase.
A kind of preparation method of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst, the active ingredient are straight by melting raw material
It connects ammonification to be prepared, or first passes through sol-gal process, PC method or coprecipitation and metal oxide precursor is prepared, then
Calcination is prepared under ammonia atmosphere protection, calcination temperature 1023K, and the time is 5 hours.
Further, raw material melts direct ammonification preparation method particularly includes: by potassium chloride, calcium nitrate tetrahydrate, four water
Magnesium acetate and five two girls of oxidation are closed by metering than being uniformly mixed, the calcination under ammonia atmosphere protection, gained powder is washed with deionized water
It washs, dry, calcination temperature 1023K, the time is 5 hours.
Further, the sol-gal process specific steps are as follows:
(1) under conditions of temperature is 298K, acetic acid and acetic anhydride is mixed, S1 is obtained, by columbium pentachloride and anhydrous second
Alcohol mixing, is made S2, solution S 1 is mixed, and be vigorously stirred with solution S 2, obtain mixed solution S3；
(2) calcium nitrate tetrahydrate, four acetate hydrate magnesium are added mixed solution S3, and are vigorously stirred, until solution is clarified,
Obtain solution S 4；
(3) solution S 4 is placed in baking oven, keeps the temperature 2-72 hours under the conditions of 323K, obtains white precipitate P1, white
Precipitating P1, which is filtered under the conditions of 323K and kept the temperature 12-72 hours, to be placed under the conditions of inert atmosphere protection in 523K-623K calcination
3-8 hours, continue to obtain metal oxide precursor at 873K-973K calcination 5-24 hours under oxygen protection.
Further, the PC method specific steps are as follows:
(1) under conditions of temperature is 298K, anhydrous citric acid is dissolved into ethylene glycol and is stirred, clear solution is obtained
Columbium pentachloride is dissolved into ethyl alcohol by S1, obtains clear solution S2, and by solution S 2, calcium nitrate tetrahydrate, four acetate hydrate magnesium add
Enter and stirred in solution S 1, obtains clear solution S3；
(2) solution S 3 is continuously heating to 473K-523K under agitation, until become brownish red clear solution S4, temperature
Degree is further increased to 563K-583K, and brownish red clear solution S4 polymerize to form brownish red colloid G1；
(3) in air atmosphere, colloid G1 is placed in Muffle furnace under the conditions of 873-923K calcination 5-24 hours, obtains gold
Belong to oxide precursor.
Further, the coprecipitation specific steps are as follows: under conditions of 298K, by calcium nitrate tetrahydrate, four hydrations
Magnesium acetate and the dissolution of columbium pentachloride ethanol solution obtain clear solution S1 in deionized water, and sodium hydroxide is dissolved in deionization
In water, clear solution S2 is obtained, S2 solution is added drop-wise in the S1 solution of stirring, rate of addition is 35-45 drop per minute, from opening
Beginning is added drop-wise to end stirring, and the whole process time is 6 hours, and product is flocculent white oxide, is washed with deionized water to pH value
It for neutrality, is placed in baking oven, obtains metal oxide precursor.
Active component supported co-catalyst (cobalt oxide, Platinum Nanoparticles, nano silver) promotes the separation of light induced electron, hole, mentions
High photocatalysis performance.Wherein support cobalt oxide, Platinum Nanoparticles form photolysis water hydrogen photocatalyst；Support cobalt oxide, nano silver is formed
Degradation of formaldehyde photocatalyst；Support the coating crystallized ability that laccase increases photocatalyst.
Compared with prior art, the invention has the following advantages that photocatalysis photocatalyst provided by the invention, active constituent are
CaNb1-xMgxO2+yN1-y, with the difference of the amount of magnesium doping, its visible absorption continuously may be used at 550 nanometers to 600 nanometers
It adjusts, the photocatalyst prepared by different synthetic methods shows excellent sunlight photocatalysis after supporting suitable co-catalyst
Water decomposition hydrogen manufacturing and light degradation formaldehyde ability, in terms of photocatalytic water splitting hydrogen manufacturing and degradation of formaldehyde, effect is good.
The present invention mainly utilizes itself high efficiency photocatalysis activity of photocatalyst activity material effectively to convert indoor organic pollutant
Formaldehyde, active material used have very excellent visible light absorption capacity, and it is anti-can to efficiently use sunlight progress photocatalysis
It answers, remove formaldehyde products (active carbon etc.) from market mainstream has essence different by Adsorption formaldehyde.The invention patent it is excellent
Gesture is effectively to convert formaldehyde pollutants, and reducing concentration of formaldehyde not by adsorption effect, (later period is easy two
Secondary release formaldehyde).
Detailed description of the invention
Fig. 1 is that PC method prepares CaNb1-xMgxO2+yN1-yThe relationship of (wherein, 0≤x, y≤1) absorptance and x.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
Embodiment 1-5
CaNb is prepared using sol-gal process1-xMgxO2+yN1-y
Using sol-gal process according to the different Nb/Mg proportion preparation CaNb in table 11-xMgxO2+yN1-yAnd carry out performance survey
Examination.Under conditions of temperature is 298K, acetic acid and acetic anhydride are mixed, clear solution S1 is obtained；By columbium pentachloride and anhydrous second
Alcohol mixing, is made clear solution S2；Solution S 1 is mixed with solution S 2, and is vigorously stirred, mixed solution S3 is obtained；By four hydrations
Calcium nitrate, mixed solution S3 is added in four acetate hydrate magnesium, and is vigorously stirred, until solution is clarified, is labeled as solution S 4；By solution
S4 is placed in baking oven, is kept the temperature 2-72 hours under the conditions of 323K, is obtained white precipitate P1；White precipitate P1 is under the conditions of 323K
It filters and keeps the temperature 12-72 hours and be placed under inert atmosphere (nitrogen or argon gas) protective condition and is small at 523K-623K calcination 3-8
When, continue to obtain white powder P2 (metallic oxide precursor in 5-24 hour of 873K-973K calcination under oxygen protection
Body)；Preparation gained metal oxide precursor powder is placed in alumina crucible, under ammonia atmosphere protection, in 1023K calcination
5 hours, obtain CaNb1-xMgxO2+yN1-yNitrogen oxides powder.
Supported co-catalyst cobalt oxide, Platinum Nanoparticles form sunlight photocatalysis water decomposition hydrogen manufacturing photocatalyst preparation；Support oxygen
Change cobalt, nano silver and laccase form light degradation formaldehyde photocatalyst preparation, the photocatalytic water performance and according to GB/ under the conditions of AM 1.5G
Formaldehyde performance is gone in T16129 detection, as shown in table 2.
1 embodiment 1-5 difference Nb/Mg raw material proportioning of table
2 embodiment 1-5 photocatalytic water performance of table and go formaldehyde performance
Embodiment 6-10
CaNb is prepared using PC method1-xMgxO2+yN1-y
Using sol-gal process according to the different Nb/Mg proportion preparation CaNb in table 31-xMgxO2+yN1-yAnd carry out performance survey
Examination.Under conditions of temperature is 298K, 7.8g anhydrous citric acid is dissolved into 30mL ethylene glycol, stirs 30 minutes, obtains
Bright solution S 1；Columbium pentachloride is dissolved into ethyl alcohol, clear solution S2 is obtained；By solution S 2, calcium nitrate tetrahydrate, four hydration second
Sour magnesium is added in solution S 1, continues stirring 30 minutes, obtains clear solution S3；Solution S 3 is continuously heating under stirring conditions
473K-523K, until becoming brownish red clear solution S4；Stop stirring, temperature is further increased to 563K-583K, and brownish red is saturating
Further polymerization forms brownish red colloid G1 to bright solution S 4；In air atmosphere, colloid G1 is placed in Muffle furnace in 873-923K
Under the conditions of calcination 5-24 hours, obtain white powder P1 (metal oxide precursor)；Preparation gained metal oxide precursor
Powder is placed in alumina crucible, under ammonia atmosphere protection, in 5 hours of 1023K calcination, obtains CaNb1-xMgxO2+yN1-y
Nitrogen oxides powder.
Supported co-catalyst cobalt oxide, Platinum Nanoparticles form sunlight photocatalysis water decomposition hydrogen manufacturing photocatalyst preparation；Support oxygen
Change cobalt, nano silver and laccase and forms light degradation formaldehyde photocatalyst preparation.Test its photocatalytic water splitting hydrogen manufacturing and light degradation formaldehyde
Performance, under the conditions of AM 1.5G photocatalytic water performance and according to GB/T16129 detection go formaldehyde performance, as shown in table 4.
3 embodiment 6-10 difference Nb/Mg raw material proportioning of table
| Reagent name | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 |
| x | 0.05 | 0.10 | 0.15 | 0.20 | 0.10 |
| Calcium nitrate tetrahydrate | 45.49 | 45.74 | 46.00 | 46.26 | 45.74 |
| Four acetate hydrate magnesium | 2.07 | 4.16 | 6.27 | 8.40 | 4.16 |
| Columbium pentachloride | 49.44 | 47.10 | 44.73 | 42.34 | 47.10 |
| Chloroplatinic acid | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 |
| Cobalt nitrate | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 |
| Silver nitrate | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 |
| Laccase | 0.00 | 0.00 | 0.00 | 0.00 | 0.50 |
4 embodiment 6-10 photocatalytic water performance of table and go formaldehyde performance
Embodiment 11-15
Coprecipitation prepares CaNb1-xMgxO2+yN1-y
Using coprecipitation according to the different Nb/Mg proportion preparation CaNb in table 51-xMgxO2+yN1-yAnd carry out performance survey
Examination.In temperature under conditions of 298K, by calcium nitrate tetrahydrate, four acetate hydrate magnesium and columbium pentachloride ethanol solution are dissolved in
Clear solution S1 is obtained in 100mL deionized water；The sodium hydroxide of 20g is dissolved in 100mL deionized water, is obtained transparent molten
Liquid S2；S2 solution is added drop-wise to dropwise in the S1 solution of stirring, rate of addition is 40 drop per minute left and right, from starting to be added drop-wise to knot
Beam stirring, whole process time are 6 hours, and product is flocculent white oxide, and being washed with deionized water to pH value is neutrality, are placed in
In baking oven, powder P1 (metal oxide precursor) is obtained；Preparation gained metal oxide precursor powder is placed in aluminium oxide
In crucible, under ammonia atmosphere protection, in 5 hours of 1023K calcination, CaNb is obtained1-xMgxO2+yN1-yNitrogen oxides powder.
Supported co-catalyst cobalt oxide, Platinum Nanoparticles form sunlight photocatalysis water decomposition hydrogen manufacturing photocatalyst preparation；Support oxygen
Change cobalt, nano silver and laccase and forms light degradation formaldehyde photocatalyst preparation.Test its photocatalytic water splitting hydrogen manufacturing and light degradation formaldehyde
Performance, as shown in table 6.
5 embodiment 11-15 difference Nb/Mg raw material proportioning of table
| Reagent name | Embodiment 11 | Embodiment 12 | Embodiment 13 | Embodiment 14 | Embodiment 15 |
| x | 0.05 | 0.10 | 0.15 | 0.20 | 0.10 |
| Calcium nitrate tetrahydrate | 45.49 | 45.74 | 46.00 | 46.26 | 45.74 |
| Four acetate hydrate magnesium | 2.07 | 4.16 | 6.27 | 8.40 | 4.16 |
| Columbium pentachloride | 49.44 | 47.10 | 44.73 | 42.34 | 47.10 |
| Chloroplatinic acid | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 |
| Cobalt nitrate | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 |
| Silver nitrate | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 |
| Laccase | 0.00 | 0.00 | 0.00 | 0.00 | 0.50 |
6 embodiment 11-15 photocatalytic water performance of table and go formaldehyde performance
Embodiment 16-20
Molte-salt synthesis prepares CaNb1-xMgxO2+yN1-y
Using molte-salt synthesis according to the different Nb/Mg proportion preparation CaNb in table 71-xMgxO2+yN1-yAnd carry out performance survey
Examination.In temperature under conditions of 298K, by potassium chloride, calcium nitrate tetrahydrate, four acetate hydrate magnesium, five two girls of oxidation by metering ratio
Mixing is placed in mortar to be ground to and be sufficiently mixed uniformly, and mixed powder is placed in alumina crucible, under ammonia atmosphere protection,
In 5 hours of 1023K calcination, gained powder is washed with deionized 5~6 times, and drying obtains nitrogen oxides powder, in AM
Under the conditions of 1.5G photocatalytic water performance and according to GB/T16129 detection go formaldehyde performance, as shown in table 8.
7 embodiment 16-20 difference Nb/Mg raw material proportioning of table
| Reagent name | Embodiment 16 | Embodiment 17 | Embodiment 18 | Embodiment 19 | Embodiment 20 |
| x | 0.05 | 0.10 | 0.15 | 0.20 | 0.10 |
| Calcium nitrate tetrahydrate | 30.74 | 30.36 | 30.04 | 29.73 | 30.36 |
| Four acetate hydrate magnesium | 1.33 | 2.76 | 3.38 | 4.44 | 2.76 |
| Niobium pentaoxide | 16.43 | 15.38 | 15.08 | 14.33 | 15.38 |
| Potassium chloride | 48.5 | 48.5 | 48.5 | 48.5 | 48.5 |
| Chloroplatinic acid | 1.00 | 1.00 | 1.00 | 1.00 | 1.00 |
| Cobalt nitrate | 2.00 | 2.00 | 2.00 | 2.00 | 2.00 |
| Silver nitrate | 0.00 | 0.00 | 0.00 | 0.00 | 0.00 |
| Laccase | 0.00 | 0.00 | 0.00 | 0.00 | 0.50 |
8 embodiment 16-20 photocatalytic water performance of table and go formaldehyde performance
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. a kind of magnesium adulterates calcium niobium oxygen nitrogen photocatalyst catalyst, which is characterized in that including active ingredient and co-catalyst, the work
The molecular formula of sexual element is CaNb1-xMgxO2+yN1-y, wherein 0≤x, y≤1.
2. a kind of magnesium according to claim 1 adulterates calcium niobium oxygen nitrogen photocatalyst catalyst, which is characterized in that the co-catalysis
Agent is selected from one of cobalt oxide, Platinum Nanoparticles or nano silver or a variety of.
3. a kind of magnesium according to claim 1 adulterates calcium niobium oxygen nitrogen photocatalyst catalyst, which is characterized in that the photocatalyst is urged
Agent supports laccase.
4. a kind of preparation method of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst as described in any one of claims 1-3, special
Sign is that the active ingredient is prepared by the way that raw material is melted direct ammonification, or first pass through sol-gal process, PC method or
Metal oxide precursor is prepared in coprecipitation, then calcination is prepared under ammonia atmosphere protection.
5. a kind of preparation method of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst according to claim 4, which is characterized in that
Raw material is melted into direct ammonification preparation, method particularly includes: by potassium chloride, calcium nitrate tetrahydrate, four acetate hydrate magnesium and five oxidations
By metering than being uniformly mixed, the calcination under ammonia atmosphere protection, gained powder is washed with deionized, dries two girls.
6. a kind of preparation method of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst according to claim 5, which is characterized in that
Calcination temperature is 1023K under ammonia atmosphere protection, and the time is 5 hours.
7. a kind of preparation method of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst according to claim 4, which is characterized in that
The sol-gal process specific steps are as follows:
(1) under conditions of temperature is 298K, acetic acid and acetic anhydride is mixed, S1 is obtained, columbium pentachloride and dehydrated alcohol is mixed
It closes, S2 is made, solution S 1 is mixed, and be vigorously stirred with solution S 2, obtains mixed solution S3；
(2) calcium nitrate tetrahydrate, four acetate hydrate magnesium are added mixed solution S3, and are vigorously stirred, until solution is clarified, obtained
Solution S 4；
(3) solution S 4 is placed in baking oven, keeps the temperature 2-72 hours under the conditions of 323K, obtains white precipitate P1, white precipitate
P1 is filtered under the conditions of 323K and is kept the temperature 12-72 hours and be placed on and is small in 523K-623K calcination 3-8 under the conditions of inert atmosphere protection
When, continue to obtain metal oxide precursor at 873K-973K calcination 5-24 hours under oxygen protection.
8. a kind of preparation method of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst according to claim 4, which is characterized in that
The PC method specific steps are as follows:
(1) under conditions of temperature is 298K, anhydrous citric acid is dissolved into ethylene glycol and is stirred, clear solution S1 is obtained, it will
Columbium pentachloride is dissolved into ethyl alcohol, obtains clear solution S2, and by solution S 2, calcium nitrate tetrahydrate, four acetate hydrate magnesium are added molten
It is stirred in liquid S1, obtains clear solution S3；
(2) solution S 3 is continuously heating to 473K-523K under agitation, until become brownish red clear solution S4, temperature into
One step rises to 563K-583K, and brownish red clear solution S4 polymerize to form brownish red colloid G1；
(3) in air atmosphere, colloid G1 is placed in Muffle furnace under the conditions of 873-923K calcination 5-24 hours, obtains metal oxygen
Compound presoma.
9. a kind of preparation method of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst according to claim 4, which is characterized in that
The coprecipitation specific steps are as follows:
Under conditions of 298K, by calcium nitrate tetrahydrate, four acetate hydrate magnesium and columbium pentachloride ethanol solution are dissolved in deionization
Clear solution S1 is obtained in water, in deionized water by sodium hydroxide dissolution, obtains clear solution S2, S2 solution is added drop-wise to and is stirred
In the S1 solution mixed, rate of addition is 35-45 drop per minute, terminates stirring from starting to be added drop-wise to, the whole process time is 6 small
When, product is flocculent white oxide, and being washed with deionized water to pH value is neutrality, is placed in baking oven, before obtaining metal oxide
Drive body.
10. a kind of preparation method of magnesium doping calcium niobium oxygen nitrogen photocatalyst catalyst according to claim 4, feature exist
In metal oxide precursor obtains nitrogen oxides powder in 5 hours of 1023K calcination.
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