CN106345484A - Selective composite photo-catalyst powder and preparation method and application thereof - Google Patents
Selective composite photo-catalyst powder and preparation method and application thereof Download PDFInfo
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- CN106345484A CN106345484A CN201610986448.4A CN201610986448A CN106345484A CN 106345484 A CN106345484 A CN 106345484A CN 201610986448 A CN201610986448 A CN 201610986448A CN 106345484 A CN106345484 A CN 106345484A
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- 239000000843 powder Substances 0.000 title claims abstract description 102
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012153 distilled water Substances 0.000 claims abstract description 24
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical class [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 18
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 13
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 13
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 13
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 claims abstract description 11
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 11
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 10
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical class [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 8
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical class [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 7
- 239000010842 industrial wastewater Substances 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 150000003839 salts Chemical class 0.000 claims abstract 5
- 238000000034 method Methods 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000005516 engineering process Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000000875 high-speed ball milling Methods 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 6
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 230000014759 maintenance of location Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims 1
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 229910052750 molybdenum Inorganic materials 0.000 claims 1
- 239000011733 molybdenum Substances 0.000 claims 1
- 150000002815 nickel Chemical class 0.000 claims 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims 1
- 229910001948 sodium oxide Inorganic materials 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 11
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 238000000498 ball milling Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 229910002221 La2NiO4 Inorganic materials 0.000 abstract 2
- 238000005303 weighing Methods 0.000 abstract 2
- 239000002244 precipitate Substances 0.000 abstract 1
- 238000000967 suction filtration Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 58
- 238000009413 insulation Methods 0.000 description 12
- 238000001802 infusion Methods 0.000 description 10
- 238000005286 illumination Methods 0.000 description 6
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 5
- 229940078494 nickel acetate Drugs 0.000 description 5
- JNRLEMMIVRBKJE-UHFFFAOYSA-N 4,4'-Methylenebis(N,N-dimethylaniline) Chemical group C1=CC(N(C)C)=CC=C1CC1=CC=C(N(C)C)C=C1 JNRLEMMIVRBKJE-UHFFFAOYSA-N 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 description 4
- 241001062009 Indigofera Species 0.000 description 3
- 229910009440 Y2(CO3)3 Inorganic materials 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- QVOIJBIQBYRBCF-UHFFFAOYSA-H yttrium(3+);tricarbonate Chemical compound [Y+3].[Y+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O QVOIJBIQBYRBCF-UHFFFAOYSA-H 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- DUSUCKWNBGMKRV-UHFFFAOYSA-N acetic acid;yttrium Chemical compound [Y].CC(O)=O DUSUCKWNBGMKRV-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- JLRJWBUSTKIQQH-UHFFFAOYSA-K lanthanum(3+);triacetate Chemical compound [La+3].CC([O-])=O.CC([O-])=O.CC([O-])=O JLRJWBUSTKIQQH-UHFFFAOYSA-K 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- BXJPTTGFESFXJU-UHFFFAOYSA-N yttrium(3+);trinitrate Chemical compound [Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O BXJPTTGFESFXJU-UHFFFAOYSA-N 0.000 description 2
- 229910017569 La2(CO3)3 Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- NZPIUJUFIFZSPW-UHFFFAOYSA-H lanthanum carbonate Chemical compound [La+3].[La+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O NZPIUJUFIFZSPW-UHFFFAOYSA-H 0.000 description 1
- 229960001633 lanthanum carbonate Drugs 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 1
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 1
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000957 no side effect Toxicity 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000007704 transition Effects 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/887—Molybdenum containing in addition other metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8871—Rare earth metals or actinides
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The invention belongs to the technical field of photo-catalysts and composite adsorbing materials and in particular relates to selective composite photo-catalyst powder and a preparation method and application thereof. The chemical formula of the composite photo-catalyst powder is La2NiO4/Y2Mo4O15. The preparation method comprises the following steps: weighing soluble salts of nickel and soluble salts of lanthanum according to a molar ratio of 1 to 2, dissolving the salts in distilled water, thereby obtaining a solution A; slowly adding a sodium hydroxide solution, stirring, performing suction filtration on the solution, thereby obtaining a precipitate B; calcining and maintaining the temperature in a muffle furnace, thereby obtaining catalyst powder C; adding the powder C into an alcoholic solution, performing ball milling at high speed, thereby obtaining powder D (La2NiO4); weighing a proper amount of soluble salts of yttrium, measuring a certain amount of ammonium molybdate, dissolving in a proper amount of distilled water, thereby obtaining a solution E; and mixing the solution E and the powder D, drying, calcining, thereby obtaining the composite catalyst powder. The composite photo-catalyst powder can be used in degradation treatment of insoluble organic matters in industrial wastewater and particularly has an obvious catalytic degradation effect on methylene blue.
Description
Technical field
The invention belongs to photocatalyst and composite adsorbing material technical field, more particularly, to a kind of selectivity composite photocatalyst
Agent powder body and its preparation method and application.
Background technology
Light-catalyzed reaction, refers to be catalyzed the generation of certain reaction under conditions of by natural light.Photocatalysis are to utilize nature
Boundary exist known luminaire, irradiate certain catalyst, through electron transition etc. a series of change after, by the luminous energy in nature
It is transformed into the chemical energy required for chemical reaction, thus producing catalytic action.
Nickel acid lanthanum is a kind of functional material of extensive application prospect, generally to be made using coprecipitation and reducing process
Standby.Coprecipitation, the metal salt solution containing different component is carried out mixed dissolution, then is aided with suitable precipitant, fully molten
Mix after solution, generate precipitation, form suspension；Carry out sucking filtration, the method finally obtaining filter cake after stirring；Coprecipitation is adding
When entering precipitant, the concentration of local may be made to be significantly larger than other parts, easily producing reunites makes composition uneven.Reduction
Method, the slaine of several difference constituent elements is dissolved, mixing, adds certain complexant, then add appropriate water；?
Carry out heating in water bath under certain condition, after amount of solution is reduced to certain, put into drying baker, after being fully dried, obtain similar glue
The material of body, is then sintered, finally in the medium equipment of stove with non-oxidizing atmosphere (such as ammonia stove, nitrogen furnace etc.)
Obtain related powder；Reducing process reducibility gas to be ensured in sintering process are unimpeded always, and necessary tracking reaction process, consumption
When laborious；And long with the sintering period, cooling rate is slow, and reducibility gas are usually pollution gas, cause environmental pollution.
In sum, study a kind of preparation method simple, effective, the high photocatalyst of catalysis activity, it appears particularly necessary.
Content of the invention
The deficiency existing for above-mentioned technology, the present invention provides a kind of new selective composite photo-catalyst powder body and its system
Preparation Method.This catalyst is composite catalyst, can achieve the maximization effect of two kinds of powder body functions, has catalysis activity height,
Preparation method is simple, can be used in the degradation treatment of insoluble organic in industrial wastewater.
To achieve these goals, the present invention provides a kind of new selective composite photo-catalyst powder body, described photocatalysis
The chemical formula of agent is: la2nio4/y2mo4o15.
To achieve these goals, the present invention also provides a kind of infusion process to prepare above-mentioned composite photo-catalyst powder body, including
Following steps.
(1) weigh the soluble-salt of nickel, the soluble-salt of lanthanum according to mol ratio 1:2, be dissolved in appropriate distilled water, obtain molten
Liquid a.
(2) it is slowly added to sodium hydroxide solution in solution a, adjustment ph value is 9.5-10.5, stirring a period of time, subsequently
Solution is carried out sucking filtration, is precipitated b.
(3) b will be precipitated to calcine in Muffle furnace, be incubated, obtain catalyst powder c.
(4) powder body c is put in alcoholic solution, for a period of time, diameter of particle is 1 μm -2 μm to high speed ball milling, dries, obtains powder
Body d (i.e. la2nio4).
(5) soluble-salt of appropriate yttrium, the ammonium molybdate ((nh of measured amounts are weighed respectively4)6mo7o24·4h2O), dissolve
In appropriate distilled water, mix homogeneously, obtain solution e.
(6) solution e is mixed with powder body d, dry a period of time in an oven, be ground to diameter of particle and be 1 μm -2 μm, put
Enter calcining a period of time in Muffle furnace, take out, obtain composite catalyst powder body.
The soluble-salt of described nickel is one or more of nitrate, carbonate or acetate；The soluble-salt of lanthanum
For one or more of nitrate, carbonate or acetate；In the soluble-salt nitrate of yttrium, carbonate or acetate one
Plant or several.
In described step (1), the volumetric usage of distilled water is the soluble-salt of nickel, the soluble-salt integral molar quantity of lanthanum
20-40 times.
In described step (2), the concentration of sodium hydroxide is 1/300-1/500mol l-1；Described stirring is stirred for magnetic force
Mix or mechanical agitation, revolution is 500-800r/min, mixing time is 1-2h.
In described step (3), the calcining heat of Muffle furnace is 750-900 DEG C, and temperature retention time is 1-3h.
In described step (4), alcoholic solution is one kind of the solubility alcoholic solution such as methanol or ethanol；The volumetric usage of alcoholic solution
5-10 times of the soluble-salt integral molar quantity of the soluble-salt for nickel and lanthanum；Described drying temperature is 40-90 DEG C, and the time is
30-90min.
In described step (5), the volumetric usage of distilled water is the soluble-salt of yttrium and the 20-40 of ammonium molybdate integral molar quantity
Times.
The soluble-salt of described yttrium is 1:2 with the y in ammonium molybdate with mo mol ratio.
In described step (6), drying temperature is 60-90 DEG C, and the time is 1-3h, and Muffle furnace calcining heat is 500-650 DEG C,
Insulation 1-2h.
Described composite granule can be used for the degradation treatment of insoluble organic in industrial wastewater；Described Organic substance is methylene
Base is blue.
Beneficial effects of the present invention.
The infusion process that the present invention provides prepares a kind of new selective composite photo-catalyst powder body la2nio4/y2mo4o15Multiple
Mould assembly photocatalyst, the purity of this photocatalyst is high, stable chemical nature, and photocatalytic activity is high, safety non-toxic, has no side effect,
Long service life.Powder granularity is uniform in size, grain shape is regular.Preparation method-the infusion process of photocatalyst of the present invention is one
Plant the better method preparing composite, powder body mixing can be made to be more uniformly distributed, be more likely formed cladded type composite, and prepare bar
Part is gently controlled, low cost, suitable large-scale production.Can be used in the degradation treatment of insoluble organic in industrial wastewater, especially
It is notable to methylene blue catalytic degradation effect.
Brief description
Fig. 1 is la of the present invention2nio4The xrd figure of photocatalyst；Wherein la under a-800 degree2nio4Powder body xrd collection of illustrative plates, b-
900 degree of lower la2nio4Powder body xrd collection of illustrative plates.
Fig. 2 is y of the present invention2mo4o15The xrd figure of photocatalyst；Wherein y under a-500 degree2mo4o15Powder body xrd collection of illustrative plates, b-
600 degree of lower y2mo4o15Powder body xrd collection of illustrative plates.
Fig. 3 is the la of the present invention2nio4/ y2mo4o15The sem figure of photocatalyst powder body；Under wherein 3-1 is 850 degree
la2nio4The sem figure of photocatalyst powder body, 3-2 is 500 degree of lower y2mo4o15The sem figure of photocatalyst powder body, 3-3 is complex light
The sem figure of catalyst powder.
Fig. 4 is la2nio4/y2mo4o15Photocatalyst changes over to the catalytic effect of methylene blue composite photo-catalyst
Figure；Wherein 1- does not add catalyst of the present invention, and 2- adds embodiment 5 catalyst illumination 20min catalytic effect figure.
Fig. 5 is la2nio4/y2mo4o15Photocatalyst changes over to the catalytic effect of methylene blue composite photo-catalyst
Figure；Wherein 1- does not add catalyst of the present invention, and 2- adds embodiment 6 catalyst illumination 40min catalytic effect figure.
Fig. 6 is la2nio4/y2mo4o15Photocatalyst changes over to the catalytic effect of methylene blue composite photo-catalyst
Figure；Wherein 1- does not add catalyst of the present invention, and 2- adds embodiment 7 catalyst illumination 60min catalytic effect figure.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1.
Infusion process prepares new selective composite photo-catalyst powder body la2nio4/y2mo4o15, comprise the following steps: weigh
1mmol nickel acetate, 2mmol lanthanum acetate, are dissolved in 60ml distilled water, obtain solution a；Being slowly added to concentration in solution a is 1/
The sodium hydroxide solution of 300mol l-1, adjustment solution ph is 10, stirs 1h, and revolution is 500r/min, subsequently enters solution
Row sucking filtration, is precipitated b；B will be precipitated and calcine 800 DEG C, insulation 1h in Muffle furnace, obtain catalyst powder c；Powder body c is put
Enter in 30ml dehydrated alcohol, high speed ball milling, ball mill revolution is 2000r/min, ball milling 2h, and drying temperature is 40 DEG C, and the time is
90min, obtains powder body d；Weigh 1mmol acetic acid yttrium, weigh 2mmol ammonium molybdate, be dissolved in the distilled water of 60ml, obtain solution e；
Solution e is mixed with powder body d, puts in 60 DEG C of baking ovens, dry 3h, grind, put in Muffle furnace and calcine 500 DEG C, be incubated 1h, take
Go out, obtain composite catalyst powder body.
Embodiment 2.
Infusion process prepares new selective composite photo-catalyst powder body la2nio4/y2mo4o15, comprise the following steps: weigh
2mmol nickel acetate, 4mmol lanthanum acetate, are dissolved in 120ml distilled water, obtain solution a；Being slowly added to concentration in solution a is 1/
300mol l-1 sodium hydroxide solution, stir 1.5h, revolution be 800r/min, subsequently solution is carried out sucking filtration, is sunk
Shallow lake b；B will be precipitated and calcine 900 DEG C, insulation 1.5h in Muffle furnace, obtain catalyst powder c；Powder body c is put into the anhydrous second of 40ml
In alcohol, high speed ball milling, ball mill revolution is 4000r/min, ball milling 4h, and drying temperature is 90 DEG C, and the time is 30min, obtains powder
Body d；Weigh 1mmol Yttrium trinitrate, 2mmol ammonium molybdate, be dissolved in the distilled water of 60ml, obtain solution e；Solution e is mixed with powder body d
Close, put in 70 DEG C of baking ovens, dry 1.5h, grind, put in Muffle furnace and calcine 500 DEG C, be incubated 1h, take out, obtain compound urging
Agent powder body.
Embodiment 3.
Infusion process prepares new selective composite photo-catalyst powder body la2nio4/y2mo4o15, comprise the following steps: weigh
2mmol nickel acetate, 4mmol Lanthanum (III) nitrate, are dissolved in 120ml distilled water, obtain solution a；Being slowly added to concentration in solution a is 1/
400mol l-1 sodium hydroxide solution, adjustment ph value be 9.5, stir 2h, revolution be 700r/min, subsequently solution is entered
Row sucking filtration, is precipitated b；B will be precipitated and calcine 850 DEG C, insulation 2h in Muffle furnace, obtain catalyst powder c；Powder body c is put
Enter in 30ml methanol, high speed ball milling, ball mill revolution is 3000r/min, ball milling 4h, and drying temperature is 50 DEG C, and the time is
75min, obtains powder body d；Weigh 2mmol Yttrium trinitrate, weigh 4mmol ammonium molybdate, be dissolved in the distilled water of 120ml, obtain solution
e；Solution e is mixed with powder body d, puts in 70 DEG C of baking ovens, dry 1.5h, grind, put in Muffle furnace and calcine 550 DEG C, insulation
1.5h, takes out, obtains composite catalyst powder body.
Embodiment 4.
Infusion process prepares new selective composite photo-catalyst powder body la2nio4/y2mo4o15, comprise the following steps: weigh
3mmol nickelous carbonate, 6mmol lanthanum carbonate, are dissolved in 270ml distilled water, obtain solution a；Being slowly added to concentration in solution a is 1/
500mol l-1 sodium hydroxide solution, adjustment solution ph be 10.5, stir 2h, revolution be 600r/min, subsequently will be molten
Liquid carries out sucking filtration, is precipitated b；B will be precipitated and calcine 750 DEG C, insulation 3h in Muffle furnace, obtain catalyst powder c；By powder body
C puts in 90ml dehydrated alcohol, high speed ball milling, and ball mill revolution is 5000r/min, ball milling 3h, and drying temperature is 80 DEG C, the time
For 40min, obtain powder body d；Weigh 2mmol Yttrium carbonate (Y2(CO3)3), weigh 4mmol ammonium molybdate, be dissolved in the distilled water of 200ml, obtain molten
Liquid e；Solution e is mixed with powder body d, puts in 90 DEG C of baking ovens, dry 1h, grind, put in Muffle furnace and calcine 550 DEG C, insulation
2h, takes out, obtains composite catalyst powder body.
Embodiment 5.
Infusion process prepares new selective composite photo-catalyst powder body la2nio4/y2mo4o15, comprise the following steps: weigh
2mmol nickel acetate, 4mmol Lanthanum (III) nitrate, are dissolved in 200ml distilled water, obtain solution a；Being slowly added to concentration in solution a is 1/
The sodium hydroxide solution of 400mol l-1, adjustment solution ph is 10, stirs 2h, and solution is subsequently entered by revolution for 650r/min
Row sucking filtration, is precipitated b；, b will be precipitated and calcine 750 DEG C, insulation 3h in Muffle furnace, obtain catalyst powder c；Powder body c is put
Enter in 40ml dehydrated alcohol, high speed ball milling, ball mill revolution is 6000r/min, ball milling 2h, and drying temperature is 50 DEG C, and the time is
60min, obtains powder body d；Weigh 2mmol Yttrium carbonate (Y2(CO3)3), weigh 4mmol ammonium molybdate, be dissolved in the distilled water of 120ml, obtain solution
e；Solution e is mixed with powder body d, puts in 80 DEG C of baking ovens, dry 50min, grind, put in Muffle furnace and calcine 650 DEG C, insulation
2h, takes out, obtains composite catalyst powder body.
This powder body is put into illumination 20min in methylene blue solution it is seen that the absworption peak at 660nm is obvious, to methylene
Base indigo plant has obvious degradation to act on, and sees Fig. 4.
Embodiment 6.
Infusion process prepares new selective composite photo-catalyst powder body la2nio4/y2mo4o15, comprise the following steps: weigh
5mmol nickel acetate, 10mmol Lanthanum (III) nitrate, are dissolved in 300ml distilled water, obtain solution a；Being slowly added to concentration in solution a is
The sodium hydroxide solution of 1/400mol l-1, adjustment solution ph is 10.5, stirs 2h, and revolution is 500r/min, subsequently will be molten
Liquid carries out sucking filtration, is precipitated b；B will be precipitated and calcine 900 DEG C, insulation 3h in Muffle furnace, obtain catalyst powder c；By powder body
C puts in 60ml dehydrated alcohol, high speed ball milling, and ball mill revolution is 6000r/min, ball milling 3h, and drying temperature is 90 DEG C, the time
For 35min, obtain powder body d；Weigh 4mmol Yttrium carbonate (Y2(CO3)3), weigh 8mmol ammonium molybdate, be dissolved in the distilled water of 250ml, obtain molten
Liquid e；Solution e is mixed with powder body d, puts into drying 50min in 80 DEG C of baking ovens, grind, put in Muffle furnace and calcine 600 DEG C, protect
Warm 2h, takes out, obtains composite catalyst powder body.
This powder body is put into illumination 40min in methylene blue solution it is seen that the absworption peak at 660nm is obvious, to methylene
Base indigo plant has obvious degradation to act on, and sees Fig. 5.
Embodiment 7.
Infusion process prepares new selective composite photo-catalyst powder body la2nio4/y2mo4o15, comprise the following steps: weigh
3mmol nickel nitrate, 6mmol Lanthanum (III) nitrate, are dissolved in 200ml distilled water, obtain solution a；Being slowly added to concentration in solution a is 1/
The sodium hydroxide solution of 500mol l-1, adjustment solution ph is 10, stirs 2h, and solution is subsequently entered by revolution for 800r/min
Row sucking filtration is precipitated b；B will be precipitated and calcine 800 DEG C, insulation 3h in Muffle furnace, obtain catalyst powder c；Powder body c is put into
In 40ml ethanol solution, high speed ball milling, ball mill revolution is 4000r/min, ball milling 2h, and drying temperature is 40 DEG C, and the time is
85min, obtains powder body d；Weigh 4mmol acetic acid yttrium, weigh 8mmol ammonium molybdate, be dissolved in the distilled water of 400ml, obtain solution
e；Solution e is mixed with powder body d, puts in 80 DEG C of baking ovens, dry 50min, grind, put in Muffle furnace and calcine 600 DEG C, insulation
2h, takes out, obtains composite catalyst powder body.
This powder body is put into illumination 60min in methylene blue solution it is seen that the absworption peak at 660nm is obvious, to methylene
Base indigo plant has obvious degradation to act on, and sees Fig. 6.
Using dx2500 type x-ray diffraction instrument to pure la2nio4With pure y2mo4o15It is tested, scanning speed is
0.04 °/min, 2 θ scopes are 10-90 °.Experiment preparation la2nio4(pdf #01-0728), in pdf card, summit exists
31.64°；la2nio4The xrd figure of photocatalyst, is shown in Fig. 1, and wherein a is 800 degree of lower la2nio4 powder body xrd collection of illustrative plates；B is 900 degree
Lower la2nio4Powder body xrd collection of illustrative plates.Preparation y2mo4o15(pdf #53-0358), in pdf card, summit is at 25.529 °；
y2mo4o15The xrd figure of photocatalyst, is shown in Fig. 2, and wherein a is 500 degree of lower y2mo4o15Powder body xrd collection of illustrative plates；Under b is 600 degree
y2mo4o15Powder body xrd collection of illustrative plates.
The sem figure of the photocatalyst powder body of the present invention, is shown in Fig. 3.3-1 is 850 degree of lower la2nio4Photocatalyst powder body scans
Electron microscope；3-2 is 500 degree of lower y2mo4o15The sem figure of photocatalyst powder body；3-3 is the sem figure of composite photo-catalyst powder body；By
In figure understands, the photocatalyst powder body of present invention preparation, and powder granularity is uniform in size, grain shape rule.Granular size is
100nm-150nm.
Carry out the light degradation experiment of methylene blue with the photocatalyst of embodiment 5-7 preparation, as Figure 4-Figure 6.From Fig. 4-6
Understand, catalyst of the present invention has better effects to methylene blue.The catalyst of the present invention is used in light degradation experiment, experiment
The weight of catalyst does not change in front and back.
Claims (10)
1. a kind of selectivity composite photo-catalyst powder body is it is characterised in that the chemical formula of described photocatalyst is:
la2nio4y2mo4o15.
2. composite photo-catalyst raw powder's production technology as claimed in claim 1 is it is characterised in that comprise the following steps:
(1) weigh the soluble-salt of nickel, the soluble-salt of lanthanum according to mol ratio 1:2, be dissolved in appropriate distilled water, obtain solution a；
(2) it is slowly added to sodium hydroxide solution in solution a, adjustment ph value is 9.5-10.5, stirring a period of time, subsequently will be molten
Liquid carries out sucking filtration, obtains solution b；
(3) b will be precipitated to calcine in Muffle furnace, be incubated, obtain catalyst powder c；
(4) powder body c is put in alcoholic solution, for a period of time, diameter of particle is 1 m-2 m to high speed ball milling, dries, obtains powder body d
(la2nio4)；
(5) appropriate hundred million soluble-salt, the ammonium molybdate ((nh of measured amounts are weighed respectively4)6mo7o24·4h2O), be dissolved in suitable
In amount distilled water, mix homogeneously, obtain solution e；
(6) solution e is mixed with powder body d, dry a period of time in an oven, grind, diameter of particle is 1 μm -2 μm, puts into horse
Not calcining a period of time in stove, take out, obtain composite catalyst powder body.
3. composite photo-catalyst raw powder's production technology as claimed in claim 1 is it is characterised in that the solubility of described nickel
Salt is one of nitrate, carbonate or acetate and several；The soluble-salt of lanthanum is in nitrate, carbonate or acetate
One kind and several；One or more of the soluble-salt nitrate of yttrium, carbonate or acetate.
4. composite photo-catalyst raw powder's production technology as claimed in claim 2 is it is characterised in that in described step (1), steam
The consumption of distilled water be nickel soluble-salt, 20-40 times of the soluble-salt integral molar quantity of lanthanum.
5. composite photo-catalyst raw powder's production technology as claimed in claim 2 is it is characterised in that in described step (1), hydrogen
The concentration of sodium oxide is 1/300-1/500mol l-1；Described stirring is magnetic agitation or mechanical agitation, and revolution is 500-
800r/min, mixing time is 1-2h.
6. composite photo-catalyst raw powder's production technology as claimed in claim 2 is it is characterised in that in described step (3), horse
Not the calcining heat of stove is 750-900 DEG C, and temperature retention time is 1-3h.
7. composite photo-catalyst raw powder's production technology as claimed in claim 2 is it is characterised in that in described step (4), alcohol
Solution is one kind of the solubility alcoholic solution such as methanol or ethanol；The volumetric usage of alcoholic solution is the solvable of the soluble-salt of nickel and lanthanum
5-10 times of property salt integral molar quantity；Described drying temperature is 40-90 DEG C, and the time is 30-90min.
8. composite photo-catalyst raw powder's production technology as claimed in claim 2 is it is characterised in that in described step (5), steam
The volumetric usage of distilled water is 20-40 times of the soluble-salt of yttrium and ammonium molybdate integral molar quantity；The soluble-salt of described yttrium and molybdenum
Y in sour ammonium and mo is than for 1:2.
9. composite photo-catalyst raw powder's production technology as claimed in claim 2 is it is characterised in that in described step (6), dry
Dry temperature is 60-90 DEG C, and the time is 1-3h, and Muffle furnace calcining heat is 500-650 DEG C, is incubated 1-2h.
10. described composite photo-catalyst powder body as arbitrary in claim 2-9 is used for the degraded of insoluble organic in industrial wastewater
Process；Described Organic substance is methylene blue.
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| CN113019383A (en) * | 2021-03-10 | 2021-06-25 | 中国科学院兰州化学物理研究所 | Nickel/lanthanum oxide catalyst and preparation method and application thereof |
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