CN108355679A - A kind of Fe3O4/MoS2/BiVO4Preparation method, product and its application of material - Google Patents
A kind of Fe3O4/MoS2/BiVO4Preparation method, product and its application of material Download PDFInfo
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- CN108355679A CN108355679A CN201810076011.6A CN201810076011A CN108355679A CN 108355679 A CN108355679 A CN 108355679A CN 201810076011 A CN201810076011 A CN 201810076011A CN 108355679 A CN108355679 A CN 108355679A
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 64
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 64
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 239000000463 material Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title description 3
- 239000002131 composite material Substances 0.000 claims abstract description 41
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 35
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 30
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229940056319 ferrosoferric oxide Drugs 0.000 claims abstract description 17
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 239000001632 sodium acetate Substances 0.000 claims abstract description 13
- 235000017281 sodium acetate Nutrition 0.000 claims abstract description 13
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 11
- NASFKTWZWDYFER-UHFFFAOYSA-N sodium;hydrate Chemical compound O.[Na] NASFKTWZWDYFER-UHFFFAOYSA-N 0.000 claims abstract description 9
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000000376 reactant Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 13
- 239000011941 photocatalyst Substances 0.000 claims description 12
- 235000015393 sodium molybdate Nutrition 0.000 claims description 11
- 239000011684 sodium molybdate Substances 0.000 claims description 11
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 11
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 10
- 239000011609 ammonium molybdate Substances 0.000 claims description 10
- 229940010552 ammonium molybdate Drugs 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 9
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 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 description 8
- 239000000203 mixture Substances 0.000 claims description 5
- -1 molybdic acid hydrates Chemical class 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 4
- 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 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- XDBSEZHMWGHVIL-UHFFFAOYSA-M hydroxy(dioxo)vanadium Chemical compound O[V](=O)=O XDBSEZHMWGHVIL-UHFFFAOYSA-M 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- XWNOTOKFKBDMAP-UHFFFAOYSA-N [Bi].[N+](=O)(O)[O-] Chemical compound [Bi].[N+](=O)(O)[O-] XWNOTOKFKBDMAP-UHFFFAOYSA-N 0.000 claims 2
- 229910000831 Steel Inorganic materials 0.000 claims 1
- 239000010959 steel Substances 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 22
- 238000007146 photocatalysis Methods 0.000 abstract description 20
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 17
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 abstract description 13
- 239000002351 wastewater Substances 0.000 abstract description 12
- 230000015556 catabolic process Effects 0.000 abstract description 11
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 239000003054 catalyst Substances 0.000 abstract description 10
- 238000004064 recycling Methods 0.000 abstract description 10
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 abstract description 2
- 239000000843 powder Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 239000004202 carbamide Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 235000011091 sodium acetates Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
- B01J27/0515—Molybdenum with iron group metals or platinum group metals
-
- 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
- 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
-
- 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
- C02F2101/38—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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (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)
Abstract
The invention discloses a kind of Fe3O4/MoS2/BiVO4Iron(III) chloride hexahydrate, sodium acetate and polyethylene glycol are dissolved in ethylene glycol first, react 8~9h at 180~200 DEG C, obtain ferroso-ferric oxide by material preparation method, product and its application；Then, two molybdic acid hydrate sodium, four molybdic acid hydrate sodium and thiocarbamide are uniformly mixed, ferroso-ferric oxide is added, reaction 22 at 180~200 DEG C~for 24 hours, obtain Fe3O4/MoS2Material；Finally, five nitric hydrate bismuths and ammonium metavanadate are dissolved in deionized water, Fe is added3O4/MoS2Material is uniformly mixed, and 15~17h is reacted at 160~170 DEG C, obtains Fe3O4/MoS2/BiVO4Composite material.The composite material of the present invention is as photochemical catalyst for when handling quadracycline waste water, degradation rate to improve photocatalysis efficiency up to 90% or more, simultaneously as Fe3O4Presence, can be more convenient simply to recycle photochemical catalyst, to repeat test in, reduce the cost recovery of photochemical catalyst, improve the recycling rate of waterused of photochemical catalyst.
Description
Technical field
The invention belongs to environmental protection technical fields, and in particular to a kind of Fe3O4/MoS2/BiVO4Preparation method, the party
Composite material and its application prepared by method.
Background technology
With the getting worse of environmental problem, and people increasingly pay attention to environmental problem, more and more new material quilts
It is found that and to handle waste water.Wherein, catalysis material with its can utilize luminous energy, react the ratio of progress more thoroughly and
The characteristics of non-secondary pollution, shows one's talent.1972, Fuyishima etc. had found optoelectronic pole under the irradiation of ultraviolet light, can incite somebody to action
Water decomposition is H2And O2, open photochemistry field.BiVO4It is a kind of flaxen inorganic dyestuff, there is nontoxic, corrosion resistance
The features such as good, due to visible light-responded good, energy gap is small, and people is caused adequately to pay close attention to.But pure BiVO4Due to its separation
The ability of photo-generate electron-hole pair is poor, also can not meet people's needs to the degradation effect of pollutant, therefore improves vanadic acid
The photocatalysis efficiency of bismuth is extremely urgent.
MoS2As a kind of typical class graphene transition metal dichalcogenide, there is good light, electricity and catalytic property.
Due to MoS2Have controllable many unsaturated bonds, energy gap, conduction band (CB) and valence band (VB) edge current potential (- 0.1eV }+
2eV) than most of photosensitive semiconductor highers and there is huge specific surface area, therefore can be used as photocatalysis assistant regulating and controlling material.And
And MoS2When photocatalyst itself, since its absorption optical wavelength range is narrow, sunlight cannot be made full use of, thus is independently made
With when photocatalysis efficiency it is not high.
Invention content
For the defect and deficiency of existing technology of preparing, the object of the present invention is to provide a kind of Fe3O4/MoS2/BiVO4
Preparation method, product and its application of material improve the photocatalytic activity and catalytic efficiency of composite material, reinforce the utilization to light
Rate, and improve the recycling rate of waterused of photochemical catalyst.
To achieve the goals above, the present invention is realised by adopting the following technical scheme：
A kind of Fe3O4/MoS2/BiVO4The preparation method of composite material,
Fe is prepared first3O4/MoS2Composite material；Then according to Bi3+And Mo6+Molar ratio be 20~10：1 ratio will
Bismuth nitrate, ammonium metavanadate and Fe3O4/MoS2Composite material mixes, and 15~17h is reacted at 160~170 DEG C, rinses drying, obtains
To Fe3O4/MoS2/BiVO4Composite material.
Further, the bismuth nitrate and ammonium metavanadate are according to molar ratio 1:1 ratio mixes.
Further, 30~40min of magnetic agitation, adds after bismuth nitrate and metavanadic acid being dissolved in deionized water
Fe3O4/MoS220~30min of material ultrasonic vibration obtains mixed liquor, mixed liquor is poured into polytetrafluoroethylliner liner, compactedness
It is 80%, polytetrafluoroethylliner liner is put into stainless steel cauldron, is placed in electrothermostat, with the heating rate of 5 DEG C/min
160~170 DEG C are heated to, 15~17h is reacted；
It uses distilled water and absolute ethyl alcohol to rinse respectively reactant, 5min is then centrifuged with the speed of 6000r/min, it will
Product after centrifugation is placed in vacuum drying chamber, the dry 3h at 50 DEG C, dry 3h at 60 DEG C, dry 3h at 70 DEG C, at 80 DEG C
Dry 3h.
Further, the Fe3O4/MoS2The preparation of material includes：
Step 1：Ferric trichloride, sodium acetate and polyethylene glycol are dissolved in ethylene glycol, at 180~200 DEG C react 8~
Reactant rinsing, drying is obtained ferroso-ferric oxide by 9h；
Step 2：Sodium molybdate, ammonium molybdate and thiocarbamide are uniformly mixed, the ferroso-ferric oxide that step 1 obtains is added,
Reaction 22 at 180~200 DEG C~for 24 hours, by reactant rinsing, drying, obtain Fe3O4/MoS2Material.
Further, in the step 1, ferric trichloride and sodium acetate are 1.25 according to molar ratio:1 ratio mixing；It is poly-
The addition of ethylene glycol is 5wt%~6wt% of ferric trichloride and sodium acetate gross mass.
Further, in the step 2, sodium molybdate and ammonium molybdate are 1 according to molar ratio:(8~9) it mixes；The sulphur
The addition of urea is according to Mo6+Total mole number and thiocarbamide molar ratio be 1:2 ratio mixing；The ferroso-ferric oxide adds
Enter amount be two molybdic acid hydrate sodium, four molybdic acid hydrate sodium and thiocarbamide gross mass 2.5%~3%.
Further, in the step 1, the mixture magnetic force of ferric trichloride, sodium acetate, polyethylene glycol and ethylene glycol is stirred
Mix 30~40min, 10~20min of ultrasonic vibration；8~9h is reacted at 180~200 DEG C, and reactant is used into deionized water respectively
It is rinsed with absolute ethyl alcohol, the dry 5h at 40 DEG C, then the dry 7h at 50 DEG C.
Further, in the step 2,30~40min of magnetic agitation after sodium molybdate, ammonium molybdate and thiocarbamide mixing, then add
Enter ferroso-ferric oxide 20~30min of ultrasonic vibration, at 180~200 DEG C react 22~for 24 hours, reactant is used into deionization respectively
Water and absolute ethyl alcohol rinse, the dry 5h at 40 DEG C, the dry 7h at 50 DEG C.
The invention also discloses Fe prepared by above-mentioned preparation method3O4/MoS2/BiVO4Composite material.
The invention also discloses by above-mentioned Fe3O4/MoS2/BiVO4The application of composite material photocatalyst.
Compared with prior art, the beneficial effects of the invention are as follows：
The Fe of the present invention3O4/MoS2/BiVO4Composite material is for when handling quadracycline waste water, degradation rate to be reachable
90% or more, photocatalysis efficiency is improved, simultaneously as Fe3O4Presence, can be more convenient simply to recycle photochemical catalyst, use
In repeating to test, the cost recovery of photochemical catalyst is reduced, the recycling rate of waterused of photochemical catalyst is improved；
Powder made from the preparation method of the present invention has grain development complete, and granularity is small, and is evenly distributed, particle agglomeration
It is relatively light, raw material inexpensively can be used, be easy to get to suitable stoichiometry object and crystalline form；And preparation process is controllable, energy consumption is few.
Explanation is further explained in detail to the particular content of the present invention with reference to embodiments.
Description of the drawings
Fig. 1 is the Fe that the embodiment of the present invention 1 obtains3O4/MoS2/BiVO4The shape appearance figure of composite material.
Fig. 2 is the XRD diagram for the material that the embodiment of the present invention 1 obtains.
Specific implementation mode
The invention discloses a kind of Fe3O4/MoS2/BiVO4The preparation method of composite material, prepares Fe first3O4/MoS2It is multiple
Condensation material；Then according to Bi3+And Mo6+Molar ratio be 20~10：1 ratio is by bismuth nitrate, ammonium metavanadate and Fe3O4/MoS2
Composite material mixes, and 15~17h is reacted at 160~170 DEG C, rinses drying, obtains Fe3O4/MoS2/BiVO4Composite material.
Wherein, bismuth nitrate and ammonium metavanadate are 1 according to molar ratio:1 ratio mixes.
Specifically, Fe3O4/MoS2/BiVO4The specific preparation method of composite material includes：Bismuth nitrate and metavanadic acid are dissolved in
30~40min of magnetic agitation, adds Fe after in deionized water3O4/MoS220~30min of material ultrasonic vibration obtains mixed liquor,
Mixed liquor is poured into polytetrafluoroethylliner liner, polytetrafluoroethylliner liner is put into stainless steel cauldron, set by compactedness 80%
In in electrothermostat, 160~170 DEG C are heated to the heating rate of 5 DEG C/min, reacts 15~17h；Reactant is made respectively
It is rinsed with distilled water and absolute ethyl alcohol, 5min is then centrifuged with the speed of 6000r/min, the product after centrifugation is placed in vacuum and is done
In dry case, the dry 3h at 50 DEG C, dry 3h at 60 DEG C, dry 3h at 70 DEG C, dry 3h at 80 DEG C.
Wherein, Fe3O4/MoS2The preparation method of composite material includes：
Step 1：Ferric trichloride, sodium acetate and polyethylene glycol are dissolved in ethylene glycol, at 180~200 DEG C react 8~
Reactant rinsing, drying is obtained ferroso-ferric oxide by 9h；
Wherein, ferric trichloride and sodium acetate are 1.25 according to molar ratio:1 ratio mixing；The addition of polyethylene glycol is
5wt%~6wt% of ferric trichloride and sodium acetate gross mass.
Step 2：Sodium molybdate, ammonium molybdate and thiocarbamide are uniformly mixed, the ferroso-ferric oxide that step 1 obtains is added,
Reaction 22 at 180~200 DEG C~for 24 hours, by reactant rinsing, drying, obtain Fe3O4/MoS2Material.
Wherein, sodium molybdate and ammonium molybdate are 1 according to molar ratio:(8~9) it mixes；The addition of the thiocarbamide is according to Mo6+
Total mole number and thiocarbamide molar ratio be 1:2 ratio mixing；The addition of the ferroso-ferric oxide is two molybdic acid hydrates
The 2.5%~3% of sodium, four molybdic acid hydrate sodium and thiocarbamide gross mass.
Specifically, the specific preparation process of step 1 ferroso-ferric oxide is：By ferric trichloride, sodium acetate, polyethylene glycol and second
Mixture 30~the 40min of magnetic agitation, 10~20min of ultrasonic vibration of glycol；8~9h is reacted at 180~200 DEG C, it will be anti-
Answer object that deionized water and absolute ethyl alcohol is used to rinse respectively, the dry 5h at 40 DEG C, the dry 7h at 50 DEG C obtain four oxidations three
Iron.
Specifically, Fe in step 23O4/MoS2Specific preparation process be：Magnetic force after sodium molybdate, ammonium molybdate and thiocarbamide mixing
Stir 30~40min, add ferroso-ferric oxide 20~30min of ultrasonic vibration, at 180~200 DEG C react 22~for 24 hours, will
Reactant uses deionized water and absolute ethyl alcohol to rinse respectively, and the dry 5h at 40 DEG C, dry 7h, obtains Fe at 50 DEG C3O4/
MoS2Material.
Specific embodiments of the present invention are given below, it should be noted that the invention is not limited in following specific examples
In, all equivalent transformations made on the basis of the technical solutions of the present application each falls within protection scope of the present invention.
It is raw materials used in the following embodiment of the present invention to be respectively：
Ferric trichloride is Iron(III) chloride hexahydrate, and analysis is pure, commercially available；Sodium acetate, analysis is pure, commercially available；Polyethylene glycol, analysis
It is pure, it is commercially available；Sodium molybdate is two molybdic acid hydrate sodium, and analysis is pure, commercially available；Sodium molybdate is four molybdic acid hydrate sodium, and analysis is pure, commercially available；Sulphur
Urea, analysis is pure, commercially available；Bismuth nitrate is five nitric hydrate bismuths, and analysis is pure, commercially available；Ammonium metavanadate, analysis is pure, commercially available；Ethylene glycol,
It is commercially available；Distilled water, it is commercially available；Absolute ethyl alcohol, it is commercially available.
Embodiment 1
2.7g Iron(III) chloride hexahydrates and 7.2g sodium acetates are weighed, and 0.6g polyethylene glycol is added, dissolves in 70mL ethylene glycol
In, 30~40min of magnetic agitation is carried out, 10~20min of ultrasonic vibration transfers them to the reaction kettle of polytetrafluoroethyllining lining
In, compactedness 80% reacts 8h at 200 DEG C, is respectively washed 3 times with deionized water and absolute ethyl alcohol, with 6000r/min's
Speed is centrifuged, under conditions of in vacuum drying chamber with vacuum degree being -0.1MPa, the dry 5h at 40 DEG C, at 50 DEG C
Dry 7h, obtains ferroso-ferric oxide；
Bis- molybdic acid hydrate sodium of 0.36g, 2.38g Ammonium Molybdate Tetrahydrates and 2.28g thiocarbamides are weighed respectively, are mixed, magnetic force
30min is stirred, the ferroso-ferric oxide that 0.10g is prepared, ultrasonic vibration 30min is then added；It is then transferred to polytetrafluoro
It in the reaction kettle of ethylene liner, and reacts for 24 hours at 200 DEG C, after being cooled to room temperature, is distinguished with deionized water and absolute ethyl alcohol
Cleaning 3 times, centrifuged with the speed of 6000r/min, in vacuum drying chamber with vacuum degree be -0.1MPa under conditions of,
Dry 5h at 40 DEG C, dry 7h, obtains Fe at 50 DEG C3O4/MoS2Powder；
Five nitric hydrate bismuths of 4.850g and 1.170g ammonium metavanadates are weighed, is dissolved in deionized water, magnetic agitation 30min,
Then the Fe prepared in addition 0.080g3O4/MoS2Powder (Bi3+With Mo6+Molar ratio=20:1), ultrasonic vibration 30min, will
It is transferred in the reaction kettle of polytetrafluoroethyllining lining, reacts 16h at 160 DEG C, after being cooled to room temperature, with deionized water and
Absolute ethyl alcohol is respectively washed 3 times, is centrifuged with the speed of 6000r/min, with vacuum degree for -0.1MPa in vacuum drying chamber
Under conditions of, dry 12h, obtains composite material at 80 DEG C, and the pattern of the material is as shown in Figure 1, the material to acquisition carries out
XRD energy spectrum analysis, as Fe3O4/MoS2/BiVO4Composite material.
By magnetic Fe obtained3O4/MoS2/BiVO4Composite photo-catalyst is used for Photocatalytic Activity for Degradation quadracycline
The application example of waste water：
The quadracycline waste water for preparing 20mg/L, weighs the above-mentioned Fe of 30mg3O4/MoS2/BiVO4Composite photo-catalyst in
In quartz glass tube, it is thoroughly mixed with 50ml quadracycline waste water.Above-mentioned mixed solution is first ultrasonically treated 5min, makes photocatalysis
Agent is fully dispersed in waste water.Magnetic rotor will be added in the mixture of above-mentioned catalyst and waste water, it is small to be placed in dark place reaction half
When.Again using 400WXe lamps as light source, above-mentioned processing waste water is irradiated, sample detection absorbance after 2h.Inverted calculating, hydrochloric acid four
Ring element waste water is effectively degraded, and photocatalysis treatment efficiency has reached 91%.Again being used for the composite photo-catalyst after recycling can
Light-exposed photocatalytic degradation quadracycline waste water, photocatalysis treatment efficiency reach 85% or so.
Embodiment 2
The present embodiment and embodiment 1 difference lies in：In the mixed liquor of five nitric hydrate bismuths and ammonium metavanadate, Fe3O4/
MoS2The addition of powder is 0.107g, i.e. Bi3+With Mo6+Molar ratio=15:1.
Obtained magnetic Fe3O4/MoS2/BiVO4Composite photo-catalyst carries out photocatalysis experiment, 2h under the same conditions
The degradation rate of quadracycline solution is 87.5% afterwards.Its photocatalysis treatment efficiency reaches 80% or so after recycling.
Embodiment 3
The present embodiment and embodiment 1 difference lies in：In the mixed liquor of five nitric hydrate bismuths and ammonium metavanadate, Fe3O4/
MoS2The addition of powder is 0.160g, i.e. Bi3+With Mo6+Molar ratio 10:1.
Obtained magnetic Fe3O4/MoS2/BiVO4Composite photo-catalyst carries out photocatalysis experiment, 2h under the same conditions
The degradation rate of quadracycline solution is 85% afterwards.Its photocatalysis treatment efficiency reaches 80% or so after recycling.
Embodiment 4
The present embodiment and embodiment 1 difference lies in：The mixed liquor and Fe of five nitric hydrate bismuths and ammonium metavanadate3O4/MoS2
Reaction temperature of the powder in the reaction kettle of polytetrafluoroethyllining lining is 170 DEG C.
Obtained magnetic Fe3O4/MoS2/BiVO4Composite photo-catalyst carries out photocatalysis experiment, 2h under the same conditions
The degradation rate of quadracycline solution is 89% afterwards.Its photocatalysis treatment efficiency reaches 82% or so after recycling.
Embodiment 5
The present embodiment and embodiment 1 difference lies in：Five nitric hydrate bismuths and ammonium metavanadate are dissolved in deionized water, magnetic force
40min is stirred, Fe is then added3O4/MoS2Powder, ultrasonic vibration 20min,
Obtained magnetic Fe3O4/MoS2/BiVO4Composite photo-catalyst carries out photocatalysis experiment, 2h under the same conditions
The degradation rate of quadracycline solution is 91% afterwards.Its photocatalysis treatment efficiency reaches 85% or so after recycling.
Embodiment 6
The present embodiment and embodiment 1 difference lies in：In Fe3O4In preparation process, reaction temperature is 190 DEG C.
Obtained magnetic Fe3O4/MoS2/BiVO4Composite photo-catalyst carries out photocatalysis experiment, 2h under the same conditions
The degradation rate of quadracycline solution is 90% afterwards.Its photocatalysis treatment efficiency reaches 85% or so after recycling.
Embodiment 7
The present embodiment and embodiment 1 difference lies in：In Fe3O4/MoS2In preparation process, reaction temperature is 190 DEG C.
Obtained magnetic Fe3O4/MoS2/BiVO4Composite photo-catalyst carries out photocatalysis experiment, 2h under the same conditions
The degradation rate of quadracycline solution is 90% afterwards.Its photocatalysis treatment efficiency reaches 85% or so after recycling.
Comparative example 1
With five nitric hydrate bismuths, ammonium metavanadate is raw material, and using EDTA as dispersant, isopropanol is solvent, anti-at 180 DEG C
20h is answered, after showing that product separation is dry, 3h is calcined at 500 DEG C, obtains pucherite.
Using product as catalyst, under the irradiation of 400W xenon lamps, to handle quadracycline waste water, after 2h, hydrochloric acid four
Ring element degradation rate is 75%.
Claims (10)
1. a kind of Fe3O4/MoS2/BiVO4The preparation method of composite material, which is characterized in that
Fe is prepared first3O4/MoS2Composite material；Then according to Bi3+And Mo6+Molar ratio be 20~10：1 ratio is by nitric acid
Bismuth, ammonium metavanadate and Fe3O4/MoS2Composite material mixes, and 15~17h is reacted at 160~170 DEG C, rinses drying, obtains
Fe3O4/MoS2/BiVO4Composite material.
2. Fe as described in claim 13O4/MoS2/BiVO4The preparation method of composite material, which is characterized in that the nitric acid
Bismuth and ammonium metavanadate are according to molar ratio 1:1 ratio mixes.
3. Fe as described in claim 13O4/MoS2/BiVO4The preparation method of composite material, which is characterized in that by bismuth nitrate and
30~40min of magnetic agitation, adds Fe after metavanadic acid is dissolved in deionized water3O4/MoS220~30min of material ultrasonic vibration
Mixed liquor is obtained, mixed liquor is poured into polytetrafluoroethylliner liner, polytetrafluoroethylliner liner is put into stainless by compactedness 80%
Steel reaction kettle, is placed in electrothermostat, is heated to 160~170 DEG C with the heating rate of 5 DEG C/min, reacts 15~17h；
It uses distilled water and absolute ethyl alcohol to rinse respectively reactant, 5min is then centrifuged with the speed of 6000r/min, will be centrifuged
Product afterwards is placed in vacuum drying chamber, the dry 3h at 50 DEG C, dry 3h at 60 DEG C, dry 3h at 70 DEG C, dry at 80 DEG C
3h。
4. Fe as described in claim 13O4/MoS2/BiVO4The preparation method of composite material, which is characterized in that described
Fe3O4/MoS2The preparation of material includes：
Step 1：Ferric trichloride, sodium acetate and polyethylene glycol are dissolved in ethylene glycol, 8~9h is reacted at 180~200 DEG C, it will
Reactant rinsing, drying obtains ferroso-ferric oxide；
Step 2：Sodium molybdate, ammonium molybdate and thiocarbamide are uniformly mixed, the ferroso-ferric oxide that step 1 obtains is added, 180~
Reaction 22 at 200 DEG C~for 24 hours, by reactant rinsing, drying, obtain Fe3O4/MoS2Material.
5. the Fe described in claim 43O4/MoS2/BiVO4The preparation method of composite material, which is characterized in that in the step 1,
Ferric trichloride and sodium acetate are 1.25 according to molar ratio:1 ratio mixing；The addition of polyethylene glycol is ferric trichloride and acetic acid
5wt%~6wt% of sodium gross mass.
6. the Fe described in claim 43O4/MoS2/BiVO4The preparation method of composite material, which is characterized in that in the step 2,
Sodium molybdate and ammonium molybdate are 1 according to molar ratio:(8~9) it mixes；The addition of the thiocarbamide is according to Mo6+Total mole number with
The molar ratio of thiocarbamide is 1:2 ratio mixing；The addition of the ferroso-ferric oxide is two molybdic acid hydrate sodium, four molybdic acid hydrates
The 2.5%~3% of sodium and thiocarbamide gross mass.
7. the Fe described in claim 43O4/MoS2/BiVO4The preparation method of composite material, which is characterized in that in the step 1,
By mixture 30~40min of magnetic agitation of ferric trichloride, sodium acetate, polyethylene glycol and ethylene glycol, ultrasonic vibration 10~
20min；8~9h is reacted at 180~200 DEG C, is used deionized water and absolute ethyl alcohol to rinse respectively reactant, is done at 40 DEG C
Dry 5h, then the dry 7h at 50 DEG C.
8. the Fe described in claim 43O4/MoS2/BiVO4The preparation method of composite material, which is characterized in that in the step 2,
30~40min of magnetic agitation after sodium molybdate, ammonium molybdate and thiocarbamide mixing, adds ferroso-ferric oxide 20~30min of ultrasonic vibration,
The reaction 22~for 24 hours at 180~200 DEG C, uses deionized water and absolute ethyl alcohol to rinse reactant respectively, dry at 40 DEG C
5h, the dry 7h at 50 DEG C.
9. Fe prepared by the preparation method described in claim 1~8 any one3O4/MoS2/BiVO4Composite material.
10. the Fe described in claim 93O4/MoS2/BiVO4The application of composite material photocatalyst.
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