CN108940332A - A kind of high activity MoS2/g-C3N4/Bi24O31Cl10The preparation method of composite photo-catalyst - Google Patents
A kind of high activity MoS2/g-C3N4/Bi24O31Cl10The preparation method of composite photo-catalyst Download PDFInfo
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- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 60
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 60
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 230000000694 effects Effects 0.000 title claims abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 129
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 54
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 36
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 20
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 7
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 7
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 7
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000005119 centrifugation Methods 0.000 claims abstract description 5
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 4
- 238000009841 combustion method Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000012719 thermal polymerization Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 50
- 239000007787 solid Substances 0.000 claims description 32
- 239000011259 mixed solution Substances 0.000 claims description 30
- 238000002604 ultrasonography Methods 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- 238000005516 engineering process Methods 0.000 claims description 11
- 239000000428 dust Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 6
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims description 6
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 18
- 239000000463 material Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000000356 contaminant Substances 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 238000001782 photodegradation Methods 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 22
- 150000001875 compounds Chemical class 0.000 description 11
- 230000001699 photocatalysis Effects 0.000 description 10
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 9
- 239000004098 Tetracycline Substances 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 8
- 229940043267 rhodamine b Drugs 0.000 description 8
- 229960002180 tetracycline Drugs 0.000 description 8
- 229930101283 tetracycline Natural products 0.000 description 8
- 235000019364 tetracycline Nutrition 0.000 description 8
- 150000003522 tetracyclines Chemical class 0.000 description 8
- 238000005286 illumination Methods 0.000 description 6
- -1 price be low Substances 0.000 description 6
- 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 description 3
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000000703 high-speed centrifugation Methods 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001621 bismuth Chemical class 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005713 exacerbation Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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 belongs to new material, utilization of new energy resources and technical field of environment pollution control, are related to a kind of high activity MoS2/g‑C3N4/Bi24O31Cl10The preparation method of composite photo-catalyst.Using bismuth nitrate, ammonium chloride, citric acid as raw material, Bi is prepared using improved solution combustion method24O31Cl10;Using melamine, acetic acid as raw material, g-C is prepared using a step thermal polymerization3N4;Using ammonium molybdate, thiocarbamide as raw material, dimethylformamide is solvent, prepares MoS using hydro-thermal method2;The Bi that will be handled through ultrasonic disperse24O31Cl10With g-C3N4、MoS2In methanol solution after ultrasonic mixing reaction, washing, centrifugation, drying are to get the composite photo-catalyst.This method is simple and easy, low in cost, reproducible, is with a wide range of applications in fields such as photodegradation water, photochemical catalytic oxidation environmental contaminants.
Description
Technical field
The invention belongs to new material, utilization of new energy resources and technical field of environment pollution control, are related to a kind of high activity MoS2/
g-C3N4/Bi24O31Cl10The preparation method of composite photo-catalyst.
Background technique
With the increasingly exacerbation of problem of environmental pollution, photocatalysis technology is in terms of photolysis water hydrogen and degradable organic pollutant
More and more paid attention to.Wherein, TiO2Have many advantages, such as that at low cost, photocatalysis stability is good, photocatalysis efficiency is high, is light
Common used material in catalytic field.But TiO2Photochemical catalyst is since its forbidden bandwidth is wide, about 3.1eV, can only by ultraviolet excitation, and
Ultraviolet light only accounts for 5% or so of solar spectrum, low to the utilization rate of sunlight, limits it to a certain extent in environmental improvement
The application of aspect.Therefore, utmostly to utilize solar energy, R and D can be mesh by the new catalyst of excited by visible light
Preceding research emphasis and hot spot.
Bismuth series catalysts are current a kind of novel visible catalysts of greatest concern, it becomes at aspect of curbing environmental pollution
It is now good, increasingly liked by domestic and international researcher.Their most prominent advantages are exactly that forbidden bandwidth is relatively narrow, this
Feature is conducive to its organic pollutant in photocatalytic degradation environment under visible light.Wherein Bi24O31Cl10As a kind of oxygen-enriched
Bismuth series catalysts, due to having the advantage that forbidden bandwidth is small, about 2.8eV can be by excited by visible light;It is chemically and physically stable
Property is good;It is high with unique crystal structure, quantum efficiency, just becoming research hotspot in recent years.Such as Jin uses hydro-thermal legal system
For with a thickness of 300nm, the Bi that width is 1-3 μm24O31Cl10Photochemical catalyst, compared with BiOCl, Bi24O31Cl10In visible light
Visible light can be preferably absorbed under (> 420 nm) irradiation, and effectively can generate O by activating molecules oxygen2·-, to enhance
Bi24O31Cl10Visible light photocatalysis active.The method that Yin etc. is combined using hydro-thermal and heat treatment, is prepared for Bi24O31Cl10
Nanometer sheet is used for the degradation of quadracycline, illumination 150min under visible light, to the degradation rate of quadracycline up to 80% with
On.However, pure Bi24O31Cl10Photoproduction-electron hole it is easily compound, and specific surface area is smaller, causes its photocatalytic activity lower,
Actual industrial application is not able to satisfy still, for this purpose, also need to adopt various measures to improve its photocatalytic activity, such as by energy band position
It is compound to set the different semiconductor materials progress to match, forms hetero-junctions, the compound of material internal electrons and holes can be reduced
Rate.
MoS2It is the photon that a type graphene hexagonal closs packing layer structure material can absorb visible frequency, and it is led
The edge current potential of band and valence band is high, when compound with other photochemical catalysts, can effectively enhance the absorbability to light, and can play fast
The effect of speed transmission electronics.And g-C3N4It is a kind of polymer semiconductor similar to graphene-structured, C, N atom are with sp2 hydridization
Form the pi-conjugated system of height delocalization.g-C3N4Have many advantages, such as that the from a wealth of sources of polymer material, price be low, chemical stabilization,
And have certain absorption to visible light, there is preferable photocatalysis performance.And MoS2With g-C3N4Valence band and conduction band positions with
Bi24O31Cl10Energy good match, forms hetero-junctions, on the one hand enhances Bi24O31Cl10Light absorpting ability, and can effectively subtract
Few Bi24O31Cl10The recombination rate of internal electron and hole, and in Bi24O31Cl10The thin layer MoS of particle surface cladding2With g-C3N4
Nanometer sheet increases the specific surface area of catalyst, the pre- adsorbance of catalyst surface in organic pollutant is increased, to also have
Conducive to the raising of light-catalyzed reaction efficiency.
In view of this, it is necessary to provide a kind of MoS2/g-C3N4/Bi24O31Cl10The preparation method of heterojunction photocatalyst.
Summary of the invention
To solve the above problems, the present invention provides a kind of high activity MoS2/g-C3N4/Bi24O31Cl10Composite photo-catalyst
Preparation method.
Preparation method of the invention, first using bismuth nitrate, ammonium chloride, citric acid as raw material, the improvement solution combustion of use
Method prepares Bi24O31Cl10, the then ultrasonic disperse in methanol solution;Secondly using melamine, acetic acid as raw material, using step heat
Polymerization prepares g-C3N4, the then ultrasonic disperse in methanol solution;Using ammonium molybdate, thiocarbamide as raw material, dimethylformamide is molten
Agent prepares MoS using hydro-thermal method2, ultrasonic disperse is handled in methanol solution.It will finally handle through ultrasonic disperse
Bi24O31Cl10With g-C3N4、MoS2It is dry after then washed, centrifugation after ultrasonic mixing is sufficiently reacted in methanol solution, i.e.,
Obtain MoS2/g-C3N4/Bi24O31Cl10Composite photo-catalyst.
Technical solution of the present invention:
A kind of high activity MoS2/g-C3N4/Bi24O31Cl10The preparation method of composite photo-catalyst, steps are as follows:
(1) using bismuth nitrate, ammonium chloride, citric acid as raw material, Bi is prepared using improved solution combustion method24O31Cl10
Five nitric hydrate bismuths and citric acid are mixed and are dissolved in dust technology, dilute nitre of five nitric hydrate bismuths and citric acid is obtained
The mixed solution of acid, wherein five nitric hydrate bismuths and citric acid molar ratio are 1:2;Ammonium chloride is dissolved in distilled water, until complete
Dissolution, obtains ammonium chloride solution;Under agitation, ammonium chloride solution is added to dilute nitre of five nitric hydrate bismuths and citric acid
In the mixed solution of acid, wherein five nitric hydrate bismuths are 1:1 with ammonium chloride molar ratio, are uniformly mixed to solution in clear state
When, solution ph is adjusted to 5~6 with ammonium hydroxide;3~4h of heating stirring under the conditions of 60 DEG C~80 DEG C, then under the conditions of 600 DEG C
3h is calcined, obtains pale yellow powder, as pure Bi24O31Cl10;
(2) using melamine, acetic acid as raw material, g-C is prepared using a step thermal polymerization3N4
Melamine is uniformly mixed with acetic acid according to the molar ratio of 10:1,2h is calcined at 500 DEG C, obtains yellowish toner
End, as pure g-C3N4;
(3) using ammonium molybdate, thiocarbamide as raw material, dimethylformamide is solvent, prepares MoS using hydro-thermal method2
Compound concentration is the mixed solution of the Ammonium Molybdate Tetrahydrate of 4.8~5.0g/L and the dimethylformamide of thiocarbamide,
In, the mass ratio of Ammonium Molybdate Tetrahydrate and thiocarbamide is 1:2;Stirring, until the dimethylformamide of Ammonium Molybdate Tetrahydrate and thiocarbamide
The transparent state of mixed solution;After reacting for 24 hours at 200 DEG C in a kettle, it is cooled to room temperature;Deionized water washing, centrifugation,
Obtain black solid, by black solid dry 12 at 60 DEG C~100 DEG C~for 24 hours, obtain MoS2;
(4) Bi that step (1) is prepared24O31Cl10Be added in methanol solution, ultrasound, obtain concentration be 40~
The Bi of 50g/L24O31Cl10With the mixed solution of methanol;The g-C that step (2) is prepared3N4It is added to Bi24O31Cl10With first
In the mixed solution of alcohol, wherein g-C3N4With Bi24O31Cl10Mass ratio is 0.01~0.1;Continue ultrasound, be then centrifuged for, wash,
It is centrifuged again, obtains solid matter;Solid matter is dried into for 24 hours~48h under the conditions of 60 DEG C~80 DEG C, grinds, obtains after cooling
1%~10%g-C3N4/ Bi24O31Cl10Composite photo-catalyst;
(5) 5%g-C that step (4) is prepared3N4/Bi24O31Cl10It is added in methanol solution, ultrasound obtains concentration
For the 5%g-C of 40~50g/L3N4/Bi24O31Cl10With the mixed solution of methanol;The MoS that step (3) is prepared2It is added
To 5%g-C3N4/Bi24O31Cl10In the mixed solution of methanol, wherein MoS2With 5%g-C3N4/Bi24O31Cl10Mass ratio
It is 0.03~0.07;Continue ultrasound, is then centrifuged for, washs, is centrifuged again, obtain solid matter;By solid matter 60 DEG C~80
Dry 24~48h at DEG C, grinds after cooling to get 3%~7%MoS2/ 5%g-C3N4/Bi24O31Cl10Composite photo-catalyst.
Beneficial effects of the present invention: after tested, 5%MoS2/ 5%g-C3N4/Bi24O31Cl10To the catalytic degradation of rhodamine B
Rate can reach 99%, while the composite catalyst can also reach 90% or more in 50min to the degradation rate of tetracycline, purer
Bi24O31Cl10, 5%MoS2/Bi24O31Cl10, 5%g-C3N4/Bi24O31Cl10Photocatalysis efficiency be significantly improved.We
Method is simple and easy, low in cost, reproducible, has in fields such as photodegradation water, photochemical catalytic oxidation environmental contaminants extensive
Application prospect.
Detailed description of the invention
Fig. 1 is Bi24O31Cl1、MoS2、g-C3N4, 5%g-C3N4/Bi24O31Cl10, 5%MoS2/Bi24O31Cl10, 5%
MoS2/ 5%g-C3N4/Bi24O31Cl10The XRD spectrum of photochemical catalyst;
Fig. 2 (a) is Bi24O31Cl10The SEM of photochemical catalyst schemes;
Fig. 2 (b) is 5%MoS2/ 5%g-C3N4/Bi24O31Cl10The SEM spectrum of photochemical catalyst;
Fig. 2 (c) is EDS map;
Fig. 3 is the UV-Vis map of photochemical catalyst;Wherein, a indicates Bi24O31Cl10, b indicate 5%g-C3N4/
Bi24O31Cl10, c indicate 5%MoS2/Bi24O31Cl10, d indicate 5%MoS2/ 5%g-C3N4/ Bi24O31Cl10, e indicate MoS2Light
The UV-Vis map of catalyst;
Fig. 4 is Bi24O31Cl10, 5%g-C3N4/Bi24O31Cl10, 5%MoS2/Bi24O31Cl10, 5%MoS2/ 5%g-
C3N4/Bi24O31Cl10The PL map of photochemical catalyst;
Fig. 5 is for photochemical catalyst to the degradation efficiency of rhodamine B under visible light photograph;Wherein, a indicates Bi24O31Cl10, b table
Show 1%g-C3N4/Bi24O31Cl10, c indicate 3%g-C3N4/Bi24O31Cl10, d indicate 5%g-C3N4/Bi24O31Cl10, e indicate
10%g-C3N4/Bi24O31Cl10, f indicate 5%MoS2/Bi24O31Cl10, g indicate 3%MoS2/ 5%g-C3N4/Bi24O31Cl10、h
Indicate 5%MoS2/ 5%g-C3N4/Bi24O31Cl10, i indicate 7%MoS2/ 5%g-C3N4/Bi24O31Cl10;
The Bi of Fig. 6 preparation24O31Cl10, 5%g-C3N4/Bi24O31Cl10, 5%MoS2/Bi24O31Cl10, 5%MoS2/ 5%
g-C3N4/Bi24O31Cl10Photochemical catalyst is under visible light photograph to the degradation efficiency of tetracycline.
Specific embodiment
Below in conjunction with attached drawing and technical solution, a specific embodiment of the invention is further illustrated.
Preparation method through the invention prepares 3%~7%MoS2/ 5%g-C3N4/Bi24O31Cl10Composite photo-catalyst,
And prepare 5%MoS2/Bi24O31Cl10Composite photo-catalyst compares the effect of each composite photo-catalyst.
Embodiment 1
(1)Bi24O31Cl10Preparation: take five nitric hydrate bismuth of 0.01mol to be dissolved in the dust technology of 10% volumetric concentration of 50ml
In, 0.02mol citric acid is then added, is uniformly mixed until being completely dissolved;In addition the ammonium chloride of 0.01mol is dissolved in 50ml
In distilled water, it is uniformly mixed until being completely dissolved.Under constant temperature blender with magnetic force stirring, ammonium chloride solution is slowly injected to five water
In the mixed solution for closing the dust technology of bismuth nitrate and citric acid, when being uniformly mixed to solution in clear state, adjusted using ammonium hydroxide
Then mixed solution pH value continues heating stirring 4h at 60 DEG C, is poured into crucible with cover, then in muffle furnace to 6
3h is calcined at 600 DEG C, obtains pale yellow powder, as pure Bi24O31Cl10。
(2)g-C3N4Preparation: 3g melamine is uniformly mixed with 10 milliliters of acetic acid (concentration 36%), has been put in lid
In crucible, 2h then is calcined at 500 DEG C in muffle furnace, obtains pale yellow powder, as pure g-C3N4。
(3)MoS2Preparation: 80 milligrams of Ammonium Molybdate Tetrahydrates and 160 milligrams of thiocarbamides are dissolved in 50 milliliters of dimethylformamides
Solvent, magnetic agitation until reaction raw materials be dissolved as it is transparent, then go to 100 milliliters of liners be tetrafluoroethene stainless steel hydro-thermal
Reaction kettle is reacted for 24 hours at 200 DEG C, is cooled to room temperature, then high speed centrifugation, distillation water washing 5 under 10000r/min revolving speed
Black solid is obtained after secondary, drying for 24 hours, obtains MoS in drying box 60 DEG C2。
(4) by 2 grams of Bi obtained by step (1)24O31Cl10It is separately added into 40 ml methanol solution, under 1000KW power
Ultrasonic 1h, then in Bi24O31Cl10Be separately added into methanol mixed solution prepared by step (2) 0.02 gram, 0.06 gram,
0.10 gram and 0.2 gram of g-C3N4Powder then proceedes to the ultrasound 1h under 1000KW power, then solid and methanol solution exists
It is centrifuged under 10000r/min revolving speed, is then washed with distilled water, then be centrifuged, the solid obtained after being repeated four times, in drying box
Drying for 24 hours, is ground after cooling up to 1%~10%g-C at 60 DEG C3N4/Bi24O31Cl10Composite photo-catalyst.
(5) 1 gram of 5%g-C for obtaining step (4)3N4/Bi24O31Cl10Sample is added in 20 ml methanol solution,
Ultrasound 1h under 1000KW power, then in 5%g-C3N4/Bi24O31Cl10It is made that step (3) is separately added into methanol mixed solution
Standby 0.3g MoS2Powder then proceedes to the ultrasound 1h under 1000KW power, then by solid and methanol solution in 10000r/
It is centrifuged under min revolving speed, is then washed with distilled water, then be centrifuged, the solid obtained after being repeated four times is done in drying box 60 DEG C
Dry 48h is ground after cooling up to 3%MoS2/ 5%g-C3N4/Bi24O31Cl10Composite photo-catalyst.
(6) by 1 gram of Bi obtained by step (1)24O31Cl10It is added in 20 ml methanol solution, it is ultrasonic under 1000KW power
1h, then in Bi24O31Cl10With 0.5 gram of MoS prepared by addition step (3) in methanol mixed solution2Powder then proceedes to
Solid and methanol solution, are then centrifuged under 10000r/min revolving speed, then use distilled water by the ultrasound 1h under 1000KW power
Washing, then be centrifuged, the solid obtained after being repeated four times, drying for 24 hours, is ground after cooling up to 5% in drying box 60 DEG C
MoS2/Bi24O31Cl10Composite photo-catalyst.
Embodiment 2
(1)Bi24O31Cl10Preparation: take five nitric hydrate bismuth of 0.01mol to be dissolved in the dust technology of 10% volumetric concentration of 50ml
In, 0.02mol citric acid is then added, is uniformly mixed until being completely dissolved;In addition the ammonium chloride of 0.01mol is dissolved in 50ml
In distilled water, it is uniformly mixed until being completely dissolved.Under constant temperature blender with magnetic force stirring, ammonium chloride solution is slowly injected to five water
In the mixed solution for closing the dust technology of bismuth nitrate and citric acid, when being uniformly mixed to solution in clear state, adjusted using ammonium hydroxide
Then mixed solution pH value continues heating stirring 3h at 80 DEG C, is poured into crucible with cover, then in muffle furnace to 5
3h is calcined at 600 DEG C, obtains pale yellow powder, as pure Bi24O31Cl10。
(2)g-C3N4Preparation: 3g melamine is uniformly mixed with 10 milliliters of acetic acid (concentration 36%), has been put in lid
In crucible, 2h then is calcined at 500 DEG C in muffle furnace, obtains pale yellow powder, as pure g-C3N4。
(3)MoS2Preparation: 60 milligrams of Ammonium Molybdate Tetrahydrates and 120 milligrams of thiocarbamides are dissolved in 36 milliliters of dimethylformamides
Solvent, magnetic agitation until reaction raw materials be dissolved as it is transparent, then go to 50 milliliters of liners be tetrafluoroethene stainless steel hydro-thermal
Reaction kettle is reacted for 24 hours at 200 DEG C, is cooled to room temperature, then high speed centrifugation, distillation water washing 5 under 10000r/min revolving speed
Black solid is obtained after secondary, dry 12h, obtains MoS in drying box 100 DEG C2。
(4) by 1 gram of Bi obtained by step (1)24O31Cl10It is separately added into 25 ml methanol solution, under 1000KW power
Ultrasonic 1h, then in Bi24O31Cl10Be separately added into methanol mixed solution prepared by step (2) 0.01 gram, 0.03 gram,
0.05 gram and 0.1 gram of g-C3N4Powder then proceedes to the ultrasound 1h under 1000KW power, then solid and methanol solution exists
It is centrifuged under 10000r/min revolving speed, is then washed with distilled water, then be centrifuged, the solid obtained after being repeated four times, in drying box
Dry 48h, grinds after cooling up to 1%~10%g-C at 80 DEG C3N4/Bi24O31Cl10Composite photo-catalyst.
(5) 1.8 grams of 5%g-C for obtaining step (4)3N4/Bi24O31Cl10Sample is added in 40 ml methanol solution,
Ultrasound 1h under 1000KW power, then in 5%g-C3N4/Bi24O31Cl10It is made that step (3) is separately added into methanol mixed solution
Standby 0.09g MoS2Powder then proceedes to the ultrasound 1h under 1000KW power, then by solid and methanol solution in 10000r/
It is centrifuged under min revolving speed, is then washed with distilled water, then be centrifuged, the solid obtained after being repeated four times is done in drying box 80 DEG C
It is dry for 24 hours, ground after cooling up to 5%MoS2/ 5%g-C3N4/Bi24O31Cl10Composite photo-catalyst.
(6) by 1 gram of Bi obtained by step (1)24O31Cl10It is added in 20 ml methanol solution, it is ultrasonic under 1000KW power
1h, then in Bi24O31Cl10With 0.5 gram of MoS prepared by addition step (3) in methanol mixed solution2Powder then proceedes to
Solid and methanol solution, are then centrifuged under 10000r/min revolving speed, then use distilled water by the ultrasound 1h under 1000KW power
Washing, then be centrifuged, the solid obtained after being repeated four times, drying for 24 hours, is ground after cooling up to 5% in drying box 60 DEG C
MoS2/Bi24O31Cl10Composite photo-catalyst.
Embodiment 3
(1)Bi24O31Cl10Preparation: take five nitric hydrate bismuth of 0.01mol to be dissolved in the dust technology of 10% volumetric concentration of 50ml
In, 0.02mol citric acid is then added, is uniformly mixed until being completely dissolved;In addition the ammonium chloride of 0.01mol is dissolved in 50ml
In distilled water, it is uniformly mixed until being completely dissolved.Under constant temperature blender with magnetic force stirring, ammonium chloride solution is slowly injected to five water
In the mixed solution for closing the dust technology of bismuth nitrate and citric acid, when being uniformly mixed to solution in clear state, adjusted using ammonium hydroxide
Then mixed solution pH value continues heating stirring 3.5h at 60 DEG C, is poured into crucible with cover, then in muffle furnace to 6
In calcine 3h at 600 DEG C, obtain pale yellow powder, as pure Bi24O31Cl10。
(2)g-C3N4Preparation: 3g melamine is uniformly mixed with 10 milliliters of acetic acid (concentration 36%), has been put in lid
In crucible, 2h then is calcined at 500 DEG C in muffle furnace, obtains pale yellow powder, as pure g-C3N4。
(3)MoS2Preparation: 45 milligrams of Ammonium Molybdate Tetrahydrates and 90 milligrams of thiocarbamides are dissolved in 27.5 milliliters of dimethyl formyls
Amine solvent, magnetic agitation until reaction raw materials be dissolved as it is transparent, then go to 50 milliliters of liners be tetrafluoroethene stainless steel water
Thermal response kettle is reacted for 24 hours at 200 DEG C, is cooled to room temperature, then high speed centrifugation, distillation water washing under 10000r/min revolving speed
Black solid is obtained after 5 times, dry 18h, obtains MoS in drying box 80 DEG C2。
(4) by 9 grams of Bi obtained by step (1)24O31Cl10It is separately added into 200 ml methanol solution, under 1000KW power
Ultrasonic 1h, then in Bi24O31Cl10Be separately added into methanol mixed solution prepared by step (2) 0.09 gram, 0.27 gram,
0.45 gram and 0.9 gram of g-C3N4Powder then proceedes to the ultrasound 1h under 1000KW power, then solid and methanol solution exists
It is centrifuged under 10000r/min revolving speed, is then washed with distilled water, then be centrifuged, the solid obtained after being repeated four times, in drying box
Dry 36h, grinds after cooling up to 1%~10%g-C at 70 DEG C3N4/Bi24O31Cl10Composite photo-catalyst.
(5) 1.5 grams of 5%g-C for obtaining step (4)3N4/Bi24O31Cl10Sample is added in 30 ml methanol solution,
Ultrasound 1h under 1000KW power, then in 5%g-C3N4/Bi24O31Cl10It is made that step (3) is separately added into methanol mixed solution
Standby 0.105g MoS2Powder then proceedes to the ultrasound 1h under 1000KW power, then solid and methanol solution exists
It is centrifuged under 10000r/min revolving speed, is then washed with distilled water, then be centrifuged, the solid obtained after being repeated four times, in drying box
Dry 36h, grinds after cooling up to 7%MoS at 70 DEG C2/ 5%g-C3N4/Bi24O31Cl10Composite photo-catalyst.
(6) by 1 gram of Bi obtained by step (1)24O31Cl10It is added in 20 ml methanol solution, it is ultrasonic under 1000KW power
1h, then in Bi24O31Cl10With 0.5 gram of MoS prepared by addition step (3) in methanol mixed solution2Powder then proceedes to
Solid and methanol solution, are then centrifuged under 10000r/min revolving speed, then use distilled water by the ultrasound 1h under 1000KW power
Washing, then be centrifuged, the solid obtained after being repeated four times, drying for 24 hours, is ground after cooling up to 5% in drying box 60 DEG C
MoS2/Bi24O31Cl10Composite photo-catalyst.
Structure and morphology characterization:
It will be seen from figure 1 that the Bi of preparation24O31Cl10With JCPDS standard card number (No.75-0887) tetragonal crystal system
Bi24O31Cl10Diffraction maximum matches.5%g-C3N4/Bi24O31Cl10Without g-C in sample3N4Peak, 5%MoS2/Bi24O31Cl10、
Without MoS in sample2Peak, 5%MoS2/ 5%g-C3N4/Bi24O31Cl105% there are no g-C3N4And MoS2Peak, mainly by
In compound g-C3N4And MoS2Amount it is less caused by.
From Fig. 2 (a), 2 (b) and 2 (c) as can be seen that the 5%MoS of preparation2/ 5%g-C3N4/Bi24O31Cl10In sample at
Function is compounded with g-C3N4And MoS2。
From figure 3, it can be seen that working as Bi24O31Cl10With MoS2Or g-C3N4After compound, the absorbing properties of sample are obtained obviously
It is promoted, wherein compound MoS2The more compound g-C of the absorbing properties of sample afterwards3N4It is promoted more significant, works as MoS2With g-C3N4Simultaneously
Compound Bi24O31Cl10When absorbing properties promoted maximum, have apparent light absorption within the scope of 200-800nm.
From fig. 4, it can be seen that 5%MoS2/ 5%g-C3N4/Bi24O31Cl10PL peak intensity it is minimum, illustrate the photochemical catalyst
Minimum, the lower recombination rate of photoexcited electron-hole recombination rate, be conducive to the raising of photocatalytic activity.
Photocatalytic activity test experiments:
Taking initial concentration is 5mgL-1Rhodamine B (RhB) solution 100mL or 20mgL-1Quadracycline solution
50mL is placed in 250mL beaker as target degradation product, then adds 0.03g photochemical catalyst in rhodamine B or quadracycline
In solution, it is uniformly mixed.Before illumination, first by this suspension in darkroom magnetic agitation 30min, make photochemical catalyst and rhodamine
Reach adsorption-desorption balance between B or tetracycline, is then placed on visible light source (the 250W gold halogen away from liquid level 14cm
Lamp) under carry out photocatalysis experiment.Light application time is 50min, wherein the rubber head dropper every 10min cleaning takes supernatant,
Centrifugation is placed in cuvette, its absorbance, root are surveyed at the maximum absorption wavelength 554nm and 356nm of rhodamine B and tetracycline
According to langbobier law, the removal rate D of rhodamine B or tetracycline can be calculated by formula (1):
D=(C0-C)/C0× 100%=(A0’-A)/A0' × 100% (1)
In formula: C0, C --- before illumination and illumination after the concentration of rhodamine B or tetracycline;
A0', A --- before illumination and illumination after the absorbance of rhodamine B or tetracycline
5%MoS as shown in Figure 52/ 5%g-C3N4/Bi24O31Cl10It can in 50min to the catalysis degradation modulus of rhodamine B
Reach 90%, while the composite catalyst can also reach 88% or so (as shown in Figure 6) in 50min to the degradation rate of tetracycline,
Purer Bi24O31Cl10, 5%MoS2/Bi24O31Cl10, 5%g-C3N4/ Bi24O31Cl10Photocatalysis efficiency obtained significantly mentioning
Height illustrates using MoS2And g-C3N4It is compound to Bi simultaneously24O31Cl10Activity promoted it is obvious.
Claims (1)
1. a kind of high activity MoS2/g-C3N4/Bi24O31Cl10The preparation method of composite photo-catalyst, which is characterized in that step is such as
Under:
(1) using bismuth nitrate, ammonium chloride, citric acid as raw material, Bi is prepared using improved solution combustion method24O31Cl10
Five nitric hydrate bismuths and citric acid are mixed and are dissolved in dust technology, the dust technology of five nitric hydrate bismuths and citric acid is obtained
Mixed solution, wherein five nitric hydrate bismuths and citric acid molar ratio are 1:2;Ammonium chloride is dissolved in distilled water, until completely molten
Solution, obtains ammonium chloride solution;Under agitation, ammonium chloride solution is added to the dust technology of five nitric hydrate bismuths and citric acid
Mixed solution in, wherein five nitric hydrate bismuths and ammonium chloride molar ratio are 1:1, when being uniformly mixed to solution in clear state,
Solution ph is adjusted to 5~6 with ammonium hydroxide;3~4h of heating stirring under the conditions of 60 DEG C~80 DEG C, is then forged under the conditions of 600 DEG C
3h is burnt, obtains pale yellow powder, as pure Bi24O31Cl10;
(2) using melamine, acetic acid as raw material, g-C is prepared using a step thermal polymerization3N4
Melamine is uniformly mixed with acetic acid according to the molar ratio of 10:1,2h is calcined at 500 DEG C, obtains pale yellow powder,
As pure g-C3N4;
(3) using ammonium molybdate, thiocarbamide as raw material, dimethylformamide is solvent, prepares MoS using hydro-thermal method2Compound concentration is 4.8
The mixed solution of the dimethylformamide of the Ammonium Molybdate Tetrahydrate and thiocarbamide of~5.0g/L, wherein Ammonium Molybdate Tetrahydrate and thiocarbamide
Mass ratio be 1:2;Stirring, until the transparent state of mixed solution of the dimethylformamide of Ammonium Molybdate Tetrahydrate and thiocarbamide;
After reacting for 24 hours at 200 DEG C in a kettle, it is cooled to room temperature;Deionized water washing, centrifugation, obtain black solid, black are consolidated
Body dry 12 at 60 DEG C~100 DEG C~for 24 hours, obtain MoS2;
(4) Bi that step (1) is prepared24O31Cl10It is added in methanol solution, ultrasound, obtaining concentration is 40~50g/L
Bi24O31Cl10With the mixed solution of methanol;The g-C that step (2) is prepared3N4It is added to Bi24O31Cl10With mixing for methanol
It closes in solution, wherein g-C3N4With Bi24O31Cl10Mass ratio is 0.01~0.1;Continue ultrasound, be then centrifuged for, wash, again from
The heart obtains solid matter;By solid matter under the conditions of 60 DEG C~80 DEG C it is dry for 24 hours~48h, ground after cooling, obtain 1%~
10%g-C3N4/Bi24O31Cl10Composite photo-catalyst;
(5) 5%g-C that step (4) is prepared3N4/Bi24O31Cl10It is added in methanol solution, ultrasound, obtaining concentration is 40
The 5%g-C of~50g/L3N4/Bi24O31Cl10With the mixed solution of methanol;The MoS that step (3) is prepared2It is added to 5%
g-C3N4/Bi24O31Cl10In the mixed solution of methanol, wherein MoS2With 5%g-C3N4/Bi24O31Cl10Mass ratio be 0.03
~0.07;Continue ultrasound, is then centrifuged for, washs, is centrifuged again, obtain solid matter;Solid matter is done at 60 DEG C~80 DEG C
Dry 24~48h is ground after cooling to get 3%~7%MoS2/ 5%g-C3N4/Bi24O31Cl10Composite photo-catalyst.
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