CN106994360A - A kind of preparation method of Z configurations visible light catalytic decomposition water composite - Google Patents
A kind of preparation method of Z configurations visible light catalytic decomposition water composite Download PDFInfo
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- CN106994360A CN106994360A CN201710217326.3A CN201710217326A CN106994360A CN 106994360 A CN106994360 A CN 106994360A CN 201710217326 A CN201710217326 A CN 201710217326A CN 106994360 A CN106994360 A CN 106994360A
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- molybdenum disulfide
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000002131 composite material Substances 0.000 title claims abstract description 35
- 238000003421 catalytic decomposition reaction Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 92
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 80
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 48
- 239000007788 liquid Substances 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 31
- 239000002243 precursor Substances 0.000 claims abstract description 30
- 239000006185 dispersion Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 21
- 239000010452 phosphate Substances 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 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 abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 239000011734 sodium Substances 0.000 claims abstract description 16
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 16
- 239000001488 sodium phosphate Substances 0.000 claims abstract description 16
- 238000013019 agitation Methods 0.000 claims abstract description 15
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 9
- 229910000162 sodium phosphate Inorganic materials 0.000 claims abstract description 8
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims abstract description 6
- 238000001556 precipitation Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- 238000005452 bending Methods 0.000 claims abstract description 3
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 239000002135 nanosheet Substances 0.000 claims abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 27
- 229910052760 oxygen Inorganic materials 0.000 claims description 27
- 239000001301 oxygen Substances 0.000 claims description 27
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 4
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 235000015393 sodium molybdate Nutrition 0.000 claims description 2
- 239000011684 sodium molybdate Substances 0.000 claims description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 29
- 230000001699 photocatalysis Effects 0.000 abstract description 22
- 239000011941 photocatalyst Substances 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000003643 water by type Substances 0.000 description 24
- 229910052961 molybdenite Inorganic materials 0.000 description 22
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 description 13
- 239000012153 distilled water Substances 0.000 description 12
- 239000012467 final product Substances 0.000 description 12
- 238000005406 washing Methods 0.000 description 12
- 238000007146 photocatalysis Methods 0.000 description 11
- 239000011733 molybdenum Substances 0.000 description 10
- 229910052750 molybdenum Inorganic materials 0.000 description 10
- NFIYTPYOYDDLGO-UHFFFAOYSA-N phosphoric acid;sodium Chemical compound [Na].OP(O)(O)=O NFIYTPYOYDDLGO-UHFFFAOYSA-N 0.000 description 9
- 235000011008 sodium phosphates Nutrition 0.000 description 9
- 239000007921 spray Substances 0.000 description 9
- 238000002604 ultrasonography Methods 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 229910000397 disodium phosphate Inorganic materials 0.000 description 4
- 235000019800 disodium phosphate Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- -1 molybdenum disulfide compound Chemical class 0.000 description 3
- 239000002057 nanoflower Substances 0.000 description 3
- NDYNABNWLRVCDO-UHFFFAOYSA-N phosphoric acid silver Chemical compound [Ag].P(O)(O)(O)=O NDYNABNWLRVCDO-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910021389 graphene Inorganic materials 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000021317 phosphate Nutrition 0.000 description 2
- 238000006303 photolysis reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000004577 artificial photosynthesis Methods 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 239000012482 calibration solution Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
-
- 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
-
- B01J35/39—
Abstract
The present invention relates to photocatalytic water material, a kind of Z configurations visible light catalytic decomposition water composite and preparation method thereof is refered in particular to.Silver nitrate solution is added dropwise in flower-shaped molybdenum disulfide dispersion liquid under stirring condition, stirring obtains mixing precursor solution；Weigh phosphate to be dissolved in deionized water, obtain phosphate solution；Under agitation, sodium radio-phosphate,P-32 solution is added in the mixing precursor solution prepared, as the addition solution of sodium phosphate gradually becomes celadon precipitation, completion of dropping mixed solution continues to stir 3h, and final reaction thing precipitation respectively washes three vacuum dryings using deionized water and ethanol.The bending basal plane of flower-shaped molybdenum disulfide formation can turn into the chief active position of light-catalyzed reaction, and be better than molybdenum disulfide nano sheet in the absorption region of visible ray, can further improve the performance of composite photo-catalyst.
Description
Technical field
The present invention relates to photocatalytic water material, a kind of Z configurations visible light catalytic decomposition water composite and its preparation side are refered in particular to
Method, particularly relates to one kind and prepares phosphoric acid silver-based composite visible light catalysis material using ion-exchange electrostatic self-assembled in aqueous
The method of material, belongs to nano composite material, photocatalytic water technology and photocatalysis field.
Background technology
In recent years, the Z configuration photochemical catalyzing semiconductor composite systems based on artificial photosynthesis are by extensive
Two kinds of semi-conducting materials in concern, Z configuration compound systems need to only meet the oxidation-reduction process at light decomposition water two ends respectively, electricity
The presence of sub- transmission medium realizes effective transmission and separation in electronics and hole, and light decomposition water process is relatively easy and efficiency
It is high.In addition alternative water oxygen and the semiconductor material combinations of proton reduction are also more, are solar energy photocatalytic decomposition water
The design of semi-conducting material provides larger selection space, while also constructing for Z configuration photochemical catalyzing compound systems
New thinking is opened up.
Leaf golden flower seminars report that silver orthophosphate under visible light illumination there is preferable photodissociation aquatic products oxygen to live for 2010 first
Property.With good valence band (2.9eV or so) and conduction band potential (0.45eV or so), the narrower energy absorbing wavelength of its band gap is less than
530nm visible ray.After excited by visible light is absorbed, the oxidability for staying in hole in silver orthophosphate valence band location is strong, Neng Gougao
Effect decomposes aquatic products oxygen.But there is clearly disadvantageous part in pure phosphoric acid ag material：(1) light induced electron produced in photocatalytic process
Generation self-corrosion can not be efficiently separated, causes photocatalytic activity and bad stability；(2) pure phosphoric acid ag material is applied to photocatalytic water
Produce oxygen system cost relatively higher.Related seminar is by by silver orthophosphate and TiO in recent years2、BiVO4、Co3O4Deng semiconductor material
The carbon-based material such as material or graphene, carbon quantum dot is effectively combined, and prepares stability and the enhanced phosphoric acid silver-based of photocatalytic activity
Composite photocatalyst material.The bending basal plane of flower-shaped molybdenum disulfide formation can turn into the chief active position of light-catalyzed reaction, and
It is better than molybdenum disulfide nano sheet in the absorption region of visible ray, in this experiment, we utilize silver orthophosphate and flower-shaped curing
Molybdenum is combined, and is compared, is urged further to probe into and improve complex light by the flaky molybdenum disulfide compound system peeled off with ultrasound
The performance of agent.
MoS2As a kind of typical transition metal stratiform compound, the main component of molybdenite is MoS in nature2,
It has similar sandwich structure, in theory MoS2Compare TiO2There is a more preferable photocatalysis performance, the correspondence absorbing wavelength upper limit is 690~
1030nm, has good matching with sunshine, especially in visible region, is utilized in theory with higher sunshine
Rate, and its conduction band and the edge current potential of valence band are high, photo-generated carrier can be separated in time, and it is introduced using molybdenum disulfide as carrier
Its nano-particle, sets up Z configuration carrier transport passages, can be effectively increased photocatalysis performance.
The content of the invention
It is an object of the invention to provide a kind of flow is simple, environment-friendly, the Z configurations with low cost for preparing controllable appearance
Visible light catalytic decomposition water composite and preparation method thereof, the composite photocatalyst material of preparation have controllable appearance structure,
Good visible light-responded characteristic and excellent photocatalytic water performance.
The technical solution adopted in the present invention is：The flower-shaped molybdenum disulfide prepared using conventional hydrothermal method is presoma, is led to
Crossing ion-exchange makes nano silver particle effectively be assembled on molybdenum disulfide matrix, and its specific preparation method step is as follows：
(1) a molybdate and a thiocarbamide are quantitatively weighed, both are mixed by certain mol proportion, and 150mL beaker is put into together
In, the inside adds 70mL deionized water, stirring 0.5h to dissolving；
(2) above-mentioned solution is transferred in 100mL reactor, tightens and be put into 180 DEG C of heating 24h in baking oven, be made flower-shaped two
Molybdenum sulfide, it is standby that subsequent taking-up sample respectively cleans three vacuum dryings with deionized water and ethanol；(3) next weigh obtained
Flower-shaped molybdenum disulfide, ultrasonic disperse uniformly obtains the flower-shaped molybdenum disulfide dispersion liquid that concentration is 0.04~0.04wt%；
(4) weigh silver nitrate to be dissolved into deionized water, obtain silver nitrate solution；Under stirring condition by silver nitrate solution by
It is added dropwise in flower-shaped molybdenum disulfide dispersion liquid A, stirs 6-12h, obtain mixing precursor solution, silver nitrate is dense in mixed solution
Spend for 0.15mol/L；
(5) will be 3 by silver nitrate and sodium phosphate mol ratio:1 ratio, weighs phosphate and is dissolved in deionized water, obtain
0.2mol/L phosphate solution；
(6) under agitation, it is molten that the sodium radio-phosphate,P-32 solution prepared by step (5) is slowly added into the mixing precursor prepared
In liquid, as the addition solution of sodium phosphate gradually becomes celadon precipitation, completion of dropping mixed solution continues to stir 3h, last anti-
Thing precipitation is answered respectively to wash three vacuum dryings using deionized water and ethanol.
Molybdate described in step 1 is sodium molybdate or ammonium molybdate.
The ratio between sulfur content and molybdenum element content are 3 in the molybdenum disulfide preparation process:1~9:1.
The present invention has advantages below compared with prior art：
A) flower-shaped molybdenum disulfide nano material has controllable pattern and uniform-dimension, and silver orthophosphate can be controllable in its surface in situ
Growth, so as to form the composite with controllable appearance and interface；
B) by the cooperative effect between silver orthophosphate and molybdenum disulfide, obtained catalysis material has wider visible light-responded
Scope, higher photocatalytic water efficiency and preferable cyclical stability；
C) composite prepared by forms the Z configuration photocatalysis based on total solidity electronic transmission medium under visible optical drive
System, so as to effectively improve the efficiency and stability of photocatalytic water material.
D) using molybdenum disulfide as presoma, the active attachment point on molybdenum disulfide surface can effectively control silver orthophosphate
The size of grain.
E) molybdenum disulfide has class graphene-structured, makes to be combined with larger specific surface area and higher carrier transport
Catalysis material has good dispersiveness, adsorptivity and relatively low electron-hole plyability, makes material under visible light action
With efficient photocatalysis performance.
F) prepare technique is simple, with low cost, the superior performance of energy-conserving and environment-protective and material.
G) molybdenum disulfide does not have the shortcoming of the band gap of graphene zero, and platelike molybdenumdisulfide specific surface area is big, electron transport ability
By force, there is good absorption under visible light, the visible luminous effect of composite is fast, and photocatalysis effect is further improved.
Brief description of the drawings
Fig. 1 is visible relatively thin flower of taking measurements greatly in the scanning electron microscope (SEM) photograph of prepared molybdenum disulfide nano floral material, figure
Shape molybdenum disulfide material；The size of resulting molybdenum disulfide nano flower is between 50-200nm.Molybdenum disulfide nano is spent in Fig. 2
Transmission electron microscope picture show that the thickness of resulting molybdenum disulfide nano flower is between 2~10nm.
Fig. 3 is Z configurations catalytic decomposition spray shape MoS2The scanning electron microscope diagram of composite.
Fig. 4 is Z configurations catalytic decomposition water sheet MoS2The scanning electron microscope diagram of composite.
Fig. 5 is Z configurations catalytic decomposition spray shape MoS2The transmission electron microscope figure of composite.
Fig. 6 is Z configurations catalytic decomposition spray shape MoS2The X-ray diffractogram of composite.
Fig. 7 is Z configurations catalytic decomposition spray shape MoS2The UV-vis DRS spectrogram of composite.
Fig. 8 is Z configurations catalytic decomposition spray shape MoS2The photocatalysis Decomposition aquatic products oxygen design sketch of composite.
Fig. 9 is Z configurations catalytic decomposition water sheet MoS2The photocatalysis Decomposition aquatic products oxygen design sketch of composite.
Embodiment
Present disclosure, typical but non-limiting reality of the invention is expanded on further below in conjunction with specific embodiment
Under for example：
Embodiment 1
By the flower-shaped molybdenum disulfide ultrasonic disperses of 20mg in 50mL deionized waters, ultrasound 10 minutes obtains molybdenum disulfide dispersion liquid,
Weigh 3.06g silver nitrates to be dissolved in 50mL distilled water, obtain silver nitrate solution, toward flower-shaped curing under magnetic stirrer
The silver nitrate solution configured is added in molybdenum dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh 2.28g phosphoric acid
Sodium, is dissolved in 30mL deionized waters, obtains sodium radio-phosphate,P-32 solution, equally under the conditions of magnetic agitation, by sodium radio-phosphate,P-32 solution by
Mixing precursor solution is added dropwise to, reaction system engenders that celadon is muddy, and mixed solution continues to stir 3 after completion of dropping
Hour, final product is washed three times through washing three alcohol.
Embodiment 2
By the flower-shaped molybdenum disulfide ultrasonic disperses of 50mg in 50mL deionized waters, ultrasound 10 minutes obtains molybdenum disulfide dispersion liquid,
Weigh 3.06g silver nitrates to be dissolved in 30mL distilled water, obtain silver nitrate solution, toward flower-shaped curing under magnetic stirrer
The silver nitrate solution configured is added in molybdenum dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh 2.28g phosphoric acid
Sodium, is dissolved in 30mL deionized waters, obtains sodium radio-phosphate,P-32 solution, equally under the conditions of magnetic agitation, by sodium radio-phosphate,P-32 solution by
Mixing precursor solution is added dropwise to, reaction system engenders that celadon is muddy, and mixed solution continues to stir 3 after completion of dropping
Hour, final product is washed three times through washing three alcohol.
Embodiment 3
By the flower-shaped molybdenum disulfide ultrasonic disperses of 100mg in 50mL deionized waters, ultrasound 10 minutes obtains molybdenum disulfide and disperseed
Liquid, weighs 3.06g silver nitrates and is dissolved in 30mL distilled water, obtain silver nitrate solution, toward curing under magnetic stirrer
The silver nitrate solution configured is added in molybdenum dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh 2.28g phosphoric acid
Sodium, is dissolved in 30mL deionized waters, obtains sodium radio-phosphate,P-32 solution, equally under the conditions of magnetic agitation, by sodium radio-phosphate,P-32 solution by
Mixing precursor solution is added dropwise to, reaction system engenders that celadon is muddy, and mixed solution continues to stir 3 after completion of dropping
Hour, final product is washed three times through washing three alcohol.
Embodiment 4
By the flower-shaped molybdenum disulfide ultrasonic disperses of 200mg in 50mL deionized waters, ultrasound 10 minutes obtains molybdenum disulfide and disperseed
Liquid, weighs 3.06g silver nitrates and is dissolved in 30mL distilled water, obtain silver nitrate solution, slowly toward two under magnetic stirrer
The silver nitrate solution configured is added in molybdenum sulfide dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh 2.28g
Sodium phosphate, is dissolved in 30mL deionized waters, obtains sodium radio-phosphate,P-32 solution, equally under the conditions of magnetic agitation, sodium phosphate is molten
Mixing precursor solution is added dropwise in liquid, and reaction system engenders that celadon is muddy, and mixed solution continues to stir after completion of dropping
Mix 3 hours, final product is washed three times through washing three alcohol.
Embodiment 5
By the flower-shaped molybdenum disulfide ultrasonic disperses of 20mg in 50mL deionized waters, ultrasound 10 minutes obtains molybdenum disulfide dispersion liquid,
Weigh 3.06g silver nitrates to be dissolved in 30mL distilled water, obtain silver nitrate solution, toward molybdenum disulfide point under magnetic stirrer
The silver nitrate solution configured is added in dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh 2.15g phosphoric acid hydrogen two
Sodium, is dissolved in 30mL deionized waters, obtains disodium phosphate soln, equally under the conditions of magnetic agitation, sodium phosphate is molten
Mixing precursor solution is added dropwise in liquid, and reaction system engenders that celadon is muddy, and mixed solution continues to stir after completion of dropping
Mix 3 hours, final product is washed three times through washing three alcohol.
Embodiment 6
By the flower-shaped molybdenum disulfide ultrasonic disperses of 50mg in 50mL deionized waters, ultrasound 10 minutes obtains molybdenum disulfide dispersion liquid,
Weigh 3.06g silver nitrates to be dissolved in 30mL distilled water, obtain silver nitrate solution, in the case where magnetic stirring apparatus is quickly stirred slowly toward two
The silver nitrate solution configured is added in molybdenum sulfide dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh 2.15g
Disodium hydrogen phosphate, is dissolved in 30mL deionized waters, obtains disodium phosphate soln, equally under the conditions of magnetic agitation, will
Mixing precursor solution is added dropwise in sodium radio-phosphate,P-32 solution, and reaction system engenders that celadon is muddy, mixes molten after completion of dropping
Liquid continues to stir 3 hours, and final product is washed three times through washing three alcohol.
Embodiment 7
By the flower-shaped molybdenum disulfide ultrasonic disperses of 100mg in 50mL deionized waters, ultrasound 10 minutes obtains molybdenum disulfide and disperseed
Liquid, weighs 3.06g silver nitrates and is dissolved in 30mL distilled water, obtain silver nitrate solution, toward curing under magnetic stirrer
The silver nitrate solution configured is added in molybdenum dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh 2.15g phosphoric acid
Disodium hydrogen, is dissolved in 30mL deionized waters, obtains disodium phosphate soln, equally under the conditions of magnetic agitation, by phosphoric acid
Sodium solution is added dropwise mixing precursor solution, and reaction system engenders that celadon is muddy, after completion of dropping mixed solution after
3 hours of continuous stirring, final product is washed three times through washing three alcohol.
Embodiment 8
By the flower-shaped molybdenum disulfide ultrasonic disperses of 200mg in 50mL deionized waters, ultrasound 10 minutes obtains molybdenum disulfide and disperseed
Liquid, weighs 3.06g silver nitrates and is dissolved in 30mL distilled water, obtain silver nitrate solution, toward curing under magnetic stirrer
The silver nitrate solution configured is added in molybdenum dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh 2.15g phosphoric acid
Disodium hydrogen, is dissolved in 30mL deionized waters, obtains disodium phosphate soln, equally under the conditions of magnetic agitation, by phosphoric acid
Sodium solution is added dropwise mixing precursor solution, and reaction system engenders that celadon is muddy, after completion of dropping mixed solution after
3 hours of continuous stirring, final product is washed three times through washing three alcohol.
Embodiment 9
By 20mg flaky molybdenum disulfides ultrasonic disperse in 50mL deionized waters, ultrasonic time is 20min, obtains sheet curing
Molybdenum dispersion liquid, weighs 3.06g silver nitrates and is dissolved in 30mL distilled water, obtain silver nitrate solution, past under magnetic stirrer
The silver nitrate solution configured is added in molybdenum disulfide dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh
2.28g sodium phosphates, are dissolved in 30mL deionized waters, obtain sodium radio-phosphate,P-32 solution, equally under the conditions of magnetic agitation, by phosphoric acid
Sodium solution is added dropwise mixing precursor solution, and reaction system engenders that celadon is muddy, after completion of dropping mixed solution after
3 hours of continuous stirring, final product is washed three times through washing three alcohol.
Embodiment 10
By 50mg flaky molybdenum disulfides ultrasonic disperse in 50mL deionized waters, ultrasonic time is 20min, obtains sheet curing
Molybdenum dispersion liquid, weighs 3.06g silver nitrates and is dissolved in 30mL distilled water, obtain silver nitrate solution, past under magnetic stirrer
The silver nitrate solution configured is added in molybdenum disulfide dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh
2.28g sodium phosphates, are dissolved in 30mL deionized waters, obtain sodium radio-phosphate,P-32 solution, equally under the conditions of magnetic agitation, by phosphoric acid
Sodium solution is added dropwise mixing precursor solution, and reaction system engenders that celadon is muddy, after completion of dropping mixed solution after
3 hours of continuous stirring, final product is washed three times through washing three alcohol.
Embodiment 11
By 100mg flaky molybdenum disulfides ultrasonic disperse in 50mL deionized waters, ultrasonic time is 20min, obtains the sulphur of sheet two
Change molybdenum dispersion liquid, weigh 3.06g silver nitrates and be dissolved in 30mL distilled water, obtain silver nitrate solution, under magnetic stirrer
The silver nitrate solution configured is added into molybdenum disulfide dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh
2.28g sodium phosphates, are dissolved in 30mL deionized waters, obtain sodium radio-phosphate,P-32 solution, equally under the conditions of magnetic agitation, by phosphoric acid
Sodium solution is added dropwise mixing precursor solution, and reaction system engenders that celadon is muddy, after completion of dropping mixed solution after
3 hours of continuous stirring, final product is washed three times through washing three alcohol.
Embodiment 12
By 200mg flaky molybdenum disulfides ultrasonic disperse in 50mL deionized waters, ultrasonic time is 20min, obtains the sulphur of sheet two
Change molybdenum dispersion liquid, weigh 3.06g silver nitrates and be dissolved in 30mL distilled water, obtain silver nitrate solution, under magnetic stirrer
The silver nitrate solution configured is added into molybdenum disulfide dispersion liquid, is stirred 12 hours, obtains mixing precursor solution；Weigh
2.28g sodium phosphates, are dissolved in 30mL deionized waters, obtain sodium radio-phosphate,P-32 solution, equally under the conditions of magnetic agitation, by phosphoric acid
Sodium solution is added dropwise mixing precursor solution, and reaction system engenders that celadon is muddy, after completion of dropping mixed solution after
3 hours of continuous stirring, final product is washed three times through washing three alcohol.
Fig. 1 and Fig. 2 is respectively flower-shaped MoS2ESEM and transmission electron microscope picture, hydro-thermal method prepare MoS2Pattern is to receive
Popped rice shape, size is basically identical, and bouquet is combined together to form in cluster-shaped, does not reunite and still maintains a certain distance, flower
Shape size is between 100 nanometers, and transmission electron microscope sees flower-shaped MoS2 very thin thickness, and edge also will be thinner than sample medially
Band, in irregular shape, the edge thickness of fold is between several nanometers, with very big specific surface area, is that the attachment of silver ion is carried
For huge reaction active site；Fig. 3 is prepared Z configurations catalytic decomposition spray shape MoS2The scanning electron microscope (SEM) photograph of composite,
By figure it can be seen that phosphoric acid Argent grain wraps or be deposited on molybdenum disulfide nano flower surface by flower-shaped molybdenum disulfide；Fig. 4 is made
Standby Z configurations catalytic decomposition water sheet MoS2The scanning electron microscope (SEM) photograph of composite, by figure it can be seen that phosphoric acid silver nano-grain is few
Amount sticks to the sheet MoS of stripping2Surface；Fig. 5 is Z configurations catalytic decomposition spray shape MoS2The transmission electron microscope picture of composite, figure
In it can be seen that nano silver is attached on molybdenum disulfide thin slice, particle is tiny, illustrate both Compound Degrees height；Fig. 6 is institute
The Z configurations catalytic decomposition spray shape MoS of preparation2The X-ray diffractogram of composite, diffraction maximum corresponds to silver orthophosphate material well
Material, molybdenum disulfide addition is few and its pattern is irregular, so diffraction maximum is relatively weak, so as to can't see the diffraction of molybdenum disulfide
Peak；Fig. 7 is prepared Z configurations catalytic decomposition spray shape MoS2The UV-vis DRS spectrogram of composite, can by figure
To find out that material has light absorbs between 200 and 800nm.
It is the specific photocatalysis performance of research material in addition, we are using advanced oxygen analyser in its unit interval
Photocatalysis Decomposition aquatic products oxygen effect is tested, and specific experiment is as follows：
Photocatalysis production oxygen is main to be carried out in sealed Double-layer flask, and flask is connected with cooling water system, the oxygen concentration of generation
Detected by oxygen probe (GmbH FIBOX3 optical fiber oxygen sensors).Before illumination experiment, with calibration solution 0# (anaerobic water) and school
Quasi- solution 100 (saturation of the air water) carries out temperature compensation calibration to oxygen probe.Under light illumination, connection cooling water makes reaction system
Temperature keeps constant, and the temperature sensors of high precision that system is equipped with can exclude shadow of the system temperature change to generation oxygen concentration
Ring.Catalysis material (0.3g) is added into AgNO3Solution (100mL, 10g/L), ultrasonic mixing liquid 10min makes catalysis material equal
It is even to be scattered in solution.To remove the O dissolved in mixed liquor2, White LED light is then turned on after leading to nitrogen, 30min into solution
According to producing O by measuring in the same reaction period2Concentration characterize the oxygen performance processed of different catalysis materials.In addition, also
A series of control contrast experiments, including blank sample are carried out, dark condition and light is urged under the conditions of being not added with silver nitrate sacrifice agent
Change the oxygen performance processed of material.
Fig. 8 is the prepared flower-shaped MoS of Z configurations2Photochemical catalyzing composite photodissociation aquatic products oxygen under the irradiation such as LED
Rate diagram, after turning on light as seen from the figure, the oxygen concentration in the aqueous solution is in rising trend quickly, and quickly, concentration is bent for speed
Line slope is very high, after 30min, and curve regions tend towards stability, and water oxygen concentration maintains 42 μm of ol/L, and pure silver orthophosphate production oxygen is very
Weak, after a certain amount of molybdenum disulfide of addition is compound, overall oxygen-producing amount is improved.Fig. 9 is prepared Z configuration sheets
MoS2The production oxygen design sketch of photochemical catalyzing composite, same production oxygen speed maintains higher level in 30min, illustrates phosphorus
Sour silver and MoS2It is compound, generally improve production oxygen efficiency.Flower-shaped MoS2Composite photocatalyst decompose aqueous systems and pure silver orthophosphate,
Sheet MoS2/ silver orthophosphate is compared, stronger 7 times than simple silver orthophosphate production oxygen efficiency, than sheet MoS2/ silver orthophosphate composite photocatalyst material
Material production oxygen efficiency is high by 1/6.
Claims (5)
1. a kind of preparation method of Z configurations visible light catalytic decomposition water composite, it is characterised in that comprise the following steps that：
(1) flower-shaped molybdenum disulfide is weighed, ultrasonic disperse uniformly obtains the flower-shaped molybdenum disulfide point that concentration is 0.04~0.04wt%
Dispersion liquid；
(2) weigh silver nitrate to be dissolved into deionized water, obtain silver nitrate solution；Under stirring condition by silver nitrate solution by
It is added dropwise in flower-shaped molybdenum disulfide dispersion liquid, stirs 6-12h, obtain mixing precursor solution, silver nitrate is dense in mixed solution
Spend for 0.15mol/L；
(3) will be 3 by silver nitrate and sodium phosphate mol ratio:1 ratio, weighs phosphate and is dissolved in deionized water, obtain
0.2mol/L phosphate solution；
(4) under agitation, sodium radio-phosphate,P-32 solution is added in the mixing precursor solution prepared, with sodium phosphate
Add solution gradually become celadon precipitation, completion of dropping mixed solution continue stir 3h, final reaction thing precipitation using go from
Sub- water and ethanol respectively wash three vacuum dryings.
2. a kind of preparation method of Z configurations visible light catalytic decomposition water composite as claimed in claim 1, its feature exists
In the preparation method of the flower-shaped molybdenum disulfide is as follows：
(1) molybdate and thiocarbamide are quantitatively weighed, both are mixed by certain mol proportion, are put into together in 150mL beaker, the inside adds
Enter 70mL deionized water, stirring 0.5h to dissolving；
(2) above-mentioned solution is transferred in 100mL reactor, tightens and be put into 180 DEG C of heating 24h in baking oven, be made flower-shaped two
Molybdenum sulfide, it is standby that subsequent taking-up sample respectively cleans three vacuum dryings with deionized water and ethanol.
3. a kind of preparation method of Z configurations visible light catalytic decomposition water composite as claimed in claim 2, its feature exists
In the molybdate described in step 1 is sodium molybdate or ammonium molybdate.
4. a kind of preparation method of Z configurations visible light catalytic decomposition water composite as claimed in claim 2, its feature exists
In the ratio between sulfur content and molybdenum element content are 3 in the molybdenum disulfide preparation process:1~9:1.
5. a kind of preparation method of Z configurations visible light catalytic decomposition water composite as claimed in claim 1, its feature exists
In, the bending basal plane of flower-shaped molybdenum disulfide formation can turn into the chief active position of light-catalyzed reaction, and in the suction of visible ray
Receive scope and be better than molybdenum disulfide nano sheet, can further improve the oxygen performance processed of composite.
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| CN108479838A (en) * | 2018-03-28 | 2018-09-04 | 江苏大学 | A kind of binary channels Z configurations photochemical catalyzing composite material and preparation method |
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| CN109589993A (en) * | 2018-12-17 | 2019-04-09 | 浙江工商大学 | Pucherite-molybdenum sulfide-cobaltosic oxide catalysis electrode of electrochemical modification and its preparation method and application |
| CN110614104A (en) * | 2019-07-29 | 2019-12-27 | 西安工程大学 | Preparation method of photocatalyst for efficiently treating sewage |
| CN111063468A (en) * | 2019-12-10 | 2020-04-24 | 西南科技大学 | MoS for treating radioactive wastewater2Preparation method of/reduced graphene oxide nanosheet |
| CN113559845A (en) * | 2021-08-27 | 2021-10-29 | 陕西科技大学 | Bismuth vanadate/silver nitrate composite photocatalyst and preparation method thereof |
| CN114291864A (en) * | 2021-11-19 | 2022-04-08 | 山东大学 | Based on MoS2/BiVO4Method for degrading pollutants by using photo-Fenton system with photocatalyst activated peroxymonosulfate |
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| CN107744818A (en) * | 2017-10-23 | 2018-03-02 | 南昌航空大学 | Molybdenum disulfide loads the preparation method of silver-colored photochemical catalyst |
| CN108525686A (en) * | 2018-03-22 | 2018-09-14 | 江苏大学 | A kind of selenizing molybdenum compounded visible light photocatalyst of silver orthophosphate/bis- and preparation method and application |
| CN108479838A (en) * | 2018-03-28 | 2018-09-04 | 江苏大学 | A kind of binary channels Z configurations photochemical catalyzing composite material and preparation method |
| CN108745380A (en) * | 2018-06-28 | 2018-11-06 | 合肥工业大学 | A kind of preparation method carrying silver-colored molybdenum disulfide nano tube composite electro catalytic liberation of hydrogen material |
| CN109589993A (en) * | 2018-12-17 | 2019-04-09 | 浙江工商大学 | Pucherite-molybdenum sulfide-cobaltosic oxide catalysis electrode of electrochemical modification and its preparation method and application |
| CN109589993B (en) * | 2018-12-17 | 2021-06-29 | 浙江工商大学 | Electrochemically modified bismuth vanadate-molybdenum sulfide-cobaltosic oxide catalytic electrode and preparation method and application thereof |
| CN110614104A (en) * | 2019-07-29 | 2019-12-27 | 西安工程大学 | Preparation method of photocatalyst for efficiently treating sewage |
| CN111063468A (en) * | 2019-12-10 | 2020-04-24 | 西南科技大学 | MoS for treating radioactive wastewater2Preparation method of/reduced graphene oxide nanosheet |
| CN113559845A (en) * | 2021-08-27 | 2021-10-29 | 陕西科技大学 | Bismuth vanadate/silver nitrate composite photocatalyst and preparation method thereof |
| CN113559845B (en) * | 2021-08-27 | 2023-10-27 | 陕西科技大学 | Bismuth vanadate silver phosphate composite photocatalyst and preparation method thereof |
| CN114291864A (en) * | 2021-11-19 | 2022-04-08 | 山东大学 | Based on MoS2/BiVO4Method for degrading pollutants by using photo-Fenton system with photocatalyst activated peroxymonosulfate |
| CN116440927A (en) * | 2023-04-25 | 2023-07-18 | 景德镇陶瓷大学 | Preparation method of silver-modified molybdenum sulfide nanoflower |
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