CN108636436A - Effectively construct the preparation method of Z-type ternary heterojunction photochemical catalyst - Google Patents
Effectively construct the preparation method of Z-type ternary heterojunction photochemical catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 39
- 229910052961 molybdenite Inorganic materials 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002244 precipitate Substances 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004202 carbamide Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 7
- 235000019795 sodium metasilicate Nutrition 0.000 claims abstract description 7
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 7
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 5
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract 4
- 229910004619 Na2MoO4 Inorganic materials 0.000 claims abstract 2
- 239000011684 sodium molybdate Substances 0.000 claims abstract 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000006243 chemical reaction Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 101710134784 Agnoprotein Proteins 0.000 claims description 6
- 229910015667 MoO4 Inorganic materials 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 6
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical compound FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 abstract 2
- 238000013019 agitation Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910003243 Na2SiO3·9H2O Inorganic materials 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 235000013339 cereals Nutrition 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 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 3
- 235000009566 rice Nutrition 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011806 microball Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000007540 photo-reduction reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000012702 metal oxide precursor Substances 0.000 description 1
- 229920005588 metal-containing polymer Polymers 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000013097 stability assessment Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- 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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
A kind of preparation method for effectively constructing Z-type ternary heterojunction photochemical catalyst of the present invention, step include：1) urea is heat-treated, cooling obtains g C3N4；2) by g C3N4It dissolves in deionized water, sequentially adds Na2MoO4·2H2O、CH3CSNH2And sodium metasilicate；3) pH value is adjusted to neutrality；Suspension is transferred in autoclave；4) reacted under the conditions of 200~250 DEG C, after autoclave is cooled to room temperature；Black precipitate is collected, is washed with strong base solution；It is washed again with absolute ethyl alcohol and deionized water, vacuum drying obtains g C3N4/MoS2；5) by AgNO3G C are added in solution3N4/MoS2In, it is vigorously stirred in dark；It is transferred in water cooling reactor, Xe light irradiations suspension under magnetic agitation, in MoS2Ag nano particles are formed on surface；Finally vacuum drying.
Description
Technical field
The invention belongs to Z-type hetero-junctions preparing technical fields, are related to one kind and effectively constructing Z-type ternary heterojunction photochemical catalyst
Preparation method.
Background technology
The aggravation of the problem of due to energy crisis and environmental pollution, semiconductor light-catalyst have attracted wide attention,
It is contaminant degradation, photochemical catalyzing generates hydrogen (H2) and by carbon dioxide conversion be that energy etc. provides " green "
Approach.Carboritride (the g-C of graphene-like3N4), it is a kind of new without metal-containing polymer semiconductor, there is higher chemistry
A kind of and thermal stability, it has also become photochemical catalyst of effective visible optical drive.Due to its relatively narrow band gap, only about 2.7eV,
So it can directly play a role in visibility region.However, pure g-C3N4Specific surface area is smaller and internal light induced electron-
Hole is to (e-/h+) recombination rate is higher, this leads to g-C3N4Visible optical drive photocatalysis performance it is relatively low.Therefore, develop new
Preparation method solves the defect that nano particle is easily reunited when content of metal increases in traditional handicraft, for alleviating sternness increasingly
Environment and energy problem have great importance.
However there are still some shortcomings for the method reported at present, overcome the oneself factor restricted problem of semiconductor, it is necessary to
Set about in terms of two：On the one hand, reduce the energy gap of semiconductor, spectral response range can be widened.On the other hand, make conduction band
Potential is more negative, the corrigendum of valence band potential, the redox reaction being thermodynamically more advantageous in photocatalytic system.However this 2 points
It runs counter to, first point requires band gap to narrow；Conduction band potential is more negative in second point, and the corrigendum of valence band potential can make band gap broaden.
For the photochemical catalyst of one pack system, it is impossible to while accomplishing above 2 points, novel artificial Z-type catalysis material, by multigroup
Divide and constitute, the above 2 points requirement can be met simultaneously.Therefore, commercially the widely used raw material of industry sets out, and lives on no surface
Property agent and additional reducing agent under the conditions of, realize Z-type g-C3N4/Ag/MoS2The synthesis of ternary heterojunction photochemical catalyst and structure tune
Control is still a major challenge of current research.If method associated with hydro-thermal method/photo-reduction can be utilized to synthesize golden Z-type g-C3N4/
Ag/MoS2Ternary heterojunction photochemical catalyst, can greatly simplify the preparation process flow and cost of such material, and such method exists
There is not been reported in relevant document and patent.
Invention content
The object of the present invention is to provide a kind of preparation methods for effectively constructing Z-type ternary heterojunction photochemical catalyst, solve
Band gap narrows in the prior art, conduction band potential is difficult to compatible problem with valence band potential.
The technical solution adopted in the present invention is a kind of preparation method for effectively constructing Z-type ternary heterojunction photochemical catalyst,
Implement according to the following steps：
Step 1) carries out heat treatment 3~5 hours, natural cooling at 450~550 DEG C in alumina crucible to urea
To environment temperature, pure sheet g-C is obtained3N4；
Under step 2) stirring condition, in three-necked flask, by the g-C of 0.1~1g3N4It is dissolved in 20~50mL deionized waters
In, then sequentially add the Na of 1~50mL2MoO4·2H2O, the CH of 1~50mL3CSNH2And the sodium metasilicate of 0.5g；
The HCl solution of 0.1~0.3M is added dropwise in step 3), and the pH value of solution is adjusted to 6.0~7.0；By gained suspension
Be transferred in autoclave and stirring 1~3 hour after tight seal；
Step 4) is reacted under the conditions of 200~250 DEG C, when reaction a length of 24~48h, after reaction by autoclave
Cooled to room temperature；Black precipitate is collected, with strong base solution washing precipitate to remove remaining silicic acid；Then, it uses successively
Absolute ethyl alcohol and deionized water washing, are finally dried in vacuo 5~24 hours to get to g-C under the conditions of 50~80 DEG C3N4/
MoS2；
Step 5) is by the AgNO of 1~10mL3Solution is added to the g-C of 50mL3N4/MoS2In, and acutely stir in the dark
It mixes, until all reagents are completely dissolved；Then, it is transferred in water cooling reactor, under magnetic stirring with the Xe of 300~800W
Light irradiation suspension 0.5~5 hour, in MoS2Ag nano particles are formed on the surface of microballoon；Finally, by the powder of acquisition 50
It is 8~24 hours dry under~90 DEG C of vacuum environment,.
The invention has the advantages that metal oxide precursor is introduced into reaction system under certain pH value condition
In, one-step method realizes the tune for constructing Z-type g-C3N4/Ag/MoS2 ternary heterojunction photocatalyst granular sizes and load capacity
Control.The raw material for preparing of this method is easy to get, easy to operate.
Description of the drawings
Fig. 1 is Z-type g-C prepared by the present invention3N4/Ag/MoS2The flow chart of photochemical catalyst；
Fig. 2 is Z-type g-C prepared by the present invention3N4/Ag/MoS2The photocatalytic degradation rhodamine B assessment figure of photochemical catalyst；
Fig. 3 is Z-type g-C prepared by the present invention3N4/Ag/MoS2The photocatalytic water assessment figure of photochemical catalyst.
Specific implementation mode
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
Referring to Fig.1, the present invention is that one kind effectively constructing Z-type ternary heterojunction photochemical catalyst (g-C3N4/Ag/MoS2) system
Preparation Method is implemented according to the following steps：
Step 1) is heat-treated urea at 450~550 DEG C and (is capped processing to ensure it in alumina crucible
Reacted in the atmosphere of oneself) 3~5 hours, environment temperature is naturally cooled to, pure sheet g-C is obtained3N4；
Under step 2) stirring condition, in three-necked flask, by the g-C of 0.1~1g3N4It is dissolved in 20~50mL deionized waters
In, then sequentially add the Na of 1~50mL2MoO4·2H2The CH of O (molar concentration 3mM), 1~50mL3CSNH2(TAA) it (rubs
You a concentration of 9mM) and 0.5g sodium metasilicate (Na2SiO3·9H2O)；
Step 3) then, is added dropwise the HCl solution of 0.1~0.3M, the pH value of solution is adjusted to 6.0~7.0；Gained is hanged
Supernatant liquid is transferred in the tetrafluoroethene autoclave of 50~100mL and the tight seal after stirring 1~3 hour；
Step 4) is reacted (solvent thermal reaction) under the conditions of 200~250 DEG C, when reaction a length of 24~48h, reaction knot
By autoclave cooled to room temperature after beam；Collect black precipitate, with strong base solution (such as NaOH solution or KOH solution, it is mole dense
Degree is 1~5M) washing precipitate is repeatedly to remove remaining silicic acid；Then, it is washed successively with absolute ethyl alcohol and deionized water, most
5~24 hours are dried in vacuo under the conditions of 50~80 DEG C afterwards to get to flower-shaped g-C3N4/MoS2Microballoon；
Step 5) is by the AgNO of 1~10mL3Solution (molar concentration 1mg/mL) is added to the g-C of 50mL3N4/MoS2Dispersion
It in body (1mM), and is vigorously stirred in the dark, until all reagents are completely dissolved；Then, the water cooling for being transferred to 200mL is anti-
It answers in device, (is carried out photoreduction with the Xe light irradiations suspension of 300~800W under magnetic stirring, obtained within 0.5~5 hour
Silver-colored simple substance), to allow in MoS2Ag nano particles are formed on the surface of microballoon；Finally, by the powder of acquisition at 50~90 DEG C
It is 8~24 hours dry under vacuum environment,.
Wherein, g-C3N4Molar ratio with molybdenum disulfide presoma is：1:2-48, g-C3N4Molar ratio with metallic silver is
10-20:1。
Drying means used in above-mentioned step 4) is dried for vacuum constant temperature.
Z-type g-C prepared by the method for the present invention3N4/Ag/MoS2Ternary heterojunction photochemical catalyst has higher photocatalytic water system
Hydrogen performance.
Above-mentioned each raw material is marketable material, and no special instruction purity is chemical pure or the pure grade of analysis.
Embodiment 1
Step 1) carries out heat treatment 3 hours to urea at 550 DEG C, naturally cools to environment temperature in alumina crucible
Degree, obtains pure sheet g-C3N4；
Under step 2) stirring condition, in three-necked flask, by the g-C of 0.5g3N4It is dissolved in 30mL deionized waters, then
Sequentially add the Na of the 3mM concentration of 15mL2MoO4·2H2O, the CH of the 9mM of 15mL3CSNH2(TAA) and the sodium metasilicate of 0.5g
(Na2SiO3·9H2O)；
Then, the HCl solution of 0.1M is added dropwise in step 3), and the pH value of solution is adjusted to 6.0；Gained suspension is transferred to
In the tetrafluoroethene autoclave of 100mL and after stirring for 2 hours tight seal；
Step 4) is reacted under the conditions of 220 DEG C, and when reaction is a length of for 24 hours, after reaction by autoclave natural cooling
To room temperature；Black precipitate is collected, with the NaOH solution washing precipitate of 2M repeatedly to remove remaining silicic acid；Then, it uses successively
Absolute ethyl alcohol and deionized water washing, are finally dried in vacuo 12 hours to get to flower-shaped g-C under the conditions of 60 DEG C3N4/MoS2It is micro-
Ball；
Step 5) is by the AgNO of 2mL3Solution (molar concentration 1mg/mL) is added to the g-C of 50mL3N4/MoS2Dispersion
It in (1mM), and is vigorously stirred in the dark, until all reagents are completely dissolved；Then, it is transferred to the water cooling reaction of 200mL
In device, the Xe light irradiations suspension of 500W is used under magnetic stirring 2 hours, to allow in MoS2Ag is formed on the surface of microballoon to receive
Rice grain；Finally, the powder of acquisition is 12 hours dry under 70 DEG C of vacuum environment, obtain Z-type g-C3N4/Ag/MoS2Ternary
Heterojunction photocatalyst.
Embodiment 2
Step 1) carries out heat treatment 5 hours to urea at 500 DEG C, naturally cools to environment temperature in alumina crucible
Degree, obtains pure sheet g-C3N4；
Under step 2) stirring condition, in three-necked flask, by the g-C of 1g3N4Be dissolved in 30mL deionized waters, then according to
The Na of the secondary 3mM concentration that 30mL is added2MoO4·2H2O, the CH of the 9mM of 30mL3CSNH2(TAA) and the sodium metasilicate of 0.5g
(Na2SiO3·9H2O)；
Then, the HCl solution of 0.1M is added dropwise in step 3), and the pH value of solution is adjusted to 7.0；Gained suspension is transferred to
In the tetrafluoroethene autoclave of 100mL and stirring 3 hours after tight seal；
Step 4) is reacted under the conditions of 220 DEG C, when reaction a length of 20h, after reaction by autoclave natural cooling
To room temperature；Black precipitate is collected, with the NaOH solution washing precipitate of 2M repeatedly to remove remaining silicic acid；Then, it uses successively
Absolute ethyl alcohol and deionized water washing, are finally dried in vacuo 18 hours to get to flower-shaped g-C under the conditions of 50 DEG C3N4/MoS2It is micro-
Ball；
Step 5) is by the AgNO of 4mL3Solution (molar concentration 1mg/mL) is added to the g-C of 50mL3N4/MoS2Dispersion
It in (1mM), and is vigorously stirred in the dark, until all reagents are completely dissolved；Then, it is transferred to the water cooling reaction of 200mL
In device, the Xe light irradiations suspension of 800W is used under magnetic stirring 2 hours, to allow in MoS2Ag is formed on the surface of microballoon to receive
Rice grain；Finally, the powder of acquisition is 20 hours dry under 50 DEG C of vacuum environment, obtain Z-type g-C3N4/Ag/MoS2Ternary
Heterojunction photocatalyst.
Embodiment 3
Step 1) carries out heat treatment 5 hours to urea at 450 DEG C, naturally cools to environment temperature in alumina crucible
Degree, obtains pure sheet g-C3N4；
Under step 2) stirring condition, in three-necked flask, by the g-C of 0.1g3N4It is dissolved in 40mL deionized waters, then
Sequentially add the Na of the 3mM concentration of 50mL2MoO4·2H2O, the CH of the 9mM of 50mL3CSNH2(TAA) and the sodium metasilicate of 0.5g
(Na2SiO3·9H2O)；
Then, the HCl solution of 0.3M is added dropwise in step 3), and the pH value of solution is adjusted to 6.5；Gained suspension is transferred to
In the tetrafluoroethene autoclave of 100mL and after one hour of the stirring tight seal；
Step 4) is reacted under the conditions of 250 DEG C, and when reaction is a length of for 24 hours, after reaction by autoclave natural cooling
To room temperature；Black precipitate is collected, with the KOH solution washing precipitate of 4M repeatedly to remove remaining silicic acid；Then, nothing is used successively
Water-ethanol and deionized water washing, are finally dried in vacuo 20 hours to get to flower-shaped g-C under the conditions of 50 DEG C3N4/MoS2Microballoon；
Step 5) is by the AgNO of 10mL3Solution (molar concentration 1mg/mL) is added to the g-C of 50mL3N4/MoS2Dispersion
It in (1mM), and is vigorously stirred in the dark, until all reagents are completely dissolved；Then, it is transferred to the water cooling reaction of 200mL
In device, the Xe light irradiations suspension of 300W is used under magnetic stirring 5 hours, to allow in MoS2Ag is formed on the surface of microballoon to receive
Rice grain；Finally, the powder of acquisition is 8 hours dry under 90 DEG C of vacuum environment, obtain Z-type g-C3N4/Ag/MoS2Ternary
Heterojunction photocatalyst.
Fig. 2 is under visible light illumination that the performance of different sample photocatalytic degradation rhodamine Bs compares, and illustrates present invention side
The efficiency highest of product photocatalytic degradation rhodamine B prepared by method.
Fig. 3 is the assessment of different samples Photocatalyzed Hydrogen Production ability under visible light illumination：(a)MoS2、(b)g-C3N4、(c)
Ag/MoS2, (d) g-C3N4/MoS2 and (e) g-C3N4/Ag/MoS2 and during producing hydrogen sample stability assessment figure,
Illustrate the efficiency highest of product Photocatalyzed Hydrogen Production ability under visible light illumination prepared by the method for the present invention.
Claims (6)
1. a kind of preparation method for effectively constructing Z-type ternary heterojunction photochemical catalyst, which is characterized in that real according to the following steps
It applies：
Step 1) carries out heat treatment 3~5 hours to urea at 450~550 DEG C, naturally cools to ring in alumina crucible
Border temperature, obtains g-C3N4；
Under step 2) stirring condition, in three-necked flask, by the g-C of 0.1~1g3N4It is dissolved in 20~50mL deionized waters, with
The Na of 1~50mL is sequentially added afterwards2MoO4·2H2O, the CH of 1~50mL3CSNH2And the sodium metasilicate of 0.5g；
The HCl solution of 0.1~0.3M is added dropwise in step 3), and the pH value of solution is adjusted to 6.0~7.0；Gained suspension is shifted
To in autoclave and stirring 1~3 hour after tight seal；
Step 4) is reacted under the conditions of 200~250 DEG C, when reaction a length of 24~48h, after reaction by autoclave nature
It is cooled to room temperature；Black precipitate is collected, remaining silicic acid is removed with strong base solution washing precipitate；Then, successively with anhydrous second
Alcohol and deionized water washing, are finally dried in vacuo 5~24 hours to get to g-C under the conditions of 50~80 DEG C3N4/MoS2；
Step 5) is by the AgNO of 1~10mL3Solution is added to the g-C of 50mL3N4/MoS2In, and be vigorously stirred in the dark, until
All reagents are completely dissolved；Then, it is transferred in water cooling reactor, under magnetic stirring with the Xe light irradiations of 300~800W
Suspension 0.5~5 hour, in MoS2Surface on formed Ag nano particles；Finally, the powder of acquisition is true at 50~90 DEG C
It is 8~24 hours dry under Altitude,.
2. the preparation method according to claim 1 for effectively constructing Z-type ternary heterojunction photochemical catalyst, it is characterised in that：
It is 1~5M that the strong base solution, which selects NaOH solution or KOH solution, molar concentration,.
3. the preparation method according to claim 1 for effectively constructing Z-type ternary heterojunction photochemical catalyst, it is characterised in that：
The Na2MoO4·2H2O molar concentrations are 3mM；CH3CSNH2Molar concentration is 9mM.
4. the preparation method according to claim 1 for effectively constructing Z-type ternary heterojunction photochemical catalyst, it is characterised in that：
The autoclave selects the tetrafluoroethene autoclave of 50~100mL.
5. the preparation method according to claim 1 for effectively constructing Z-type ternary heterojunction photochemical catalyst, it is characterised in that：
The g-C3N4Molar ratio with molybdenum disulfide presoma is：1:2-48, g-C3N4Molar ratio with metallic silver is 10-20:1.
6. the preparation method according to claim 1 for effectively constructing Z-type ternary heterojunction photochemical catalyst, it is characterised in that：
The AgNO3The molar concentration of solution is 1mg/mL, g-C3N4/MoS2The molar concentration of dispersion is 1mM.
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