CN110152700A - A kind of carbon cloth load molybdenum disulfide/silver carbonate composite photo-catalyst and its preparation method and application - Google Patents
A kind of carbon cloth load molybdenum disulfide/silver carbonate composite photo-catalyst and its preparation method and application Download PDFInfo
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- CN110152700A CN110152700A CN201910313950.2A CN201910313950A CN110152700A CN 110152700 A CN110152700 A CN 110152700A CN 201910313950 A CN201910313950 A CN 201910313950A CN 110152700 A CN110152700 A CN 110152700A
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- carbon cloth
- catalyst
- composite photo
- carbonate
- molybdenum disulfide
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 95
- 239000004744 fabric Substances 0.000 title claims abstract description 95
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 51
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 title claims abstract description 46
- 229910052982 molybdenum disulfide Inorganic materials 0.000 title claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 38
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 229910001958 silver carbonate Inorganic materials 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 36
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 31
- 238000007654 immersion Methods 0.000 claims abstract description 26
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 22
- KQTXIZHBFFWWFW-UHFFFAOYSA-L silver(I) carbonate Inorganic materials [Ag]OC(=O)O[Ag] KQTXIZHBFFWWFW-UHFFFAOYSA-L 0.000 claims abstract description 21
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 17
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 16
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 14
- 238000005530 etching Methods 0.000 claims abstract description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 230000004087 circulation Effects 0.000 claims abstract description 12
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 11
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 11
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000004140 cleaning Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000004108 freeze drying Methods 0.000 claims abstract description 5
- 238000011068 loading method Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 229910052961 molybdenite Inorganic materials 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 7
- 239000001099 ammonium carbonate Substances 0.000 claims description 7
- 230000001699 photocatalysis Effects 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 5
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000011733 molybdenum Substances 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 14
- 238000004064 recycling Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 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 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 229920001661 Chitosan Polymers 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- HWRJVZIUPBOVBP-UHFFFAOYSA-N [C].[Mo]=S Chemical compound [C].[Mo]=S HWRJVZIUPBOVBP-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- WIKQEUJFZPCFNJ-UHFFFAOYSA-N carbonic acid;silver Chemical compound [Ag].[Ag].OC(O)=O WIKQEUJFZPCFNJ-UHFFFAOYSA-N 0.000 description 1
- -1 carboxyl phthalocyanine cobalt Chemical compound 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001132 ultrasonic dispersion 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
- B01J27/20—Carbon compounds
- B01J27/232—Carbonates
-
- 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
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to catalysis material technical field, a kind of carbon cloth load molybdenum disulfide/silver carbonate composite photo-catalyst and its preparation method and application is disclosed.The carbon cloth load molybdenum disulfide/silver carbonate composite photo-catalyst is to be immersed in the carbon cloth of cleaning in nitric acid to carry out surface acid etching and drying；Then the carbon cloth of processing is immersed in in the mixed aqueous solution of sodium molybdate and thiocarbamide the hydro-thermal reaction at 180~200 DEG C, obtain the carbon cloth of load molybdenum sulfide；The carbon cloth for loading molybdenum sulfide is impregnated in carbonate solution, then take out and is put into silver nitrate solution after immersion, then is immersed in carbonate solution, the circulation immersion in silver nitrate solution and carbonate solution, is made after freeze-drying.Method and process of the invention is simple, the MoS of gained carbon cloth load2/Ag2CO3Composite photocatalyst material activity is high, and is conducive to recycling and reusing.
Description
Technical field
The invention belongs to catalysis material technical fields, load molybdenum disulfide/silver carbonate more particularly, to a kind of carbon cloth
(MoS2/Ag2CO3) composite photo-catalyst and its preparation method and application.
Background technique
In recent decades, conductor photocatalysis material has potential application in the purification of organic pollutant and causes
Extensive concern.In various catalysis materials, TiO2With good oxidability, photostability it is strong, it is environmentally friendly,
The advantages that inexpensive.However, TiO2It can only be by ultraviolet excitation.It is well known that ultraviolet light only accounts for the 3-5% of sunlight, much
Lower than the ratio (about 45%) of visible light.Therefore, there is an urgent need to develop the visible lights with greater activity and good stability
The photochemical catalyst of response.
In recent years, a series of Ag based photocatalyst such as AgBr and Ag2CO3Deng degradable organic pollutant under visible light illumination
When show excellent photocatalytic activity.It is difficult to separate however, these Ag based photocatalysts powder after light-catalyzed reaction exists
Recycling and recycling the shortcomings that, this may cause secondary pollution and increase catalysis material in practical applications at
This.The fixed load technology of photochemical catalyst is one of the effective way to solve the above problems.Business carbon cloth is because having good electricity
Sub- transmittability, higher mechanical strength and mechanical property and the carrier for being widely used as catalysis material.It is loaded on carbon cloth
Molybdenum disulfide and with silver carbonate is compound that its photocatalytic activity not only can be improved, but also be also easy to recycling and reusing.For example, application
Number be CN201710249287.5 Chinese invention patent " a kind of recyclable chitosan magnetic phthalocyanine catalyst and application ",
Preparation method is that four carboxyl phthalocyanine cobalt is added in the reaction vessel for filling dimethylformamide, and stirring dissolves it sufficiently, with
The ferroferric oxide magnetic carrier powder ultrasonic dispersion for being coated with chitosan is added afterwards, solvent dimethylformamide is extracted in stirring out,
The chitosan magnetic phthalocyanine catalyst for being washed out, drying recyclable.Although the method increase the repetitions of catalysis material
Utilization rate, but more chemical reagent has been used, and preparation process is complex.
Summary of the invention
In order to solve above-mentioned the shortcomings of the prior art, primary and foremost purpose of the present invention is to provide a kind of carbon cloth negative
Carry MoS2/Ag2CO3Composite photo-catalyst.
Another object of the present invention is to provide above-mentioned carbon cloths to load MoS2/Ag2CO3The preparation method of composite photo-catalyst.
The purpose of the present invention is to provide above-mentioned carbon cloths to load MoS2/Ag2CO3The application of composite photo-catalyst.
The purpose of the present invention is realized by following technical proposals:
A kind of carbon cloth load molybdenum disulfide/silver carbonate composite photo-catalyst, the carbon cloth load molybdenum disulfide/silver carbonate are multiple
Light combination catalyst is to be immersed in the carbon cloth of cleaning in nitric acid to carry out surface acid etching and drying；Then the carbon cloth of processing is impregnated
In sodium molybdate-thiocarbamide aqueous solution at 180~200 DEG C hydro-thermal reaction, obtain load molybdenum sulfide carbon cloth；Load is vulcanized
The carbon cloth of molybdenum impregnates in carbonate solution, then takes out and is put into silver nitrate solution after immersion, then is immersed in carbonic acid
In salting liquid, the circulation immersion in silver nitrate solution and carbonate solution is made after freeze-drying.
Preferably, the solvent of the cleaning is acetone, ethyl alcohol and deionized water, and the time of the cleaning is 10~20min；
The concentration of the nitric acid is 60~65%；The time of the surface acid etching be 10~for 24 hours；The time of the hydro-thermal reaction is 5
~10h.
Preferably, in the aqueous solution of the sodium molybdate-thiocarbamide quality of sodium molybdate, the quality of thiocarbamide and deionized water body
Product is than being (0.1~0.2) g:(0.1~0.2) g:(30~40) mL.
Preferably, the number of the circulation immersion is 10~20 times.
Preferably, the carbonate solution is one or more of ammonium hydrogen carbonate, sodium bicarbonate, sodium carbonate or ammonium carbonate.
Preferably, the concentration of the silver nitrate solution is 0.1~0.2mol/L, and the concentration of the carbonate solution is 0.05
~0.2mol/L.
Preferably, the condition of the freeze-drying are as follows: the temperature of freezing is -40~-46 DEG C, and vacuum degree is 35~45MPa.
The carbon cloth loads molybdenum disulfide/silver carbonate composite photo-catalyst preparation method, comprises the following specific steps that:
S1. carbon cloth is successively cleaned with acetone, ethyl alcohol and deionized water, then carbon cloth is immersed in the nitric acid of 60-65%
Middle progress surface acid etching and drying；
S2. carbon cloth processed in step S1 is immersed in sodium molybdate and thiocarbamide mixed aqueous solution and is transferred to reaction kettle
In at 180-200 DEG C hydro-thermal reaction, obtain load molybdenum sulfide carbon cloth；
S3. the carbon cloth for loading molybdenum sulfide is impregnated in carbonate solution I, takes out and be put into silver nitrate solution and impregnates
Ⅱ；III is impregnated in carbonate solution again；
S4. step S3 is repeated to recycle 10~20 times, it is freeze-dried, carbon cloth is made and loads MoS2/Ag2CO3Composite photocatalyst
Material.
Preferably, described in step S3 immersion I time be 10~for 24 hours；The time of the immersion II is 10~20s, institute
The time for stating immersion III is 10~20s.
The carbon cloth loads molybdenum disulfide/application of the silver carbonate composite photo-catalyst in photocatalysis field.
Compared with prior art, the invention has the following advantages:
1. the MoS that carbon cloth of the invention loads2/Ag2CO3Composite photocatalyst material is with higher photocatalytic activity and surely
It is qualitative.Under visible light illumination, the light induced electron of molybdenum disulfide can be transferred on silver carbonate conduction band, and carbon cloth is also beneficial to
The transfer of light induced electron promotes the light induced electron on silver carbonate conduction band that can be further diverted on carbon cloth, and photohole is distinguished
It stays on molybdenum disulfide and silver carbonate, this process is conducive to the separation in light induced electron and hole, and then improves to rhodamine B
Degradation rate.
2. preparation method simple process of the invention, required organic solvent is less, and carbon cloth loads catalysis material,
It has degraded under illumination after organic pollutants, carbon cloth need to only have been taken out, be conducive to the recycling and benefit again of catalysis material
With so as to avoid the secondary pollution of water body.
Detailed description of the invention
Fig. 1 is that the carbon cloth of embodiment 1 loads MoS2/Ag2CO3The scanning electron microscope (SEM) photograph of composite photocatalyst material.
Fig. 2 is that the carbon cloth of embodiment 1 loads MoS2/Ag2CO3Binary made from composite photocatalyst material and comparative example 1 is compound
The rate curve of catalysis material rhodamine B degradation under visible light.
Specific embodiment
The contents of the present invention are further illustrated combined with specific embodiments below, but should not be construed as limiting the invention.
Unless otherwise specified, the conventional means that technological means used in embodiment is well known to those skilled in the art.Except non-specifically
Illustrate, reagent that the present invention uses, method and apparatus is the art conventional reagents, method and apparatus.
Embodiment 1
1. carbon cloth is successively cleaned 20min with acetone, ethyl alcohol and deionized water, then carbon cloth is immersed in 65% nitric acid
Middle progress surface acid etching is for 24 hours and dry.
2. the thiocarbamide of the sodium molybdate of 120mg and 190mg is dissolved in 30mL deionized water.
3. carbon cloth processed in step 1 is impregnated in mixed solution in step 2 and is transferred in 50mL reaction kettle
The hydro-thermal reaction 5h at 200 DEG C obtains the carbon cloth of load molybdenum sulfide.
4. the carbon cloth for taking a surface to grow molybdenum sulfide impregnates for 24 hours in the ammonium bicarbonate soln of 0.075mol/L.
5. the carbon cloth impregnated in step 4 is taken out and is put into the silver nitrate solution of 0.15mol/L and impregnates 10s.
6. carbon cloth in step 5 is impregnated 10s in step 4 again.
7. repeating step 5 and 6 circulations 20 times, at -40 DEG C of condensation temperature, vacuum degree is to be freeze-dried under 35MPa, is obtained
MoS is loaded to carbon cloth2/Ag2CO3Composite photocatalyst material.
Fig. 1 is that carbon cloth made from the present embodiment loads MoS2/Ag2CO3The scanning electron microscope (SEM) photograph of composite photocatalyst material.From Fig. 1
In it is found that molybdenum disulfide and silver carbonate are supported on carbon cloth well；Illustrate that carbon cloth loads MoS2/Ag2CO3Composite photocatalyst material
Material successfully prepares.Fig. 2 is that carbon cloth made from the present embodiment loads MoS2/Ag2CO3Composite photocatalyst material and right
Carbon cloth loaded Ag made from ratio 12CO3The rate curve of material rhodamine B degradation under visible light.Compare from Fig. 2 it is found that
When the rhodamine B solution of same concentrations of degrading and volume, carbon cloth loads MoS2/Ag2CO3The composite photocatalyst material used time is most short, says
Bright carbon cloth loads MoS2/Ag2CO3Composite photocatalyst material is loaded compared to carbon cloth in the comparative example 1 prepared under the same terms
Ag2CO3Catalysis material has higher photocatalytic activity and stability.
Embodiment 2
1. carbon cloth is successively cleaned 20min with acetone, ethyl alcohol and deionized water, then carbon cloth is immersed in 65% nitric acid
Middle progress surface acid etching is for 24 hours and dry.
2. the thiocarbamide of the sodium molybdate of 120mg and 190mg is dissolved in 30mL deionized water.
3. carbon cloth processed in step 1 is impregnated in mixed solution in step 2 and is transferred in 50mL reaction kettle
The hydro-thermal reaction 5h at 200 DEG C obtains the carbon cloth of load molybdenum sulfide.
4. the carbon cloth for taking a surface to grow molybdenum sulfide impregnates for 24 hours in the sodium carbonate liquor of 0.075mol/L.
5. the carbon cloth impregnated in step 4 is taken out and is put into the silver nitrate solution of 0.15mol/L and impregnates 10s.
6. carbon cloth in step 5 is impregnated 10s in step 4 again.
7. repeating step 5 and 6 circulations 20 times, at -40 DEG C of condensation temperature, vacuum degree is to be freeze-dried under 35MPa, is made
It obtains carbon cloth and loads MoS2/Ag2CO3Composite photocatalyst material.
Embodiment 3
1. carbon cloth is successively cleaned 20min with acetone, ethyl alcohol and deionized water, then carbon cloth is immersed in 65% nitric acid
Middle progress surface acid etching is for 24 hours and dry.
2. the thiocarbamide of the sodium molybdate of 120mg and 190mg is dissolved in 30mL deionized water.
3. carbon cloth processed in step 1 is impregnated in mixed solution in step 2 and is transferred in 50mL reaction kettle
The hydro-thermal reaction 5h at 200 DEG C obtains the carbon cloth of load molybdenum sulfide.
4. the carbon cloth for taking a surface to grow molybdenum sulfide impregnates for 24 hours in the sodium bicarbonate solution of 0.075mol/L.
5. the carbon cloth impregnated in step 4 is taken out and is put into the silver nitrate solution of 0.15mol/L and impregnates 10s.
6. carbon cloth in step 5 is impregnated 10s in step 4 again.
7. repeating step 5 and 6 circulations 20 times, at -40 DEG C of condensation temperature, vacuum degree is to be freeze-dried under 35MPa, is made
It obtains carbon cloth and loads MoS2/Ag2CO3Composite photocatalyst material.
Embodiment 4
Different from embodiment 1 is: the time of cleaning described in step 1 is 10min；The concentration of the nitric acid is
60%, the time of the surface acid etching is 10h；The thiocarbamide of the sodium molybdate of 200mg and 200mg is dissolved in 40mL in step 2
In deionized water；Described in step 3 at 180 DEG C hydro-thermal reaction 10h；The concentration of ammonium bicarbonate soln described in step 4 is
0.2mol/L, the time of the immersion are 10h；The concentration of silver nitrate solution described in step 5 is 0.2mol/L, the immersion
Time is 20s；The time of immersion described in step 6 is 20s；The number of circulation immersion described in step 7 is 10 times, described cold
Solidifying temperature is -46 DEG C, vacuum degree 45MPa.
Embodiment 5
Different from embodiment 2 is: the time of cleaning described in step 1 is 15min；The concentration of the nitric acid is
62%, the time of the surface acid etching is 20h；The thiocarbamide of the sodium molybdate of 100mg and 200mg is dissolved in 40mL in step 2
In deionized water；Described in step 3 at 190 DEG C hydro-thermal reaction 8h；The concentration of sodium carbonate liquor described in step 4 is
0.1mol/L, the time of the immersion are 15h；The concentration of silver nitrate solution described in step 5 is 0.05mol/L, the immersion
Time be 15s；The time of immersion described in step 6 is 15s；The number of circulation immersion described in step 7 be 15 times, it is described
Condensation temperature is -46 DEG C, vacuum degree 40MPa.
Embodiment 6
Different from embodiment 3 is: the time of cleaning described in step 1 is 17min；The concentration of the nitric acid is
62%, the time of the surface acid etching is 20h；The thiocarbamide of the sodium molybdate of 100mg and 100mg is dissolved in 30mL in step 2
In deionized water；Described in step 3 at 190 DEG C hydro-thermal reaction 8h；The concentration of sodium bicarbonate solution described in step 4 is
0.15mol/L, the time of the immersion are 10h；The concentration of silver nitrate solution described in step 5 is 0.1mol/L, the immersion
Time be 18s；The time of immersion described in step 6 is 15s；The number of circulation immersion described in step 7 be 18 times, it is described
Condensation temperature is -40 DEG C, vacuum degree 35MPa.
Comparative example 1
1. carbon cloth is successively cleaned 20min with acetone, ethyl alcohol and deionized water, then carbon cloth is immersed in 65% nitric acid
Middle progress surface acid etching is for 24 hours and dry.
2. taking an above-mentioned carbon cloth to be put into the ammonium bicarbonate soln of 0.075mol/L to impregnate for 24 hours.
3. the carbon cloth impregnated in step 2 is taken out and is put into the silver nitrate solution of 0.15mol/L and impregnates 10s.
4. carbon cloth in step 3 is immersed in 10s in 2 again.
5. repeating step 3 and 4 circulations 20 times, carbon cloth loaded Ag is obtained2CO3Catalysis material.
6. the carbon cloth loaded Ag that step 5 is obtained2CO3Catalysis material, at -40 DEG C of condensation temperature, vacuum degree 35MPa
Under be freeze-dried, obtain carbon cloth loaded Ag2CO3Catalysis material.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by change, modification, substitution, combination and simplify,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of carbon cloth loads molybdenum disulfide/silver carbonate composite photo-catalyst, which is characterized in that the carbon cloth loads curing
Molybdenum/silver carbonate composite photo-catalyst is to be immersed in the carbon cloth of cleaning in nitric acid to carry out surface acid etching and drying；It then will place
The carbon cloth of reason is immersed in sodium molybdate-thiocarbamide aqueous solution the hydro-thermal reaction at 180~200 DEG C, obtains the carbon of load molybdenum sulfide
Cloth；The carbon cloth for loading molybdenum sulfide is impregnated in carbonate solution, then take out and is put into silver nitrate solution after immersion, then will
It is immersed in carbonate solution, the circulation immersion in silver nitrate solution and carbonate solution, is made after freeze-drying.
2. carbon cloth according to claim 1 loads molybdenum disulfide/silver carbonate composite photo-catalyst, which is characterized in that described
The solvent of cleaning is acetone, ethyl alcohol and deionized water, and the time of the cleaning is 10~20min；The concentration of the nitric acid is 60
~65%；The time of the surface acid etching be 10~for 24 hours；The time of the hydro-thermal reaction is 5~10h.
3. carbon cloth according to claim 1 loads molybdenum disulfide/silver carbonate composite photo-catalyst, which is characterized in that described
The volume ratio of the quality of sodium molybdate, the quality of thiocarbamide and deionized water is (0.1~0.2) g in sodium molybdate-thiocarbamide aqueous solution:
(0.1~0.2) g:(30~40) mL.
4. carbon cloth according to claim 1 loads molybdenum disulfide/silver carbonate composite photo-catalyst, which is characterized in that described
The number of circulation immersion is 10~20 times.
5. carbon cloth according to claim 1 loads molybdenum disulfide/silver carbonate composite photo-catalyst, which is characterized in that described
Carbonate solution is one or more of ammonium hydrogen carbonate, sodium bicarbonate, sodium carbonate or ammonium carbonate.
6. carbon cloth according to claim 1 loads molybdenum disulfide/silver carbonate composite photo-catalyst, which is characterized in that described
The concentration of silver nitrate solution is 0.1~0.2mol/L, and the concentration of the carbonate solution is 0.05~0.2mol/L.
7. carbon cloth according to claim 1 loads molybdenum disulfide/silver carbonate composite photo-catalyst, which is characterized in that described
The condition of freeze-drying are as follows: the temperature of freezing is -40~-46 DEG C, and vacuum degree is 35~45MPa.
8. carbon cloth according to claim 1-7 loads molybdenum disulfide/silver carbonate composite photo-catalyst preparation side
Method, which is characterized in that comprise the following specific steps that:
S1. carbon cloth is successively cleaned with acetone, ethyl alcohol and deionized water, then by carbon cloth be immersed in the nitric acid of 60-65% into
Row surface acid etching and drying；
S2. carbon cloth processed in step S1 is immersed in sodium molybdate and thiocarbamide mixed aqueous solution and is transferred in reaction kettle
Hydro-thermal reaction at 180-200 DEG C obtains the carbon cloth of load molybdenum sulfide；
S3. the carbon cloth for loading molybdenum sulfide is impregnated in carbonate solution I, takes out and be put into silver nitrate solution and impregnates II；Again
It is secondary that III is impregnated in carbonate solution；
S4. step S3 is repeated to recycle 10~20 times, it is freeze-dried, carbon cloth is made and loads MoS2/Ag2CO3Composite photocatalyst material
Material.
9. carbon cloth according to claim 8 loads molybdenum disulfide/silver carbonate composite photo-catalyst preparation method, feature
Be, described in step S3 immersion I time be 10~for 24 hours；The time of the immersion II is 10~20s, the immersion III
Time is 10~20s.
10. the described in any item carbon cloth load molybdenum disulfide/silver carbonate composite photo-catalysts of claim 1-7 are in photocatalysis field
In application.
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| CN110873473A (en) * | 2019-11-25 | 2020-03-10 | 云南大学 | Photo-thermal conversion material, preparation method thereof and solar photo-thermal conversion device |
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