CN110302804A - A kind of VS4-TiO2/ AC photochemical catalyst and preparation method thereof - Google Patents
A kind of VS4-TiO2/ AC photochemical catalyst and preparation method thereof Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 59
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 35
- 239000002245 particle Substances 0.000 claims abstract description 18
- 238000011068 loading method Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 33
- 239000011259 mixed solution Substances 0.000 claims description 30
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 7
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 7
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 7
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 7
- 229910000166 zirconium phosphate Inorganic materials 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 230000015556 catabolic process Effects 0.000 description 8
- 238000006731 degradation reaction Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000013019 agitation Methods 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000003610 charcoal Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- 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
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to catalyst fields, and in particular to a kind of VS4‑TiO2/ AC photochemical catalyst and preparation method thereof.The photochemical catalyst includes VS4、TiO2And active carbon, and VS4And TiO2Compound back loading is on the activated carbon.The present invention also provides VS4‑TiO2The preparation method of/AC photochemical catalyst.The present invention is by VS4And TiO2It is compound, widen TiO2Optical response range so that VS4‑TiO2Photochemical catalyst can efficiently use sunlight, with more excellent catalytic efficiency when for light-catalyzed reaction, be catalyst carrier by active carbon particle, solve the problems, such as the fixation of photochemical catalyst and recycling, while improving the utilization rate of photochemical catalyst.
Description
Technical field
The invention belongs to catalyst fields, and in particular to a kind of VS4-TiO2/ AC photochemical catalyst and preparation method thereof.
Background technique
For photocatalysis technology as a kind of novel green environment purification techniques, reaction condition is mild and easily controllable, right
Contaminant degradation is thoroughly without secondary pollution, so that it has broad application prospects in sewage treatment field, is widely used at present
Photochemical catalyst be TiO2, because of TiO2Semiconductor has unique photochemical properties, excellent thermostabilization as photochemical catalyst
Property, good biologically inert, the advantages such as nontoxic, the production is simple and convenient, its shortcoming is that its forbidden band is wider, it can only be ultraviolet
Light excitation generates photocatalytic activity, it is seen that light utilization efficiency is low, and visible light accounts for the 45% of solar energy gross energy, Er Qie electricity
Son-hole is easy compound, causes photocatalysis efficiency low.Therefore the forbidden bandwidth for shortening catalyst expands absorption spectrum to visible light
Exhibition is the key problem in technology for improving solar energy utilization ratio.
VS4It is a kind of emerging semiconductor material, there is very big specific surface area and very narrow band gap (0.8-1.2eV),
This makes it a kind of promising near infrared light driving photochemical catalyst.
Chinese patent CN109012697A discloses a kind of preparation method of sunlight all band TiO/VS photochemical catalyst, point
TiO is not prepared2Colloidal sol and VS4Then colloidal sol first applies TiO on aluminium substrate2Colloidal sol, then apply VS4After colloidal sol, drying, vacuum-sintering
Obtain TiO2/VS4Photochemical catalyst, the method for this spin coating catalyst colloidal sol on metal substrate, so that catalyst is in metal substrate
On adhesive force it is poor, be easy to fall off, influence subsequent catalytic effect.
Summary of the invention
It cannot efficiently use visible light in order to solve photochemical catalyst existing in the prior art and cause catalytic efficiency low
Problem, the invention proposes a kind of VS4-TiO2/ AC photochemical catalyst and preparation method thereof.
The present invention is achieved through the following technical solutions:
A kind of VS4-TiO2/ AC photochemical catalyst, including VS4、TiO2And active carbon, and VS4And TiO2Compound back loading is in work
On property charcoal.
It is another object of the present invention to provide the VS described in one kind4-TiO2The preparation method of/AC photochemical catalyst, including
Following steps:
S1: the pretreatment of active carbon: active carbon is impregnated under nitric acid solution and NaOH solution room temperature respectively, and with ultrasound
Wave concussion cleaning, then deionized water cleans, dries, is cooling, spare；
S2:VS4Preparation: sodium vanadate and thioacetamide are dissolved in deionized water, stirring to dissolve, then carry out
Products therefrom centrifugation, washing, vacuum drying, grinding are obtained VS by hydro-thermal reaction4Powder particle；
S3: dehydrated alcohol, acetic acid and butyl titanate are sufficiently mixed, and stirring and dissolving is clear solution, are added thereto
Above-mentioned VS4Powder particle obtains mixed solution A；
S4: dehydrated alcohol and distilled water are sufficiently mixed, and are stirred evenly, and are adjusted pH and obtained mixed solution B to acidity, are incited somebody to action
Mixed solution B is slowly dropped into the mixed solution A kept stirring, and mixed solution C is obtained after dripping off；
S5: pretreated active carbon is put into above-mentioned mixed solution C, hot bath after stirring, is obtained active carbon and is coagulated
The mixture of glue is placed at room temperature for ageing, then drying, calcining, obtains VS4-TiO2/ AC photochemical catalyst.
Preferably, the concentration of nitric acid solution described in step S1 is 0.01-0.02mol/L；The concentration of NaOH solution is
0.01-0.02mol/L；The temperature of the drying is 100-120 DEG C, time 12-16h；The mesh number of the grinding is 2-4 mesh,
Active carbon at this time is graininess, has the advantages that recycling is convenient compared to conventional powder catalyst.
Preferably, the molar ratio of sodium vanadate described in step S2 and the thioacetamide is 1:2-7；Hydro-thermal reaction
140-160 DEG C of temperature, reaction time 12-48h.
Preferably, the volume ratio of dehydrated alcohol described in step S3, acetic acid and butyl titanate is (4-6): 1:(2-3).
Preferably, adjusting pH described in step S4 is to acid specially with the HNO of 0.5mol/L3Solution adjusting pH to 2~
3。
Preferably, the temperature of hot bath described in step S5 is 50-60 DEG C, time 30-60min；The ageing when
Between be 24-36h；It is described drying for 100-120 DEG C at a temperature of dry 10-12h；The calcining is with the liter of 3-4 DEG C/min
Warm rate rises to 450-550 DEG C, keeps the temperature 2-3h.
Beneficial effects of the present invention:
(1) of the invention by VS4And TiO2It is compound, widen TiO2Optical response range so that VS4-TiO2Photochemical catalyst energy
Sunlight is enough efficiently used, with more excellent catalytic efficiency when for light-catalyzed reaction.
(2) present invention is catalyst carrier by active carbon particle, solves the problems, such as the fixation of photochemical catalyst and recycling, compared with
For metal substrate in the prior art as carrier, active carbon particle property is more stable, wants in the processing stronger waste water of corrosivity
Better than metal substrate carrier, (metal substrate is easy to be corroded in the stronger waste water of corrosivity, and leads to urging for area load
Agent is easy to fall off), application range is wider；Active carbon particle in waste water at three-dimensional scatter state, will be dirty by suction-operated
Dye object is enriched to surface, can come into full contact with pollutant, then recycle the VS of load4-TiO2Photochemical catalyst is to water pollution
Object carries out catalytic degradation, is that the adsorption capacity of active carbon is regenerated, while improving the utilization rate of photochemical catalyst, improves light
It is catalyzed the efficiency of reaction.
(3) present invention is by VS4, active carbon and TiO2The VS that colloidal sol is calcined after being sufficiently mixed4-TiO2/ AC light
Catalyst, so that VS4And TiO2In conjunction with more stable and uniform, be supported on not easily to fall off in active carbon, can reuse.
Detailed description of the invention
Fig. 1 is VS prepared by embodiment 14XRD spectrum.
Fig. 2 is TiO2Photochemical catalyst, VS4-TiO2Photochemical catalyst and VS4-TiO2/ AC photochemical catalyst is 30mg/L's to concentration
The degradation rate curve graph of methylene blue solution.
Specific embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment 1
S1: the pretreatment of active carbon: the nitric acid solution for being respectively 0.01mol/L with molar concentration by the active carbon of 2-4 mesh
It is impregnated under the NaOH solution room temperature of 0.01mol/L, and cleans 30min with ultrasonic oscillation, it is then repeatedly clear with deionized water
It washes, then by treated, active carbon is put into 100 DEG C of drying 16h in baking oven, and cooling is spare；
S2:VS4Preparation: 2.7g sodium vanadate and 7.5g thioacetamide are dissolved in 90mL deionized water, in 340r/
Magnetic agitation 0.5h under min revolving speed is transferred in 150mL high temperature hydrothermal reaction kettle, keeps the temperature 12h, natural cooling in 150 DEG C of baking ovens
To room temperature, products therefrom is centrifuged, is washed, ethanol washing, VS is ground to obtain in vacuum drying4Catalyst；
S3: 60mL dehydrated alcohol, 10mL acetic acid and 30mL butyl titanate are sufficiently mixed, and are clear solution after stirring,
Weigh the VS of 0.5g4Powder particle is put into clear solution and stirs to obtain mixed solution A；
S4: 30mL dehydrated alcohol and 30mL distilled water being sufficiently mixed, stirred evenly, and are 0.5mol/L's with concentration
HNO3Solution adjusts pH to 2~3 and obtains mixed solution B, and mixed solution B is slowly dropped into the mixed solution A kept stirring, drips
Mixed solution C is obtained after complete；
S5: pretreated active carbon particle is put into mixed solution C, is stirred 2h, then 60 DEG C of hot bath 30min, is obtained
To the mixture of active carbon particle and gel, it is placed at room temperature for ageing for 24 hours, then obtains VS after 100 DEG C of drying, 500 DEG C of calcinings4-
TiO2/ AC photochemical catalyst.
The VS of step S2 preparation4The XRD diagram of catalyst is as shown in Figure 1, show to be successfully prepared VS4Catalyst.
Processing test: under visible light, with the VS of 20g4-TiO2/ AC photocatalyst treatment 200mL concentration is 30mg/L's
Methylene blue solution, degradation rate is up to 85.3%, as shown in Figure 1.
Embodiment 2
S1: the pretreatment of active carbon: the nitric acid solution for being respectively 0.01mol/L with molar concentration by the active carbon of 2-4 mesh
It is impregnated under the NaOH solution room temperature of 0.01mol/L, and cleans 30min with ultrasonic oscillation, it is then repeatedly clear with deionized water
It washes, then by treated, active carbon is put into 110 DEG C of drying 12h in baking oven, and cooling is spare；
S2:VS4Preparation: 1.8g sodium vanadate and 1.65g thioacetamide are dissolved in 60ml deionized water,
Magnetic agitation 1h under 440r/min revolving speed is transferred in 100ml high temperature hydrothermal reaction kettle, is kept the temperature for 24 hours in 160 DEG C of baking ovens, natural
It is cooled to room temperature, products therefrom is centrifuged, wash, ethanol washing, VS is ground to obtain in vacuum drying4Catalyst；
S3: 60mL dehydrated alcohol, 20mL acetic acid and 30mL butyl titanate are sufficiently mixed, and are clear solution after stirring,
Weigh the VS of 0.6g4Powder particle is put into clear solution and stirs to obtain mixed solution A；
S4: 30mL dehydrated alcohol and 30mL distilled water being sufficiently mixed, stirred evenly, and are 0.5mol/L's with concentration
HNO3Solution adjusts pH to 2~3 and obtains mixed solution B, and mixed solution B is slowly dropped into the mixed solution A kept stirring, drips
Mixed solution C is obtained after complete；
S5: pretreated active carbon particle is put into mixed solution C, is stirred 2h, then 60 DEG C of hot bath 40min, is obtained
To the mixture of active carbon particle and gel, it is placed at room temperature for ageing 36h, then obtains VS after 110 DEG C of drying, 520 DEG C of calcinings4-
TiO2/ AC photochemical catalyst.
Processing test: under visible light, with the VS of 20g4-TiO2/ AC photocatalyst treatment 200mL concentration is 30mg/L's
Methylene blue solution, degradation rate is up to 82.1%.
Embodiment 3
S1: the pretreatment of active carbon: the nitric acid solution for being respectively 0.01mol/L with molar concentration by the active carbon of 2-4 mesh
It is impregnated under the NaOH solution room temperature of 0.01mol/L, and cleans 30min with ultrasonic oscillation, be then cleaned multiple times with distilled water,
Then by treated, active carbon is put into 120 DEG C of drying 12h in baking oven, and cooling is spare；
S2:VS4Preparation: 1.8g sodium vanadate and 1.65g thioacetamide are dissolved in 60mL deionized water,
Magnetic agitation 1.5h under 540r/min revolving speed is transferred in 100mL high temperature hydrothermal reaction kettle, keeps the temperature 48h in 160 DEG C of baking ovens, from
It is so cooled to room temperature, products therefrom is centrifuged, wash, be dried in vacuo, it is cooling, grind to obtain VS4Catalyst；
S3: 40mL dehydrated alcohol, 10mL acetic acid and 20mL butyl titanate are sufficiently mixed, and are clear solution after stirring,
Weigh the VS of 0.5g4Powder particle is put into clear solution and stirs to obtain mixed solution A；
S4: 20mL dehydrated alcohol and 40mL distilled water being sufficiently mixed, stirred evenly, and are 0.5mol/L's with concentration
HNO3Solution adjusts pH to 2~3 and obtains mixed solution B, and mixed solution B is slowly dropped into the mixed solution A kept stirring, drips
Mixed solution C is obtained after complete；
S5: pretreated active carbon particle is put into mixed solution C, is stirred 2h, then 60 DEG C of hot bath 60min, is obtained
To the mixture of active carbon particle and gel, it is placed at room temperature for ageing 48h, then obtains VS after 120 DEG C of drying, 550 DEG C of calcinings4-
TiO2/ AC photochemical catalyst.
Processing test: under visible light, with the VS of 20g4-TiO2/ AC photocatalyst treatment 200mL concentration is 30mg/L's
Methylene blue solution, degradation rate is up to 78.4%.
Comparative example 1
It is substantially the same manner as Example 1, the difference is that, the step S1 in embodiment 1 is omitted, and work is not added in step S5
Property charcoal particle, finally obtains VS4-TiO2Photochemical catalyst.
VS prepared by embodiment 14-TiO2VS prepared by/AC photochemical catalyst, comparative example 14-TiO2Photochemical catalyst and single
TiO2Photochemical catalyst is used to the light-catalyzed reaction for the methylene blue solution that concentration is 30mg/L, photocatalysis under visible light
The additive amount of agent is 20g/200mL, and degradation rate curve is as shown in Figure 1, it is seen then that VS prepared by embodiment 14-TiO2/ AC light
The degradation effect of catalyst is substantially better than VS4-TiO2Photochemical catalyst and single TiO2Photochemical catalyst.
Claims (7)
1. a kind of VS4-TiO2/ AC photochemical catalyst, which is characterized in that the VS4-TiO2/ AC photochemical catalyst includes VS4、TiO2With
Active carbon, the VS4And TiO2Compound back loading is on the activated carbon.
2. a kind of VS as described in claim 14-TiO2The preparation method of/AC photochemical catalyst, which is characterized in that including walking as follows
It is rapid:
S1: the pretreatment of active carbon: active carbon is impregnated under nitric acid solution and NaOH solution room temperature respectively, and is shaken with ultrasonic wave
Cleaning is swung, then deionized water cleans, dries, is cooling, spare；
S2:VS4Preparation: sodium vanadate and thioacetamide are dissolved in deionized water, stirring to dissolve, then carry out hydro-thermal
Products therefrom centrifugation, washing, vacuum drying, grinding are obtained VS by reaction4Powder particle；
S3: dehydrated alcohol, acetic acid and butyl titanate are sufficiently mixed, and stirring and dissolving is clear solution, are added thereto above-mentioned
VS4Powder particle obtains mixed solution A；
S4: dehydrated alcohol and distilled water are sufficiently mixed, and are stirred evenly, and are adjusted pH and obtained mixed solution B to acidity, will be mixed
Solution B is slowly dropped into the mixed solution A kept stirring, and mixed solution C is obtained after dripping off；
S5: pretreated active carbon is put into above-mentioned mixed solution C, hot bath after stirring, obtains active carbon and gel
Mixture is placed at room temperature for ageing, then drying, calcining, obtains VS4-TiO2/ AC photochemical catalyst.
3. a kind of VS according to claim 24-TiO2The preparation method of/AC photochemical catalyst, which is characterized in that in step S1
The concentration of the nitric acid solution is 0.01-0.02mol/L；The concentration of the NaOH solution is 0.01-0.02mol/L；The baking
Dry temperature is 100-120 DEG C, time 12-16h；The mesh number of the active carbon is 2-4 mesh.
4. a kind of VS according to claim 24-TiO2The preparation method of/AC photochemical catalyst, which is characterized in that in step S2
The molar ratio of the sodium vanadate and the thioacetamide is 1:2-7；140-160 DEG C of the temperature of hydro-thermal reaction, when reaction
Between be 12-48h.
5. a kind of VS according to claim 24-TiO2The preparation method of/AC photochemical catalyst, which is characterized in that in step S3
The volume ratio of the dehydrated alcohol, acetic acid and butyl titanate is (4-6): 1:(2-3).
6. a kind of VS according to claim 24-TiO2The preparation method of/AC photochemical catalyst, which is characterized in that in step S4
It is described to adjust pH to acid specially with the HNO of 0.5mol/L3Solution adjusts pH to 2~3.
7. a kind of VS according to claim 24-TiO2The preparation method of/AC photochemical catalyst, which is characterized in that in step S5
The temperature of the hot bath is 50-60 DEG C, time 30-60min；The time of the ageing is 24-36h；It is described drying for
10-12h is dried at a temperature of 100-120 DEG C；The calcining is rises to 450-550 DEG C with the heating rate of 3-4 DEG C/min, heat preservation
2-3h。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910543369.XA CN110302804B (en) | 2019-06-21 | 2019-06-21 | VS (virtual switch)4-TiO2AC photocatalyst and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910543369.XA CN110302804B (en) | 2019-06-21 | 2019-06-21 | VS (virtual switch)4-TiO2AC photocatalyst and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
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| CN110302804B CN110302804B (en) | 2022-01-04 |
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| CN113413905A (en) * | 2021-07-30 | 2021-09-21 | 陕西科技大学 | Vanadium tetrasulfide-nickel sulfide/graphite phase carbon nitride photocatalyst and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923652A (en) * | 2016-04-29 | 2016-09-07 | 陕西科技大学 | Multilevel-structured VS4 nano-powder, and preparation method and application thereof |
| CN108889310A (en) * | 2018-08-04 | 2018-11-27 | 徐靖才 | A kind of sunlight all band photocatalysis composite film and preparation method thereof |
| CN109012697A (en) * | 2018-08-04 | 2018-12-18 | 徐靖才 | A kind of sunlight all band TiO2/VS4The preparation method of photochemical catalyst |
-
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105923652A (en) * | 2016-04-29 | 2016-09-07 | 陕西科技大学 | Multilevel-structured VS4 nano-powder, and preparation method and application thereof |
| CN108889310A (en) * | 2018-08-04 | 2018-11-27 | 徐靖才 | A kind of sunlight all band photocatalysis composite film and preparation method thereof |
| CN109012697A (en) * | 2018-08-04 | 2018-12-18 | 徐靖才 | A kind of sunlight all band TiO2/VS4The preparation method of photochemical catalyst |
Non-Patent Citations (1)
| Title |
|---|
| 闫春燕 等: "TiO2/AC复合催化剂光催化降解布洛芬", 《化工环保》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113413905A (en) * | 2021-07-30 | 2021-09-21 | 陕西科技大学 | Vanadium tetrasulfide-nickel sulfide/graphite phase carbon nitride photocatalyst and preparation method thereof |
| CN113413905B (en) * | 2021-07-30 | 2022-06-21 | 陕西科技大学 | Vanadium tetrasulfide-nickel sulfide/graphite phase carbon nitride photocatalyst and preparation method thereof |
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