CN110302804B - VS (virtual switch)4-TiO2AC photocatalyst and preparation method thereof - Google Patents
VS (virtual switch)4-TiO2AC photocatalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 78
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000002245 particle Substances 0.000 claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 238000013329 compounding Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 32
- 239000011259 mixed solution Substances 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- 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
- 238000001035 drying Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims description 9
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 9
- IHIXIJGXTJIKRB-UHFFFAOYSA-N trisodium vanadate Chemical compound [Na+].[Na+].[Na+].[O-][V]([O-])([O-])=O IHIXIJGXTJIKRB-UHFFFAOYSA-N 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 8
- 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
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 7
- 239000012153 distilled water Substances 0.000 claims description 6
- 230000002431 foraging effect Effects 0.000 claims description 5
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- 238000002791 soaking Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 230000032683 aging Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims 1
- 239000003054 catalyst Substances 0.000 abstract description 15
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000013032 photocatalytic reaction Methods 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 3
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- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 239000000758 substrate Substances 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 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 4
- 238000005516 engineering process Methods 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 3
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- 238000002441 X-ray diffraction Methods 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- MHOFGBJTSNWTDT-UHFFFAOYSA-M 2-[n-ethyl-4-[(6-methoxy-3-methyl-1,3-benzothiazol-3-ium-2-yl)diazenyl]anilino]ethanol;methyl sulfate Chemical compound COS([O-])(=O)=O.C1=CC(N(CCO)CC)=CC=C1N=NC1=[N+](C)C2=CC=C(OC)C=C2S1 MHOFGBJTSNWTDT-UHFFFAOYSA-M 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 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
- 150000001721 carbon Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 230000007613 environmental effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
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- 238000004528 spin coating 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
-
- B01J35/39—
-
- 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
Abstract
The invention belongs to the field of catalysts, and particularly relates to VS4‑TiO2A/AC photocatalyst and a preparation method thereof. The photocatalyst comprises VS4、TiO2And activated carbon, and VS4And TiO2After compounding, the mixture is loaded on active carbon. The invention also provides VS4‑TiO2A method for preparing an AC photocatalyst. The invention converts VS4And TiO2Compound and widen TiO2So that VS4‑TiO2The photocatalyst can effectively utilize sunlight, has excellent catalytic efficiency when used for photocatalytic reaction, solves the problems of fixation and recovery of the photocatalyst by taking the activated carbon particles as catalyst carriers, and simultaneously improves the utilization rate of the photocatalyst.
Description
Technical Field
The invention belongs to the field of catalysts, and particularly relates to VS4-TiO2A/AC photocatalyst and a preparation method thereof.
Background
Photocatalytic technology as a novel green environmental cleanerThe chemical technology has mild reaction condition and easy control, and has thorough degradation of pollutants without secondary pollution, so that the chemical technology has wide application prospect in the field of sewage treatment, and the photocatalyst widely applied at present is TiO2Due to TiO2The semiconductor used as the photocatalyst has the advantages of unique photochemical performance, excellent thermal stability, good biological inertia, no toxicity, no harm, simple and convenient manufacture and the like, and has the defects of wider forbidden band, only being excited by ultraviolet light to generate photocatalytic activity, low utilization rate of visible light, and low photocatalytic efficiency caused by the fact that visible light accounts for 45 percent of the total energy of solar energy and electrons and holes are easily compounded. Therefore, shortening the forbidden band width of the catalyst to expand the absorption spectrum to visible light is the key technology for improving the solar energy utilization rate.
VS4Is an emerging semiconductor material with a large specific surface area and a very narrow band gap (0.8-1.2eV), which makes it a promising near-infrared optical drive photocatalyst.
Chinese patent CN109012697A discloses a method for preparing a full-waveband TiO/VS photocatalyst for sunlight, and TiO/VS photocatalysts are respectively prepared2Sol and VS4Sol, then coating TiO on the aluminum substrate2Sol, recoat VS4Sol, drying and vacuum sintering to obtain TiO2/VS4The photocatalyst and the method for spin-coating the catalyst sol on the metal substrate ensure that the catalyst has poor adhesive force on the metal substrate and is easy to fall off, thereby influencing the subsequent catalytic effect.
Disclosure of Invention
In order to solve the problem that the photocatalyst in the prior art cannot effectively utilize visible light to cause low catalytic efficiency, the invention provides VS4-TiO2A/AC photocatalyst and a preparation method thereof.
The invention is realized by the following technical scheme:
VS (virtual switch)4-TiO2/AC photocatalyst comprising VS4、TiO2And activated carbon, and VS4And TiO2After compounding, the mixture is loaded on active carbon.
The inventionIt is another object of to provide a said VS4-TiO2The preparation method of the/AC photocatalyst comprises the following steps:
s1: pretreatment of activated carbon: respectively soaking the activated carbon in a nitric acid solution and a NaOH solution at normal temperature, washing the activated carbon by ultrasonic oscillation, and then washing the activated carbon by deionized water, drying and cooling the activated carbon for later use;
S2：VS4the preparation of (1): dissolving sodium orthovanadate and thioacetamide in deionized water, stirring until the sodium orthovanadate and the thioacetamide are dissolved, then carrying out hydrothermal reaction, centrifuging, washing, vacuum drying and grinding the obtained product to obtain VS4Powder particles;
s3: mixing anhydrous ethanol, acetic acid and tetrabutyl titanate thoroughly, stirring to dissolve to obtain clear solution, adding the above VS4Powder particles to obtain a mixed solution A;
s4: fully mixing absolute ethyl alcohol and distilled water, uniformly stirring, adjusting the pH value to acidity to obtain a mixed solution B, slowly dripping the mixed solution B into the continuously stirred mixed solution A, and obtaining a mixed solution C after dripping;
s5: putting the pretreated activated carbon into the mixed solution C, stirring, carrying out hot water bath to obtain a mixture of the activated carbon and gel, standing at room temperature for aging, drying, and calcining to obtain VS4-TiO2an/AC photocatalyst.
Preferably, the concentration of the nitric acid solution in the step S1 is 0.01-0.02 mol/L; the concentration of the NaOH solution is 0.01-0.02 mol/L; the drying temperature is 100-120 ℃, and the drying time is 12-16 h; the ground mesh number is 2-4 meshes, and the active carbon is granular, so that the catalyst has the advantage of convenience in recovery compared with the traditional powder catalyst.
Preferably, the molar ratio of the sodium orthovanadate to the thioacetamide in the step S2 is 1: 2-7; the temperature of the hydrothermal reaction is 140 ℃ to 160 ℃, and the reaction time is 12-48 h.
Preferably, the volume ratio of the absolute ethyl alcohol, the acetic acid and the tetrabutyl titanate in the step S3 is (4-6) to 1 (2-3).
Preferably, the pH adjustment to acidity in step S4 is specifically performed with 0.5mol/L of HNO3And adjusting the pH value of the solution to 2-3.
Preferably, the temperature of the hot water bath in the step S5 is 50-60 ℃, and the time is 30-60 min; the aging time is 24-36 h; the drying is carried out at the temperature of 100-120 ℃ for 10-12 h; the calcination is carried out by raising the temperature to 550 ℃ at the heating rate of 3-4 ℃/min and preserving the temperature for 2-3 h.
The invention has the beneficial effects that:
(1) the invention converts VS4And TiO2Compound and widen TiO2So that VS4-TiO2The photocatalyst can effectively utilize sunlight and has excellent catalytic efficiency when used for photocatalytic reaction.
(2) The invention solves the problems of fixing and recycling the photocatalyst by taking the active carbon particles as the catalyst carrier, has more stable properties than the prior art which takes the metal substrate as the carrier, is superior to the metal substrate carrier in treating the wastewater with stronger corrosivity (the metal substrate is easy to corrode in the wastewater with stronger corrosivity and causes the surface-loaded catalyst to fall off easily), and has wider application range; the active carbon particles are in a three-dimensional dispersion state in the wastewater, the pollutants are enriched to the surface through the adsorption effect, can be fully contacted with the pollutants, and then the loaded VS is utilized4-TiO2The photocatalyst carries out catalytic degradation on water pollutants, the adsorption capacity of the activated carbon is regenerated, the utilization rate of the photocatalyst is improved, and the efficiency of the photocatalytic reaction is improved.
(3) The invention is to turn VS4Activated carbon and TiO2VS obtained by calcining after fully mixing sol4-TiO2/AC photocatalyst, make VS4And TiO2The combination is more stable and uniform, and the active carbon loaded in the composite material is not easy to fall off and can be repeatedly used.
Drawings
FIG. 1 is VS prepared in example 14An XRD pattern of (a);
FIG. 2 is TiO2Photocatalyst, VS4-TiO2Photocatalyst and VS4-TiO2a/AC photocatalyst pair concentration ofDegradation rate curve chart of 30mg/L methylene blue solution.
Detailed Description
The invention will be further described with reference to the accompanying drawings and specific embodiments.
Example 1
S1: pretreatment of activated carbon: respectively soaking 2-4 meshes of activated carbon in a nitric acid solution with the molar concentration of 0.01mol/L and a NaOH solution with the molar concentration of 0.01mol/L at normal temperature, washing for 30min by ultrasonic oscillation, washing for multiple times by deionized water, then putting the treated activated carbon into an oven, drying for 16h at 100 ℃, and cooling for later use;
S2：VS4the preparation of (1): dissolving 2.7g of sodium orthovanadate and 7.5g of thioacetamide in 90mL of deionized water, magnetically stirring for 0.5h at the rotating speed of 340r/min, transferring to a 150mL high-temperature hydrothermal reaction kettle, keeping the temperature in an oven at 150 ℃ for 12h, naturally cooling to room temperature, centrifuging the obtained product, washing with water, washing with ethanol, drying in vacuum, and grinding to obtain VS4A catalyst;
s3: fully mixing 60mL of absolute ethyl alcohol, 10mL of acetic acid and 30mL of tetrabutyl titanate, stirring to obtain a clear solution, and weighing 0.5g of VS4Putting the powder particles into the clarified solution and stirring to obtain a mixed solution A;
s4: fully mixing 30mL of absolute ethyl alcohol and 30mL of distilled water, uniformly stirring, and using HNO with the concentration of 0.5mol/L3Adjusting the pH value of the solution to 2-3 to obtain a mixed solution B, slowly dripping the mixed solution B into the continuously stirred mixed solution A, and obtaining a mixed solution C after dripping;
s5: putting the pretreated activated carbon particles into the mixed solution C, stirring for 2h, then carrying out hot water bath at 60 ℃ for 30min to obtain a mixture of the activated carbon particles and gel, standing at room temperature for aging for 24h, drying at 100 ℃ and calcining at 500 ℃ to obtain VS4-TiO2an/AC photocatalyst.
VS prepared in step S24The XRD pattern of the catalyst is shown in FIG. 1, indicating successful preparation of VS4A catalyst.
Treatment test: in the visible, with a VS of 20g4-TiO2AC photocatalyst treatment 200mL of methylene with a concentration of 30mg/LThe degradation rate of the basic blue solution can reach 85.3 percent, as shown in figure 2.
Example 2
S1: pretreatment of activated carbon: respectively soaking 2-4 meshes of activated carbon in a nitric acid solution with the molar concentration of 0.01mol/L and a NaOH solution with the molar concentration of 0.01mol/L at normal temperature, washing for 30min by ultrasonic oscillation, washing for multiple times by deionized water, then putting the treated activated carbon into an oven, drying for 12h at 110 ℃, and cooling for later use;
S2：VS4the preparation of (1): dissolving 1.8g of sodium orthovanadate and 1.65g of thioacetamide in 60ml of deionized water, magnetically stirring for 1h at the rotating speed of 440r/min, transferring to a 100ml high-temperature hydrothermal reaction kettle, preserving heat for 24h in a 160 ℃ oven, naturally cooling to room temperature, centrifuging, washing with water, washing with ethanol, drying in vacuum, and grinding to obtain VS4A catalyst;
s3: fully mixing 60mL of absolute ethyl alcohol, 20mL of acetic acid and 30mL of tetrabutyl titanate, stirring to obtain a clear solution, and weighing 0.6g of VS4Putting the powder particles into the clarified solution and stirring to obtain a mixed solution A;
s4: fully mixing 30mL of absolute ethyl alcohol and 30mL of distilled water, uniformly stirring, and using HNO with the concentration of 0.5mol/L3Adjusting the pH value of the solution to 2-3 to obtain a mixed solution B, slowly dripping the mixed solution B into the continuously stirred mixed solution A, and obtaining a mixed solution C after dripping;
s5: putting the pretreated activated carbon particles into the mixed solution C, stirring for 2h, then carrying out hot water bath at 60 ℃ for 40min to obtain a mixture of the activated carbon particles and gel, standing at room temperature for aging for 36h, drying at 110 ℃ and calcining at 520 ℃ to obtain VS4-TiO2an/AC photocatalyst.
Treatment test: in the visible, with a VS of 20g4-TiO2The degradation rate can reach 82.1 percent when 200mL of methylene blue solution with the concentration of 30mg/L is treated by the AC photocatalyst.
Example 3
S1: pretreatment of activated carbon: respectively soaking 2-4 meshes of activated carbon in a nitric acid solution with the molar concentration of 0.01mol/L and a NaOH solution with the molar concentration of 0.01mol/L at normal temperature, washing for 30min by ultrasonic oscillation, washing for multiple times by distilled water, then putting the treated activated carbon into an oven, drying for 12h at 120 ℃, and cooling for later use;
S2：VS4the preparation of (1): dissolving 1.8g of sodium orthovanadate and 1.65g of thioacetamide in 60mL of deionized water, magnetically stirring for 1.5h at the rotating speed of 540r/min, transferring to a 100mL high-temperature hydrothermal reaction kettle, keeping the temperature in an oven at 160 ℃ for 48h, naturally cooling to room temperature, centrifuging, washing, vacuum drying, cooling, and grinding to obtain VS4A catalyst;
s3: fully mixing 40mL of absolute ethyl alcohol, 10mL of acetic acid and 20mL of tetrabutyl titanate, stirring to obtain a clear solution, and weighing 0.5g of VS4Putting the powder particles into the clarified solution and stirring to obtain a mixed solution A;
s4: fully mixing 20mL of absolute ethyl alcohol and 40mL of distilled water, uniformly stirring, and using HNO with the concentration of 0.5mol/L3Adjusting the pH value of the solution to 2-3 to obtain a mixed solution B, slowly dripping the mixed solution B into the continuously stirred mixed solution A, and obtaining a mixed solution C after dripping;
s5: putting the pretreated activated carbon particles into the mixed solution C, stirring for 2h, then carrying out hot water bath at 60 ℃ for 60min to obtain a mixture of the activated carbon particles and gel, standing at room temperature for aging for 48h, drying at 120 ℃ and calcining at 550 ℃ to obtain VS4-TiO2an/AC photocatalyst.
Treatment test: in the visible, with a VS of 20g4-TiO2The degradation rate can reach 78.4 percent when 200mL of methylene blue solution with the concentration of 30mg/L is treated by the AC photocatalyst.
Comparative example 1
Substantially the same as example 1, except that step S1 in example 1 was omitted and no activated carbon particles were added in step S5 to obtain VS4-TiO2A photocatalyst. VS prepared in example 14-TiO2AC photocatalyst, VS prepared in comparative example 14- TiO2Photocatalyst and single TiO2The photocatalysts are all used for photocatalytic reaction of methylene blue solution with the concentration of 30mg/L under visible light, the adding amount of the photocatalysts is 20g/200mL, and the degradation rate curve is shown in the figure2, it can be seen that VS was prepared as in example 14- TiO2The degradation effect of the/AC photocatalyst is obviously superior to that of VS4-TiO2Photocatalyst and single TiO2A photocatalyst.
Claims (6)
1. VS (virtual switch)4-TiO2/AC photocatalyst, characterized in that said VS4-TiO2the/AC photocatalyst comprises VS4、TiO2And activated carbon, said VS4And TiO2Loading on active carbon after compounding;
the VS4-TiO2The preparation method of the/AC photocatalyst comprises the following steps:
s1: pretreatment of activated carbon: respectively soaking the activated carbon in a nitric acid solution and a NaOH solution at normal temperature, washing the activated carbon by ultrasonic oscillation, and then washing the activated carbon by deionized water, drying and cooling the activated carbon for later use;
S2：VS4the preparation of (1): dissolving sodium orthovanadate and thioacetamide in deionized water, stirring until the sodium orthovanadate and the thioacetamide are dissolved, then carrying out hydrothermal reaction, centrifuging, washing, vacuum drying and grinding the obtained product to obtain VS4Powder particles;
s3: mixing anhydrous ethanol, acetic acid and tetrabutyl titanate thoroughly, stirring to dissolve to obtain clear solution, adding the above VS4Powder particles to obtain a mixed solution A;
s4: fully mixing absolute ethyl alcohol and distilled water, uniformly stirring, adjusting the pH value to acidity to obtain a mixed solution B, slowly dripping the mixed solution B into the continuously stirred mixed solution A, and obtaining a mixed solution C after dripping;
s5: putting the pretreated activated carbon into the mixed solution C, stirring, carrying out hot water bath to obtain a mixture of the activated carbon and gel, standing at room temperature for aging, drying, and calcining to obtain VS4-TiO2an/AC photocatalyst.
2. A VS as claimed in claim 14-TiO2the/AC photocatalyst is characterized in that the concentration of the nitric acid solution in the step S1 is 001-0.02 mol/L; the concentration of the NaOH solution is 0.01-0.02 mol/L; the drying temperature is 100-120 ℃, and the drying time is 12-16 h; the mesh number of the active carbon is 2-4 meshes.
3. A VS as claimed in claim 14-TiO2the/AC photocatalyst is characterized in that the molar ratio of the sodium orthovanadate to the thioacetamide in the step S2 is 1: 2-7; the temperature of the hydrothermal reaction is 140 ℃ to 160 ℃, and the reaction time is 12-48 h.
4. A VS as claimed in claim 14-TiO2the/AC photocatalyst is characterized in that the volume ratio of the absolute ethyl alcohol, the acetic acid and the tetrabutyl titanate in the step S3 is (4-6) to 1 (2-3).
5. A VS as claimed in claim 14-TiO2the/AC photocatalyst is characterized in that the pH is adjusted to acidity in step S4, specifically 0.5mol/L HNO3And adjusting the pH value of the solution to 2-3.
6. A VS as claimed in claim 14-TiO2the/AC photocatalyst is characterized in that the temperature of the hot water bath in the step S5 is 50-60 ℃, and the time is 30-60 min; the aging time is 24-36 h; the drying is carried out at the temperature of 100-120 ℃ for 10-12 h; the calcination is carried out by raising the temperature to 550 ℃ at the heating rate of 3-4 ℃/min and preserving the temperature for 2-3 h.
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| 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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| 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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| TiO2/AC复合催化剂光催化降解布洛芬;闫春燕 等;《化工环保》;20140630;第34卷(第3期);第1.2节 * |
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