CN106881094A - A kind of Fe/Zn codopes TiO with visible light catalysis activity2Preparation method - Google Patents
A kind of Fe/Zn codopes TiO with visible light catalysis activity2Preparation method Download PDFInfo
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- 238000000034 method Methods 0.000 title abstract description 9
- 238000006555 catalytic reaction Methods 0.000 title abstract 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 42
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 15
- 230000003197 catalytic effect Effects 0.000 claims abstract description 14
- 239000011592 zinc chloride Substances 0.000 claims abstract description 8
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 38
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 10
- 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 9
- 239000012153 distilled water Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 abstract description 21
- 239000002351 wastewater Substances 0.000 abstract description 7
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 abstract description 5
- 238000004043 dyeing Methods 0.000 abstract description 5
- 239000003344 environmental pollutant Substances 0.000 abstract description 5
- 231100000719 pollutant Toxicity 0.000 abstract description 5
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000001988 toxicity Effects 0.000 abstract description 2
- 231100000419 toxicity Toxicity 0.000 abstract description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 11
- 229940012189 methyl orange Drugs 0.000 description 11
- 230000001699 photocatalysis Effects 0.000 description 10
- 239000013078 crystal Substances 0.000 description 9
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 6
- 239000004753 textile Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 238000005273 aeration Methods 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000001055 reflectance spectroscopy Methods 0.000 description 4
- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
- 239000000987 azo dye Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000000979 synthetic dye Substances 0.000 description 1
- 238000004065 wastewater treatment 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with zinc, cadmium or mercury
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
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- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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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Abstract
The present invention provides a kind of Fe/Zn codopes TiO with visible light catalysis activity2Preparation method, belong to catalyst preparation technique field.The method is by by butyl titanate, FeCl3And ZnCl2Codope TiO is prepared by sol-gal process2Catalyst, and for the treatment of dyeing waste water, as a result show, 500 DEG C of calcining Fe/Zn codopes TiO2With good catalytic effect.It is an advantage of the invention that：The catalyst of preparation does not have toxicity, cheap, with stronger resistance to corrosion, pollutant is degraded using visible ray.
Description
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to Fe/Zn co-doped TiO with visible light catalytic activity2The preparation method of (1).
Background
In recent years, with the development of the textile industry, a large amount of waste water in the textile industry is discharged into water. The total amount of wastewater discharged by the textile industry in 2014 is 19.6 hundred million tons, which accounts for 9.55 percent of the total amount of wastewater discharged by the industrial industry in China. In addition, the water quality standard is stricter when the discharge standard of pollutants in textile dyeing and finishing industry water (GB4287-2012) is implemented.
80% of the textile industry wastewater comes from printing and dyeing, has the characteristics of high organic matter concentration, complex components, deep chromaticity and the like, and belongs to the industrial wastewater which is difficult to treat. Azo dyes are the most widely used synthetic dyes in printing and dyeing processes, have toxicity and carcinogenicity, and are difficult to remove by the traditional sewage treatment technology. Methyl orange is a typical azo dye and is commonly used for the research of wastewater treatment process in textile industry.
The photocatalytic oxidation technology can effectively remove organic matters in water. In the photocatalyst, with TiO2Most commonly. TiO 22The preparation method of the TiO compound is multiple, wherein the sol-gel method is simple and convenient, the shape, the uniformity and the like of the product can be controlled by simply controlling experimental conditions, and the TiO compound is relatively ideal TiO2A preparation method.
Disclosure of Invention
The invention aims to solve the technical problem of providing Fe/Zn co-doped TiO with visible light catalytic activity2The preparation method of (1).
The method comprises the following specific preparation steps:
(1) dropping tetrabutyl titanate into absolute ethyl alcohol, and adding a proper amount of FeCl3And ZnCl2Stirring at constant speed for 30min to obtain solution A;
(2) adding acetic acid and distilled water into absolute ethyl alcohol to prepare a solution B;
(3) uniformly dropping the solution B prepared in the step (2) into the solution A prepared in the step (1) while stirring to form sol;
(4) standing the sol obtained in the step (3) at room temperature to form gel, and drying at 105 ℃ to form xerogel;
(5) grinding the xerogel obtained in the step (4), calcining at the temperature of 450-550 ℃, and grinding to obtain Fe/Zn co-doped TiO2。
Wherein,
the volume ratio of tetrabutyl titanate to absolute ethyl alcohol in the step (1) is as follows: 1:2-3: 5; FeCl3The mass ratio of the mixed solution to tetrabutyl titanate is 0.0002:68, ZnCl2The mass ratio of the titanium oxide to tetrabutyl titanate is 0.0001: 68.
The volume ratio of the absolute ethyl alcohol, the acetic acid and the distilled water in the step (2) is 12:8: 3.
FeCl in step (2)3The molar doping amount of (1) is 0.0006 percent, ZnCl2The molar doping amount of (b) was 0.0004%.
The volume ratio of the solution A to the solution B in the step (3) is 4:5-5: 6.
The calcination temperature in the step (5) is 500 ℃, and the effect is best.
Fe/Zn co-doped TiO obtained in step (5)2The specific surface area of (1) is 100-120m2Per g, canAbsorbing light waves with wavelength less than 425 nm.
The Fe/Zn co-doped TiO2Can be used for treating printing and dyeing wastewater, in particular to wastewater containing organic pollutant methyl orange.
The technical scheme of the invention has the following beneficial effects:
1) Fe/Zn co-doped TiO2The catalyst has the advantages of no toxicity, low price, strong corrosion resistance and high efficiency of catalyzing pollutants.
2) The Fe/Zn co-doped TiO2The catalyst can degrade organic matters at normal temperature and normal pressure; visible light can be used for decomposing pollutants, and the catalytic effect under ultraviolet light is better; low selectivity to pollutants, thorough decomposition, no secondary pollution and high application value.
Drawings
FIG. 1 shows different kinds of TiO in examples of the present invention2XRD spectrogram;
FIG. 2 shows the doping ratio of Fe/Zn co-doped TiO2Influence of the effect of photocatalytic oxidation of methyl orange.
Detailed Description
In order to make the technical problems, technical solutions and advantages of the present invention more apparent, the following detailed description is given with reference to the accompanying drawings and specific embodiments.
The invention provides Fe/Zn co-doped TiO with visible light catalytic activity2The preparation method of (1). The method mainly comprises the following steps:
(1) mixing tetrabutyl titanate and FeCl3And ZnCl2Dripping into anhydrous ethanol, and stirring at constant speed for 30min to obtain solution A;
(2) adding acetic acid and distilled water into absolute ethyl alcohol to prepare a solution B;
(3) uniformly dropping the solution B prepared in the step (2) into the solution A prepared in the step (1) while stirring to form sol;
(4) standing the sol obtained in the step (3) at room temperature to form gel, and drying at 105 ℃ to form xerogel;
(5) grinding the xerogel obtained in the step (4), calcining at the temperature of 450-550 ℃, and grinding to obtain Fe/Zn co-doped TiO2。
The following examples are given by way of illustration.
Example 1
Dripping 68mL (0.2mol) of butyl titanate into 120mL of absolute ethyl alcohol at room temperature, and magnetically stirring at a constant speed for 30min to obtain a uniform and transparent yellow solution A; taking 80mL of acetic acid as a hydrolysis inhibitor, and taking 120mL of absolute ethyl alcohol and 30mL of distilled water, and uniformly mixing to form a solution B; and slowly dropping the solution B into the solution A (after 1 h) under magnetic stirring to form sol. Aging at 30 deg.C for 7d to form gel. Drying at 105 ℃ to obtain dry gel, grinding the dry gel, calcining at 500 ℃ for 5h, and grinding again to obtain TiO2And (3) powder.
Analysis of 500 ℃ calcined TiO Using Dmax-RB Rotary Anode diffractometer (XRD)2As shown in fig. 1, the result indicates that undoped TiO was obtained as a crystal phase of (Cu K α target, λ 0.1506nm)2The crystal phase of (A) is mainly anatase phase. Ultraviolet-visible diffuse reflectance spectroscopy for TiO determination2The forbidden band width of the crystal is 3.02 eV; the specific surface area of the catalyst measured by a specific surface area measuring instrument is 60m2/g。
The application of the catalyst is as follows: calcination of undoped TiO at 500 deg.C2Degrading methyl orange. The reaction is carried out in a photocatalytic reactor, into which the TiO is first introduced2The catalyst was maintained at a concentration of 0.1 g/L. Opening oxygen generator, regulating air flow rate to 1.0L/min, aerating for 30min, and then introducing into reactorMethyl orange solution was added to make the initial concentration 50 mg/L. Starting a visible light wave band of a xenon lamp light source, and keeping continuous aeration on the solution. Samples were taken every 30min and after centrifugation their absorbance at 600nm was determined as shown in FIG. 2. The results show that the undoped TiO is calcined at 500 DEG C2The removal rate of methyl orange by photocatalytic oxidation is 31.3 percent respectively.
Example 2
68mL (0.2mol) of butyl titanate is dropped into 120mL of absolute ethyl alcohol at room temperature, FeCl is added30.00033g, and magnetically stirring at a constant speed for 30min to obtain a uniform and transparent yellow solution A; taking 80mL of acetic acid as a hydrolysis inhibitor, and taking 120mL of absolute ethyl alcohol and 30mL of distilled water, and uniformly mixing to form a solution B; and slowly dropping the solution B into the solution A (after 1 h) under magnetic stirring to form sol. Aging at 30 deg.C for 7d to form gel. Drying at 105 ℃ to obtain dry gel, grinding the dry gel, calcining at 500 ℃ for 5h, and grinding again to obtain TiO2And (3) powder.
Analysis of 500 ℃ calcined Fe-doped TiO Using Dmax-RB Rotary Anode diffractometer (XRD)2With a crystal phase of (CuK α target, λ 0.1506nm), as shown in fig. 1, the results indicate that Fe is doped with TiO2The crystal phase of (A) is mainly anatase phase. Ultraviolet-visible diffuse reflectance spectroscopy for TiO determination2The forbidden band width of the crystal is 2.95 eV; the specific surface area of the catalyst measured by a specific surface area measuring instrument is 67m2/g。
The application of the catalyst is as follows: calcination of Fe-doped TiO at 500 deg.C2(the mol doping amount of Fe is 0.001%) to degrade methyl orange. The reaction is carried out in a photocatalytic reactor, into which the TiO is first introduced2The catalyst was maintained at a concentration of 0.1 g/L. And opening the oxygen generator, adjusting the air flow to be 1.0L/min, aerating for 30min, and then adding the methyl orange solution into the reactor to ensure that the initial concentration of the methyl orange solution is 50 mg/L. Starting a visible light wave band of a xenon lamp light source, and keeping continuous aeration on the solution. Samples were taken every 30min and after centrifugation their absorbance at 600nm was determined as shown in FIG. 2. The results show that calcination of Fe-doped TiO at 500 deg.C2The removal rate of methyl orange by photocatalytic oxidation is 50.7 percent respectively.
Example 3
68mL (0.2mol) of butyl titanate is dropped into 120mL of absolute ethyl alcohol at room temperature, and ZnCl is added20.00025g, and magnetically stirring at a constant speed for 30min to obtain a uniform and transparent yellow solution A; taking 80mL of acetic acid as a hydrolysis inhibitor, and taking 120mL of absolute ethyl alcohol and 30mL of distilled water, and uniformly mixing to form a solution B; and slowly dropping the solution B into the solution A (after 1 h) under magnetic stirring to form sol. Aging at 30 deg.C for 7d to form gel. Drying at 105 ℃ to obtain dry gel, grinding the dry gel, calcining at 500 ℃ for 5h, and grinding again to obtain TiO2And (3) powder.
Analysis of calcined Zn-doped TiO at 500 ℃ Using Dmax-RB Rotary Anode diffractometer (XRD)2(molar doping amount of Zn is 0.001%) of a crystalline phase (Cu K α target, λ 0.1506nm), as shown in fig. 1, and the results show that Zn-doped TiO2The crystal phase of (A) is mainly anatase phase. Ultraviolet-visible diffuse reflectance spectroscopy for TiO determination2The forbidden band width of the crystal is 2.99 eV; the specific surface area of the catalyst measured by a specific surface area measuring instrument is 93m2/g。
The application of the catalyst is as follows: calcining Zn doped TiO at 500 deg.C2(Zn mol doping amount is 0.001%) methyl orange is degraded. The reaction is carried out in a photocatalytic reactor, into which the TiO is first introduced2The catalyst was maintained at a concentration of 0.1 g/L. And opening the oxygen generator, adjusting the air flow to be 1.0L/min, aerating for 30min, and then adding the methyl orange solution into the reactor to ensure that the initial concentration of the methyl orange solution is 50 mg/L. Starting a visible light wave band of a xenon lamp light source, and keeping continuous aeration on the solution. Samples were taken every 30min and after centrifugation their absorbance at 600nm was determined as shown in FIG. 2. The results show that Zn-doped TiO is calcined at 500 DEG C2The removal rate of methyl orange by photocatalytic oxidation is 44.2 percent respectively.
Example 4
68mL (0.2mol) of butyl titanate was added dropwise to 120mL of absolute ethanol at room temperature, and 0.0002g of FeCl was added3And 0.0001g ZnCl2Uniformly stirring for 30min to obtain a uniform and transparent yellow solution A; taking 80mL of acetic acid as a hydrolysis inhibitor, and taking 120mL of absolute ethyl alcohol and 30mL of distilled water, and uniformly mixing to form a solution B; and slowly dropping the solution B into the solution A (after 1 h) under magnetic stirring to form sol. Aging at 30 deg.C for 7d to form gel. Drying at 105 ℃ to obtain dry gel, grinding the dry gel, calcining at 500 ℃ for 5h, and grinding again to obtain TiO2And (3) powder.
Analysis of 500 ℃ calcined Fe/Zn-codoped TiO Using Dmax-RB Rotary Anode diffractometer (XRD)2As shown in fig. 1, the result indicates that Fe/Zn co-doped TiO is present (Cu K α target, λ 0.1506nm)2The crystal phase of (A) is mainly anatase phase. Ultraviolet-visible diffuse reflectance spectroscopy for TiO determination2The forbidden band width of (A) is 2.93 eV; the specific surface area of the catalyst measured by a specific surface area measuring instrument is 115m2/g。
The application of the catalyst is as follows: calcination of Fe/Zn co-doped TiO at 500 deg.C2(the mol doping amount of Fe is 0.0006%, and the mol doping amount of Zn is 0.0004%) degraded methyl orange. The reaction is carried out in a photocatalytic reactor, into which the TiO is first introduced2The catalyst was maintained at a concentration of 0.1 g/L. And opening the oxygen generator, adjusting the air flow to be 1.0L/min, aerating for 30min, and then adding the methyl orange solution into the reactor to ensure that the initial concentration of the methyl orange solution is 50 mg/L. Starting a visible light wave band of a xenon lamp light source, and keeping continuous aeration on the solution. Samples were taken every 30min and after centrifugation their absorbance at 600nm was determined as shown in FIG. 2. The results show that the Fe/Zn co-doped TiO is calcined at 500 DEG C2The removal rate of methyl orange by photocatalytic oxidation is 65.6 percent respectively.
The results show that the catalytic effect of the catalyst is enhanced after the metal is doped, and the results are related to the synergistic effect of the anatase content in the catalyst and the specific surface area of the catalyst.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. Fe/Zn co-doped TiO with visible light catalytic activity2The preparation method is characterized by comprising the following steps: the preparation method comprises the following specific steps:
(1) dropping tetrabutyl titanate into absolute ethyl alcohol, and adding FeCl3And ZnCl2Stirring at constant speed for 30min to obtain solution A;
(2) adding acetic acid and distilled water into absolute ethyl alcohol to prepare a solution B;
(3) uniformly dropping the solution B prepared in the step (2) into the solution A prepared in the step (1) while stirring to form sol;
(4) standing the sol obtained in the step (3) at room temperature to form gel, and drying at 105 ℃ to form xerogel;
(5) grinding the xerogel obtained in the step (4), calcining at the temperature of 450-550 ℃, and grinding to obtain Fe/Zn co-doped TiO2。
2. Fe/Zn co-doped TiO with visible light catalytic activity according to claim 12The preparation method is characterized by comprising the following steps: the volume ratio of tetrabutyl titanate to absolute ethyl alcohol in the step (1) is as follows: 1:2-3:5.
3. Fe/Zn co-doped TiO with visible light catalytic activity according to claim 12The preparation method is characterized by comprising the following steps: FeCl in the step (1)3The mass ratio of the mixed solution to tetrabutyl titanate is 0.0002:68, ZnCl2The mass ratio of the titanium oxide to tetrabutyl titanate is 0.0001: 68.
4. Fe/Zn co-doped TiO with visible light catalytic activity according to claim 12The preparation method is characterized by comprising the following steps: the volume ratio of the absolute ethyl alcohol to the acetic acid to the distilled water in the step (2) is as follows: 12:8:3.
5. Fe/Zn co-doped TiO with visible light catalytic activity according to claim 12The preparation method is characterized by comprising the following steps: the volume ratio of the solution A to the solution B in the step (3) is as follows: 4:5-5:6.
6. Fe/Zn co-doped TiO with visible light catalytic activity according to claim 12The preparation method is characterized by comprising the following steps: the calcination temperature in the step (5) is 500 ℃.
7. Fe/Zn co-doped TiO with visible light catalytic activity according to claim 12The preparation method is characterized by comprising the following steps: said step (c) is(5) The obtained Fe/Zn co-doped TiO2The specific surface area of (1) is 100-120m2And/g, can absorb light waves with the wavelength less than 425 nm.
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| CN1751785A (en) * | 2004-09-20 | 2006-03-29 | 中国科学院过程工程研究所 | The preparation method of titania based catalysis material |
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| ZHI-HAO YUAN等: "Influence of co-doping of Zn(II) + Fe(III) on the photocatalytic activity of TiO2 for phenol degradation", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| 汪多仁编著: "《绿色化工助剂》", 31 January 2006, 科学技术文献出版社 * |
| 王中华等: "掺铁 TiO2 的制备及其光催化性能研究", 《山东化工》 * |
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