CN102500426B - Low-temperature two-step method for preparing composite anatase type titanium dioxide visible light catalyst - Google Patents
Low-temperature two-step method for preparing composite anatase type titanium dioxide visible light catalyst Download PDFInfo
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- CN102500426B CN102500426B CN 201110282801 CN201110282801A CN102500426B CN 102500426 B CN102500426 B CN 102500426B CN 201110282801 CN201110282801 CN 201110282801 CN 201110282801 A CN201110282801 A CN 201110282801A CN 102500426 B CN102500426 B CN 102500426B
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Abstract
The invention discloses a low-temperature two-step method for preparing a composite anatase type titanium dioxide visible light catalyst, and belongs to the visible light catalyst. The preparation method comprises the following steps of: 1, adding titanium-containing precursor into alcohol, uniformly mixing and then adding a dopant, fully stirring, then adding an inhibitor and de-ionized water respectively, and performing water bath heating to prepare colloid containing titanium and doping element; and 2, cooling the prepared colloid to room temperature, transferring into a high-pressure-resistant container, adding a thermal decomposition type compound into the colloid, then quickly sealing the container, heating to perform reaction, preserving heat, obtaining precipitate after the reaction is finished, filtering the precipitate and washing with the de-ionized water and then drying to prepare the composite anatase type titanium dioxide visible light catalyst. The method has the advantages that: 1, the catalyst is prepared under the condition of 80-100 DEG C, and the energy consumption is favorably reduced during preparation; and 2, subsequent high-temperature treatment is not required in the method, the defect of high probability of losing the doping element through the high-temperature treatment is avoided, and the photo-catalytic performance is favorably improved.
Description
Technical field
The present invention relates to a kind of visible light catalyst, particularly a kind of low temperature two-step method prepares the composite octahedrite type titanium dioxide visible light catalyst.
Background technology
Anatase titanium dioxide is desirable catalysis material, but because its energy gap only has 3.2eV, need the ultraviolet light of higher-energy that the electronics in its valence band is excited, this part ultraviolet light only accounts for about 4% in the solar spectrum, accounts for 45% most visible lights part in the solar spectrum and then fails effectively to utilize.Also have the problem such as compound in electronics and hole in addition, cause quantum yield very low, these have all limited the application in practice of optically catalytic TiO 2 technology.Many studies show for preparing composite titanium dioxide by element doping in recent years, can widen spectral response range, more effectively utilizes solar energy.Simultaneously, element doping also can suppress the compound of electronics and hole, improves photocatalysis efficiency and the quantum yield of titanium dioxide.
The preparation method of titanium dioxide is divided into physical deposition method and chemical deposition at present.The common depositing temperature of physical deposition method is higher, and the depositing device complex and expensive.Chemical method prepares titanium dioxide and mainly contains liquid-phase precipitation method, sol-gal process and hydro-thermal method.What liquid-phase precipitation method and Prepared by Sol Gel Method went out is amorphous titania, is transformed into anatase crystal as need, then will carry out follow-up high-temperature process; Although hydro-thermal method can be prepared anatase titanium dioxide, reaction temperature is usually more than 150 ℃.If can realize that low temperature prepares anatase titanium dioxide, be conducive to reduce the energy consumption of preparation process, and can overcome the catalyst agglomeration phenomenon that follow-up high-temperature process causes.Even more important, the dioxide composite Ti-base catalyst usually can be because of follow-up high-temperature process, and make doped chemical particularly the nonmetal doping element run off, reduce photocatalysis performance.
Summary of the invention
The objective of the invention is to provide a kind of low temperature two-step method to prepare the composite octahedrite type titanium dioxide visible light catalyst, energy consumption is bigger in the process of solution preparation visible light catalyst, the catalyst agglomeration that follow-up high-temperature process causes, doped chemical particularly nonmetal doping element runs off, and reduces the problem of photocatalysis performance.
The object of the present invention is achieved like this: the concrete preparation method of composite octahedrite type titanium dioxide catalyst is:
The first step, the presoma that in alcohol, adds titaniferous, the mol ratio of the presoma of titaniferous and alcohol is 1:5～100, mix the back and add alloy, add inhibitor and deionized water respectively after fully stirring, the mol ratio of the presoma of titaniferous, alloy, inhibitor and deionized water is 1:0.05～5:0.01～50:0.5～50, the water-bath heating, water bath heating temperature fully makes the colloid of titaniferous and doped chemical after the reaction between 30～100 ℃;
Second step, after the colloid that makes is cooled to room temperature, in the immigration high-pressure-resistant vessel, in colloid, add thermal decomposition type compound, the mol ratio of the presoma of the titaniferous in the step 1 and thermal decomposition type compound is 1:0.1～100, then rapidly with seal of vessel, heating is reacted under 80～100 ℃ cryogenic conditions, be incubated 10～30 hours, after finishing, reaction obtains sediment, sediment is filtered and spends deionised water, dry under 50～100 ℃ of conditions then, make the composite octahedrite type titanium dioxide visible light catalyst.
The presoma of described titaniferous, any in employing butyl titanate, titanium tetrachloride, the isopropyl titanate.
Described alloy is to contain in Ag, Zn, Cu, Fe, Al, Co, Sn, Pt, V, Ta, Nb, Mo, Mn, F, Cl, Br, I, S, B, C, Si, N, the P water soluble compound any, or with any two of any mixed in molar ratio, or with wantonly three kinds of any mixed in molar ratio.
Described alcohol is any in ethanol, propyl alcohol, isopropyl alcohol, butanols, ethylene glycol, the propane diols.
Described inhibitor is divided into acidity, alkalescence and neutral three kinds, wherein acid inhibitor is any in nitric acid, hydrochloric acid, sulfuric acid, lactic acid, the citric acid, the alkalescence inhibitor is MEA, in diethanol amine, triethanolamine, ammoniacal liquor, NaOH, the potassium hydroxide any, neutral inhibitor are any in polyethylene glycol, the PVP.
Described thermal decomposition type compound is any in hydrogen peroxide, ammonium carbonate, carbonic hydroammonium, sodium acid carbonate, ammonium phosphate, ammonium dihydrogen phosphate (ADP), diammonium hydrogen phosphate, zinc carbonate, ammonium nitrate, ammonium nilrite, the azodiisobutyronitrile.
Beneficial effect owing to adopted such scheme, is prepared the colloid of titaniferous and doped chemical by adopting the water-bath heating in advance, adds thermal decomposition type compound in colloid cooling back then, prepares composite titanium dioxide visible light catalyst.The principle of this method utilization reaction supercharging, under 80～100 ℃ cryogenic conditions, make the heat-decomposing compound reaction decomposes of adding, increase system internal pressure, promote the crystallization of titanium dioxide, solved the problem that under the cryogenic conditions below 100 ℃, is difficult to synthetic composite octahedrite type titanium dioxide catalyst.Because the colloidal dispersion that the adding of breakdown type compound makes is uniformly dispersed, end product particle agglomeration degree reduces simultaneously.
Advantage:
1, realized preparation composite octahedrite type titanium dioxide catalyst under 80～100 ℃ cryogenic conditions, be conducive to reduce the energy consumption in the preparation process, simultaneously can expand its range of application, as can directly carry out the in-situ preparing of catalyst at the carrier of non-refractory.
2, this method does not need to carry out follow-up high-temperature process, and the catalyst agglomeration of having avoided follow-up high-temperature process to cause, and the shortcoming of having avoided high-temperature process that doped chemical is run off are conducive to improve photocatalysis performance.
The specific embodiment
Below by embodiment in detail the present invention is described in detail.
Embodiment 1: the 0.06mol butyl titanate is added in the 1.80mol ethanol, after mixing, add the 0.01mol zinc acetate, fully stir the back and drip the 0.04mol red fuming nitric acid (RFNA), slowly drip the 0.10mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 60 ℃ of water-baths to continue to stir in container, make the colloidal tio 2 of mixing zinc behind the reaction 1.5h.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, move in the high-pressure-resistant vessel, add the 0.04mol zinc carbonate then, container is airtight, under 90 ℃ of conditions, be incubated 18h, sediment is filtered and use deionized water rinsing, make after 60 ℃ of dryings and mix zinc anatase titanium dioxide powder.(Scherrer equation) calculates the X ray diffracting spectrum that makes powder by the Scherrer formula, and its crystal average diameter is 8.8nm.
Visible light catalytic experiment: get the catalyst of 0.2g preparation, add and fill in the beaker of methyl orange aqueous solution that 200mL concentration is 10mg/L, magnetic agitation 0.5h makes catalyst keep even suspended state in the darkroom, reaches adsorption equilibrium.Be light source with the 500W xenon lamp, between beaker and light source, add the 400nm filter plate, the light of wavelength less than 400nm is filtered.React after 4 hours, get supernatant liquor after the centrifugation, measure absorbance at the 464nm place with ultraviolet-uisible spectrophotometer.Test result shows that the catalyst of preparation has visible light catalysis activity preferably, and the methyl orange degradation rate is 88.9%.
Embodiment 2: the 0.02mol isopropyl titanate is added in the 1.40mol ethanol, after mixing, add the 0.003mol silver nitrate, fully stir the back and drip 0.05mol lactic acid, slowly drip the 0.05mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 50 ℃ of water-baths to continue to stir in container, make the colloidal tio 2 of mixing silver behind the reaction 2h.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add the 0.008mol ammonium carbonate then, container is airtight, under 98 ℃ of conditions, be incubated 26h, sediment is filtered and use deionized water rinsing, make after 75 ℃ of dryings and mix silver-colored anatase titanium dioxide powder, the crystal average diameter is 10.8nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 90.5%.
Embodiment 3: the 0.09mol butyl titanate is added in the 1.98mol isopropyl alcohol, after mixing, add the 0.005mol ethanol tantalum, fully stir the back and drip the 0.08mol concentrated hydrochloric acid, slowly drip the 0.15mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 75 ℃ of water-baths to continue to stir in container, make the colloidal tio 2 of mixing tantalum behind the reaction 1.5h.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add the 1.05mol hydrogen peroxide then, container is airtight, under 92 ℃ of conditions, be incubated 22h, sediment is filtered and use deionized water rinsing, make after 65 ℃ of dryings and mix tantalum anatase titanium dioxide powder, the crystal average diameter is 9.7nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 93.6%.
Embodiment 4: the 0.05mol titanium tetrachloride is added in the 0.50mol ethanol, after mixing, add 0.09mol urea, fully stir the back and add the 0.009mol triethanol ammonium, slowly drip the 0.10mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 90 ℃ of water-baths to continue to stir in container, make the colloidal tio 2 of nitrating behind the reaction 20min.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add 0.01mol carbonic hydroammonium then, container is airtight, under 88 ℃ of conditions, be incubated 18h, sediment is filtered and use deionized water rinsing, make nitrating anatase titanium dioxide powder after 90 ℃ of dryings, the crystal average diameter is 10.2nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 89.8%.
Embodiment 5: the 0.07mol butyl titanate is added in the 1.05mol ethylene glycol, after mixing, add 0.012mol butter of tin and 0.006mol aluminum nitrate, fully stir the back and add the 0.002mol polyethylene glycol, slowly drip the 0.12mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 70 ℃ of water-baths to continue to stir in container, make the colloidal tio 2 of tin, aluminium codope behind the reaction 1.5h.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add the 0.03mol ammonium carbonate then, container is airtight, under 96 ℃ of conditions, be incubated 20h, sediment is filtered and uses deionized water rinsing, make the anatase titanium dioxide powder of tin, aluminum binary codope after 80 ℃ of dryings, the crystal average diameter is 10.1nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 89.2%.
Embodiment 6: the 0.055mol isopropyl titanate is added in the 4.06mol ethanol, after mixing, add 0.004mol ferric nitrate and 0.28mol ammonium fluoride, fully stir the back and drip the 0.15mol red fuming nitric acid (RFNA), slowly drip the 0.25mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 40 ℃ of water-baths to continue to stir in container, make iron, fluorin-doped colloidal tio 2 behind the reaction 2h.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add 0.026mol ammonium nitrate then, container is airtight, under 92 ℃ of conditions, be incubated 22h, sediment is filtered and uses deionized water rinsing, make iron, fluorin-doped anatase titanium dioxide powder after 60 ℃ of dryings, the crystal average diameter is 10.3nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 95.5%.
Embodiment 7: the 0.04mol butyl titanate is added in the 1.05mol isopropyl alcohol, after mixing, add 0.015mol copper nitrate and 0.03mol ethyl orthosilicate, fully stir the back and drip the 0.20mol red fuming nitric acid (RFNA), slowly drip the 0.20mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 70 ℃ of water-baths to continue to stir in container, make copper, silicon coblended colloidal tio 2 behind the reaction 1.5h.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add the 0.28mol hydrogen peroxide then, container is airtight, under 82 ℃ of conditions, be incubated 18h, sediment is filtered and uses deionized water rinsing, make copper, silicon coblended anatase titanium dioxide powder after 60 ℃ of dryings, the crystal average diameter is 8.3nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 83.6%.
Embodiment 8: the 0.16mol isopropyl titanate is added in the 3.05mol butanols, after mixing, add 0.05mol manganese sulfate, 0.02mol cobalt nitrate and 0.09mol ammonium chloride, fully stir the back and add 0.04mol diethanol ammonium, slowly drip the 0.30mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 50 ℃ of water-baths to continue to stir in container, make manganese, cobalt, chlorine co-doped colloidal tio 2 behind the reaction 2h.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add the 0.07mol ammonium dihydrogen phosphate (ADP) then, container is airtight, under 85 ℃ of conditions, be incubated 21h, sediment is filtered and uses deionized water rinsing, make manganese, cobalt, chlorine co-doped anatase titanium dioxide powder after 70 ℃ of dryings, the crystal average diameter is 9.2nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 94.8%.
Embodiment 9: the 0.23mol butyl titanate is added in the 3.05mol propane diols, after mixing, add the 0.012mol zirconium oxychloride, 0.035mol glucose, 0.012mol boric acid fully stirs the back and drips the 0.04mol citric acid, slowly drip the 0.30mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 80 ℃ of water-baths to continue to stir in container, make the colloidal tio 2 of zirconium, carbon, boron codope behind the reaction 30min.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add the 0.29mol ammonium nilrite then, container is airtight, under 99 ℃ of conditions, be incubated 30h, sediment is filtered and uses deionized water rinsing, make the anatase titanium dioxide powder of zirconium, carbon, boron codope after 60 ℃ of dryings, the crystal average diameter is 11.3nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 92.1%.
Embodiment 10: the 0.10mol butyl titanate is added in the 3.02mol ethanol, after mixing, add 0.005mol ethanol niobium, 0.008mol ammonium bromide and 0.007mol ammonium iodide, fully stir the back and add the 0.10mol MEA, slowly drip the 0.20mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 85 ℃ of water-baths to continue to stir in container, make the colloidal tio 2 of niobium, bromine, iodine codope behind the reaction 0.5h.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add the 0.05mol azodiisobutyronitrile then, container is airtight, under 82 ℃ of conditions, be incubated 19h, sediment is filtered and uses deionized water rinsing, make the anatase titanium dioxide powder of niobium, bromine, iodine codope after 60 ℃ of dryings, the crystal average diameter is 8.7nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 82.2%.
Embodiment 11: the 0.20mol isopropyl titanate is added in the 2.51mol ethanol, after mixing, add 0.01mol chloroplatinic acid, 0.01mol ruthenium trichloride, 0.02mol thiocarbamide, fully stir the back and drip the 0.12mol concentrated sulfuric acid, slowly drip the 0.40mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 45 ℃ of water-baths to continue to stir in container, make the colloidal tio 2 of platinum, ruthenium, sulphur codope behind the reaction 2h.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add 0.04mol ammonium nitrate then, container is airtight, under 97 ℃ of conditions, be incubated 19h, sediment is filtered and uses deionized water rinsing, make the anatase titanium dioxide powder of platinum, ruthenium, sulphur codope after 95 ℃ of dryings, the crystal average diameter is 11.5nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 92.3%.
Embodiment 12: the 0.35mol butyl titanate is added in the 9.55mol ethanol, after mixing, add 0.02mol vanadium trichloride, 0.02mol molybdenum pentachloride and 0.01mol Boratex, fully stir the back and add the 0.01mol PVP, slowly drip the 0.50mol deionized water after stirring 5min, keep vigorous stirring in the dropping process, place 70 ℃ of water-baths to continue to stir in container, make the colloidal tio 2 of vanadium, molybdenum, boron codope behind the reaction 0.5h.After the colloid for the treatment of above-mentioned preparation is cooled to room temperature, in the immigration high-pressure-resistant vessel, add the 0.24mol diammonium hydrogen phosphate then, container is airtight, under 86 ℃ of conditions, be incubated 22h, sediment is filtered and uses deionized water rinsing, make the anatase titanium dioxide powder of vanadium, molybdenum, boron codope after 80 ℃ of dryings, the crystal average diameter is 9.0nm.The visible light catalytic performance test is identical with embodiment 1, and the result shows that the methyl orange degradation rate is 86.8%.
Claims (1)
1. a low temperature two-step method prepares the composite octahedrite type titanium dioxide visible light catalyst, it is characterized in that: the concrete preparation method of composite octahedrite type titanium dioxide catalyst is:
The first step, the presoma that in alcohol, adds titaniferous, the mol ratio of the presoma of titaniferous and alcohol is 1:5～100, mix the back and add alloy, add inhibitor and deionized water respectively after fully stirring, the mol ratio of the presoma of titaniferous, alloy, inhibitor and deionized water is 1:0.05～5:0.01～50:0.5～50, the water-bath heating, water bath heating temperature fully makes the colloid of titaniferous and doped chemical after the reaction between 30～100 ℃;
Second step, after the colloid that makes is cooled to room temperature, in the immigration high-pressure-resistant vessel, in colloid, add thermal decomposition type compound, the mol ratio of the presoma of the titaniferous in the step 1 and thermal decomposition type compound is 1:0.1～100, then rapidly with seal of vessel, heating is reacted under 80～100 ℃ cryogenic conditions, be incubated 10～30 hours, after finishing, reaction obtains sediment, sediment is filtered and spends deionised water, dry under 50～100 ℃ of conditions then, make the composite octahedrite type titanium dioxide visible light catalyst;
Described alloy is to contain in Ag, Zn, Cu, Fe, Al, Co, Sn, Pt, V, Ta, Nb, Mo, Mn, F, Cl, Br, I, S, B, C, Si, N, the P water soluble compound any, or with any two of any mixed in molar ratio, or with wantonly three kinds of any mixed in molar ratio;
Described thermal decomposition type compound is any in hydrogen peroxide, ammonium carbonate, carbonic hydroammonium, sodium acid carbonate, ammonium phosphate, ammonium dihydrogen phosphate (ADP), diammonium hydrogen phosphate, zinc carbonate, ammonium nitrate, ammonium nilrite, the azodiisobutyronitrile.
2, low temperature two-step method according to claim 1 prepares the composite octahedrite type titanium dioxide visible light catalyst, it is characterized in that: the presoma of described titaniferous, any in employing butyl titanate, titanium tetrachloride, the isopropyl titanate.
3, low temperature two-step method according to claim 1 prepares the composite octahedrite type titanium dioxide visible light catalyst, it is characterized in that: described alcohol is any in ethanol, propyl alcohol, isopropyl alcohol, butanols, ethylene glycol, the propane diols.
4, low temperature two-step method according to claim 1 prepares the composite octahedrite type titanium dioxide visible light catalyst, it is characterized in that: described inhibitor is divided into acidity, alkalescence and neutral three kinds, wherein acid inhibitor is any in nitric acid, hydrochloric acid, sulfuric acid, lactic acid, the citric acid, the alkalescence inhibitor is any in MEA, diethanol amine, triethanolamine, ammoniacal liquor, NaOH, the potassium hydroxide, and neutral inhibitor is any in polyethylene glycol, the PVP.
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| CN117658207A (en) * | 2023-11-09 | 2024-03-08 | 广州市浩立生物科技有限公司 | Preparation method and application of nano titanium dioxide powder |
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| CN100998937A (en) * | 2007-01-05 | 2007-07-18 | 华南理工大学 | Multi element daged-anatase type TiO2 collosol photo catalyst and its preparation method |
| CN101053839A (en) * | 2007-05-18 | 2007-10-17 | 浙江大学 | Sulfur doped titanium dioxide photocatalyst with anatase structure water-heating preparation method |
| CN101508464A (en) * | 2009-02-09 | 2009-08-19 | 武汉理工大学 | Process for preparing anatase type nano-titanium dioxide |
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| CN100998937A (en) * | 2007-01-05 | 2007-07-18 | 华南理工大学 | Multi element daged-anatase type TiO2 collosol photo catalyst and its preparation method |
| CN101053839A (en) * | 2007-05-18 | 2007-10-17 | 浙江大学 | Sulfur doped titanium dioxide photocatalyst with anatase structure water-heating preparation method |
| CN101508464A (en) * | 2009-02-09 | 2009-08-19 | 武汉理工大学 | Process for preparing anatase type nano-titanium dioxide |
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