CN104353468A - Copper-silver double-doped TiO2 photocatalytic material and preparation method thereof - Google Patents
Copper-silver double-doped TiO2 photocatalytic material and preparation method thereof Download PDFInfo
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- CN104353468A CN104353468A CN201410715496.0A CN201410715496A CN104353468A CN 104353468 A CN104353468 A CN 104353468A CN 201410715496 A CN201410715496 A CN 201410715496A CN 104353468 A CN104353468 A CN 104353468A
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Abstract
The invention belongs to the technical field of photocatalytic materials and in particular relates to a copper-silver double-doped TiO2 photocatalytic material and a preparation method thereof. The preparation method comprises the following steps: (1) uniformly mixing absolute ethyl alcohol, dibutyl phthalate and glacial acetic acid to obtain a solution A; (2) uniformly mixing absolute ethyl alcohol, deionized water, copper nitrate crystals and silver nitrate and regulating the pH value of the solution to be 3-5 to obtain the solution B; (3) dropwise adding the solution B into the solution A according to the molar ratio of Ti to Cu to Ag being 1:(0.02-0.07):(0.01-0.04)) under a rapid stirring condition, stirring uniformly to form a precursor solution, ageing the precursor solution to form gel, drying at constant temperature, and grinding the dried gel into powder; and (4) calcining the powder obtained in the step 3 in a muffle furnace at 400-600 DEG C for 1-3h, thereby obtaining the copper-silver double-doped TiO2 photocatalytic material. The copper-silver double-doped TiO2 photocatalytic material has the advantages that the visible light absorptivity is improved, the combination of photogenerated electrons and electro hole pairs is inhibited, and the photocatalytic performance is improved.
Description
Technical field
The invention belongs to catalysis material technical field, be specifically related to a kind of copper-Yin codope TiO
2catalysis material and preparation method thereof.
Background technology
Day by day serious environmental pollution, seriously have impact on life and the development of the mankind.Photocatalysis technology is using its room temperature reaction and can directly utilize solar energy to drive the special performances such as reaction as light source, becomes a kind of desirable environmental pollution treatment technology and clear energy sources production technology.Due to nano-TiO
2photochemical catalyst has the advantages such as larger specific area, higher photochemical stability, stronger oxidation-reduction quality and nontoxic, low cost, effectively utilizes it, is expected to solve day by day serious problem of environmental pollution.
But, due to TiO
2energy gap be 3.2eV, absorbing wavelength can only be less than the photon of 387nm, and the sunshine medium ultraviolet light radiation part arriving earth surface only account for about 4% of whole sunshine power spectrum, therefore TiO
2the efficiency of sunshine is utilized to be very limited.In addition, light induced electron and hole (e in carrier
-and h
+) recombination rate high, quantum utilization rate is low, and this reduces photocatalysis efficiency dramatically.
Therefore TiO is probed into
2modification, improves its absorptivity to sunshine and the palliating degradation degree to pollutant to a greater extent, all has very great meaning for economize energy, environmental protection.At present, researchers improve TiO mainly through noble metal loading, ion doping, composite semiconductor, the means such as organic dye sensitized
2photocatalysis performance, improve its photocatalysis efficiency.Wherein ion doping is the most general method, takes TiO
2with the mode of doped transition metal ions, its degradation property can be increased, greatly improve TiO
2photocatalytic activity, and then improve its degradation capability to multiple organic wastewater.
Summary of the invention
The object of the invention is to the defect for prior art existence and deficiency, provide a kind of and expand TiO
2visible light-responded scope, reduce the recombination rate in electronics and hole, thus improve the copper-Yin codope TiO of its photocatalysis performance under sunshine
2catalysis material and preparation method thereof.
For achieving the above object, the present invention is by the following technical solutions:
Copper-Yin codope TiO of the present invention
2the Ti:Cu:Ag mol ratio of catalysis material is 1:(0.02 ~ 0.07): (0.01 ~ 0.04).
Part catalysis material preparation method of the present invention, comprises the following steps:
Step 1), by analytically pure absolute ethyl alcohol, Butyl Phthalate, glacial acetic acid Homogeneous phase mixing, obtain solution A;
Step 2), by analytically pure absolute ethyl alcohol, deionized water, copper nitrate crystal, silver nitrate Homogeneous phase mixing, and solution ph is adjusted to 3 ~ 5, obtains B solution;
Step 3), under rapid stirring, be 1:(0.02 ~ 0.07 by Ti:Cu:Ag mol ratio): (0.01 ~ 0.04), B solution is dropwise added in solution A, precursor sol is formed after stirring, form gel by after the ageing of gained precursor sol, then constant temperature drying, then the xerogel after drying is ground to form powder;
Step 4), by step 3) gained powder use Muffle furnace 400 ~ 600 DEG C calcining 1 ~ 3h, namely obtain copper-Yin codope TiO
2catalysis material.
Further, step 1) described absolute ethyl alcohol, Butyl Phthalate, glacial acetic acid in molar ratio (10 ~ 20): 1:(1 ~ 5) ratio uniform mixing.
Further, step 2) described absolute ethyl alcohol, deionized water, copper nitrate crystal, silver nitrate is in molar ratio for (1 ~ 2): 1:(0.0018 ~ 0.0119): the ratio of (0.00096 ~ 0.0068) mixes.
Further, step 3) described A, B solution mixing, in solution A, in butyl titanate and B solution, the mol ratio of deionized water is 1:(5 ~ 10).
Further, step 2) described adjustment solution ph adopts concentration to be the aqueous solution of nitric acid of 2 ~ 4mol/L.
Further, step 2) described copper nitrate crystal employing Gerhardite crystal.
Further, step 3) described ripening is ageing 24 ~ 48h in atmosphere.
Further, step 3) temperature of described constant temperature drying is 80 ~ 100 DEG C, the time is 12 ~ 20h, and described oven dry adopts thermostatic drying chamber.
Compared with prior art, the present invention has following useful technique effect: due to Cu
2+radius (0.072nm) and Ti
4+radius (0.065nm) difference is very little, therefore, and Cu
2+tiO can be entered
2lattice, replaces Ti
4+, cause distortion of lattice, produce the trap bit in electronics or hole, strengthen the separating power of electron-hole pair; And Ag
+radius (about 0.126nm), much larger than Ti
4+radius, therefore Ag
+tiO can not be entered
2lattice, in calcination process, can be diffused into catalyst grain surface.Ag is to TiO
2the improvement of photocatalysis performance, mainly improves from introducing impurity energy level aspect.Copper-Yin codope TiO
2, by the synergy of two kinds of element doping modifications, improve TiO
2to the absorptivity of visible ray, suppress its photo-generate electron-hole to compound, improve TiO
2photocatalysis performance.
Accompanying drawing explanation
Fig. 1 is TiO prepared by comparative example of the present invention
2with copper-Yin codope TiO prepared by embodiment 1
2xRD figure; Wherein a is TiO prepared by comparative example
2, b is copper-Yin codope TiO prepared by embodiment 1
2;
Fig. 2 is TiO prepared by comparative example of the present invention
2with copper-Yin codope TiO prepared by embodiment 4
2uv-visible absorption spectra figure; Wherein a is copper-Yin codope TiO prepared by embodiment 4
2uv-visible absorption spectra, b is TiO prepared by comparative example
2uv-visible absorption spectra;
Fig. 3 is copper-Yin codope TiO prepared by the embodiment of the present invention 3
2sEM figure;
Fig. 4 is TiO prepared by comparative example of the present invention
2with copper-Yin codope TiO prepared by embodiment 2
2to the photocatalytic degradation curve of methyl orange under sunshine; Wherein a is copper-Yin codope TiO prepared by embodiment 2
2the curve of degraded methyl orange, b is TiO prepared by comparative example
2the curve of degraded methyl orange.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail.
A kind of copper-Yin codope TiO provided by the invention
2catalysis material, its Ti:Cu:Ag mol ratio is 1:(0.02 ~ 0.07): (0.01 ~ 0.04).
A kind of copper-Yin codope TiO provided by the invention
2the preparation method of catalysis material, comprises the following steps:
Step 1), by analytically pure absolute ethyl alcohol, Butyl Phthalate, glacial acetic acid in molar ratio (10 ~ 20): 1:(1 ~ 5) ratio uniform mixing, obtain solution A;
Step 2), be (1 ~ 2) in molar ratio by analytically pure absolute ethyl alcohol, deionized water, Gerhardite crystal, silver nitrate: 1:(0.0018 ~ 0.0119); (0.00096 ~ 0.0068) Homogeneous phase mixing, employing concentration is that solution ph is adjusted to 3 ~ 5 by the aqueous solution of nitric acid of 2 ~ 4mol/L, obtains B solution;
Step 3), under rapid stirring, B solution is dropwise added in solution A, after stirring, forms precursor sol; In described solution A, in butyl titanate and B solution, the mol ratio of deionized water is 1:(5 ~ 10); By gained precursor sol ageing 24 ~ 48h formation gel in atmosphere, then use thermostatic drying chamber constant temperature drying at 80 ~ 100 DEG C, then the xerogel after drying is ground to form powder;
Step 4), by step 3) gained powder use Muffle furnace 400 ~ 600 DEG C calcining 1 ~ 3h, namely obtain copper-Yin codope TiO
2catalysis material, gained copper-Yin codope TiO
2catalysis material Ti:Cu:Ag mol ratio is 1:(0.02 ~ 0.07): (0.01 ~ 0.04).
It is pure that agents useful for same is analysis.
Embodiment 1
30ml absolute ethyl alcohol, 10ml butyl titanate, 4ml glacial acetic acid are uniformly mixed, obtain solution A.Be 1:0.05:0.01 by the mol ratio of Ti:Cu:Ag element, accurately take Gerhardite crystal and silver nitrate, and they are joined in the mixed solution of 10ml absolute ethyl alcohol and 3ml deionized water, be uniformly mixed, and adjust its pH value to be 3 ~ 5 with 2 ~ 4mol/L salpeter solution, obtain B solution.Under rapid stirring, slowly B solution is dropwise added in solution A, after stirring, form precursor sol.By precursor sol ageing 24 ~ 48h in atmosphere, form gel, be put in 80 DEG C of oven dry 20h in thermostatic drying chamber, obtain xerogel.Xerogel is pulverized, and with 400 DEG C of calcining 3h in Muffle furnace, copper-Yin codope TiO can be obtained
2catalysis material.
Photocatalysis is tested: experimental light sources is the sunshine between Xi'an on the 7th Weiyang District 12:00 ~ 15:00 May in 2014, and the same day, weather condition was: fine, 17 ~ 30 DEG C, northeaster gentle breeze.Copper-Yin codope TiO obtained in methyl orange solution and 0.1g embodiment 1 is added in 250mL glass beaker
2, the initial concentration of methyl orange is 10mg/L, and reaction solution volume is 100mL, and pH value is 3.First reaction solution lucifuge is stirred 30min in experiment, to reaching adsorption-desorption balance.Get supernatant liquor, after centrifugation, survey initial absorbance with 721 visible spectrophotometers.In light-catalyzed reaction process, make catalyst keep suspended state with magnetic stirring apparatus, every 30min timing sampling, after centrifugation, survey supernatant liquor absorbance.Determine the change of methyl orange in course of reaction according to the absorbance at methyl orange solution maximum wavelength place, and calculate degradation rate.
Embodiment 2
20ml absolute ethyl alcohol, 10ml butyl titanate, 2ml glacial acetic acid are uniformly mixed, obtain solution A.It is pure that agents useful for same is analysis.Be 1:0.06:0.01 by the mol ratio of Ti:Cu:Ag element, accurately take Gerhardite crystal and silver nitrate, and they are joined in the mixed solution of 10ml absolute ethyl alcohol and 3ml deionized water, be uniformly mixed, and adjust its pH value to be 3 ~ 5 with 2mol/L salpeter solution, obtain B solution.It is pure that agents useful for same is analysis.Under rapid stirring, slowly B solution is dropwise added in solution A, after stirring, form precursor sol.By precursor sol ageing 24 ~ 48h in atmosphere, form gel, be put in 100 DEG C of oven dry 12h in thermostatic drying chamber, obtain xerogel.Xerogel is pulverized, and with 500 DEG C of calcining 2h in Muffle furnace, copper-Yin codope TiO can be obtained
2catalysis material.
According to the photocatalysis experiment in embodiment 1, take the sample obtained in 0.1g embodiment 2 and carry out photocatalysis experiment.
Embodiment 3
20ml absolute ethyl alcohol, 10ml butyl titanate, 3ml glacial acetic acid are uniformly mixed, obtain solution A.It is pure that agents useful for same is analysis.Be 1:0.05:0.015 by the mol ratio of Ti:Cu:Ag element, accurately take Gerhardite crystal and silver nitrate, and they are joined in the mixed solution of 10ml absolute ethyl alcohol and 3ml deionized water, be uniformly mixed, and adjust its pH value to be 3 ~ 5 with 2mol/L salpeter solution, obtain B solution.It is pure that agents useful for same is analysis.Under rapid stirring, slowly B solution is dropwise added in solution A, after stirring, form precursor sol.By precursor sol ageing 24 ~ 48h in atmosphere, form gel, be put in 90 DEG C of oven dry 18h in thermostatic drying chamber, obtain xerogel.Xerogel is pulverized, and with 600 DEG C of calcining 1h in Muffle furnace, copper-Yin codope TiO can be obtained
2catalysis material.
According to the photocatalysis experiment in embodiment 1, take the sample obtained in 0.1g embodiment 3 and carry out photocatalysis experiment.
Embodiment 4
20ml absolute ethyl alcohol, 10ml butyl titanate, 3ml glacial acetic acid are uniformly mixed, obtain solution A.It is pure that agents useful for same is analysis.Be 1:0.04:0.01 by the mol ratio of Ti:Cu:Ag element, accurately take Gerhardite crystal and silver nitrate, and they are joined in the mixed solution of 10ml absolute ethyl alcohol and 3ml deionized water, be uniformly mixed, and adjust its pH value to be 3 ~ 5 with 2mol/L salpeter solution, obtain B solution.It is pure that agents useful for same is analysis.Under rapid stirring, slowly B solution is dropwise added in solution A, after stirring, form precursor sol.By precursor sol ageing 24 ~ 48h in atmosphere, form gel, be put in 95 DEG C of oven dry 18h in thermostatic drying chamber, obtain xerogel.Xerogel is pulverized, and with 500 DEG C of calcining 2h in Muffle furnace, copper-Yin codope TiO can be obtained
2catalysis material.
According to the photocatalysis experiment in embodiment 1, take the sample obtained in 0.1g embodiment 4 and carry out photocatalysis experiment.
Embodiment 5
30ml absolute ethyl alcohol, 10ml butyl titanate, 5ml glacial acetic acid are uniformly mixed, obtain solution A.It is pure that agents useful for same is analysis.Be 1:0.03:0.02 by the mol ratio of Ti:Cu:Ag element, accurately take Gerhardite crystal and silver nitrate, and they are joined in the mixed solution of 10ml absolute ethyl alcohol and 5ml deionized water, be uniformly mixed, and adjust its pH value to be 3 ~ 5 with 3mol/L salpeter solution, obtain B solution.It is pure that agents useful for same is analysis.Under rapid stirring, slowly B solution is dropwise added in solution A, after stirring, form precursor sol.By precursor sol ageing 24 ~ 48h in atmosphere, form gel, be put in 85 DEG C of oven dry 18h in thermostatic drying chamber, obtain xerogel.Xerogel is pulverized, and with 500 DEG C of calcining 3h in Muffle furnace, copper-Yin codope TiO can be obtained
2catalysis material.
According to the photocatalysis experiment in embodiment 1, take the sample obtained in 0.1g embodiment 5 and carry out photocatalysis experiment.
Embodiment 6
20ml absolute ethyl alcohol, 10ml butyl titanate, 3ml glacial acetic acid are uniformly mixed, obtain solution A.It is pure that agents useful for same is analysis.Be 1:0.06:0.015 by the mol ratio of Ti:Cu:Ag element, accurately take Gerhardite crystal and silver nitrate, and they are joined in the mixed solution of 15ml absolute ethyl alcohol and 3ml deionized water, be uniformly mixed, and adjust its pH value to be 3 ~ 5 with 2mol/L salpeter solution, obtain B solution.It is pure that agents useful for same is analysis.Under rapid stirring, slowly B solution is dropwise added in solution A, after stirring, form precursor sol.By precursor sol ageing 24 ~ 48h in atmosphere, form gel, be put in 80 DEG C of oven dry 20h in thermostatic drying chamber, obtain xerogel.Xerogel is pulverized, and with 600 DEG C of calcining 2h in Muffle furnace, copper-Yin codope TiO can be obtained
2catalysis material.
According to the photocatalysis experiment in embodiment 1, take the sample obtained in 0.1g embodiment 6 and carry out photocatalysis experiment.
Comparative example
According to embodiment 2, but do not add Gerhardite crystal and silver nitrate in B solution, obtained plain TiO
2.
According to the photocatalysis experiment in embodiment 1, take the sample obtained in 0.1g comparative example and carry out photocatalysis experiment.
Fig. 1 is TiO prepared by comparative example
2with copper-Yin codope TiO prepared by embodiment 1
2xRD figure.As seen from Figure 1, near 25.4 °, 37.8 °, 48.1 ° etc., curve a (TiO prepared by comparative example
2) and b (copper-Yin codope TiO prepared by embodiment 1
2) have obvious diffraction maximum to occur, copper-Yin codope TiO prepared by the present invention is described
2the TiO prepared with comparative example
2all mainly anatase crystal.
Fig. 2 is TiO prepared by comparative example
2with copper-Yin codope TiO prepared by embodiment 4
2uv-visible absorption spectra figure.As seen from Figure 2, the copper-Yin codope TiO for preparing of the present invention
2a () is obviously better than TiO prepared by ratio in the absorption of visible region
2(b), the TiO that ABSORPTION EDGE is prepared relative to comparative example
2also have obvious red shift, this will be conducive to the carrying out of light-catalyzed reaction under sunshine.
Fig. 4 is TiO prepared by comparative example
2with copper-Yin codope TiO prepared by embodiment 2
2to the photocatalytic degradation curve of methyl orange under sunshine.As can be seen from Figure 4, the copper-Yin codope TiO for preparing of the present invention
2a () reaches more than 90% to the degradation rate of methyl orange under sunshine, the TiO that degradation rate is prepared apparently higher than comparative example
2(b).
Claims (9)
1. a copper-Yin codope TiO
2catalysis material, is characterized in that, described copper-Yin codope TiO
2the Ti:Cu:Ag mol ratio of catalysis material is 1:(0.02 ~ 0.07): (0.01 ~ 0.04).
2. a copper-Yin codope TiO
2the preparation method of catalysis material, is characterized in that, comprises the following steps:
Step 1), by analytically pure absolute ethyl alcohol, Butyl Phthalate, glacial acetic acid Homogeneous phase mixing, obtain solution A;
Step 2), by analytically pure absolute ethyl alcohol, deionized water, copper nitrate crystal, silver nitrate Homogeneous phase mixing, and solution ph is adjusted to 3 ~ 5, obtains B solution;
Step 3), under rapid stirring, be 1:(0.02 ~ 0.07 by Ti:Cu:Ag mol ratio): (0.01 ~ 0.04), B solution is dropwise added in solution A, precursor sol is formed after stirring, form gel by after the ageing of gained precursor sol, then constant temperature drying, then the xerogel after drying is ground to form powder;
Step 4), by step 3) gained powder use Muffle furnace 400 ~ 600 DEG C calcining 1 ~ 3h, namely obtain copper-Yin codope TiO
2catalysis material.
3. a kind of copper-Yin codope TiO according to claim 2
2the preparation method of catalysis material, is characterized in that, step 1) described absolute ethyl alcohol, Butyl Phthalate, glacial acetic acid in molar ratio (10 ~ 20): 1:(1 ~ 5) ratio uniform mixing.
4. a kind of copper-Yin codope TiO according to Claims 2 or 3
2the preparation method of catalysis material, it is characterized in that, step 2) described absolute ethyl alcohol, deionized water, copper nitrate crystal, silver nitrate is in molar ratio for (1 ~ 2): 1:(0.0018 ~ 0.0119): the ratio of (0.00096 ~ 0.0068) mixes.
5. a kind of copper-Yin codope TiO according to claim 4
2the preparation method of catalysis material, is characterized in that, step 3) described A, B solution mixing, in solution A, in butyl titanate and B solution, the mol ratio of deionized water is 1:(5 ~ 10).
6. a kind of copper-Yin codope TiO according to claim 2
2the preparation method of catalysis material, is characterized in that, step 2) described adjustment solution ph adopts concentration to be the aqueous solution of nitric acid of 2 ~ 4mol/L.
7. a kind of copper-Yin codope TiO according to claim 2 or 6
2the preparation method of catalysis material, is characterized in that, step 2) described copper nitrate crystal employing Gerhardite crystal.
8. a kind of copper-Yin codope TiO according to claim 2
2the preparation method of catalysis material, is characterized in that, step 3) described ripening is ageing 24 ~ 48h in atmosphere.
9. a kind of copper-Yin codope TiO according to claim 2 or 8
2the preparation method of catalysis material, is characterized in that, step 3) temperature of described constant temperature drying is 80 ~ 100 DEG C, the time is 12 ~ 20h, and described oven dry adopts thermostatic drying chamber.
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Cited By (5)
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| CN106111158A (en) * | 2016-06-22 | 2016-11-16 | 深圳市开天源自动化工程有限公司 | The method of improvement photocatalyst activity |
| CN106311235A (en) * | 2016-08-16 | 2017-01-11 | 曹健 | Preparation method of copper doped TiO2 photocatalyst |
| CN111054442A (en) * | 2019-12-19 | 2020-04-24 | 东北师范大学 | Preparation method of titanium dioxide-based nano composite photocatalyst for rapidly removing phenolic organic pollutants in water |
| CN112264042A (en) * | 2020-11-19 | 2021-01-26 | 中南大学 | High-activity modified titanium dioxide catalyst for formaldehyde degradation and preparation method and application thereof |
| CN112841223A (en) * | 2020-12-30 | 2021-05-28 | 黑龙江莱恩检测有限公司 | Preparation method of modified nano antibacterial material and product thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111158A (en) * | 2016-06-22 | 2016-11-16 | 深圳市开天源自动化工程有限公司 | The method of improvement photocatalyst activity |
| CN106111158B (en) * | 2016-06-22 | 2018-10-16 | 深圳市水务科技有限公司 | The method for improveing photocatalyst activity |
| CN106311235A (en) * | 2016-08-16 | 2017-01-11 | 曹健 | Preparation method of copper doped TiO2 photocatalyst |
| CN111054442A (en) * | 2019-12-19 | 2020-04-24 | 东北师范大学 | Preparation method of titanium dioxide-based nano composite photocatalyst for rapidly removing phenolic organic pollutants in water |
| CN111054442B (en) * | 2019-12-19 | 2022-06-07 | 东北师范大学 | Preparation method of titanium dioxide-based nano composite photocatalyst for rapidly removing phenolic organic pollutants in water |
| CN112264042A (en) * | 2020-11-19 | 2021-01-26 | 中南大学 | High-activity modified titanium dioxide catalyst for formaldehyde degradation and preparation method and application thereof |
| CN112264042B (en) * | 2020-11-19 | 2021-12-07 | 中南大学 | High-activity modified titanium dioxide catalyst for formaldehyde degradation and preparation method and application thereof |
| CN112841223A (en) * | 2020-12-30 | 2021-05-28 | 黑龙江莱恩检测有限公司 | Preparation method of modified nano antibacterial material and product thereof |
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