CN103212392B - Method for preparing TiO2/kieselguhr composite photocatalytic material by using sol-gel method - Google Patents
Method for preparing TiO2/kieselguhr composite photocatalytic material by using sol-gel method Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 41
- 239000000463 material Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000003980 solgel method Methods 0.000 title claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000725 suspension Substances 0.000 claims abstract description 35
- 238000003756 stirring Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 17
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 17
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 229910000000 metal hydroxide Inorganic materials 0.000 claims abstract description 8
- 150000004692 metal hydroxides Chemical class 0.000 claims abstract description 8
- 229910001960 metal nitrate Inorganic materials 0.000 claims abstract description 8
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 34
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 23
- 229960000583 acetic acid Drugs 0.000 claims description 16
- 239000012362 glacial acetic acid Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 229910052684 Cerium Inorganic materials 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- 238000011282 treatment Methods 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 238000013021 overheating Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 9
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 3
- 230000031700 light absorption Effects 0.000 abstract 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract 1
- 238000007669 thermal treatment Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 48
- 239000003054 catalyst Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 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
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 238000005282 brightening Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 2
- 230000000505 pernicious effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- JLDSOYXADOWAKB-UHFFFAOYSA-N aluminium nitrate Chemical compound [Al+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O JLDSOYXADOWAKB-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 description 1
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 1
- GJKFIJKSBFYMQK-UHFFFAOYSA-N lanthanum(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GJKFIJKSBFYMQK-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 1
Abstract
The invention provides a method for preparing a TiO2/kieselguhr composite photocatalytic material by using a sol-gel method, belonging to the technical field of environmental pollution improvement and photocatalytic functional material preparation. The method comprises the following steps of: adding butyl titanate into absolute ethyl alcohol, then adding absolute ethyl alcohol, and stirring to form a faint yellow transparent solution A; adding deionized water and nitric acid into absolute ethyl alcohol so as to prepare a transparent solution B; adding kieselguhr into deionized water, stirring so as to form a suspension liquid; adding a metal nitrate solution into the suspension and then adding a sodium hydroxide solution into the suspension till the metal ions are converted into metal hydroxides, thus forming a mixed suspension liquid C; sequentially adding the solution B and the mixed suspension liquid C into the solution A, standing still and aging to form gel; and drying and carrying out thermal treatment so as to obtain the TiO2/kieselguhr composite photocatalytic material. The method is simple, low in cost and free of secondary pollution, the prepared material has visible light activity and is high in photocatalytic degradation rate; and the absorption edge of the material is obviously deviated to a visible light absorption range.
Description
Technical field
The present invention relates to a kind of sol-gel process and prepare TiO
2the method of/diatomite composite photocatalytic material, belongs to environmental pollution improvement, Photocatalysis Function Material preparing technical field.
Background technology
Along with the progress of human society, problem of environmental pollution is more and more serious, and the removing of these pollutants needs to consume a large amount of energy, and this proposes stern challenge to the day by day exhausted energy.How reasonably to utilize the limited resources of occurring in nature, effectively control and solve problem of environmental pollution, become the hot issue of the world and numerous domestic scholar's research at present.In recent years, the photocatalysis technology received much concern can using solar energy as the energy to the pollutant of degrading in environment, but, pure TiO
2photochemical catalyst natural daylight utilization rate is not high; TiO
2a kind of wide bandgap semiconductor, its Detitanium-ore-type TiO
2energy gap be 3.2ev, the ultraviolet light (300 ~ 400nm) only having wavelength shorter just can be absorbed and utilize, and in sunshine, mainly visible ray accounts for 43%, and ultraviolet light only accounts for 5%, this greatly limits TiO
2the range of application of photochemical catalyst; And rutile TiO
2energy gap (3.0eV) than Detitanium-ore-type TiO
2narrow, body mutually in Rutile Type when increasing, also correspondingly there is red shift in the absorption band edge of spectrum, the method by regulating and controlling heat treatment temperature controls the ratio of rutile and anatase, thus makes the absorption band edge of spectrum that correspondingly red shift occur.
We can take two methods to solve TiO
2the problem that photocatalytic activity is not high: one is pass through doped metal ion.Doped metal ion can give TiO
2there is provided electricity to give acceptor, be conducive to the transfer of electronics, extend the disengaging time in electronics and hole, reduce the compound in electronics and hole, thus improve TiO
2photocatalytic activity.Two are titanium dichloride loads is on carrier at abundance, diatomite that is cheap and stable in properties.Diatomite is porosity surface adsorbent, it and TiO
2prepare composite photo-catalyst and can realize catching of photohole better, suppress the compound that electronics-hole is right; Meanwhile, diatomite has good absorption property, not only effectively can remove the organic pollution in water, reduces photocatalysis treatment cost, also can by Adsorption of Organic to TiO
2grain surface, increases the contact probability of catalyst and pollutant, reaches raising the disposal efficiency, increases the object of degradation rate.
Summary of the invention
The present invention is directed to current TiO
2catalysis material Problems existing, proposes a kind of sol-gel process and prepares TiO
2the method of/diatomite composite photocatalytic material, this TiO
2/ diatomite composite photocatalytic material is not by means of only by metal-doped TiO
2the method of load on the diatomite of porous improves its photocatalytic activity, and controls the ratio of rutile and anatase by the method regulating and controlling heat treatment temperature, thus improves its photocatalytic activity and the absorption realized visible ray, utilization.
The present invention is realized by following technical proposal: a kind of sol-gel process prepares TiO
2the method of/diatomite composite photocatalytic material, through following each step:
(1) be 20 ~ 28:48 ~ 54:2 ~ 8 by the volume ratio of butyl titanate, absolute ethyl alcohol and glacial acetic acid, butyl titanate joined in absolute ethyl alcohol, then adds glacial acetic acid, then stir the solution A that 20 ~ 50min forms pale yellow transparent;
(2) be 8 ~ 13:1 ~ 3.5:47 ~ 55 by the volume ratio of deionized water, nitric acid and absolute ethyl alcohol, remove ionized water, nitric acid joins solution B obtained transparent in absolute ethyl alcohol;
(3) diatomite is joined deionized water for stirring and become suspension, then in suspension, the metal-nitrate solutions that concentration is 1 ~ 10mol/L is added, mixing and stirring, the mass concentration of metal ion is made to be 0 ~ 5%, add the NaOH ethanolic solution that concentration is 1 ~ 5mol/L more wherein, until make metal ion change metal hydroxides into, form mixing suspension C;
(4) be 78 ~ 82:58 ~ 64:105 ~ 114 by the volume ratio of solution A, solution B and mixing suspension C, the mix suspending C of the solution B of step (2) gained and step (3) gained is joined with the speed of 0.1 ~ 1.0ml/min in the solution A of step (1) gained successively, and with stirring 0.5 ~ 1h, more still aging rear formation gel;
(5) step (4) gained gel is carried out drying, after drying, namely obtain TiO through Overheating Treatment
2/ diatomite composite photocatalytic material.
Gained TiO
2/ diatomite composite photocatalytic material to be cooled to room temperature time, can be ground into powder on demand; And can need itself and indoor coating by user, brightening agent mixing is coated in wall surface has pernicious gases such as removing formaldehyde, has antimildew and antibacterial ability, also its pulverulent product can be used for administering organic water and pollute field.
It is pure that the butyl titanate of described step (1), absolute ethyl alcohol and glacial acetic acid are commercial analysis.
It is pure that the nitric acid of described step (2) and absolute ethyl alcohol are commercial analysis.
The suspension of described step (3) is diatomite and deionized water is that 1 ~ 20:100 carries out being uniformly mixed forming by solid-to-liquid ratio (g/mL).
The metal-nitrate solutions of described step (3) is one or more the metal-nitrate solutions in Fe, Cr, La, Ce and Al.
Described step (4) still aging is at room temperature ageing 1 ~ 4h.
The drying of described step (5) is dry 1 ~ 5h at 50 ~ 100 DEG C.
The heat treatment temperature of described step (5) is 500 ~ 700 DEG C, insulation 1 ~ 6h.
The invention provides that one is prepared simply, low cost, and it is high and absorb the TiO that band edge obviously offsets to visible-range to have visible light activity, photocatalytic activity
2the preparation method of/diatomite composite photocatalytic material.This method preparation is simple, low cost, non-secondary pollution, TiO
2/ diatomite composite photocatalytic material has the high and ABSORPTION EDGE of visible light activity, photocatalytic activity and obviously offsets to visible-range, has excellent visible light photocatalysis active.Made fine catalyst can need itself and indoor coating by user, brightening agent mixing is coated in inner wall surface has pernicious gases such as removing formaldehyde, has antimildew and antibacterial ability, its pulverulent product can be used for administering organic water and pollute field.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
(1) be 25:50:5 by the volume ratio of butyl titanate, absolute ethyl alcohol and glacial acetic acid, pure for analysis butyl titanate joined and analyzes in pure absolute ethyl alcohol, then add and analyze pure glacial acetic acid, then stir the solution A that 30min forms pale yellow transparent;
(2) be 10:2:50 by deionized water, the volume ratio analyzing pure nitric acid and analyze pure absolute ethyl alcohol, remove ionized water, nitric acid joins solution B obtained transparent in absolute ethyl alcohol;
(3) by diatomite and deionized water by solid-to-liquid ratio (g/mL) for 8:100 carries out stirring into suspension, then in suspension, the iron nitrate solution that 1mL concentration is 3mol/L is added, mixing and stirring, the mass concentration of metal ion is made to be 1%, add the NaOH ethanolic solution that concentration is 5mol/L more wherein, until make metal ion change metal hydroxides into, form mixing suspension C;
(4) be 80:60:110 by the volume ratio of solution A, solution B and mixing suspension C, the mix suspending C of the solution B of step (2) gained and step (3) gained is joined with the speed of 0.5ml/min in the solution A of step (1) gained successively, and with stirring 0.5h, more at room temperature form gel after still aging 2h;
(5) step (4) gained gel is carried out dry 1h at 100 DEG C, be incubated 4h through 600 DEG C of heat treatments after drying, namely obtain TiO
2/ diatomite composite photocatalytic material.Fe-doped Ti O
2the absorption band edge of/diatomite composite photocatalytic material obviously offsets to visible-range, and energy gap is 2.85eV, and absorption band is 423nm, shows good visible light activity.
Embodiment 2
(1) be 20:48:2 by the volume ratio of butyl titanate, absolute ethyl alcohol and glacial acetic acid, pure for analysis butyl titanate joined and analyzes in pure absolute ethyl alcohol, then add and analyze pure glacial acetic acid, then stir the solution A that 20min forms pale yellow transparent;
(2) be 13:3.5:47 by deionized water, the volume ratio analyzing pure nitric acid and analyze pure absolute ethyl alcohol, remove ionized water, nitric acid joins solution B obtained transparent in absolute ethyl alcohol;
(3) by diatomite and deionized water by solid-to-liquid ratio (g/mL) for 1:100 carries out stirring into suspension, then in suspension, the lanthanum nitrate hexahydrate that concentration is 1mol/L is added, mixing and stirring, the mass concentration of metal ion is made to be 0 ~ 5%, add the NaOH ethanolic solution that concentration is 3mol/L more wherein, until make metal ion change metal hydroxides into, form mixing suspension C;
(4) be 78:58:105 by the volume ratio of solution A, solution B and mixing suspension C, the mix suspending C of the solution B of step (2) gained and step (3) gained is joined with the speed of 1.0ml/min in the solution A of step (1) gained successively, and with stirring 0.8h, more at room temperature form gel after still aging 1h;
(5) step (4) gained gel is carried out dry 3h at 80 DEG C, be incubated 6h through 500 DEG C of heat treatments after drying, namely obtain TiO
2/ diatomite composite photocatalytic material.La-doped Ti O
2the absorption band edge of/diatomite composite photocatalytic material obviously offsets to visible-range, and energy gap is 3.03eV, and absorption band is 401nm, shows certain visible light activity.
Embodiment 3
(1) be 28:54:8 by the volume ratio of butyl titanate, absolute ethyl alcohol and glacial acetic acid, pure for analysis butyl titanate joined and analyzes in pure absolute ethyl alcohol, then add and analyze pure glacial acetic acid, then stir the solution A that 50min forms pale yellow transparent;
(2) be 8:1:55 by deionized water, the volume ratio analyzing pure nitric acid and analyze pure absolute ethyl alcohol, remove ionized water, nitric acid joins solution B obtained transparent in absolute ethyl alcohol;
(3) by diatomite and deionized water by solid-to-liquid ratio (g/mL) for 12:100 carries out stirring into suspension, then in suspension, add the metal nitrate aluminum solutions that concentration is 6mol/L, mixing and stirring, the mass concentration of metal ion is made to be 0 ~ 5%, add the NaOH ethanolic solution that concentration is 5mol/L more wherein, until make metal ion change metal hydroxides into, form mixing suspension C;
(4) be 82:64:114 by the volume ratio of solution A, solution B and mixing suspension C, the mix suspending C of the solution B of step (2) gained and step (3) gained is joined with the speed of 0.5ml/min in the solution A of step (1) gained successively, and with stirring 0.5h, more at room temperature form gel after still aging 3h;
(5) step (4) gained gel is carried out dry 5h at 50 DEG C, be incubated 4h through 650 DEG C of heat treatments after drying, namely obtain TiO
2/ diatomite composite photocatalytic material.Al-doped Ti O
2the absorption band edge of/diatomite composite photocatalytic material obviously offsets to visible-range, and energy gap is 3.06eV, and absorption band is 390nm, shows certain visible light activity.
Embodiment 4
(1) be 23:52:7 by the volume ratio of butyl titanate, absolute ethyl alcohol and glacial acetic acid, pure for analysis butyl titanate joined and analyzes in pure absolute ethyl alcohol, then add and analyze pure glacial acetic acid, then stir the solution A that 30min forms pale yellow transparent;
(2) be 9:3.5:55 by deionized water, the volume ratio analyzing pure nitric acid and analyze pure absolute ethyl alcohol, remove ionized water, nitric acid joins solution B obtained transparent in absolute ethyl alcohol;
(3) by diatomite and deionized water by solid-to-liquid ratio (g/mL) for 15:100 carries out stirring into suspension, then in suspension, add 0.5ml concentration be 6mol/L aluminum nitrate and 0.5ml concentration is 3mol/L ferric nitrate mixed solution, mixing and stirring, the mass concentration of metal ion is made to be 0 ~ 5%, add the NaOH ethanolic solution that concentration is 5mol/L more wherein, until make metal ion change metal hydroxides into, form mixing suspension C;
(4) be 78:64:105 by the volume ratio of solution A, solution B and mixing suspension C, the mix suspending C of the solution B of step (2) gained and step (3) gained is joined with the speed of 0.5ml/min in the solution A of step (1) gained successively, and with stirring 1h, more at room temperature form gel after still aging 2h;
(5) step (4) gained gel is carried out dry 2h at 60 DEG C, be incubated 2h through 700 DEG C of heat treatments after drying, namely obtain TiO
2/ diatomite composite photocatalytic material.Al and Fe codope TiO
2the absorption band edge of/diatomite composite photocatalytic material obviously offsets to visible-range, and energy gap is 2.72eV, and absorption band is 435nm, shows obvious visible light catalysis activity.
Embodiment 5
(1) be 28:48:6 by the volume ratio of butyl titanate, absolute ethyl alcohol and glacial acetic acid, pure for analysis butyl titanate joined and analyzes in pure absolute ethyl alcohol, then add and analyze pure glacial acetic acid, then stir the solution A that 50min forms pale yellow transparent;
(2) be 8:1:49 by deionized water, the volume ratio analyzing pure nitric acid and analyze pure absolute ethyl alcohol, remove ionized water, nitric acid joins solution B obtained transparent in absolute ethyl alcohol;
(3) by diatomite and deionized water by solid-to-liquid ratio (g/mL) for 20:100 carries out stirring into suspension, then in suspension, the chromic nitrate that concentration is 10mol/L and cerous nitrate solution is added, mixing and stirring, the mass concentration of metal ion is made to be 0 ~ 5%, add the NaOH ethanolic solution that concentration is 1mol/L more wherein, until make metal ion change metal hydroxides into, form mixing suspension C;
(4) be 82:62:110 by the volume ratio of solution A, solution B and mixing suspension C, the mix suspending C of the solution B of step (2) gained and step (3) gained is joined with the speed of 0.1ml/min in the solution A of step (1) gained successively, and with stirring 1h, more at room temperature form gel after still aging 4h;
(5) step (4) gained gel is carried out dry 3h at 100 DEG C, be incubated 1h through 700 DEG C of heat treatments after drying, namely obtain TiO
2/ diatomite composite photocatalytic material.Cr and Ce codope TiO
2the absorption band edge of/diatomite composite photocatalytic material obviously offsets to visible-range, and energy gap is 2.92eV, and absorption band is 405nm, shows obvious visible light catalysis activity.
Claims (8)
1. a sol-gel process prepares TiO
2the method of/diatomite composite photocatalytic material, is characterized in that through following each step:
(1) be 20 ~ 28:48 ~ 54:2 ~ 8 by the volume ratio of butyl titanate, absolute ethyl alcohol and glacial acetic acid, butyl titanate joined in absolute ethyl alcohol, then adds glacial acetic acid, then stir the solution A that 20 ~ 50min forms pale yellow transparent;
(2) be 8 ~ 13:1 ~ 3.5:47 ~ 55 by the volume ratio of deionized water, nitric acid and absolute ethyl alcohol, remove ionized water, nitric acid joins solution B obtained transparent in absolute ethyl alcohol;
(3) diatomite is joined deionized water for stirring and become suspension, then in suspension, the metal-nitrate solutions that concentration is 1 ~ 10mol/L is added, mixing and stirring, the mass concentration of metal ion is made to be 0 ~ 5%, add the NaOH ethanolic solution that concentration is 1 ~ 5mol/L more wherein, until make metal ion change metal hydroxides into, form mixing suspension C;
(4) be 78 ~ 82:58 ~ 64:105 ~ 114 by the volume ratio of solution A, solution B and mixing suspension C, the mix suspending C of the solution B of step (2) gained and step (3) gained is joined with the speed of 0.1 ~ 1.0ml/min in the solution A of step (1) gained successively, and with stirring 0.5 ~ 1h, more still aging rear formation gel;
(5) step (4) gained gel is carried out drying, after drying, namely obtain TiO through Overheating Treatment
2/ diatomite composite photocatalytic material.
2. sol-gel process according to claim 1 prepares TiO
2the method of/diatomite composite photocatalytic material, is characterized in that: it is pure that the butyl titanate of described step (1), absolute ethyl alcohol and glacial acetic acid are commercial analysis.
3. sol-gel process according to claim 1 prepares TiO
2the method of/diatomite composite photocatalytic material, is characterized in that: it is pure that the nitric acid of described step (2) and absolute ethyl alcohol are commercial analysis.
4. sol-gel process according to claim 1 prepares TiO
2the method of/diatomite composite photocatalytic material, is characterized in that: the suspension of described step (3) is diatomite and deionized water is that 1 ~ 20:100 carries out being uniformly mixed forming by solid-to-liquid ratio.
5. sol-gel process according to claim 1 prepares TiO
2the method of/diatomite composite photocatalytic material, is characterized in that: the metal-nitrate solutions of described step (3) is one or more the metal-nitrate solutions in Fe, Cr, La, Ce and Al.
6. sol-gel process according to claim 1 prepares TiO
2the method of/diatomite composite photocatalytic material, is characterized in that: described step (4) still aging is at room temperature ageing 1 ~ 4h.
7. sol-gel process according to claim 1 prepares TiO
2the method of/diatomite composite photocatalytic material, is characterized in that: the drying of described step (5) is dry 1 ~ 5h at 50 ~ 100 DEG C.
8. sol-gel process according to claim 1 prepares TiO
2the method of/diatomite composite photocatalytic material, is characterized in that: the heat treatment temperature of described step (5) is 500 ~ 700 DEG C, insulation 1 ~ 6h.
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| CN105080528A (en) * | 2014-05-08 | 2015-11-25 | 东北大学 | Preparation method of TiO2 photocatalyst by loading TiO2 to diatomite formed in advance and doping rare earth |
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| JP6552090B2 (en) * | 2015-05-08 | 2019-07-31 | 国立研究開発法人物質・材料研究機構 | Photocatalyst composite material and method for producing the same |
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| CN101628236A (en) * | 2009-08-03 | 2010-01-20 | 浙江理工大学 | Preparation method of kieselguhr load type compound photocatalyst with iron ions doped titanium dioxide |
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