CN103212392A - 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 37
- 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 23
- 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000003756 stirring Methods 0.000 claims abstract description 25
- 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 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 32
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 21
- 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 8
- 229910052684 Cerium 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
- 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 15
- 230000000694 effects Effects 0.000 abstract description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 230000031700 light absorption Effects 0.000 abstract 1
- 238000007669 thermal treatment Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 48
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- 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
- 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 2
- 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
- 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
- 230000000505 pernicious effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 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
- 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
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000002035 prolonged effect Effects 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
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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, photo-catalysis function technical field of material.
Background technology
Along with the progress of human society, problem of environmental pollution is more and more serious, and removing of these pollutants needs to consume a large amount of energy, and this proposes stern challenge for the exhausted day by day energy.How problem of environmental pollution is effectively controlled and solved to the limited resources of reasonable use occurring in nature, becomes the hot issue of the present world and numerous domestic scholar's research.In recent years, the photocatalysis technology that receives much concern can be with solar energy as degrade pollutant in the environment of the energy, still, and pure TiO
2Photochemical catalyst natural daylight utilization rate is not high; TiO
2Be a kind of wide bandgap semiconductor, its Detitanium-ore-type TiO
2Energy gap be 3.2ev, (300～400nm) just can be absorbed and utilize, and mainly are that visible light accounts for 43% in the sunshine, and ultraviolet light only accounts for 5%, and this has greatly limited TiO to have only the short ultraviolet light of wavelength
2The range of application of photochemical catalyst; And rutile TiO
2Energy gap (3.0eV) than Detitanium-ore-type TiO
2Narrow, body mutually in rutile when increasing mutually, red shift also correspondingly takes place in the absorption band edge of spectrum, can control the ratio of rutile and anatase by the method for regulation and control heat treatment temperature, thereby make the absorption band edge of spectrum that correspondingly red shift take place.
We can take two methods to solve TiO
2The problem that the photocatalytic degradation rate is not high: the one, pass through doped metal ion.Doped metal ion can be given TiO
2Provide electricity to give acceptor, help the transfer of electronics, prolonged the disengaging time in electronics and hole, reduced the compound of electronics and hole, thereby improved TiO
2The photocatalytic degradation rate.The 2nd, titanium dichloride load is on the carrier at source diatomite abundant, cheap and stable in properties.Diatomite is the porosity surface adsorbent, it and TiO
2The preparation composite photo-catalyst can be realized catching of photohole better, suppresses right compound in electronics-hole; Simultaneously, diatomite has the good adsorption performance, not only can effectively remove the organic pollution in the water, reduces the photocatalysis treatment cost, also organic matter can be adsorbed to TiO
2Grain surface, the contact probability of increase catalyst and pollutant reaches the raising the disposal efficiency, increases the purpose of degradation rate.
Summary of the invention
The present invention is directed to present TiO
2The problem that catalysis material exists proposes a kind of sol-gel process and prepares TiO
2The method of/diatomite composite photocatalytic material, this TiO
2/ diatomite composite photocatalytic material not only passes through metal-doped TiO
2The method that loads on the diatomite of porous improves its photocatalytic degradation rate, and controls the ratio of rutile and anatase by the method for regulation and control heat treatment temperature, thereby improves its photocatalytic activity and realize absorption, utilization to visible light.
The present invention realizes by following technical proposal: a kind of sol-gel process prepares TiO
2The method of/diatomite composite photocatalytic material, following each step of process:
(1) volume ratio by butyl titanate, absolute ethyl alcohol and glacial acetic acid is 20～28:48～54:2～8, and butyl titanate is joined in the absolute ethyl alcohol, adds glacial acetic acid again, stirs 20～50min then and forms faint yellow transparent solution A;
(2) volume ratio by deionized water, nitric acid and absolute ethyl alcohol is 8～13:1～3.5:47～55, removes ionized water, nitric acid joins and makes transparent solution B in the absolute ethyl alcohol;
(3) diatomite is joined deionized water for stirring and become suspension, adding concentration then in suspension is the metal-nitrate solutions of 1～10mol/L, mixing and stirring, the mass concentration that makes metal ion is 0～5%, again to wherein adding the NaOH ethanolic solution that concentration is 1～5mol/L, until making metal ion change metal hydroxides into, form mixing suspension C;
(4) volume ratio by solution A, solution B and mixing suspension C is 78～82:58～64:105～114, the solution B of step (2) gained and the mix suspending C of step (3) gained are joined in the solution A of step (1) gained with the speed of 0.1～1.0ml/min successively, and follow and stir 0.5～1h, still aging again back forms gel;
(5) step (4) gained gel is carried out drying, drying is after Overheating Treatment promptly obtains TiO
2/ diatomite composite photocatalytic material.
Gained TiO
2/ diatomite composite photocatalytic material is to be cooled when the room temperature, can be ground into powder on demand; And can itself and indoor coating, brightening agent need be mixed by the user and be coated in the wall surface and pernicious gas such as the formaldehyde of removal is arranged, have the antimildew and antibacterial ability, also its pulverulent product can be used for administering organic water and pollute the field.
It is pure that butyl titanate, absolute ethyl alcohol and the glacial acetic acid of described step (1) is 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 by solid-to-liquid ratio (g/mL) is that 1～20:100 mixes and forms.
The metal-nitrate solutions of described step (3) is one or more the metal-nitrate solutions among Fe, Cr, La, Ce and the Al.
Described step (4) still aging is ageing 1～4h at room temperature.
The drying of described step (5) is at 50～100 ℃ of down dry 1～5h.
The heat treatment temperature of described step (5) is 500～700 ℃, insulation 1～6h.
It is simple, low-cost to the invention provides a kind of preparation, and has visible light activity, the photocatalytic degradation rate is high and absorbs band edge to the obvious TiO that is offset of visible-range
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 visible light activity, photocatalytic degradation rate height and ABSORPTION EDGE and obviously is offset to visible-range, has good visible light photocatalysis active.Made fine catalyst can need mix itself and indoor coating, brightening agent by the user and be coated in inner wall surface and pernicious gas such as the formaldehyde of removal is arranged, have the antimildew and antibacterial ability, its pulverulent product can be used for administering organic water and pollute the field.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
The specific embodiment
Below in conjunction with embodiment the present invention is described further.
Embodiment 1
(1) volume ratio by butyl titanate, absolute ethyl alcohol and glacial acetic acid is 25:50:5, will analyze pure butyl titanate and join in the pure absolute ethyl alcohol of analysis, adds and analyzes pure glacial acetic acid, stirs 30min then and forms faint yellow transparent solution A;
(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 and makes transparent solution B in the absolute ethyl alcohol;
(3) diatomite and deionized water are stirred into suspension by solid-to-liquid ratio (g/mL) for 8:100, adding 1mL concentration then in suspension is the iron nitrate solution of 3mol/L, mixing and stirring, the mass concentration that makes metal ion is 1%, again to wherein adding the NaOH ethanolic solution that concentration is 5mol/L, until making metal ion change metal hydroxides into, form mixing suspension C;
(4) volume ratio by solution A, solution B and mixing suspension C is 80:60:110, the solution B of step (2) gained and the mix suspending C of step (3) gained are joined in the solution A of step (1) gained with the speed of 0.5ml/min successively, and follow and stir 0.5h, form gel behind the at room temperature still aging again 2h;
(5) step (4) gained gel is carried out dry 1h under 100 ℃, through 600 ℃ of heat treatments and be incubated 4h, promptly obtain TiO after the drying
2/ diatomite composite photocatalytic material.Fe-doped Ti O
2The absorption band edge of/diatomite composite photocatalytic material obviously is offset to visible-range, and energy gap is 2.85eV, and absorption band is 423nm, shows good visible light activity.
Embodiment 2
(1) volume ratio by butyl titanate, absolute ethyl alcohol and glacial acetic acid is 20:48:2, will analyze pure butyl titanate and join in the pure absolute ethyl alcohol of analysis, adds and analyzes pure glacial acetic acid, stirs 20min then and forms faint yellow transparent solution A;
(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 and makes transparent solution B in the absolute ethyl alcohol;
(3) diatomite and deionized water are stirred into suspension by solid-to-liquid ratio (g/mL) for 1:100, adding concentration then in suspension is the lanthanum nitrate hexahydrate of 1mol/L, mixing and stirring, the mass concentration that makes metal ion is 0～5%, again to wherein adding the NaOH ethanolic solution that concentration is 3mol/L, until making metal ion change metal hydroxides into, form mixing suspension C;
(4) volume ratio by solution A, solution B and mixing suspension C is 78:58:105, the solution B of step (2) gained and the mix suspending C of step (3) gained are joined in the solution A of step (1) gained with the speed of 1.0ml/min successively, and follow and stir 0.8h, form gel behind the at room temperature still aging again 1h;
(5) step (4) gained gel is carried out dry 3h under 80 ℃, through 500 ℃ of heat treatments and be incubated 6h, promptly obtain TiO after the drying
2/ diatomite composite photocatalytic material.La-doped Ti O
2The absorption band edge of/diatomite composite photocatalytic material obviously is offset to visible-range, and energy gap is 3.03eV, and absorption band is 401nm, shows certain visible light activity.
Embodiment 3
(1) volume ratio by butyl titanate, absolute ethyl alcohol and glacial acetic acid is 28:54:8, will analyze pure butyl titanate and join in the pure absolute ethyl alcohol of analysis, adds and analyzes pure glacial acetic acid, stirs 50min then and forms faint yellow transparent solution A;
(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 and makes transparent solution B in the absolute ethyl alcohol;
(3) diatomite and deionized water are stirred into suspension by solid-to-liquid ratio (g/mL) for 12:100, adding concentration then in suspension is the metal aluminum nitrate solution of 6mol/L, mixing and stirring, the mass concentration that makes metal ion is 0～5%, again to wherein adding the NaOH ethanolic solution that concentration is 5mol/L, until making metal ion change metal hydroxides into, form mixing suspension C;
(4) volume ratio by solution A, solution B and mixing suspension C is 82:64:114, the solution B of step (2) gained and the mix suspending C of step (3) gained are joined in the solution A of step (1) gained with the speed of 0.5ml/min successively, and follow and stir 0.5h, form gel behind the at room temperature still aging again 3h;
(5) step (4) gained gel is carried out dry 5h under 50 ℃, through 650 ℃ of heat treatments and be incubated 4h, promptly obtain TiO after the drying
2/ diatomite composite photocatalytic material.Al-doped Ti O
2The absorption band edge of/diatomite composite photocatalytic material obviously is offset to visible-range, and energy gap is 3.06eV, and absorption band is 390nm, shows certain visible light activity.
Embodiment 4
(1) volume ratio by butyl titanate, absolute ethyl alcohol and glacial acetic acid is 23:52:7, will analyze pure butyl titanate and join in the pure absolute ethyl alcohol of analysis, adds and analyzes pure glacial acetic acid, stirs 30min then and forms faint yellow transparent solution A;
(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 and makes transparent solution B in the absolute ethyl alcohol;
(3) diatomite and deionized water are stirred into suspension by solid-to-liquid ratio (g/mL) for 15:100, adding 0.5ml concentration then in suspension is that 6mol/L aluminum nitrate and 0.5ml concentration are 3mol/L ferric nitrate mixed solution, mixing and stirring, the mass concentration that makes metal ion is 0～5%, again to wherein adding the NaOH ethanolic solution that concentration is 5mol/L, until making metal ion change metal hydroxides into, form mixing suspension C;
(4) volume ratio by solution A, solution B and mixing suspension C is 78:64:105, the solution B of step (2) gained and the mix suspending C of step (3) gained are joined in the solution A of step (1) gained with the speed of 0.5ml/min successively, and follow and stir 1h, form gel behind the at room temperature still aging again 2h;
(5) step (4) gained gel is carried out dry 2h under 60 ℃, through 700 ℃ of heat treatments and be incubated 2h, promptly obtain TiO after the drying
2/ diatomite composite photocatalytic material.Al and Fe codope TiO
2The absorption band edge of/diatomite composite photocatalytic material obviously is offset to visible-range, and energy gap is 2.72eV, and absorption band is 435nm, shows tangible visible light catalysis activity.
Embodiment 5
(1) volume ratio by butyl titanate, absolute ethyl alcohol and glacial acetic acid is 28:48:6, will analyze pure butyl titanate and join in the pure absolute ethyl alcohol of analysis, adds and analyzes pure glacial acetic acid, stirs 50min then and forms faint yellow transparent solution A;
(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 and makes transparent solution B in the absolute ethyl alcohol;
(3) diatomite and deionized water are stirred into suspension by solid-to-liquid ratio (g/mL) for 20:100, adding concentration then in suspension is chromic nitrate and the cerous nitrate solution of 10mol/L, mixing and stirring, the mass concentration that makes metal ion is 0～5%, again to wherein adding the NaOH ethanolic solution that concentration is 1mol/L, until making metal ion change metal hydroxides into, form mixing suspension C;
(4) volume ratio by solution A, solution B and mixing suspension C is 82:62:110, the solution B of step (2) gained and the mix suspending C of step (3) gained are joined in the solution A of step (1) gained with the speed of 0.1ml/min successively, and follow and stir 1h, form gel behind the at room temperature still aging again 4h;
(5) step (4) gained gel is carried out dry 3h under 100 ℃, through 700 ℃ of heat treatments and be incubated 1h, promptly obtain TiO after the drying
2/ diatomite composite photocatalytic material.Cr and Ce codope TiO
2The absorption band edge of/diatomite composite photocatalytic material obviously is offset to visible-range, and energy gap is 2.92eV, and absorption band is 405nm, shows tangible 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) volume ratio by butyl titanate, absolute ethyl alcohol and glacial acetic acid is 20～28:48～54:2～8, and butyl titanate is joined in the absolute ethyl alcohol, adds glacial acetic acid again, stirs 20～50min then and forms faint yellow transparent solution A;
(2) volume ratio by deionized water, nitric acid and absolute ethyl alcohol is 8～13:1～3.5:47～55, removes ionized water, nitric acid joins and makes transparent solution B in the absolute ethyl alcohol;
(3) diatomite is joined deionized water for stirring and become suspension, adding concentration then in suspension is the metal-nitrate solutions of 1～10mol/L, mixing and stirring, the mass concentration that makes metal ion is 0～5%, again to wherein adding the NaOH ethanolic solution that concentration is 1～5mol/L, until making metal ion change metal hydroxides into, form mixing suspension C;
(4) volume ratio by solution A, solution B and mixing suspension C is 78～82:58～64:105～114, the solution B of step (2) gained and the mix suspending C of step (3) gained are joined in the solution A of step (1) gained with the speed of 0.1～1.0ml/min successively, and follow and stir 0.5～1h, still aging again back forms gel;
(5) step (4) gained gel is carried out drying, drying is after Overheating Treatment promptly obtains TiO
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 butyl titanate, absolute ethyl alcohol and the glacial acetic acid of described step (1) is 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 by solid-to-liquid ratio is that 1～20:100 mixes and forms.
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 among Fe, Cr, La, Ce and the 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 ageing 1～4h at room temperature.
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 at 50～100 ℃ of down dry 1～5h.
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 ℃, insulation 1～6h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN105195129A (en) * | 2014-05-30 | 2015-12-30 | 东北大学 | Columbate-loaded diatomite ball visible-light-driven photocatalyst and preparation method thereof |
| CN105251493A (en) * | 2015-10-28 | 2016-01-20 | 昆明理工大学 | Preparing method for photocatalytic material |
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| CN110194606A (en) * | 2019-06-20 | 2019-09-03 | 中建西部建设新疆有限公司 | A kind of preparation method of Photocatalytic Regeneration micro mist, concrete material and preparation method |
| CN110665535A (en) * | 2019-11-05 | 2020-01-10 | 辽宁大学 | Diatomite loaded La/N co-doped TiO2Photocatalytic composite sphere and preparation method and application thereof |
| CN110665534A (en) * | 2019-11-05 | 2020-01-10 | 辽宁大学 | Ce/N codoped TiO2Preparation method and application of acid-leaching diatomite composite sphere |
| CN112371092A (en) * | 2020-10-23 | 2021-02-19 | 郭竹春 | Formaldehyde-removing and peculiar smell-removing active material and preparation method thereof |
| CN115869965A (en) * | 2021-09-26 | 2023-03-31 | 上海乔昔环境工程有限公司 | Visible light response type nano photocatalyst aqueous solution |
| CN115569646A (en) * | 2022-09-08 | 2023-01-06 | 杭州润涞科技服务有限公司 | Preparation method of rare earth compound capable of decomposing formaldehyde and other pollutant gases |
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