CN106238028A - TiO2/ Al rice husk load light complex catalyst and preparation method thereof - Google Patents
TiO2/ Al rice husk load light complex catalyst and preparation method thereof Download PDFInfo
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- CN106238028A CN106238028A CN201610596415.9A CN201610596415A CN106238028A CN 106238028 A CN106238028 A CN 106238028A CN 201610596415 A CN201610596415 A CN 201610596415A CN 106238028 A CN106238028 A CN 106238028A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 44
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 235000007164 Oryza sativa Nutrition 0.000 title claims abstract description 41
- 235000009566 rice Nutrition 0.000 title claims abstract description 41
- 239000010903 husk Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 240000007594 Oryza sativa Species 0.000 title 1
- 241000209094 Oryza Species 0.000 claims abstract description 40
- 238000001354 calcination Methods 0.000 claims abstract description 40
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 12
- 238000000703 high-speed centrifugation Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 9
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 229910010298 TiOSO4 Inorganic materials 0.000 claims abstract description 6
- 229910000329 aluminium sulfate Inorganic materials 0.000 claims abstract description 6
- 239000011521 glass Substances 0.000 claims abstract description 6
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 6
- 239000011941 photocatalyst Substances 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 5
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 5
- 239000012535 impurity Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract description 5
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 abstract description 3
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract 2
- 238000003801 milling Methods 0.000 abstract 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 7
- 229940012189 methyl orange Drugs 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000000523 sample Substances 0.000 description 6
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000010453 quartz Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- KADRTWZQWGIUGO-UHFFFAOYSA-L oxotitanium(2+);sulfate Chemical compound [Ti+2]=O.[O-]S([O-])(=O)=O KADRTWZQWGIUGO-UHFFFAOYSA-L 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 3
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000006552 photochemical reaction Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910010062 TiCl3 Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 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
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- LQJVOKWHGUAUHK-UHFFFAOYSA-L disodium 5-amino-4-hydroxy-3-phenyldiazenylnaphthalene-2,7-disulfonate Chemical compound [Na+].[Na+].OC1=C2C(N)=CC(S([O-])(=O)=O)=CC2=CC(S([O-])(=O)=O)=C1N=NC1=CC=CC=C1 LQJVOKWHGUAUHK-UHFFFAOYSA-L 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of TiO2/ Al rice husk load light complex catalyst, it is characterised in that: with rice husk as carrier, it is loaded with TiO2/ Al and the composite photo-catalyst that formed, wherein the mol ratio of Ti, Al and Si element is 1: 1: 1.The preparation method of this catalyst: take rice husk and be soaked in 1mol/L HCl, after making metal ion remove completely, pulverizes after washing, be dried, cooling down, grinds in glass pot；Respectively by TiOSO4And Na2C2O4Presoma is made with some PEG400 mixed grindings again after respectively grinding by the mol ratio of 1: 1；By anhydrous Al2(SO4)3Mix after milling with described presoma, addition powdered rice hulls remixes to mill makes composite precursor；Putting in Muffle furnace after described composite precursor is dried, is cooled down and calcine, calcining heat is 300 500 DEG C, and calcination time is 1 2h；Wash through high speed centrifugation washing, alcohol again, grind into powder after gained solid matter drying, cooling be can be prepared by.The catalyst photocatalytic activity prepared is higher, has preferable application prospect.
Description
Technical field
The invention belongs to photocatalyst technology field, be specifically related to a kind of TiO2/ Al rice husk load light complex catalyst
And preparation method thereof.
Background technology
This novel photocatalysis material of titanium dioxide have nontoxic, rapidly and efficiently, cheap, stable performance, clean
Only, the advantage such as energy consumption is low and easy and simple to handle, in recent ten years, along with development and people's awakening to environmental conservation of society, two
The research of titanium oxide photochemical catalyst material causes the extensive concern of the field scientists such as domestic and international physics, chemistry, material and environment,
By scientist the aspects such as the structure of matter of titanium dioxide, preparation method, catalytic performance, catalytic mechanism are goed deep into system
Research so that it is processing waste water, purifying air, health care, construction material, textile, luminous energy conversion, many necks such as military
Territory is obtained for and is widely applied, and has good development prospect.
At home, someone utilizes infusion process to be prepared for Cr, 6 kinds of doped transition metal ionses of Mn, Fe, Co, Ni, Cu respectively
Modified TiO2Nanoparticle, with acetic acid and CO2Photo catalytic reduction be that its performance is studied by probe reaction；Abroad, there is people
With sol-gel method at TiCl3, and Ti (OC4H9)4Hydrolytic process introduces boric acid and cerous nitrate is prepared for B and Ce codope
B1.6Ce0.5-TiO2, evaluate catalyst activity under ultraviolet light with visible ray with the decolorization experiment of Acid Red B.
Summary of the invention
Present invention aims to the problems referred to above of the prior art, utilize rice husk and TiO2Collaborative complex effect,
Doping Al3+Prepare the rice husk load TiO that a kind of good stability, photocatalytic activity are high2/ Al photocatalyst and preparation method thereof.
For achieving the above object, present invention employs following technical scheme:
A kind of TiO2/ Al rice husk load light complex catalyst, with rice husk as carrier, is loaded with TiO2/ Al and answering of being formed
Closing photocatalyst, wherein the mol ratio of Ti, Al and Si element is 1: 1: 1.
One TiO according to claim 12The preparation method of/Al rice husk load light complex catalyst, the method bag
Include following steps:
1) take rice husk to be soaked in 1mol/L HCl, after making metal ion remove completely, be washed to neutrality, be then dried,
Pulverize after being cooled to room temperature, stand-by after grinding 15min in glass pot；
2) respectively by TiOSO4And Na2C2O4Mol ratio by 1: 1 is mixed with some PEG400s after respectively grinding 15min
Close grinding 50min and make presoma；
3) by anhydrous Al2(SO4)3Mix with described presoma after the 30min that mills, add powdered rice hulls and remix the 50min that mills
Making composite precursor, in presoma, the mol ratio of Ti, Al and Si element is 1: 1: 1；
4) described composite precursor is cooled to room temperature after drying, is then placed in Muffle furnace calcining, calcining heat
For 300-500 DEG C, calcination time is 1-2h；
5) the complex catalyst that after calcining, gained contains impurity is washed, by gained solids through high speed centrifugation washing, alcohol
Matter drying, be cooled to room temperature after can be prepared by described TiO with Achates grind into powder2The load light complex catalysis of/Al rice husk
Agent.
Above-mentioned TiO2The preparation method of/Al rice husk load light complex catalyst, step 5) described high speed centrifugation washing 4-6
Secondary, alcohol is washed 2-4 time, and condition is centrifugal speed 8000r/min, centrifugation time 5-10min.
Compared to prior art, present invention have an advantage that
The present invention provides a kind of TiO2/ Al rice husk load light complex catalyst, and establish corresponding preparation method.Adopt
It is carrier with natural rice husk, utilizes solid phase method to prepare Al doping TiO2/ rice husk optic catalytic composite material, powdered rice hulls has uniformly
Pore passage structure, can be that reaction provides place, have good absorption property simultaneously, compensate for single use TiO2Deficiency；Al3+
The smooth surface being entrained in quasiconductor introduces defective locations or changes the degree of crystallinity of quasiconductor, have impact on electronics and hole
It is combined or makes TiO2Excitation wavelength change, thus improve TiO2Catalytic efficiency；Use the present invention prepared by solid phase precursor process
Catalyst, technique is simple, and easy and simple to handle, photocatalysis effect is good, and the catalyst prepared has higher photocatalytic activity, tool
There is preferable application prospect.
Accompanying drawing explanation
Fig. 1 is that the preparation method of the present invention is in fall to methyl orange of the different calcination time catalyst of calcining heat 300 DEG C
Solution curve.
Fig. 2 is that the preparation method of the present invention is in fall to methyl orange of the different calcination time catalyst of calcining heat 400 DEG C
Solution curve.
Fig. 3 is that the preparation method of the present invention is in fall to methyl orange of the different calcination time catalyst of calcining heat 500 DEG C
Solution curve.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing thereof, technical solution of the present invention is further non-limitingly described in detail.
One, TiO2/ Al rice husk load light complex catalyst, it is characterised in that: with rice husk as carrier, it is loaded with TiO2/Al
And the composite photo-catalyst formed, wherein the mol ratio of Ti, Al and Si element is 1: 1: 1.
Two, TiO2The preparation of/Al rice husk load light complex catalyst
Preparation method comprises the steps:
Embodiment 1
1) take a certain amount of rice husk and be soaked in 12h in 1mol/L HCl, after making metal ion remove completely, be washed to neutrality,
It is placed in 80 DEG C of baking ovens and is dried, then be cooled to room temperature in being put in exsiccator, after pulverizer is pulverized, carry out in glass pot
After grinding 15min, load in sample sack stand-by；
2) respectively by a certain amount of titanyl sulfate (TiOSO4) and Disodium oxalate. (Na2C2O4) respectively grind by the mol ratio of 1: 1
Presoma is made with some PEG400 mixed grinding 50min after 15min；
3) by 5.2g anhydrous slufuric acid aluminum (Al2(SO4)3) mix after the 30min that mills with 2.5g presoma, add 6.8g rice husk
Powder remixes the 50min that mills and makes composite precursor, and in presoma, the mol ratio of Ti, Al and Si element is 1: 1: 1；
4) by composite precursor in 80 DEG C of baking ovens dried, be cooled to room temperature in being put in exsiccator, be then placed in crucible
Calcining in Muffle furnace, calcining heat is 300 DEG C, and calcination time is 2h；
5) the complex catalyst that after calcining, gained contains impurity is washed 4 times through high speed centrifugation, and alcohol washes 2 times, and condition is
Centrifugal speed 8000r/min, centrifugation time 10min, centrifugal rear gained solid matter is placed in 80 DEG C of drying in oven, places into
Exsiccator is cooled to room temperature, with the TiO prepared under the i.e. available different calcination conditions of Achates grind into powder2/ Al rice husk is born
Carry light complex catalyst.
Embodiment 2
1) take a certain amount of rice husk and be soaked in 12h in 1mol/L HCl, after making metal ion remove completely, be washed to neutrality,
It is placed in 80 DEG C of baking ovens and is dried, then be cooled to room temperature in being put in exsiccator, after pulverizer is pulverized, carry out in glass pot
After grinding 15min, load in sample sack stand-by；
2) respectively by a certain amount of titanyl sulfate (TiOSO4) and Disodium oxalate. (Na2C2O4) respectively grind by the mol ratio of 1: 1
After 15min, 7 glycol 400 mixed grinding 50mins poly-with some make presoma；
3) by 10.4g anhydrous slufuric acid aluminum (Al2(SO4)3) mix after the 30min that mills with 5g presoma, add 6.8g powdered rice hulls
Remixing the 50min that mills and make composite precursor, in presoma, the mol ratio of Ti, Al and Si element is 1: 1: 1；
4) by composite precursor in 80 DEG C of baking ovens dried, be cooled to room temperature in being put in exsiccator, be then placed in crucible
Calcining in Muffle furnace, calcining heat is 400 DEG C, and calcination time is 2h；
5) the complex catalyst that after calcining, gained contains impurity is washed 5 times through high speed centrifugation, and alcohol washes 3 times, and condition is
Centrifugal speed 8000r/min, centrifugation time 7min, centrifugal rear gained solid matter is placed in 80 DEG C of drying in oven, places into
Exsiccator is cooled to room temperature, with the TiO prepared under the i.e. available different calcination conditions of Achates grind into powder2/ Al rice husk is born
Carry light complex catalyst.
Embodiment 3
1) take a certain amount of rice husk and be soaked in 12h in 1mol/L HCl, after making metal ion remove completely, be washed to neutrality,
It is placed in 80 DEG C of baking ovens and is dried, then be cooled to room temperature in being put in exsiccator, after pulverizer is pulverized, carry out in glass pot
After grinding 15min, load in sample sack stand-by；
2) respectively by a certain amount of titanyl sulfate (TiOSO4) and Disodium oxalate. (Na2C2O4) mol ratio by 1: 1 respectively grinds 15min
Presoma is made afterwards with some PEG400 mixed grinding 50min；
3) by 21.0g anhydrous slufuric acid aluminum (Al2(SO4)3) mix after the 30min that mills with 10.1g presoma, add 6.8g rice
Shell powder remixes the 50min that mills and makes composite precursor, and in presoma, the mol ratio of Ti, Al and Si element is 1: 1: 1；
4) by composite precursor in 80 DEG C of baking ovens dried, be cooled to room temperature in being put in exsiccator, be then placed in crucible
Calcining in Muffle furnace, calcining heat is 500 DEG C, and calcination time is 1h；
5) the complex catalyst that after calcining, gained contains impurity is washed 6 times through high speed centrifugation, and alcohol washes 4 times, and condition is
Centrifugal speed 8000r/min, centrifugation time 5min, centrifugal rear gained solid matter is placed in 80 DEG C of drying in oven, places into
Exsiccator is cooled to room temperature, with the T prepared under the i.e. available different calcination conditions of Achates grind into powderiO2/ Al rice husk loads
Light complex catalyst.
Three, TiO2/ Al rice husk load light complex catalyst catalytic performance research experiment
Research experiment comprises the steps:
1) take some quartz cuvette, in quartz cuvette, be separately added into rotor, 0.1g difference calcining temperature in order
Degree different the complex catalyst sample of calcination time, 50mL 20mg/L, the methyl orange (C of PH=7.014H14N3NaO3S) molten
Liquid, is then placed in the groove of photochemical reaction instrument, opens reactor switch, after solution uniform stirring, carries out dark reaction
30min；
2), after dark reaction terminates, close reactor switch, pipette 10mL reactant liquor and be placed in centrifuge tube, with 10000r/min
Speed high speed centrifugation separate 5min；
3) at 464nm wavelength, measure its absorbance with needle tubing extraction supernatant 722 visible spectrophotometers, record number
According to, the most again complete soln is refunded quartz cuvette；
4) quartz cuvette is reentered in the groove of photochemical reaction instrument, opens cooling water, reactor switch successively, treat
After solution uniform stirring, open light source and carry out photoreaction, take a sample every 5min, before sampling, close light source switch, anti-successively
Answer device switch, cooling water, repeat step 2) and 3), recording corresponding data, photoreaction carries out 60min altogether；
5) examine phenomenon, and conscientiously process experimental data.
Four, data analysis
Gained presoma is put into crucible and is calcined in Muffle furnace, calcining heat be controlled as 300 DEG C, 400 DEG C and
500 DEG C, calcination time is 1-4h, and gained calcined powder carries out light-catalyzed reaction respectively, inhales with the detection of visible spectrophotometric instrument
Luminosity, result is as follows:
Fig. 1 be the catalyst made of 300 DEG C of different calcination times in visible ray graded irradiation 60min to methyl orange
Degradation curve, along with the prolongation of light application time, the surplus ratio of methyl orange solution is gradually reduced, due in cloudy, turbid phase, compound
Body catalyst has reached saturated to the absorption of methyl orange solution, so the catalyst that 300 DEG C of different calcination times are made has
Certain photocatalysis performance.
Fig. 2 be the catalyst made of 400 DEG C of different calcination times in visible ray graded irradiation 60min to methyl orange
Degradation curve, along with the prolongation of light application time, the surplus ratio of methyl orange solution is gradually increased, due in cloudy, turbid phase, 1h and
The complex catalyst of 2h has reached saturated to the absorption of methyl orange solution, so the catalyst that 300 DEG C of 1h, 2h time makes
There is certain photocatalysis performance, and the catalyst photocatalysis performance that 3h and the 4h time makes is not sufficiently good.
Fig. 3 be the catalyst made of 500 DEG C of different calcination times in visible ray graded irradiation 60min to methyl orange
Degradation curve, along with the prolongation of light application time, the surplus ratio of methyl orange solution is gradually reduced, due in cloudy, turbid phase, compound
Body catalyst has reached saturated to the absorption of methyl orange solution, so the catalyst that 500 DEG C of different calcination times are made has
Certain photocatalysis performance.
Five, result of study
TiO2/ Al rice husk load light complex catalyst has higher photocatalytic activity, has preferable application prospect.
Claims (3)
1. a TiO2/ Al rice husk load light complex catalyst, it is characterised in that: with rice husk as carrier, it is loaded with TiO2/Al
And the composite photo-catalyst formed, wherein the mol ratio of Ti, Al and Si element is 1: 1: 1.
2. a TiO according to claim 12The preparation method of/Al rice husk load light complex catalyst, it is characterised in that
The method comprises the steps:
1) take rice husk to be soaked in 1mol/L HCl, after making metal ion remove completely, be washed to neutrality, be then dried, cool down
Pulverize to room temperature, stand-by after grinding 15min in glass pot；
2) respectively by TiOSO4And Na2C2O4Mol ratio by 1: 1 mixes with some PEG400s after respectively grinding 15min grinds
Mill 50min makes presoma；
3) by anhydrous Al2(SO4)3Mixing with described presoma after the 30min that mills, addition powdered rice hulls remixes the 50min that mills and makes
Composite precursor, in presoma, the mol ratio of Ti, Al and Si element is 1: 1: 1；
4) described composite precursor being cooled to room temperature after drying, be then placed in Muffle furnace calcining, calcining heat is
300-500 DEG C, calcination time is 1-2h；
5) the complex catalyst that after calcining, gained contains impurity is washed, by gained solid matter warp through high speed centrifugation washing, alcohol
Dry, be cooled to room temperature after can be prepared by described TiO with Achates grind into powder2/ Al rice husk load light complex catalyst.
3. a TiO according to claim 22The preparation method of/Al rice husk load light complex catalyst, it is characterised in that:
Step 5) described high speed centrifugation wash 4-6 time, alcohol is washed 2-4 time, and condition is centrifugal speed 8000r/min, centrifugation time 5-
10min。
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| CN111557859A (en) * | 2019-11-06 | 2020-08-21 | 成都理工大学 | Pyrophyllite loaded nano ZnO composite uvioresistant agent and preparation method thereof |
| CN113042053A (en) * | 2021-02-25 | 2021-06-29 | 福建师范大学 | Co applied to propane catalytic oxidation in rice hull powder mediated preparation3O4-SiO2Method for preparing catalyst |
| CN115055192A (en) * | 2022-06-16 | 2022-09-16 | 中南大学 | Al 3+ /Zn 0.4 (CuGa) 0.3 Ga 2 S 4 Composite material and preparation method and application thereof |
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| CN106984293A (en) * | 2017-05-06 | 2017-07-28 | 山西兰花华明纳米材料股份有限公司 | TiO 2 visible light catalyst of doping vario-property and preparation method thereof |
| CN111557859A (en) * | 2019-11-06 | 2020-08-21 | 成都理工大学 | Pyrophyllite loaded nano ZnO composite uvioresistant agent and preparation method thereof |
| CN113042053A (en) * | 2021-02-25 | 2021-06-29 | 福建师范大学 | Co applied to propane catalytic oxidation in rice hull powder mediated preparation3O4-SiO2Method for preparing catalyst |
| CN115055192A (en) * | 2022-06-16 | 2022-09-16 | 中南大学 | Al 3+ /Zn 0.4 (CuGa) 0.3 Ga 2 S 4 Composite material and preparation method and application thereof |
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