CN107308927A - A kind of preparation method of titanium dioxide homojunction nano-photocatalyst - Google Patents
A kind of preparation method of titanium dioxide homojunction nano-photocatalyst Download PDFInfo
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- CN107308927A CN107308927A CN201710507839.8A CN201710507839A CN107308927A CN 107308927 A CN107308927 A CN 107308927A CN 201710507839 A CN201710507839 A CN 201710507839A CN 107308927 A CN107308927 A CN 107308927A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 145
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 68
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 127
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 99
- 239000000243 solution Substances 0.000 claims abstract description 64
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 239000002127 nanobelt Substances 0.000 claims abstract description 28
- 239000002244 precipitate Substances 0.000 claims abstract description 25
- 239000000725 suspension Substances 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 18
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011259 mixed solution Substances 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 11
- 238000001291 vacuum drying Methods 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 238000000151 deposition Methods 0.000 claims abstract description 4
- 230000008021 deposition Effects 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 6
- HGWOWDFNMKCVLG-UHFFFAOYSA-N [O--].[O--].[Ti+4].[Ti+4] Chemical compound [O--].[O--].[Ti+4].[Ti+4] HGWOWDFNMKCVLG-UHFFFAOYSA-N 0.000 claims 1
- 239000006228 supernatant Substances 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 38
- 239000000047 product Substances 0.000 description 11
- 238000013019 agitation Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910003087 TiOx Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- HLLICFJUWSZHRJ-UHFFFAOYSA-N tioxidazole Chemical compound CCCOC1=CC=C2N=C(NC(=O)OC)SC2=C1 HLLICFJUWSZHRJ-UHFFFAOYSA-N 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Classifications
-
- B01J35/39—
-
- 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
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
Abstract
The invention discloses a kind of preparation method of titanium dioxide homojunction nano-photocatalyst, it is specially:Step 1, the preparation of titanium dioxide nano-belts:Titanium dioxide is scattered in NaOH solution, is sufficiently stirred for, hydro-thermal reaction is carried out, centrifuge washing is then carried out, is dried to obtain titanium dioxide nano-belts;Step 2, obtained titanium dioxide nano-belts are weighed to be scattered in ethylene glycol and sodium hydroxide mixed solution, ultrasonic disperse, obtains tio_2 suspension, then measure butyl titanate being added in tio_2 suspension, stirred, obtain reaction solution;Step 3, obtained reaction solution is transferred in the reactor with polytetrafluoroethyllining lining, hydro-thermal reaction, reaction naturally cools to room temperature after terminating, and obtains white precipitate;Step 4, white depositions are used into deionized water, absolute ethyl alcohol centrifuge washing successively, is subsequently placed in vacuum drying chamber and dries.Adopt homogeneous, the regular appearance that is obtained by the present invention titanium dioxide homojunction nano-photocatalyst particle size.
Description
Technical field
The invention belongs to photocatalyst technology field, it is related to a kind of preparation side of titanium dioxide homojunction nano-photocatalyst
Method.
Background technology
Photocatalysis technology is the emerging green technology progressively grown up from 1970s, and it is mainly used
Semiconductor oxide materials under conditions of illumination surface can by activation characteristic, can effectively oxidation Decomposition organic matter, also
Original weight metal ion, killing bacterium and elimination peculiar smell, have a wide range of applications in many fields such as wastewater treatment, gas purification.
Titanium dioxide (TiO2) because it is inexpensive, be easy to get, nontoxic, high chemical stability, strong anti-light corrosion
The advantages of property, become and up to the present study also most deep a kind of semiconductor light-catalyst the most extensive.But it is higher
Photo-generate electron-hole combined efficiency is to influence a key factor of titanium dioxide application.To solve this problem, we are two
On the basis of titanium oxide exposure crystal face research, the thinking that composite is constructed based on homojunction is introduced, composite construction is explained
Photoelectric-synergetic strengthens mechanism, so as to effectively reduce the electron-hole recombinations efficiency of composite titania material material to be lifted
Its photoelectric properties and its reality under sun light action.So we are attempted using crystal face effect or the symmetry of crystal face two
Nanostructured formation homojunction is selectively constructed in titanium oxide particular crystal plane, this is to full appreciation crystal face effect and improves photocatalysis
Performance has important scientific meaning and practical value.It is therefore desirable to provide a kind of simple and low titanium dioxide homogeneity of cost
Tie the preparation method of nano-photocatalyst.
The content of the invention
It is an object of the invention to provide a kind of preparation method of titanium dioxide homojunction nano-photocatalyst, preparation method work
Skill is simple, cost is low.
The technical solution adopted in the present invention is that a kind of preparation method of titanium dioxide homojunction nano-photocatalyst has
Body is implemented according to following steps:
Step 1, the preparation of titanium dioxide nano-belts:A certain amount of titanium dioxide P25 is scattered in a certain amount of NaOH molten
In liquid, it is sufficiently stirred for, then carries out 12~24h of hydro-thermal reaction at 160~200 DEG C, then carries out centrifuge washing, is dried to obtain two
TiOx nano band;
Step 2, obtained titanium dioxide nano-belts in a certain amount of step 1 are weighed and are scattered in a certain amount of ethylene glycol and hydrogen-oxygen
Change in sodium mixed solution, ultrasonic disperse obtains tio_2 suspension, then the butyl titanate of measured amounts is added to titanium dioxide
In titanium suspension, 10~20min is stirred, reaction solution is obtained;
Step 3, the reaction solution that step 2 is obtained is transferred in the reactor with polytetrafluoroethyllining lining, 160~
10~12h of hydro-thermal reaction under the conditions of 200 DEG C, reaction naturally cools to room temperature after terminating, and obtains white precipitate;
Step 4, white depositions step 3 obtained use deionized water, absolute ethyl alcohol centrifuge washing successively, are subsequently placed in
10~12h is dried in 60~80 DEG C of vacuum drying chambers, titanium dioxide homojunction nano-photocatalyst is obtained.
The features of the present invention is also resided in,
The quality of titanium dioxide P25 in step 1 and the volume ratio of NaOH solution are 0.1~0.5g:50~100mL;
NaOH solution concentration in step 1 is 5~10M.
The quality of the titanium dioxide nano-belts of step 2 and ethylene glycol and sodium hydroxide mixed liquor volume ratio is 0.1~
0.5g:25~75mL.
It is 99% to be given in step 2 in tio_2 suspension and add the concentration of butyl titanate, and volume is 0.1~1mL.
The sodium hydroxide that the ethylene glycol solution and concentration that ethylene glycol and sodium hydroxide mixed solution are 99% by concentration are 1M
Solution is 1 according to volume ratio:1 is mixed to prepare.
The beneficial effects of the invention are as follows process of the present invention is simple, and cost is low, is suitable for extensive life
Production, and the raw material such as used P25 and butyl titanate is easy to get, it is pollution-free.Experimental period is short, is easy to operation, and energy consumption is low, great work
Industry prospect.Product particle size uniformity prepared by the present invention, regular appearance, and titanium dioxide homojunction nano-photo catalytic
Agent has higher light-catalyzed reaction efficiency.
Brief description of the drawings
Fig. 1 is two prepared by a kind of preparation method embodiment 1 of titanium dioxide homojunction nano-photocatalyst of the invention
Titanium oxide homojunction nano-photocatalyst X ray diffracting spectrum;
Fig. 2 is two prepared by a kind of preparation method embodiment 2 of titanium dioxide homojunction nano-photocatalyst of the invention
Titanium oxide homojunction nano-photocatalyst stereoscan photograph;
Fig. 3 is two prepared by a kind of preparation method embodiment 3 of titanium dioxide homojunction nano-photocatalyst of the invention
Titanium oxide homojunction nano-photocatalyst transmits photo;
Fig. 4 is two prepared by a kind of preparation method embodiment 4 of titanium dioxide homojunction nano-photocatalyst of the invention
Titanium oxide homojunction nano-photocatalyst cyclic voltammetry curve photo.
Embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
A kind of preparation method of titanium dioxide homojunction nano-photocatalyst of the present invention, it is specifically real according to following steps
Apply:
Step 1, the preparation of titanium dioxide nano-belts:0.1~0.5g titanium dioxide P25 is scattered in 50~100mL dense
Spend in 5~10M NaOH solutions, to be sufficiently stirred for, then 160~200 DEG C carry out 12~24h of hydro-thermal reaction, then carry out from
The heart washs, is dried to obtain titanium dioxide nano-belts;
Step 2, weigh in 0.1~0.5g steps 1 obtained titanium dioxide nano-belts be scattered in 25~75mL ethylene glycol and
In sodium hydroxide mixed solution, ultrasonic disperse obtains tio_2 suspension, then measures 0.1~1mL, and concentration is 99% titanium
Acid butyl ester is added in tio_2 suspension, is stirred 10~20min, is obtained reaction solution;Wherein, ethylene glycol and sodium hydroxide
The sodium hydroxide solution that the ethylene glycol solution and concentration that mixed solution is 99% by concentration are 1M is 1 according to volume ratio:1 mixing system
;
Step 3, the reaction solution that step 2 is obtained is transferred in the reactor with polytetrafluoroethyllining lining, 160~
10~12h of hydro-thermal reaction under the conditions of 200 DEG C, reaction naturally cools to room temperature after terminating, and obtains white precipitate;
Step 4, white depositions step 3 obtained use deionized water, absolute ethyl alcohol centrifuge washing successively, are subsequently placed in
10~12h is dried in 60~80 DEG C of vacuum drying chambers, titanium dioxide homojunction nano-photocatalyst is obtained.
Embodiment 1
Step 1,0.1g P25 are weighed and are added to 50mL concentration in 5M NaOH solutions, magnetic agitation 10min, by gained
Solution is transferred in the reactor with polytetrafluoroethyllining lining, the conventional hydrothermal 12h under the conditions of 160 DEG C, and reaction is natural after terminating
Room temperature is cooled to, white precipitate is obtained, precipitated product is collected and uses deionized water, absolute ethyl alcohol centrifuge washing successively, in air
In 60 DEG C of dry 12h, obtain titanium dioxide nano-belts;
Step 2, weigh obtained titanium dioxide nano-belts powder 0.1g and be scattered in 25mL sodium hydroxides and ethylene glycol
In mixed solution, ultrasonic disperse 10min obtains tio_2 suspension, then measures the butyl titanate that 0.1mL concentration is 99% and add
Enter into obtained tio_2 suspension, stir 10min, obtain reaction solution;Wherein, ethylene glycol and sodium hydroxide mixing are molten
The sodium hydroxide solution that the ethylene glycol solution and concentration that liquid is 99% by concentration are 1M is 1 according to volume ratio:1 is mixed to prepare;
Step 3, then resulting solution is transferred in the reactor with polytetrafluoroethyllining lining, passed under the conditions of 160 DEG C
Unite hydro-thermal 10h, and reaction naturally cools to room temperature after terminating, obtains white precipitate;
Step 4, collect white precipitate and use deionized water, absolute ethyl alcohol centrifuge washing successively, be placed in vacuum drying chamber
60 DEG C of dry 10h, obtain titanium dioxide homojunction nano-photocatalyst.
As shown in figure 1, being the titanium dioxide nano-belts prepared by embodiment 1 and the XRD of homojunction nano-photocatalyst
Spectrum, it can be seen that all diffraction maximums in the XRD spectrum of composite are relative with the standard diffraction peak of titanium dioxide
Should, do not occur the diffraction maximum of any impurity.
Embodiment 2
Step 1,0.5g P25 are weighed and are added to 100mL concentration in 10M NaOH solutions, magnetic agitation 10min, by institute
Obtain solution to be transferred in the reactor with polytetrafluoroethyllining lining, the conventional hydrothermal 24h under the conditions of 200 DEG C, react after terminating certainly
Room temperature so is cooled to, white precipitate is obtained, precipitated product is collected and uses deionized water, absolute ethyl alcohol centrifuge washing successively, in sky
60 DEG C of dry 12h, obtain titanium dioxide nano-belts in gas;
Step 2, weigh obtained titanium dioxide nano-belts powder 0.5g and be scattered in 75mL sodium hydroxides and ethylene glycol
In mixed solution, ultrasonic disperse 10min obtains tio_2 suspension.The butyl titanate that 1mL concentration is 99% is measured again to add
Into obtained tio_2 suspension, 10min is stirred, reaction solution is obtained;Wherein, ethylene glycol and sodium hydroxide mixed solution
The sodium hydroxide solution that the ethylene glycol solution and concentration for being 99% by concentration are 1M is 1 according to volume ratio:1 is mixed to prepare;
Step 3, then gained reaction solution is transferred in the reactor with polytetrafluoroethyllining lining, in 200 DEG C of conditions
Lower conventional hydrothermal 12h, reaction naturally cools to room temperature after terminating, and obtains white precipitate;
Step 4, collect white precipitate and use deionized water, absolute ethyl alcohol centrifuge washing successively, be placed in vacuum drying chamber
80 DEG C of dry 12h, obtain titanium dioxide homojunction nano-photocatalyst.
As shown in Fig. 2 the titanium dioxide homojunction nano-photocatalyst size uniformity prepared by embodiment 2, is one-dimensional
Banding, width is 200nm~500nm, and length is several microns, regular appearance.
Embodiment 3
Step 1,0.25g P25 are weighed and are added to 50mL concentration in 5M NaOH solutions, magnetic agitation 20min, by gained
Solution is transferred in the reactor with polytetrafluoroethyllining lining, the conventional hydrothermal 18h under the conditions of 180 DEG C, and reaction is natural after terminating
Room temperature is cooled to, white precipitate is obtained, precipitated product is collected and uses deionized water, absolute ethyl alcohol centrifuge washing successively, in air
In 60 DEG C of dry 20h, obtain titanium dioxide nano-belts;
Step 2, weigh obtained titanium dioxide nano-belts powder 0.5g and be scattered in 50mL sodium hydroxides and ethylene glycol
In mixed solution, ultrasonic disperse 10min obtains tio_2 suspension.The butyl titanate that 0.5mL concentration is 99% is measured again to add
Enter into obtained tio_2 suspension, stir 10min, obtain reaction solution;Wherein, ethylene glycol and sodium hydroxide mixing are molten
The sodium hydroxide solution that the ethylene glycol solution and concentration that liquid is 99% by concentration are 1M is 1 according to volume ratio:1 is mixed to prepare;
Step 3, then gained reaction solution is transferred in the reactor with polytetrafluoroethyllining lining, in 180 DEG C of conditions
Lower conventional hydrothermal 10h, reaction naturally cools to room temperature after terminating, and obtains white precipitate;
Step 4, collect white precipitate and use deionized water, absolute ethyl alcohol centrifuge washing successively, be placed in vacuum drying chamber
80 DEG C of dry 12h, obtain titanium dioxide homojunction nano-photocatalyst,
As shown in figure 3, it is evident that photocatalysis composite size uniformity, regular appearance from figure.
Embodiment 4
Step 1, weigh 0.2g P25 to be added in the NaOH solution that 75mL concentration is 10M, magnetic agitation 20min, by institute
Obtain solution to be transferred in the reactor with polytetrafluoroethyllining lining, the conventional hydrothermal 24h under the conditions of 160 DEG C, react after terminating certainly
Room temperature so is cooled to, white precipitate is obtained, precipitated product is collected and uses deionized water, absolute ethyl alcohol centrifuge washing successively, in sky
60 DEG C of dry 10h, obtain titanium dioxide nano-belts in gas.
Step 2, weigh obtained titanium dioxide nano-belts powder 0.3g and be scattered in 50mL sodium hydroxides and ethylene glycol
In mixed solution, ultrasonic disperse 10min obtains tio_2 suspension.1mL butyl titanates are measured again is added to obtained dioxy
Change in titanium suspension, stir 10min, obtain reaction solution;Wherein, ethylene glycol and sodium hydroxide mixed solution are 99% by concentration
The sodium hydroxide solution that ethylene glycol solution and concentration are 1M is 1 according to volume ratio:1 is mixed to prepare;
Step 3, then resulting solution is transferred in the reactor with polytetrafluoroethyllining lining, passed under the conditions of 200 DEG C
Unite hydro-thermal 10h, and reaction naturally cools to room temperature after terminating, obtains white precipitate;
Step 4, collect white precipitate and use deionized water, absolute ethyl alcohol centrifuge washing successively, be placed in vacuum drying chamber
60 DEG C of dry 10h, obtain titanium dioxide homojunction nano-photocatalyst.
As shown in figure 4, substantially it can be seen that photocatalysis composite has excellent contaminant degradation from Fig. 4
Energy.
Embodiment 5
Step 1, weigh 0.2g P25 to be added in the NaOH solution that 75mL concentration is 5M, magnetic agitation 10min, by gained
Solution is transferred in the reactor with polytetrafluoroethyllining lining, the conventional hydrothermal 24h under the conditions of 170 DEG C, and reaction is natural after terminating
Room temperature is cooled to, white precipitate is obtained, precipitated product is collected and uses deionized water, absolute ethyl alcohol centrifuge washing successively, in air
In 60 DEG C of dry 20h, obtain titanium dioxide nano-belts.
Step 2, weigh obtained titanium dioxide nano-belts powder 0.4g and be scattered in 50mL sodium hydroxides and ethylene glycol
In mixed solution, ultrasonic disperse 10min obtains tio_2 suspension.0.25mL butyl titanates are measured again is added to what is obtained
In tio_2 suspension, 10min is stirred, reaction solution is obtained;Wherein, ethylene glycol and sodium hydroxide mixed solution are by concentration
The sodium hydroxide solution that 99% ethylene glycol solution and concentration is 1M is 1 according to volume ratio:1 is mixed to prepare;
Step 3, then gained reaction solution is transferred in the reactor with polytetrafluoroethyllining lining, in 200 DEG C of conditions
Lower conventional hydrothermal 12h, reaction naturally cools to room temperature after terminating, and obtains white precipitate;
Step 4, collect white precipitate product and use deionized water, absolute ethyl alcohol centrifuge washing successively, be placed in vacuum drying
70 DEG C of dry 11h, obtain titanium dioxide homojunction nano-photocatalyst in case.
Embodiment 6
Step 1, weigh 0.3g P25 to be added in the NaOH solution that 50mL concentration is 10M, magnetic agitation 10min, by institute
Obtain solution to be transferred in the reactor with polytetrafluoroethyllining lining, the conventional hydrothermal 12h under the conditions of 200 DEG C, react after terminating certainly
Room temperature so is cooled to, white precipitate is obtained, precipitated product is collected and uses deionized water, absolute ethyl alcohol centrifuge washing successively, in sky
60 DEG C of dry 10h, obtain titanium dioxide nano-belts in gas.
Step 2, weigh obtained titanium dioxide nano-belts powder 0.3g and be scattered in 50mL sodium hydroxides and ethylene glycol
In mixed solution, ultrasonic disperse 10min obtains tio_2 suspension.The butyl titanate that 0.2mL concentration is 99% is measured again to add
Enter into obtained tio_2 suspension, stir 15min, obtain reaction solution;Wherein, ethylene glycol and sodium hydroxide mixing are molten
The sodium hydroxide solution that the ethylene glycol solution and concentration that liquid is 99% by concentration are 1M is 1 according to volume ratio:1 is mixed to prepare;
Step 3, then gained reaction solution is transferred in the reactor with polytetrafluoroethyllining lining, in 160 DEG C of conditions
Lower conventional hydrothermal 11h, reaction naturally cools to room temperature after terminating, and obtains white precipitate;
Step 4, collect white precipitate product and use deionized water, absolute ethyl alcohol centrifuge washing successively, be placed in vacuum drying
70 DEG C of dry 12h, obtain titanium dioxide homojunction nano-photocatalyst in case.
Embodiment 7
Step 1, weigh 0.25g P25 to be added in the NaOH solution that 75mL concentration is 7M, magnetic agitation 10min, by institute
Obtain solution to be transferred in the reactor with polytetrafluoroethyllining lining, the conventional hydrothermal 12h under the conditions of 200 DEG C, react after terminating certainly
Room temperature so is cooled to, white precipitate is obtained, precipitated product is collected and uses deionized water, absolute ethyl alcohol centrifuge washing successively, in sky
60 DEG C of dry 10h, obtain titanium dioxide nano-belts in gas.
Step 2, weigh obtained titanium dioxide nano-belts powder 0.3g and be scattered in 50mL sodium hydroxides and ethylene glycol
In mixed solution, ultrasonic disperse 10min obtains tio_2 suspension.The butyl titanate that 0.2mL concentration is 99% is measured again to add
Enter into obtained tio_2 suspension, stir 20min, obtain reaction solution;Wherein, ethylene glycol and sodium hydroxide mixing are molten
The sodium hydroxide solution that the ethylene glycol solution and concentration that liquid is 99% by concentration are 1M is 1 according to volume ratio:1 is mixed to prepare;
Step 3, then gained reaction solution is transferred in the reactor with polytetrafluoroethyllining lining, in 160 DEG C of conditions
Lower conventional hydrothermal 11h, reaction naturally cools to room temperature after terminating, and obtains white precipitate;
Step 4, collect white precipitate product and use deionized water, absolute ethyl alcohol centrifuge washing successively, be placed in vacuum drying
70 DEG C of dry 12h, obtain titanium dioxide homojunction nano-photocatalyst in case.
Claims (6)
1. a kind of preparation method of titanium dioxide homojunction nano-photocatalyst, it is characterised in that specific real according to following steps
Apply:
Step 1, the preparation of titanium dioxide nano-belts:A certain amount of titanium dioxide P25 is scattered in a certain amount of NaOH solution,
It is sufficiently stirred for, then carries out 12~24h of hydro-thermal reaction at 160~200 DEG C, then carries out centrifuge washing, is dried to obtain titanium dioxide
Titanium nanobelt;
Step 2, obtained titanium dioxide nano-belts in a certain amount of step 1 are weighed and are scattered in a certain amount of ethylene glycol and sodium hydroxide
In mixed solution, ultrasonic disperse obtains tio_2 suspension, then the butyl titanate of measured amounts is added to titanium dioxide and hanged
In supernatant liquid, 10~20min is stirred, reaction solution is obtained;
Step 3, the reaction solution that step 2 is obtained is transferred in the reactor with polytetrafluoroethyllining lining, at 160~200 DEG C
Under the conditions of 10~12h of hydro-thermal reaction, reaction terminate after naturally cool to room temperature, obtain white precipitate;
Step 4, white depositions step 3 obtained use deionized water, absolute ethyl alcohol centrifuge washing successively, it is subsequently placed in 60~
10~12h is dried in 80 DEG C of vacuum drying chambers, titanium dioxide homojunction nano-photocatalyst is obtained.
2. a kind of preparation method of titanium dioxide homojunction nano-photocatalyst according to claim 1, it is characterised in that
The quality of titanium dioxide P25 described in step 1 and the volume ratio of NaOH solution are 0.1~0.5g:50~100mL.
3. a kind of preparation method of titanium dioxide homojunction nano-photocatalyst according to claim 1, it is characterised in that
NaOH solution concentration described in step 1 is 5~10M.
4. a kind of preparation method of titanium dioxide homojunction nano-photocatalyst according to claim 1, it is characterised in that
The quality of titanium dioxide nano-belts described in step 2 is 0.1~0.5g with ethylene glycol and sodium hydroxide mixed liquor volume ratio:25
~75mL.
5. a kind of preparation method of titanium dioxide homojunction nano-photocatalyst according to claim 1, it is characterised in that
It is 99% to be given in the step 2 in tio_2 suspension and add the concentration of butyl titanate, and volume is 0.1~1mL.
6. a kind of preparation method of titanium dioxide homojunction nano-photocatalyst according to claim 4, it is characterised in that
The sodium hydroxide solution that the ethylene glycol solution and concentration that ethylene glycol and the sodium hydroxide mixed solution is 99% by concentration are 1M
It is 1 according to volume ratio:1 is mixed to prepare.
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