CN107570179B - A kind of TiO2The preparation method of/BiOCl hetero-junctions visible light catalyst - Google Patents
A kind of TiO2The preparation method of/BiOCl hetero-junctions visible light catalyst Download PDFInfo
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Abstract
The invention discloses a kind of TiO2The preparation method of/BiOCl hetero-junctions visible light catalyst, comprising the following steps: in Bi2O3、TiO2, dehydrated alcohol is added in NaCl and KCl powder mixture, mixing is milled, and mixture is dried to obtain powder A after mixing；Powder A is calcined into 0.5~2h at 750~1100 DEG C, cools to room temperature with the furnace, after obtained product is washed, dry, obtains pre-reaction material B；It drives in object B before the reaction and deionized water is added, and hydrochloric acid is added, be ultrasonically treated 0.2~1h, obtain mixture C；Mixture C is heated into 2~4h at 100~120 DEG C, obtains TiO2/ BiOCl hetero-junctions powder.Raw material of the invention is simple and from a wealth of sources, obtained TiO2Catalytic effect is excellent under visible light for/BiOCl hetero-junctions catalyst, than single commercial TiO2(P25) and BiOCl obviously has higher photocatalytic activity.
Description
Technical field
The present invention relates to TiO2Visible light catalyst, more particularly to a kind of TiO2/ BiOCl hetero-junctions visible light catalyst
Preparation method, belong to semiconductor light-catalyst preparation technical field.
Background technique
Photocatalitic Technique of Semiconductor can convert solar energy to chemical energy and electric energy, and can directly utilize the sun
Various pollutants in light degradation and mineralized water and air have great potential in terms of the depollution of environment and new energy development.
TiO2Nontoxic with safety, tasteless, the good advantage of thermal stability is the representative of catalysis material.But TiO2It is a kind of broad stopband
Semiconductor, the ultraviolet excitation of band-gap energy 3.2eV, only wavelength less than 388nm can just make it produce light induced electron and hole, and
Ultraviolet light accounts for sunshine gross energy less than 5%, TiO2Photocatalysis technology is faced with quantum yield low low with solar energy utilization ratio two
Hang-up.
BiOCl is a kind of Bi stratiform multi-element compounds.And its structure is by 2 layers of Cl‐Sheath and 1 layer of (Bi2O2)2+Along C axis
It is alternately stacked.Since its layer structure makes inside can produce induced dipole square, photo-generate electron-hole is more easier point
From possessing compare TiO under the irradiation of ultraviolet light2Stronger photocatalytic activity.But bismuth oxychloride (BiOCl) is forbidden bandwidth
For the semiconductor of 3.46eV, the ultraviolet light in sunlight can only be also utilized.
All there is photo-generated carriers to be easy to compound, photocatalysis effect to some extent when being used alone for both catalyst
The lower problem of rate.
The compound separation rate that can obviously accelerate photo-generated carrier of semiconductor, and its recombination is effectively hindered, it is compound partly to lead
The activity of body material is generally greater than single semiconductor material.Therefore, by TiO2The half of both different bandwidths with BiOCl
It compounds to conductor material science together, both to expand the absorption region to spectrum, prepares a kind of photo-catalysis capability and obtain
The composite photocatalyst significantly improved is actually necessary.
Document " Wang Lei, Wang Zhijun, Wang Yuting etc., BiOCl/TiO2The visible light activity and mechanism study of composite material, ring
Border science journal, 2015,1,222-228 ", which is disclosed, a kind of prepares BiOCl/TiO2Method, but need first with hydro-thermal legal system
Standby BiOCl, then BiOCl powder is added in titanium glue, then BiOCl/TiO is prepared with sol-gal process2, preparation process is multiple
It is miscellaneous；Document " Miguel Guerrero, Ainhoa Altube, Eva Garc í a-Lecina, Facile in situ
synthesis of BiOCl nanoplates stacked to highly porous TiO2:A synergistic
Combination for environmental remediation ", which is disclosed, a kind of prepares BiOCl piece/porous TiO2It is compound
The method of material, but the hydro-thermal method that first use twice is needed to prepare BiOCl/TiO2Precursor, then use sol-gel method
Prepare BiOCl piece/porous TiO2, preparation process complexity is cumbersome；And need to use Ti [O (CH2)3CH3]4, BiCl3It is tried Deng chemistry
Agent and P123 (polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer) are used as template agent, and raw material is multiple
It is miscellaneous；In addition, the document does not study BiOCl piece/porous TiO2It can be seen that optical property, and it irradiates (light radiation in ultraviolet-visible light
Wavelength X=320~500nm) 180min is 86% to the degradation rate of rhodamine B, photocatalysis efficiency is not high.Document " Yunyu
Cai,Panpan Wang,Yixing Ye,Grafting BiOCl nanosheets onto TiO2tubular arrays
To form a hierarchical structure with improved photocatalytic performance, RSC
Advances, 2013,3,19064-19069 " disclose a kind of BiOCl nanometer sheet/TiO2The method of pipe array, but need
It uses anodizing and prepares TiO2Pipe array, preparation process is complicated, and the document only has studied it under ultraviolet light
The photocatalysis performance of sample, and be 60% in degradation rate of ultraviolet light (light radiation wavelength X=365nm) 5h to methyl orange,
Photocatalysis efficiency is not high.
Summary of the invention
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of TiO2/ BiOCl heterojunction photocatalysis
The preparation method of agent；The TiO of this method preparation2/ BiOCl visible light catalysis activity is good, and raw material needed for preparing is common agents, honest and clean
Valence is easy to get, and method and process is simple, and reaction condition controllability is strong, and required synthesis institute equipment is simple.
To achieve the goals above, the present invention will adopt the following technical scheme that
A kind of TiO2The preparation method of/BiOCl hetero-junctions visible light catalyst, comprising the following steps:
1) in Bi2O3、TiO2, dehydrated alcohol is added in NaCl and KCl powder mixture, mixing is milled, and is mixed after mixing
It closes object and is dried to obtain powder A；The molar ratio of the KCl and NaCl is 1:1~2:1；The Bi2O3Molar ratio with KCl is 1:
50~1:20；The Bi2O3With TiO2Molar ratio be 2:3~11:15；
2) powder A is calcined to 0.5~2h at 750~1100 DEG C, cools to room temperature with the furnace, by obtained product through washing
After washing, drying, pre-reaction material B is obtained；
3) it drives in object B before the reaction and deionized water is added, and hydrochloric acid is added, be ultrasonically treated 0.2~1h, obtain mixture C；
4) mixture C is heated to 2~4h at 100~120 DEG C, obtains TiO2/ BiOCl hetero-junctions powder.
To further realize the object of the invention, it is preferable that the mixing is milled to be carried out by ball milling, and the time of ball milling is
2~5h.
Preferably, step 1) and the temperature of the step 2) drying are 80 DEG C~100 DEG C.
Preferably, every gram of TiO in step 1)2It is added dehydrated alcohol 50-200 milliliters.
Preferably, the step 2) washing is that deionized water is sufficiently cleaned to remove NaCl and KCl.
Preferably, step 3) the pre-reaction material B and the mass ratio of deionized water are 1/300~1/100.
Preferably, the volume ratio of the hydrochloric acid and deionized water is 1:60~1:20.
Preferably, the concentration of the hydrochloric acid is 36.5%.
Compared with prior art, the present invention has the following advantages and beneficial effects:
(1) synthesis TiO of the invention2The preparation method of/BiOCl hetero-junctions visible light catalyst, raw material needed for preparing are
Common agents, cheap and easy to get, method and process is simple, and reaction condition controllability is strong, and required synthesis institute equipment is simple.
(2) synthesis TiO of the invention2The preparation method of/BiOCl hetero-junctions visible light catalyst, the TiO of this method preparation2/
BiOCl hetero-junctions has high visible light catalysis activity, and catalytic activity is much better than single commercial TiO2(P25) and
BiOCl, in field of environment protection extensive application prospect.
Detailed description of the invention
Fig. 1 is TiO prepared by the embodiment of the present invention 12The X-ray diffraction picture of/BiOCl hetero-junctions.
Fig. 2 is TiO prepared by the embodiment of the present invention 12The transmission electron microscope picture of/BiOCl hetero-junctions.
Fig. 3 is TiO prepared by the embodiment of the present invention 12The high-resolution-ration transmission electric-lens picture of/BiOCl hetero-junctions.
Fig. 4 is TiO prepared by the embodiment of the present invention 12/ BiOCl hetero-junctions and the TiO of commercialization2(P25) and BiOCl
The activity figure of (λ > 420nm) photocatalytic degradation rhodamine B (10mg/L) under visible light.
Fig. 5 is TiO prepared by the embodiment of the present invention 12/ BiOCl hetero-junctions and the TiO of commercialization2(P25) and BiOCl
The photo-catalytic degradation of methyl-orange (10mg/L) after visible light (λ > 420nm) irradiates 40min, methyl blue (10mg/L), phenol
The efficiency chart of (10mg/L).
Specific embodiment
Preferably to support the present invention, the present invention is further described below with reference to embodiment, but reality of the invention
It is without being limited thereto to apply mode.
Embodiment 1:
Weigh the Bi of 1.18g2O3, 0.30g TiO2, 4.68g KCl and 3.67g NaCl, place it in ball grinder
And 50ml dehydrated alcohol is added, mixing and ball milling 3h is dried to obtain powder A at 80 DEG C after ball milling mixing is uniform；Powder A is put into
2h is calcined at 800 DEG C in Muffle furnace, cools to room temperature with the furnace, obtained product is sufficiently cleaned through deionized water, is removed
NaCl and KCl obtains pre-reaction material B after dry at 80 DEG C；0.12g pre-reaction material B is put into beaker, is added
30ml deionized water, and the hydrochloric acid that 0.5ml mass fraction is 36.5% is added, it is ultrasonically treated 0.5h, obtains mixture C；It will mix
It closes object C and heats 2h at 100 DEG C, obtain TiO after dry2/ BiOCl hetero-junctions powder.
Fig. 1 is TiO manufactured in the present embodiment2The X ray diffracting spectrum of/BiOCl hetero-junctions, as shown in Figure 1, the present embodiment
The product of preparation is TiO2/ BiOCl compound, and the peak BiOCl is sharp, illustrates BiOCl well-crystallized.
Fig. 2 is TiO manufactured in the present embodiment2The transmission electron microscope picture of/BiOCl hetero-junctions.As shown in Figure 2, the present embodiment 1
The BiOCl of preparation is laminated structure, and the nano particle being grown in laminated structure is TiO2。
Fig. 3 is TiO manufactured in the present embodiment2The high-resolution-ration transmission electric-lens picture of/BiOCl hetero-junctions.It can be understood by Fig. 3
The lattice fringe of sample is observed on ground, wherein (110) crystal face of interplanar distance d=0.275nm corresponding to BiOCl, and interplanar
Correspond to TiO away from d=0.354nm2Anatase (101) crystal face, illustrate TiO2Carlo Model for Nano-Crystal Growth in BiOCl on piece, and
And Fig. 3 is shown in the different crystal contact face of two classes and forms firm knot (hetero-junctions), that is, forms TiO2/ BiOCl is heterogeneous
Knot.
TiO2The photocatalytic activity evaluation of/BiOCl hetero-junctions powder: precise 0.06gTiO2/ BiOCl hetero-junctions powder
Photochemical catalyst is added in 80mL rhodamine B solution (10mg/L), and solution, which is then placed in dark light protected environment stirring 30min, makes
Material reaches absorption-dissociation equilibrium；5mL suspension is taken out after balance to be placed in centrifuge tube.Luxuriant and rich with fragrance Lay photocatalysis instrument is moored using Beijing
As light source, radiation wavelength λ > 420nm, reactor is away from light source 15cm, using rhodamine B as target degradation product, connects circularly cooling
Machine takes 5mL suspension to be placed in centrifuge tube, total reaction time 40min to maintain the temperature at (25 ± 3) DEG C, every 5min；Reaction
Terminate, centrifuge tube is placed in supercentrifuge and is centrifugated, take supernatant with ultraviolet-visible spectrophotometer survey its
Then the absorbance of 553nm or so calculates C/C according to standard curve0, TiO is reflected with this2Degradation sieve of/BiOCl hetero-junctions
The effect of red bright B.
Fig. 4 is TiO prepared by the embodiment of the present invention 12/ BiOCl hetero-junctions, commercial TiO2(P25) and BiOCl is can
The activity figure of (λ > 420nm) photocatalytic degradation rhodamine B (10mg/L) under light-exposed.As shown in Figure 4, in radiation of visible light 40min
Afterwards, TiO manufactured in the present embodiment2/ BiOCl hetero-junctions is and commercial under the same terms to the degradation rate about 95% of rhodamine B solution
It is 31% to the degradation rate of rhodamine B that titanium dioxide (P25), which is 17%, BiOCl to the degradation rate of rhodamine B, it was demonstrated that this implementation
The TiO of example preparation2The visible light catalytic performance of/BiOCl hetero-junctions is much better than single commercial TiO2(P25) and BiOCl.TiO2
It with the combination of BiOCl, can obviously accelerate the separation rate of photo-generated carrier, and effectively hinder its recombination, it can to significantly improve
Light-exposed photocatalytic activity.
Fig. 5 is TiO prepared by the embodiment of the present invention 12/ BiOCl hetero-junctions and the TiO of commercialization2(P25) and BiOCl
The photo-catalytic degradation of methyl-orange after visible light (λ > 420nm) irradiates 40min, methyl blue, the efficiency chart of phenol.It can from Fig. 5
Out, after visible light (λ > 420nm) irradiates 40min, TiO2/ BiOCl hetero-junctions is to methyl orange, methyl blue, the degradation effect of phenol
Rate is respectively 89%, 92%, 77%, and commercial titanium dioxide (P25) is to methyl orange, methyl blue, the drop of phenol under the same terms
Solving efficiency is respectively 12%, 17%, and 8%, BiOCl is to methyl orange, and methyl blue, the degradation efficiency of phenol is respectively 26%,
29%, 21%.This illustrates TiO2/ BiOCl hetero-junctions to different organic pollutants visible optical property all with higher, and
And Visible Light Induced Photocatalytic efficiency is all higher than commercial TiO2(P25) and BiOCl, in field of environment protection extensive application prospect.
Embodiment 2:
Weigh the Bi of 2.36g2O3, 0.61g TiO2, 9.36g KCl and 7.31g NaCl, place it in ball grinder
And 60ml dehydrated alcohol is added, mixing and ball milling 5h is dried to obtain powder A at 100 DEG C after ball milling mixing is uniform；Powder A is put into
1h is calcined at 1000 DEG C in Muffle furnace, cools to room temperature with the furnace, obtained product is sufficiently cleaned through deionized water, is removed
NaCl and KCl obtains pre-reaction material B after dry at 80 DEG C；0.20g pre-reaction material B is put into beaker, is added
60ml deionized water, and the hydrochloric acid that 2ml mass fraction is 36.5% is added, ultrasonic 1h obtains mixture C；Mixture C is existed
3h is heated at 120 DEG C, obtains TiO after dry2/ BiOCl hetero-junctions powder.
With above-mentioned photocatalytic activity evaluation method, after radiation of visible light 40min, TiO manufactured in the present embodiment2/
BiOCl hetero-junctions is about 91% to the degradation rate of rhodamine B, and commercial titanium dioxide (P25) is to rhodamine B under the same terms
Degradation rate be 17%, BiOCl be 31% to the degradation rate of rhodamine B, it was demonstrated that TiO manufactured in the present embodiment2/ BiOCl is heterogeneous
The visible light catalytic performance of knot is much better than single commercial TiO2(P25) and BiOCl.
Embodiment 3:
Weigh the Bi of 1.18g2O3, 0.30g TiO2, 7.45g KCl and 5.84g NaCl, place it in ball grinder
And 50ml dehydrated alcohol is added, mixing and ball milling 4h is dried to obtain powder A at 100 DEG C after ball milling mixing is uniform；Powder A is put into
2h is calcined at 900 DEG C in Muffle furnace, cools to room temperature with the furnace, obtained product is sufficiently cleaned through deionized water, is removed
NaCl and KCl obtains pre-reaction material B after dry at 80 DEG C；0.15g pre-reaction material B is put into beaker, is added
30ml deionized water, and the hydrochloric acid that 1.2ml mass fraction is 36.5% is added, ultrasonic 0.5h obtains mixture C；By mixture C
2h is heated at 120 DEG C, obtains TiO after dry2/ BiOCl hetero-junctions powder.
With above-mentioned photocatalytic activity evaluation method, after radiation of visible light 40min, TiO2/ manufactured in the present embodiment
BiOCl hetero-junctions is about 89% to the degradation rate of rhodamine B, and commercial titanium dioxide (P25) is to rhodamine B under the same terms
Degradation rate be 17%, BiOCl be 31% to the degradation rate of rhodamine B, it was demonstrated that TiO manufactured in the present embodiment2/ BiOCl is heterogeneous
The visible light catalytic performance of knot is much better than single commercial TiO2(P25) and BiOCl.
Embodiment 4:
Weigh the Bi of 1.18g2O3, 0.30g TiO2, 7.45g KCl and 4.41g NaCl, place it in ball grinder
And 60ml dehydrated alcohol is added, mixing and ball milling 3h is dried to obtain powder A at 80 DEG C after ball milling mixing is uniform；Powder A is put into
0.5h is calcined at 1100 DEG C in Muffle furnace, cools to room temperature with the furnace, obtained product is sufficiently cleaned through deionized water, is removed
NaCl and KCl obtains pre-reaction material B after dry at 100 DEG C；0.18g pre-reaction material B is put into beaker, is added
45ml deionized water, and the hydrochloric acid that 1.2ml mass fraction is 36.5% is added, ultrasonic 1h obtains mixture C；By mixture C
4h is heated at 120 DEG C, obtains TiO2/BiOCl hetero-junctions powder after dry.
With above-mentioned photocatalytic activity evaluation method, after radiation of visible light 40min, TiO manufactured in the present embodiment2/
BiOCl hetero-junctions is about 93% to the degradation rate of rhodamine B, and commercial titanium dioxide (P25) is to rhodamine B under the same terms
Degradation rate be 17%, BiOCl be 31% to the degradation rate of rhodamine B, it was demonstrated that TiO manufactured in the present embodiment2/ BiOCl is heterogeneous
The visible light catalytic performance of knot is much better than single commercial TiO2(P25) and BiOCl.
Embodiment 5:
Weigh the Bi of 2.36g2O3, 0.61g TiO2, 9.36g KCl and 4.41g NaCl, place it in ball grinder
And 50ml dehydrated alcohol is added, mixing and ball milling 5h is dried to obtain powder A at 100 DEG C after ball milling mixing is uniform；Powder A is put into
1h is calcined at 900 DEG C in Muffle furnace, cools to room temperature with the furnace, obtained product is sufficiently cleaned through deionized water, is removed
NaCl and KCl obtains pre-reaction material B after dry at 100 DEG C；0.15g pre-reaction material B is put into beaker, is added
40ml deionized water, and the hydrochloric acid that 1ml mass fraction is 36.5% is added, ultrasonic 0.5h obtains mixture C；By mixture C
3h is heated at 100 DEG C, obtains TiO after dry2/ BiOCl hetero-junctions powder.
With above-mentioned photocatalytic activity evaluation method, after radiation of visible light 40min, TiO2/ manufactured in the present embodiment
BiOCl hetero-junctions is about 88% to the degradation rate of rhodamine B, and commercial titanium dioxide (P25) is to rhodamine B under the same terms
Degradation rate be 17%, BiOCl be 31% to the degradation rate of rhodamine B, it was demonstrated that TiO manufactured in the present embodiment2/ BiOCl is heterogeneous
The visible light catalytic performance of knot is much better than single commercial TiO2(P25) and BiOCl.
Embodiment 6:
Weigh the Bi of 2.36g2O3, 0.61g TiO2, 8.95g KCl and 7.01g NaCl, place it in ball grinder
And 60ml dehydrated alcohol is added, mixing and ball milling 3h is dried to obtain powder A at 90 DEG C after ball milling mixing is uniform；Powder A is put into
1h is calcined at 1000 DEG C in Muffle furnace, cools to room temperature with the furnace, obtained product is sufficiently cleaned through deionized water, is removed
NaCl and KCl obtains pre-reaction material B after dry at 90 DEG C；0.2g pre-reaction material B is put into beaker, is added
60ml deionized water, and the hydrochloric acid that 2.5ml mass fraction is 36.5% is added, ultrasonic 1h obtains mixture C；Mixture C is existed
4h is heated at 100 DEG C, obtains TiO after dry2/ BiOCl hetero-junctions powder.
With above-mentioned photocatalytic activity evaluation method, after radiation of visible light 40min, TiO2/ manufactured in the present embodiment
BiOCl hetero-junctions is about 85% to the degradation rate of rhodamine B, and commercial titanium dioxide (P25) is to rhodamine B under the same terms
Degradation rate be 17%, BiOCl be 31% to the degradation rate of rhodamine B, it was demonstrated that TiO manufactured in the present embodiment2/ BiOCl is heterogeneous
The visible light catalytic performance of knot is much better than single commercial TiO2(P25) and BiOCl.
Embodiments of the present invention are simultaneously not restricted by the embodiments, other any real without departing from spirit of the invention
Made changes, modifications, substitutions, combinations, simplifications under matter and principle, should be equivalent substitute mode, are included in the present invention
Protection scope within.
Claims (7)
1. a kind of TiO2The preparation method of/BiOCl hetero-junctions visible light catalyst, it is characterised in that the following steps are included:
1) in Bi2O3、TiO2, dehydrated alcohol is added in NaCl and KCl powder mixture, mixing is milled, after mixing mixture
It is dried to obtain powder A；The molar ratio of the KCl and NaCl is 1:1 ~ 2:1；The Bi2O3Molar ratio with KCl is 1:50 ~ 1:
20；The Bi2O3With TiO2Molar ratio be 2:3 ~ 11:15；
2) powder A is calcined to 0.5 ~ 2h at 750 ~ 1100 DEG C, cools to room temperature with the furnace, it is obtained product is washed, dry
Afterwards, pre-reaction material B is obtained；
3) it drives in object B before the reaction and deionized water is added, and hydrochloric acid is added, be ultrasonically treated 0.2 ~ 1h, obtain mixture C；According to
Mass concentration meter, the concentration of the hydrochloric acid are 36.5%；
4) mixture C is heated to 2 ~ 4h at 100 ~ 120 DEG C, obtains TiO2/ BiOCl hetero-junctions powder.
2. TiO according to claim 12The preparation method of/BiOCl hetero-junctions visible light catalyst, which is characterized in that institute
It states mixing to mill to carry out by ball milling, the time of ball milling is 2 ~ 5h.
3. TiO according to claim 12The preparation method of/BiOCl hetero-junctions visible light catalyst, which is characterized in that step
Rapid temperature dry 1) and described in step 2 is 80 DEG C ~ 100 DEG C.
4. TiO according to claim 12The preparation method of/BiOCl hetero-junctions visible light catalyst, which is characterized in that step
It is rapid 1) in every gram of TiO2It is added dehydrated alcohol 50-200 milliliters.
5. TiO according to claim 12The preparation method of/BiOCl hetero-junctions visible light catalyst, which is characterized in that step
Rapid 2) the described washing is that deionized water is sufficiently cleaned to remove NaCl and KCl.
6. TiO according to claim 12The preparation method of/BiOCl hetero-junctions visible light catalyst, which is characterized in that step
Rapid 3) the described pre-reaction material B and the mass ratio of deionized water are 1/300 ~ 1/100.
7. TiO according to claim 12The preparation method of/BiOCl hetero-junctions visible light catalyst, which is characterized in that institute
The volume ratio for stating hydrochloric acid and deionized water is 1:60 ~ 1:20.
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| CN113856659B (en) * | 2021-10-27 | 2024-04-05 | 合肥工业大学 | N-doped TiO modified by BiOCl nanosheets 2 Method for preparing nanotube array |
| CN115155624B (en) * | 2022-08-09 | 2024-05-03 | 深圳市康弘智能健康科技股份有限公司 | Heterojunction composite material for removing aldehyde through visible light catalysis, preparation method of heterojunction composite material and method for degrading VOCs through visible light catalysis |
| CN115536276B (en) * | 2022-09-19 | 2023-09-26 | 中国科学院赣江创新研究院 | Antibacterial microcrystalline glass ceramic, preparation method thereof, antibacterial regeneration method and application |
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