CN109433186A - A kind of WO3The preparation and experimental method of/ZnO composite photo-catalyst - Google Patents
A kind of WO3The preparation and experimental method of/ZnO composite photo-catalyst Download PDFInfo
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- CN109433186A CN109433186A CN201811373731.5A CN201811373731A CN109433186A CN 109433186 A CN109433186 A CN 109433186A CN 201811373731 A CN201811373731 A CN 201811373731A CN 109433186 A CN109433186 A CN 109433186A
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- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 35
- 238000002474 experimental method Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 10
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000001110 calcium chloride Substances 0.000 claims abstract description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 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 claims description 18
- 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 claims description 16
- 229940012189 methyl orange Drugs 0.000 claims description 16
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000002835 absorbance Methods 0.000 claims description 9
- 238000010521 absorption reaction Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000011701 zinc Substances 0.000 claims description 8
- 238000004458 analytical method Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 6
- 238000005286 illumination Methods 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 238000005070 sampling Methods 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 229910020347 Na2WO3 Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000031700 light absorption Effects 0.000 claims description 3
- 238000013507 mapping Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000002371 ultraviolet--visible spectrum Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 238000000862 absorption spectrum Methods 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 238000006731 degradation reaction Methods 0.000 abstract description 11
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 238000001354 calcination Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 3
- 238000001556 precipitation Methods 0.000 abstract description 3
- 238000010183 spectrum analysis Methods 0.000 abstract description 3
- 238000003911 water pollution Methods 0.000 abstract description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910003893 H2WO4 Inorganic materials 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002906 microbiologic effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/30—Tungsten
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
- C02F2101/34—Organic compounds containing oxygen
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- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
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- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a kind of WO3The preparation method of/ZnO composite photo-catalyst, specifically includes the following steps: a1, at normal temperature, takes 50mL, the CaCl of 1mol/L2Solution is added in there-necked flask, then takes 50mL, the Na of 0.2mol/L2WO3·2H2O is added to CaCl2In solution, then white precipitate being generated immediately, being reacted in the water-bath for being immediately placed in 80 DEG C after ten minutes in room temperature, and be put into 40mL, the HCl solution of 2mol/L, reaction can become faint yellow afterwards a little while, can finally become yellow, be related to water-treatment technology field.The WO3The two is mixed on this basis and calcining obtains WO in Muffle furnace, it can be achieved that be prepared for yellow wolframic acid and basic zinc carbonate by using direct precipitation method by preparation and the experimental method of/ZnO composite photo-catalyst3The composite material of/ZnO, while the WO3/ZnO composite photo-catalyst effect obtained by ultraviolet spectral analysis and after calcining 2h hours in Muffle furnace is more preferable, it is possible to so that composite photo-catalyst is improved degradation rate, outstanding contributions are had for improvement such as water pollutions.
Description
Technical field
The present invention relates to water-treatment technology field, specially a kind of WO3The preparation of/ZnO composite photo-catalyst and experiment side
Method.
Background technique
In recent years, modern times rapid industrial development also brings many environment and energy problem simultaneously, such as: waste water,
Disorderly row leaves about for exhaust gas, waste residue, and the conventional method that China handles this problem at present has physisorphtion, microbiological treatment technology
Deng, but this traditional method cannot efficiently and completely go to solve this problem of environmental pollution, and be easy to cause secondary dirt
Dye, so in order to better solve this problem of water environment pollution, Photocatalitic Technique of Semiconductor is gradually suggested.
In numerous nano semiconductor materials, it is believed that the catalytic efficiency highest and its application range of TiO2 when beginning
It is most wide, in recent years in the research to all types of inorganic semiconductor materials photocatalytic of the discovery than TiO2 preferably one is
ZnO, but since ZnO forbidden bandwidth is higher, application is greatly limited, therefore Recent study improves from many aspects
The paper of the photocatalysis performance of ZnO is increasing, so by WO3Compound its light that can dramatically improve is carried out with ZnO to urge
Change property, shows that composite material has higher catalytic activity than single nano material.
Yellow wolframic acid and basic zinc carbonate are prepared for using direct precipitation method in this paper, on this basis mix the two simultaneously
Calcining obtains WO in Muffle furnace3The composite material of/ZnO, is obtained by ultraviolet spectral analysis: being calcined 2h hours in Muffle furnace
The WO3/ZnO composite photo-catalyst effect obtained afterwards is more preferable, it is possible to so that composite photo-catalyst is improved degradation rate, for water dirt
The improvement such as dye have outstanding contributions.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of WO3The preparation of/ZnO composite photo-catalyst and experiment side
Method, it is poor to solve existing nano-photocatalyst catalytic effect, cannot question number degradation rate significantly, to can not be carried out to water pollution
The problem of improving very well.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs: a kind of WO3/ ZnO composite photo-catalyst
Preparation method, specifically includes the following steps:
A1, at normal temperature, takes 50mL, the CaCl of 1mol/L2Solution is added in there-necked flask, then takes 50mL, 0.2mol/L
Na2WO3·2H2O is added to CaCl2In solution, then white precipitate is generated immediately, react in room temperature and put immediately after ten minutes
Enter in 80 DEG C of water-bath, and be put into 40mL, the HCl solution of 2mol/L, reaction can become faint yellow afterwards a little while, can finally become
For yellow, electric stirring, which reacts to take out after 2.5 hours to be put into bottle,suction, filter with vacuum pump using circulatory water and with distilling
Sample is finally put into drying in 80 DEG C of air dry oven and obtains sample after 2 hours, ground after taking-up by water washing 2-3 times
Mill, can be obtained yellow wolframic acid H2WO4Sample；
A2,50mL, the Zn (NO of 0.2mol are taken3)2It is added in there-necked flask with the CTAB of 10mL, 0.02mol/L, separately takes
The Na of 50mL, 0.3mol/L2CO3It is added to Zn (NO3)2In solution, takes out and put after electric stirring 2 hours in constant water bath box
Enter in bottle,suction and filtered and be washed with distilled water 2-3 times with vacuum pump using circulatory water, sample is finally put into 80 DEG C of air blast
It obtains sample within dry 2 hours in drying box, is ground after taking-up, basic zinc carbonate ZnCO can be obtained3Sample；
A3, the yellow wolframic acid H for obtaining a12WO4The basic zinc carbonate ZnCO obtained with a23It is put after being ground by equal mass mixings
Enter and obtains WO after calcining 1 hour in 500 DEG C of Muffle furnace3/ ZnO composite photo-catalyst will be changed to respectively 1.5h later the time,
2h, 2.5h, 3h repeat above step and five groups of different WO are made3/ ZnO composite photocatalyst sample.
Preferably, Muffle furnace used in the step a3 is electric furnace heating wire Muffle furnace, can control rated temperature at 1000 DEG C
Below.
The invention also discloses a kind of WO3The experimental method of/ZnO composite photo-catalyst, specifically includes the following steps:
B1, first precise 25mg methyl orange are added a certain amount of distilled water and make it dissolve in beaker, after be transferred to
It is configured to the methyl orange solution of 100ppm in the volumetric flask of 250mL, then takes a certain amount of WO3/ ZnO composite photocatalyst sample is put
Enter in beaker, the methyl orange of 10mL concentration 100ppm is then taken to be added in beaker, adds 90mL distilled water and form the outstanding of sample
Turbid；
B2, the suspension ultrasonic disperse 5min for later obtaining b1, are uniformly distributed powder using ultrasonic wave, are formed
After the methyl orange solution of 10mg/L, the first sub-sampling is carried out with magnetic stirrer 30min in darkroom, then beaker is put into
With under the fluorescent lamp of 500W, illumination is carried out to it, the distance of holding light source to liquid is 20cm, in this process every 0.5h
It is sampled, takes four times, then sampled every 1h, taken twice, about measure 3mg every time；
B3, it is then left away the sample dispersed in methyl orange with centrifuge, the methyl orange solution after taking supernatant to be degraded,
It is measured with solution of the ultraviolet-uisible spectrophotometer to acquisition, and then measures the absorbance of methyl orange solution characteristic absorption peak
Value repeats experimental procedure, finishes until five groups of samples measure, ultimate analysis experimental data.
It preferably, the use of the ultraviolet-visible spectrum analysis of ultraviolet-uisible spectrophotometer is characterization material in the step b3
A kind of most popular method of absorbing properties, allows the light successively permeable material of different wave length, measures substance under each wavelength respectively
To the degree of absorption of light, then using absorbance as ordinate, wavelength is abscissa mapping, and obtained curve is the suction of the substance
Receive spectrum.
(3) beneficial effect
The present invention provides a kind of WO3The preparation and experimental method of/ZnO composite photo-catalyst.Have compared with prior art
It is standby following the utility model has the advantages that the WO3The preparation and experimental method of/ZnO composite photo-catalyst, specifically includes the following steps: a1, normal
Under temperature, 50mL, the CaCl of 1mol/L are taken2Solution is added in there-necked flask, then takes 50mL, the Na of 0.2mol/L2WO3·2H2O adds
Enter to CaCl2In solution, then white precipitate is generated immediately, react in room temperature and be immediately placed in 80 DEG C of water-bath after ten minutes
In, and it is put into 40mL, the HCl solution of 2mol/L, reaction can become faint yellow afterwards a little while, a2, take 50mL, the Zn of 0.2mol
(NO3)2It is added in there-necked flask with the CTAB of 10mL, 0.02mol/L, separately takes 50mL, the Na of 0.3mol/L2CO3It is added to Zn
(NO3)2In solution, takes out to be put into bottle,suction after electric stirring 2 hours in constant water bath box and be taken out with vacuum pump using circulatory water
It filters and is washed with distilled water 2-3 times, a3, the yellow wolframic acid H for obtaining a12WO4The basic zinc carbonate ZnCO obtained with a23By etc. matter
It is put into after amount mixed grinding after being calcined 1 hour in 500 DEG C of Muffle furnace and obtains WO3/ ZnO composite photo-catalyst, later by the time
It is changed to 1.5h, 2h, 2.5h, 3h respectively, repeats above step and five groups of different WO is made3/ ZnO composite photocatalyst sample, tool
Body the following steps are included: b1, first precise 25mg methyl orange in beaker, are added a certain amount of distilled water and make it dissolve, after
It is transferred to the methyl orange solution for being configured to 100ppm in the volumetric flask of 250mL, then takes a certain amount of WO3/ ZnO composite photo-catalyst
Sample is put into beaker, and the methyl orange of 10mL concentration 100ppm is then taken to be added in beaker, is added 90mL distilled water and is formed sample
The suspension of product, b2, the suspension ultrasonic disperse 5min for later obtaining b1, is uniformly distributed powder using ultrasonic wave, is formed
After the methyl orange solution of 10mg/L, the first sub-sampling is carried out with magnetic stirrer 30min in darkroom, then beaker is put into
With under the fluorescent lamp of 500W, illumination is carried out to it, the distance of holding light source to liquid is 20cm, in this process every 0.5h
It is sampled, takes four times, then sampled every 1h, taken twice, about measure 3mg every time, b3, then left away methyl orange with centrifuge
The sample of middle dispersion, the methyl orange solution after taking supernatant to be degraded, with ultraviolet-uisible spectrophotometer to the solution of acquisition
It is measured, and then measures the absorbance value of methyl orange solution characteristic absorption peak, repeat experimental procedure, until five groups of samples measure
It finishes, ultimate analysis experimental data is, it can be achieved that be prepared for yellow wolframic acid and basic zinc carbonate by using direct precipitation method, in this base
The two is mixed on plinth and calcining obtains WO in Muffle furnace3The composite material of/ZnO, at the same by ultraviolet spectral analysis and
The WO3/ZnO composite photo-catalyst effect obtained after calcining 2h hours in Muffle furnace is more preferable, it is possible to make composite photo-catalyst
Degradation rate is improved, outstanding contributions are had for improvement such as water pollutions.
Detailed description of the invention
Fig. 1 is the ultraviolet figure figure of gained sample Photodegradation of Methyl Orange under 2h of the present invention；
Fig. 2 is the calculation formula figure of degradation rate of the present invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The embodiment of the present invention provides a kind of technical solution referring to FIG. 1-2: a kind of WO3The system of/ZnO composite photo-catalyst
Preparation Method, specifically includes the following steps:
A1, at normal temperature, takes 50mL, the CaCl of 1mol/L2Solution is added in there-necked flask, then takes 50mL, 0.2mol/L
Na2WO3·2H2O is added to CaCl2In solution, then white precipitate is generated immediately, react in room temperature and put immediately after ten minutes
Enter in 80 DEG C of water-bath, and be put into 40mL, the HCl solution of 2mol/L, reaction can become faint yellow afterwards a little while, can finally become
For yellow, electric stirring, which reacts to take out after 2.5 hours to be put into bottle,suction, filter with vacuum pump using circulatory water and with distilling
Sample is finally put into drying in 80 DEG C of air dry oven and obtains sample after 2 hours, ground after taking-up by water washing 2-3 times
Mill, can be obtained yellow wolframic acid H2WO4Sample；
A2,50mL, the Zn (NO of 0.2mol are taken3)2It is added in there-necked flask with the CTAB of 10mL, 0.02mol/L, separately takes
The Na of 50mL, 0.3mol/L2CO3It is added to Zn (NO3)2In solution, takes out and put after electric stirring 2 hours in constant water bath box
Enter in bottle,suction and filtered and be washed with distilled water 2-3 times with vacuum pump using circulatory water, sample is finally put into 80 DEG C of air blast
It obtains sample within dry 2 hours in drying box, is ground after taking-up, basic zinc carbonate ZnCO can be obtained3Sample；
A3, the yellow wolframic acid H for obtaining a12WO4The basic zinc carbonate ZnCO obtained with a23It is put after being ground by equal mass mixings
Enter and obtains WO after calcining 1 hour in 500 DEG C of Muffle furnace3/ ZnO composite photo-catalyst will be changed to respectively 1.5h later the time,
2h, 2.5h, 3h repeat above step and five groups of different WO are made3/ ZnO composite photocatalyst sample.
In the present invention, Muffle furnace used in step a3 be electric furnace heating wire Muffle furnace, can control rated temperature 1000 DEG C with
Under.
The invention also discloses a kind of WO3The experimental method of/ZnO composite photo-catalyst, specifically includes the following steps:
B1, first precise 25mg methyl orange are added a certain amount of distilled water and make it dissolve in beaker, after be transferred to
It is configured to the methyl orange solution of 100ppm in the volumetric flask of 250mL, then takes a certain amount of WO3/ ZnO composite photocatalyst sample is put
Enter in beaker, the methyl orange of 10mL concentration 100ppm is then taken to be added in beaker, adds 90mL distilled water and form the outstanding of sample
Turbid；
B2, the suspension ultrasonic disperse 5min for later obtaining b1, are uniformly distributed powder using ultrasonic wave, are formed
After the methyl orange solution of 10mg/L, the first sub-sampling is carried out with magnetic stirrer 30min in darkroom, then beaker is put into
With under the fluorescent lamp of 500W, illumination is carried out to it, the distance of holding light source to liquid is 20cm, in this process every 0.5h
It is sampled, takes four times, then sampled every 1h, taken twice, about measure 3mg every time；
B3, it is then left away the sample dispersed in methyl orange with centrifuge, the methyl orange solution after taking supernatant to be degraded,
It is measured with solution of the ultraviolet-uisible spectrophotometer to acquisition, and then measures the absorbance of methyl orange solution characteristic absorption peak
Value repeats experimental procedure, finishes until five groups of samples measure, ultimate analysis experimental data.
In the present invention, the ultraviolet-visible spectrum analysis in step b3 using ultraviolet-uisible spectrophotometer is characterization material light
A kind of most popular method of absorbent properties, allows the light successively permeable material of different wave length, measures substance pair under each wavelength respectively
The degree of absorption of light, then using absorbance as ordinate, wavelength is abscissa mapping, and obtained curve is the absorption of the substance
Spectrum is analyzed by carrying out ultraviolet-uisible spectrophotometer to the methyl orange after sample degradation in this experiment, is passed through
Its degradation rate is calculated using formula, it can be deduced that the sample prepared under which has highest photocatalytic activity, Fig. 2 time
In formula: A0, At are respectively that for methyl orange solution in the absorbance of maximum absorption wave strong point, Fig. 1 is most upper before illumination and after the illumination t time
One line in face is the ultraviolet-visible absorption spectroscopy of methyl orange degradation 0.5h, and the absorption peak of methyl orange solution exists as seen from the figure
At 470nm, apparent variation is had occurred in the characteristic absorption peak of solution in degradation process, with the increase of light application time, degradation rate
It is gradually increased；With the progress of reaction, the absorbance of methyl orange is gradually decreased, i.e., concentration reduces, and is calculated by Fig. 2 formula
The degradation rate of gained sample is 25.7% under 3h.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (4)
1. a kind of WO3The preparation method of/ZnO composite photo-catalyst, it is characterised in that: specifically includes the following steps:
A1, at normal temperature, takes 50mL, the CaCl of 1mol/L2Solution is added in there-necked flask, then takes 50mL, 0.2mol/L's
Na2WO3·2H2O is added to CaCl2In solution, then white precipitate is generated immediately, react in room temperature and be immediately placed in after ten minutes
In 80 DEG C of water-bath, and it is put into 40mL, the HCl solution of 2mol/L, reaction can become faint yellow afterwards a little while, can finally become
Yellow, taking-up, which is put into bottle,suction, after electric stirring 2.5 hours of reaction is filtered with vacuum pump using circulatory water and uses distilled water
Sample is finally put into drying in 80 DEG C of air dry oven and obtains sample after 2 hours, ground after taking-up by washing 2-3 times,
Yellow wolframic acid H can be obtained2WO4Sample；
A2,50mL, the Zn (NO of 0.2mol are taken3)2It is added in there-necked flask with the CTAB of 10mL, 0.02mol/L, separately takes 50mL,
The Na of 0.3mol/L2CO3It is added to Zn (NO3)2In solution, is taken out after electric stirring 2 hours in constant water bath box and be put into suction filtration
It is filtered and is washed with distilled water 2-3 times with vacuum pump using circulatory water in bottle, sample is finally put into 80 DEG C of air dry oven
Middle drying obtains sample for 2 hours, grinds after taking-up, and basic zinc carbonate ZnCO can be obtained3Sample；
A3, the yellow wolframic acid H for obtaining a12WO4The basic zinc carbonate ZnCO obtained with a23500 are put into after grinding by equal mass mixings
DEG C Muffle furnace in calcine 1 hour after obtain WO3/ ZnO composite photo-catalyst will be changed to respectively 1.5h, 2h later the time,
2.5h, 3h repeat above step and five groups of different WO are made3/ ZnO composite photocatalyst sample.
2. a kind of WO according to claim 13The preparation and experimental method of/ZnO composite photo-catalyst, it is characterised in that: institute
Stating Muffle furnace used in step a3 is electric furnace heating wire Muffle furnace, can control rated temperature at 1000 DEG C or less.
3. a kind of WO according to claim 13The experimental method of/ZnO composite photo-catalyst, it is characterised in that: specifically include
Following steps:
B1, first precise 25mg methyl orange are added a certain amount of distilled water and make it dissolve in beaker, after be transferred to 250mL
Volumetric flask in be configured to the methyl orange solution of 100ppm, then take a certain amount of WO3/ ZnO composite photocatalyst sample is put into burning
In cup, the methyl orange of 10mL concentration 100ppm is then taken to be added in beaker, adds the suspension that 90mL distilled water forms sample；
B2, the suspension ultrasonic disperse 5min for later obtaining b1, are uniformly distributed powder using ultrasonic wave, form 10mg/L's
After methyl orange solution, the first sub-sampling is carried out with magnetic stirrer 30min in darkroom, then beaker is put into 500W's
Under fluorescent lamp, illumination is carried out to it, the distance of holding light source to liquid is 20cm, is taken in this process every 0.5h
Sample takes four times, then samples every 1h, takes twice, about measures 3mg every time；
B3, it is then left away the sample dispersed in methyl orange with centrifuge, the methyl orange solution after taking supernatant to be degraded, with purple
Outer visible spectrophotometer is measured the solution of acquisition, and then measures the absorbance value of methyl orange solution characteristic absorption peak,
Experimental procedure is repeated, is finished until five groups of samples measure, ultimate analysis experimental data.
4. a kind of WO according to claim 33The preparation and experimental method of/ZnO composite photo-catalyst, it is characterised in that: institute
Stating the ultraviolet-visible spectrum analysis in step b3 using ultraviolet-uisible spectrophotometer is to characterize one kind of material absorbing properties
Most popular method, allows the light successively permeable material of different wave length, measures substance under each wavelength respectively to the degree of absorption of light, so
Afterwards using absorbance as ordinate, wavelength is abscissa mapping, and obtained curve is the absorption spectrum of the substance.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101703948A (en) * | 2009-12-02 | 2010-05-12 | 淮北煤炭师范学院 | Novel method for preparing compound high-activity photocatalyst |
| CN103894183A (en) * | 2014-04-14 | 2014-07-02 | 河北工程大学 | Preparation method for energy storage type WO3/ZnO composite photocatalyst |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101703948A (en) * | 2009-12-02 | 2010-05-12 | 淮北煤炭师范学院 | Novel method for preparing compound high-activity photocatalyst |
| CN103894183A (en) * | 2014-04-14 | 2014-07-02 | 河北工程大学 | Preparation method for energy storage type WO3/ZnO composite photocatalyst |
Non-Patent Citations (2)
| Title |
|---|
| YU CHANGLIN等: "Preparation of WO3/ZnO Composite Photocatalyst and Its Photocatalytic Performance", 《CHINESE JOURNAL OF CATALYSIS》 * |
| 印协世: "《钨丝生产原理、工艺及其性能》", 31 May 1998, 冶金工业出版社 * |
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