CN107020080A - A kind of WO3Visible-light photocatalyst and its preparation and application - Google Patents
A kind of WO3Visible-light photocatalyst and its preparation and application Download PDFInfo
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- CN107020080A CN107020080A CN201710304761.XA CN201710304761A CN107020080A CN 107020080 A CN107020080 A CN 107020080A CN 201710304761 A CN201710304761 A CN 201710304761A CN 107020080 A CN107020080 A CN 107020080A
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- hexamethylenetetramine
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 17
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 84
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 39
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 39
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 230000015556 catabolic process Effects 0.000 claims abstract description 18
- 238000006731 degradation reaction Methods 0.000 claims abstract description 18
- 229910003893 H2WO4 Inorganic materials 0.000 claims abstract description 17
- 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 abstract description 13
- 229940012189 methyl orange Drugs 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 238000007654 immersion Methods 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000007605 air drying Methods 0.000 claims description 8
- 239000002351 wastewater Substances 0.000 claims description 6
- 239000000975 dye Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 230000003197 catalytic effect Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 9
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 238000004134 energy conservation Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 32
- 230000003760 hair shine Effects 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 4
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000010919 dye waste Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- VOZKAJLKRJDJLL-UHFFFAOYSA-N 2,4-diaminotoluene Chemical compound CC1=CC=C(N)C=C1N VOZKAJLKRJDJLL-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of WO3Visible-light photocatalyst and its preparation and application, H2WO4Calcined at different temperatures after being pre-processed through hexamethylenetetramine solution.What is prepared concretely comprises the following steps：(1) hexamethylenetetramine solution is prepared, (2) take the hexamethylenetetramine solution prepared in step (1), by H2WO4It is soaked in hexamethylenetetramine solution after certain time, washs, dries, then calcine at different temperatures.It was found that the WO prepared under non-calcination condition3Visible-light photocatalyst, with higher photocatalytic activity.Under the irradiation of 8w fluorescent lamps, after 8h, the degradation rate about 67% of methyl orange.The preparation method of this catalyst has the effect of energy-conservation.
Description
Technical field
The present invention relates to a kind of WO3The technology of preparing of photochemical catalyst.Pass through methyl orange of degrading, it was demonstrated that it has excellent visible
The effect of light photocatalytic degradation organic wastewater.
Background technology
In recent years, developing rapidly with dye industry, the discharge of waste water from dyestuff is also more and more.These waste water from dyestuff have
By colourity it is big, constitute complicated, content of organics height, environmental pollution is big the features such as, it is difficult to find efficient processing method.Industrially
Conventional dye waste water treatment method has flocculent precipitation, absorption method, bioanalysis, photocatalytic oxidation degradation method etc..Wherein, apply
The features such as semiconductor catalyst photocatalysis degradation organic contaminant has low energy consumption, high easy to operate, degradation efficiency, non-secondary pollution
And attract attention, the focus studied as environment in recent years pollutant abatement technology.
Semiconductor plays very important effect in photocatalytic degradation of dye waste water：(1) semiconductor is in photochemical catalytic oxidation
Technical field has the advantages that simple to operate, reaction condition is gentle, energy consumption is low and secondary pollution is few, thus in field of waste water treatment
Receive much concern；(2)WO3It is a kind of energy gap about 2.5-2.8eV n-type semiconductor, main absorb is less than 443nm wavelength
Light, stability is good；(3)WO3The organic pollutions such as energy efficient degradation waste water, environmental pollution is small, cheap.And with regard to ring
For the purification of border, also there is very big application value for the interior without ultraviolet light.
Main component is visible ray in sunshine, and ultraviolet light composition only accounts for 5% or so.Therefore, it is lower under visible light to degrade
Waste water from dyestuff has significant practical significance to improve the health of environmental quality and the mankind.
The content of the invention
An object of the present invention is to provide a kind of WO3Visible-light photocatalyst.
The second object of the present invention is to provide a kind of above-mentioned WO3The preparation method of visible-light photocatalyst, this method section
Can and it is simple and easy to apply, it is not necessary to the equipment of complex and expensive.
Technical scheme
A kind of WO3Visible-light photocatalyst, by (20-200ml) hexamethylenetetramine solution and (2-20g) H2WO4Immersion and
Into optimal immersion is than being 10:1.
A kind of above-mentioned WO3The preparation method of visible-light photocatalyst, is concretely comprised the following steps：
(1) the hexamethylenetetramine solution prepared, that is, weigh a certain amount of C6H12N4, appropriate deionized water is added, so
Side 30min is stirred afterwards, is subsequently transferred in 100mL volumetric flask.
(2) with hexamethylenetetramine solution pretreatment H obtained by step (1)2WO4, i.e., above-mentioned six methine is taken by a certain percentage
Four amine aqueous solutions and H2WO4In beaker, 20-28h is soaked, is washed with absolute ethyl alcohol and deionized water, natural air drying, Ran Hou
WO can be made by calcining and not calcining down for 300-700 DEG C3。
Beneficial effects of the present invention：
A kind of WO of the present invention3Visible-light photocatalyst, due to WO3Band-gap energy it is smaller, be 2.5-2.8eV, in visible ray
Lower energy efficient degradation organic pollution, environmental pollution is small, cheap.For the interior without ultraviolet light also have it is very big should
With value.
It was found that the WO prepared under non-calcination condition3Visible-light photocatalyst, with higher photocatalytic activity.On 8w
Under the irradiation of light lamp, after 8h, the degradation rate about 67% of methyl orange.The preparation method of this catalyst has the effect of energy-conservation.
Further, a kind of WO of the invention3The preparation method of visible-light photocatalyst is saved and simple and easy to apply, it is not necessary to multiple
Miscellaneous expensive equipment, is easy to large-scale production.
Brief description of the drawings
Fig. 1 .WO3XRD；
WO under Fig. 2 visible rays3To the degradation effect figure of methyl orange solution.
Embodiment
Invention will be further elaborated by specific embodiment below.
Embodiment 1
The hexamethylenetetramine solution of preparation, that is, weigh a certain amount of C6H12N4, appropriate deionized water is added, is then stirred
30min is mixed, is subsequently transferred in 100mL volumetric flask, hexamethylenetetramine solution concentration is obtained for 40g/ml.Take six first of 50ml
Urotropine solution and 5gH2WO4In beaker, 24h is soaked, is washed respectively with absolute ethyl alcohol and deionized water, natural air drying is dried,
Produce WO3。
It can be seen that without calcining gained WO after pretreatment from Fig. 1 XRD3。
Take the methyl orange solution 50ml that initial concentration is 20mg/L in 100ml beakers, be separately added into after pretreatment not
Photochemical catalyst 0.1g and 0.5ml30% hydrogen peroxide are calcined, it is well mixed with glass bar stirring, is then placed in ultrasonic wave clear
Device ultrasound 5min is washed, 30min is stirred, is constantly stirred with 8w daylight light irradiation, takes supernatant a little every 2h, uses light splitting light
Degree meter measurement methyl orange solution absorbance.Finally calculate degradation rates of its 8h to methyl orange.
Embodiment 2
The hexamethylenetetramine solution of preparation, that is, weigh a certain amount of C6H12N4, appropriate deionized water is added, is then stirred
30min is mixed, is subsequently transferred in 100mL volumetric flask, hexamethylenetetramine solution concentration is obtained for 20g/ml.Take six first of 50ml
Urotropine solution and 5gH2WO4In beaker, 24h is soaked, is washed respectively with absolute ethyl alcohol and deionized water, natural air drying is dried,
Produce WO3。
After 8w visible ray shines 8h, hexamethylenetetramine solution immersion H2WO4WO is made under non-calcination condition afterwards3It is right
The degradation rate of methyl orange about 50%.
Embodiment 3
The hexamethylenetetramine solution of preparation, that is, weigh a certain amount of C6H12N4, appropriate deionized water is added, is then stirred
30min is mixed, is subsequently transferred in 100mL volumetric flask, hexamethylenetetramine solution concentration is obtained for 40g/ml.Take six first of 50ml
Urotropine solution and 10gH2WO4In beaker, 24h is soaked, is washed respectively with absolute ethyl alcohol and deionized water, natural air drying is done
It is dry, produce WO3。
After 8w visible ray shines 8h, hexamethylenetetramine solution immersion H2WO4WO is made under non-calcination condition afterwards3It is right
The degradation rate of methyl orange about 48%.
Embodiment 4
The hexamethylenetetramine solution of preparation, that is, weigh a certain amount of C6H12N4, appropriate deionized water is added, is then stirred
30min is mixed, is subsequently transferred in 100mL volumetric flask, hexamethylenetetramine solution concentration is obtained for 40g/ml.Take six first of 50ml
Urotropine solution and 5gH2WO4In beaker, 20h is soaked, is washed respectively with absolute ethyl alcohol and deionized water, natural air drying is dried,
Produce WO3。
After 8w visible ray shines 8h, hexamethylenetetramine solution immersion H2WO4WO is made under non-calcination condition afterwards3It is right
The degradation rate of methyl orange about 53%.
Embodiment 5
The hexamethylenetetramine solution of preparation, that is, weigh a certain amount of C6H12N4, appropriate deionized water is added, is then stirred
30min is mixed, is subsequently transferred in 100mL volumetric flask, hexamethylenetetramine solution concentration is obtained for 40g/ml.Take six first of 50ml
Urotropine solution and 5gH2WO4In beaker, 24h is soaked, is washed respectively with absolute ethyl alcohol and deionized water, natural air drying is dried,
Produce WO3。
After 8w visible ray shines 8h, hexamethylenetetramine solution immersion H2WO4WO is made under non-calcination condition afterwards3It is right
The degradation rate of methyl orange about 67%.
WO under visible ray as can be seen from Figure 23To the degradation effect figure of methyl orange.
It can be found that hexamethylenetetramine solution concentration is 40g/ml from Fig. 2, hexamethylenetetramine solution immersion H2WO4
Time is 24h, hexamethylenetetramine solution and H2WO4Immersion is than being 10ml：1g, spontaneously dries obtained WO3To the drop of methyl orange
Solution rate highest, after 8w visible ray shines 8h, about 67%.
Embodiment 6
The hexamethylenetetramine solution of preparation, that is, weigh a certain amount of C6H12N4, appropriate deionized water is added, is then stirred
30min is mixed, is subsequently transferred in 100mL volumetric flask, hexamethylenetetramine solution concentration is obtained for 40g/ml.Take six first of 50ml
Urotropine solution and 5gH2WO4In beaker, 24h is soaked, is washed respectively with absolute ethyl alcohol and deionized water, natural air drying is dried,
After drying WO is produced in 300-700 DEG C of calcining3。
It can be seen that through calcining gained WO after pretreatment from Fig. 1 XRD3。
WO under visible ray as can be seen from Figure 23To the degradation effect figure of methyl orange.
From Fig. 2 it can be found that after 8w visible ray shines 8h, its degraded to methyl orange is raised with calcining heat
Rate is gradually reduced.
Embodiment 7
Be the same as Example 6, difference from Example 6 is, WO is produced in 50-250 DEG C of calcining after drying3.It is to methyl
It is consistent substantially when the degradation rate of orange is not with calcining.
It is 40g/ml, hexamethylenetetramine solution immersion H in hexamethylenetetramine solution concentration2WO4Time is 24h, six times
Tetramine solution and H2WO4Immersion is than being 10ml：1g, illustrates that hexamethylenetetramine solution soaks H2WO4Afterwards in non-calcination condition
WO is made down3To the degradation rate highest of methyl orange, about 67%, illustrate the WO prepared under non-calcination condition3Photocatalytic activity most
Height, this achievement in research has the effect of energy-conservation.
Claims (9)
1. a kind of WO3Visible-light photocatalyst, it is characterised in that：It is by H2WO4Formed after being soaked through hexamethylenetetramine solution
WO3Visible-light photocatalyst.
2. the WO described in a kind of claim 13The preparation method of visible-light photocatalyst, it is characterised in that：Described WO3It can be seen that
Light photochemical catalyst is by H2WO4The WO formed after being soaked through hexamethylenetetramine solution3。
3. according to the preparation method described in claim 2, it is characterised in that：Specific immersion process is, by 2-20g H2WO4Immersion
The WO formed in 20-200ml hexamethylenetetramine solution3, hexamethylenetetramine solution concentration is 10-80g/ml.
4. according to the WO described in claim 33The preparation method of visible-light photocatalyst, it is characterised in that：Hexamethylenetetramine is molten
Liquid and H2WO4Optimal immersion is than being 10ml：1g, hexamethylenetetramine solution optimal concentration is 40-60g/ml.
5. the preparation method as described in claim 2,3 or 4, it is characterised in that：
(1) hexamethylenetetramine solution is prepared；
(2) with hexamethylenetetramine solution pretreatment H obtained by step (1)2WO4, i.e., above-mentioned hexamethylenetetramine is taken by a certain percentage
Solution and H2WO4In container, immersion 20-28h (more excellent is 24-26h) is washed, solid with absolute ethyl alcohol and deionized water successively
Product, which is dried, obtains product.
6. according to the preparation method described in claim 5, it is characterised in that：
The drying is natural air drying, is then directly obtained without calcining and does not calcine WO3, or at 50-700 DEG C calcine 4-8h can
WO is made3, calcining heat preferably is 50-400 DEG C, and preferred calcining heat is 50-250 DEG C.
7. preparation method as claimed in claim 5, it is characterised in that：
The hexamethylenetetramine solution of preparation, that is, weigh a certain amount of C6H12N4, deionized water is added, 30min is then stirred, with
After be transferred in volumetric flask.
8. the WO described in a kind of claim 13Application of the visible-light photocatalyst in catalytic degradation organic pollution.
9. application as claimed in claim 8, it is characterised in that：
Described WO3Visible-light photocatalyst is used for the degraded to the methyl orange in water or the processing to waste water from dyestuff.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710304761.XA CN107020080B (en) | 2017-05-03 | 2017-05-03 | A kind of WO3Visible-light photocatalyst and its preparation and application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710304761.XA CN107020080B (en) | 2017-05-03 | 2017-05-03 | A kind of WO3Visible-light photocatalyst and its preparation and application |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201039A (en) * | 2018-10-25 | 2019-01-15 | 天津工业大学 | Tungstic acid has children outside the state plan catalysis material and synthetic method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101898139A (en) * | 2010-06-25 | 2010-12-01 | 张麒 | Formula of titanium dioxide photochemical catalyst doped with tungstic oxide and preparation method |
| CN102926030A (en) * | 2012-10-15 | 2013-02-13 | 东华大学 | Preparation method of nano fiber containing TiO2/WO3 heterojunction |
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2017
- 2017-05-03 CN CN201710304761.XA patent/CN107020080B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101898139A (en) * | 2010-06-25 | 2010-12-01 | 张麒 | Formula of titanium dioxide photochemical catalyst doped with tungstic oxide and preparation method |
| CN102926030A (en) * | 2012-10-15 | 2013-02-13 | 东华大学 | Preparation method of nano fiber containing TiO2/WO3 heterojunction |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109201039A (en) * | 2018-10-25 | 2019-01-15 | 天津工业大学 | Tungstic acid has children outside the state plan catalysis material and synthetic method |
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