CN106868527A - A kind of tungsten oxide raw powder's production technology - Google Patents
A kind of tungsten oxide raw powder's production technology Download PDFInfo
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- CN106868527A CN106868527A CN201710033796.4A CN201710033796A CN106868527A CN 106868527 A CN106868527 A CN 106868527A CN 201710033796 A CN201710033796 A CN 201710033796A CN 106868527 A CN106868527 A CN 106868527A
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- 239000000843 powder Substances 0.000 title claims abstract description 36
- 238000005516 engineering process Methods 0.000 title claims abstract description 23
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 229910001930 tungsten oxide Inorganic materials 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- 239000003792 electrolyte Substances 0.000 claims abstract description 26
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 239000013049 sediment Substances 0.000 claims abstract description 5
- 230000005611 electricity Effects 0.000 claims description 12
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 5
- 229910000838 Al alloy Inorganic materials 0.000 claims description 3
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 20
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 239000010842 industrial wastewater Substances 0.000 abstract description 4
- 238000013459 approach Methods 0.000 abstract description 2
- 230000002194 synthesizing effect Effects 0.000 abstract description 2
- -1 simply Substances 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 230000003407 synthetizing effect Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910020350 Na2WO4 Inorganic materials 0.000 description 3
- 239000004411 aluminium Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 3
- 229940012189 methyl orange Drugs 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000008151 electrolyte solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 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 2
- 238000003980 solgel method Methods 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- FIPWRIJSWJWJAI-UHFFFAOYSA-N Butyl carbitol 6-propylpiperonyl ether Chemical compound C1=C(CCC)C(COCCOCCOCCCC)=CC2=C1OCO2 FIPWRIJSWJWJAI-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005524 ceramic coating Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000001048 orange dye Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of tungsten oxide raw powder's production technology, the preparation method is electrolysed using plasma electrolytic oxidation technology with the aqueous solution of tungstates as electrolyte to electrolyte, isolates the sediment that electrolyte is generated after electrolysis, dried after sediment is washed, obtain tungsten oxide powder.The invention provides a kind of completely new approach for synthesizing tungsten oxide powder, simply, electrolyte can be reused technique, the equipment that the method is used, and environmental pollution is very small, the WO that the present invention is obtained3Photocatalysis effect is good, has huge potentiality the aspects such as industrial wastewater are decomposed.
Description
Technical field
It is more particularly to a kind of to be based on plasma electrolytic oxidation skill the present invention relates to a kind of tungsten oxide raw powder's production technology
Art synthetizing micro-nano WO3The method of powder.
Background technology
With modern industry high speed development, a large amount of industrial wastewaters etc. are unprocessed or process and below standard be directly discharged to nature
In boundary, huge pollution is caused to destroy to environment, it is serious to the healthy of the influence mankind.And there is energy in traditional environmental improvement
The problems such as consumption is high, control expense is high, efficiency is low and administers not thorough.In recent years, the fast development of nanometer technology is to every field
There is provided new platform, such as：Photocatalysis.During semiconductor powder i.e. in radiation of visible light to the aqueous solution, dye molecule is decomposed
It is CO2、H2The environmental sound thing such as O.And doing catalyst treatment industrial wastewater using semi-conducting material has that handling rate is high, energy consumption
Low feature.All kinds of organic pollutions of sun light degradation can be directly utilized at room temperature because photocatalysis technology has, without secondary
The good characteristics such as pollution, are one of most active research fields in recent years as a kind of preferable environmental pollution treatment technology.Respectively
In class photochemical catalyst, WO3There is band-gap energy low (about 2.7eV), specific surface area is big, surface-active is high, photostability is high,
It is after TiO2The semiconductor light-catalyst of potentiality is had much afterwards.With conventional photochemical catalyst TiO2, ZnO etc. compare, WO3With compared with
Small energy gap and larger light abstraction width, can more effectively using the visible ray for accounting for the nearly half of solar radiation energy, its
Bulk effect, skin effect, quantum size effect and macro quanta tunnel effect are notable.Conventional nano WO3Preparation method have
Vapor phase method, solid phase method and liquid phase method etc..Vapor phase method has the shortcomings that apparatus expensive, high cost, complex operation are unfavorable for industrialization
Production；Solid phase method is also easy to produce some toxic gases when decomposing, and dirty adverse effect is produced to environment；In liquid phase method, mainly have colloidal sol-
Gel method, the precipitation method, micro emulsion method etc..There is expensive raw material price in sol-gel process, the shortcomings of synthesis cycle is long；The precipitation method have
The shortcomings of impurity hardly possible is removed, easily reunited；And micro emulsion rule consumes surfactant and capacity is a lot, hardly possible removal, high cost.
The content of the invention
Present invention aim at a kind of brand-new synthetizing micro-nano WO of offer3The method of powder, that is, use plasma electrolysis
Oxidation technology synthetizing micro-nano WO3Powder.
The technical scheme is that, there is provided a kind of tungsten oxide raw powder's production technology, is electricity with the aqueous solution of tungstates
Solution liquid, is electrolysed using plasma electrolytic oxidation technology to electrolyte, isolates the precipitation that electrolyte is generated after electrolysis
Thing, dries after sediment is washed, and obtains tungsten oxide powder.
Further, the tungstates is sodium tungstate.
Further, the concentration of the aqueous solution of the tungstates is 3-100g/L, preferably 6-100g/L, further preferred 6-
30g/L。
Further, when being electrolysed to electrolyte using plasma electrolytic oxidation technology, anode is aluminum or aluminum alloy.
Further, when being electrolysed to electrolyte using plasma electrolytic oxidation technology, power parameter is set to：Just
Current density is 5-100A/dm2Interior a certain steady state value, negative electricity current density is 0-100A/dm2Interior a certain steady state value, frequency is 50-
A certain steady state value in 3000Hz, positive dutycycle is 5%-80%, and negative duty is 5%-80%.
Further, the temperature of electrolyte is 0-60 DEG C.
Further, the time of electrolysis is 0.5-5h.
Further, the average grain diameter of the tungsten oxide powder is 400-600nm.
Further, the tungsten oxide powder is the tungstic acid powder of monoclinic phase (monoclinic).
Plasma electrolytic oxidation (Plasma electrolytic oxidation, PEO) is also known as differential arc oxidation
(Micro-arc oxidation, MAO), the technology is widely used in the table of valve metal (such as Al, Mg, Ti, Zr) and its alloy
Face is modified, and the ceramic coating of the performances such as wear-resisting, anti-corrosion, biocompatibility is generated in metal surface.The technology is from conventional anodes
Oxidation is developed, unlike its operating voltage higher than oxide-film breakdown voltage so as to workpiece surface generate plasma
Spark, in the presence of plasma spark, metallic matrix is oxidized generation oxide-film, while according to the difference of electrolyte, electrolysis
Anion in liquid can also participate in film forming.But oxide powder is directly prepared using plasma electrolysis oxidation technology and is never reported
Road.The present invention has successfully synthesized micro-nano WO using the technology3Powder, has invented a kind of synthetizing micro-nano WO3Brand-new side
Method, has widened the range of application of plasma electrolytic oxidation technology, and the method has equipment cost low, without special pre-treatment
Operation, efficiency high, simple operation and other advantages.Additionally, electrolysis liquid energy is reused, environmental pollution is few, and meeting current environmental protection will
Ask.
The present invention can with the following methods realize above-mentioned purpose：With pretreated technical pure aluminum or aluminum alloy as anode,
Steel plate is negative electrode, using Na2WO4·2H2The aqueous solution of O is electrolyte, using the method control of the outer applied cyclic water cooling of electrolytic cell
Electrolyte temperature processed is in room temperature.Test the power supply for using identical with metal differential arc oxidation treatment power supply.Differential arc oxidation electricity is set
Source parameter, is turned on the power, and power supply is closed after treatment 1h, pours out electrolyte, leaches powder, that is, obtain tungsten oxide powder.
The setting of power parameter can be selected during differential arc oxidation can mainly use following two modes：1. constant current side is used
Method, its positive electricity current density is (5-100) A/dm2Interior a certain steady state value, negative electricity current density is (5-100) A/dm2Interior a certain steady state value
(negative current can also be cancelled), frequency is a certain steady state value in 50-3000Hz, and positive negative duty is a certain number between 5-80%
Value；2. constant-voltage method is used, its positive voltage is a certain numerical value between 400-600V, negative voltage is that (negative voltage also can use 50-200V
Disappear, only work at constant pressure).
The beneficial effects of the invention are as follows, there is provided a kind of completely new approach for synthesizing tungsten oxide powder, the work that the method is used
Skill, equipment are simple, and electrolyte can be reused, and environmental pollution is very small, the WO that the present invention is obtained3Photocatalysis effect is good,
There are huge potentiality the aspects such as industrial wastewater are decomposed.
Brief description of the drawings
Fig. 1 is the WO that the present invention is obtained3Powder transmission electron microscope photo；
Fig. 2 is the WO that the present invention is obtained3Powder XRD diffracting spectrums；
Fig. 3 is the WO that the present invention is obtained3Powder photocatalysis methyl orange uv-visible absorption spectra；
Fig. 4 is the WO that the present invention is obtained3Degradation curve of the powder to methyl orange solution.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1：Differential arc oxidization technique prepares micro-nano WO3Method, including：
(1) pretreatment of fine aluminium sample；
Commercial-purity aluminium sample is cut into the sample that size is 20 × 10mm, copper conductor is connected with sample, use epoxy resin
Sealing sample, sample is polished after resin solidification with the SiC sand paperings of 600#, 1000#, 2000# successively.Rushed with running water
Wash, be cleaned by ultrasonic with alcohol, then, drying. with deionized water rinsing for several times.
(2) preparation of electrolyte；
The electrolytic solution composition is contained per 1000mL deionized waters：Na2WO4·2H2O：10g；
(3) mao power source parameter setting；
Using constant current alternating-current pulse pattern, positive electricity current density：50A/dm2, negative electricity current density：0, frequency：100Hz, it is positive and negative
Dutycycle is：20%.
(4) micro-nano WO3Powder step of preparation process；
Using fine aluminium sample as anode, steel plate is put into electrolyte and connecting wire as negative electrode, and magnetic is put into electrolyte
Son, is placed on magnetic stirrer and is stirred.Electrolyte is cooled down with circulating cooling system ensure that system is in 20 DEG C
Constant temperature.Power parameter is set, is turned on the power, after treatment 1h, close power supply, take out sample, electrolyte is poured out, by electricity
Solution liquid stands a few houres, pours out supernatant liquor, by precipitation with deionized water rinsing for several times, drying, both.
Embodiment 2：In addition to power parameter is set, remaining is all with embodiment 1；
Mao power source parameter setting：Using constant current alternating-current pulse pattern, positive electricity current density：10A/dm2, negative current is close
Degree：0, frequency：1000Hz, positive negative duty is：20%.
Embodiment 3：In addition to bath composition, remaining is all with embodiment 1；
The preparation of micro-arc oxidation electrolyte：The electrolytic solution composition is contained per 1000mL deionized waters：Na2WO4·
2H2O：16g.
Embodiment 4：In addition to power parameter is set, remaining is all with embodiment 3；
Mao power source parameter setting：Using constant current alternating-current pulse pattern, positive electricity current density：80A/dm2, negative current is close
Degree：0, frequency：1000Hz, positive negative duty is：20%.
The WO obtained under different condition in the embodiment of the present invention of table 13Powder average particle size
The instrument and equipment that powder property and feature detection in the present invention are used is as follows：
Transmission electron microscope (TEM, JEM-3010, JOEL, Japan)；
X-ray diffractometer (place of production Japan, model Rigaku D/MAX 2500)；
WO is surveyed with nano particle size and zeta potential instrument (model Zeta Plus, the U.S.)3Powder diameter；
Xenon source (PLS-SXE300UV) simulated solar irradiation carries out photocatalysis experiment；
Ultraviolet-uisible spectrophotometer (UV-visible spectrophotometer, CARY 300conc) measures solution
Absorbance.
The WO of present invention treatment3Powder the key technical indexes feature is：
From table 1, Fig. 1 and Fig. 2, WO3Powder granule size：Average grain diameter 400-600nm；Powder is crystalline state, XRD knots
It is mutually tungstic acid (the monoclinic WO of monoclinic phase that fruit shows thing3)。
From Fig. 3 and Fig. 4, photocatalytic：Micro-nano WO3With photocatalysis performance, the coloured dye such as the methyl orange that can degrade
The pollutants such as liquid.By WO3Powder sticks to 2 × 1cm2Slide on, be placed in 50mL concentration be 5mg/L methyl orange solution in,
Under ultraviolet-visible light irradiate two hours, can degrade 92.4% methyl orange dye.Wherein, in Fig. 4, C represents the degraded some time
Actual concentrations afterwards, C0Represent initial concentration.
Claims (10)
1. a kind of tungsten oxide raw powder's production technology, it is characterised in that the aqueous solution with tungstates as electrolyte, using plasma
Body electrolytic oxidation technology is electrolysed to electrolyte, isolates the sediment that electrolyte is generated after electrolysis, and sediment is washed
After dry, obtain tungsten oxide powder.
2. preparation method as claimed in claim 1, it is characterised in that the tungstates is sodium tungstate.
3. preparation method as claimed in claim 1 or 2, it is characterised in that the concentration of the aqueous solution of the tungstates is 3-
100 g/L。
4. preparation method as claimed in claim 1 or 2, it is characterised in that the concentration of the aqueous solution of the tungstates is 6-30
g/L。
5. preparation method as claimed in claim 1, it is characterised in that entered to electrolyte using plasma electrolytic oxidation technology
During row electrolysis, anode is aluminum or aluminum alloy.
6. preparation method as claimed in claim 1, it is characterised in that using plasma electrolytic oxidation technology to electrolyte
When being electrolysed, power parameter is set to：Positive electricity current density is 5-100A/dm2Interior a certain steady state value, negative electricity current density is 0-
100A/dm2Interior a certain steady state value, frequency is a certain steady state value in 50-3000 Hz, and positive dutycycle is 5%-80%, negative duty
It is 5%-80%.
7. preparation method as claimed in claim 1, it is characterised in that the temperature of electrolyte is 0-60 DEG C.
8. preparation method as claimed in claim 1, it is characterised in that the time of electrolysis is 0.5-5h.
9. preparation method as claimed in claim 1, it is characterised in that the average grain diameter of the tungsten oxide powder is 400-
600nm。
10. preparation method as claimed in claim 1, it is characterised in that the tungsten oxide powder is the tungstic acid of monoclinic phase
Powder.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541746A (en) * | 2017-09-13 | 2018-01-05 | 西北师范大学 | The method that a kind of liquid phase cathode glow discharging plasma of sacrificial anode leaf prepares nano tungsten trioxide |
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| CN105568341A (en) * | 2016-02-22 | 2016-05-11 | 深圳市威勒科技股份限公司 | Tungsten oxide thin film and preparation method thereof |
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2017
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|---|---|---|---|---|
| JP2007029859A (en) * | 2005-07-27 | 2007-02-08 | Nisshin Seifun Group Inc | Production method of fine particles and apparatus |
| CN101224420A (en) * | 2008-01-22 | 2008-07-23 | 安徽大学 | Uses of light degradation catalyst tungstic oxide nano-powder |
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Cited By (1)
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| CN107541746A (en) * | 2017-09-13 | 2018-01-05 | 西北师范大学 | The method that a kind of liquid phase cathode glow discharging plasma of sacrificial anode leaf prepares nano tungsten trioxide |
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