CN106367772B - A kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst - Google Patents
A kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst Download PDFInfo
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- CN106367772B CN106367772B CN201610843179.6A CN201610843179A CN106367772B CN 106367772 B CN106367772 B CN 106367772B CN 201610843179 A CN201610843179 A CN 201610843179A CN 106367772 B CN106367772 B CN 106367772B
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- 239000011701 zinc Substances 0.000 title claims abstract description 61
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 56
- 239000002253 acid Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000003054 catalyst Substances 0.000 title claims abstract description 19
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 10
- 239000003792 electrolyte Substances 0.000 claims abstract description 8
- 125000002091 cationic group Chemical group 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 11
- 239000012528 membrane Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 239000004005 microsphere Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011734 sodium Substances 0.000 claims description 5
- 241000446313 Lamella Species 0.000 claims description 4
- CMZUMMUJMWNLFH-UHFFFAOYSA-N sodium metavanadate Chemical compound [Na+].[O-][V](=O)=O CMZUMMUJMWNLFH-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 229910052801 chlorine Inorganic materials 0.000 claims 1
- 230000005611 electricity Effects 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 8
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 23
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229910001415 sodium ion Inorganic materials 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 238000012512 characterization method Methods 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000011684 sodium molybdate Substances 0.000 description 2
- 235000015393 sodium molybdate Nutrition 0.000 description 2
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 2
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 description 2
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910007541 Zn O Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000571 coke Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000009938 salting Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- -1 transition metal vanadate Chemical class 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
-
- 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
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- B01J35/39—
Abstract
The invention discloses a kind of preparation methods of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst.The present invention prepares different structure and the pyrovanadic acid zinc of particle size by the way of DC electrolysis, by controlling current density, concentration of electrolyte and temperature, consisting of Zn3V2O7(OH)2·2H2O.The method of the present invention is easy to operate, and control, product is facilitated to be easy to collect, and products therefrom pattern is the three dimensional micron bouquet structure that nanoscale twins intersect composition.
Description
Technical field
The invention belongs to inorganic catalysis material technical field more particularly to pyrovanadic acid zinc, a kind of specifically 3D flowers
The preparation method of shot coke Zinc vanadate photochemical catalyst.
Background technology
With the high speed development of global industry, environmental pollution is also increasingly prominent, and strong as influence social development and the mankind
The No.1 problem of health.In recent years, Nano semiconductor photocatalyst technology has attracted largely in the application potential of field of environmental improvement
Scientific research concern, relevant achievement in research is also commonplace.3D hierarchical structures are because of its special property and in many fields
Potential application and widely paid close attention to.Research finds hierarchical structure because it is with higher specific surface area, in light-catalyzed reaction
In more reactivity sites can be provided, therefore hierarchical structure catalyst has higher photocatalytic activity under equal conditions.
In addition, nano material causes to be difficult to separate and recover since its sample particle is too small, reusing for catalyst is influenced, and micron order
Grading structure material both possessed many advantages of nanometer materials, also have the characteristics that easily to recycle.
Pyrovanadic acid zinc Zn3V2O7(OH)2·2H2O is a kind of important transition metal vanadate.Its crystal structure category hexagonal crystal
Frame structure is presented in system, and by Zn-O tetrahedrons and V-O octahedral layers, alternately connection is formed pyrovanadic acid zinc crystal framework, wherein V-O
There are stratiform channel, this structures to be conducive to the migration in light induced electron and hole for interlayer, is photo-generated carrier more accessible to catalysis
Agent surface carries out further redox reaction, and sample is made to have higher photocatalysis property.
In terms of pyrovanadic acid zinc synthesis, include mainly using more method：Chemical precipitation method, supercritical ultrasonics technology, hydro-thermal method,
Microwave etc..But it haves the shortcomings that common is to have the presence of additive or reaction time longer (up to even several days a few houres
Time).
Publication No. CN 104388970A, entitled " a method of preparing zinc molybdate using cationic membrane electrolysis "
Chinese patent in, using zinc metal sheet as anode, using inert electrode as cathode, using sodium molybdate aqueous solution as anolyte, with acid solution, alkali
Solution or salting liquid are catholyte；In the two-compartment cell that cationic membrane is diaphragm, using constant-current electrolysis or constant-potential electrolysis
Mode, control temperature range is that room temperature carries out electrolysis sodium molybdate aqueous solution to 90 DEG C, until Na+Ion is transferred completely into cathode
Room；Obtained product is filtered with deionized water when cleaning after being electrolysed, can be obtained being calcined after obtained filtration cakes torrefaction
Pure zinc molybdate, the method carries out target product by the way of cationic membrane electrolysis and quickly synthesizes, by controlling electric current
Density, concentration of electrolyte and temperature control product morphology, and product is made to obtain wider development and application.
Invention content
It is long in order to solve the reaction time in pyrovanadic acid zinc preparation process in the prior art, additive mostly with it is complicated for operation, production
The technical problems such as more than object impurity, the purpose of the present invention is to provide a kind of preparation sides of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst
Method uses DC electrolysis method to prepare, and different structure and grain size are prepared by controlling current density, concentration of electrolyte and temperature
The pyrovanadic acid zinc of size.The preparation process is simple and easily operated, and anolyte ingredient is single, without other additives, product
Without dephasign, it is easy to industrialized production.
Technical scheme of the present invention is specific as follows.
The present invention provides a kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst, is as follows：
(1) using zinc metal sheet as anode, using inert electrode as cathode, using sodium metavanadate aqueous solution as anolyte, with hydrochloric acid solution
Or sodium chloride solution is that catholyte by the way of constant-current electrolysis, passes through control in the two-compartment cell that cationic membrane is diaphragm
Current density, concentration of electrolyte and temperature processed prepare different structure and the pyrovanadic acid zinc of particle size；
(2) after being electrolysed, the product obtained on anode is collected, cleaning, filtering, drying are to get 3D flower ball-shaped structures
Pyrovanadic acid zinc photochemical catalyst, consisting of Zn3V2O7(OH)2·2H2O；.
In above-mentioned steps (1), a concentration of 0.1mol/L-0.3mol/L of the sodium metavanadate.
In above-mentioned steps (1), a concentration of 0.1mol/L-0.3mol/L of the catholyte.
In above-mentioned steps (1), the temperature using water bath with thermostatic control control electrolysis is 20-70 DEG C.
In above-mentioned steps (1), control anodic current density is 10-50mA/cm2。
In above-mentioned steps (1), the inert electrode is glass-carbon electrode or titanium net.
In above-mentioned steps (2), drying temperature is 60-90 DEG C, drying time 2-4h.
The 3D flower ball-shaped pyrovanadic acid zinc photochemical catalyst grain sizes that preparation method of the present invention obtains are between 1-5 μm；The shape of product
Looks structure intersects micro-sphere structure variation from two lamellas to multi-slice.
Compared to the prior art, the beneficial effects of the present invention are：
A kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst of the present invention uses cationic membrane to be electrolysed legal system
It is standby, prepare different structure and the pyrovanadic acid zinc (electrolyte of particle size by controlling current density, concentration of electrolyte and temperature
Concentration increases, and current density increases, and grain size is bigger, and structure is changed into multi-slice from biplate layer or three lamella petal-like structures and intersects
Micro-sphere structure).Preparation process is simple and easily operated, and anolyte ingredient is single, without other additives, product without dephasign,
It is easy to industrialized production；On the other hand, product is the solid powder of three-dimensional micro-nano rank, and standing can precipitate, be easy to
It washes and detaches.Therefore the pyrovanadic acid zinc product purity of the final gained of the preparation method of the present invention is high, and no dephasign carries out product
Zinc vanadate can be obtained after high-temperature calcination, can be used as LITHIUM BATTERY material.
Further, the preparation method of a kind of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst of the invention, it is only necessary to which one-step electrolysis is
Pyrovanadic acid zinc can be prepared, therefore its preparation process is simple for process, easy to operate, investment is small, and synthetic quantity is big, may be directly applied to
Industrialized production.
Description of the drawings
The SEM of the pyrovanadic acid zinc obtained in Fig. 1, embodiment 1 schemes.
The SEM of the pyrovanadic acid zinc obtained in Fig. 2, embodiment 2 schemes.
The SEM of the pyrovanadic acid zinc obtained in Fig. 3, embodiment 3 schemes.
The SEM of the pyrovanadic acid zinc obtained in Fig. 4, embodiment 4 schemes.
The EDS of the pyrovanadic acid zinc obtained in Fig. 5, embodiment 1-4 schemes.
The XRD diagram of the pyrovanadic acid zinc obtained in Fig. 6, embodiment 1-4.
Fig. 7,3D flower ball-shaped pyrovanadic acid zinc are to methylene blue (10-5Mol/L ultraviolet catalytic degradation curve figure).
Specific implementation mode
It is expanded on further below by specific embodiment and in conjunction with attached drawing to the present invention, but is not intended to limit the present invention.
Embodiment 1
A kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst, specifically comprises the following steps：
(1), using zinc metal sheet as anode, using glass-carbon electrode as cathode, using the aqueous solution of 0.1mol/L sodium metavanadates as anolyte,
Using 0.1mol/L hydrochloric acid solutions as catholyte, in the two-compartment cell that cationic membrane is diaphragm, it is 70 DEG C to control in temperature
Under the conditions of carry out constant-current electrolysis, current density 10mA/cm2；
(2), after being electrolysed, the product obtained on anode is filtered with deionized water when cleaning, so as to by Na+Cleaning
Totally, then filtered filter cake is dried to 4h, cooled to room temperature after drying at a temperature of 90 DEG C, you can obtain pyrovanadium
Sour zinc powder.
Morphology characterization, SEM are carried out to the pyrovanadic acid zinc of above-mentioned gained using Hitachi S-3400N types scanning electron microscope
Figure as shown in Figure 1, from figure 1 it appears that obtained product be biplate layer or three lamella petal-like structures, particle size 2-
3μm。
Embodiment 2
A kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst, specifically comprises the following steps：
(1), using zinc metal sheet as anode, using titanium net as cathode, using the aqueous solution of 0.2mol/L sodium metavanadates as anolyte, with
0.2mol/L sodium chloride solutions are catholyte, and in the two-compartment cell that cationic membrane is diaphragm, it is 50 DEG C to control in temperature
Under the conditions of carry out constant-current electrolysis, current density 50mA/cm2；
(2), after being electrolysed, the product obtained on anode is filtered with deionized water when cleaning, so as to by Na+Cleaning
Totally, then filtered filter cake is dried to 5h, cooled to room temperature after drying at a temperature of 80 DEG C, you can obtain pyrovanadium
Sour zinc powder.
Morphology characterization, SEM are carried out to the pyrovanadic acid zinc of above-mentioned gained using Hitachi S-3400N types scanning electron microscope
For figure as shown in Fig. 2, from figure 2 it can be seen that obtained product is to be that multi-slice intersects micro-sphere structure, particle size is 4-5 μ
m。
Embodiment 3
A kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst, specifically comprises the following steps：
(1), using zinc metal sheet as anode, using titanium net as cathode, using the aqueous solution of 0.3mol/L sodium metavanadates as anolyte, with
0.3mol/L hydrochloric acid solutions are catholyte, in the two-compartment cell that cationic membrane is diaphragm, control the item for being 20 DEG C in temperature
Constant-current electrolysis, current density 20mA/cm are carried out under part2；
(2), after being electrolysed, the product obtained on anode is filtered with deionized water when cleaning, so as to by Na+Cleaning
Totally, then filtered filter cake is dried to 6h, cooled to room temperature after drying at a temperature of 60 DEG C, you can obtain pyrovanadium
Sour zinc powder.
Morphology characterization, SEM are carried out to the pyrovanadic acid zinc of above-mentioned gained using Hitachi S-3400N types scanning electron microscope
For figure as shown in figure 3, from figure 3, it can be seen that obtained product, which is multi-slice, intersects micro-sphere structure, particle size is 1-2 μm.
Embodiment 4
A kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst, specifically comprises the following steps：
(1), using zinc metal sheet as anode, using titanium net as cathode, using the aqueous solution of 0.2mol/L sodium metavanadates as anolyte, with
0.2mol/L sodium chloride solutions are catholyte, and in the two-compartment cell that cationic membrane is diaphragm, it is 20 DEG C to control in temperature
Under the conditions of carry out constant-current electrolysis, current density 30mA/cm2；
(2), after being electrolysed, the product obtained on anode is filtered with deionized water when cleaning, so as to by Na+Cleaning
Totally, then filtered filter cake is dried to 5h, cooled to room temperature after drying at a temperature of 70 DEG C, you can obtain pyrovanadium
Sour zinc powder.
Morphology characterization, SEM are carried out to the pyrovanadic acid zinc of above-mentioned gained using Hitachi S-3400N types scanning electron microscope
For figure as shown in figure 4, figure 4, it is seen that obtained product, which is multi-slice, intersects microballoon interconnection architecture, particle size is 2-3 μ
m。
Using 4010 type X-ray detection instrument of German Brooker ALX companies to the pyrovanadic acid zinc obtained by above-mentioned all examples
It is measured, EDS figures are as shown in figure 5, from figure 5 it can be seen that obtain there was only tetra- kinds of elements of Zn, V, O-H in product, thus
The method products therefrom of the invention for using cationic membrane electrolysis to prepare 3D flower ball-shaped pyrovanadic acid zinc is shown for pure phase, without miscellaneous
Matter.
Using the D8Advance types x-ray diffractometer of German Brooker AXS companies to gained in above-mentioned all examples
Pyrovanadic acid zinc is measured, and obtained product is Zn3V2O7(OH)2·2H2O, as shown in Figure 6.
The pyrovanadic acid zinc bouquet prepared using example 3 is to methylene blue (10-5Mol/L ultraviolet catalytic degradation) is carried out,
Degradation curve is as shown in fig. 7, illustrate that the product of the present invention has good Photocatalytic Degradation Property.
In conclusion a kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc of the present invention, by controlling concentration of electrolyte, temperature
Degree and current density；Different structure and the pyrovanadic acid zinc of particle size can be obtained, the pyrovanadic acid zinc of final gained is pure phase, nothing
Dephasign.
The above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, without departing from the technical principles of the invention, several improvements and modifications can also be made, these improve and become
Type also should be regarded as protection scope of the present invention.
Claims (2)
1. a kind of preparation method of 3D flower ball-shapeds pyrovanadic acid zinc photochemical catalyst, which is characterized in that be as follows：
(1) using zinc metal sheet as anode, using inert electrode as cathode, using sodium metavanadate aqueous solution as anolyte, with hydrochloric acid solution or chlorine
Change sodium solution is catholyte, in the two-compartment cell that cationic membrane is diaphragm, by the way of constant-current electrolysis, by controlling electricity
Current density, concentration of electrolyte and temperature prepare different structure and the pyrovanadic acid zinc of particle size；
(2) after being electrolysed, the product obtained on anode, cleaning, filtering, the dry pyrovanadium to get 3D flower ball-shaped structures are collected
Sour zinc photochemical catalyst, consisting of Zn3V2O7(OH)2·2H2The grain size of O, obtained 3D flower ball-shaped pyrovanadic acid zinc photochemical catalysts is
1-5 μm, the appearance structure of product intersects micro-sphere structure variation from two lamellas to multi-slice；Wherein：
In step (1), a concentration of 0.1mol/L-0.3mol/L of the sodium metavanadate；A concentration of 0.1mol/ of the catholyte
L-0.3mol/L；Using the temperature of water bath with thermostatic control control electrolysis between 20-70 DEG C；Control anodic current density is 10-50mA/
cm2。
2. preparation method as described in claim 1, which is characterized in that in step (2), drying temperature is 60-90 DEG C, when dry
Between be 4-6h.
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Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55102288A (en) * | 1979-01-31 | 1980-08-05 | Furukawa Circuit Foil | Printed circuit copper foil and method of manufacturing same |
| CN104073835A (en) * | 2014-06-23 | 2014-10-01 | 上海应用技术学院 | Method for preparing cupric tungstate via electrolysis of cation membrane |
| CN104099633A (en) * | 2014-06-23 | 2014-10-15 | 上海应用技术学院 | Method for preparing copper molybdate by using cation membrane electrolysis method |
| CN104357876A (en) * | 2014-10-31 | 2015-02-18 | 上海应用技术学院 | Method for preparing nickel tungstate by using cationic membrane electrolysis process |
| CN104357875A (en) * | 2014-10-31 | 2015-02-18 | 上海应用技术学院 | Method for preparing iron molybdate by using cationic membrane electrolysis process |
| CN104357874A (en) * | 2014-10-31 | 2015-02-18 | 上海应用技术学院 | Method for preparing nickel molybdate by using cationic membrane electrolysis process |
| CN104357877A (en) * | 2014-10-31 | 2015-02-18 | 上海应用技术学院 | Method for preparing zinc tungstate by using cationic membrane electrolysis process |
| CN104388970A (en) * | 2014-10-31 | 2015-03-04 | 上海应用技术学院 | Method for preparing zinc molybdate by using cationic membrane electrolysis method |
| CN104789982A (en) * | 2015-04-09 | 2015-07-22 | 上海应用技术学院 | Method for preparing silver molybdate with cationic membrane electrolysis method |
| CN104789983A (en) * | 2015-04-09 | 2015-07-22 | 上海应用技术学院 | Method for preparing aluminum molybdate with cationic membrane electrolysis method |
| CN104831304A (en) * | 2015-04-09 | 2015-08-12 | 上海应用技术学院 | Method for preparing aluminum tungstate by cation membrane electrolytic method |
| CN104831305A (en) * | 2015-04-09 | 2015-08-12 | 上海应用技术学院 | Method for preparing liver tungstate by cation membrane electrolytic method |
| CN104966835A (en) * | 2015-06-19 | 2015-10-07 | 合肥国轩高科动力能源股份公司 | Method for manufacturing AgVO<3> thin films on Ag substrates by means of electrolysis |
-
2016
- 2016-09-23 CN CN201610843179.6A patent/CN106367772B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS55102288A (en) * | 1979-01-31 | 1980-08-05 | Furukawa Circuit Foil | Printed circuit copper foil and method of manufacturing same |
| CN104073835A (en) * | 2014-06-23 | 2014-10-01 | 上海应用技术学院 | Method for preparing cupric tungstate via electrolysis of cation membrane |
| CN104099633A (en) * | 2014-06-23 | 2014-10-15 | 上海应用技术学院 | Method for preparing copper molybdate by using cation membrane electrolysis method |
| CN104357876A (en) * | 2014-10-31 | 2015-02-18 | 上海应用技术学院 | Method for preparing nickel tungstate by using cationic membrane electrolysis process |
| CN104357875A (en) * | 2014-10-31 | 2015-02-18 | 上海应用技术学院 | Method for preparing iron molybdate by using cationic membrane electrolysis process |
| CN104357874A (en) * | 2014-10-31 | 2015-02-18 | 上海应用技术学院 | Method for preparing nickel molybdate by using cationic membrane electrolysis process |
| CN104357877A (en) * | 2014-10-31 | 2015-02-18 | 上海应用技术学院 | Method for preparing zinc tungstate by using cationic membrane electrolysis process |
| CN104388970A (en) * | 2014-10-31 | 2015-03-04 | 上海应用技术学院 | Method for preparing zinc molybdate by using cationic membrane electrolysis method |
| CN104789982A (en) * | 2015-04-09 | 2015-07-22 | 上海应用技术学院 | Method for preparing silver molybdate with cationic membrane electrolysis method |
| CN104789983A (en) * | 2015-04-09 | 2015-07-22 | 上海应用技术学院 | Method for preparing aluminum molybdate with cationic membrane electrolysis method |
| CN104831304A (en) * | 2015-04-09 | 2015-08-12 | 上海应用技术学院 | Method for preparing aluminum tungstate by cation membrane electrolytic method |
| CN104831305A (en) * | 2015-04-09 | 2015-08-12 | 上海应用技术学院 | Method for preparing liver tungstate by cation membrane electrolytic method |
| CN104966835A (en) * | 2015-06-19 | 2015-10-07 | 合肥国轩高科动力能源股份公司 | Method for manufacturing AgVO<3> thin films on Ag substrates by means of electrolysis |
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