CN106400044B - A kind of preparation method of lead vanadate - Google Patents
A kind of preparation method of lead vanadate Download PDFInfo
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- CN106400044B CN106400044B CN201610844529.0A CN201610844529A CN106400044B CN 106400044 B CN106400044 B CN 106400044B CN 201610844529 A CN201610844529 A CN 201610844529A CN 106400044 B CN106400044 B CN 106400044B
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- 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
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- 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
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
- C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
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Abstract
The invention discloses a kind of preparation methods of lead vanadate.The present invention prepares different structure and the lead vanadate presoma of particle size first by the way of DC electrolysis, by controlling current density, concentration of electrolyte and temperature；Then the product obtained in anolyte is collected, is filtered, is washed, it is dry；400 600 DEG C finally are warming up to the heating rate of 25 DEG C/min under air atmosphere, the lead vanadate that 3 5h of high-temperature roasting is high to get purity, cleanliness factor is high, consisting of Pb2V2O7, the present invention is spherical nanoparticle, nanoscale twins pilotaxitic texture and flowers structure by controlling the main pattern of corresponding conditions products therefrom.
Description
Technical field
The invention belongs to inorganic functional material preparing technical field, a kind of specifically preparation method of lead vanadate.
Background technology
Vanadate crystal obtains related scientific research worker and largely pays close attention to and go deep into because of changeable structure, pattern and performance
Research, achieve more great successes.Currently, various vanadate have been synthesized, and study its performance, it is found that they have
Wide application prospect, organic synthesis catalyst, photochromic material, embedded photoluminescent material, electrooptical device are such as can be used as
With the photochemical catalyst etc. of sewage degradation.As multifunctional material, lead vanadate can generate larger spontaneous polarization, can be used as anti-iron
Magnetic ferroelectric material.Just because of the excellent properties of vanadic acid lead material, and there are also some document reports lead vanadates
The synthetic method (composite-hydroxide-mediated) of dependency structure and performance study achievement, but the synthetic method of lead vanadate at present
Still more complicated, low output is not suitable for industrialization production.
Publication No. " CN 104099633A ", a kind of entitled " side preparing copper molybdate using cationic membrane electrolysis
The Chinese patent of method ", using copper sheet as anode, using inert electrode as cathode, with Na2MoO4.2H2O solution is anolyte, with pH models
It is catholyte to enclose for 0~14 solution, and sodium molybdate solution is electrolysed using cationic membrane, will be dried after obtained product cleaning,
By the product high-temperature roasting after drying, pure molybdic acid copper crystal is obtained.
Invention content
It is long in order to solve the reaction time in lead vanadate preparation process in the prior art, additive mostly with it is complicated for operation, production
It measures low, is unable to the technical problem of industrialization production etc., the purpose of the present invention is to provide a kind of preparation method of lead vanadate, the party
The method reaction time is short, easily separated, and anolyte is single without other additives, and product is easy to operate without dephasign, is easy to industrialize
Production.
Technical scheme of the present invention is specifically described as follows.
The present invention provides a kind of preparation method of lead vanadate, is as follows：
(1) using stereotype as anode, using inert electrode as cathode, using sodium metavanadate aqueous solution as anolyte, with hydrochloric acid
Solution or sodium chloride solution are catholyte, in the two-compartment cell that cationic membrane is diaphragm, by the way of constant-current electrolysis, are led to
It crosses control current density, concentration of electrolyte and temperature and prepares different structure and the lead vanadate of particle size；
(2) after being electrolysed, the product obtained on anode is collected, cleaning filters, is dry, cooled to room temperature, finally
It is warming up to 400-600 DEG C with the heating rate of 2-5 DEG C/min under air atmosphere, high-temperature roasting 3-5h is high to get purity, clean
High lead vanadate is spent, consisting of Pb2V2O7。
In the present invention, in step (1), a concentration of 0.1mol/L-0.3mol/L of the sodium metavanadate.
In the present invention, in step (1), a concentration of 0.1mol/L-0.3mol/L of the catholyte.
It it is 20-70 DEG C using water bath with thermostatic control control electrolysis temperature in step (1) in the present invention.
In the present invention, in step (1), control anodic current density is 10-50mA/cm2。
In the present invention, in step (1), the inert electrode is glass-carbon electrode or titanium net.
In the present invention, in step (2), drying temperature is 60-90 DEG C, drying time 2-4h.
For the grain size for the lead vanadate that preparation method of the present invention obtains between 1-5 μm, pattern is spherical nanoparticle, nanometer sheet
Layer pilotaxitic texture or flowers structure.
Compared to the prior art, beneficial effects of the present invention are as follows：
A kind of preparation method of lead vanadate of the present invention uses cationic membrane electrolysis to prepare, close by controlling electric current
Degree, concentration of electrolyte and temperature prepare the lead vanadate of different structure and particle size, and (temperature improves, and current density increases, and obtains
To the structure of product become nanoscale twins pilotaxitic texture from spherical nanoparticle, become flowers structure again).Preparation process is simple
And it is easily operated, anolyte ingredient is single, without other additives, and product is easy to industrialized production without dephasign；Another party
Face, product are the other solid powder of micro/nano level, and standing can precipitate, and are easy to washing and detach.Therefore the system of the present invention
The characteristics of Preparation Method has the lead vanadate product purity of final gained high, no dephasign, vanadium can be obtained after product is carried out high-temperature calcination
Lead plumbate is characterized as Pb through X-ray diffraction2V2O7。
Further, a kind of preparation method of lead vanadate of the present invention, it is only necessary to which one-step electrolysis can prepare lead vanadate, therefore its
Preparation process is simple for process, easy to operate, and investment is small, and synthetic quantity is big, may be directly applied to industrialized production.
Description of the drawings
The SEM of the lead vanadate obtained in Fig. 1, the embodiment of the present invention 1 schemes.
The powerful SEM figures of lead vanadate obtained in Fig. 2, the embodiment of the present invention 1.
The SEM of the lead vanadate obtained in Fig. 3, the embodiment of the present invention 2 schemes.
The SEM of the lead vanadate obtained in Fig. 4, the embodiment of the present invention 3 schemes.
The EDS of the lead vanadate obtained in Fig. 5, the embodiment of the present invention schemes.
The XRD diagram of the lead vanadate obtained in Fig. 6, the embodiment of the present invention.
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 lead vanadate, specifically comprises the following steps：
(1), using stereotype 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, and will be after filtering
Filter cake controlled at 80 DEG C of dry 4h, it is dry after cooled to room temperature, it is dry after under air atmosphere with 2
DEG C/heating rate of min is warming up to 500 DEG C of progress high-temperature roasting 3h, roast afterwards cooled to room temperature to get pure vanadium
Lead plumbate.
Morphology characterization, SEM figures are carried out to the lead vanadate of above-mentioned gained using Hitachi S-3400N types scanning electron microscope
As depicted in figs. 1 and 2, as can be seen that prepared product morphology is spheric granules structure from Fig. 1 and Fig. 2, particle size is about
For 100nm.
Embodiment 2
A kind of preparation method of lead vanadate, is as follows：
(1), using stereotype as anode, using glass-carbon electrode as cathode, using the aqueous solution of 0.2mol/L sodium metavanadates as anolyte,
Using 0.2mol/L sodium chloride solutions as catholyte, in the two-compartment cell that cationic membrane is diaphragm, control is 50 DEG C in temperature
Under 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, and will be after filtering
Filter cake controlled at 90 DEG C of dry 4h, it is dry after cooled to room temperature, it is dry after under air atmosphere with 5
DEG C/heating rate of min is warming up to 600 DEG C of progress high-temperature roasting 3h, roast afterwards cooled to room temperature to get pure vanadium
Lead plumbate.
Morphology characterization, SEM figures are carried out to the lead vanadate of above-mentioned gained using Hitachi S-3400N types scanning electron microscope
As shown in figure 3, from figure 3, it can be seen that prepared product morphology is nanoscale twins pilotaxitic texture..
Embodiment 3
A kind of preparation method of lead vanadate, is as follows：
(1), using lead as anode, using glass-carbon electrode 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 50mA/cm are carried out under part2；
(2), after being electrolysed, the product obtained on anode is filtered with deionized water when cleaning, and will be after filtering
Filter cake controlled at 80 DEG C of dry 4h, it is dry after cooled to room temperature, it is dry after under air atmosphere with 5
DEG C/heating rate of min is warming up to 400 DEG C of progress high-temperature roasting 5h, roast afterwards cooled to room temperature to get pure vanadium
Lead plumbate.
Morphology characterization, SEM figures are carried out to the lead vanadate of above-mentioned gained using Hitachi S-3400N types scanning electron microscope
As shown in figure 4, figure 4, it is seen that prepared product morphology is flowers structure.
The pyrovanadic acid zinc of above-mentioned gained is measured using 4010 type X-ray detection instrument of German Brooker ALX companies,
Its EDS schemes, as shown in figure 5, from figure 5 it can be seen that obtain there was only tetra- kinds of elements of Pb, V, O, C in product, to be indicated above this
It is more pure that invention using electrolysis prepares the lead vanadate obtained by the method for lead vanadate；
The lead vanadate of above-mentioned gained is carried out using the D8Advance types x-ray diffractometer of German Brooker AXS companies
It measures, XRD diagram is as shown in fig. 6, from fig. 6 it can be seen that obtained product is Pb2V2O7, correspondence PDF cards are 47-
1735。
In conclusion a kind of preparation method of lead vanadate of the present invention, close by controlling concentration of electrolyte, temperature and electric current
Degree；Different structure and the lead vanadate of particle size can be obtained, is laid the foundation to expand its application.
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 (3)
1. a kind of preparation method of lead vanadate, which is characterized in that be as follows：
(1) using stereotype 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 lead vanadate of particle size；
(2) after being electrolysed, the product obtained on anode, cleaning, filtering, dry, cooled to room temperature, finally in sky are collected
Atmosphere with the heating rate of 2-5 DEG C/min is warming up to 400-600 DEG C under enclosing, and high-temperature roasting 3-5h is high to get purity, cleanliness factor is high
Lead vanadate, consisting of Pb2V2O7：For the grain size of obtained lead vanadate between 1-5 μm, pattern is spherical nanoparticle, nanometer
Lamella pilotaxitic texture or flowers structure；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；Temperature using water bath with thermostatic control control electrolysis is 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 (1), the inert electrode be glass-carbon electrode or
Titanium net.
3. 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 2-4h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5912039B2 (en) * | 1979-01-31 | 1984-03-19 | 古河サ−キツトフオイル株式会社 | Copper foil for printed circuits and its manufacturing method |
| CN101275232B (en) * | 2008-05-08 | 2011-01-26 | 紫金矿业集团股份有限公司 | Preparation for gold salt and device therefor |
| 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 |
| CN104966835B (en) * | 2015-06-19 | 2017-03-15 | 合肥国轩高科动力能源有限公司 | One kind electrolytic preparation AgVO in Ag substrates3The method of thin film |
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