CN109292819A - A kind of method that step hydro-thermal prepares vanadium trioxide powder - Google Patents
A kind of method that step hydro-thermal prepares vanadium trioxide powder Download PDFInfo
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Abstract
The present invention relates to the methods that one step hydro-thermal of one kind prepares vanadium trioxide powder, reducing agent is added in the aqueous solution of vanadium source and is transferred to closed reactor, then it hydro-thermal reaction 6~48 hours at 0.1~20Mpa pressure, 200~300 DEG C, then is centrifuged to obtain the vanadium trioxide powder；The vanadium source is positive vanadium (V) hydrochlorate or/and vanadyl (IV) salt, preferably Na3VO4、K3VO4、Rb3VO4、Cs3VO4、VOSO4、VOCl2, vanadyl acetylacetonate, at least one of vanadyl oxalate；The reducing agent is at least one of oxalic acid, hydrazine, alcohol；Preferably, the alcohol is at least one of methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol.
Description
Technical field
The present invention relates to the methods that one step hydro-thermal of one kind prepares vanadium trioxide, belong to chemical materials synthesis and functional material
Technical field.
Background technique
Vanadium trioxide V2O3Property (also referred to as MST or MIT) with Metal-nonmetal transition, low temperature phase change feature
Good, sudden change of resistivity is up to 6 orders of magnitude, and also with lattice and anti-ferromagnetic variation, low temperature is monocline antiferromagnetic semiconducter state,
It has there are two transformation temperature: 150~170K and 500~530K, and magnetic susceptibility, light transmission and reflectivity, which also generate, when phase transformation dashes forward
Become.Since it is with excellent light, electricity, magnetic property, in the Series oxides of vanadium, vanadium trioxide (V2O3) be it is a kind of very
Important product all has extensively in the multiple fields such as electricity, magnetic, photoswitch and gas sensor, storage material, resistance material
Application prospect.In addition, V2O3During producing vanadium iron and nitrogen-vanadium alloy, there is spy more superior than other barium oxides
Property, it is the desirable feedstock for producing vanadium series alloy, commercially produces the production line of vanadium nitride both at home and abroad at present mostly with three oxidations two
Vanadium powder is raw material.
V2O3It is widely used in high vanadium ferroalloy and VN alloy production, sensor, new electronic component and battery production etc.
Field.Wherein, V2O3It is had a good application prospect in all-vanadium redox flow battery electrolyte production process, the reason is that with V2O3For
Reducing agent restores the method that vanadic anhydride prepares+3.5 valence V electrolytes, and simple production process, reduction effect is good, and without
The advantages of entering other impurity, having both chemical reduction method and electrolysis method is reduced the production cost of V electrolyte, therefore, this
Extensive concern of the method once proposition i.e. by relevant industries.However, due to current V2O3Preparation cost it is high, product purity is low,
It is restricted the method for this production V electrolyte.
Currently, V2O3Mainly it is made by high-valence state vfanadium compound through restoring.The method of reduction includes additional solid reductant
(e.g., sulphur, carbon dust, graphite etc.) reduction, reducibility gas (such as H2, CO etc.) reduction, ammonium vanadate decomposes, ammonia cracking reduction etc..
Wherein, the method simple production process for adding the reducing agents such as graphite and carbon to restore, but required reduction temperature is high, and is easy in product residual
It stays carbon or brings other impurities into；H2Or the reducing gas such as CO reduction effect is good, product purity is high, but exist burning, explosion or
The danger such as release of toxic gas；Ammonium vanadate decomposes, and the ammonia of generation is cracked into H2And N2Reduction preparation V2O3Method cleaning, ring
It protects, without adding any reducing agent, but not exclusively due to ammonia cracking, reduction is insufficient, and the high requirements on the equipment.In addition to
Except above several main preparation methods, also it can synthesize uniform particle sizes by liquid phase reductions such as hydrothermal synthesis or solvent heats
Tiny V2O3.Relevant report has: patent 1 (Chinese publication number CN101962207A) is disclosed using vanadate as raw material, and use is organic
Solvent carries out reduction reaction in the reactor；Patent 2 (Chinese application number 200510018838.4) is using vanadyl oxalate as raw material
Reaction prepares nanoscale V in organic solution2O3；And patent 3 (Chinese application number 201010513698.9) and patent 4 (in
State publication number CN 1724385A) etc. be required to organic matter as solvent, a large amount of uses of organic matter will increase production cost and
It is not environmentally protective.
Separately there is publication there are also using water as solvent, also needs to handle by high-temperature calcination after reacting under high pressure.Patent 5
(Chinese publication number CN107662946A) discloses the ammonium vanadate of+5 valences and oxalic acid carries out liquid-phase reduction, but product need to also be 700
DEG C or more calcining reduction；Patent 6 (Chinese application number 201210479174.1) proposes that tartaric acid restores V2O5Prepare V2O3, through water
It is also needed after thermal response under inert gas protection in 350-650 DEG C of calcination processing.Patent 7 (Chinese publication number CN106006733A)
It discloses in hydro-thermal reaction of the high price vanadium solution hydrogen partial pressure greater than 1MPa and prepares V2O3Although its using water as reaction dissolvent simultaneously
And without post-processing, but the method uses hydrogen reducing, not easy to operate and there are security risks.
Preceding V2O3Technology of preparing is mostly using ammonium metavanadate, poly ammonium vanadate or vanadic anhydride as raw material, certain
Gained is reacted at temperature and reducing atmosphere, reaction temperature is generally higher than 500 DEG C, and energy consumption is high, high production cost.For example, patent 8
(SU1006375) a kind of vanadium metal reduction vanadic anhydride preparation V is disclosed2O3Method, although in 2-3 minutes just
It can obtain 100% V2O3, but 1200~1600 DEG C and 7~9Pa of reaction condition is excessively harsh.(the Chinese publication number of patent 9
CN1118765A it) discloses a kind of with industrial gas reduction ammonium vanadate or vanadic anhydride preparation V2O3The method of powder, but it is anti-
Answering temperature is 550~650 DEG C.Ammonium metavanadate, poly ammonium vanadate are mostly by the obtained vanadium solution that contains of vanadium extraction industry through ammonium salt
Precipitating gained；Vanadic anhydride is ammonium metavanadate, poly vanadic acid through thermal decomposition gained.Ammonium metavanadate, more is prepared in ammonium salt precipitating
A large amount of ammonia nitrogen waste water can be generated during poly- ammonium vanadate, thermal decomposition ammonium metavanadate, poly ammonium vanadate prepare vanadic anhydride
Process can discharge a large amount of ammonia, these waste water and exhaust gas can all cause serious pollution to environment；In addition, with ammonium metavanadate
Or poly ammonium vanadate is raw material, a large amount of ammonia can be decomposited during preparing vanadium trioxide, unreacted ammonia is released
Being put into atmosphere equally can cause environmental pollution.Therefore, existing vanadium trioxide preparation process is in the presence of environmental pollution is serious
The problem of.
Summary of the invention
For above-mentioned the problems of the prior art, cheap and easy to get, reaction temperature that the purpose of the present invention is to provide a kind of raw materials
Spend that low, synthetic thread is short out and the method for easily controllable vanadium trioxide micro-powder.
On the one hand, the present invention provides the methods that one step hydro-thermal of one kind prepares vanadium trioxide micro-powder, in vanadium source water
Reducing agent is added in solution and is transferred to closed reactor, then the hydro-thermal reaction 6 at 0.1~20Mpa pressure, 200~300 DEG C
~48 hours, then be centrifuged to obtain the vanadium trioxide powder；
The vanadium source is positive vanadium (V) hydrochlorate or/and vanadyl (IV) salt, preferably Na3VO4、K3VO4、Rb3VO4、Cs3VO4、VOSO4、
VOCl2, vanadyl acetylacetonate, at least one of vanadyl oxalate, the reducing agent is at least one of oxalic acid, hydrazine, alcohol；
Preferably, the alcohol is at least one of methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol.
Vanadium (V) hydrochlorate/vanadyl (IV) salt that is positive of vanadium source used in the present invention can be directly dissolved in water, reducing agent used under room temperature
(for example, oxalic acid, hydrazine, alcohol etc.) can be directly dissolved in water, and the redox reaction occurred after the two is mixed is uniform and fast
Speed, there is no parts to cross the inhomogeneities for restoring and owing reduction, obtains high-purity+trivalent, has prevented the mixing of vanadium multivalent state
It coexists, is not necessarily to subsequent heat treatment, self assembly V can be generated2O3Micro-powder.With oxalic acid and Na3VO4As example, oxalic acid is one
Kind important auxiliary agent and reducing agent, can make the V of high-valence state5+It is reduced into the V of lower valency4+、V3+, and due to Na3VO4It is dissolved in aquatic products
Raw NaOH (Na3VO4+H20=2NaOH+NaVO3), under the week reduction of oxalic acid, V can be made5+It is reduced into V3+, oxalic acid restoring
Play the role of controlling intermediate product and final product pattern and partial size in the process, ultimately generates self assembly V2O3Micro-powder.
Preferably, vanadium source concentration is 0.01~10mol/L in the aqueous solution of the vanadium source.
Preferably, the mass ratio of the material of the vanadium source and reducing agent is 1:(1.5~4).
Preferably, the reducing agent is oxalic acid.
Preferably, ligand is added in the aqueous solution of vanadium source, the ligand is selected from carboxylic acid, carboxylate, edetate
At least one of EDTA, cetyl ammonium bromide CTAB, citric acid, dodecyl benzene sulfonate；The vanadium source and ligand
The mass ratio of the material is 1:(0.1~10).
Preferably, being additionally added doped source in the aqueous solution of vanadium source, the doped source is the salt containing respective metal element,
The metallic element be preferably scandium, titanium, chromium, manganese, iron, cobalt, nickel, copper, zinc, tin, indium, antimony, tin, gallium, germanium, lead, bismuth, tungsten, molybdenum,
At least one of ruthenium, niobium, tantalum, magnesium elements.
Also, preferably, the mass ratio of the material in the vanadium source and metal-doped source is 1:(0.01~1).
Preferably, before centrifuge separation, by mixed solution cooled to room temperature in closed reactor, or with 100~
0.01 DEG C/sec of cooling rate is cooled to room temperature.
On the other hand, the present invention also provides a kind of vanadium trioxide powder prepared according to above-mentioned method, described three
The partial size of V 2 O powder is 500nm~50 μm.Gained V2O3The space group of powder is R3c, and 3m point group belongs to trigonal system.
In the present invention, the method is simple and easy, and raw material is cheap and easy to get, and reaction temperature is low, easily controllable, and low energy consumption, peace
Entirely, the production cost of vanadium trioxide can be significantly reduced, is suitble to industrialization large-scale production, in electricity, magnetic, photoswitch and gas
The multiple fields such as dependent sensor, storage material, resistance material all have a wide range of applications.In the present invention, vanadium source used can be normal
It is directly dissolved in water under temperature, and after being added and being dissolved in the reducing agent of water, it is uniform and fast that the two mixes redox reaction occurred
Speed, there is no parts to cross the inhomogeneities for restoring and owing reduction, obtains high-purity+trivalent.The method has prevented vanadium multivalent state
Mixing coexists, and higher reaction temperature and corresponding pressure facilitate the vanadium trioxide powder that a step generates well-crystallized
End.In addition, vanadium source is not limited solely to vanadyl oxalate in the present invention, reducing agent is not limited solely to alcohol, there is stronger universal applicability
And promotional value；Solvent for use is mainly water, cheap, environmentally protective, is conducive to industrialized production；Production disclosed by the invention
Object pattern, partial size can illustrate be added water after the reaction nucleation and growth course change, water can be used as three oxygen wherein
Change pattern controlling agent obtained by two vanadium preferential growths.
Beneficial effects of the present invention are as follows:
(1) raw material is simple, and solvent for use is water, cheap, environmentally protective, is conducive to industrialized production；
(2) reaction route is short, and reaction condition is easily controllable；
(3) reaction temperature is low；
(4) resulting V2O3Powder is self assembly micron-sized powder, and its pattern can be adjusted by the way that ligand is added；
(5) V obtained after hydro-thermal reaction2O3Powder, which is not required to subsequent heat treatment just, has good crystallinity.
Detailed description of the invention
Fig. 1 is V prepared by embodiment 12O3Scanning electron microscope (SEM) photo of powder；
Fig. 2 is V prepared by embodiment 12O3X-ray diffraction (XRD) map of powder.
Specific embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, is not intended to limit the present invention.
In the disclosure, using positive vanadium (V) hydrochlorate/vanadyl (IV) salt as vanadium source, using oxalic acid, connection with week reduction
Ammonia, alcohol etc. are used as reducing agent, take water as a solvent and are placed in reactor, and the vanadium trioxide of well-crystallized is made through a step hydro-thermal
V2O3Powder.
In an embodiment of the present invention, vanadium source is dissolved in the water, and reducing agent is added, reaction solution is transferred to closed
In reactor, and it is heated, so that temperature of reactor is reached 200~300 DEG C, pressure reaches 0.1~20Mpa, and in the state
It is lower to be kept for 6~48 hours, stop heating, when temperature of reactor is down to room temperature, is centrifugated out solid powder to get crystallization is arrived
Good vanadium trioxide powder.
In alternative embodiments, vanadium source is preferably Na3VO4、K3VO4、Rb3VO4、Cs3VO4、VOSO4、VOCl2, second
It is one or more in acyl acetone vanadyl, vanadyl oxalate.Reducing agent is preferably oxalic acid, hydrazine, methanol, ethyl alcohol, normal propyl alcohol, isopropyl
It is alcohol, n-butanol, one or more in isobutanol.
In alternative embodiments, the mass ratio of the material of vanadium source and reducing agent can be 1:(1.5~4) between.Vanadium source exists
Concentration in water can be 0.01~10mol/L.Wherein, reactor (closed reactor) temperature is down to room temperature and is referred to by naturally cold
But or cooling method is forced to cool down reactor.
In order to obtain the V of specific morphology2O3Ligand, including carboxylic acid, carboxylate, ethylenediamine can be added in powder into reaction solution
Tetraacetate (EDTA), cetyl ammonium bromide (CTAB), citric acid, one or more of mixing in dodecyl benzene sulfonate.
Wherein, the mass ratio of the material in ligand and vanadium source can be 1:(0.1~10) between.
In order to obtain the V of element doping2O3Powder, corresponding doped chemical can be added into reaction solution, and (doped chemical can be
21~30 transition elements, tin and its members such as neighbouring element and tungsten, molybdenum, ruthenium, niobium, tantalum, magnesium in the periodic table of elements near vanadium
One in element or any combination.Wherein, 21~30 transition elements in the periodic table of elements near vanadium include scandium, titanium, chromium, manganese,
Iron, cobalt, nickel, copper and zinc, the tin and its neighbouring element include indium, antimony, tin, gallium, germanium, lead and bismuth) water-soluble salt (example
Such as, W6+、Mo6+、Ru4+、Nb5+、Os4+、Fe3+、Cr3+、Ge4+、Ga3+、Al3+In it is one or more), while do not influence pure phase doping
V2O3The generation of powder.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this
Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair
Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific
Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
Weigh 1.218g Na3VO4It is dissolved in 40mL water under magnetic agitation effect, obtains clear transparent solutions, then thereto
1.67g C is added2H2O4·2H2O, solution colour become yellow.Reaction solution is transferred in autoclave, is heated to 270
DEG C, 48h is reacted, heating is stopped, when temperature of reactor is down to room temperature, is centrifugated out solid powder, it is dry to get to three oxygen
Change two vanadium micro-powders, partial size is 10~20 μm.
Embodiment 2
Weigh 1.218g Na3VO4It is dissolved in 40mL water under magnetic agitation effect, obtains clear transparent solutions, then thereto
1.67g C is added2H2O4·2H2O, solution colour become yellow.Reaction solution is transferred in autoclave, is heated to 300
DEG C, 6h is reacted, heating is stopped, when temperature of reactor is down to room temperature, is centrifugated out solid powder, it is dry to get to three oxygen
Change two vanadium micro-powders, partial size is 1~10 μm.
Embodiment 3
Weigh 1.218g Na3VO4It is dissolved in 40mL water under magnetic agitation effect, obtains clear transparent solutions, then thereto
3.34g C is added2H2O4·2H2O, solution colour become yellow, and 0.165g wolframic acid is then added thereto again.Reaction solution is turned
It moves in autoclave, is heated to 200 DEG C, react 48h, stop heating, when temperature of reactor is down to room temperature, centrifuge separation
Solid powder out, dry to get witch culture vanadium trioxide micro-powder is arrived, partial size is 5~20 μm.
Embodiment 4
Weigh 1.218g Na3VO4It is dissolved in 40mL water under magnetic agitation effect, obtains clear transparent solutions, then thereto
1.67g C is added2H2O4·2H2O, solution colour become yellow, and 1.39g monohydrate potassium is then added thereto again
C6H8O7·H2O (as ligand).Reaction solution is transferred in autoclave, is heated to 270 DEG C, reacts 6h, stops heating,
When temperature of reactor is down to room temperature, it is centrifugated out solid powder, dry to get product, partial size is 500nm~1 μm.
Embodiment 5
Weigh 1.218g Na3VO4It is dissolved in 40mL water under magnetic agitation effect, obtains clear transparent solutions, then thereto
1.67g C is added2H2O4·2H2O, solution colour become yellow, and 0.165g wolframic acid is then added thereto again.Reaction solution is turned
It moves in autoclave, is heated to 270 DEG C, react 48h, stop heating, when temperature of reactor is down to room temperature, centrifuge separation
Solid powder out, dry to get witch culture vanadium trioxide powder, partial size is 10~20 μm.
Embodiment 6
Weigh 1g VOSO4It is dissolved in 40mL water under magnetic agitation effect, obtains clear transparent solutions, be then added thereto
1.67g C2H2O4·2H2O.Reaction solution is transferred in autoclave, is heated to 270 DEG C, reacts 48h, stops heating, to
When temperature of reactor is down to room temperature, be centrifugated out solid powder, it is dry to get vanadium trioxide powder, partial size be 500nm~
10μm。
Embodiment 7
Weigh 0.92g Na3VO4It is dissolved in 40mL water under magnetic agitation effect, obtains clear transparent solutions, then thereto
Mono- hydrazine hydrate of 2.5g 10wt% is added.Reaction solution is transferred in autoclave, is heated to 270 DEG C, reacts 48h, is stopped
Heating is centrifugated out solid powder, dry to get vanadium trioxide powder, partial size is when temperature of reactor is down to room temperature
500nm~1 μm.
Fig. 1 is V prepared by embodiment 12O3Scanning electron microscope (SEM) photo of powder, polygon pleat is presented in particle as we know from the figure
Wrinkle shape, particle diameter distribution is about 5~15 μm；
Fig. 2 is V prepared by embodiment 12O3X-ray diffraction (XRD) map of powder, products therefrom is crystallinity as we know from the figure
Good V2O3, no remaining miscellaneous phase is detected.
Embodiment 9
Weigh 1.218g Na3VO4It is dissolved in 40mL water under magnetic agitation effect, obtains clear transparent solutions, then thereto
10g normal propyl alcohol is added.Reaction solution is transferred in autoclave, is heated to 270 DEG C, reacts 48h, stops heating, wait react
When device temperature is down to room temperature, it is centrifugated out solid powder, it is dry to get arriving vanadium trioxide micro-powder, partial size is 10~
50μm。
Above embodiments are served only for that invention is further explained, should not be understood as the limit to the scope of the present invention
System, some nonessential modifications and adaptations that those skilled in the art's above content according to the present invention is made belong to this hair
Bright protection scope.
Claims (8)
1. a kind of method that a step hydro-thermal prepares vanadium trioxide powder, which is characterized in that reduction is added in the aqueous solution of vanadium source
Agent is simultaneously transferred to closed reactor, then hydro-thermal reaction 6~48 hours at 0.1~20Mpa pressure, 200~300 DEG C, then passes through
It is centrifugally separating to obtain the vanadium trioxide powder；
The vanadium source is positive vanadium (V) hydrochlorate or/and vanadyl (IV) salt, preferably Na3VO4、K3VO4、Rb3VO4、Cs3VO4、VOSO4、
VOCl2, vanadyl acetylacetonate, at least one of vanadyl oxalate；
The reducing agent is at least one of oxalic acid, hydrazine, alcohol；Preferably, the alcohol is methanol, ethyl alcohol, normal propyl alcohol, isopropyl
At least one of alcohol, n-butanol, isobutanol.
2. the method according to claim 1, wherein in the aqueous solution of the vanadium source vanadium source concentration be 0.01~
10mol/L。
3. method according to claim 1 or 2, which is characterized in that the mass ratio of the material of the vanadium source and reducing agent is 1:
(1.5~4).
4. method according to any one of claim 1-3, which is characterized in that ligand is added in the aqueous solution of vanadium source, institute
It states ligand and is selected from carboxylic acid, carboxylate, edetate EDTA, cetyl ammonium bromide CTAB, citric acid, detergent alkylate
At least one of sulfonate；The mass ratio of the material of the vanadium source and ligand is 1:(0.1~10).
5. method according to any of claims 1-4, which is characterized in that be additionally added doping in the aqueous solution of vanadium source
Source, the doped source be the salt containing respective metal element, the metallic element be preferably scandium, titanium, chromium, manganese, iron, cobalt,
At least one of nickel, copper, zinc, tin, indium, antimony, tin, gallium, germanium, lead, bismuth, tungsten, molybdenum, ruthenium, niobium, tantalum, magnesium elements.
6. according to the method described in claim 5, it is characterized in that, the mass ratio of the material in the vanadium source and metal-doped source is 1:
(0.01~1).
7. method according to claim 1 to 6, which is characterized in that before centrifuge separation, by confined reaction
Mixed solution cooled to room temperature in device, or room temperature is cooled to 100~0.01 DEG C/sec of cooling rate.
8. the vanadium trioxide powder of method according to any one of claims 1-7 preparation, which is characterized in that described three
The partial size of V 2 O powder is 500nm~50 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109721102A (en) * | 2019-03-20 | 2019-05-07 | 东北石油大学 | A kind of preparation method of chromium tungsten codope hypovanadic oxide powder |
| CN110021746A (en) * | 2019-04-24 | 2019-07-16 | 青海民族大学 | A kind of preparation method and lithium ion battery of carbon coating vanadium trioxide |
| CN114284485A (en) * | 2021-12-31 | 2022-04-05 | 齐鲁工业大学 | V-shaped groove2O3Preparation method of/C hollow nanosphere electrode material |
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