CN101962207B - Method for preparing vanadium trioxide powder - Google Patents
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- CN101962207B CN101962207B CN201010513696XA CN201010513696A CN101962207B CN 101962207 B CN101962207 B CN 101962207B CN 201010513696X A CN201010513696X A CN 201010513696XA CN 201010513696 A CN201010513696 A CN 201010513696A CN 101962207 B CN101962207 B CN 101962207B
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Abstract
The invention discloses a method for preparing vanadium trioxide powder, and relates to a method for preparing a chemical material. The method comprises the following steps of: adding an organic solvent into vanadate serving as a raw material, then reacting in a reactor for 0.1 to 6.0 hours, wherein the temperature of the reactor is controlled to be between 150 and 450 DEG C, and a pressure is controlled to be 1.5 to 25.0MPa; and after reaction is finished, separating the solvent from a product to obtain the uniform vanadium trioxide powder. The method for preparing the vanadium trioxide powder has the advantages of low cost and readily available raw material and organic solvent, simple process, suitability for mass production, and wide application prospect in the various fields, such as electricity, magnetism, an optical switch, a gas sensitive sensor, a storage material, a resistive material and the like.
Description
Technical field
The present invention relates to a kind of preparation method of chemical materials, particularly relate to a kind of preparation method of vanadous oxide powder.
Background technology
V
2O
3Have the character (being also referred to as MST or MIT) of metal-nonmetal transition, the low temperature phase change characteristic is good, and sudden change of resistivity can reach 6 one magnitude, also follows lattice and anti-ferromagnetic variation, and low temperature is monocline antiferromagnetic semiconducter group.V
2O
3Have two transformation temperature: 150～170K and 500～530K.V
2O
3Also be a kind of gunn material, susceptibility, optical transmittance and reflectivity also produce sudden change during phase transformation.
Since have excellent light, electricity, magnetic property, in the serial oxide compound of vanadium, vanadous oxide (V
2O
3) be a kind of crucial product, at electricity, magnetic, photoswitch, the multiple fields such as gas sensor, storage medium, resistive material that reach all are with a wide range of applications.In addition, V
2O
3In the process of producing vanadium iron and nitrogen-vanadium alloy, have than other barium oxide superior characteristic more, be the desirable feedstock of producing the vanadium series alloy, commercially producing both at home and abroad at present more than the production line of vanadium nitride with the vanadous oxide powder is raw material.
Chinese patent CN1118765A discloses a kind of working method of vanadous oxide.This method adds the ammonium vanadate or the Vanadium Pentoxide in FLAKES of certain particle size in the external-heat container; In its container, feed industrial gas; Make through outer heating that the high-temperature zone reaches 500～650 ℃ in the container; Make furnace charge pass through this zone and reduction reaction takes place 15～40 minutes, making its decomposition-reduction is vanadous oxide.The providing of this document adopted common shaft furnace and the rotary kiln embodiment as production unit.The shortcoming of this method is: the temperature of reaction general requirement is being carried out more than 900 ℃ in the actual industrial production implementation process; Though the rotary kiln structure is simpler relatively simultaneously,, there are the technological difficulties of high temperature dynamic seal because the hot environment and the scantlings of the structure of its operation are bigger; Receive the material selection of reacting in rotary kiln device and the restriction of ME and installation in addition, also have certain potential safety hazard in the production process; The filling ratio of reacting in rotary kiln device lower (about 5%) in addition, so production efficiency is lower, also very big for the waste of reducing gas such as industrial gas.
" mining metallurgical engineering " (2005,25 (6): 61～65) having introduced a kind of is that reducing gas is gone back the method for preparing vanadous oxide originally to ammonium meta-vanadate in the reacting in rotary kiln device with urban life coal gas.Though this method reaction times is short to be 50min, however the temperature of reacting required higher be 873～933K, in addition, used reducing gas contains a large amount of CO toxic gases for life coal gas.There are the technological difficulties of high temperature dynamic seal in the reacting in rotary kiln device, so also there is the shortcoming of the higher and bigger potential safety hazard of energy consumption in this method.
" Chengdu Univ. of Science & Technology's journal " (1984, (3): 27～30) introduced a kind of ammonia that utilizes to ammonium hexavanadate (NH
4)
2V
6O
16Carry out thermal reduction and prepare the method for vanadous oxide.This process is carried out in tube furnace, and ammonia flow is 10 ± 0.5L/h, and temperature of reaction is controlled at 850 ± 50 ℃, and the reaction times is 30min, and cooling can obtain vanadous oxide in ammonia atmosphere.The shortcoming of this method is: the reaction process temperature is too high, and the actual consumption amount of reacting used reductive agent ammonia is 2 times of theoretical consumption.
Chinese patent CN101028938A provides a kind of method of utilizing fluidization technology to prepare vanadous oxide.This method is powder ammonium vanadate or Vanadium Pentoxide in FLAKES (granularity is between 0.05mm～10.00mm) to be joined as furnace charge add in the hot fluidized bed furnace boiler tube, makes the filling ratio of boiler tube reach 10%～55%; In boiler tube, feed industrial gas from the fluidized bed furnace bottom, simultaneously the fluidized bed furnace boiler tube is heated to 600～650 ℃, insulation reduction 3～9 minutes; Come out and the secluding air cooling from discharge port, promptly obtain product.In fact under the pellet density condition of confirming; Too small or excessive particle diameter all can cause operational difficulty for the realization of fluidized, and the wide meeting of feed particles diameter Distribution simultaneously brings bigger operation easier for the control of the residence time of feed particles in reactor drum.This method temperature of reaction is higher simultaneously, and used reducing gas consumption is bigger.
" steel vanadium titanium " (2008,29 (3): 27～30) introduced the method for utilizing fluidization technology reduction ammonium poly-vanadate (APV) to produce vanadous oxide.This method is similar with the method that patent CN101028938A introduces; Different is: be controlled at 650 ℃～750 ℃ rather than 600 ℃～650 ℃; Recovery time was controlled at 5～20 minutes rather than 3～9 minutes, and the grain graininess of used reactant is at 0.067mm～0.25mm rather than 0.05mm～10.00mm.But this method needs higher temperature of reaction, the large usage quantity of reducing gas equally.
" J.Photopolym.Sci.Technol. " (1997; 10 (2): 211-215;) (Synthesis offineparticles of Sn; Ti, and V oxides by laser-induced vapor-phase reaction) introduced the method for the vanadous oxide that utilizes induced with laser method synthesis nano.Used raw material is VOCl
3, through with H
2, O
2With
6.4kpa:1.6kpa mixed after, induced with laser generates V
2O
3Shortcoming is: the raw material VOCl that this method is used
3Itself add the water moulding after by pentachloro-ization two vanadium and coke burden, dry back introduce chlorine gas to make reaction makes, the feedstock production cost is high, is not easy to obtain, and be liquid, is difficult for storage, receives the heat-flash decomposition can emit poisonous gas, be prone to set off an explosion.In addition, the raw material chance time of tide is corrosive to most metal, and is therefore strict to production unit.
Chinese patent CN101717117A provides a kind of ammonium vanadate or Vanadium Pentoxide in FLAKES and sticker, carbon dust has been mixed and made into pelletizing, in reducing gas, reacts the method for preparing vanadous oxide then.This method be with ammonium vanadate or Vanadium Pentoxide in FLAKES powder with make ball after stickers such as dextrin, starch, wilkinite, water glass mix in mixing machine; Join pelletizing in the reactor drum continuously after the drying; And reducing gas such as reverse feeding industrial gas, hydrogen, ammonia or Sweet natural gas; React 10～30min down at 500～650 ℃, under the protection of secluding air or rare gas element argon gas, be cooled to 100 ℃ at last and obtain vanadous oxides.The shortcoming of this method is: not only need use stickers such as dextrin, starch, water glass in the preparation process increases impurity to reaction system, influences the quality purity of product, and temperature of reaction is higher simultaneously, and this technological process is complicated, and the production cycle is longer.
Chinese patent CN101817558A discloses a kind of industrial microwave oven that utilizes ammonium vanadate has been reduced the method for preparing vanadous oxide.Ammonium vanadate is heated to 600～900 ℃ in the industrial microwave oven of reducing gas or inert atmosphere protection, the recovery time is 5～60min, finally obtains vanadous oxide.The shortcoming of this method is that temperature of reaction is too high, and energy consumption is bigger, and the gas vol that consumes in the reaction process simultaneously is bigger, has increased production cost.
It is the method for feedstock production nano grade vanadium trioxide with the Vanadium Pentoxide in FLAKES that Chinese patent CN1300002C discloses a kind of.This method is earlier with V
2O
5And H
2C
2O
4Backflow 2h obtains VOC in absolute ethyl alcohol
2O
4Ethanolic soln, reduction obtains nano level V under the condition of HTHP then
2O
3This method steps is complicated, need prepare intermediate VOC in advance for obtaining nano grade vanadium trioxide
2O
4, increased preparation cost.In addition, the raw material of this method only is confined to Vanadium Pentoxide in FLAKES.
It is the method that feedstock production has the vanadous oxide of crystal formation with the Vanadium Pentoxide in FLAKES that Chinese patent CN1724385A discloses a kind of.This method through solvent method make Vanadium Pentoxide in FLAKES under the pressure condition of 200～300 ℃ temperature and 3～15Mpa, reaction is 0.5～5h, obtains vanadous oxide.The used raw material of this method only is limited as Vanadium Pentoxide in FLAKES.
It is the method for feedstock production vanadium sesquioxide powder with the vanadium tetraoxide that Chinese patent CN1974407A provides a kind of.Temperature of reaction is 550～600 ℃ in this method, and the reaction times is less than 3min, and used reducing gas comprises industrial gas, hydrogen or ammonia.The shortcoming of this method is: temperature of reaction is higher, and the raw material vanadium tetraoxide is not easy to obtain simultaneously, and price is more expensive.
" Zhongshan University's journal " (natural science edition) (2003,42 (1): 116～118) introduced: at H
2In the atmosphere to vanadyl (IV) basic carbonate ammonium (NH
4)
5[(VO)
6(CO
3)
4(OH)
9] 10H
2O obtains the spherical pure V of the about 30nm of granularity under the condition of 900 ℃ of insulation 30min
2O
3Powder.The shortcoming of this method is: temperature of reaction is too high, and reaction raw materials vanadyl (IV) basic carbonate ammonium is difficult simultaneously obtains, and synthetic cost is high, is difficult to realize suitability for industrialized production.
In sum, produce the used raw material of vanadous oxide and be ammonium meta-vanadate, many (gathering) ammonium vanadate or Vanadium Pentoxide in FLAKES mostly, and other raw materials such as VOCl
3, existence such as vanadyl (IV) basic carbonate ammonium problem such as is difficult to obtain.And current working method all exists some drawback or weak point.On the one hand; When using ammonium meta-vanadate or ammonium poly-vanadate, need to pass through the reduction reaction process like reducing gas such as life coal gas, industrial gas, hydrogen or carbonaceous reducing agent (600 ℃～1000 ℃) under the condition of high temperature and prepare with a large amount of reductive agents as the feedstock production vanadous oxide; The industriallization equipment used is used rotary reactor more at present, has the technological difficulties of high temperature dynamic seal, is easy to generate the leakage of reducing gas, makes Working environment have bigger danger and contaminative; The fluidization reaction does not still have the industrialized unit report, itself has technological difficulties of fluidisation control or the like yet; Thereby the method that has also need use the sticker granulation to introduce impurity element, influences quality product.On the other hand, some method uses Vanadium Pentoxide in FLAKES to be raw material, though can realize producing the simplification of vanadous oxide technological process.But Vanadium Pentoxide in FLAKES is to be decomposed to produce by ammonium meta-vanadate or many (gathering) ammonium vanadate heated oxide to obtain in the industry; Just there is very high cost in itself; The process environment of suitability for industrialized production Vanadium Pentoxide in FLAKES pollutes bigger simultaneously; When using Vanadium Pentoxide in FLAKES as the feedstock production vanadous oxide, just meaning has increased extra preparation raw materials cost and Environmental costs.
Therefore, the production of vanadous oxide needs a kind of novel method that overcomes above drawback, simplifies production technique, reduces production costs.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of vanadous oxide powder.This preparing method's production technique is simple, cost is low, is raw material with the vannadate, preparation vanadous oxide powder in closely critical or supercritical medium.
The objective of the invention is to realize through following technical scheme:
A kind of preparation method of vanadous oxide powder, this method comprises the steps: vannadate is joined in the reactor drum, and adds organic solvent; To the reactor drum heating, make temperature of reactor reach 150～450 ℃, pressure reaches 1.5～25.0Mpa; And under this state, keep 0.1～6.0h, and reduce reactor pressure to 0～5.0Mpa then, isolate organic solvent; Stop heating, when the question response actuator temperature is reduced to room temperature, can obtain the vanadous oxide powder.
The preparation method of described a kind of vanadous oxide powder, its described vannadate comprises one or both mixtures in ammonium meta-vanadate and many (gathering) ammonium vanadate.
The preparation method of described a kind of vanadous oxide powder; Its organic solvent comprises methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, sulfur alcohol, propylmercaptan, formic acid, acetate, n-caproic acid, acetone, 2-butanone, pimelinketone, N, one or both in the dinethylformamide or multiple mixed solvent.
The preparation method of described a kind of vanadous oxide powder, it reduces reactor pressure to 0～5.0Mpa and is meant that the used time of step-down process is 0.1～3.0h.
The preparation method of described a kind of vanadous oxide powder, its organic solvent is reusable after separating purification.
The preparation method of described a kind of vanadous oxide powder, its temperature of reactor is reduced to room temperature and is meant through naturally cooling or forces the refrigerative method that reactor drum is lowered the temperature.Vannadate is joined in the reactor drum, and add organic solvent,, make temperature of reactor reach 150～450 ℃ the reactor drum heating; Pressure reaches 1.5～25.0Mpa, and under this state sustained reaction 0.1～6.0h, reduce reactor pressure then; Isolate organic solvent, and the condensation and collection distillate, system pressure drops to 0～5.0Mpa; Stop heating, when temperature is reduced to room temperature in the question response device, can obtain the vanadous oxide powder.
In the present invention, organic solvent can reclaim after reaction finishes, and reuses through separating the back of purifying again.
In operation steps; Used raw material is one or both mixtures of ammonium meta-vanadate, many (gathering) ammonium vanadate; But not Vanadium Pentoxide in FLAKES; So just omitted the process that is prepared Vanadium Pentoxide in FLAKES by ammonium vanadate, thereby the production energy consumption of the synthetic vanadous oxide of this method reduces, reduces environmental pollution, reduces cost, technological process is also simplified.
Wherein, Used organic solvent is methyl alcohol, ethanol, methyl alcohol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, sulfur alcohol, propylmercaptan, organic acid formic acid, acetate, n-caproic acid, acetone, 2-butanone, pimelinketone, N, one or both in the dinethylformamide or multiple mixed solvent.
In operation steps, used temperature of reaction is 150～450 ℃, is lower than the required high temperature of traditional reduction method (600 ℃～1000 ℃), reduces energy consumption.
In the present invention, used reaction pressure is 1.5～25.0Mpa; Reaction times is 0.1～6.0h.
In the present invention; Under temperature of reaction and pressure condition; Solvent for use has reached nearly critical (Near-Critical) or overcritical (Super-Critical) state, makes the decomposition-reduction reaction process of ammonium vanadate in nearly critical or postcritical medium, carry out, and improves speed of reaction.
Advantage of the present invention and effect are:
The whole process operation of the present invention is simple; Raw materials used and organic solvent is cheap, be easy to get; Reduced the raw materials cost of producing vanadous oxide, in closely critical or supercritical medium system, prepared vanadous oxide, the reaction times is short, temperature of reaction is low; Use ammonium vanadate to be raw material, energy-conserving and environment-protective with Vanadium Pentoxide in FLAKES as raw material.
Description of drawings
Fig. 1 is V
2O
3The XRD spectra of powder.
Annotate: figure of the present invention is the analysis synoptic diagram of product state, the unintelligible understanding that does not influence technical scheme of the present invention of figure Chinese words.
Embodiment
With reference to the accompanying drawings the present invention is elaborated.
Embodiment 1:
The mixture of 60.0g ammonium meta-vanadate and ammonium poly-vanadate is placed reactor drum, add the mixed solvent of 240mL ethanol and 120mL Virahol, after the reactor drum sealing; Be heated to 242 ℃, reactor pressure is 6.1Mpa, and under this condition, reacts 1.0h; Under the situation of 242 ℃ of maintenances, behind reactor drum pressure release 1.6h, pressure becomes 0; Distillate is collected in pressure release simultaneously, stops heating, lets reactor drum naturally cool to room temperature.In reactor drum, obtain the vanadous oxide black powder, quality is 35.4g.
Embodiment 2:
Take by weighing the 10.0g ammonium meta-vanadate and place 1L volumetrical reactor drum, add the 345mL absolute ethyl alcohol, after the reactor drum sealing, reactor drum vacuumized emptying gas after; Heating at 250 ℃, is reacted 0.2h under the condition of 7.1MPa, under the situation that keeps temperature; With the slow pressure release of reactor drum, collect distillate, behind the 0.8h, pressure becomes 3.0Mpa; Temperature is 260 ℃, and powered-down lets the reactor drum naturally cooling.Obtaining the 6.0g product is black vanadous oxide powder.
Embodiment 3:
Take by weighing the 30.0g ammonium meta-vanadate and place reactor drum, add the 350mL absolute ethyl alcohol, after the reactor drum sealing, heating; At 240 ℃, react 3.0h under the condition of 6.5Mpa, under the situation that keeps temperature, with the slow pressure release of reactor drum; Collect distillate, when reactor pressure is reduced to 5.0Mpa, powered-down; Let the reactor drum naturally cooling, separate reactor internal solvent and solid product, after drying, obtaining the 17.0g product is black vanadous oxide powder.
Embodiment 4:
52.0g many (gathering) ammonium vanadate places reactor drum, the adding solvent is an acetate, and add-on is 340mL, after air eliminates in the reactor drum; Reactor drum is heated to 300 ℃, and pressure is 5.5Mpa, and under this condition, reacts 0.1h, after reaction finishes; With the slow pressure release 2.7h of reactor drum, collect distillate, when reactor pressure becomes 0.5Mpa; Temperature is increased to 310 ℃, and powered-down cools off reactor drum with water of condensation fast.Obtain the 28.4g product, be black vanadous oxide powder.
Embodiment 5:
Take by weighing the mixture of 49.8g many (gathering) ammonium vanadate and ammonium meta-vanadate, join in the reactor drum, add 343mL n-caproic acid and ethanol mixed solvent then, reactor drum is heated; Be warming up to 260 ℃, pressure reaches 5.8Mpa, and reacts 4.4h under these conditions; Under the situation that keeps temperature, the solvent in the reactor drum is slowly released, and collect distillate simultaneously; When reactor pressure became 2.6Mpa, powered-down let the reactor drum naturally cooling.Collection obtains the 29.5g product, is black vanadous oxide powder.
Embodiment 6:
Take by weighing 20.0g many (gathering) ammonium vanadate and 20.0g ammonium meta-vanadate respectively, both are scattered in the mixed solvent of 150mL methyl alcohol and 200mL propylmercaptan, above-mentioned aaerosol solution is placed in the reactor drum, be heated to 238 ℃; 6.4Mpa condition under react 0.9h, keeping under the situation of temperature, the slow pressure release of reactor drum; Collect distillate, behind the 1.7h, pressure becomes 4.1Mpa; Temperature is 246 ℃, and powered-down lets the reactor drum naturally cooling.Obtain the 23.3g product, be black vanadous oxide powder.
Embodiment 7:
The 58.0g ammonium meta-vanadate is placed reactor drum, to wherein adding the 358mL pimelinketone, with reactor drum with water pump vacuumize eliminate air after; Begin heating, it is 5.5h that temperature of reactor and pressure are respectively 390 ℃, 4.5Mpa reaction times, under the situation of maintenance temperature; In 2.1h, leak out solvent, collect distillate, temperature rises to 397 ℃; Powered-down is forced to make reactor cooling, in reactor drum, collects V
2O
3Powder 36.1g.
Embodiment 8:
Take by weighing the 40.0g ammonium meta-vanadate and place 1L volumetrical reactor drum, add the 342mL2-butanone, after the reactor drum sealing, reactor drum vacuumized emptying gas after, heating; At 265 ℃, react 6.0h under the condition of 4.3Mpa, under the situation that keeps temperature, with the slow pressure release of reactor drum; Collect distillate, behind the 3.6h, pressure becomes 3.0Mpa, powered-down; Let the reactor drum naturally cooling, separate reactor internal solvent and solid product obtain the 23.4g product after drying, be black vanadous oxide powder.
Claims (3)
1. the preparation method of a vanadous oxide powder is characterized in that this method comprises the steps: vannadate is joined in the reactor drum, and adds organic solvent; To the reactor drum heating, make temperature of reactor reach 150～450 ℃, pressure reaches 1.5～25.0MPa; And under this state, keep 0.1～6.0h, and reduce reactor pressure to 0～5.0MPa then, isolate organic solvent; Stop heating, when the question response actuator temperature is reduced to room temperature, can obtain the vanadous oxide powder;
Described vannadate is one or both mixtures in ammonium meta-vanadate and the poly ammonium vanadate; Organic solvent is methyl alcohol, ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, sulfur alcohol, propylmercaptan, formic acid, acetate, n-caproic acid, acetone, 2-butanone, pimelinketone, N, one or both in the dinethylformamide or multiple mixed solvent; Reduce reactor pressure to 0～5.0MPa and be meant that the used time of step-down process is 0.1～3.0h.
2. the preparation method of a kind of vanadous oxide powder according to claim 1 is characterized in that organic solvent is reusable after separating purification.
3. the preparation method of a kind of vanadous oxide powder according to claim 1 is characterized in that temperature of reactor reduces to room temperature and be meant through naturally cooling or force the refrigerative method that reactor drum is lowered the temperature.
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| CN103633309A (en) * | 2013-12-13 | 2014-03-12 | 黑龙江大学 | Preparation method of core-shell structure vanadium trioxide microspheres |
| WO2017208892A1 (en) * | 2016-05-30 | 2017-12-07 | コニカミノルタ株式会社 | Process for producing vanadium-dioxide-containing particles |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724385A (en) * | 2005-06-03 | 2006-01-25 | 武汉大学 | Process for preparing crystal vanadium trioxide |
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|---|---|---|---|---|
| CN1724385A (en) * | 2005-06-03 | 2006-01-25 | 武汉大学 | Process for preparing crystal vanadium trioxide |
Non-Patent Citations (2)
| Title |
|---|
| F. Sediri et al..Hydrothermal synthesis and characterization of V2O3.《Materials Science and Engineering B》.2005,第123卷第136-138页. * |
| Tie-Zhen Ren et al..Crystal growth of mixed-valence ammonium vanadates.《Cryst. Res. Technol.》.2007,第42卷(第4期),第317-320页. * |
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