CN108314083B - Method for preparing vanadium trioxide from vanadium-containing solution - Google Patents
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Abstract
The invention relates to a method for preparing vanadium trioxide by using a vanadium-containing solution, which comprises the following steps: adding an organic amine compound into the vanadium-containing solution for vanadium precipitation reaction, and performing solid-liquid separation after the reaction is finished to obtain a vanadium-containing complex and a vanadium precipitation supernatant; and calcining the obtained vanadium-containing complex for reduction reaction to obtain vanadium trioxide after the reaction is finished. The invention introduces the organic amine compound as a vanadium precipitation agent, can form large-particle vanadium-containing complex, and reduces Fe in a liquid phase3+、SO4 2‑、SiO3 2‑The product purity is improved due to the entrainment of soluble harmful impurities; the carbon element in the vanadium-containing complex and the hydrogen generated by decomposition in the reaction process can also serve as a reducing agent in the reduction preparation of vanadium trioxide, and no additional reducing agent is needed, so that the production cost is greatly reduced. The invention has the advantages of feasible technology, simple equipment, easy realization of automation, good economic benefit and wide application prospect.
Description
Technical Field
The invention relates to the technical field of vanadium chemical metallurgy, in particular to a method for preparing vanadium trioxide by using a vanadium-containing solution.
Background
Vanadium trioxide is an important vanadium metal oxide and can be applied to industrial departments of metallurgy, electronics, chemical industry and the like. Vanadium trioxide is an ideal raw material for producing vanadium series alloy, and has more excellent characteristics than other vanadium oxides in the process of producing ferrovanadium and vanadium-nitrogen alloy. In addition, the vanadium trioxide has the property of metal-nonmetal transition, the low-temperature phase change characteristic is good, the resistance mutation can reach 6 orders of magnitude, and the vanadium trioxide is a monoclinic antiferromagnetic semiconductor group at low temperature along with the change of crystal lattices and antiferromagnetic properties, so that the vanadium trioxide has wide application prospects in low-temperature devices due to the excellent low-temperature phase change performance.
At present, the method for preparing vanadium trioxide mainly comprises two methods: one is ammonium metavanadate or ammonium polyvanadate thermolysis pyrolysis method without adding reducing agent, for example CN101028938A has provided a method for producing powdered vanadium trioxide, utilize and heat the initial hydrogen produced by pyrolysis of ammonia released while heating ammonium metavanadate to reduce ammonium metavanadate, this method does not adopt and adds reducing gas, although can reduce some costs, the ammonia pyrolysis that the raw materials decompose is incomplete, not merely cause the reducing atmosphere to be insufficient, and the ammonia that does not split will cause the environmental pollution by the exclusion.
Another method for preparing vanadium trioxide is a direct high-temperature reduction method with an additional reducing agent, which is often C, NH3、H2、CH4CO or industrial gas and the like are used as reducing agents, and high-valence vanadium compounds such as ammonium metavanadate, ammonium polyvanadate, vanadium pentoxide and the like are thermally reduced to obtain vanadium trioxide, and the method is also a method for preparing vanadium trioxide which is widely applied at present. For example, CN103922404A provides a method for preparing vanadium trioxide by reducing vanadium pentoxide with carbon without the need of a protective atmosphere or vacuum. The method comprises the following specific steps: a. preparing materials: mixing vanadium pentoxide and carbon powder at a molar ratio of 2: 1; b. pressing materials: pressing the raw materials mixed in the step a into a material block, and covering carbon powder on the material block; c. firing: and c, firing the material block formed in the step b at 950-1050 ℃ for 3-5h to obtain vanadium trioxide. The invention does not need protective gas atmosphere or vacuum condition, has simple operation and lower cost, but adds burdening and ball pressing procedures.
Although the method can effectively prepare vanadium trioxide, the method generally has the disadvantages of complex process, serious environmental pollution and high production cost. At present, a preparation process of vanadium trioxide, which is simple in process, environment-friendly and low in production cost, is urgently needed.
Disclosure of Invention
In view of the problems in the prior art, the invention provides a method for preparing vanadium trioxide from a vanadium-containing solution, wherein an organic amine compound is introduced as a vanadium precipitation agent to carry out vanadium precipitation reaction, so that the product purity is improved, and the vanadium trioxide can be used as a reducing agent to carry out reduction reaction, so that the production cost is reduced. The technology is feasible, simple in equipment, easy to realize automation and good in application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for preparing vanadium trioxide from a vanadium-containing solution, which comprises the following steps:
(1) adding an organic amine compound into the vanadium-containing solution for vanadium precipitation reaction, and performing solid-liquid separation after the reaction is finished to obtain a vanadium-containing complex and a vanadium precipitation supernatant;
(2) calcining the vanadium-containing complex obtained in the step (1), and carrying out reduction reaction by using carbon element in the vanadium-containing complex and hydrogen decomposed in the reaction process as reducing agents to obtain vanadium trioxide after the reaction is finished.
The invention utilizes the organic amine compound as the vanadium precipitation agent to carry out vanadium precipitation reaction, can form large-particle vanadium-containing complex, and reduces Fe in liquid phase3+、SO4 2-、SiO3 2-The product purity is improved due to the entrainment of soluble harmful impurities; the carbon element in the vanadium-containing complex and the hydrogen generated by decomposition in the reaction process (after the vanadium-containing complex decomposes ammonia gas, the ammonia gas decomposes to generate hydrogen) can be used as a reducing agent in the reduction preparation of vanadium trioxide, and no reducing agent is added, so that the production cost is greatly reduced.
The vanadium-containing solution is a solution containing vanadium element, preferably a purified vanadium solution.
The organic amine compound is an organic substance generated by the chemical reaction of an organic substance and ammonia, and can be any one or the combination of at least two of aliphatic amines, alcamines, amides, alicyclic amines, aromatic amines, naphthalene amines and other amines; for example, monomethylamine, dipropylamine, n-butylamine, 1, 2-dimethylpropylamine, ethylenediamine, monoethanolamine, formamide, diphenylamine, 2-naphthylamine, hydroxylamine, and the like, for reasons of space and brevity. The present invention is not exhaustive.
According to the invention, the molar ratio of vanadium in the vanadium-containing solution in step (1) to nitrogen in the organic amine compound is (0.5-3):1, and may be, for example, 0.5:1, 1:1, 1.5:1, 2:1, 2.5:1 or 3:1, and the specific values between the above values are limited to space and for the sake of brevity and are not exhaustive.
According to the invention, the pH of the solution is adjusted to 1.0-7.0, for example 1,2, 3, 4, 5, 6 or 7 during the vanadium precipitation reaction in step (1), and the specific values between the above values are not exhaustive for reasons of space and simplicity.
According to the present invention, the temperature of the vanadium precipitation reaction in step (1) is 30-60 ℃, for example, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃ or 60 ℃, and the specific values therebetween are limited by space and for brevity, and the present invention is not exhaustive.
According to the invention, before the calcination in the step (2), the vanadium-containing complex obtained in the step (1) is refined and sodium-removed, and the method comprises the following steps: and (2) mixing the vanadium-containing complex obtained in the step (1) with acid liquor to carry out sodium removal reaction, and carrying out solid-liquid separation after the reaction is finished to obtain a refined vanadium-containing complex.
The present invention can select acid solution commonly used in the art for sodium removing reaction, for example, hydrochloric acid, sulfuric acid, nitric acid, etc., but not limited thereto, and other suitable acid solution is also suitable for the present invention.
According to the invention, the acid solution has a concentration of 10-20 wt%, for example 10 wt%, 11 wt%, 12 wt%, 13 wt%, 14 wt%, 15 wt%, 16 wt%, 17 wt%, 18 wt%, 19 wt% or 20 wt%, and the specific values between the above values, which are limited by space and for the sake of brevity, are not exhaustive.
According to the invention, the liquid-solid ratio of the vanadium-containing complex to the acid solution in the refined sodium removal process is (2-5):1, for example, 2:1, 2.5:1, 3:1, 3.5:1, 4:1, 4.5:1 or 5:1, and the specific values between the above values are limited by space and for the sake of brevity, and are not exhaustive.
The unit of the liquid-solid ratio is mL/g.
According to the invention, the temperature of the sodium removal reaction is 20-50 ℃, for example 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃ or 50 ℃, and the specific values between the above values are limited by space and for the sake of brevity, and are not exhaustive.
According to the invention, the stirring is carried out during the refined sodium removal at a speed of 50-500r/min, such as 50r/min, 100r/min, 150r/min, 200r/min, 250r/min, 300r/min, 350r/min, 400r/min, 450r/min or 500r/min, and the specific values therebetween are limited to space and for the sake of brevity and are not exhaustive.
According to the present invention, the temperature of the calcination in step (2) is 700-.
According to the invention, the calcination time in step (2) is 10-120min, for example, 10min, 20min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min or 120min, and the specific values therebetween are not limited to the space and for the sake of brevity, and the invention is not exhaustive.
The calcination in step (2) of the present invention is preferably performed in a rotary kiln, but is not limited thereto, and other apparatuses capable of performing calcination are also suitable for the present invention.
According to the invention, the gas discharged in the calcining process in the step (2) is ignited for recycling after being collected, and can be used for adjusting the pH value of the solution in the vanadium precipitation reaction process in the step (1).
The solid-liquid separation operation is carried out by the method commonly used in the field, such as filtration, suction filtration, centrifugation, sedimentation and the like, but the method is not limited to the operation and should be specifically selected according to the actual situation.
As a preferred technical scheme, the method for preparing vanadium trioxide by using the vanadium-containing solution comprises the following steps:
(1) adding an organic amine compound into the vanadium-containing solution according to the vanadium-nitrogen molar ratio of (0.5-3) to 1 to carry out vanadium precipitation reaction, adjusting the pH to be 1.0-7.0 in the reaction process, controlling the reaction temperature to be 30-60 ℃, and carrying out solid-liquid separation after the reaction is finished to obtain a vanadium-containing complex and a vanadium precipitation supernatant;
(2) mixing the vanadium-containing complex obtained in the step (1) with acid liquor with the concentration of 10-20 wt% to carry out sodium removal reaction, controlling the liquid-solid ratio to be (2-5):1 in the reaction process, controlling the temperature to be 20-50 ℃, stirring at the speed of 50-500r/min, and carrying out solid-liquid separation after the reaction is finished to obtain a refined vanadium-containing complex;
(3) and (3) heating the refined vanadium-containing complex obtained in the step (2) to 700-900 ℃ in a rotary kiln, calcining for 10-120min, performing reduction reaction by using carbon element in the vanadium-containing complex and hydrogen decomposed in the reaction process as reducing agents, collecting dust from gas discharged in the calcining process, igniting and recovering, and adjusting the pH value of the solution in the vanadium precipitation reaction process in the step (1) to obtain vanadium trioxide after the reaction is finished.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) the organic amine medicament introduced by the invention can be used as a vanadium precipitation agent in a vanadium precipitation reaction to form a large-particle vanadium complex, so that Fe in a liquid phase is reduced3+、SO4 2-、SiO3 2-And soluble harmful impurities are carried, so that the product purity is improved.
(2) The vanadium-containing complex formed by introducing the organic amine compound can be used as a reducing agent at high temperature, and the carbon element contained in the vanadium-containing complex and hydrogen decomposed in the reaction process are used for reduction reaction, so that the reducing agent is not added, and the production cost is greatly reduced.
(3) The invention has the advantages of feasible technology, simple equipment, low production cost, easy realization of automation and good application prospect.
Drawings
FIG. 1 is a process flow diagram provided by one embodiment of the present invention, wherein the S-solid phase, L-liquid phase, and G-gas phase.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
As shown in fig. 1, a process flow provided by one embodiment of the present invention may be: adding organic amine into the purified vanadium liquid, adjusting the pH value, controlling the reaction temperature to carry out vanadium precipitation reaction, and filtering and separating after the reaction is finished to obtain a solid-phase vanadium-containing complex and a liquid-phase vanadium precipitation supernatant; mixing the obtained vanadium-containing complex with acid liquor for sodium removal reaction, filtering and separating after the reaction is finished to obtain a solid-phase refined vanadium-containing complex, wherein the obtained liquid phase can be used for adjusting the pH value in the vanadium precipitation process; and (3) carrying out reduction calcination on the refined vanadium-containing complex, purifying the gas phase generated in the calcination process, and then adjusting the pH value in the vanadium precipitation process, thus obtaining a vanadium trioxide product after the calcination is finished.
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
(1) Adding ethylenediamine into the purified vanadium liquid with the vanadium concentration of 25.32g/L according to the vanadium-nitrogen molar ratio of 3:1, adjusting the pH to 5.0, carrying out vanadium precipitation reaction at the reaction temperature of 50 ℃, and filtering after the reaction is finished to obtain a solid phase vanadium-containing complex and a vanadium precipitation supernatant;
(2) adding the vanadium-containing complex obtained in the step (1) into hydrochloric acid with the concentration of 10 wt% for carrying out sodium removal reaction, controlling the liquid-solid ratio to be 5:1 in the reaction process, stirring at the temperature of 30 ℃ at the speed of 300r/min, and filtering after the reaction is finished to obtain filtrate and refined vanadium-containing complex;
(3) and (3) adding the refined vanadium-containing complex obtained in the step (2) into a closed rotary kiln for calcination, wherein the calcination temperature is 900 ℃, the heat preservation time is 30min, a reduction reaction is carried out by using a carbon element in the vanadium-containing complex and hydrogen decomposed in the reaction process, and a vanadium trioxide product is obtained after the reaction is finished.
Through detection, according to the mass percentage content, the vanadium content of the vanadium trioxide obtained in the embodiment is 64.65%, and the impurity content of Na: 0.43%, Si: 0.28%, Fe: 0.25%, P: 0.15 percent.
Example 2
(1) Adding ethylenediamine into the purified vanadium liquid with the vanadium concentration of 20.16g/L according to the vanadium-nitrogen molar ratio of 2.5:1, adjusting the pH value to 3.0, carrying out vanadium precipitation reaction at the reaction temperature of 40 ℃, and filtering after the reaction is finished to obtain a solid-phase vanadium-containing complex and a vanadium precipitation supernatant;
(2) adding the vanadium-containing complex obtained in the step (1) into hydrochloric acid with the concentration of 12 wt% for carrying out sodium removal reaction, controlling the liquid-solid ratio to be 4:1 in the reaction process, stirring at the temperature of 40 ℃ at the speed of 500r/min, and filtering after the reaction is finished to obtain filtrate and refined vanadium-containing complex;
(3) and (3) adding the refined vanadium-containing complex obtained in the step (2) into a closed rotary kiln for calcination, wherein the calcination temperature is 850 ℃, the heat preservation time is 60min, a carbon element in the vanadium-containing complex and hydrogen decomposed in the reaction process are utilized for reduction reaction, discharged gas in the calcination process is ignited for recovery after dust collection, and the refined vanadium-containing complex can be used for adjusting the pH value of the solution in the vanadium precipitation reaction process in the step (1), and a vanadium trioxide product is obtained after the reaction is completed.
Through detection, according to the mass percentage content, the vanadium content of the vanadium trioxide obtained in the embodiment is 63.89%, and the impurity content Na: 0.51%, Si: 0.23%, Fe: 0.29%, P: 0.11 percent.
Example 3
(1) Adding ethylenediamine into the purified vanadium liquid with the vanadium concentration of 28.07g/L according to the vanadium-nitrogen molar ratio of 1.5:1, adjusting the pH value to 5.0, carrying out vanadium precipitation reaction at the reaction temperature of 60 ℃, and filtering after the reaction is finished to obtain a solid phase vanadium-containing complex and a vanadium precipitation supernatant;
(2) adding the vanadium-containing complex obtained in the step (1) into sulfuric acid with the concentration of 14 wt% for carrying out sodium removal reaction, controlling the liquid-solid ratio to be 4:1 in the reaction process, stirring at the temperature of 50 ℃ at the speed of 200r/min, and filtering after the reaction is finished to obtain filtrate and refined vanadium-containing complex;
(3) and (3) adding the refined vanadium-containing complex obtained in the step (2) into a closed rotary kiln for calcination, wherein the calcination temperature is 700 ℃, the heat preservation time is 120min, a reduction reaction is carried out by using a carbon element in the vanadium-containing complex and hydrogen decomposed in the reaction process, and a vanadium trioxide product is obtained after the reaction is finished.
Through detection, according to the mass percentage content, the vanadium content of the vanadium trioxide obtained in the embodiment is 63.45%, and the impurity content Na: 0.53%, Si: 0.24%, Fe: 0.26%, P: 0.13 percent.
Example 4
(1) Adding ethylenediamine into the purified vanadium liquid with the vanadium concentration of 23.07g/L according to the vanadium-nitrogen molar ratio of 1:1, adjusting the pH to 2.0 to carry out vanadium precipitation reaction at the reaction temperature of 35 ℃, and filtering after the reaction is finished to obtain a solid phase vanadium-containing complex and a vanadium precipitation supernatant;
(2) adding the vanadium-containing complex obtained in the step (1) into hydrochloric acid with the concentration of 16 wt% for carrying out sodium removal reaction, controlling the liquid-solid ratio to be 2:1 in the reaction process, stirring at the temperature of 30 ℃ at the speed of 100r/min, and filtering after the reaction is finished to obtain filtrate and refined vanadium-containing complex;
(3) and (3) adding the refined vanadium-containing complex obtained in the step (2) into a closed rotary kiln for calcination, wherein the calcination temperature is 750 ℃, the heat preservation time is 90min, a carbon element in the vanadium-containing complex and hydrogen decomposed in the reaction process are utilized for reduction reaction, discharged gas in the calcination process is ignited for recovery after dust collection, and the refined vanadium-containing complex can be used for adjusting the pH value of the solution in the vanadium precipitation reaction process in the step (1), and a vanadium trioxide product is obtained after the reaction is completed.
Through detection, according to the mass percentage content, the vanadium content of the vanadium trioxide obtained in the embodiment is 64.56%, and the impurity content of Na: 0.48%, Si: 0.26%, Fe: 0.23%, P: 0.10 percent.
Example 5
(1) Adding ethylenediamine into the purified vanadium liquid with the vanadium concentration of 15.07g/L according to the vanadium-nitrogen molar ratio of 0.5:1, adjusting the pH to 1.0, carrying out vanadium precipitation reaction at the reaction temperature of 30 ℃, and filtering after the reaction is finished to obtain a solid phase vanadium-containing complex and a vanadium precipitation supernatant;
(2) adding the vanadium-containing complex obtained in the step (1) into hydrochloric acid with the concentration of 18 wt% for carrying out sodium removal reaction, controlling the liquid-solid ratio to be 3:1 in the reaction process, stirring at the temperature of 20 ℃ at the speed of 250r/min, and filtering after the reaction is finished to obtain filtrate and refined vanadium-containing complex;
(3) adding the refined vanadium-containing complex obtained in the step (2) into a closed rotary kiln for calcination, wherein the calcination temperature is 820 ℃, the heat preservation time is 10min, carrying out reduction reaction by using carbon element in the vanadium-containing complex and hydrogen decomposed in the reaction process, igniting and recycling gas discharged in the calcination process after dust collection, and being used for adjusting the pH value of the solution in the vanadium precipitation reaction process in the step (1) to obtain a vanadium trioxide product after the reaction is finished.
Through detection, according to the mass percentage content, the vanadium content of the vanadium trioxide obtained in the embodiment is 63.82%, and the impurity content Na: 0.51%, Si: 0.24%, Fe: 0.29%, P: 0.18 percent.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (6)
1. A method for preparing vanadium trioxide from a vanadium-containing solution is characterized by comprising the following steps:
(1) adding an organic amine compound into the vanadium-containing solution for vanadium precipitation reaction, and performing solid-liquid separation after the reaction is finished to obtain a vanadium-containing complex and a vanadium precipitation supernatant; the molar ratio of vanadium in the vanadium-containing solution in the step (1) to nitrogen in the organic amine compound is (0.5-3) to 1;
(2) calcining the vanadium-containing complex obtained in the step (1), and carrying out reduction reaction by using carbon element in the vanadium-containing complex and hydrogen decomposed in the reaction process as a reducing agent to obtain vanadium trioxide after the reaction is finished;
the vanadium-containing solution is a purified vanadium solution;
in the vanadium precipitation reaction process in the step (1), adjusting the pH value of the solution to 1.0-7.0;
the temperature of the vanadium precipitation reaction in the step (1) is 30-60 ℃;
the calcining temperature in the step (2) is 820-900 ℃; the calcining time is 10-120 min;
before the calcination in the step (2), refining and sodium removal are carried out on the vanadium-containing complex obtained in the step (1), and the method comprises the following steps: mixing the vanadium-containing complex obtained in the step (1) with acid liquor with the concentration of 5-20 wt% for sodium removal reaction, and performing solid-liquid separation after the reaction is finished to obtain a refined vanadium-containing complex;
the liquid-solid ratio of the vanadium-containing complex to the acid liquor in the refining and sodium removal process is (2-5): 1.
2. The method of claim 1, wherein the temperature of the sodium removal reaction is 20-50 ℃.
3. The method of claim 1, wherein stirring is performed during the fine sodium removal at a rate of 50 to 500 r/min.
4. The method of claim 1, wherein said calcining of step (2) is performed in a rotary kiln.
5. The method of claim 1, wherein the gas discharged in the calcining process in the step (2) is ignited for recycling after dust collection, and can be used for adjusting the pH value of the solution in the vanadium precipitation reaction process in the step (1).
6. The method of claim 1, wherein the method comprises the steps of:
(1) adding an organic amine compound into the vanadium-containing solution according to the vanadium-nitrogen molar ratio of (0.5-3) to 1 to carry out vanadium precipitation reaction, adjusting the pH to be 1.0-7.0 in the reaction process, controlling the reaction temperature to be 30-60 ℃, and carrying out solid-liquid separation after the reaction is finished to obtain a vanadium-containing complex and a vanadium precipitation supernatant;
(2) mixing the vanadium-containing complex obtained in the step (1) with acid liquor with the concentration of 10-20 wt% to carry out sodium removal reaction, controlling the liquid-solid ratio to be (2-5):1 in the reaction process, controlling the temperature to be 20-50 ℃, stirring at the speed of 50-500r/min, and carrying out solid-liquid separation after the reaction is finished to obtain a refined vanadium-containing complex;
(3) and (3) heating the refined vanadium-containing complex obtained in the step (2) to 820-900 ℃ in a rotary kiln, calcining for 10-120min, performing reduction reaction by using carbon element in the vanadium-containing complex and hydrogen decomposed in the reaction process as reducing agents, collecting dust from gas discharged in the calcining process, igniting and recovering, and adjusting the pH value of the solution in the vanadium precipitation reaction process in the step (1) to obtain vanadium trioxide after the reaction is finished.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001233616A (en) * | 2000-02-22 | 2001-08-28 | Shinko Kagaku Kogyo Kk | Production of vanadium (iii) oxide |
| CN1347856A (en) * | 2001-11-23 | 2002-05-08 | 中山大学 | Nanometer V2O3-based powder and its prepn |
| CN101817558A (en) * | 2010-04-01 | 2010-09-01 | 长沙隆泰微波热工有限公司 | Production method of vanadium trioxide |
| CN101993111A (en) * | 2010-10-21 | 2011-03-30 | 沈阳化工大学 | Method for preparing nanometer vanadous oxide |
| CN102560635A (en) * | 2012-03-21 | 2012-07-11 | 电子科技大学 | Preparation method of vanadium trioxide film |
| CN105197995A (en) * | 2015-09-11 | 2015-12-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing vanadium trioxide |
| CN106044854A (en) * | 2016-08-05 | 2016-10-26 | 北京有色金属研究总院 | Preparation method of submicron-level vanadium trioxide powder |
| CN106935860A (en) * | 2017-03-24 | 2017-07-07 | 华中科技大学 | A kind of carbon intercalation V2O3Nano material, its preparation method and application |
| CN107434259A (en) * | 2017-08-09 | 2017-12-05 | 河钢股份有限公司承德分公司 | A kind of method by preparing vanadium trioxide containing vanadium solution |
| CN107591522A (en) * | 2017-08-22 | 2018-01-16 | 中南大学 | A kind of preparation method of the spherical V2O3/C materials of sodium-ion battery negative pole |
| CN107662946A (en) * | 2017-08-11 | 2018-02-06 | 攀枝花学院 | The preparation method of vanadium trioxide |
-
2018
- 2018-04-04 CN CN201810296853.2A patent/CN108314083B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001233616A (en) * | 2000-02-22 | 2001-08-28 | Shinko Kagaku Kogyo Kk | Production of vanadium (iii) oxide |
| CN1347856A (en) * | 2001-11-23 | 2002-05-08 | 中山大学 | Nanometer V2O3-based powder and its prepn |
| CN101817558A (en) * | 2010-04-01 | 2010-09-01 | 长沙隆泰微波热工有限公司 | Production method of vanadium trioxide |
| CN101993111A (en) * | 2010-10-21 | 2011-03-30 | 沈阳化工大学 | Method for preparing nanometer vanadous oxide |
| CN102560635A (en) * | 2012-03-21 | 2012-07-11 | 电子科技大学 | Preparation method of vanadium trioxide film |
| CN105197995A (en) * | 2015-09-11 | 2015-12-30 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing vanadium trioxide |
| CN106044854A (en) * | 2016-08-05 | 2016-10-26 | 北京有色金属研究总院 | Preparation method of submicron-level vanadium trioxide powder |
| CN106935860A (en) * | 2017-03-24 | 2017-07-07 | 华中科技大学 | A kind of carbon intercalation V2O3Nano material, its preparation method and application |
| CN107434259A (en) * | 2017-08-09 | 2017-12-05 | 河钢股份有限公司承德分公司 | A kind of method by preparing vanadium trioxide containing vanadium solution |
| CN107662946A (en) * | 2017-08-11 | 2018-02-06 | 攀枝花学院 | The preparation method of vanadium trioxide |
| CN107591522A (en) * | 2017-08-22 | 2018-01-16 | 中南大学 | A kind of preparation method of the spherical V2O3/C materials of sodium-ion battery negative pole |
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