CN108314083A - A method of by preparing vanadium trioxide containing vanadium solution - Google Patents

A method of by preparing vanadium trioxide containing vanadium solution Download PDF

Info

Publication number
CN108314083A
CN108314083A CN201810296853.2A CN201810296853A CN108314083A CN 108314083 A CN108314083 A CN 108314083A CN 201810296853 A CN201810296853 A CN 201810296853A CN 108314083 A CN108314083 A CN 108314083A
Authority
CN
China
Prior art keywords
vanadium
reaction
complex
solution
precipitation
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201810296853.2A
Other languages
Chinese (zh)
Other versions
CN108314083B (en
Inventor
李兰杰
陈东辉
祁健
赵备备
刘静
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HBIS Co Ltd Chengde Branch
Original Assignee
HBIS Co Ltd Chengde Branch
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by HBIS Co Ltd Chengde Branch filed Critical HBIS Co Ltd Chengde Branch
Priority to CN201810296853.2A priority Critical patent/CN108314083B/en
Publication of CN108314083A publication Critical patent/CN108314083A/en
Application granted granted Critical
Publication of CN108314083B publication Critical patent/CN108314083B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00Compounds of vanadium
    • C01G31/02Oxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The present invention relates to a kind of method by preparing vanadium trioxide containing vanadium solution, the method is:To containing organic amine compound progress precipitation reaction is added in vanadium solution, it is separated by solid-liquid separation after the completion of reaction, obtains containing vanadium complex and precipitation supernatant;It will obtain the calcining containing vanadium complex and carry out reduction reaction, vanadium trioxide is obtained after the completion of reaction.Present invention introduces organic amine compounds as precipitation agent, and can form bulky grain contains vanadium complex, reduces Fe in liquid phase3+、SO4 2‑、SiO3 2‑Equal soluble detrimentals impurity entrainment, improves product purity;And containing in vanadium complex carbon and reaction process in decompose the hydrogen of generation and can serve as reducing agent in reduction prepares vanadium trioxide, do not have to additional reducing agent again, and then substantially reduce production cost.The technology of the present invention is feasible, equipment is simple, it is easy to accomplish automation, application prospect with good economic efficiency and wide.

Description

A method of by preparing vanadium trioxide containing vanadium solution
Technical field
The present invention relates to vanadium field of chemical metallurgical technology, and in particular to a kind of side by preparing vanadium trioxide containing vanadium solution Method.
Background technology
Vanadium trioxide is a kind of important vanadium metal oxide, can be applied to the industrial departments such as metallurgy, electronics, chemical industry. Desirable feedstock of the vanadium trioxide as production vanadium series alloy, has during producing vanadium iron and VN alloy than other The more superior characteristic of barium oxide.In addition, vanadium trioxide has the property of Metal-nonmetal transition, low temperature phase change characteristic is good, Sudden change of resistivity is accompanied by lattice and anti-ferromagnetic variation up to 6 orders of magnitude, it partly leads for monocline is antiferromagnetic at low temperature Body group, excellent low temperature phase change performance make it be had broad application prospects in Cryo Equipment.
Currently, preparing there are mainly two types of the methods of vanadium trioxide:One is the ammonium metavanadates of not additional reducing agent or more Poly- ammonium vanadate thermally decomposes cracking process, such as CN101028938A provides a kind of method producing vanadium sesquioxide powder, utilizes The nascent hydron of the thermal cracking generation of the ammonia released when ammonium metavanadate is heated to restore ammonium metavanadate, this method does not use additional Also Primordial Qi, although departmental cost can be reduced, the ammonia cracking that raw material decomposes go out is incomplete, does not only result in reducing atmosphere not It is enough, and the exclusion for the ammonia not cracked can cause environmental pollution.
The method that another kind prepares vanadium trioxide is the direct high temperature reduction method of additional reducing agent, mostly with C, NH3、H2、 CH4, CO or industrial gas etc. be reducing agent, the high prices vfanadium compound such as thermal reduction ammonium metavanadate, poly ammonium vanadate, vanadic anhydride And vanadium trioxide is obtained, such method is also the method for preparing vanadium trioxide being widely used at present.Such as CN103922404A provides a kind of reduction with carbon vanadic anhydride three oxygen of preparation being not required under protective gas atmosphere or vacuum condition Change the method for two vanadium.The specific steps are:A, dispensing:The ratio of vanadic anhydride and carbon dust 2 ︰ 1 in molar ratio are uniformly mixed;b、 Binder:The mixed raw materials of step a are pressed into material block, then carbon dust is covered on material block;C, it fires:By the molding material of step b Block fires 3-5h at 950 DEG C -1050 DEG C and obtains vanadium trioxide.Although the invention is not required to protective gas atmosphere or vacuum condition, operation Simply, cost is lower, but increases dispensing and pressure ball process.
It is serious, raw in the prevalence of complex process, environmental pollution although the above method can effectively prepare vanadium trioxide Produce this high disadvantage.Currently, being badly in need of seeking a kind of vanadium trioxide preparation work simple for process, environmental-friendly, production cost is low Skill.
Invention content
In view of problems of the prior art, the side that the present invention provides a kind of by preparing vanadium trioxide containing vanadium solution Method introduces organic amine compound and carries out precipitation reaction as precipitation agent, improves product purity, and can be used as reducing agent in itself Reduction reaction is carried out, production cost is reduced.The technical feasibility, equipment are simple, it is easy to accomplish automation, before there is applications well Scape.
For this purpose, the present invention uses following technical scheme:
The present invention provides a kind of methods by preparing vanadium trioxide containing vanadium solution, the described method comprises the following steps:
(1) it to containing organic amine compound progress precipitation reaction is added in vanadium solution, is separated by solid-liquid separation, obtains after the completion of reaction Containing vanadium complex and precipitation supernatant;
(2) calcined what step (1) obtained containing vanadium complex, using containing in vanadium complex carbon and reacted The hydrogen decomposed in journey carries out reduction reaction as reducing agent, and vanadium trioxide is obtained after the completion of reaction.
The present invention carries out precipitation reaction using organic amine compound as precipitation agent, can form matching containing vanadium for bulky grain Object is closed, Fe in liquid phase is reduced3+、SO4 2-、SiO3 2-Equal soluble detrimentals impurity entrainment, improves product purity;And coordinate containing vanadium Decomposed in carbon and reaction process in object generation hydrogen (after decompositing ammonia containing vanadium complex, ammonia decompose generate hydrogen Gas) reducing agent can be used as in reduction prepares vanadium trioxide, do not have to additional reducing agent again, and then substantially reduce production cost.
It is of the present invention containing vanadium solution be the solution containing v element, preferably purify vanadium liquid.
Organic amine compound of the present invention is the organic object that organic species occur that chemical reaction is generated with ammonia Matter can be appointing in fatty amines, alcamines, amides, alicyclic ring amine, aromatic amine, naphthalene system amine and other amines It anticipates a kind of or at least two combinations;Such as can be monomethyl amine, di-n-propylamine, n-butylamine, 1,2- dimethyl propylamines, ethylenediamine, Monoethanolamine, formamide, diphenylamines, 2- naphthylamines, azanol etc., as space is limited and for concise consideration.The present invention no longer limit It enumerates.
According to the present invention, the molar ratio containing the nitrogen in the vanadium and organic amine compound in vanadium solution is described in step (1) (0.5-3):1, such as can be 0.5:1、1:1、1.5:1、2:1、2.5:1 or 3:It is specific between 1 and above-mentioned numerical value Value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, in step (1) the precipitation reaction process, the pH for adjusting solution is 1.0-7.0, such as can be 1, the specific point value between 2,3,4,5,6 or 7 and above-mentioned numerical value, as space is limited and for concise consideration, the present invention is no longer Exclusive list.
According to the present invention, the temperature of step (1) precipitation reaction is 30-60 DEG C, for example, can be 30 DEG C, 35 DEG C, 40 DEG C, 45 DEG C, 50 DEG C, 55 DEG C or the specific point value between 60 DEG C and above-mentioned numerical value, as space is limited and for concise consideration, The present invention no longer exclusive list.
According to the present invention, before step (2) described calcining, refined removing sodium is carried out containing vanadium complex to what step (1) obtained, The method is:It is reacted what step (1) obtained with acid solution mixing progress removing sodium containing vanadium complex, solid-liquid point after the completion of reaction From obtaining refined containing vanadium complex.
The present invention may be selected acid solution commonly used in the art and carry out removing sodium reaction, such as can select hydrochloric acid, sulfuric acid, nitric acid Deng, but it is non-be only limitted to this, other suitable acid solutions are equally applicable to the present invention.
According to the present invention, a concentration of 10-20wt% of the acid solution, such as can be 10wt%, 11wt%, 12wt%, Tool between 13wt%, 14wt%, 15wt%, 16wt%, 17wt%, 18wt%, 19wt% or 20wt% and above-mentioned numerical value Body point value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the liquid-solid ratio containing vanadium complex and acid solution is (2-5) during the refined removing sodium:1, such as can To be 2:1、2.5:1、3:1、3.5:1、4:1、4.5:1 or 5:Specific point value between 1 and above-mentioned numerical value, as space is limited and For concise consideration, the present invention no longer exclusive list.
The unit of the above-mentioned liquid-solid ratio of the present invention is mL/g.
According to the present invention, the temperature of removing sodium reaction is 20-50 DEG C, for example, can be 20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, Specific point value between 40 DEG C, 45 DEG C or 50 DEG C and above-mentioned numerical value, as space is limited and for concise consideration, the present invention is not Exclusive list again.
It is stirred according to the present invention, during the refined removing sodium, stir speed (S.S.) 50-500r/min, such as can be with Be 50r/min, 100r/min, 150r/min, 200r/min, 250r/min, 300r/min, 350r/min, 400r/min, Specific point value between 450r/min or 500r/min and above-mentioned numerical value, as space is limited and for concise consideration, the present invention No longer exclusive list.
According to the present invention, the temperature of step (2) described calcining is 700-900 DEG C, for example, can be 700 DEG C, 730 DEG C, 750 DEG C, 780 DEG C, 800 DEG C, 830 DEG C, 850 DEG C, 880 DEG C or the specific point value between 900 DEG C and above-mentioned numerical value, as space is limited and For concise consideration, the present invention no longer exclusive list.
According to the present invention, time of step (2) described calcining is 10-120min, for example, can be 10min, 20min, 30min, 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min or 120min and above-mentioned numerical value Between specific point value, as space is limited and for concise consideration, the present invention no longer exclusive list.
Step (2) the of the present invention calcining carries out preferably in rotary kiln, but it is non-be only limitted to this, other can complete to calcine Equipment be equally applicable to the present invention.
According to the present invention, the gas that is discharged in step (2) described calcination process is lighted after gathering dust and is recycled, and can be used for adjusting Save the pH of solution in step (1) described precipitation reaction process.
The present invention selects the operation that means commonly used in the art are separated by solid-liquid separation, for example, can be filtering, filter, from The heart, sedimentation etc., but it is non-be only limitted to this, should be specifically chosen according to actual conditions.
Of the present invention as a preferred technical solution, by the method for preparing vanadium trioxide containing vanadium solution includes following step Suddenly:
(1) according to (0.5-3):1 vanadium nitrogen molar ratio is anti-to precipitation is carried out containing addition organic amine compound in vanadium solution It answers, it is 1.0-7.0 that pH is adjusted in reaction process, and controlling reaction temperature is 30-60 DEG C, is separated by solid-liquid separation, is contained after the completion of reaction Vanadium complex and precipitation supernatant;
(2) it is reacted what step (1) obtained with the acid solution of a concentration of 10-20wt% mixing progress removing sodium containing vanadium complex, It is (2-5) that liquid-solid ratio is controlled in reaction process:1, temperature is 20-50 DEG C, is stirred with the rate of 50-500r/min, is reacted It is separated by solid-liquid separation, obtains refined containing vanadium complex after the completion;
(3) it refined it is heated to 700-900 DEG C in rotary kiln containing vanadium complex calcines 10- by what step (2) obtained 120min, using containing in vanadium complex carbon and reaction process in the hydrogen that decomposes carry out reduction reaction as reducing agent, The gas being discharged in calcination process is lighted after gathering dust and is recycled, and can be used for molten in regulating step (1) the precipitation reaction process The pH of liquid obtains vanadium trioxide after the completion of reaction.
Compared with prior art, the present invention at least has the advantages that:
(1) present invention introduces organic amine medicament can precipitation reaction in be used as precipitation agent, the vanadium for forming bulky grain is matched Object is closed, Fe in liquid phase is reduced3+、SO4 2-、SiO3 2-Equal soluble detrimentals impurity entrainment, improves product purity.
(2) present invention introduces what organic amine compound was formed can be used as reducing agent at high temperature containing vanadium complex, utilizes The hydrogen decomposited in the carbon and reaction process that itself contain carries out reduction reaction, does not have to additional reducing agent again, Jin Er great It is big to reduce production cost.
(3) the technology of the present invention is feasible, equipment is simple, and production cost is low and easy to automate, has good application Foreground.
Description of the drawings
Fig. 1 is the process flow chart that a kind of specific implementation mode of the present invention provides, wherein S- solid phases, L- liquid phases, G- gas phases.
The present invention is described in more detail below.But following examples is only the simple example of the present invention, not generation Table or limitation the scope of the present invention, protection scope of the present invention are subject to claims.
Specific implementation mode
Technical solution to further illustrate the present invention below with reference to the accompanying drawings and specific embodiments.
As shown in Figure 1, the technological process that a kind of specific implementation mode of the present invention provides can be:It is added into purification vanadium liquid Organic amine adjusts pH, controlling reaction temperature progress precipitation reaction, is separated by filtration after the completion of reaction, obtains solid phase and contain vanadium complex And liquid phase precipitation supernatant;Gained is mixed progress removing sodium with acid solution containing vanadium complex to react, is separated by filtration, obtains after the completion of reaction Contain vanadium complex to solid phase is refined, gained liquid phase can be used for the adjusting of precipitation process pH;It is restored refined containing vanadium complex It calcines, the gas phase generated in calcination process is equally applicable to the adjusting of precipitation process pH after purification, is obtained after the completion of calcining Vanadium trioxide product.
For the present invention is better described, it is easy to understand technical scheme of the present invention, of the invention is typical but non-limiting Embodiment is as follows:
Embodiment 1
(1) according to 3:Ethylenediamine is added into the purification vanadium liquid of a concentration of 25.32g/L of vanadium for 1 vanadium nitrogen molar ratio, adjusts pH Precipitation reaction is carried out for 5.0, reaction temperature is 50 DEG C, is reacted to filtering after the completion, obtains solid phase containing on vanadium complex and precipitation Clear liquid;
(2) progress removing sodium reaction is added into the hydrochloric acid of a concentration of 10wt% containing vanadium complex by what step (1) obtained, instead Should control liquid-solid ratio be in the process 5:1,30 DEG C of temperature is stirred with the rate of 300r/min, is filtered after the completion of reaction, Obtain filtered fluid and refined containing vanadium complex;
(3) refined be added in closed rotary kiln containing vanadium complex that step (2) obtains is calcined, calcination temperature is 900 DEG C, soaking time 30min, using containing in vanadium complex carbon and reaction process in the hydrogen that decomposites restored Reaction obtains vanadium trioxide product after the completion of reaction.
By detection, based on mass percentage, the vanadium content of the vanadium trioxide obtained in the present embodiment is 64.65%, impurity content Na:0.43%, Si:0.28%, Fe:0.25%, P:0.15%.
Embodiment 2
(1) according to 2.5:Ethylenediamine is added into the purification vanadium liquid of a concentration of 20.16g/L of vanadium in 1 vanadium nitrogen molar ratio, adjusts PH is 3.0 progress precipitation reactions, and reaction temperature is 40 DEG C, is reacted to filtering after the completion, obtains solid phase and contains vanadium complex and precipitation Supernatant;
(2) progress removing sodium reaction is added into the hydrochloric acid of a concentration of 12wt% containing vanadium complex by what step (1) obtained, instead Should control liquid-solid ratio be in the process 4:1,40 DEG C of temperature is stirred with the rate of 500r/min, is filtered after the completion of reaction, Obtain filtered fluid and refined containing vanadium complex;
(3) refined be added in closed rotary kiln containing vanadium complex that step (2) obtains is calcined, calcination temperature is 850 DEG C, soaking time 60min, using containing in vanadium complex carbon and reaction process in the hydrogen that decomposites restored It reacts, the gas being discharged in calcination process is lighted after gathering dust and recycled, and regulating step (1) the precipitation reaction process is can be used for The pH of middle solution obtains vanadium trioxide product after the completion of reaction.
By detection, based on mass percentage, the vanadium content of the vanadium trioxide obtained in the present embodiment is 63.89%, impurity content Na:0.51%, Si:0.23%, Fe:0.29%, P:0.11%.
Embodiment 3
(1) according to 1.5:Ethylenediamine is added into the purification vanadium liquid of a concentration of 28.07g/L of vanadium in 1 vanadium nitrogen molar ratio, adjusts PH is 5.0 progress precipitation reactions, and reaction temperature is 60 DEG C, is reacted to filtering after the completion, obtains solid phase and contains vanadium complex and precipitation Supernatant;
(2) progress removing sodium reaction is added into the sulfuric acid of a concentration of 14wt% containing vanadium complex by what step (1) obtained, instead Should control liquid-solid ratio be in the process 4:1, temperature 50 C is stirred with the rate of 200r/min, is filtered after the completion of reaction, Obtain filtered fluid and refined containing vanadium complex;
(3) refined be added in closed rotary kiln containing vanadium complex that step (2) obtains is calcined, calcination temperature is 700 DEG C, soaking time 120min, using containing in vanadium complex carbon and reaction process in the hydrogen that decomposites restored Reaction obtains vanadium trioxide product after the completion of reaction.
By detection, based on mass percentage, the vanadium content of the vanadium trioxide obtained in the present embodiment is 63.45%, impurity content Na:0.53%, Si:0.24%, Fe:0.26%, P:0.13%.
Embodiment 4
(1) according to 1:Ethylenediamine is added into the purification vanadium liquid of a concentration of 23.07g/L of vanadium for 1 vanadium nitrogen molar ratio, adjusts pH Precipitation reaction is carried out for 2.0, reaction temperature is 35 DEG C, is reacted to filtering after the completion, obtains solid phase containing on vanadium complex and precipitation Clear liquid;
(2) progress removing sodium reaction is added into the hydrochloric acid of a concentration of 16wt% containing vanadium complex by what step (1) obtained, instead Should control liquid-solid ratio be in the process 2:1,30 DEG C of temperature is stirred with the rate of 100r/min, is filtered after the completion of reaction, Obtain filtered fluid and refined containing vanadium complex;
(3) refined be added in closed rotary kiln containing vanadium complex that step (2) obtains is calcined, calcination temperature is 750 DEG C, soaking time 90min, using containing in vanadium complex carbon and reaction process in the hydrogen that decomposites restored It reacts, the gas being discharged in calcination process is lighted after gathering dust and recycled, and regulating step (1) the precipitation reaction process is can be used for The pH of middle solution obtains vanadium trioxide product after the completion of reaction.
By detection, based on mass percentage, the vanadium content of the vanadium trioxide obtained in the present embodiment is 64.56%, impurity content Na:0.48%, Si:0.26%, Fe:0.23%, P:0.10%.
Embodiment 5
(1) according to 0.5:Ethylenediamine is added into the purification vanadium liquid of a concentration of 15.07g/L of vanadium in 1 vanadium nitrogen molar ratio, adjusts PH is 1.0 progress precipitation reactions, and reaction temperature is 30 DEG C, is reacted to filtering after the completion, obtains solid phase and contains vanadium complex and precipitation Supernatant;
(2) progress removing sodium reaction is added into the hydrochloric acid of a concentration of 18wt% containing vanadium complex by what step (1) obtained, instead Should control liquid-solid ratio be in the process 3:1,20 DEG C of temperature is stirred with the rate of 250r/min, is filtered after the completion of reaction, Obtain filtered fluid and refined containing vanadium complex;
(3) refined be added in closed rotary kiln containing vanadium complex that step (2) obtains is calcined, calcination temperature is 820 DEG C, soaking time 10min, using containing in vanadium complex carbon and reaction process in the hydrogen that decomposites restored It reacts, the gas being discharged in calcination process is lighted after gathering dust and recycled, and regulating step (1) the precipitation reaction process is can be used for The pH of middle solution obtains vanadium trioxide product after the completion of reaction.
By detection, based on mass percentage, the vanadium content of the vanadium trioxide obtained in the present embodiment is 63.82%, impurity content Na:0.51%, Si:0.24%, Fe:0.29%, P:0.18%.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above Detail can carry out a variety of simple variants to technical scheme of the present invention within the scope of the technical concept of the present invention, this A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally The thought of invention, it should also be regarded as the disclosure of the present invention.

Claims (10)

1. a kind of method by preparing vanadium trioxide containing vanadium solution, which is characterized in that the described method comprises the following steps:
(1) it to containing organic amine compound progress precipitation reaction is added in vanadium solution, is separated by solid-liquid separation after the completion of reaction, obtains containing vanadium Complex and precipitation supernatant;
(2) it is calcined what step (1) obtained containing vanadium complex, using containing in the carbon and reaction process in vanadium complex The hydrogen of decomposition carries out reduction reaction as reducing agent, and vanadium trioxide is obtained after the completion of reaction.
2. the method as described in claim 1, which is characterized in that step (1) is described containing the vanadium and organic amine in vanadium solution The molar ratio for closing the nitrogen in object is (0.5-3):1.
3. method as claimed in claim 1 or 2, which is characterized in that in step (1) the precipitation reaction process, adjust solution PH be 1.0-7.0;
Preferably, the temperature of step (1) the precipitation reaction is 30-60 DEG C.
4. method as described in any one of claims 1-3, which is characterized in that before step (2) described calcining, to step (1) What is obtained carries out refined removing sodium containing vanadium complex, and the method is:It is mixed into what step (1) obtained with acid solution containing vanadium complex Row removing sodium is reacted, and is separated by solid-liquid separation after the completion of reaction, obtains refined containing vanadium complex.
5. method as claimed in claim 4, which is characterized in that a concentration of 5-20wt% of the acid solution;
Preferably, the liquid-solid ratio containing vanadium complex and acid solution is (2-5) during the refined removing sodium:1.
6. method as described in claim 4 or 5, which is characterized in that the temperature of the removing sodium reaction is 20-50 DEG C;
Preferably, it is stirred during the refined removing sodium, stir speed (S.S.) 50-500r/min.
7. method as claimed in any one of claims 1 to 6, which is characterized in that the temperature of step (2) described calcining is 700-900 ℃;
Preferably, the time of step (2) described calcining is 10-120min.
8. such as claim 1-7 any one of them methods, which is characterized in that step (2) calcining carries out in rotary kiln.
9. such as claim 1-8 any one of them methods, which is characterized in that the gas being discharged in step (2) described calcination process Body is lighted after gathering dust and is recycled, and the pH of solution in regulating step (1) the precipitation reaction process is can be used for.
10. such as claim 1-9 any one of them methods, which is characterized in that the described method comprises the following steps:
(1) according to (0.5-3):1 vanadium nitrogen molar ratio carries out precipitation reaction to containing addition organic amine compound in vanadium solution, instead It is 1.0-7.0 that pH should be adjusted in the process, and controlling reaction temperature is 30-60 DEG C, and reaction is separated by solid-liquid separation after the completion, obtains coordinating containing vanadium Object and precipitation supernatant;
(2) it reacts, reacts with the acid solution of a concentration of 10-20wt% mixing progress removing sodium containing vanadium complex by what step (1) obtained Control liquid-solid ratio is (2-5) in the process:1, temperature is 20-50 DEG C, is stirred with the rate of 50-500r/min, and reaction is completed After be separated by solid-liquid separation, obtain refined containing vanadium complex;
(3) by step (2) obtain it is refined 700-900 DEG C of calcining 10-120min is heated in rotary kiln containing vanadium complex, it is sharp Use containing in vanadium complex carbon and reaction process in the hydrogen that decomposes carry out reduction reaction as reducing agent, in calcination process The gas of discharge is lighted after gathering dust and is recycled, and the pH of solution in regulating step (1) the precipitation reaction process is can be used for, reaction Vanadium trioxide is obtained after the completion.
CN201810296853.2A 2018-04-04 2018-04-04 Method for preparing vanadium trioxide from vanadium-containing solution Active CN108314083B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810296853.2A CN108314083B (en) 2018-04-04 2018-04-04 Method for preparing vanadium trioxide from vanadium-containing solution

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810296853.2A CN108314083B (en) 2018-04-04 2018-04-04 Method for preparing vanadium trioxide from vanadium-containing solution

Publications (2)

Publication Number Publication Date
CN108314083A true CN108314083A (en) 2018-07-24
CN108314083B CN108314083B (en) 2020-11-03

Family

ID=62897378

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810296853.2A Active CN108314083B (en) 2018-04-04 2018-04-04 Method for preparing vanadium trioxide from vanadium-containing solution

Country Status (1)

Country Link
CN (1) CN108314083B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110867592A (en) * 2019-11-01 2020-03-06 四川星明能源环保科技有限公司 Treatment method of failure vanadium electrolyte
CN113651360A (en) * 2021-08-18 2021-11-16 江南大学 Synthesis method and application of vanadium oxide
CN116462227A (en) * 2023-04-20 2023-07-21 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing vanadium pentoxide from calcified clinker

Citations (11)

* Cited by examiner, † Cited by third party
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

Patent Citations (11)

* Cited by examiner, † Cited by third party
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

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110867592A (en) * 2019-11-01 2020-03-06 四川星明能源环保科技有限公司 Treatment method of failure vanadium electrolyte
CN113651360A (en) * 2021-08-18 2021-11-16 江南大学 Synthesis method and application of vanadium oxide
CN116462227A (en) * 2023-04-20 2023-07-21 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing vanadium pentoxide from calcified clinker

Also Published As

Publication number Publication date
CN108314083B (en) 2020-11-03

Similar Documents

Publication Publication Date Title
AU2019262261B2 (en) Method for clean metallurgy of molybdenum
CN108314083A (en) A method of by preparing vanadium trioxide containing vanadium solution
CN112646977B (en) Method for recovering vanadium, molybdenum, nickel and aluminum from petroleum refining waste catalyst
CN109022763B (en) Treatment method and equipment for tungsten-containing waste
CN108516588B (en) Method for preparing tungsten product from crude sodium tungstate solution
CN111994952A (en) Method for preparing high-purity vanadium pentoxide by vacuum sublimation of metallurgical-grade vanadium pentoxide
CN103526013A (en) Comprehensive recovery method of complex molybdenum sulfide ore
CN109897962B (en) Method and device for recovering tungsten in tungsten-containing waste by adopting oxidation smelting method
CN114058853B (en) Method for recovering titanium, vanadium and tungsten from waste SCR denitration catalyst
CN101914678A (en) Method for producing industry molybdenum oxide from molybdenum concentrate
CN108588446A (en) A method of extracting molybdenum and rhenium from rhenium-containing molybdenum concntrate
CN104129814B (en) A kind of method that is raw material production ammonium meta-vanadate with oil hydrogenation spent catalyst
CN108728674B (en) Method for extracting molybdenum from crude molybdic acid and preparing molybdenum product
CN110964922A (en) Method for recovering refined platinum from crude ammonium chloroplatinate
CN102259000B (en) Recycling method for dead catalyst containing nickel
CN104973627B (en) A kind of method for producing chrome green as raw material with carbon ferrochrome
CN107287411A (en) A kind of method of arsenic in removing arsenic-containing ores
CN108611503B (en) Method for decomposing wolframite and preparing tungsten oxide and tungsten powder by oxygen pressure
CN105543506B (en) A kind of method for producing high-purity metal chromium
CN103952534B (en) A kind of method utilizing nickel-molybdenum ore to prepare Sodium orthomolybdate
CN114606385B (en) Selective leaching method of molybdenum and vanadium in molybdenum-vanadium-containing spent catalyst
CN103754839A (en) Preparation method of nanocrystal vanadium nitride powder
CN109722533B (en) Method for preparing vanadium trioxide by using stone coal vanadium extraction pickle liquor
CN103539207B (en) A kind of preparation method of red iron oxide
CN110436519B (en) Method for preparing vanadium trioxide from vanadium slag in short process

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant