CN103194603B - Preparation method of high-purity vanadium pentoxide - Google Patents

Preparation method of high-purity vanadium pentoxide Download PDF

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CN103194603B
CN103194603B CN201310111038.1A CN201310111038A CN103194603B CN 103194603 B CN103194603 B CN 103194603B CN 201310111038 A CN201310111038 A CN 201310111038A CN 103194603 B CN103194603 B CN 103194603B
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vanadium
solution
controls
impurity
precipitation
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CN201310111038.1A
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CN103194603A (en
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李亮
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攀枝花学院
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

The invention discloses a preparation method of high-purity vanadium pentoxide. The method comprises the following steps of: a, grinding a vanadium-containing raw material, and removing iron; b, performing sodium roasting on the raw material treated in the step a, and leaching to obtain the vanadium-containing solution; c, removing cation impurities and anion impurities from the vanadium-containing solution obtained in the step b, and filtering to obtain the purified vanadium-containing solution; d, adding ammonium sulfate into the purified vanadium-containing solution to perform molybdenum precipitation treatment, filtering, washing and removing impurities to obtain vanadate precipitate; and e, pulping and filtering the vanadate precipitate, washing, further removing impurities in the vanadate precipitate, drying and roasting to obtain a vanadium pentoxide product. By virtue of the strict and effective impurity removal treatment, the purity of the vanadium pentoxide product can be increased, and can be over 99 percent.

Description

The preparation method of high purity vanadic anhydride
Technical field
The invention belongs to field of metallurgy, be specifically related to a kind of preparation method of high purity vanadic anhydride.
Background technology
High-purity vanadium oxide has higher added value, can be used for the industries such as metallurgy, chemical industry, medicine, the energy, environmental protection, aerospace.According to statistics, 2007, domestic to high-purity vanadium oxide product consumption about 3500 tons, the Vanadium Pentoxide in FLAKES demand for the production of vananum just reached about 1600 tons.Along with the development of new industry, estimate that the domestic demand to high-purity vanadium oxide also will increase further.Such as: domestic large Aircraft Project and vanadium cell project, need high-purity vanadium oxide.Therefore the domestic demand to high-purity vanadium oxide also can increase further.Abroad, larger to high-purity vanadium pentoxide demand area mainly European Union, the U.S., Japan, Korea S.
The raw material of vanadium extraction has a variety of, and main vanadium extraction raw material has vanadium titano-magnetite concentrate, vanadium slag, yeath etc., also has the secondary resource such as spent catalyst, oil lime-ash.Process for extracting vanadium comparatively ripe is now: containing vanadium raw materials → grinding → sodium oxide roasting → leaching → removal of impurities → acid ammonium salt precipitation → calcining → Vanadium Pentoxide in FLAKES product.This technique is the more ripe process for extracting vanadium of existing industrialization.Because the removal situation of existing impurity-removing method to impurity is undesirable and precipitation technique is mingled with impurity, the purity of vanadium pentoxide that this technique is produced is generally 98% ~ 99%.
In order to produce purity > 99% Vanadium Pentoxide in FLAKES product, a large amount of research work has been carried out in Domestic Scientific Research work, define the novel method preparing high-purity vanadium pentoxide, these methods are in the laboratory study stage at present, do not carry out Industry Promotion.Such as: (1) extraction process prepares high purity vanadic anhydride.Be extracted to roasting Vanadium Pentoxide in FLAKES from vanadium liquid, product purity reaches more than 98%.Containing the foreign ion that can be extracted in vanadium liquid, after back extraction, these foreign ions enter vanadium liquid, and affect vanadium product purity, cannot accomplish that a step removal of impurities obtains high purity vanadic anhydride.(2) ion exchange method prepares high purity vanadic anhydride.The method can obtain more than 99.5% high purity vanadic anhydride.Also need further removal of impurities after ion-exchange, because resin adsorbs other impurity while absorption vanadium, disposable removal of impurities can not obtain high purity vanadic anhydride.(3) alkali solution technique prepares high purity vanadic anhydride.By thick vanadium product after alkali is molten again by the method producing Vanadium Pentoxide in FLAKES after ammonium hydroxide, calcium hydroxide, sodium metaaluminate, water glass removal of impurities, this method must the molten and substep removal of impurities through alkali, still can not obtained high-purity vanadium pentoxide after disposable removal of impurities.
In order to work out the method for suitable high purity vanadic anhydride, and Industry Promotion can be carried out.Adopt the method for efficient removal of impurities, the processing condition optimizing precipitation reduce impurity and carry secretly, carry out making beating washing, effectively remove impurity, can produce high-grade Vanadium Pentoxide in FLAKES product the vanadate settled out.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of novel preparation method of high purity vanadic anhydride.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method of high purity vanadic anhydride, comprises the steps:
A, will be levigate and do deironing process containing vanadium raw materials;
B, the raw material after step a process is carried out sodium roasting, then leach and obtain containing vanadium solution;
C, step b is obtained carry out decationize impurity containing vanadium solution and except anionic impurity process, filter after being purified containing vanadium solution;
D, to carrying out precipitation process containing adding ammonium sulfate in vanadium solution after purification, then after filtration, obtain vanadate throw out after washing impurity-removing;
E, pull an oar to vanadate throw out, filter, then carry out carrying out washing treatment, the impurity be mingled with in removing vanadate throw out further, then drying, roasting obtain Vanadium Pentoxide in FLAKES product.
Wherein, in aforesaid method step c, decationize impurity is adjusted to different pH value by containing vanadium solution, makes to change precipitation of hydroxide removing into containing the metallic cation in vanadium solution.
Wherein, removing anionic impurity in aforesaid method step c is remove containing the phosphorus in vanadium solution and silicon: dephosphorization agent is CaCl 2, CaCl 2add with solid particle forms or be mixed with concentration be 8 ~ 12% solution morphology add, add-on is 1m 3add 0.4 ~ 1.2kg calcium chloride containing vanadium solution, dephosphorization temperature controls at>=85 DEG C, and dephosphorization pH value controls 8 ~ 9, and constant temperature churning time is not less than 30min, and constant temperature time of repose is not less than 30min; Desiliconizing agent is Al 2(SO 4) 3, Al 2(SO 4) 3add-on be 1m 3add 8.5 ~ 10.5kg containing vanadium solution, silica removal temperature controls at>=85 DEG C, and silica removal pH value controls 9 ~ 10, and constant temperature churning time is not less than 30min, and constant temperature time of repose is not less than 30min.
Wherein, after aforesaid method step c purifies containing no suspended substance in vanadium solution, [V]=25 ~ 30g/L, [P]≤0.015g/L, [Si]≤0.05g/L, pH=8 ~ 11.
Wherein, aforesaid method steps d precipitation processing controls precipitation temperature >=85 DEG C; The additional proportion of ammonium sulfate is: precipitation adds ammonium coefficient and controls 1 ~ 2.8; Through twice acid adding, pH value of solution=5 ~ 7 after an acid adding, pH value of solution=2 ~ 3 after secondary acid adding.
Wherein, ammonium sulfate is before an acid adding, adds after secondary acid adding.
Wherein, in aforesaid method step e, when vanadate throw out is pulled an oar, control making beating temperature >=80 DEG C, beating time 10 ~ 40min.
Wherein, described in aforesaid method step a is vanadium extraction by converter blowing gained vanadium slag containing vanadium raw materials.
Wherein, in aforesaid method step a, 0.1mm will be less than containing vanadium raw materials is levigate to granularity, and-120 order >=80%.
Wherein, during aforesaid method step b sodium roasting, allocate industrial sodium carbonate into by 1 ~ 2.5 times of vanadium quality in raw material, control maturing temperature 600 ~ 850 DEG C, roasting time is no less than 1.5h.
Wherein, the liquid-solid ratio leached in aforesaid method step b is 3 ~ 6 ︰ 1, and leaching agent is water, extraction temperature > 75 DEG C, extraction time > 15min, leaches pH value and controls 7 ~ 9.5.Liquid-solid ratio is the ratio of liquid mass (kilogram) and solid masses (kilogram).
The invention has the beneficial effects as follows: the present invention carries out decationize impurity and anionic impurity process to containing vanadium solution, washing impurity-removing after precipitation, the solvable elements such as effective removing sodium, chromium, and carry out dispersion treatment again, namely making beating makes impurity component stripping, then filtration washing, makes final obtained Vanadium Pentoxide in FLAKES product purity improve.The decationize impurity that the present invention specifically adopts and the measure of anionic impurity, as specifically selected which kind of dephosphorization agent, control temperature, pH value, constant temperature churning time and time of repose etc., enable main impurity effectively remove, and ensures the high purity of the finished product.The precipitation measure that the present invention specifically adopts also can improve the purity of product further, adsorbs the elements such as a large amount of silicon, sodium, chromium, iron, affect impurity washing effect when avoiding ammonium vanadate to precipitate.The inventive method fully can remove impurity, and the purity of Vanadium Pentoxide in FLAKES can reach more than 99%.
Embodiment
Below by embodiment, the present invention is further described.
The inventive method is mainly divided into next step:
1, Raw material processing
First adopt crusher will to be crushed to certain granularity containing vanadium raw materials, then adopt ball mill or Raymond mill will containing vanadium raw materials grinding to certain fineness, grinding fineness be less than 0.1mm, and granularity is greater than 120 order >=80%.Improve the specific surface area containing vanadium raw materials by grinding, can ensure can be fully oxidized in the process of oxidizing roasting containing vanadium raw materials.
2, deironing
Adopt magnetic method, sieve method or air blast process to carrying out deironing process containing vanadium raw materials after levigate, ensure metallic iron residual volume < 8%, the main purpose of deironing: prevent from releasing amount of heat during metallic iron oxidizing reaction, cause charging binding, what impact was produced normally carries out.
3, roasting
By certain proportion scale, by mixing with additive (additive, mainly based on soda, also can allocate some sodium sulfate or sodium-chlor into, the amount of allocating into according to the content determination additive containing vanadium in vanadium raw materials) containing vanadium raw materials of processing.Send in rotary kiln or Multiple hearth furnace and calcine, be converted into water-soluble vanadic acid sodium by roasting by containing the vanadium in vanadium raw materials.
4, leach
Adopt water seaoning to leach grog, mode of operation can select continous way or intermittent type, is dissolved in the aqueous solution by the solubility vanadic acid sodium in grog and goes.Obtain containing vanadium solution by filtering solution to be separated with residue.
5, removal of impurities
Grog is in the process leached, and impurity is immersed in solution with vanadic acid sodium and goes, and the impurities affect of existence to Vanadium Pentoxide in FLAKES product of these impurity is larger.The not high major cause of Vanadium Pentoxide in FLAKES product purity is caused to be: because the removal of impurity before precipitation is thorough, in the process of precipitation, impurity enters in the particle of ammonium metavanadate precipitate, not thorough to ammonium metavanadate precipitate washing.Therefore, adopt effective impurity-removing method more crucial for the Vanadium Pentoxide in FLAKES product of high purity.Removal of impurities concrete grammar, regulates different pH values, makes to become precipitation of hydroxide removing containing the metal ion in vanadium solution; Add-on is 1m 3add 0.4 ~ 1.2kg calcium chloride containing vanadium solution, dephosphorization temperature controls at>=85 DEG C, and dephosphorization pH value controls 8 ~ 9, and constant temperature churning time is not less than 30min, and constant temperature time of repose is not less than 30min; Desiliconizing agent is Al 2(SO 4) 3, Al 2(SO 4) 3add-on be 1m 3add 8.5 ~ 10.5kg containing vanadium solution, silica removal temperature controls at>=85 DEG C, and silica removal pH value controls 9 ~ 10, and constant temperature churning time is not less than 30min, and constant temperature time of repose is not less than 30min.
6, precipitation
Precipitation technology controlling and process is bad, and vanadic acid ammonium salt is more abundant flaky crystalline grain agglomerating particles, likeness in form chrysanthemum shape, and when the ammonium vanadate salt particle of this shape precipitates, the elements such as a large amount of silicon, sodium, chromium, iron can be adsorbed in surface, affects impurity washing removing effect.Control suitable precipitation technique, precipitated product is ammonium meta-vanadate mainly, and more serious reunion occurs ammonium meta-vanadate particle hardly, and the solvable element such as sodium during precipitation in solution, chromium can lessly enter in vanadate.During washing, ammonium meta-vanadate particle is comparatively large and loose, and the solvable element such as sodium, chromium is easier to washing removing.Therefore, the precipitation technique that research is suitable for is more crucial for the absorption reducing impurity, precipitation processing controls precipitation temperature >=85 DEG C; The additional proportion of ammonium sulfate is: precipitation adds ammonium coefficient and controls 1 ~ 2.8; Through twice acid adding, pH value of solution=5 ~ 7 after an acid adding, pH value of solution=2 ~ 3 after secondary acid adding.
7, dispersion is washed again
In order to the Vanadium Pentoxide in FLAKES product of high purity, redispersion (making beating) is precipitated again to the vanadate after filtration washing, makes impurity component stripping, then carry out filtration washing, effectively can remove impurity component.
8, dry, calcining
Vanadate after removal of impurities first through super-dry, then through calcining, can obtain higher-grade Vanadium Pentoxide in FLAKES product.
Below by embodiment, the specific embodiment of the present invention is further described, but not therefore by protection scope of the present invention restriction in one embodiment.
Embodiment one
First by levigate through ball mill for vanadium extraction by converter blowing gained vanadium slag, granularity is less than 0.1mm, and granularity is greater than 120 orders and controls 90%; Do deironing process to the vanadium raw materials that contains after levigate, metallic iron residual volume is 6%; The vanadium raw materials that contains after deironing allocates industrial sodium carbonate (soda) into, the amount of allocating into of sodium carbonate controls: allocate into by 1 ~ 2.5 times of content of vanadium, maturing temperature controls at 780 DEG C, roasting time controls at 3h, to add water leachings containing vanadium raw materials after roasting, leach liquor is consolidated mass ratio and is controlled at 4:1, and extraction temperature controls at 85 DEG C, extraction time controls at 25 minutes, leaches pH value and controls 8; Carry out decationize process to containing vanadium solution, be adjusted to different pH values by containing vanadium solution, make metal ion in solution become precipitation of hydroxide.Except anionic treatments, CaCl is selected to carrying out containing vanadium solution 2make dephosphorization agent, adding with solid particle forms or being mixed with concentration is that the form of the solution of about 10% adds, and add-on is 1m 3qualifying liquid adds 1kg calcium chloride, and dephosphorization temperature controls at 85 DEG C, and dephosphorization pH value controls 8.5, and constant temperature churning time controls at 40min, and constant temperature time of repose controls at 40min.Desiliconizing agent selects Al 2(SO4) 3, Al 2(SO4) 3the amount of allocating into control at 9.5g/l, silica removal temperature controls at 90 DEG C, and silica removal pH value controls 9.5, and constant temperature churning time controls at 40min, and constant temperature time of repose controls at 40min; Carry out precipitation process to the vanadium solution that contains after removing impurity, qualifying liquid controls: [V]=27g/l, [P]≤0.015g/l, [Si]≤0.05g/l, pH=10, solution clear, no suspended substance.The control of precipitation temperature is at 85 DEG C, and the additional proportion of ammonium sulfate controls: precipitation adds ammonium coefficient 1.5, and precipitation temperature controls at >=85 DEG C, pH value of solution=5 ~ 7 after an acid adding, pH value of solution=2 ~ 3 after secondary acid adding; Vanadate is disperseed, carrying out washing treatment, discrete volume than control appropriate, jitter time controls at 30 minutes, and dispersion temperature controls at 80 DEG C.The purity of the Vanadium Pentoxide in FLAKES obtained by above art breading is 99.2%.
Embodiment two
First by levigate through ball mill for vanadium extraction by converter blowing gained vanadium slag, granularity is less than 0.1mm, and granularity is greater than 120 orders and controls about 90%; Do deironing process to the vanadium raw materials that contains after levigate, metallic iron residual volume is respectively 5%; The vanadium raw materials that contains after deironing allocates industrial sodium carbonate (soda) into, the amount of allocating into of sodium carbonate controls: allocate into by 1 ~ 2.5 times of content of vanadium, maturing temperature controls at 780 DEG C, roasting time controls at 3h, to add water leachings containing vanadium raw materials after roasting, leach liquor is consolidated mass ratio and is controlled at 4:1, and extraction temperature controls at 85 DEG C, extraction time controls at 25 minutes, leaches pH value and controls 8; Carry out decationize process to containing vanadium solution, be adjusted to different pH values by containing vanadium solution, make metal ion in solution become precipitation of hydroxide.Except anionic treatments, CaCl is selected to carrying out containing vanadium solution 2make dephosphorization agent, adding with solid particle forms or being mixed with concentration is that the form of the solution of about 10% adds, and add-on is 1m 3qualifying liquid adds 1.2kg calcium chloride respectively, and dephosphorization temperature controls at 85 DEG C, and dephosphorization pH value controls 8.5, and constant temperature churning time controls at 40min, and constant temperature time of repose controls at 40min.Desiliconizing agent selects Al 2(SO4) 3, Al 2(SO4) 3the amount of allocating into control at 10g/l, silica removal temperature controls at 90 DEG C, and silica removal pH value controls 9.5, and constant temperature churning time controls at 40min, and constant temperature time of repose controls at 40min; Carry out precipitation process to the vanadium solution that contains after removing impurity, qualifying liquid controls: [V]=27g/l, [P]≤0.015g/l, [Si]≤0.05g/l, pH=10, solution clear, no suspended substance.The control of precipitation temperature is at 85 DEG C, and the additional proportion of ammonium sulfate controls: it is 2 that precipitation adds ammonium coefficient, and precipitation temperature controls at >=85 DEG C, pH value of solution=5 ~ 7 after an acid adding, pH value of solution=2 ~ 3 after secondary acid adding; Vanadate is disperseed, carrying out washing treatment, discrete volume than control appropriate, jitter time controls at 30 minutes, and dispersion temperature controls at 80 DEG C.The purity of the Vanadium Pentoxide in FLAKES obtained by above art breading is 99.5%.

Claims (2)

1. the preparation method of high purity vanadic anhydride, is characterized in that comprising the steps:
A, will be levigate and do deironing process containing vanadium raw materials; Levigately be less than 0.1mm to granularity, and-120 order >=80%;
B, the raw material after step a process is carried out sodium roasting, then leach and obtain containing vanadium solution; During sodium roasting, allocate industrial sodium carbonate into by 1 ~ 2.5 times of vanadium quality in raw material, control maturing temperature 600 ~ 850 DEG C, roasting time is no less than 1.5h; The liquid-solid ratio leached is 3 ~ 6 ︰ 1, and leaching agent is water, extraction temperature > 75 DEG C, extraction time > 15min, leaches pH value and controls 7 ~ 9.5;
C, step b is obtained carry out decationize impurity containing vanadium solution and except anionic impurity process, filter after being purified containing vanadium solution;
Decationize impurity is adjusted to different pH value by containing vanadium solution, makes to change precipitation of hydroxide removing into containing the metallic cation in vanadium solution;
Except anionic impurity removes containing the phosphorus in vanadium solution and silicon: dephosphorization agent is CaCl 2, CaCl 2add with solid particle forms or be mixed with concentration be 8 ~ 12% solution morphology add, add-on is 1m 3add 0.4 ~ 1.2kg calcium chloride containing vanadium solution, dephosphorization temperature controls at>=85 DEG C, and dephosphorization pH value controls 8 ~ 9, and constant temperature churning time is not less than 30min, and constant temperature time of repose is not less than 30min; Desiliconizing agent is Al 2(SO 4) 3, Al 2(SO 4) 3add-on be 1m 3add 8.5 ~ 10.5kg containing vanadium solution, silica removal temperature controls at>=85 DEG C, and silica removal pH value controls 9 ~ 10, and constant temperature churning time is not less than 30min, and constant temperature time of repose is not less than 30min;
After purification containing no suspended substance in vanadium solution, [V]=25 ~ 30g/L, [P]≤0.015g/L, [Si]≤0.05g/L, pH=8 ~ 11;
D, to carrying out precipitation process containing adding ammonium sulfate in vanadium solution after purification, then after filtration, obtain vanadate throw out after washing impurity-removing; Precipitation processing controls precipitation temperature >=85 DEG C; The additional proportion of ammonium sulfate is: precipitation adds ammonium coefficient and controls 1 ~ 2.8; Through twice acid adding, pH value of solution=5 ~ 7 after an acid adding, pH value of solution=2 ~ 3 after secondary acid adding;
E, pull an oar to vanadate throw out, filter, then carry out carrying out washing treatment, the impurity be mingled with in removing vanadate throw out further, then drying, roasting obtain Vanadium Pentoxide in FLAKES product; When vanadate throw out is pulled an oar, control making beating temperature >=80 DEG C, beating time 10 ~ 40min.
2. the preparation method of high purity vanadic anhydride according to claim 1, is characterized in that: described in step a is vanadium extraction by converter blowing gained vanadium slag containing vanadium raw materials.
CN201310111038.1A 2013-04-01 2013-04-01 Preparation method of high-purity vanadium pentoxide CN103194603B (en)

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Address before: 617000 Airport Road, East District, Panzhihua, Sichuan Province, No. 10

Patentee before: Panzhihua University

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