CN106430305B - A kind of production method of high density ammonium metavanadate - Google Patents

A kind of production method of high density ammonium metavanadate Download PDF

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Publication number
CN106430305B
CN106430305B CN201610792574.6A CN201610792574A CN106430305B CN 106430305 B CN106430305 B CN 106430305B CN 201610792574 A CN201610792574 A CN 201610792574A CN 106430305 B CN106430305 B CN 106430305B
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ammonium
potassium
ammonium metavanadate
high density
magnesium
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CN106430305A (en
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宋明明
陈彦博
曾繁武
郝玥
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Dalian Bolong New Materials Co ltd
Dalian Rongke Energy Storage Group Co ltd
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Dalian Bo Rong New Material Ltd By Share Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10—Inorganic compounds or compositions
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • C30B29/30—Niobates; Vanadates; Tantalates
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of production method of high density ammonium metavanadate.Mainly comprise the following steps：(1) auxiliary agent is added in containing vanadium solution in advance；(2) solution is heated up；(3) add ammonium salt and obtain ammonium metavanadate precipitate；(4) cooling makes vanadium precipitation complete；(5) dry.It is an advantage of the invention that the ammonium metavanadate produced is the thick perfect monocrystalline of particle, apparent density is more than 1g/cm3, can effectively prevent dust problem during operation.

Description

A kind of production method of high density ammonium metavanadate
Technical field
The present invention relates to the production method of high density ammonium metavanadate, belong to the field of metallurgical chemistry of vanadium.
Background technology
The production method of ammonium metavanadate, it is to obtain to contain vanadium leachate first, by neutralization, purification and impurity removal, adjusts pH to 7- 9, vanadium exists in the form of metavanadic acid root anion, adds ammonium salt and obtains ammonium metavanadate precipitate.
During industrial production ammonium metavanadate, in order to improve production efficiency, excessive ammonium salt is often added into solution, in short-term Interior thoroughly to precipitate vanadium completely, so, the precipitation reaction degree of supersaturation of vanadium is very big, therefore obtained ammonium metavanadate accumulation The universal very little of density, it is 0.3-0.9g/cm3, microexamination is shown as the reunion (such as Fig. 1) of irregular fine particle.Operation During ammonium metavanadate powder, such as dry, shift, calcining, inevitably produce substantial amounts of dust, especially given birth in calcinations of ammonium metavanadate When producing barium oxide, ammonium metavanadate is thermally decomposed, aggregate efflorescence, and dust is even more unmanageable, seriously endangers environment and personnel Health.
When carrying out the smelting of vanadium alloy using barium oxide, operator particularlys hope to use highdensity barium oxide Grain, because during charging, highdensity particle is easily accessible inside metal liquid, so as to obtain more preferable mixed effect, The better quality of final alloy.Not only dust is big for low-density, tiny barium oxide, alloy smelting layered, it is difficult to which mixing is equal Even, product quality is low.
After highdensity ammonium metavanadate calcining, highdensity barium oxide can be obtained, how to obtain highdensity inclined vanadium Sour ammonium, the problem of just becoming a key.
The content of the invention
Present invention solves the technical problem that being the provision of a kind of production technology, current industrial ammonium metavanadate can be improved Physical characteristic, it is transformed into the state of monocrystalline, high density, bulky grain by the aggregate of fine particle, it is follow-up so as to reduce Dust during operation, improve operating environment.
The technical scheme is that：
A kind of production method of high density ammonium metavanadate, it is characterised in that comprise the steps of：
A. auxiliary agent, stirring to dissolving are added in containing vanadium solution；
B. solution is warming up to 40-100 DEG C；
C. adding precipitating reagent ammonium salt makes vanadium be precipitated in the form of ammonium metavanadate；
D. solution is cooled to room temperature；
E. filter, wash, drying, obtaining high density ammonium metavanadate；
In step a, described contains vanadium solution, can be that the burnning ash of oil containing scherbinaite adds alkali sodium roasting, is obtained by water-soluble leaching The solution obtained；
Further described contains vanadium solution, can be bone coal ore through sulfuric acid leaching, the acid solution of acquisition；
Further, the described solution for containing vanadium solution, being dead catalyst obtains through sodium roasting, water-soluble leaching；
Further described contain vanadium solution, can be vanadium-containing compound through water-soluble, alkali soluble, molten, the aqueous solution of acquisition of acid.
The one kind of auxiliary agent described in step a in sodium ion, potassium ion, magnesium ion or organic flocculant PAM；
In step a, concentration is after the auxiliary agent dissolving：Sodium ion or potassium ion 0.1-3mol/L, magnesium ion 0.05- 1mol/L, organic flocculant PAM 0.1-10g/L.
Further, in the above-mentioned technical solutions, the aqueous solution containing vanadium solution for metavanadate described in step a, its PH is 7-10；
Further, in the above-mentioned technical solutions, the pH more excellent containing vanadium solution described in step a is 8-9.5.
Further, in the above-mentioned technical solutions, vanadium solution is contained described in step a, the concentration of vanadium therein is 0.4- 2mol/L。
Further, in the above-mentioned technical solutions, sodium ion is selected from sodium sulphate, sodium carbonate, chlorine in auxiliary agent described in step a Change sodium, sodium acid carbonate, vulcanized sodium；Potassium ion be selected from potassium hydroxide, potassium chloride, potassium sulfate, potassium carbonate, saleratus, potassium nitrate, One kind in potassium sulfide, potassium rhodanate, potassium oxalate, potassium phosphate, potassium dihydrogen phosphate, potassium hydrogen phosphate, magnesium ion are selected from magnesium sulfate, nitre One kind in sour magnesium, magnesium carbonate, magnesium bicarbonate, magnesium stearate, magnesium hydroxide, organic flocculant PAM molecular weight is 1-3000 Ten thousand.
Further, in the above-mentioned technical solutions, the temperature of solution is 40-100 DEG C in step b；
Further, the optimum temperature of solution is 60-90 DEG C in step b；
Further, in the above-mentioned technical solutions, the precipitating reagent ammonium salt described in step c is selected from ammonium chloride, ammonium sulfate, grass One kind in sour ammonium, ammonium carbonate, ammonium hydrogen carbonate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate, addition are the amount of the material of ammonium root and vanadium Ratio is 1.2-3:1.
Invention beneficial effect
The production method of a kind of high density ammonium metavanadate provided by the invention, by adding metal ion in containing vanadium solution Or PAM, improve surface tension, the density of solution, change solubility of the AMV in water, additive inhibits ammonium metavanadate Forming core is broken out, hinders short grained reunion, the AMV for making newly to precipitate grows up on existing nucleus, so as to improve AMV crystallization Characteristic, obtain monocrystalline, apparent density is higher than 1g/cm3Ammonium metavanadate crystal.
Brief description of the drawings
Fig. 1 is low-apparent-density ammonium metavanadate (AMV) microphoto that common process produces to obtain；
Fig. 2 is high apparent density ammonium metavanadate AMV microphoto (the scale minimum scales that the low temperature of embodiment 1 obtains 10um)；
Fig. 3 is the microphoto (scale minimum scale 10um) for the high apparent density AMV that the high temperature of embodiment 2 obtains.
Embodiment
The conventional production process of ammonium metavanadate, it is to obtain to contain vanadium leachate first, by neutralization, purification and impurity removal, adjusts pH To 7-9, vanadium exists in the form of metavanadic acid root anion, adds ammonium salt and obtains ammonium metavanadate precipitate.Industrial production obtains inclined Ammonium vanadate bulk density very little, it is 0.3-0.9g/cm3, microexamination is shown as the group of 1um or so tiny spherical ammonium metavanadate Poly- particle, as shown in Figure 1.
Substantial amounts of dust is inevitably produced when operating ammonium metavanadate dry powder, especially produces vanadium in calcinations of ammonium metavanadate During oxide, ammonium metavanadate is thermally decomposed, aggregate efflorescence, and dust is even more unmanageable, seriously endangers environment and personnel health.
The invention provides a kind of production method of high density ammonium metavanadate.Mainly comprise the following steps：(1) in advance to containing vanadium solution Middle addition auxiliary agent；(2) solution is heated up；(3) add ammonium salt and obtain ammonium metavanadate precipitate；(4) cooling makes vanadium precipitation complete；(5) Drying.
It is an advantage of the invention that the ammonium metavanadate produced is the thick perfect monocrystalline of particle, apparent density is more than 1g/ cm3, can effectively prevent dust problem during operation.
Below for the production method mentioned in the content of the invention, illustrated with instantiation, but it is of the invention and unlimited In following examples.
Embodiment 1
By 46g sodium hydroxides, 100gV2O5Powder is added sequentially in water, stirring and dissolving, filters insoluble matter, constant volume 1000ml, obtain the sodium metavanadate solution of clarification, pH9,1.05mol/L containing V.
The PAM that 1g molecular weight is 1,000,000 is added, stirring is complete to dissolving；
Solution is warming up to 45 DEG C, adds 120g ammonium chlorides, keeping temperature stirring 2h；
25 DEG C are cooled to, continues to stir 1h；
Filtering, washs and dries ammonium metavanadate, actual measurement apparent density is 1.1g/cm3, use micro- sem observation graininess State, such as Fig. 2.
Comparison diagram 1 and Fig. 2, it is seen that the crystal structure of ammonium metavanadate is transformed into monocrystalline by the aggregate of fine particle Grain.
Embodiment 2
100g ammonium metavanadates are added in 900ml water, stirring adds 1mol potassium sulfates；
It is warming up to 85 DEG C to dissolve ammonium metavanadate, is removed by filtration insoluble matter, be settled to 1000ml, V concentration is 1.28mol/ L, potassium concn 2mol/L；
Ammonification water adjusts pH to 9；
80 DEG C of solution is kept, adds 150g ammonium sulfate, stirring precipitation 2h；
Room temperature is cooled to, continues to stir 1h；
Filtering, washs and dries ammonium metavanadate, actual measurement apparent density is 1.05g/cm3
AMV displaing micro picture is shown in Fig. 3, and comparison diagram 1, Fig. 2 and Fig. 3 are understood, ammonium metavanadate can be made by more by adding additive Crystalline substance polymerization becomes tiny monocrystalline, adds additive and raises precipitation temperature, can obtain the ammonium metavanadate of monocrystalline, bulky grain Crystal.
Embodiment 3
Use the leachate 1000ml, NaVO containing 0.7mol/L after v-bearing steel slag sodium roasting3, sulfur acid sodium 2mol/l, PH value of solution 9.5.
Magnesium sulfate 10g is added, stirring is to being completely dissolved；
Solution is warming up to 90 DEG C；
Add 130g ammonium sulfate, stirred crystallization 2h；
Room temperature is cooled to, continues to stir 1h；
Filtering, washs and dries ammonium metavanadate, actual measurement apparent density is 1.15g/cm3。

Claims (6)

1. a kind of production method of high density ammonium metavanadate, it is characterised in that comprise the steps of：
A. auxiliary agent, stirring to dissolving are added in containing vanadium solution；
B. solution is warming up to 40-100 DEG C；
C. adding precipitating reagent ammonium salt makes vanadium be precipitated in the form of ammonium metavanadate；
D. solution is cooled to room temperature；
E. filter, wash, drying, obtaining high density ammonium metavanadate；
In step a, the one kind of the auxiliary agent in sodium ion, potassium ion, magnesium ion or organic flocculant PAM；Sodium ion Selected from sodium sulphate, sodium chloride, vulcanized sodium；Potassium ion is selected from potassium chloride, potassium sulfate, potassium nitrate, potassium sulfide, potassium rhodanate, oxalic acid One kind in potassium, potassium phosphate, potassium dihydrogen phosphate, potassium hydrogen phosphate；
In step a, concentration is after the auxiliary agent dissolving：Sodium ion or potassium ion 0.1-3mol/L, magnesium ion 0.05-1mol/L, Organic flocculant PAM 0.1-10g/L.
2. the production method of a kind of high density ammonium metavanadate according to claim 1, it is characterised in that described in step a Containing the aqueous solution that vanadium solution is vanadate, its pH is 7-10.
3. the production method of a kind of high density ammonium metavanadate according to claim 1, it is characterised in that described in step a Containing vanadium solution, the concentration of vanadium therein is 0.4-2mol/L.
4. the production method of a kind of high density ammonium metavanadate according to claim 1, it is characterised in that helped described in step a The one kind of magnesium ion in magnesium sulfate, magnesium nitrate, magnesium carbonate, magnesium bicarbonate, magnesium stearate, magnesium hydroxide, You Jixu in agent Solidifying agent PAM molecular weight is 1-3000 ten thousand.
5. the production method of a kind of high density ammonium metavanadate according to claim 1, it is characterised in that described in step c Precipitating reagent ammonium salt is in ammonium chloride, ammonium sulfate, ammonium oxalate, ammonium carbonate, ammonium hydrogen carbonate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate It is a kind of.
6. the production method of a kind of high density ammonium metavanadate according to claim 1, it is characterised in that described in step c For the addition of precipitating reagent ammonium salt in terms of ammonium root, the ratio between ammonium root and vanadium V amount of material is 1.2-3:1.
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CN107445205A (en) * 2017-08-17 2017-12-08 芜湖人本合金有限责任公司 A kind of method for producing sodium metavanadate and products thereof and application
CN107416900A (en) * 2017-08-31 2017-12-01 攀钢集团钒业有限公司 A kind of method for efficiently preparing high-purity sodium metavanadate
PL237761B1 (en) * 2018-03-01 2021-05-31 Politechnika Gdanska Method for producing ammonium metavanadate
CN108975398A (en) * 2018-09-05 2018-12-11 大连博融新材料有限公司 A kind of high density potassium metavanadate and preparation method thereof
CN109179504B (en) * 2018-10-19 2020-12-04 河钢股份有限公司承德分公司 Method for preparing large-particle-size ammonium metavanadate
CN110963528B (en) * 2019-12-20 2022-06-28 大连博融新材料有限公司 Spherical high-density ammonium metavanadate, and preparation method and application thereof

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CN102502823A (en) * 2011-10-21 2012-06-20 攀钢集团攀枝花钢铁研究院有限公司 Preparation method for preparing high-tap density ammonium poly-vanadate
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Address after: No. 20, Yingchun Street, Huayuankou Economic Zone, Dalian, Liaoning Province, 116000

Patentee after: Dalian Rongke Energy Storage Group Co.,Ltd.

Address before: No. 20, Yingchun Street, Huayuankou Economic Zone, Dalian, Liaoning Province, 116000

Patentee before: DALIAN BOLONG NEW MATERIALS Co.,Ltd.

Address after: No. 20, Yingchun Street, Huayuankou Economic Zone, Dalian, Liaoning Province, 116000

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