CN107500353A - High-purity sodium metavanadate and preparation method thereof - Google Patents

High-purity sodium metavanadate and preparation method thereof Download PDF

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Publication number
CN107500353A
CN107500353A CN201710846331.0A CN201710846331A CN107500353A CN 107500353 A CN107500353 A CN 107500353A CN 201710846331 A CN201710846331 A CN 201710846331A CN 107500353 A CN107500353 A CN 107500353A
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CN
China
Prior art keywords
silicon
preparation
metavanadate
purity
sodium
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CN201710846331.0A
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Chinese (zh)
Inventor
鲁冲
鲁爱霞
窦勇
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Wuhu Renben Alloy Co Ltd
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Wuhu Renben Alloy Co Ltd
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Priority to CN201710846331.0A priority Critical patent/CN107500353A/en
Publication of CN107500353A publication Critical patent/CN107500353A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00Compounds of vanadium
    • C01G31/003Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/10Solid density
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention discloses a kind of high-purity sodium metavanadate and preparation method thereof, the preparation method includes:(1) will contain vanadium leachate by the first alkalescence anion-exchange resin carry out silicon absorption, obtain remove silicon after contain vanadium leachate;(2) vanadium leachate is contained after obtaining except silicon and phosphorus except phosphorus absorption is carried out by the second alkalescence anion-exchange resin containing vanadium leachate after silicon by described;(3) ammonium metavanadate is obtained except containing after silicon and phosphorus adds precipitation agent in vanadium leachate to described;(4) ammonium metavanadate is dissolved in sodium hydroxide solution, obtains sodium vanadate solution;(5) by the sodium vanadate solution evaporative crystallization, high-purity sodium metavanadate is obtained.High-purity sodium metavanadate purity that the method for the present invention provides is good, can meet the needs of people are to high-purity sodium metavanadate.

Description

High-purity sodium metavanadate and preparation method thereof
Technical field
The invention belongs to field of chemicals, more particularly, to a kind of high-purity sodium metavanadate and preparation method thereof.
Background technology
Sodium metavanadate is white or flaxen crystal, relative density 2.79,630 DEG C of fusing point.It is dissolved in water, it is molten at 25 DEG C Xie Du is 21.1g/100mlH2O, it is 38.8g/100ml/H at 75 DEG C2O, it is slightly soluble in ethanol.Can be used as chemical reagent, catalyst, Drier, mordant, ammonium vanadate and potassium metavanadate are manufactured, be also used for medical treatment photograph, plant inoculating and corrosion inhibitor etc..
With the extensive use of sodium metavanadate, purity requirement more and more higher of the people to sodium metavanadate, therefore, it is necessary to carry For a kind of preparation method of high-purity sodium metavanadate, to meet the needs of people are to high-purity sodium metavanadate.
The content of the invention
It is an object of the invention to provide a kind of preparation method of high-purity sodium metavanadate, to meet people to high-purity sodium metavanadate Demand.
To achieve these goals, an aspect of of the present present invention provides a kind of preparation method of high-purity sodium metavanadate, the preparation Method includes:
(1) will contain vanadium leachate by the first alkalescence anion-exchange resin carry out silicon absorption, obtain remove silicon after contain vanadium Leachate;
(2) obtained described except phosphorus absorption is carried out by the second alkalescence anion-exchange resin containing vanadium leachate after silicon Except containing vanadium leachate after silicon and phosphorus;
(3) ammonium metavanadate is obtained except containing after silicon and phosphorus adds precipitation agent in vanadium leachate to described;
(4) ammonium metavanadate is dissolved in sodium hydroxide solution, obtains sodium vanadate solution;
(5) by the sodium vanadate solution evaporative crystallization, high-purity sodium metavanadate is obtained.
Preferably, first alkalescence anion-exchange resin is the gel-type for being capable of selective absorption silicic acid hydrogen radical ion Anion exchange resin.
Preferably, second alkalescence anion-exchange resin is the gel-type the moon for being capable of selective absorption phosphate anion Ion exchange resin.
Preferably, the precipitation agent is ammonium chloride, ammonium sulfate or ammoniacal liquor.
Preferably, using the conditioning agent regulation pH containing vanadium leachate except after silicon and phosphorus as 8.5~9.5.
Preferably, the conditioning agent is sodium hydroxide and/or sodium acid carbonate.
Another aspect of the present invention provides high-purity sodium metavanadate prepared by a kind of preparation method of above-mentioned high-purity sodium metavanadate.
Technical scheme, pass through the first alkalescence anion-exchange resin and the second alkalescence anion-exchange resin point Do not remove containing the silicon and phosphorus in vanadium leachate, then by high to purity is obtained containing addition precipitation agent in vanadium leachate after filtering Ammonium metavanadate;And then high-purity sodium metavanadate is obtained by evaporative crystallization using the high ammonium metavanadate of purity.
Other features and advantages of the present invention will be described in detail in subsequent specific embodiment part.
Embodiment
The preferred embodiment of the present invention is described in more detail below.Although the following describe being preferable to carry out for the present invention Mode, however, it is to be appreciated that may be realized in various forms the present invention without should be limited by embodiments set forth herein.Phase Instead, there is provided these embodiments be in order that the present invention is more thorough and complete, and can be by the scope of the present invention intactly It is communicated to those skilled in the art.
An aspect of of the present present invention provides a kind of preparation method of high-purity sodium metavanadate, and the preparation method includes:
(1) will contain vanadium leachate by the first alkalescence anion-exchange resin carry out silicon absorption, obtain remove silicon after contain vanadium Leachate;
(2) obtained described except phosphorus absorption is carried out by the second alkalescence anion-exchange resin containing vanadium leachate after silicon Except containing vanadium leachate after silicon and phosphorus;
(3) ammonium metavanadate is obtained except containing after silicon and phosphorus adds precipitation agent in vanadium leachate to described;
(4) ammonium metavanadate is dissolved in sodium hydroxide solution, obtains sodium vanadate solution;
(5) by the sodium vanadate solution evaporative crystallization, high-purity sodium metavanadate is obtained.
In accordance with the present invention it is preferred that first alkalescence anion-exchange resin is being capable of selective absorption silicic acid hydrogen radical The gel-type anion exchanger resin of ion.
In accordance with the present invention it is preferred that second alkalescence anion-exchange resin for can selective absorption phosphate radical from The gel-type anion exchanger resin of son.
In accordance with the present invention it is preferred that the precipitation agent is ammonium chloride, ammonium sulfate or ammoniacal liquor.
In accordance with the present invention it is preferred that using the conditioning agent regulation pH containing vanadium leachate except after silicon and phosphorus as 8.5~ 9.5。
In accordance with the present invention it is preferred that the conditioning agent is sodium hydroxide and/or sodium acid carbonate.
Preferably, each raw material of the invention for preparing high-purity sodium metavanadate can be by commercially available.
Another aspect of the present invention provides high-purity sodium metavanadate prepared by a kind of preparation method of above-mentioned high-purity sodium metavanadate.
High-purity sodium metavanadate purity that the method for the present invention provides is good, can meet need of the people to high-purity sodium metavanadate Ask.
The present invention is further illustrated by the following examples:
Embodiment 1
A kind of preparation method of high-purity sodium metavanadate is present embodiments provided, the preparation method includes:
(1) will contain vanadium leachate by the first alkalescence anion-exchange resin carry out silicon absorption, obtain remove silicon after contain vanadium Leachate, wherein, first alkalescence anion-exchange resin is the gel-type the moon for being capable of selective absorption silicic acid hydrogen radical ion Ion exchange resin;
(2) obtained described except phosphorus absorption is carried out by the second alkalescence anion-exchange resin containing vanadium leachate after silicon Except containing vanadium leachate after silicon and phosphorus, wherein, second alkalescence anion-exchange resin is being capable of selective absorption phosphate radical The gel-type anion exchanger resin of ion;
(3) ammonium metavanadate is obtained except containing after silicon and phosphorus adds precipitation agent in vanadium leachate to described, wherein, with hydrogen-oxygen It is 8.5~9.5 to change the sodium regulation pH containing vanadium leachate except after silicon and phosphorus, and the precipitation agent is ammonium chloride;
(4) ammonium metavanadate is dissolved in sodium hydroxide solution, obtains sodium vanadate solution;
(5) by the sodium vanadate solution evaporative crystallization, high-purity sodium metavanadate is obtained.
Embodiment 2
A kind of preparation method of high-purity sodium metavanadate is present embodiments provided, the preparation method includes:
(1) will contain vanadium leachate by the first alkalescence anion-exchange resin carry out silicon absorption, obtain remove silicon after contain vanadium Leachate, wherein, first alkalescence anion-exchange resin is the gel-type the moon for being capable of selective absorption silicic acid hydrogen radical ion Ion exchange resin;
(2) obtained described except phosphorus absorption is carried out by the second alkalescence anion-exchange resin containing vanadium leachate after silicon Except containing vanadium leachate after silicon and phosphorus, wherein, second alkalescence anion-exchange resin is being capable of selective absorption phosphate radical The gel-type anion exchanger resin of ion;
(3) ammonium metavanadate is obtained except containing after silicon and phosphorus adds precipitation agent in vanadium leachate to described, wherein, with carbonic acid The hydrogen sodium regulation pH containing vanadium leachate except after silicon and phosphorus is 8.5~9.5, and the precipitation agent is ammoniacal liquor;
(4) ammonium metavanadate is dissolved in sodium hydroxide solution, obtains sodium vanadate solution;
(5) by the sodium vanadate solution evaporative crystallization, high-purity sodium metavanadate is obtained.
It is described above various embodiments of the present invention, described above is exemplary, and non-exclusive, and It is not limited to disclosed each embodiment.In the case of without departing from the scope and spirit of illustrated each embodiment, for this skill Many modifications and changes will be apparent from for the those of ordinary skill in art field.

Claims (7)

1. a kind of preparation method of high-purity sodium metavanadate, it is characterised in that the preparation method includes:
(1) vanadium leachate will be contained silicon absorption is carried out by the first alkalescence anion-exchange resin, obtained except the vanadium that contains after silicon leaches Liquid;
(2) obtain removing silicon except phosphorus absorption is carried out by the second alkalescence anion-exchange resin containing vanadium leachate after silicon by described Contain vanadium leachate with after phosphorus;
(3) ammonium metavanadate is obtained except containing after silicon and phosphorus adds precipitation agent in vanadium leachate to described;
(4) ammonium metavanadate is dissolved in sodium hydroxide solution, obtains sodium vanadate solution;
(5) by the sodium vanadate solution evaporative crystallization, high-purity sodium metavanadate is obtained.
2. the preparation method of high-purity sodium metavanadate according to claim 1, wherein, first alkali anion exchanges tree Fat is the gel-type anion exchanger resin for being capable of selective absorption silicic acid hydrogen radical ion.
3. the preparation method of high-purity sodium metavanadate according to claim 1, wherein, second alkali anion exchanges tree Fat is the gel-type anion exchanger resin for being capable of selective absorption phosphate anion.
4. the preparation method of high-purity sodium metavanadate according to claim 1, wherein, the precipitation agent is ammonium chloride, sulfuric acid Ammonium or ammoniacal liquor.
5. the preparation method of high-purity sodium metavanadate according to claim 1, wherein, to remove silicon and phosphorus described in conditioning agent regulation The pH containing vanadium leachate afterwards is 8.5~9.5.
6. the preparation method of high-purity sodium metavanadate according to claim 5, wherein, the conditioning agent be sodium hydroxide and/ Or sodium acid carbonate.
7. high-purity metavanadic acid prepared by the preparation method of high-purity sodium metavanadate according to any one in claim 1-6 Sodium.
CN201710846331.0A 2017-09-19 2017-09-19 High-purity sodium metavanadate and preparation method thereof Pending CN107500353A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110723750A (en) * 2019-10-24 2020-01-24 成都先进金属材料产业技术研究院有限公司 Direct preparation of high-purity V from alkaline vanadium-containing leaching solution2O5Method (2)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102502570A (en) * 2011-11-29 2012-06-20 芜湖人本合金有限责任公司 Production method of medical sodium metavanadate
CN104628086A (en) * 2015-01-06 2015-05-20 大连东泰资源再生有限公司 Novel phosphorus removal method for alkaline leaching solution containing molybdenum and vanadium
CN104628032A (en) * 2015-01-06 2015-05-20 大连东泰资源再生有限公司 Method for preparing high-purity ammonium metavanadate from spent catalyst
CN105271406A (en) * 2015-09-28 2016-01-27 攀钢集团攀枝花钢铁研究院有限公司 Sodium metavanadate preparation method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102502570A (en) * 2011-11-29 2012-06-20 芜湖人本合金有限责任公司 Production method of medical sodium metavanadate
CN104628086A (en) * 2015-01-06 2015-05-20 大连东泰资源再生有限公司 Novel phosphorus removal method for alkaline leaching solution containing molybdenum and vanadium
CN104628032A (en) * 2015-01-06 2015-05-20 大连东泰资源再生有限公司 Method for preparing high-purity ammonium metavanadate from spent catalyst
CN105271406A (en) * 2015-09-28 2016-01-27 攀钢集团攀枝花钢铁研究院有限公司 Sodium metavanadate preparation method

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官清等: ""用偏钒酸铵制备偏钒酸钠工艺研究"", 《无机盐工业》 *
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110723750A (en) * 2019-10-24 2020-01-24 成都先进金属材料产业技术研究院有限公司 Direct preparation of high-purity V from alkaline vanadium-containing leaching solution2O5Method (2)

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Application publication date: 20171222