CN1040132C - Settling process for extracting vanadium from bone coal - Google Patents

Settling process for extracting vanadium from bone coal Download PDF

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Publication number
CN1040132C
CN1040132C CN92107097A CN92107097A CN1040132C CN 1040132 C CN1040132 C CN 1040132C CN 92107097 A CN92107097 A CN 92107097A CN 92107097 A CN92107097 A CN 92107097A CN 1040132 C CN1040132 C CN 1040132C
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China
Prior art keywords
bone coal
vanadium
calcination
charcoal
temperature
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Expired - Fee Related
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CN92107097A
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CN1082118A (en
Inventor
谢永习
谢兆伸
谢钰
周小枚
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QIANCHENG VANADIUM FACTORY HONGJIANG CITY HUNAN PROV
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QIANCHENG VANADIUM FACTORY HONGJIANG CITY HUNAN PROV
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Priority to CN92107097A priority Critical patent/CN1040132C/en
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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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The present invention discloses a comprehensive method for precipitating vanadium from stone coal, which uses stone coal whose V2O5 content is more than 1% as raw materials. The method comprises the steps of natural heap calcination and decarburization, ball preparation by ball mills, oxidation calcination (fine crushing, water addition, sulfuric acid addition and ammonium addition), impurity leaching and separation (sulfuric acid is added to a clear solution, and the pH value is from 2 to 2.5), precipitation (ammonium polyorthovanadate), drying and calcination refinement (the purity is more than 99%).

Description

Settling process for extracting vanadium from bone coal
The present invention relates to a kind of smelting process of from bone coal, extracting V2O5.
Domestic and international industrial extraction vanadium method has: and (1) sodium salt oxidizing roasting-water logging goes out-and the heavy molten ammonium salt precipitation of thick vanadium-alkali of acid-pyrolysis deoxidation produces smart vanadium; (2) oxidizing roasting-acidleach go out-intermediate salt-extraction-ammonium salt precipitation-calcination produces smart vanadium; (3) oxidizing roasting-acidleach go out-extract-ammonium salt precipitation-calcination produces smart vanadium; In the patent document of the patent No. 85102378, a kind of method of the vanadium slag bakes to burn the article infusion vanadium extraction that atomizes is disclosed.Aforesaid method all fails fundamentally to solve the oxidation and the conversion of vanadium in the bone coal, and promptly the vanadium in the coal is by being oxidizing to high price (pentavalent) at a low price, and transfers the bigger solvable vanadium of solubleness (comprising water-soluble vanadium and sour molten vanadium) to, enters solution, realizes solid-liquid separation.Thereby, V 2O 5Commentaries on classics soak rate and the rate of recovery is not high, the bone coal consumption is big, consumption of raw material is many, and is bigger to the production cost influence.Simultaneously, during roasting, contain a large amount of CL, HCL gas and a small amount of SO in the discharged gas fume 2Gas, environmental pollution is serious.
The present invention seeks to, the operational path by selecting to hold water improves V in the bone coal roasting 2O 5Transformation efficiency, leaching yield, deposition rate, direct yield and total yield, overcome above-mentioned deficiency.
Purpose of the present invention can go to realize by following processing method:
(1) bone coal takes off charcoal: will contain V 2O 5>1.0% the bone coal charcoal that takes off burnt in a heap naturally makes the bone coal ash thermal value of taking off behind the charcoal between 627~1254 joules/kilogram;
(2) ball milling system ball: the bone coal ash that will take off behind the charcoal carries out ball milling, and its granularity is 125~76 μ m;
(3) oxidizing roasting: with the ball milling powder, make the radius of a ball=5~10cm, the flat kiln of packing into, the degree roasting is 1~1.5 hour under 800~850 ℃ temperature, and is again that the grog after the roasting is in small, broken bits to 250~152 μ m;
(4) leach and separate; Grog adds water, the solid-liquid weight ratio is 1: 1.5, and add sulfuric acid by 0.8% of clinker quantity, stirring heating 15 minutes to 70~80 ℃ is controlled PH=2~2.5, adds ammoniacal liquor or the NaoH or the carbon ammonium of vanadium amount about 2 times (W/W) again, control PH=8~8.5, stirring heating 5 minutes, 80~85 ℃ of temperature, clarification;
(5) separate clear liquid: add H in the clear liquid after separation 2SO 4, with steam heating>90 ℃, stir more than 45 minutes control PH=2~2.5, and precipitation obtains ammonium poly-vanadate;
(6) calcination is refining: the oven dry ammonium poly-vanadate makes its purity V 2O 5>80%, the oxidation calcination, 450 ℃ of temperature, make the smart vanadium of purity>99.00% at 4 hours time.
The present invention has compared following advantage with existing process for extracting vanadium method:
Correct, the process simplification of operational path, alleviated labour intensity, improved production efficiency;
2. improved roasting transformation efficiency and total yield, the resource utilization height, required reagent (acid, the alkali etc.) kind of technology is few, and consumption is little, has reduced production cost;
3. HCL, CL that the salt sodium roasting produces have been eliminated 2Flue gas environmental pollution and equipment corrosion.
Lift a specific embodiment below:
1. bone coal takes off charcoal: (the bone coal ash thermal value of taking off behind the charcoal is 1045 joules/kilogram for the bone coal of φ=5~10cm), the charcoal that takes off burnt in a heap naturally with the bulk of garbled 40 tons of vanadiumcontents 1.12%.
2. ball milling system ball: take off the bone coal ash of ball milling behind the charcoal, make ball (φ=8cm), guarantee that the ball milling granularity is 125 μ m.
3. oxidizing roasting: with ball that makes (the flat kiln of packing into of φ=8cm), 850 ℃ of roasting temperatures 1.5 hours, again that this grog is in small, broken bits to 101 μ m.
4. leach and separate: grog in small, broken bits is inserted in the agitated pool, adds 60 tons of water and 0.32 ton of sulfuric acid, stirring heating 15 minutes to 80 ℃ is controlled its PH=2.5, adds 0.448 ton of ammoniacal liquor again, and stirring heating 5 minutes to 85 ℃ is controlled PH=8.0, clarifies.
5. separation clear liquid: after separation, add H in the clear liquid 2SO 4, control PH=2.5 with steam-heated cal(l)andria to 85 ℃, stirred 45 minutes, precipitation acquisition ammonium poly-vanadate.
6. calcination is refining: will precipitate the ammonium poly-vanadate oven dry that obtains, and make its purity contain V 2O 5>80%, carry out the oxidation calcination, 450 ℃ of temperature, promptly make purity and are 99.67% smart vanadium at 4 hours time.

Claims (1)

1. settling process for extracting vanadium from bone coal, it is to contain V 2O 5>1.0% bone coal is a raw material, it is characterized in that operational path and reaction formation condition are:
(1) bone coal takes off charcoal: the charcoal that takes off burnt in a heap naturally, take off bone coal ash thermal value behind the charcoal between 627~1254 joules/kilogram;
(2) ball milling system ball: granularity 125~76 μ m;
(3) oxidizing roasting: the flat kiln of packing into, 800-850 ℃ roasting temperature 1~1.5 hour, that the grog after the roasting is in small, broken bits to 250~152 μ m;
(4) leach and separate; Grog adds water, the solid-liquid weight ratio is 1: 1.5, add sulfuric acid, heated and stirred, 70~80 ℃ of Heating temperatures by 0.8% of clinker quantity, churning time 15 minutes, control PH=2~2.5, add ammoniacal liquor or the NaoH or the carbon ammonium of vanadium amount about 2 times (W/W) again, control PH=8~8.5, stirring heating 5 minutes, 80~85 ℃ of temperature, clarification;
(5) separate clear liquid; In clear liquid, add H 2SO 4, steam heating use in control PH=2~2.5, and stirred more than 45 minutes temperature>90 ℃, precipitation generation ammonium poly-vanadate;
(6) calcination is refining; The oven dry ammonium poly-vanadate, purity V 2O 5>80%, the oxidation calcination, 450 ℃ of temperature, make the smart vanadium of purity>99.00% at 4 hours time.
CN92107097A 1992-08-12 1992-08-12 Settling process for extracting vanadium from bone coal Expired - Fee Related CN1040132C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN92107097A CN1040132C (en) 1992-08-12 1992-08-12 Settling process for extracting vanadium from bone coal

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN92107097A CN1040132C (en) 1992-08-12 1992-08-12 Settling process for extracting vanadium from bone coal

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CN1082118A CN1082118A (en) 1994-02-16
CN1040132C true CN1040132C (en) 1998-10-07

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Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1055505C (en) * 1996-12-06 2000-08-16 湖南省安化县东坪钒冶炼厂 Extraction procedure for wet smelting process and its application in vanadium smelting
CN1057130C (en) * 1996-12-06 2000-10-04 湖南省安化县东坪钒冶炼厂 Vanadium pentoxide extracting method from stone coal vanadium ore
CN1074050C (en) * 1999-06-12 2001-10-31 湖南省安化县碳化硅厂 Pretreatment method for extracting vanadium pentoxide from vanadium-contained ore
CN100526486C (en) * 2006-07-13 2009-08-12 昆明理工大学 Method of oxidizing transforming leaching vanadium from stone coal under pressure field
CN102492832A (en) * 2011-12-30 2012-06-13 北京神雾环境能源科技集团股份有限公司 Method for roasting vanadium-containing bone coal by utilization of rich oxygen
CN102899488B (en) * 2012-11-05 2015-01-07 内蒙古科技大学 Resource transforming method for separating rare earth from fluorine by utilizing rare earth ore concentrate hydrochloric leachate
CN104152723B (en) * 2014-08-22 2016-06-22 武汉工程大学 A kind of method of Leaching Vanadium from high calcium magnesium types Rock coal containing alum
CN106636680B (en) * 2016-10-30 2022-08-26 武汉轻工大学 Large-scale accumulation carbonization method for extracting vanadium from high-silica coal

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1049642A (en) * 1990-07-12 1991-03-06 江西省煤炭工业科学研究所 Stone coal ash sulfuric acid is mixed the acid slaking water logging of heating and is extracted the vanadium pentoxide technical process
CN1059885A (en) * 1990-07-24 1992-04-01 湖南省煤炭科学研究所 A kind of novel method of from contain the scherbinaite coal, extracting Vanadium Pentoxide in FLAKES

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1049642A (en) * 1990-07-12 1991-03-06 江西省煤炭工业科学研究所 Stone coal ash sulfuric acid is mixed the acid slaking water logging of heating and is extracted the vanadium pentoxide technical process
CN1059885A (en) * 1990-07-24 1992-04-01 湖南省煤炭科学研究所 A kind of novel method of from contain the scherbinaite coal, extracting Vanadium Pentoxide in FLAKES

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