CN100537797C - A kind of stone coal vanadium-extracting ore decomposition method - Google Patents

A kind of stone coal vanadium-extracting ore decomposition method Download PDF

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CN100537797C
CN100537797C CNB2008100310500A CN200810031050A CN100537797C CN 100537797 C CN100537797 C CN 100537797C CN B2008100310500 A CNB2008100310500 A CN B2008100310500A CN 200810031050 A CN200810031050 A CN 200810031050A CN 100537797 C CN100537797 C CN 100537797C
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roasting
vanadium
sulfuric acid
decomposition method
scherbinaite
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CN101260464A (en
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王学文
王明玉
李青刚
肖连生
张贵清
刘万里
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Central South University
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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

Abstract

The present invention is a kind of stone coal vanadium-extracting ore decomposition method, to contain the scherbinaite colliery earlier grinds, adding sulfuric acid again mixes thoroughly, roasting at a lower temperature then, guarantee the non-volatile and decomposition at roasting process of sulfuric acid and vitriol, the calcining that roasting obtains adds water logging and goes out, and it is short to have working cycle, the leaching yield height of vanadium, advantage such as production environment is good.

Description

A kind of stone coal vanadium-extracting ore decomposition method
Technical field
The present invention relates to a kind of stone coal vanadium-extracting ore decomposition method.
Background technology
Bone coal is a kind of important vanadium resource that contains, and the vanadium in the bone coal mainly is present in the mica with the in-phase form of class matter, extract vanadium from bone coal, vanadium must be dissociated out from the mica crystalline phase.The bone coal ore decomposes and roughly is divided into full wet processing, pyrogenic process-wet method combined technology two big classes at present.Contain that the scherbinaite coal ore decomposes that full wet processing mainly contains that the sulfuric acid normal pressure leaches and two kinds of high pressure leachings.Adopt the normal pressure extract technology, bone coal is earlier levigate to particle diameter 0.106-0.071mm, presses 15~30% of bone coal mineral amount again and adds sulfuric acid, and 80~90 ℃ were leached 36~48 hours, and the leaching yield of vanadium is generally 60~70%.Bone coal normal pressure sulfuric acid leaches, and the activity duration is long, the tooling cost height.The employing high pressure leaches, and bone coal also is earlier levigate to particle diameter 0.106-0.071mm, adds 150~180 ℃ of pressures of sulfuric acid and aerating oxygen or air again and boils 4~8 hours, and sulfuric acid consumption and normal pressure leach roughly the same, and the leaching yield of vanadium is generally 70~80%.Bone coal high pressure extract technology exists operation discontinuous, defectives such as energy consumption height.The bone coal of now having developed decomposes pyrogenic process-wet method combined technology sodium roasting-water logging, empty roasting-acidleach, calcification baking-acidleach, calcification baking-low temperature sulfurization roasting-water logging etc., its hollow roasting-acid leaching process only is applicable to that minority contains the scherbinaite colliery, and calcification baking-acid leaching process, the big cost height of acid consumption, the leaching yield of vanadium generally has only 50~60%.Though the leaching yield of sodium roasting-water logging technology vanadium can reach more than 70%, and be fit to various types of bone coals ore deposit, add the sodium-chlor roasting but contain the scherbinaite coal, when temperature reaches more than 500 ℃, emit the flue gas that contains sour gas such as HCl in a large number, environment is caused serious harm.Containing the scherbinaite coal adopts sodium roasting vanadium-extracting to be subjected to the strictness restriction of environmental administration.Calcification baking-low temperature sulfurization roasting-water logging process operation environment is good, and the leaching yield of vanadium can reach 70~80%, but double roasting technology is loaded down with trivial details.
Summary of the invention
The objective of the invention is to shorten working cycle, enhance productivity, the invention provides a kind of stone coal vanadium-extracting ore decomposition method in order to accelerate extracting vanadium from stone coal ore decomposition rate.
Technical scheme of the present invention is:
The decomposition step that contains the scherbinaite colliery comprises (1) ore reduction, to contain the scherbinaite colliery earlier and be crushed to particle diameter less than 0.154mm, (2) low temperature sulfurization roasting, to add concentration by 10%~40% of bone coal quality be that 95%~98% the vitriol oil is mixed thoroughly with the scherbinaite colliery that contains of fragmentation, under 150~350 ℃ temperature, carry out roasting, roasting time is 1~4 hour, (3) water logging: the calcining that roasting is obtained adds water by solid-liquid weight ratio 1:0.8~1.5,50~100 ℃ of agitation leachs 0.5~4 hour.
To contain the scherbinaite colliery earlier grinds, adding the vitriol oil again mixes thoroughly, roasting at a lower temperature then, guarantee the non-volatile and decomposition of sulfuric acid and vitriol at roasting process, the calcining that roasting obtains adds water logging and goes out, to replace existing stone coal vanadium-extracting ore decomposition method, reach the rate of decomposition that improves vanadium, effect such as cut down finished cost.
Specific embodiment of the invention process is:
To contain the scherbinaite colliery earlier and be milled to particle diameter less than 0.154mm, after mixing thoroughly by 10~30% adding sulfuric acid of its quality again, under 150~350 ℃ temperature, carry out roasting, roasting time is 1~4 hour, and the calcining that roasting obtains adds 0.5~4 hour after-filtration of 50~100 ℃ of agitation leachs of water by solid-liquid weight ratio 1:0.8~2.2.
(V 2O 3) c+3H 2SO 4→V 2(SO 4) 3+3H 2O
(Al 2O 3) c+3H 2SO 4→Al 2(SO 4) 3+3H 2O
(Fe 2O 3) c+3H 2SO 4→Fe 2(SO 4) 3+3H 2O
(FeO) c+H 2SO 4→FeSO 4+3H 2O
(K 2O) c+H 2SO 4→K 2SO 4+H 2O
The present invention compares with existing technology and has the following advantages and effect:
1. contain the sulfurization roasting of scherbinaite coal low temperature, can avoid the decomposition and the volatilization of sulfuric acid and vitriol, sulfuric acid utilization ratio height, reagent dosage is few, and operating environment is good.
2. contain the sulfurization roasting of scherbinaite coal low temperature, can effectively destroy its mica crystal phase structure, make vanadium can be successfully from mica cleavage come out.
3. contain calcining that the sulfurization roasting of scherbinaite coal low temperature obtains and add water and stir vanadium and leach easily, working cycle is short, the production efficiency height.
Embodiment
Below in conjunction with embodiment, the present invention is further described, following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1
100g bone coal ore deposit is levigate to particle diameter less than 0.125mm, add after the 7ml vitriol oil mixes thoroughly, put retort furnace into, 200 ℃ of roastings 3 hours, calcining cooling back adds water by solvent and solute weight ratio 1:1, and 80 ℃ of agitation leachs were filtered in 2 hours, content of vanadium in sampling analysis filtrate and the filter residue, (g/L) is as follows for experimental result:
Figure C200810031050D00051
Embodiment 2
100g bone coal ore deposit is levigate to particle diameter less than 0.106mm, after the adding 20ml vitriol oil is mixed thoroughly, put retort furnace into, 250 ℃ of roastings 2 hours, calcining cooling back adds water by solvent and solute weight ratio 1.2:1,100 ℃ of agitation leachs were filtered in 2 hours, content of vanadium in sampling analysis filtrate and the filter residue, and (g/L) is as follows for experimental result:
Figure C200810031050D00052
Embodiment 3
100g bone coal ore deposit is levigate to particle diameter less than 0.071mm, after the adding 15ml vitriol oil is mixed thoroughly, put retort furnace into, 300 ℃ of roastings 1 hour, calcining cooling back adds water by solvent and solute weight ratio 1.5:1,60 ℃ of agitation leachs were filtered in 3 hours, content of vanadium in sampling analysis filtrate and the filter residue, and (g/L) is as follows for experimental result:
Figure C200810031050D00053

Claims (1)

1, a kind of stone coal vanadium-extracting ore decomposition method, it is characterized in that, the decomposition step that contains the scherbinaite colliery comprises (1) ore reduction, to contain the scherbinaite colliery earlier and be crushed to particle diameter less than 0.154mm, (2) low temperature sulfurization roasting, the scherbinaite colliery that contains of fragmentation is mixed thoroughly by 10%~40% adding sulfuric acid of bone coal quality, under 150~350 ℃ temperature, carry out roasting, roasting time is 1~4 hour, (3) water logging: the calcining that roasting is obtained adds water by solid-liquid weight ratio 1:0.8~1.5,50~100 ℃ of agitation leachs 0.5~4 hour; The sulfuric acid that step (2) adds is that concentration is 95%~98% the vitriol oil.
CNB2008100310500A 2008-04-11 2008-04-11 A kind of stone coal vanadium-extracting ore decomposition method Expired - Fee Related CN100537797C (en)

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CN101921912A (en) * 2010-03-04 2010-12-22 北京天瑞利达科技发展有限公司 Concentrated acid two-stage curing-gas liquid cyclic vanadium extraction process from stone coal
CN102616851B (en) * 2012-04-16 2014-07-30 河北钢铁股份有限公司承德分公司 Resource recycling method for 80 ferrovanadium slag
CN102828025B (en) * 2012-09-20 2014-04-16 长沙矿冶研究院有限责任公司 Method for extracting V2O5 from stone coal navajoite
CN104388679B (en) * 2014-09-30 2016-09-28 边悟 Method containing vanadium raw materials vanadium extraction
CN104789762B (en) * 2015-05-06 2017-08-08 武汉科技大学 A kind of mica-type bone coal extracts V2O5With KAl (SO4)2·12H2O method
CN106521150B (en) * 2015-09-09 2018-07-17 北京有色金属研究总院 A method of v element in roasting extraction vanadium-containing shale
CN108070711B (en) * 2016-11-28 2019-05-21 辽宁科技大学 A kind of metallurgical material and sodium carbonate calcination for activation method
CN110066920B (en) * 2019-05-31 2021-02-05 中国科学院过程工程研究所 Method for selectively leaching and separating vanadium and iron from stone coal vanadium ore
CN113136485A (en) * 2021-04-13 2021-07-20 西安三瑞非常规能源开发有限公司 Method and device for sulfating and low-temperature roasting of vanadium-containing mineral
CN113737025B (en) * 2021-07-23 2022-05-17 中南大学 Vanadium extraction method and vanadium extraction device for high-silicon refractory stone coal vanadium ore

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