CN102154559A - Process for extracting vanadium from vanadium slag containing phosphorus at low temperature - Google Patents

Process for extracting vanadium from vanadium slag containing phosphorus at low temperature Download PDF

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Publication number
CN102154559A
CN102154559A CN2011100999924A CN201110099992A CN102154559A CN 102154559 A CN102154559 A CN 102154559A CN 2011100999924 A CN2011100999924 A CN 2011100999924A CN 201110099992 A CN201110099992 A CN 201110099992A CN 102154559 A CN102154559 A CN 102154559A
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China
Prior art keywords
vanadium
water
temperature
phosphorus
rotary kiln
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CN2011100999924A
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Inventor
胡帝生
胡志强
郑建敏
胡军德
胡冠英
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CHENZHOU JINLONG FERROALLOY Co Ltd
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CHENZHOU JINLONG FERROALLOY Co Ltd
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    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to a process for extracting vanadium from vanadium slag containing phosphorus at low temperature, belonging to the technical field of smelting. The working procedure steps of the process are as follows: the vanadium slag containing phosphorus is ground and sieved, and then mixed with Na2CO3, NaCI and quicklime; the mixed material enters a 30-meter industrial revolving kiln to be roasted, and vanadium and phosphorous in the mixed material are converted into water-soluble clinkers which are discharged, put into cold water and quenched in water so that water-soluble vanadium and phosphorous are dissolved in water; and solids and liquid are separated, phosphorus salts are crystallized to be separated out of the cooled liquid, and a conventional extraction process is used for extracting vanadium. The process can reduce roasting temperature; roasted melting slag does not melt; as a primary conversion rate of the roasting reaches 40 to 45% and a secondary conversion rate reaches more than 50%, the energy consumption is low; and the process solves the difficult problem of agglomeration or ring-forming and can realize industrialization.

Description

The technology of phosphorous vanadium slag low-temperature bake vanadium extraction
Technical field
The present invention relates to a kind of process for extracting vanadium of phosphorous vanadium slag, the technology of particularly a kind of phosphorous vanadium slag low-temperature bake vanadium extraction is saved the energy and is reduced cost, and belongs to technical field of smelting.
Background technology
Phosphorous vanadium slag main component is Fe 2O 320～28%; P 6～9%; V 2O 513～22%; SiO 23～6%; CaO 1～3%; TiO 2＜0.6%; Other are 35～42% years old.This phosphorous vanadium slag, domestic do not have originally, not production precedent yet.
The existing technology of prior art from steel-making vanadium slag roasting vanadium extraction; As state's invention patent publication No. CN 101058853A in 24 days October in 2007, a kind of " industrial slag that utilization contains vanadium, chromium, iron and phosphorus reclaims the method for Chemicals " disclosed by raw material roasting, grog heat lixiviate, ferric oxide and contain vanadium, chromium, phosphorus solution and separate.Its maturing temperature generally is controlled at 800-1050 ℃, will be strict controlled in 80 ℃ to water temperature during lixiviate, and roasting time often needed more than 6 hours, just can reach reasonable recovery transformation efficiency.But for phosphorous high phosphorous vanadium slag, phosphorus is a main component, and phosphorus is again the low melting point mineral, 44 ℃ of phosphorus fusing points, 280 ℃ of boiling points.When causing the actual use of this technology roasting, the fusing of roasting slag, conglomeration or ring formation cause the reinforced and discharging of roasting apparatus to be obstructed easily, produce and are interrupted, therefore this technology not industrialization as yet up to the present.
Summary of the invention
Technical problem to be solved by this invention provides the technology of a kind of phosphorous vanadium slag low-temperature bake vanadium extraction, and this technology can reduce maturing temperature, and roasting roasting slag does not melt, and energy consumption is low; Solve the difficult problem of conglomeration or ring formation, can realize industrialization.
The present invention solves the scheme that its technical problem takes: the technology of a kind of phosphorous vanadium slag low-temperature bake vanadium extraction, and its process is:
1. raw material calcining process
With phosphorous vanadium slag through pulverizing, cross 50～80 mesh sieves; With Na 2CO 3, NaCl and unslaked lime mixes, its mixed weight ratio is 1: 0.01～0.03: 0.01～0.04: 0.05～0.1; Batch mixing enters 30 meters Industrial Rotary Kiln roastings, and control 12m is long in the rotary kiln preheating zone, 350～400 ℃ of temperature, 100 minutes batch mixing residence time; Control 12m is long in the rotary kiln high-temperature zone, 580～650 ℃ of temperature, and 100 minutes batch mixing residence time, control 6m is long in the rotary kiln cooling zone, 450～550 ℃ of temperature, 40 minutes time, wherein vanadium and phosphorus transform into water-soluble grog, come out of the stove;
2. grog lixiviate operation
To join through the grog of roasting in the cold water, and, water miscible vanadium, phosphorus will be dissolved in the water through the shrend chilling; Solid-liquid separation, microcosmic salt is separated out in the crystallisation by cooling separation from liquid, extracts vanadium with conventional extraction process.
Compared with prior art, the invention has the beneficial effects as follows: the unslaked lime that the present invention added is anti-burning and decomposition agent, the vanadium extraction transformation efficiency is significantly increased, more favourable to temperature controlling, more balanced, and solved the fusing of roasting slag and tied the phenomenon of big pelletizing, furnace charge sintering not in the Industrial Rotary Kiln roasting, to move forward smooth and easy; Porosity after vanadium slag burns increases, increases, and more helps the leaching of vanadium.Whole roasting time of the present invention is defined as 240 minutes, shortens 2 hours in 6 hours than prior art roasting, can obtain significantly on saving the energy, enhancing productivity and produce effects.Transformation efficiency of roasting transformation efficiency reaches 40～45%, and the twice transformation rate reaches more than 50%, compared with prior art saves the energy 40%, saves labour cost 15%, raises the efficiency 30%.
Embodiment
Embodiment 1
The technology of a kind of phosphorous vanadium slag low-temperature bake vanadium extraction, its process is:
1. raw material calcining process
With phosphorous vanadium slag through pulverizing, cross the 50-80 mesh sieve; With Na 2CO 3, NaCl and unslaked lime mixes, its mixed weight ratio is 1: 0.01: 0.04: 0.05; Batch mixing enters 30 meters Industrial Rotary Kiln roastings, and control 12m is long in the rotary kiln preheating zone, 360 ℃ of temperature, 100 minutes batch mixing residence time; Control 12m is long in the rotary kiln high-temperature zone, 640 ℃ of temperature, and 100 minutes batch mixing residence time, control 6m is long in the rotary kiln cooling zone, 450 ℃ of temperature, 40 minutes time, wherein vanadium and phosphorus transform into water-soluble grog, come out of the stove;
2. grog lixiviate operation
To join through the grog of roasting in the cold water, and, water miscible vanadium, phosphorus will be dissolved in the water through the shrend chilling;
3. Water Quenching Slag with contain vanadium, phosphorus solution separation circuit
To separate with the aqueous solution that is dissolved with vanadium, phosphorus compound through the grog Water Quenching Slag of shrend lixiviate by natural sedimentation or filtration, solution is as the stock liquid that extracts vanadium and phosphorus;
4. the pre-dephosphorization operation of stock liquid crystallization
To contain the stock liquid cooling of vanadium, phosphorus, the phosphorus that is dissolved in the stock liquid is separated out from stock liquid in tertiary sodium phosphate crystalline mode, gained raw phosphoric acid trisodium, and make phosphorus content reduction in the stock liquid, reach the purpose of pre-dephosphorization;
5. deep phosphorous removal, desiliconization process
To remove in advance and separate after phosphorus solution adds sulfuric acid and calcium sulfate reacts, with isolating phosphorus slag and lysate after the ferrous sulfate detoxifcation, lysate input desiliconization still is isolated white residue, and gained dephosphorization, desiliconization liquid enter and extract the vanadium compound operation;
6. contain the vanadium solution potential of hydrogen and adjust operation
In stock liquid, add sulfuric acid, adjust the potential of hydrogen of solution through dephosphorization, desiliconization;
7. extracting vanadium operation
In extraction reactor, in through the dephosphorization of adjusting potential of hydrogen, desiliconization stock liquid, add extraction agent and sulfuric acid, form phosphorus, sila matter precipitation and rich vanadium clear liquid; (extraction agent is mixed by 1: 8: 1 volume ratio by main extraction agent primary amine and thinner sulfonated kerosene and properties-correcting agent and forms); Precipitation agent is formed with calcium chloride or magnesium chloride.
8. filter operation
(add reverse-extraction agent in rich vanadium organism, form the rich vanadium aqueous solution and extraction agent, (extraction agent recycles; Strippant is by 0.5mol/L Na 2SO 4And 1.5mol/L NaOH mixed solution is formed); Change into by filtering, must contain the vanadium clear liquid and be used for precipitating, the poor vanadium slag of filter residue separation fusion roasting again soaks vanadium, gets vanadium liquid.
9. vanadium precipitates operation
In rich vanadium solution, add ammonium sulfate, make the reaction of vanadium and ammonium sulfate generate ammonium meta-vanadate and precipitation supernatant liquor;
10. ammonium meta-vanadate calcining process
The ammonium meta-vanadate that precipitates and isolates is carried out roasting, ammonium is overflowed with the form of ammonia send into ammonia absorber, obtain the Vanadium Pentoxide in FLAKES product simultaneously.
Embodiment 2
The technology of a kind of phosphorous vanadium slag low-temperature bake vanadium extraction, its process is:
1. raw material calcining process
Phosphorous vanadium slag is removed mesh sieve through pulverizing, cross 60; With Na 2CO 3, NaCl and unslaked lime mixes, its mixed weight ratio is 1: 0.03: 0.01: 0.1; Batch mixing enters 30 meters Industrial Rotary Kiln roastings, and control 12m is long in the rotary kiln preheating zone, 400 ℃ of temperature, 100 minutes batch mixing residence time; Control 12m is long in the rotary kiln high-temperature zone, 600 ℃ of temperature, and 100 minutes batch mixing residence time, control 6m is long in the rotary kiln cooling zone, 500 ℃ of temperature, 40 minutes time, wherein vanadium and phosphorus transform into water-soluble grog, come out of the stove;
2. grog lixiviate operation
To join through the grog of roasting in the cold water, and, water miscible vanadium, phosphorus will be dissolved in the water through the shrend chilling; The crystallisation by cooling separation is separated out microcosmic salt and is extracted the operation of vanadium with embodiment 1 with conventional extraction process from liquid.
Embodiment 3
The technology of a kind of phosphorous vanadium slag low-temperature bake vanadium extraction, its process is:
1. raw material calcining process
With phosphorous vanadium slag through pulverizing, cross 70 mesh sieves; With Na 2CO 3, NaCl and unslaked lime mixes, its mixed weight ratio is 1: 0.02: 0.01: 0.08; Batch mixing enters 30 meters Industrial Rotary Kiln roastings, and control 12m is long in the rotary kiln preheating zone, 380 ℃ of temperature, 100 minutes batch mixing residence time; Control 12m is long in the rotary kiln high-temperature zone, 580 ℃ of temperature, and 100 minutes batch mixing residence time, control 6m is long in the rotary kiln cooling zone, 550 ℃ of temperature, 40 minutes time, wherein vanadium and phosphorus transform into water-soluble grog, come out of the stove;
2. grog lixiviate operation
To join through the grog of roasting in the cold water, and, water miscible vanadium, phosphorus will be dissolved in the water through the shrend chilling; The crystallisation by cooling separation is separated out microcosmic salt and is extracted the operation of vanadium with embodiment 1 with conventional extraction process from liquid.
Embodiment 4
The technology of a kind of phosphorous vanadium slag low-temperature bake vanadium extraction, its process is:
1. raw material calcining process
With phosphorous vanadium slag through pulverizing, cross 80 mesh sieves; With Na 2CO 3, NaCl and unslaked lime mixes, its mixed weight ratio is 1: 0.03: 0.02: 0.06; Batch mixing enters 30 meters Industrial Rotary Kiln roastings, and control 12m is long in the rotary kiln preheating zone, 350 ℃ of temperature, 100 minutes batch mixing residence time; Control 12m is long in the rotary kiln high-temperature zone, 650 ℃ of temperature, and 100 minutes batch mixing residence time, control 6m is long in the rotary kiln cooling zone, 500 ℃ of temperature, 40 minutes time, wherein vanadium and phosphorus transform into water-soluble grog, come out of the stove;
2. grog lixiviate operation
To join through the grog of roasting in the cold water, and, water miscible vanadium, phosphorus will be dissolved in the water through the shrend chilling; The crystallisation by cooling separation is separated out microcosmic salt and is extracted the operation of vanadium with embodiment 1 with conventional extraction process from liquid.

Claims (1)

1. the technology of phosphorous vanadium slag low-temperature bake vanadium extraction is characterized in that process is:
1. raw material calcining process
With phosphorous vanadium slag through pulverizing, cross 50～80 mesh sieves; With Na 2CO 3, NaCl and unslaked lime mixes, its mixed weight ratio is 1: 0.01～0.03: 0.01～0.04: 0.05～0.1; Batch mixing enters 30 meters Industrial Rotary Kiln roastings, and control 12m is long in the rotary kiln preheating zone, 350～400 ℃ of temperature, 100 minutes batch mixing residence time; Control 12m is long in the rotary kiln high-temperature zone, 580～650 ℃ of temperature, and 100 minutes batch mixing residence time, control 6m is long in the rotary kiln cooling zone, 450～550 ℃ of temperature, 40 minutes time, wherein vanadium and phosphorus transform into water-soluble grog, come out of the stove;
2. grog lixiviate operation
To join through the grog of roasting in the cold water, and, water miscible vanadium, phosphorus will be dissolved in the water through the shrend chilling; Solid-liquid separation, microcosmic salt is separated out in the crystallisation by cooling separation from liquid, extracts vanadium with conventional extraction process.
CN2011100999924A 2011-04-12 2011-04-12 Process for extracting vanadium from vanadium slag containing phosphorus at low temperature Pending CN102154559A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102851507A (en) * 2012-08-21 2013-01-02 攀钢集团研究院有限公司 Vanadium slag sodium modification roasting method
CN103103357A (en) * 2012-11-23 2013-05-15 陈泉兴 Method for drying, calcining and cooling metal slag material
CN103710552A (en) * 2013-12-26 2014-04-09 中信锦州金属股份有限公司 Leaching technique and system for preparing vanadium solution by quenching vanadium slag roasting clinker
CN111153613A (en) * 2020-01-16 2020-05-15 衢州华友钴新材料有限公司 Method for preparing clinker by using cobalt hydrometallurgy waste residue to fix sulfur and roasting at high temperature
CN111218571A (en) * 2020-01-13 2020-06-02 攀钢集团攀枝花钢铁研究院有限公司 Method for pre-desiliconizing phosphorus by roasting vanadium slag soda lime
CN111647758A (en) * 2020-06-12 2020-09-11 攀钢集团研究院有限公司 Method for pretreating and dephosphorizing high-phosphorus vanadium slag

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86108218A (en) * 1986-12-01 1987-08-12 冶金工业部攀枝花钢铁研究院 Rotary kiln bakes to burn the article vanadium slag-water logging extraction vanadium method
CN101161831A (en) * 2007-11-09 2008-04-16 攀钢集团攀枝花钢铁研究院 Method for calcifying and roasting vanadium slag
CN101684525A (en) * 2009-08-12 2010-03-31 虹京环保有限公司 Method for extracting vanadium from vanadium-containing ferrophosphor
CN101914673A (en) * 2010-07-30 2010-12-15 四川省川威集团有限公司 Sodium-translated roasting method of vanadium minerals

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN86108218A (en) * 1986-12-01 1987-08-12 冶金工业部攀枝花钢铁研究院 Rotary kiln bakes to burn the article vanadium slag-water logging extraction vanadium method
CN101161831A (en) * 2007-11-09 2008-04-16 攀钢集团攀枝花钢铁研究院 Method for calcifying and roasting vanadium slag
CN101684525A (en) * 2009-08-12 2010-03-31 虹京环保有限公司 Method for extracting vanadium from vanadium-containing ferrophosphor
CN101914673A (en) * 2010-07-30 2010-12-15 四川省川威集团有限公司 Sodium-translated roasting method of vanadium minerals

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102851507A (en) * 2012-08-21 2013-01-02 攀钢集团研究院有限公司 Vanadium slag sodium modification roasting method
CN102851507B (en) * 2012-08-21 2014-02-19 攀钢集团研究院有限公司 Vanadium slag sodium modification roasting method
CN103103357A (en) * 2012-11-23 2013-05-15 陈泉兴 Method for drying, calcining and cooling metal slag material
CN103103357B (en) * 2012-11-23 2014-04-09 陈泉兴 Method for drying, calcining and cooling metal slag material
CN103710552A (en) * 2013-12-26 2014-04-09 中信锦州金属股份有限公司 Leaching technique and system for preparing vanadium solution by quenching vanadium slag roasting clinker
CN103710552B (en) * 2013-12-26 2014-11-26 中信锦州金属股份有限公司 Leaching technique and system for preparing vanadium solution by quenching vanadium slag roasting clinker
CN111218571A (en) * 2020-01-13 2020-06-02 攀钢集团攀枝花钢铁研究院有限公司 Method for pre-desiliconizing phosphorus by roasting vanadium slag soda lime
CN111218571B (en) * 2020-01-13 2021-05-11 攀钢集团攀枝花钢铁研究院有限公司 Method for pre-desiliconizing phosphorus by roasting vanadium slag soda lime
CN111153613A (en) * 2020-01-16 2020-05-15 衢州华友钴新材料有限公司 Method for preparing clinker by using cobalt hydrometallurgy waste residue to fix sulfur and roasting at high temperature
CN111153613B (en) * 2020-01-16 2022-05-20 衢州华友钴新材料有限公司 Method for preparing clinker by using cobalt hydrometallurgical waste residue for sulfur fixation and high-temperature roasting
CN111647758A (en) * 2020-06-12 2020-09-11 攀钢集团研究院有限公司 Method for pretreating and dephosphorizing high-phosphorus vanadium slag

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Application publication date: 20110817