CN108359806A - A kind of integrated conduct method of slag, vanadium slag, titanium white waste acid - Google Patents

A kind of integrated conduct method of slag, vanadium slag, titanium white waste acid Download PDF

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Publication number
CN108359806A
CN108359806A CN201810310898.0A CN201810310898A CN108359806A CN 108359806 A CN108359806 A CN 108359806A CN 201810310898 A CN201810310898 A CN 201810310898A CN 108359806 A CN108359806 A CN 108359806A
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slag
vanadium
titanium white
white waste
waste acid
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高俊
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Panzhihua Redwood Vanadium Products Co Ltd
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Panzhihua Redwood Vanadium Products Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/20—Obtaining niobium, tantalum or vanadium
    • C22B34/22—Obtaining vanadium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/006—Wet processes
    • C22B7/007—Wet processes by acid leaching
    • 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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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a kind of slag, vanadium slag, titanium white waste acid integrated conduct methods, include the following steps：A. it is first 20 ~ 130 in mass ratio by slag and vanadium slag：100 mixing, then in every kg slags be added 1L titanium white waste acids ratio continuously add titanium white waste acid, lump, after caking materials are crushed；B. it will be roasted through the material of step a, calcination temperature is 850 ~ 880 DEG C, and roasting time is 60 ~ 120 minutes；C. the material that grain size is 120 mesh is made in the material through step b；D. will be that 1/3.2 ~ 1/8.7 addition water mixes in mass ratio in the material through step c, the rear pH that adjusts is 1.2 ~ 1.8；E. it will be separated by solid-liquid separation through the material of step d, then liquid be subjected to resins exchange absorption, the rear resin that carries out is freed；F. magnesium sulfate removal of impurities will be added through the material of step e；G. the material pH value through step e is adjusted to 7.0 ~ 8.5, ammonium sulfate is added afterwards；The method of the present invention comprehensively utilizes slag, vanadium slag, titanium white waste acid, creates enormous benefits.

Description

A kind of integrated conduct method of slag, vanadium slag, titanium white waste acid
Technical field
The present invention relates to the integrated conduct method fields of waste material, are integrated more particularly to a kind of slag, vanadium slag, titanium white waste acid Processing method.
Background technology
Slag is one of three wastes of steel and iron industry, and the utilization rate of China's slag is extremely low, and gap is larger compared with developed countries, Slag can be used as the construction materials such as metallurgical raw material, cement, roadbed material and fertilizer by processing.Vanadium is a kind of important metal member Element is widely used, and great economic value, and market price is about 350,000/ton, vanadium except for making steel in addition to, vanadium be additionally operable to sulfuric acid industry with The catalyst of petrochemical industry, aircraft engine, aerospace cabin skeleton, the hydrofoil on naval vessel and introduce device, steam turbine plant blade and In the V-Ti and lithium vanadium high-capacity battery of rocket motor casing etc., vanadium is used as diabetes in medicine and improves the heart The drug of vascular function, or even in ceramic industry, solar industry, vanadium also has been widely used.In some steel production enterprises In, it is such as blown in the enterprise of vanadium using vanadium titano-magnetite, produces and largely contain slag, produced every year specifically, such as climbing two base of steel It is raw to contain about 300,000 tons of slag, it is mainly used for highway construction, manufacture of cement addition etc.；Desheng steel generates slag about 1.5 ten thousand every year Ton wherein pentoxide content is up to 4%.Vanadium is a kind of non-renewable resources, if directly processing contains slag, will be caused very big Waste.
Titanium white waste acid mostlys come from the enterprise of production titanium dioxide, produces titanium dioxide per ton and generates about 5 side's titanium white waste acids, and Acid content is up to 200g/L or more.In some enterprises, such as the east titanium industry of Panxi Diqu, Heng Tong titanium industry, titanium white waste acid is handled, Using the method for directly using lime neutralisation treatment, processing titanium white waste acid as wastewater treatment, the method processing cost is per side About 500 yuan, and the waste acid concentration that domestic few Some Enterprises use reuses technology, cost recovery is up to about per square sulfuric acid 1000 yuan, titanium white waste acid is hazardous waste, and recycling is not only of high cost, but also removal process is dangerous, is brought to enterprise and environment White elephant, country also extremely payes attention to the processing of titanium white waste acid.
Vanadium slag, refer to vanadium-bearing hot metal in vanadium extracting process it is oxidized blow obtain or concentrate containing vanadium iron through wet method vanadium extraction The obtained bits containing vanadium oxide, it is the raw material for smelting and producing vanadium alloy and vanadium metal.Vanadium slag is as domestic at present main The vanadium raw materials for production wanted, mainly based on sodium roasting vanadium-extracting technique and calcification baking process for extracting vanadium.Sodium roasting at present by Country forbids setting up the project, and belongs to backward and environment protection treating difficulty production technology.And calcification baking technique, such as current Xichang steel vanadium make But it is low to there is the rate of recovery in calcification baking technique（It abandons and contains vanadic anhydride 2% or so in slag）, roasting process slag easily lumps shadow The problem of ringing production efficiency, while needing that large quantities of lime stone is added in roasting, tedious process needs to expend a large amount of materials and manpower.
The present invention has studied the integrated conduct method of a kind of slag, vanadium slag, titanium white waste acid.
Invention content
Slag, vanadium slag, titanium white waste acid are the wastes generated in industrial production, are unfavorable for ecological environment, and processing cost is high, The accidental discovery of inventor, it can be achieved that waste utilization, will be conducive to ecological environment after slag, vanadium slag, titanium white waste acid integrated treatment Meanwhile, it is capable to generate huge economic benefit.Specifically, a kind of slag, vanadium slag, titanium white waste acid integrated conduct method, including with Lower step：
A. it is first 20 ~ 130 in mass ratio by slag and vanadium slag：100 mixing, then the ratio in 1kg slags addition 1L titanium white waste acids Continuously add titanium white waste acid, lump, after caking materials are crushed, it is preferred that material particular diameter is 0 ~ 10cm after broken；
B. it will be roasted through the material of step a, calcination temperature is 850 ~ 880 DEG C, and roasting time is 60 ~ 120 minutes, preferably 90 points Clock；
C. the material that grain size is 120 mesh is made in the material through step b；
D. will be that 1/3.2 ~ 8.7 addition water mixes in mass ratio in the material through step c, preferably 1/4 ~ 1/8, adjusting pH afterwards is 1.2 ~ 1.8, preferably 1.5；
E. it will be separated by solid-liquid separation through the material of step d, then liquid be subjected to resins exchange absorption, the rear resin that carries out is freed；
F. magnesium sulfate removal of impurities will be added through the material of step e, the mass ratio that magnesium sulfate and vanadic anhydride is added is 1/5 ~ 1/ 15, preferably 1:10, the removal of impurities reaction time is 30 ~ 60 minutes；
G. the material pH value through step e is adjusted to 7.0 ~ 8.5, preferably 8.0, ammonium sulfate is added afterwards.
Further, sulphur acid for adjusting pH is used in the step d.
Further, in the resins exchange, resin adsorption saturation capacity is the 25 ~ 30% of aqueous resins weight, adsorbs rear molding A concentration of 0 ~ 0.5g/L of vanadic anhydride in water；
Further, the slag grain size is 120 ~ 200 mesh, and preferably 160 mesh, the vanadium slag grain size is 100 ~ 180 mesh, preferably For 120 mesh.
The phase structure that slag can be changed when slag grain size is 120 ~ 200 mesh, the meeting when vanadium slag grain size is 100 ~ 180 mesh The phase structure for changing slag is conducive to the validity of reaction, is especially 160 mesh in slag grain size, vanadium slag grain size is 160 mesh When, reaction is most abundant.
Further, resin described in step e is freed, and is freed using 80wt% piece aqueous slkalis.
Further, ammonium sulfate addition is with vanadic anhydride mass ratio in required material in the ammonium sulfate step g 1.2 ~ 3.0, preferably 1.7.
Further, resins exchange is anion exchange resin in the step e.
Further, 150 ~ 300g/L of the titanium white waste acid sulfur acid, it is preferred that sulfur acid 200g/L.
Further, the vanadium slag composition includes V2O50 ~ 99wt%, preferably V2O50 ~ 25wt%, further preferably V2O515.2wt%。
Further, the slag contains vanadium, it is preferred that its composition includes：V2O50.3 ~ 4.5wt%, CaO30 ~ 60wt%, Fe2O325~45wt%。
Beneficial effects of the present invention are as follows,
（One）Comprehensive utilization of resources.
1, slag is used currently used for construction material, and the slag containing vanadium is also used as construction material, causes vanadium resource Significant wastage.And the vanadium in slag can be successfully recycled by the technology of the application, vanadium recovery reaches 70%, contains in waste Vanadium can be controlled in 0.5wt% to be generated using sodium vanadium extraction and calcification vanadium extraction production vanadium slag at present hereinafter, being substantially less than containing vanadium in waste Content 1.7wt% of waste or so.
2, titanium white waste acid is at present all as wastewater treatment, wherein also the sulfuric acid containing about 200g/L is not only not used, instead It needs to be handled by means such as neutralizations.
（Two）Recovery process is short, high income.
1. existing sodium roasting technology needs after baking, vanadium recovery highest also to can only achieve 88%, side of the present invention Method only needs once to roast, and vanadium recovery can reach 91.5% or more.
2. producing vanadium using vanadium slag using calcification baking vanadium extraction technology at present, vanadium recovery can only achieve 84%.
（Three）It is low to roast cost of supplementary product.
1. existing sodium roasting vanadium-extracting technique roasting auxiliary material needs sodium carbonate, sodium chloride.
2. calcification baking process for extracting vanadium needs that lime stone or quick lime is added.
3. the method for the present invention need to only be mixed into titanium white waste acid.
（Four）The technology is more environmentally friendly compared to original domestic main vanadium extraction technology.
Exhaust gas controls.In existing sodium roasting vanadium-extracting technique, especially adding sodium chloride can be in baking tail gases Appearance is difficult to handle toxic and harmful gas, hydrogen chloride, chlorine, and present techniques only need to handle sulfur dioxide gas after baking Body, and SO 2 tail gas processing is highly developed at present, operation is simple and at low cost.
（Five）The technology compares the white spent acid production technology yield higher of slag mixed with titanium.
It is although at low cost that slag directly mixes titanium white waste acid production technology, but there are problems that low output, such as same separate unit The rotary kiln production scale of 2.5 meters of diameter：
Slag mixes titanium white waste acid monthly output=38.5 ton
Slag mixing titanium white waste acid mixes vanadium slag monthly output=224.82 ton
（Six）Production cost is low.
Main domestic vanadium slag produces and processes cost at present：
1, vanadium slag processes vanadic anhydride per ton using sodium roasting technology：About 17200 yuan
2, Pan Gangpanhong companies tailings processes vanadic anhydride processing cost per ton：About 55000 yuan.
3, slag mixing vanadium slag titanium white waste acid processes vanadic anhydride cost per ton：Less than 5000 yuan.
（Seven）The technology compares calcification baking technology, has advantage prevented from caking in the process of roasting.
Specific implementation mode
Embodiment 1
A kind of slag, vanadium slag, titanium white waste acid integrated conduct method include following operating procedure successively：
1, by vanadium slag（Containing V2O5For 15.2wt%）It is levigate to be more than 90% to 120 mesh excessively, contain slag（Containing V2O5Contain CaO for 2.3wt% For 37.27wt% Fe2O3For 34wt%）It is levigate to cross 160 mesh be more than 80%；
2, it is that 1/1 ratio mixes in mass ratio by the vanadium slag powder through step " 1 " and containing steel-making slag powder；
3, titanium white waste acid（Containing H2SO4For 208g/L）The ratio mixing of 1L titanium white waste acids, material mixing are mixed into every KG steel-making slag powders Afterwards, it places 1 hour, waits for material caking molding, then be broken for fritter；
4, material is subjected to gradually heating roasting, rises to 860 DEG C, is roasted 90 minutes at 860 DEG C.Measure the mixed material after roasting Middle V2O5Content is 7.95%；
5, by the material after roasting it is levigate to 120 mesh be more than 90%；
6, it presses solid-liquid mass ratio 1/5 and water stirring, 400 revs/min of speed of agitator is added, until being uniformly mixed；
7, it is gradually added industrial sulphuric acid（98%）Adjustment slurry PH stabilizes to 1.8, mixing time 60 minutes；
8, after slurry filters separation of solid and liquid, slag contains V after leaching2O5It is 0.89%, leachate contains V2O5A concentration of 15.6g/L.It calculates It is 88.8% to leach the rate of recovery；
9, leachate swaps absorption using HD317 type resins, tail water V after absorption2O5A concentration of 0.21g/L；
10, resin adsorption V is pressed2O580% technical grade piece alkali number configuration slice aqueous slkali of quality carries out resin and frees, and obtains containing V2O5 A concentration of 96g/L deposition vanadium mother liquids；
11, according to V in deposition vanadium mother liquid2O5MgSO is added in the 10% of gross mass4, stir 30 minutes, dephosphorization carried out to mother liquor of precipitation of ammonium；
12, it is 8 industrial sulphuric acid adjustment PH to be added according to the deposition vanadium mother liquid after dephosphorization, the V in by mother liquor2O51.7 times of gross mass Ammonium sulfate is added, stirring precipitation, is settled out ammonium metavanadate at 120 minutes sedimentation times, and the solution after precipitation contains V2O5For 0.35g/ L, precipitate recovery rate 99.64%；
13, product ammonium metavanadate is prepared into vanadic anhydride, in terms of vanadic anhydride, it is 88.48% to calculate vanadium overall recovery；
14, the mixture in step " 4 " after roasting is 150 ton hours, can produce 10.55 tons of vanadic anhydride, being converted to vanadium is 5.91 ton.
Embodiment 2
A kind of slag, vanadium slag, titanium white waste acid integrated conduct method include following operating procedure successively：
1, by vanadium slag（Containing V2O5For 15.2wt%）It is levigate to be more than 90% to 120 mesh excessively, contain slag（Containing V2O5Contain CaO for 2.3wt% For 37.27wt% Fe2O3For 34wt%）It is levigate to cross 160 mesh be more than 80%；
2, it is mixed in 1/1 ratio by vanadium slag powder and containing steel-making slag powder；
3, titanium white waste acid（H2SO4For 208g/L）The ratio mixing of 1L titanium white waste acids is mixed into every KG steel-making slag powders, after material mixing, It places 1 hour, material caking molding, then is broken for fritter；
4, material is subjected to gradually heating roasting, rises to 860 DEG C, is roasted 90 minutes at 860 DEG C, the mixed material after roasting contains V2O5Content is 7.95%；
5, by the material after roasting it is levigate to 120 mesh be more than 90%；
6, it presses solid-liquid mass ratio 1/5 and water stirring, 400 revs/min of speed of agitator is added；
7, it is gradually added industrial sulphuric acid（98%）Adjustment slurry PH stabilizes to 1.5, mixing time 60 minutes；
8, after slurry filters separation of solid and liquid, slag contains V after leaching2O5It is 0.64%, leachate contains V2O5A concentration of 16.2g/L is leached The rate of recovery is 91.9%；
9, leachate swaps absorption using HD317 type resins, tail water V after absorption2O5A concentration of 0.20g/L；
10, resin adsorption V is pressed2O580% technical grade piece alkali number configuration slice aqueous slkali of quality carries out resin and frees, and obtains containing V2O5 A concentration of 93g/L deposition vanadium mother liquids；
11, according to V in deposition vanadium mother liquid2O5MgSO is added in the 10% of gross mass4, stir 30 minutes, dephosphorization carried out to mother liquor of precipitation of ammonium；
12, it is 8 industrial sulphuric acid adjustment PH to be added according to the deposition vanadium mother liquid after dephosphorization, the V in by mother liquor2O51.7 times of gross mass Ammonium sulfate is added, stirring precipitation, is settled out ammonium metavanadate at 120 minutes sedimentation times, and precipitation upper liquid contains V2O5For 0.38g/L, Precipitate recovery rate is 99.59%；
13, product ammonium metavanadate is prepared into vanadic anhydride, in terms of vanadic anhydride, it is 91.52% to calculate vanadium overall recovery；
14, it presses single rotary kiln to calculate, 10.91 tons of vanadic anhydride of conversion is then produced in 150 tons of day blanking daily.
Embodiment 3
A kind of slag, vanadium slag, titanium white waste acid integrated conduct method include following operating procedure successively：
1, by vanadium slag（It is 15.2wt% containing V2O5）It is levigate to be more than 90% to 120 mesh excessively, contain slag（Containing V2O5Contain CaO for 2.3wt% For 37.27wt% Fe2O3For 34wt%）It is levigate to cross 160 mesh be more than 80%；
2, it is mixed in 1/1 ratio by vanadium slag powder and containing steel-making slag powder；
3, titanium white waste acid（H2SO4For 208g/L）The ratio mixing of 1L titanium white waste acids is mixed into every KG steel-making slag powders, after material mixing, It places 1 hour, material caking molding, then is broken for fritter；
4, material is subjected to gradually heating roasting, rises to 860 DEG C, is roasted 90 minutes at 860 DEG C, in the mixed material after roasting V2O5Content is 7.95%；
5, by the material after roasting it is levigate to 120 mesh be more than 90%；
6, it presses solid-liquid mass ratio 1/5 and water stirring, 400 revs/min of speed of agitator is added；
7, it is gradually added industrial sulphuric acid（98%）Adjustment slurry PH stabilizes to 1.2, mixing time 60 minutes；
8, after slurry filters separation of solid and liquid, slag contains V after leaching2O5It is 0.66%, leachate contains V2O5A concentration of 16.1g/L is leached The rate of recovery is 91.7%；
9, leachate swaps absorption using HD317 type resins, tail water V after absorption2O5A concentration of 0.20g/L；
10, resin adsorption V is pressed2O580% technical grade piece alkali number configuration slice aqueous slkali of quality carries out resin and frees, and obtains containing V2O5 A concentration of 95g/L deposition vanadium mother liquids；
11, according to V in deposition vanadium mother liquid2O5MgSO is added in the 10% of gross mass4, stir 30 minutes, dephosphorization carried out to mother liquor of precipitation of ammonium；
12, it is 8 industrial sulphuric acid adjustment PH to be added according to the deposition vanadium mother liquid after dephosphorization, the V in by mother liquor2O51.7 times of gross mass Ammonium sulfate is added, stirring precipitation, is settled out ammonium metavanadate at 120 minutes sedimentation times, and precipitation upper liquid contains V2O5For 0.4g/L, sink The shallow lake rate of recovery is 99.57%；
13, product ammonium metavanadate is prepared into vanadic anhydride, in terms of vanadic anhydride, it is 91.3% to calculate vanadium overall recovery；
14, it presses single rotary kiln to calculate, 10.89 tons of vanadic anhydride of conversion is then produced in 150 tons of day blanking daily.
Embodiment 4
A kind of slag, vanadium slag, titanium white waste acid integrated conduct method include following operating procedure successively：
1, by vanadium slag（Containing V2O515.2wt%）It is levigate to be more than 90% to 120 mesh excessively, contain slag（Containing V2O5It is containing CaO for 2.3wt% 37.27wt% Fe2O3For 34wt%）It is levigate to cross 160 mesh be more than 80%；
2, it is mixed in 50/100 ratio by vanadium slag powder and containing steel-making slag powder；
3, titanium white waste acid（H2SO4For 208g/L）The ratio mixing of 1L titanium white waste acids is mixed into every KG steel-making slag powders, after material mixing, It places 1 hour, material caking molding, then is broken for fritter；
4, material is subjected to gradually heating roasting, rises to 860 DEG C, is roasted 90 minutes at 860 DEG C, the mixed material after roasting contains V2O5Content is 4.95%；
5, by the material after roasting it is levigate to 120 mesh be more than 90%；
6, it presses solid-liquid mass ratio 1/5 and water stirring, 400 revs/min of speed of agitator is added；
7, it is gradually added industrial sulphuric acid（98%）Adjustment slurry PH stabilizes to 1.5, mixing time 60 minutes；
8, after slurry filters separation of solid and liquid, slag contains V after leaching2O5It is 0.6%, liquid contains V2O5A concentration of 9.59g/L.Leach recycling Rate is 87.88%；
9, leachate swaps absorption using HD317 type resins, tail water V after absorption2O5A concentration of 0.20g/L；
10, resin adsorption V is pressed2O580% technical grade piece alkali number configuration slice aqueous slkali of quality carries out resin and frees, and obtains containing V2O5 A concentration of 95g/L deposition vanadium mother liquids；
11, according to V in deposition vanadium mother liquid2O5MgSO is added in the 10% of gross mass4, stir 30 minutes, dephosphorization carried out to mother liquor of precipitation of ammonium；
12, it is 8 industrial sulphuric acid adjustment PH to be added according to the deposition vanadium mother liquid after dephosphorization, the V in by mother liquor2O51.7 times of gross mass Ammonium sulfate is added, stirring precipitation, is settled out ammonium metavanadate at 120 minutes sedimentation times, and the solution after precipitation contains V2O5For 0.4g/L, Precipitate recovery rate is 99.57%；
13, product ammonium metavanadate is prepared into vanadic anhydride, in terms of vanadic anhydride, it is 87.5% to calculate vanadium overall recovery；
14, it presses single rotary kiln to calculate, 6.5 tons of vanadic anhydride of conversion is then produced in 150 tons of day blanking daily.
Embodiment 5
A kind of slag, vanadium slag, titanium white waste acid integrated conduct method include following operating procedure successively：
1, by vanadium slag（Containing V2O5For 15.2wt%）It is levigate to be more than 90% to 120 mesh excessively, contain slag（Containing V2O5Contain CaO for 2.3 wt% For 37.27 wt% Fe2O3For 34 wt%）It is levigate to cross 160 mesh be more than 80%；
2, it is mixed in 20/100 ratio by vanadium slag powder and containing steel-making slag powder；
3, titanium white waste acid（H2SO4For 208g/L）The ratio mixing of 1L titanium white waste acids is mixed into every KG steel-making slag powders, after material mixing, It places 1 hour, material caking molding, then is broken for fritter；
4, material is subjected to gradually heating roasting, rises to 860 DEG C, is roasted 90 minutes at 860 DEG C, the mixed material after roasting contains V2O5Content is 3.55%；
5, by the material after roasting it is levigate to 120 mesh be more than 90%；
6, it presses solid-liquid mass ratio 1/5 and water stirring, 400 revs/min of speed of agitator is added；
7, it is gradually added industrial sulphuric acid（98%）Adjustment slurry PH stabilizes to 1.5, mixing time 60 minutes；
8, after slurry filters separation of solid and liquid, slag contains V after leaching2O5It is 0.54%, liquid contains V2O5A concentration of 6.64g/L, is leached back Yield is 84.48%；
9, leachate swaps absorption using HD317 type resins, tail water V after absorption2O5A concentration of 0.20g/L；
10, resin adsorption V is pressed2O580% technical grade piece alkali number configuration slice aqueous slkali of quality carries out resin and frees, and obtains containing V2O5 A concentration of 95g/L deposition vanadium mother liquids；
11, according to V in deposition vanadium mother liquid2O5MgSO is added in the 10% of gross mass4, stir 30 minutes, dephosphorization carried out to mother liquor of precipitation of ammonium；
12, it is 8 industrial sulphuric acid adjustment PH to be added according to the deposition vanadium mother liquid after dephosphorization, the V in by mother liquor2O51.7 times of gross mass Ammonium sulfate, stirring precipitation is added, 120 minutes sedimentation times were settled out ammonium metavanadate, and solution contains V after precipitation2O5For 0.4g/L, sink The shallow lake rate of recovery is 99.57%；
13, product ammonium metavanadate is prepared into vanadic anhydride, in terms of vanadic anhydride, it is 84.11% to calculate vanadium overall recovery；
14, it presses single rotary kiln to calculate, 4.49 tons of vanadic anhydride of conversion is then produced in 150 tons of day blanking daily.
Embodiment 6
A kind of slag, vanadium slag, titanium white waste acid integrated conduct method include following operating procedure successively：
1, by vanadium slag（Containing V2O5For 15.2wt%）It is levigate to be more than 90% to 120 mesh excessively, contain slag（Containing V2O5Contain CaO for 2.3wt% For 37.27wt% Fe2O3For 34 wt%）It is levigate to cross 160 mesh be more than 80%；
2, it is mixed in 120/100 ratio by vanadium slag powder and containing steel-making slag powder；
3, titanium white waste acid（H2SO4For 208g/L）The ratio mixing of 1L titanium white waste acids is mixed into every KG steel-making slag powders, after material mixing, It places 1 hour, material caking molding, then is broken for fritter；
4, material is subjected to gradually heating roasting, rises to 860 DEG C, is roasted 90 minutes at 860 DEG C, the mixed material after roasting contains V2O5Content is 8.22%；
5, by the material after roasting it is levigate to 120 mesh be more than 90%；
6, it presses solid-liquid mass ratio 1/5 and water stirring, 400 revs/min of speed of agitator is added；
7, it is gradually added industrial sulphuric acid（98%）Adjustment slurry PH stabilizes to 1.5, mixing time 60 minutes；
8, after slurry filters separation of solid and liquid, slag contains V after leaching2O5It is 1.2%, liquid contains V2O5A concentration of 15.48g/L, is leached back Yield is 85.4%；
9, leachate swaps absorption using HD317 type resins, tail water V after absorption2O5A concentration of 0.20g/L；
10, resin adsorption V is pressed2O580% technical grade piece alkali number configuration slice aqueous slkali of quality carries out resin and frees, and obtains containing V2O5 A concentration of 95g/L deposition vanadium mother liquids；
11, according to V in deposition vanadium mother liquid2O5MgSO is added in the 10% of gross mass4, stir 30 minutes, dephosphorization carried out to mother liquor of precipitation of ammonium；
12, it is 8 industrial sulphuric acid adjustment PH to be added according to the deposition vanadium mother liquid after dephosphorization, the V in by mother liquor2O51.7 times of gross mass Ammonium sulfate, stirring precipitation is added, 120 minutes sedimentation times were settled out ammonium metavanadate, and solution contains V after precipitation2O5For 0.4g/L.It is heavy The shallow lake rate of recovery is 99.57%；
13, product ammonium metavanadate is prepared into vanadic anhydride, in terms of vanadic anhydride, it is 85.02% to calculate vanadium overall recovery；
14, it presses single rotary kiln to calculate, 10.48 tons of vanadic anhydride of conversion is then produced in 150 tons of day blanking daily.
Embodiment 7
A kind of slag, vanadium slag, titanium white waste acid integrated conduct method include following operating procedure successively：
1, by vanadium slag（Containing V2O5For 15.2wt%）It is levigate to be more than 90% to 120 mesh excessively, contain slag（Containing V2O5Contain CaO for 2.3 wt% For 37.27 wt% Fe2O3For 34 wt%）It is levigate to cross 160 mesh be more than 80%；
2, it is mixed in 130/100 ratio by vanadium slag powder and containing steel-making slag powder；
3, titanium white waste acid（H2SO4For 208g/L）The ratio mixing of 1L titanium white waste acids is mixed into every KG steel-making slag powders.After material mixing, It places 1 hour, material caking molding, then is broken for fritter；
4, material is subjected to gradually heating roasting, rises to 860 DEG C, is roasted 90 minutes at 860 DEG C.Mixed material after roasting contains V2O5Content is 8.48%；
5, by the material after roasting it is levigate to 120 mesh be more than 90%；
6, it presses solid-liquid mass ratio 1/5 and water stirring, 400 revs/min of speed of agitator is added；
7, it is gradually added industrial sulphuric acid（98%）Adjustment slurry PH stabilizes to 1.5, mixing time 60 minutes；
8, after slurry filters separation of solid and liquid, slag contains V after leaching2O5It is 2.0%, liquid contains V2O5A concentration of 16.1g/L leaches recycling Rate is 76.42%；
9, leachate swaps absorption using HD317 type resins, tail water V after absorption2O5A concentration of 0.20g/L；
10, resin adsorption V is pressed2O580% technical grade piece alkali number configuration slice aqueous slkali of quality carries out resin and frees, and obtains containing V2O5 A concentration of 95g/L deposition vanadium mother liquids；
11, according to V in deposition vanadium mother liquid2O5MgSO is added in the 10% of gross mass4, stir 30 minutes, dephosphorization carried out to mother liquor of precipitation of ammonium；
12, it is 7.0 industrial sulphuric acid adjustment PH to be added according to the deposition vanadium mother liquid after dephosphorization, the V in by mother liquor2O5The 1.7 of gross mass Ammonium sulfate is added again, stirring precipitation, is settled out ammonium metavanadate at 120 minutes sedimentation times, is settled out solution and contains V2O5For 0.4g/L, Precipitate recovery rate is 99.57%；
13, product ammonium metavanadate is prepared into vanadic anhydride, in terms of vanadic anhydride, it is 76.1% to calculate vanadium overall recovery；
14, it presses single rotary kiln to calculate, 9.67 tons of vanadic anhydride of conversion is then produced in 150 tons of day blanking daily.
Embodiment 8
A kind of slag, vanadium slag, titanium white waste acid integrated conduct method include following operating procedure successively：
1, by vanadium slag（Containing V2O5For 25wt%）It is levigate to be more than 90% to 120 mesh excessively, contain slag（Containing V2O51wt%, CaO60wt%, Fe2O325wt%）It is levigate to cross 160 mesh be more than 80%；
2, it is mixed in 1/1 ratio by vanadium slag powder and containing steel-making slag powder；
3, titanium white waste acid（H2SO4For 150 g/L）The ratio mixing of 1L titanium white waste acids, material mixing are mixed into every KG steel-making slag powders Afterwards, it places 1 hour, material caking molding, then is broken for fritter；
4, material is subjected to gradually heating roasting, rises to 860 DEG C, is roasted 90 minutes at 860 DEG C, the mixed material after roasting contains V2O5Content is 12.31%；
5, by the material after roasting it is levigate to 120 mesh be more than 90%；
6, it presses solid-liquid mass ratio 1/5 and water stirring, 400 revs/min of speed of agitator is added；
7, it is gradually added industrial sulphuric acid（98%）Adjustment slurry PH stabilizes to 1.5, mixing time 60 minutes；
8, after slurry filters separation of solid and liquid, slag contains V after leaching2O5It is 2.2%, liquid contains V2O5A concentration of 20g/L leaches the rate of recovery It is 82.12%；
9, leachate swaps absorption using HD317 type resins, tail water V after absorption2O5A concentration of 1.5g/L；
10, resin adsorption V is pressed2O580% technical grade piece alkali number configuration slice aqueous slkali of quality carries out resin and frees.It obtains containing V2O5 A concentration of 110g/L deposition vanadium mother liquids；
11, according to V in deposition vanadium mother liquid2O5MgSO is added in the 6.7% of gross mass4, stir 30 minutes, dephosphorization carried out to mother liquor of precipitation of ammonium；
12, it is 8.5 industrial sulphuric acid adjustment PH to be added according to the deposition vanadium mother liquid after dephosphorization, the V in by mother liquor2O5The 1.2 of gross mass Ammonium sulfate, stirring precipitation are added again, 120 minutes sedimentation times were settled out ammonium metavanadate, and precipitation upper liquid is containing V2O5For 0.6g/L. Precipitate recovery rate is 99.45%；
13, product ammonium metavanadate is prepared into vanadic anhydride, in terms of vanadic anhydride, it is 81.66% to calculate vanadium overall recovery；
14, it presses single rotary kiln to calculate, 15.08 tons of vanadic anhydride of conversion is then produced in 150 tons of day blanking daily.
Embodiment 9
A kind of slag, vanadium slag, titanium white waste acid integrated conduct method include following operating procedure successively：
1, by vanadium slag（Containing V2O5For 0.6wt%）It is levigate to be more than 90% to 120 mesh excessively, contain slag（Containing V2O54.5wt%, CaO30wt%, Fe2O345wt%）It is levigate to cross 160 mesh be more than 80%；
2, it is mixed in 1/1 ratio by vanadium slag powder and containing steel-making slag powder；
3, titanium white waste acid（H2SO4For 300 g/L）The ratio mixing of 1L titanium white waste acids is mixed into every KG steel-making slag powders.Material mixes Afterwards, it places 1 hour, material caking molding, then is broken for fritter；
4, material is subjected to gradually heating roasting, rises to 860 DEG C, is roasted 90 minutes at 860 DEG C.Mixed material after roasting contains V2O5Content is 8.02%；
5, by the material after roasting it is levigate to 120 mesh be more than 90%；
6, it presses solid-liquid mass ratio 1/5 and water stirring, 400 revs/min of speed of agitator is added；
7, it is gradually added industrial sulphuric acid（98%）Adjustment slurry PH stabilizes to 1.5, mixing time 60 minutes；
8, after slurry filters separation of solid and liquid, slag contains V after leaching2O5It is 1.6%, liquid contains V2O5A concentration of 12.8g/L leaches recycling Rate is 80.05%；
9, leachate swaps absorption using HD317 type resins, tail water V after absorption2O5A concentration of 0.5g/L；
10, resin adsorption V is pressed2O580% technical grade piece alkali number configuration slice aqueous slkali of quality carries out resin and frees.It obtains containing V2O5 A concentration of 95g/L deposition vanadium mother liquids；
11, according to V in deposition vanadium mother liquid2O5MgSO is added in the 20% of gross mass4, stir 30 minutes, dephosphorization carried out to mother liquor of precipitation of ammonium；
12, it is 8 industrial sulphuric acid adjustment PH to be added according to the deposition vanadium mother liquid after dephosphorization, the V in by mother liquor2O53.0 times of gross mass Ammonium sulfate, stirring precipitation, 120 minutes sedimentation times is added.It is settled out ammonium metavanadate, precipitation upper liquid contains V2O5For 0.6g/L.It is heavy The shallow lake rate of recovery is 99.32%；
13, product ammonium metavanadate is prepared into vanadic anhydride, in terms of vanadic anhydride, it is 79.51% to calculate vanadium overall recovery；
14, it presses single rotary kiln to calculate, 9.57 tons of vanadic anhydride of conversion is then produced in 150 tons of day blanking daily.
Embodiment 10
Comparative example：Sodium roasting method
Sodium roasting method includes following operating procedure successively：
1, by vanadium slag（Containing V2O5For 15wt%）It is levigate to cross 120 mesh be more than 90%；
2, steel sodium low calcium tailings is climbed（Containing V2O5Containing CaO it is 3.7wt% for 1.8wt%）120 mesh of levigate mistake sieve is more than 90%；
3, by vanadium slag and climb steel sodium low calcium tailings in mass ratio 1/1 mix, formed mixture, then by mixture quality than 8% Sodium carbonate is added, the 3% of mass ratio is added sodium chloride, is uniformly mixed；
4, material roasts after being mixed in step 3, is 860 DEG C in temperature, roasts 80 minutes
5, material pentoxide content is 8.4wt% after measuring roasting；
6, add 1KG to be added in water for ball milling by every 2 liters of water material after roasting to be milled in slurry material particular diameter and be less than 120 mesh, slurry Temperature is higher than 80 DEG C；
7, slurry is separated by solid-liquid separation（It is detached using belt type filter mode）, obtained solid survey pentoxide content be 2.85%, a concentration of 27.75g/L of gained liquid vanadic anhydride；
8, after solution containing vanadium body in above-mentioned steps 7 being stood 12 hours, bottom sediment is filtered；
9, solution containing vanadium body is adjusted into PH to 2.5, by 2 times of addition ammonium chlorides of the quality containing vanadic anhydride in liquid, in a liquid It is passed through steam to be heated to be more than 90 DEG C, and maintains to be more than 90 DEG C and precipitate 60 minutes, ammonium poly-vanadate can be obtained after precipitation, liquid after precipitation Middle pentoxide content is 0.18 g/L；
10, by obtained solid in step 7（The % of 2.85wt containing vanadic anhydride）It is added and removes 8% sodium chloride of quality after moisture, 1% sodium carbonate is uniformly mixed；
11, it is 860 DEG C by mixed material high-temperature roasting temperature, the time is 80 minutes；
12,1.5L hot water is added according to every 1KG in material after roasting（80℃）Ratio be added water for ball milling wear into slurry；
13, slurry is separated by solid-liquid separation（Belt type filter）, second of obtained solid（Pentoxide content 0.8%）, gained liquid five A concentration of 13.67g/L of V 2 O；
14,10 grams of calcium chloride are added in the liquid of every liter of step 13, react 90 minutes, then stand 12 hours, filtering bottom precipitation Object, can obtain in liquid it is phosphorous less than 0.02g/L contain vanadium solution；
15, it will first contain and adjust PH in vanadium solution to 2.5, then press 2 times of addition ammonium chlorides containing vanadic anhydride quality in vanadium solution, And it is heated to 90 DEG C or more with steam, and maintain to precipitate 60 minutes more than 90 DEG C；
16, in precipitating ammonium poly-vanadate can be obtained, a concentration of 0.18g/L of vanadic anhydride in surplus solution after precipitation；
17, according to above-mentioned steps, it is 90.47% to calculate the total leaching rate of vanadium in material, and precipitation vanadium total recovery is 99.16%；
18, product ammonium poly-vanadate is prepared into vanadic anhydride, material vanadium recovery is 89.71% in terms of vanadic anhydride.
10 production method of above-described embodiment is compared, the application vanadium slag slag titanium white waste acid integrated conduct method, there are following Advantage：
（1）The present processes only need once to roast, and sodium roasting method production model needs to carry out after baking, on an equal basis The production capacity lower production cycle doubles, and cost of labor, energy consumption will also increase accordingly.
（2）The application method only needs to be added titanium white waste acid as auxiliary material, and titanium white waste acid do not need not only cost but also 500 yuan/m3 of processing cost can be saved, in contrast, the roasting cost of supplementary product that sodium roasting method uses is high, needs to add in roasting Enter a large amount of sodium carbonate and sodium chloride, and sodium carbonate price is 2600/ ton, sodium chloride price is 700/ ton.
（3）Generation that the application method is substantially pollution-free, sodium roasting method will produce big at high temperature because sodium chloride is added Measure reluctant hypertoxic Gases Chlorine.
（4）The application method realizes the utilization of waste material comprehensive high-efficiency, and by sodium roasting method not only without using waste material As raw material, and a large amount of waste liquids are produced in its production.
（5）The application method slag mixing vanadium slag titanium white waste acid produces the processing cost of one ton of vanadic anhydride on 5000 yuan of left sides The right side, and sodium roasting method is used to produce the processing cost of one ton of vanadic anhydride at 17200 yuan or so.
Embodiment 11
Comparative example：Calcification baking method
Calcification baking method includes following operating procedure successively：
1, by vanadium slag（Containing V2O5For 15wt%）It is levigate to cross 120 mesh be more than 90%；
2, by lime stone（It is 52.2wt% containing CaO）Be milled down to 120 mesh and be more than 90%, then and vanadium slag through step 1 press 18/100 Mass ratio is mixed；
3, material carries out high-temperature roasting, 870 DEG C of temperature, roasting time 120 minutes after mixing step 2；In material after roasting Pentoxide content is 12.7wt%；
4, by the material after roasting it is levigate to 120 mesh be more than 90%；
5, slurry is made in the ratio that 3L water is added in every 1KG through step 4 material, then adjusts pH value to 2.8, and leaching 60 divides Clock；
6, by after the material of step 5 separation of solid and liquid, liquid a concentration of 38.2g/L containing vanadic anhydride is obtained, obtains in solid and contains Vanadic anhydride is 2wt%.It can be calculated, it is 84.25% to leach the rate of recovery；
7, the liquid natural subsidence in step 6 is stood 24 hours, after filter out liquid obtained by sediment as mother liquor；
8, mother liquor is adjusted into PH to 2.5, then by 2 times of addition ammonium chlorides of vanadic anhydride quality in mother liquor, Mother liquor steam 90 DEG C or more are heated to, and maintains to precipitate 60 minutes more than 90 DEG C；
9, solid is precipitated as ammonium poly-vanadate, and a concentration of 0.4g/L of remaining vanadic anhydride in solution after precipitation calculates precipitation vanadium and returns Yield is 98.95%；
10, product ammonium poly-vanadate is prepared into vanadic anhydride, being computed can obtain, and in terms of vanadic anhydride, vanadium always returns this method Yield is 83.37%；
11,11 production method of comparative example, the application vanadium slag slag titanium white waste acid integrated conduct method, there are following advantages：
（1）The application method realizes efficiently using for waste material, and only needs to be added titanium white waste acid as auxiliary material, and titanium white waste acid is not It does not only need cost and 500 yuan/m3 of processing cost can be saved, and calcification baking method can not achieve comprehensive utilization of resources, adopt Roasting auxiliary material is done with lime stone or quick lime, waste of resource and has certain cost, specifically, lime stone cost is 60 yuan/ton, Quick lime cost is 300 yuan/ton.
（2）The application method by by comprehensive utilization of waste material vanadium recovery up to 91.52%.Calcification baking method always recycles Rate is 83.37%, abandons and also has 2% vanadic anhydride greatly to waste resource in residue, and the production rate of recovery is low, resource wave Take.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks Domain is included within the scope of the present invention.

Claims (10)

1. the integrated conduct method of a kind of slag, vanadium slag, titanium white waste acid, which is characterized in that include the following steps：
A. it is first 20 ~ 130 in mass ratio by slag and vanadium slag：100 mixing, then the ratio by 1kg slags addition 1L titanium white waste acids Example, continuously add titanium white waste acid, lump, after caking materials are crushed；
B. it will be roasted through the material of step a, calcination temperature is 850 ~ 880 DEG C, and roasting time is 60 ~ 120 minutes, preferably 90 points Clock；
C. the material that grain size is 120 mesh is made in the material through step b；
D. will be that 1/3.2 ~ 8.7 addition water mixes in mass ratio in the material through step c, preferably 1/4 ~ 1/8, adjusting pH afterwards is 1.2~1.8；
E. it will be separated by solid-liquid separation through the material of step d, then liquid be subjected to resins exchange absorption, the rear resin that carries out is freed；
F. magnesium sulfate removal of impurities will be added through the material of step e, the mass ratio that magnesium sulfate and vanadic anhydride is added is 1/5 ~ 1/ 15, preferably 1:10, the removal of impurities reaction time is 30 ~ 60 minutes；
G. the material pH value through step e is adjusted to 7.0 ~ 8.5, preferably 8.0, ammonium sulfate is added afterwards.
2. a kind of slag according to claim 1, vanadium slag, titanium white waste acid integrated conduct method, which is characterized in that the step Slag is 100 in mass ratio with vanadium slag in rapid a：100.
3. a kind of slag according to claim 1, vanadium slag, titanium white waste acid integrated conduct method, which is characterized in that the step Sulphur acid for adjusting pH is used in rapid d.
4. a kind of slag according to claim 1, vanadium slag, titanium white waste acid integrated conduct method, which is characterized in that the step It is 1.5 that pH is adjusted in rapid d.
5. a kind of slag according to claim 1, vanadium slag, titanium white waste acid integrated conduct method, which is characterized in that the steel Slag particle diameter is 120 ~ 200 mesh, preferably 160 mesh.
6. a kind of slag according to claim 1, vanadium slag, titanium white waste acid integrated conduct method, which is characterized in that the vanadium 100 ~ 180 mesh of slag particle diameter, it is preferred that the vanadium slag grain size is 120 mesh.
7. a kind of slag according to claim 1, vanadium slag, titanium white waste acid integrated conduct method, which is characterized in that the sulphur Ammonium sulfate addition and vanadic anhydride mass ratio in required material are 1.2 ~ 3.0, preferably 1.7 in sour ammonium step g.
8. a kind of slag according to claim 1, vanadium slag, titanium white waste acid integrated conduct method, which is characterized in that the titanium White spent acid 150 ~ 300g/L of sulfur acid, preferably sulfur acid 208g/L.
9. a kind of slag according to claim 1, vanadium slag, titanium white waste acid integrated conduct method, which is characterized in that the vanadium Slag composition includes V2O50 ~ 99wt%, preferably V2O50 ~ 25wt%, further preferably V2O515.2wt%。
10. a kind of slag according to claim 1, vanadium slag, titanium white waste acid integrated conduct method, which is characterized in that described Composition includes in slag：V2O50.3 ~ 4.5wt%, CaO30 ~ 60wt%, Fe2O310 ~ 45 wt%, it is preferred that V2O52.3wt%, CaO37.27wt%, Fe2O320wt%。
CN201810310898.0A 2018-04-09 2018-04-09 A kind of integrated conduct method of slag, vanadium slag, titanium white waste acid Pending CN108359806A (en)

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CN112458294A (en) * 2020-11-20 2021-03-09 河南荣佳钪钒科技有限公司 Method for recovering vanadium from titanium white waste acid by chlorination process
CN113106270A (en) * 2021-03-26 2021-07-13 西部矿业股份有限公司 Method for efficiently recovering vanadium based on modified acid leaching of vanadium-containing metallurgical slag

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CN103922423A (en) * 2014-03-31 2014-07-16 攀钢集团攀枝花钢铁研究院有限公司 Method of improving vanadium slag grade by utilizing titanium white waste acid
CN104178632A (en) * 2014-08-12 2014-12-03 东北大学 Method for comprehensively utilizing titanium white waste acid
CN104388679A (en) * 2014-09-30 2015-03-04 边悟 Method for extracting vanadium from vanadium-containing raw material

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CN103922423A (en) * 2014-03-31 2014-07-16 攀钢集团攀枝花钢铁研究院有限公司 Method of improving vanadium slag grade by utilizing titanium white waste acid
CN104178632A (en) * 2014-08-12 2014-12-03 东北大学 Method for comprehensively utilizing titanium white waste acid
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CN112458294A (en) * 2020-11-20 2021-03-09 河南荣佳钪钒科技有限公司 Method for recovering vanadium from titanium white waste acid by chlorination process
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CN113106270A (en) * 2021-03-26 2021-07-13 西部矿业股份有限公司 Method for efficiently recovering vanadium based on modified acid leaching of vanadium-containing metallurgical slag

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Application publication date: 20180803