CN104129838B - Leach the sedimentation method of vanadium mud in vanadium liquid - Google Patents
Leach the sedimentation method of vanadium mud in vanadium liquid Download PDFInfo
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- CN104129838B CN104129838B CN201410343656.3A CN201410343656A CN104129838B CN 104129838 B CN104129838 B CN 104129838B CN 201410343656 A CN201410343656 A CN 201410343656A CN 104129838 B CN104129838 B CN 104129838B
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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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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- Treatment Of Sludge (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of sedimentation method for leaching vanadium mud in vanadium liquid, this method technique is：Aluminium salt is added in the leaching vanadium liquid to be purified；Flocculating polymer agent solution is added after purification in vanadium liquid, is stood after mixing, then separation of solid and liquid, you can clarification vanadium liquid and vanadium mud is obtained.This method adds flocculating polymer agent solution, enables vanadium mud rapid subsidence after aluminium salt purification is added in leaching vanadium liquid；Therefore the present invention effectively improves the sinking speed of vanadium mud, the precipitation time is shortened, and then effectively improves the purification efficiency of vanadium liquid, makes whole production process linking more smooth, so that the precipitation process precipitation time was foreshortened to 100 minutes or so by 250 minutes or so, production efficiency is improved.This method significantly reduces silicon in vanadium liquid, phosphorus impurities content, reduces concentration of the supernatant containing vanadium, significantly reduces cleanser aluminum sulfate unit consumption, reduces system vanadium damage, improves vanadium mud separative efficiency；And the muddy vanadium liquid amount of having bad luck is reduced, reduce energy consumption.
Description
Technical field
The present invention relates to a kind of vanadium liquid purification method, especially a kind of sedimentation method for leaching vanadium mud in vanadium liquid.
Background technology
Process of the Leaching of Vanadium from Vanadium slag typically by raw material preparation, roasting, leaching, vanadium liquid purification, precipitation, APV calcinings and slab,
Vanadium liquid clean-up effect directly affects later process precipitation, calcination process in said process, to semi-finished product ammonium vanadate and it is follow-up its
The quality of its vanadium product plays decisive role, therefore the selection of vanadium liquid purification method is particularly important.
Roasted vanadic slag is leached by dense, and the soluble impurity such as silicon, phosphorus enters leaching with the dissolving of sodium vanadate
Go out in vanadium liquid.In the basic conditions, leach part foreign ion in vanadium liquid and occur hydrolysis generation colloidal suspended substance, form tool
There is the particle cluster of electric double layer structure scattered in the solution, these particle clusters are difficult that aggregation is settled, and are suspended in shape in leaching vanadium liquid
Into a kind of high impurity suspension.
At present, prior art mainly using AlSnSi alloy flocculated impurities element and be suspended in leach vanadium liquid in it is tiny from
Son group purifies the purpose of vanadium liquid to reach.Though the method can effectively remove the impurity such as silicon, the phosphorus in vanadium liquid, flocculate is more, wadding
Solid content classification is obvious in liquid after solidifying, and the Solid content in turbid solution can be settled, and the part suspension being classified out can not sink
Drop and remain in vanadium liquid, these flocculate diameters are small, light specific gravity, filter is easily worn when being filtered through leaf filter or sheet frame filter；One
Aspect, sheet frame filter mud can not be molded, and carry a large amount of vanadium liquids secretly, and increase vanadium is damaged；On the other hand, vanadium after the purification containing a large amount of flocculates
Liquid continues sedimentation in vanadium liquid storage tank, and partial flocculation thing enters deposition vanadium mother liquid, returns molten as sulfuric acid is added, prolongs the precipitation time
Grow and ammonium vanadate is of poor quality.Most of flocculate is slowly settled in vanadium liquid storage tank, produces a large amount of unqualified vanadium liquids, this part vanadium
Liquid still needs to return impurity and purification process and reprocessed.Vanadium liquid causes precipitation process not have qualified vanadium liquid to make when muddy serious
With a large amount of vanadium liquids carry out circular treatment in precipitation and removal of impurities process, cause whole production system can not normally produce final parking.
To sum up, existing AlSnSi alloy can not settle siliceous, phosphorus impurities little particle flocculates, vanadium mud sinking speed
Slowly, it is difficult to obtain clarifying vanadium liquid.
The content of the invention
The technical problem to be solved in the present invention is to provide in the leaching vanadium liquid that a kind of sinking speed is fast, effect is good vanadium mud it is heavy
Drop method.
In order to solve the above technical problems, the technical solution used in the present invention is：Aluminium salt is added in the leaching vanadium liquid to enter
Row purification；Flocculating polymer agent solution is added after purification in vanadium liquid, is stood after mixing, then separation of solid and liquid, you can clarified
Vanadium liquid and vanadium mud.
Aluminium salt addition of the present invention is 1.50~8.00kg/m3（That is 1m3Leach and 1.50~8.00kg is added in vanadium liquid
Aluminium salt）.The aluminium salt is the one or more in aluminum sulfate, aluminium chloride, polyaluminium sulfate and aluminium polychloride.
High polymer coagulant of the present invention is added using the solution form of mass percent concentration 0.50 ‰~5.00 ‰；
Vanadium liquid and the volume ratio of flocculating polymer agent solution are 1.00:0.20~1.00:0.70.The high polymer coagulant is cation
Polyacrylamide, PAMA, amphiprotic polyacrylamide and one kind in poly- third epoxychloropropane-dimethylammonium or
It is several.
The concentration range of vanadium is 20.00~50.00g/L in vanadium liquid of the present invention.Silicone content is 30.00 in the vanadium liquid
~80.00mg/L, phosphorus content is 0.50~5.00mg/L.
During Leaching of Vanadium from Vanadium slag, vanadium slag must carry out sodium oxide baking through adding sodium carbonate additives, by the vanadium in vanadium slag
Spinelle is oxidized to vanadic anhydride, and it is combined into vanadic acid sodium salt with the sodium oxide molybdena generated after soda decomposition and is present in after roasting
Material in；Material warm water leaches vanadic acid sodium salt into the aqueous solution after roasting, while generating substantial amounts of sodium metasilicate and phosphorus
Sour aluminium glue body；These colloidal suspensions, extremely difficult sedimentation is free in vanadium solution.The present invention adds high polymer coagulant in vanadium liquid
（Polyacrylamide（PAM））, the suspended ion in vanadium liquid is adsorbed using the principle of its enhanced flocculation and sedimentation, makes macromolecular chain mutual
Crosslinking is twined, is formed and built bridge, so that flocculent structure increase is thicker, the sediment for being enough to overcome buoyancy resistance is eventually formed, accelerated
The sinking speed of suspension.
It is using the beneficial effect produced by above-mentioned technical proposal：1st, the present invention adds aluminium salt purification in vanadium liquid is leached
Afterwards, flocculating polymer agent solution is added, enables vanadium mud rapid subsidence, the separation of vanadium mud and vanadium liquid is then carried out.Therefore this hair
The bright sinking speed for effectively improving vanadium mud, shortens the precipitation time, and then effectively improves the purification efficiency of vanadium liquid, makes
Whole production process linking is more smooth so that the precipitation process precipitation time was foreshortened to 100 minutes or so by 250 minutes or so,
Improve production efficiency.
2nd, the present invention significantly reduces silicon in vanadium liquid, phosphorus impurities content, reduces concentration of the supernatant containing vanadium, sila matter
Concentration drops to 30.00~80.00mg/L, phosphorus impurities concentration by 70.00~200.00mg/L by 850.00~1200.00mg/L
0.50~5.00mg/L is dropped to, is that the system-wide smooth production of Leaching of Vanadium from Vanadium slag creates necessary condition.
3rd, because of the reduction of impurity content in vanadium liquid, the present invention significantly reduces cleanser aluminum sulfate unit consumption, reduces and is
Vanadium of uniting is damaged, and improves vanadium mud separative efficiency；And the muddy vanadium liquid amount of having bad luck is reduced, reduce energy consumption.
4th, the present invention provides the vanadium liquid of more high-quality for precipitation system, and supernatant concentration containing vanadium is by 0.20g/L or so reductions
To below 0.12g/L, so as to be effectively guaranteed being smoothed out for subsequent technique.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the process flow diagram of the present invention.
Embodiment
Embodiment 1：Shown in Fig. 1, the processing step of the sedimentation method of vanadium mud is as described below in this leaching vanadium liquid.
By the 200.00m that concentration containing vanadium is 26.50g/L, impurity silicone content 35.14mg/L, impurity phosphorus content 0.95g/L3
Leach vanadium liquid to import in purification reactor, 300.00kg aluminium polychlorides are added in vanadium liquid is leached, purification run is carried out.Purification
After process terminates, vanadium liquid after purification is together squeezed into PAMC solution and settled in vanadium liquid settling tank；Sun
Cationic polyacrylamide concentration is 3.00 ‰（Quality）, consumption be 40.00m3.In settling tank, vanadium mud sinks rapidly, and vanadium liquid is clear
Impurity silicone content after clear is that 75.00mg/L, phosphorus content are 4.00mg/L；After vanadium mud is separated with vanadium liquid, supernatant liquor is overflow
Stream squeezes into precipitation process precipitation, and bottom mud carries out separation of solid and liquid through vanadium mud separation equipment.The precipitation time in precipitation process is
95 minutes, gained ammonium vanadate was calcined, obtains powder vanadium pentoxide, composition by precipitation supernatant concentration 0.12g/L
For：V2O598.71wt%, Si 0.049wt%, Fe 0.051wt%, P 0.008wt%, K2O+Na2O 0.47wt%, C
0.031wt%, S 0.075wt%, meet national standard YB/T 5304-2011《Vanadic anhydride》Requirement.
Embodiment 2：The processing step of the sedimentation method of vanadium mud is as described below in this leaching vanadium liquid.
In the 200.00m that concentration containing vanadium is 37.35g/L, impurity silicone content 78.30mg/L, impurity phosphorus content 2.80g/L3
500.00kg aluminum sulfate is added in vanadium liquid, it is 0.50 ‰ that purification, which terminates to add concentration in the solution after backward purification,（Quality）Two
Property polyacrylamide 80.00m3 , the sinking of vanadium mud rapidly, clarify by vanadium liquid, impurity silicone content 105.00mg/L, phosphorus content in vanadium liquid
11.00mg/L.Using this clarification vanadium liquid precipitation, the precipitation time is 110 minutes, precipitation supernatant concentration 0.11g/L, by gained
Ammonium vanadate is calcined, and obtains powder vanadium pentoxide, and composition is：V2O599.01%, Si 0.069%, Fe 0.057%, P
0.011%, K2O+Na2O 0.58%, C 0.049%, S 0.066%, meets standard YB/T5304-2011 requirement.
Embodiment 3：The processing step of the sedimentation method of vanadium mud is as described below in this leaching vanadium liquid.
In the 200.00m that concentration containing vanadium is 40.26g/L, impurity silicone content 49.45mg/L, impurity phosphorus content 3.40g/L3
Added in addition 800.00kg aluminium chloride and 800.00kg polyaluminium sulfates in vanadium liquid, the solution after the backward purification of purification end dense
Spend for 5.00 ‰（Quality）PAMA 60.00m3 , the sinking of vanadium mud rapidly, clarify by vanadium liquid, impurity silicon in vanadium liquid
Content 98.00mg/L, phosphorus content 9.00mg/L.Use this clarification vanadium liquid precipitation, precipitation supernatant concentration 0.095g/L, precipitation
Time is 102 minutes, and gained ammonium vanadate is calcined, powder vanadium pentoxide is obtained, composition is：V2O598.98%, Si
0.053%, Fe 0.068%, P 0.007%, K2O+Na2O 0.64%, C 0.038%, S 0.086%, meets standard YB/T5304-
2011 requirement.
Embodiment 4：The processing step of the sedimentation method of vanadium mud is as described below in this leaching vanadium liquid.
In the 200.00m that concentration containing vanadium is 48.40g/L, impurity silicone content 50.80mg/L, impurity phosphorus content 0.95g/L3
800.00kg polyaluminium sulfates are added in vanadium liquid, purification terminates to add the anion poly- third that concentration is 1.00 ‰ in after backward purification
Acrylamide 70.00m3With 1.00 ‰（Quality）Poly- third epoxychloropropane-dimethylammonium 70.00m3, rapidly, vanadium liquid is clear for the sinking of vanadium mud
Clearly, impurity silicone content 67.00mg/L, phosphorus content 5.00mg/L in vanadium liquid.Using this clarification vanadium liquid precipitation, precipitation supernatant liquor is dense
0.10g/L is spent, the precipitation time is 98 minutes, and gained ammonium vanadate is calcined, powder vanadium pentoxide is obtained, composition is：V2O5
98.98%, Si 0.053%, Fe 0.068%, P 0.007%, K2O+Na2O 0.64%, C 0.038%, S 0.086%, meets standard
YB/T5304-2011 requirement.
Claims (4)
1. a kind of sedimentation method for leaching vanadium mud in vanadium liquid, it is characterised in that this method technique is：Added in the leaching vanadium liquid
One or both of aluminum sulfate and polyaluminium sulfate are purified；Flocculating polymer agent solution is added after purification in vanadium liquid, is mixed
Stood after even precipitation, separation of solid and liquid is then carried out using filter plant, you can obtain clarification vanadium liquid and vanadium mud；
Wherein, the addition of one or both of described aluminum sulfate and polyaluminium sulfate is 1.50~8.00kg/m3；
The high polymer coagulant uses mass concentration to be added for 0.50 ‰~5.00 ‰ solution form；Vanadium liquid is wadded a quilt with cotton with macromolecule
The volume ratio of solidifying agent solution is 1.00:0.20~1.00:0.70.
2. the sedimentation method according to claim 1 for leaching vanadium mud in vanadium liquid, it is characterised in that：The high polymer coagulant
For in PAMC, PAMA, amphiprotic polyacrylamide and poly- third epoxychloropropane-dimethylammonium
One or more.
3. the sedimentation method according to claim 1 for leaching vanadium mud in vanadium liquid, it is characterised in that：Vanadium is dense in the vanadium liquid
Degree scope is 20.00~50.00g/L.
4. the sedimentation method according to claim 1 for leaching vanadium mud in vanadium liquid, it is characterised in that：Silicone content in the vanadium liquid
For 30.00~80.00mg/L, phosphorus content is 0.50~5.00mg/L.
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| CN108085517A (en) * | 2017-12-15 | 2018-05-29 | 河钢股份有限公司承德分公司 | A kind of preparation method of aerospace grade tablet vanadic anhydride |
| CN111690826A (en) * | 2020-06-17 | 2020-09-22 | 中国科学院过程工程研究所 | Method for removing impurities from vanadium slag by alkali leaching solution |
| CN112095025A (en) * | 2020-08-24 | 2020-12-18 | 河钢承德钒钛新材料有限公司 | Method for removing silicon and phosphorus from blank roasting-ammonia leaching vanadium liquid |
| CN112593077B (en) * | 2020-11-25 | 2022-11-04 | 龙佰四川矿冶有限公司 | Method for acid countercurrent heap leaching of vanadium titano-magnetite alkaline oxidized pellets |
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| US3733193A (en) * | 1970-07-22 | 1973-05-15 | Union Carbide Corp | Recovery of vanadium from titaniferous iron ores |
| CN1254023A (en) * | 1999-06-12 | 2000-05-24 | 湖南省安化县碳化硅厂 | Leaching-out method for extracting vanadium from vanadium-containg ore calcines and its application in stone-coal calcination-direct vanadium-extracting process |
| CN1298872C (en) * | 2002-12-09 | 2007-02-07 | 攀枝花钢铁有限责任公司钢铁研究院 | Phosphorus-eliminating purification process of vanadium-containing chamotte leachate |
| JP4502674B2 (en) * | 2004-03-22 | 2010-07-14 | 日本キャタリストサイクル株式会社 | Method for separating phosphorus-containing material from spent catalyst |
| CN101759313B (en) * | 2009-12-08 | 2011-07-27 | 武汉科技大学 | Method for recycling high-salinity heavy metal-enriched waste water from vanadium extraction from stone coal |
| CN103643039B (en) * | 2013-11-29 | 2016-06-22 | 四川省川威集团有限公司 | A kind of solution containing vanadium body defecation method |
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