CN106521191A - Production method and production system of vanadium oxide - Google Patents
Production method and production system of vanadium oxide Download PDFInfo
- Publication number
- CN106521191A CN106521191A CN201610997499.7A CN201610997499A CN106521191A CN 106521191 A CN106521191 A CN 106521191A CN 201610997499 A CN201610997499 A CN 201610997499A CN 106521191 A CN106521191 A CN 106521191A
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- Prior art keywords
- vanadium
- leaching
- feed liquid
- tank
- filter
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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
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/02—Apparatus therefor
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- 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
Abstract
The invention provides a production method and a production system of vanadium oxide. The production method comprises the steps of performing calcium roasting, leaching and vanadium precipitation on vanadium materials, storing vanadium-containing leaching feed liquid which is obtained by leaching in a buffer tank, and controlling the pH of the vanadium-containing leaching feed liquid in the buffer tank to be less than or equal to 4.00 with sulfuric acid. The production system comprises equipment, a leaching reaction tank, the buffer tank, vanadium precipitation equipment and an acid adding device, wherein the equipment is used for performing calcium roasting on the vanadium materials, the buffer tank is used for storing the vanadium-containing leaching feed liquid which is obtained by leaching, and the acid adding device is connected with the buffer tank and is used for adjusting the pH of the vanadium-containing leaching feed liquid in the buffer tank to be less than or equal to 4.00.According to the production method and the production system, the problem of vanadium loss caused by long-time standing of unqualified acid leaching feed liquid and acid-leaching vanadium-containing leaching feed liquid of which the pH is less than 2.50 or the pH is greater than 4.00 and qualified acid leaching liquid in the production process of the vanadium oxide is effectively solved, the qualified acid leaching liquid of which the pH is between 2.50 to 4.00 and which can be stably stored for a long time can be produced so as to produce the vanadium oxide, and the vanadium recovery rate is increased.
Description
Technical field
The present invention relates to metallurgical technology field, more specifically, is related to a kind of oxidation technique for producing vanadium and production equipment.
Background technology
The main method of Leaching of Vanadium from Vanadium slag is sodium roasting-water logging extraction vanadium method, as the vanadium recovery of the method is low, is needed
Multiple roasting is carried out, the response rate of vanadium is also only 80% after multiple roasting, and repeatedly roasting can cause energy consumption higher.
Harmful HCl, Cl can be also produced in the roasting process of vanadium raw materials2Deng subversive gas, the heavy process of follow-up ammonia can obtain high salt
Degree nitrogen-containing wastewater, not only pollutes environment, and it is higher to administer cost.
In order to solve the problems, such as sodium roasting-water logging vanadium extraction, CN102560086A proposes a kind of calcification baking-acidleach and carries
Vanadium technique.The roaster that more than 600 DEG C are directly entered after vanadium slag is mixed with Calx or limestone carries out calcification baking, makes vanadium slag
In vanadium be converted into calcium vanadate, roasting grog makes solid-state vanadium enter vanadium solution under the acid effect of acid solution, and then produces vanadium oxygen
The products such as compound.
In terms of the domestic research to calcification baking-acid leaching process is concentrated mainly on the exploration and optimization of process conditions, mainly
The shadow of impact, pH value of solution of the impact, grog granularity including different acid concentrations to leaching effect to leaching effect to leaching effect
Ring etc., but it is limited only to study each condition for affecting leaching effect to obtain leaching optimum condition, and to how to control shadow
Ring leaching factors not making a search, and production Study on Problems in esse to factory is less.
The content of the invention
For the deficiencies in the prior art, an object of the present invention is to solve present in above-mentioned prior art
One or more problems.For example, an object of the present invention is to provide vanadium recovery in a kind of raising vanadium oxides producing process
Production method and production system.
To achieve these goals, one aspect of the present invention provides a kind of vanadium oxide production method, the production method bag
Include carries out calcification baking, leaches and precipitation to vanadium raw materials, wherein, the feed liquid containing vanadium leaching that leaching is obtained is stored in surge tank,
The production method also includes pH≤4.00 that feed liquid is leached containing vanadium in the surge tank are controlled with sulphuric acid.Preferably, it is described
Sulphuric acid is dilute sulfuric acid.
Further, the production method is additionally included in the sulphuric acid and controls to leach feed liquid containing vanadium in the surge tank
After the step of pH≤4.00, filter to leaching feed liquid containing vanadium, if pH >=2.50 that feed liquid is leached containing vanadium after filtering,
Then by obtain be can the qualified pickle liquor of stable storage directly carry out precipitation, otherwise by obtain after the filtration be can not be steady
It is (such as within 3h, excellent at short notice that step is leached in the unqualified acidleach of the pH ＜ 2.50 of fixed storage leaching feed liquid return containing vanadium
Select 1-3h) leached next time.Wherein, in leaching the step of feed liquid is filtered containing vanadium at described pair, filter and remove containing vanadium
Leach the vanadate precipitation in feed liquid.
Another aspect of the present invention provides a kind of vanadium oxide production system, and the production system includes carrying out calcium to vanadium raw materials
The surge tank and precipitation equipment that feed liquid is leached containing vanadium for obtaining is leached in the equipment of change roasting, Leach reaction tank, storage, and its feature exists
In the production system also includes and the tank connected acid adder of the buffering, and the acid adder is used to adjust the buffering
PH≤4.00 that feed liquid is leached containing vanadium in tank.
Further, the production system also includes with the tank connected filter of the buffering and with the filter exporting
The one-level filter tank of connection, the filter in surge tank containing vanadium leach feed liquid filter, the one-level filter tank
Outlet is connected with the Leach reaction tank and precipitation equipment respectively, when pH >=2.50 that feed liquid is leached containing vanadium in one-level filter tank
When, the outlet of the one-level filter tank is connected with the precipitation equipment, as the pH ＜ 2.50 that feed liquid is leached containing vanadium in one-level filter tank
When, the outlet of the one-level filter tank is connected with the Leach reaction tank.Wherein, the filter can filter removal and leach containing vanadium
Vanadate precipitation in feed liquid.
Compared with prior art, beneficial effects of the present invention include：The present invention can greatly improve the steady of live pickle liquor
Qualitative, acidleach brings up to 96.5% by 83% containing the qualification rate that vanadium leaches material liquid pH value (2.50≤pH≤4.00), qualifying liquid pH
The qualification rate of value (2.50≤pH≤4.00) brings up to 98% by 93%.Obtained qualified pickle liquor pH value fluctuation range was by former
2.13～4.51 change for 2.41～4.10, substantially close to the pH value range 2.50～4.00 in technological requirement, effectively keep away
Acidleach feed liquid, acidleach are exempted from and the problem of vanadium loss during feed liquid, qualified pickle liquor stand have been leached containing vanadium.Underflow slag TV contents by
13.92% is reduced to 3.00%, and the response rate of vanadium greatly improved, and the quantity of slag is significantly reduced, and reduces labor cleaning's cost
And labor intensity.
Description of the drawings
By the description for carrying out below in conjunction with the accompanying drawings, the above and other purpose and feature of the present invention will become more clear
Chu, wherein：
Fig. 1 shows the process schematic of vanadium oxide production system according to an exemplary embodiment of the present invention.
Specific embodiment
Hereinafter, accompanying drawing will be combined and exemplary embodiment will describe vanadium oxide production method of the invention in detail
And its production system.
It is found by the applicant that：Certain vanadium factory (is leached also known as pickle liquor, containing vanadium in the initial stage gone into operation, the immersion containing vanadic acid after leaching
Feed liquid, leachate) it is stored in 8Qualified flow container in, (qualified flow container be different from surge tank：Surge tank
It is the acidleach feed liquid for storing batch extractor releasing；Qualified flow container be storage 2.50≤pH≤4.00 can stable storage it is qualified
Immersion containing vanadic acid) displacement and storage time it is longer, during scene has underflow slag, TV (v element accounts for the mass fraction of underflow slag) contains
Amount high (highest can be to 26%) and the big problem of the quantity of slag, have had a strong impact on the raising and normal production of vanadium recovery.Specifically：
(1) filtration time is long, and surge tank slip pH value rises, and pickle liquor stands precipitation, affects vanadium yield.(2) leachate acid content mistake
Amount, pH value are extremely low, form vanadate precipitation, affect vanadium yield in tank field.(3) leach slip pH value higher or low, reduce
Strainability, affects production.
In order to solve the above problems, the application proposes a kind of preconditioning technique of the stability for improving qualified vanadium liquid, in mistake
Increase acid adder before filter and adjust the technical measures that fluid path line is returned in slip pH and 1 grade of filter tank increase in surge tank, it is ensured that close
The pH stable of lattice liquid is between 2.50～4.00.I.e.：
(1) increase acid adder (or referred to as means for feeding acid) before filtration in surge tank, in time adjustment slip pH value, it is to avoid
As chemical reaction causes the problem of slip pH value rising, qualification rate of the pH of leaching solution in the range of 2.50～4.00 is improved,
Simultaneously prevent from forming gelatinous precipitate and causing the problem of filtration difficulty as pH value rises.
(2) after filter, liquid process route is returned in 1 grade of filtrate tank increase.Under for abnormal conditions, pH ＜ are pumped back into
2.50 leachate is to batch extractor, in case the leachate of peracid causes the problem of vanadium precipitation (loss) into after qualified flow container.
The acidleach feed liquid of 2.50≤pH≤4.00, acidleach containing vanadium leach feed liquid, qualified pickle liquor can stable storage principle
It is as follows with the principle difference for realizing high leaching rate：
PH≤4.00 can long-time stable storage pickle liquor principle：Leaching terminates rear feed liquid and need to store in batch extractor
A period of time can just continue discharge filtration, during storage, as acid and grog also occur that chemical reaction, cause leachate
PH has been raised, particularly grog granularity is partially thick, time of repose more than more than 1h when, its slip pH value rises comparatively fast, typically all
More than 4.0；When filtration pH value is leached less than 4.1, its residue is basically identical with solution meter leaching rate, is 97% or so；When
When filtering pH=4.1～4.7, it is more or less the same under residue meter leaching rate and normal condition, and solution meter leaching rate is then with filtration
The rising of pH value and reduce, observation stands the leachate after 24h, it is found that bottom of bottle has significantly orange granule material containing vanadium to analyse
Go out, and amount of precipitation is more with the rising for filtering pH value, solution meter V leaching rate is only 75.19% during pH=4.7, and this is main
It is this cationoid due to mainly containing certain manganese, magnesium, ammonium ion in calcification grog pickle liquor, when solution ph rises
Combined rear formation to precipitate and separate out with many vanadium acid anions, cause solution meter vanadium recovery to reduce；PH value is filtered when leaching>
When 4.7, residue and solution meter V leaching rate all decline with the rising for filtering pH value, and this is to precipitate institute in a large number due to cation
Cause, and time of repose is longer, solution meter leaching rate is lower, during pH=5.0, residue and solution meter leaching rate be only 68.32%,
58.68%, that is, when pH value is filtered more than 4.7, can cause substantial amounts of vanadium loss；At the scene it has also been found that when filter material slurry pH value is raised
During to more than 4.0, often there is the problem that residue cannot not taken out dryly on band filter in Jing, or even affects production.In use for laboratory reuse
Water adjusts qualifying liquid pH to more than 4.0 and stands the test for refiltering for 4 days, as a result finds that now the qualifying liquid of precipitation is refiltered
Difficulty, is coincide substantially with field condition, and the precipitation of Jing solid-liquor separations, and which is mainly made up of gelatinous precipitate, and this is also to cause now
Field slip cannot be filtered and the high main cause of residue moisture content.
1 acidleach material liquid pH precipitation embodiment of table
| Acidleach material liquid pH | Solution meter leaching rate (%) | Residue meter leaching rate (%) |
| 3.50 | 96.88 | 97.02 |
| 3.80 | 95.62 | 95.17 |
| 4.10 | 97.41 | 96.41 |
| 4.40 | 86.71 | 96.65 |
| 4.70 | 75.19 | 96.89 |
| 5.00 | 58.68 | 68.32 |
PH >=2.50 can long-time stable storage pickle liquor principle：Qualifying liquid (pH=2.84) under normal circumstances with
And after the qualifying liquid of pH=2.5 stands 4 days, there is no significant change in its solution content of vanadium, ie in solution can stable storage；When qualified
During liquid pH value ＜ 2.5, the precipitation rate during qualifying liquid stands reduces bright with the decline of pH value and the prolongation of time of repose
Aobvious, particularly when pH value≤1.5, after 2 days, its precipitation rate can reach 83.14% to solution left standstill, and during pH value≤1.5, stand
After 6h, its precipitation rate has just reached 83.37%, very big to the stability influence of qualifying liquid.
2 acidleach of table leaches material liquid pH precipitation embodiment containing vanadium
Fig. 1 shows the process schematic of of vanadium oxide production system according to an exemplary embodiment of the present invention.Oxygen
The production method for changing vanadium includes carrying out vanadium raw materials calcification baking, leaches and precipitation, wherein, will contain vanadium raw materials carries out calcification roasting
Burn, the calcification baking grog containing vanadium is obtained.(mother solution is closed in being surge tank in batch extractor (Leach reaction tank) to be separately added into mother solution
By filtering, the low-concentration vanadium-containing after wash water washing leaches feed liquid to the acidleach feed liquid of lattice, is stored in two grades of filter tanks), smart grog
And dilute sulfuric acid, carry out sulphuric acid and soak molten, obtain feed liquid being leached containing vanadium.The feed liquid containing vanadium leaching that leaching is obtained is stored in surge tank
It is interior, in vanadium extracting process, as the time swap of feed liquid, the storage of qualified pickle liquor and vanadium is leached in acidleach feed liquid, acidleach containing vanadium
It is longer, can cause TV (v element accounts for the mass fraction of the underflow slag) highest in live underflow slag can be to 26%, and the quantity of slag
Greatly, the raising and normal production of vanadium recovery have been had a strong impact on.For this purpose, as shown in figure 1, in an exemplary enforcement of the present invention
In example, increase acid adder (automatic device of adding acid) before filtration and adjust slip pH in surge tank, specifically, when in surge tank
When leaching the pH ＞ 4.00 of feed liquid containing vanadium, with acid adder is into surge tank plus the pH value of feed liquid is leached in dilute sulfuric acid adjustment containing vanadium.
When pH≤4.00 of feed liquid being leached containing vanadium in surge tank, will contain vanadium and leach feed liquid and deliver to filter to enter to leaching feed liquid containing vanadium
Row is filtered (for example, filter and remove the vanadate precipitation leached containing vanadium in feed liquid), and the filtrate after filtration delivers to one-level filter tank, such as
Fruit filter after pH >=2.50 that feed liquid is leached containing vanadium, then obtain be can the qualified pickle liquor of stable storage directly sunk
Vanadium, otherwise by obtain after the filtration be can not stable storage pH ＜ 2.50 unqualified acidleach containing vanadium leach feed liquid return
Leaching step carries out once leaching in short time 1-3h.
In another exemplary embodiment of the present invention, vanadium oxide production system includes carrying out calcification baking to vanadium raw materials
Equipment, Leach reaction tank, storage leach obtain containing vanadium leach feed liquid surge tank and precipitation equipment, wherein, the production
System also includes with the tank connected acid adder of buffering and with the tank connected filter of buffering and with filter outlet what is be connected
One-level filter tank, acid adder can be arranged in surge tank for adjusting pH≤4.00 that feed liquid is leached containing vanadium in surge tank,
For filtering to leaching feed liquid containing vanadium in surge tank, filter can filter removal and leach in feed liquid containing vanadium filter
Vanadate is precipitated.The outlet of one-level filter tank is connected with Leach reaction tank and precipitation equipment respectively, when in one-level filter tank containing vanadium
When leaching pH >=2.50 of feed liquid, the outlet of one-level filter tank is connected with the precipitation equipment, and continuation is carried out at precipitation to leachate
Reason；When in one-level filter tank, when leaching the pH ＜ 2.50 of feed liquid containing vanadium, the outlet of one-level filter tank is connected with Leach reaction tank, will leaching
Going out liquid and returning to batch extractor carries out once leaching operation in 3h, in case the leachate of peracid is made into after qualified flow container
The problem of (loss) is precipitated into vanadium, the precipitation loss occurred in qualified flow container, in making underflow slag, vanadium increases, and in liquid, vanadium is reduced.
The acidleach that one-level filter tank is used for after temporary filtration leaches feed liquid containing vanadium, and it is once to filter that this acidleach leaches feed liquid containing vanadium
Liquid, not scrubbed, concentration is higher.Acidleach in one-level filter tank leaches feed liquid after standing sedimentation containing vanadium, and sedimentation solid is underflow
Slag, supernatant liquid are that qualifying liquid enters qualified flow container, and sending into precipitation operation carries out precipitation operation.
For further verify the application application effect, applicant carried out application example checking：Using the side of the present invention
After method, live acidleach feed liquid, acidleach are leached feed liquid, the stability of qualified pickle liquor containing vanadium and are greatly improved, and acidleach contains vanadium
The qualification rate for leaching material liquid pH value (2.50≤pH≤4.00) brings up to 96.5% by 83%, qualifying liquid pH value (2.50≤pH≤
4.00) qualification rate brings up to 98% by 93%.The maximum of pH value, minima by original 4.51,2.13 controls to 4.10,
2.41, substantially close to pH value in 2.50～4.00 technological requirement, effectively prevent and during pickle liquor stands, precipitate vanadium damage
The problem of mistake, underflow slag TV contents are reduced to 3.00% by 13.92%%, the response rate of vanadium greatly improved, and the quantity of slag is obvious
Reduce, reduce labor cleaning's cost and labor intensity, effect is fine, with obvious economic benefit.
In sum, after this employing present invention, the stability of live pickle liquor is greatly improved, it is ensured that qualifying liquid
PH stable between 2.50～4.00, acidleach leaches the qualification rate of material liquid pH value (2.50≤pH≤4.00) by 83% containing vanadium
96.5% is brought up to, the qualification rate of qualifying liquid pH value (2.50≤pH≤4.00) brings up to 98% by 93%, greatly improves acidleach
The qualification rate of liquid pH value, and the precipitation rate that solution long-time stands is reduced, the underflow quantity of slag and its TV contents are reduced, is improve
The response rate of vanadium oxide.
Although above by describing the present invention with reference to exemplary embodiment, those skilled in the art should be clear
Chu, in the case of the spirit and scope limited without departing from claim, can be carried out respectively to the exemplary embodiment of the present invention
Plant modifications and changes.
Claims (8)
1. a kind of production method of vanadium oxide, the production method include carrying out vanadium raw materials calcification baking, leach and precipitation, its
In, the feed liquid containing vanadium leaching that leaching is obtained is stored in surge tank, it is characterised in that the production method also includes using sulphuric acid control
Make pH≤4.00 that feed liquid is leached containing vanadium in the surge tank.
2. the production method of vanadium oxide according to claim 1, it is characterised in that the production method is additionally included in described
After the step of pH≤4.00 containing vanadium leaching feed liquid in the surge tank are controlled with sulphuric acid, carried out to leaching feed liquid containing vanadium
Filter, if filter after containing vanadium leach feed liquid pH >=2.50, by obtain be can stable storage qualified pickle liquor it is direct
Precipitation is carried out, the unqualified acidleach that pH ＜ 2.50 are obtained after the filtration is leached into feed liquid containing vanadium otherwise and is returned leaching step, and
Carry out once leaching in 3h.
3. the production method of vanadium oxide according to claim 2, it is characterised in that leaching feed liquid containing vanadium at described pair is carried out
In the step of filtration, filter and remove the vanadate precipitation leached containing vanadium in feed liquid.
4. the production method of vanadium oxide according to claim 2, it is characterised in that carry out once leaching in 1～3h.
5. the production method of vanadium oxide according to claim 1, it is characterised in that the sulphuric acid is dilute sulfuric acid.
6. a kind of production system of vanadium oxide, the production system include carrying out vanadium raw materials calcification baking equipment, leach it is anti-
Answer tank, the surge tank and precipitation equipment that feed liquid is leached containing vanadium that obtain are leached for storing, it is characterised in that the production system
Also include and the tank connected acid adder of the buffering, the acid adder is used to adjust the leached material containing vanadium in the surge tank
PH≤4.00 of liquid.
7. the production system of vanadium oxide according to claim 6, it is characterised in that the production system also include with it is described
The one-level filter tank for buffering tank connected filter and being connected with filter outlet, the filter is in surge tank
Containing vanadium leach feed liquid filtered, the outlet of the one-level filter tank is connected with the Leach reaction tank and precipitation equipment respectively,
When in one-level filter tank, when leaching pH >=2.50 of feed liquid containing vanadium, the outlet of the one-level filter tank is connected with the precipitation equipment,
When in one-level filter tank, when leaching the pH ＜ 2.50 of feed liquid containing vanadium, the outlet of the one-level filter tank is connected with the Leach reaction tank
It is logical.
8. the production system of vanadium oxide according to claim 6, it is characterised in that the filter can filter removal and contain
Vanadium leaches the vanadate precipitation in feed liquid.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412539A (en) * | 2008-11-18 | 2009-04-22 | 攀钢集团研究院有限公司 | Clean production process for vanadium oxide |
| CN101898793A (en) * | 2010-07-28 | 2010-12-01 | 攀钢集团冶金工程技术有限公司 | Leaching method of vanadium-containing clinker |
| CN105274336A (en) * | 2015-11-27 | 2016-01-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for stabilizing leaching solution in calcification vanadium extraction process |
-
2016
- 2016-11-11 CN CN201610997499.7A patent/CN106521191A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101412539A (en) * | 2008-11-18 | 2009-04-22 | 攀钢集团研究院有限公司 | Clean production process for vanadium oxide |
| CN101898793A (en) * | 2010-07-28 | 2010-12-01 | 攀钢集团冶金工程技术有限公司 | Leaching method of vanadium-containing clinker |
| CN105274336A (en) * | 2015-11-27 | 2016-01-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for stabilizing leaching solution in calcification vanadium extraction process |
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