CN107815547A - The clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique - Google Patents
The clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique Download PDFInfo
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- CN107815547A CN107815547A CN201711092958.8A CN201711092958A CN107815547A CN 107815547 A CN107815547 A CN 107815547A CN 201711092958 A CN201711092958 A CN 201711092958A CN 107815547 A CN107815547 A CN 107815547A
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- Prior art keywords
- vanadium
- foulant
- clean method
- acid precipitation
- precipitation
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Classifications
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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
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/02—Cleaning pipes or tubes or systems of pipes or tubes
- B08B9/027—Cleaning the internal surfaces; Removal of blockages
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
- B08B9/08—Cleaning containers, e.g. tanks
-
- 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
-
- 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 present invention relates to the clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique, belongs to vanadium oxide extraction field.The technical problems to be solved by the invention are to provide the clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique, and this method is cleaned using alkali lye.The inventive method can effectively clean caused foulant in the production equipments such as heat exchanger and settling tank, and cleaning efficiency is high, and cost is low；Moreover, the alkalescence obtained after cleaning can carry out precipitation by the acid precipitation technique of routine again containing vanadium solution, so as to reclaim vanadium therein, finished product V2O5High purity more than 98%.Compared to traditional clean method, the present invention can be saved time and cost of labor, and product purity is also obviously improved, and have significant economic benefit.
Description
Technical field
The present invention relates to the clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique, belongs to vanadium oxide extraction field.
Background technology
At present, the precipitation process generally use acid ammonium salt precipitation method (concrete technology step of vanadium oxide process for cleanly preparing
Reference can be made to Chinese patent CN200810305601, a kind of clean preparation method of vanadium oxide), in precipitation process heat exchanger tube and
Precipitation top tank structure can form foulant, and accumulation for a long time can form thicker dirty layer.Dirty layer in heat exchanger tube can make pipeline
Interior to be diminished by the flow containing vanadium solution, precipitating the dirty layer of top tank structure makes precipitation tank volume diminish, and can all have a strong impact on precipitation work
The production efficiency of sequence.Therefore, to carrying out periodic cleaning with the foulant of precipitation top tank structure in precipitation process heat exchanger tube and returning
Receipts are extremely necessary.
Irregularly to be cleared up depending on scaling degree, cleaning makes the traditional processing method of vanadium products factory after using artificial percussion
The method rinsed with giant, then collects foulant, enters follow-up process system after being mixed with the ammonium poly-vanadate normally produced
Take vanadium oxide product.There is the problem of cost of labor is high in this method for cleaning, and often lead to impurity content in vanadium oxide product
It is higher.
Up to the present, have no a kind of cleaning of efficient energy-saving and reclaim acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique
Method.
The content of the invention
It is an object of the invention to provide the clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique, to solve tradition
Method for cleaning cost of labor is high, influences the problems such as vanadium oxide product quality.
The invention provides the clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique, this method caustic dip.
Further, the foulant is caused by calcification baking acidity precipitation technique.
Further, V is contained in the foulant2O5、SO4 +、MnO、SiO2And Fe2O3。
Further, the composition of following percentage by weight is contained in the foulant：V2O5：85~95%, SO4 +：0.8~
1.3%, MnO：1.0~2.0%, SiO2：3.0~4.5%, Fe2O3：0.5~1.0%.
Further, the alkali lye is sodium hydroxide and/or potassium hydroxide aqueous solution.
Further, in the alkali lye alkali mass fraction >=30%.
Wherein, mass fraction is bad to the solvability of foulant less than 30% alkali lye.
Further, steam heating is passed through during caustic dip.
Further, steam temperature is 180~210 DEG C.
The invention provides the recovery method of vanadium in acid precipitation foulant, comprise the following steps：It is clear according to methods described
Foulant is washed, cleaning fluid is collected, acid precipitation, produces ammonium poly-vanadate product.
Further, the method for the acid precipitation is：Ammonium salt is added into cleaning fluid to NH4 +Concentration is vanadium concentration
1.2~2.0 times, cleaning fluid pH is adjusted to 2.0~2.5, more than 95 DEG C is heated to, filtering, produces ammonium poly-vanadate product.
Wherein, if NH4 +Concentration is less than 1.2 times of vanadium concentration, and precipitation is insufficient；If higher than 2.0 times can accelerating impurity precipitation,
Influence product quality.
Further, the ammonium salt is one or more kinds of in the inorganic ammonium salts such as ammonium sulfate, ammonium carbonate or ammonium chloride
Mixture.
The invention provides the clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique.Can be effective using this method
Caused foulant in the production equipment such as heat exchanger and settling tank is cleaned, cleaning efficiency is high, and cost is low；Moreover, obtained after cleaning
Alkalescence containing vanadium solution can again by routine acid precipitation technique carry out precipitation, so as to reclaim vanadium therein, finished product V2O5's
High purity more than 98%.Compared to traditional clean method, the present invention can save time and cost of labor, and product is pure
Degree is also obviously improved, and has significant economic benefit.
Brief description of the drawings
Fig. 1 is precipitation foulant clearing and retrieving flow chart in embodiment.
Embodiment
The raw material that is used in the specific embodiment of the invention, equipment are known product, are obtained by buying commercially available prod.
The invention provides the method that caused acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique is cleaned by caustic dip.
Inventor is sampled to foulant, first with the main composition of semi-quantitative analysis sample, recycles stoichiometric
The content of each component is analyzed, its main component is the composition of following percentage by weight：V2O5：85~95%, SO4 +：0.8~
1.3%, MnO：1.0~2.0%, SiO2：3.0~4.5%, Fe2O3：0.5~1.0%.In addition to pentavalent vanadium, wherein impurity contains
Amount it is higher, if traditionally the ammonium poly-vanadate directly with normally producing be mixed and fed into follow-up process produce vanadium oxide production
Product, the content of impurity in product can be increased.
Inventor selects the production equipment such as caustic dip heat exchanger and settling tank, energy according to the composition and property of foulant
It is enough to dissolve foulant therein well.
Further, inventor has investigated solvability of the variety classes alkali lye to acid precipitation foulant, and experiment is found,
Sodium hydroxide, the cleaning performance of potassium hydroxide are optimal, although ammoniacal liquor also has the effect of certain dissolution of scale thing, effect is not so good as hydrogen
Sodium oxide molybdena, potassium hydroxide.
Further, the alkalescence obtained after cleaning can carry out precipitation by the acid precipitation technique of routine again containing vanadium solution,
So as to reclaim vanadium therein, finished product V2O5High purity more than 98%.
Further, the alkalescence obtained after cleaning carries out precipitation, upper strata containing vanadium solution by the acid precipitation technique of routine
Liquid add reducing agent reduction after filter, recyclable vanadium chromium filter cake, gained filtrate evaporating, concentrating and crystallizing obtain sodium sulphate, sodium carbonate or
Sodium chloride, so as to reclaim sodium salt product.Using this method Na+, Cl- plasma can be avoided to enter water circulation system, influence work
The clean manufacturing of skill.
Embodiment 1 is using the inventive method cleaning acid ammonium salt precipitation foulant and reclaims vanadium therein
The serious end interface of heat exchanger tube two of Xichang steel vanadium vanadium products factory precipitation process A knots dirt is pulled down connect it is new
Pipeline, one end connection pump, pump is the sodium hydrate aqueous solution that mass fraction is 30% in lye tank (vat), in lye tank (vat), to heat exchange
Device is pumped into alkali lye, and alkali lye flows out from the other end returns to lye tank (vat), foulant in circulation immersion dissolving heat exchanger tube, can open and change
Hot device steam heating accelerates dissolving, and vapor (steam) temperature is 180~210 DEG C；The solution after dissolving is squeezed into inwall after immersion dissolving 2h
In the serious A1 settling tanks of fouling, it is rinsed with a small amount of new water or the former device pipeline of heat exchanging containing vanadium solution, solution one after flushing
And squeeze into A1 settling tanks, alkali lye is added into A1 settling tanks to 1/2 tank liquid level, stirring is opened and 180~210 DEG C of steam heats
Accelerate foulant dissolving, be heated to reducing quantity of steam when solution in settling tank reaches 60 DEG C, continue to stir and use pump after being incubated 4h
Solution in A1 tanks is pumped into A2 tanks, and A1 tanks are rinsed containing vanadium solution with a small amount of new water or original, then immersion dissolving A2 tanks
Foulant, repeat above step and solution in tank after dissolving is pumped into A lines after the 4 settling tank complete liquidations of A lines are clean
Standby settling tank, add ammonium sulfate NH into solution4 +Concentration is 1.2 times of vanadium, stirring, adjusts pH value of solution to 2.0~2.5,180
~210 DEG C are steam heated to (more than 95 DEG C) of boiling progress precipitations, obtained sediment ammonium poly-vanadate filtration washing post analysis into
Divide V2O5Content is 98.35%, and Upper-liquor of Precipitating Vanadate Process is filtrated to get vanadium chromium filter cake after adding reducing agent reduction, stores up, and filtrate evaporation is dense
Sheepshank crystalline substance obtains sodium sulphate.
Embodiment 2 is using the inventive method cleaning acid ammonium salt precipitation foulant and reclaims vanadium therein
The serious end interface of heat exchanger tube two of Xichang steel vanadium vanadium products factory precipitation process A knots dirt is pulled down connect it is new
Pipeline, one end connection pump, pump is the sodium hydrate aqueous solution that mass fraction is 52% in lye tank (vat), in lye tank (vat), to heat exchange
Device is pumped into alkali lye, and alkali lye flows out from the other end returns to lye tank (vat), foulant in circulation immersion dissolving heat exchanger tube, can open and change
Hot device steam heating accelerates dissolving, and vapor (steam) temperature is 180~210 DEG C；The solution after dissolving is squeezed into inwall after immersion dissolving 1h
In the serious A1 settling tanks of fouling, it is rinsed with a small amount of new water or the former device pipeline of heat exchanging containing vanadium solution, solution one after flushing
And squeeze into A1 settling tanks, alkali lye is added into A1 settling tanks to 1/2 tank liquid level, stirring is opened and 180~210 DEG C of steam heats
Accelerate foulant dissolving, be heated to reducing quantity of steam when solution in settling tank reaches 60 DEG C, continue to stir and use pump after being incubated 2h
Solution in A1 tanks is pumped into A2 tanks, and A1 tanks are rinsed containing vanadium solution with a small amount of new water or original, then immersion dissolving A2 tanks
Foulant, repeat above step and solution in tank after dissolving is pumped into A lines after the 4 settling tank complete liquidations of A lines are clean
Standby settling tank, add ammonium sulfate NH into solution4 +Concentration is 1.2 times of vanadium, stirring, adjusts pH value of solution to 2.0~2.5,180
~210 DEG C are steam heated to (more than 95 DEG C) of boiling progress precipitations, obtained sediment ammonium poly-vanadate filtration washing post analysis into
Divide V2O5Content is 98.83%, and Upper-liquor of Precipitating Vanadate Process is filtrated to get vanadium chromium filter cake after adding reducing agent reduction, stores up, and filtrate evaporation is dense
Sheepshank crystalline substance obtains sodium sulphate.
Comparative example 1 is using conventional method cleaning acid ammonium salt precipitation foulant and reclaims vanadium therein
The serious heat exchanger tube of Xichang steel vanadium vanadium products factory precipitation process B knot dirt is disassembled into 16 pipelines, 4 works
People manually taps the method rinsed with giant, and flower 8h rinses in-tube fouling thing well, and then 4 workers enter precipitation
Tank skin foulant is tapped in tank, foulant in cleaning tank is rinsed with giant, the foulant of bulk manually need to be carried to outside tank,
The cleaning of each settling tank spends about 4h, with normally producing obtained ammonium poly-vanadate after finally the foulant cleared is dried
It is mixed into follow-up producing process, the V in foulant2O5Content is less than 95%.
Embodiment 1,2 is respectively adopted the inventive method and conventional method with comparative example 1 and acid precipitation process foulant is entered
Row cleaning and recovery, contrast is understood, can be greatlyd save time and cost of labor using the inventive method, be reclaimed obtained product
Purity is also above conventional method.
Claims (10)
1. the clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique, it is characterized in that：Use caustic dip.
2. clean method as claimed in claim 1, it is characterized in that：The foulant produces for calcification baking acidity precipitation technique
's.
3. clean method as claimed in claim 1 or 2, it is characterized in that：Contain V in the foulant2O5、SO4 +、MnO、SiO2
And Fe2O3。
4. clean method as claimed in claim 3, it is characterized in that：In the foulant containing following percentage by weight into
Point：V2O5：85~95%, SO4 +：0.8~1.3%, MnO：1.0~2.0%, SiO2：3.0~4.5%, Fe2O3：0.5~
1.0%.
5. clean method as claimed in claim 1, it is characterized in that：The alkali lye is that sodium hydroxide and/or potassium hydroxide are water-soluble
Liquid.
6. the clean method as described in claim 1 or 5, it is characterized in that：Mass fraction >=30% of alkali in the alkali lye.
7. clean method as claimed in claim 1, it is characterized in that：Steam heating is passed through during caustic dip.
8. clean method as claimed in claim 7, it is characterized in that：Steam temperature is 180~210 DEG C.
9. the recovery method of vanadium in acid precipitation foulant, it is characterized in that：Comprise the following steps：It is any according to claim 1~8
One methods described cleans foulant, collects cleaning fluid, acid precipitation, produces ammonium poly-vanadate product.
10. recovery method as claimed in claim 9, it is characterized in that：The method of the acid precipitation is：Added into cleaning fluid
Ammonium salt is to NH4 +Concentration is 1.2~2.0 times of vanadium concentration, and cleaning fluid pH is adjusted to 2.0~2.5, is heated to more than 95 DEG C, mistake
Filter, produces ammonium poly-vanadate product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711092958.8A CN107815547A (en) | 2017-11-08 | 2017-11-08 | The clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711092958.8A CN107815547A (en) | 2017-11-08 | 2017-11-08 | The clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique |
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| CN107815547A true CN107815547A (en) | 2018-03-20 |
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| CN201711092958.8A Pending CN107815547A (en) | 2017-11-08 | 2017-11-08 | The clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112808689A (en) * | 2021-01-06 | 2021-05-18 | 龙岩烟草工业有限责任公司 | Cleaning method of cigarette feeding equipment |
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| CN104388683A (en) * | 2014-12-08 | 2015-03-04 | 中南大学 | Method for separating and recycling vanadium and chromium from vanadium and chromium-containing material |
| CN106082332A (en) * | 2016-06-18 | 2016-11-09 | 湖南众鑫新材料科技股份有限公司 | A kind of ammonium metavanadate removal of impurities purifying technique |
| CN106191885A (en) * | 2016-08-12 | 2016-12-07 | 攀钢集团西昌钢钒有限公司 | Vanadium produces the processing method of equipment surface fouling |
| CN106241871A (en) * | 2016-07-15 | 2016-12-21 | 攀钢集团攀枝花钢铁研究院有限公司 | High vanadium concentrations liquid acid ammonium salt precipitation method |
| CN106987732A (en) * | 2017-04-17 | 2017-07-28 | 攀钢集团研究院有限公司 | A kind of method for separating and recovering vanadium chromium |
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2017
- 2017-11-08 CN CN201711092958.8A patent/CN107815547A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104388683A (en) * | 2014-12-08 | 2015-03-04 | 中南大学 | Method for separating and recycling vanadium and chromium from vanadium and chromium-containing material |
| CN106082332A (en) * | 2016-06-18 | 2016-11-09 | 湖南众鑫新材料科技股份有限公司 | A kind of ammonium metavanadate removal of impurities purifying technique |
| CN106241871A (en) * | 2016-07-15 | 2016-12-21 | 攀钢集团攀枝花钢铁研究院有限公司 | High vanadium concentrations liquid acid ammonium salt precipitation method |
| CN106191885A (en) * | 2016-08-12 | 2016-12-07 | 攀钢集团西昌钢钒有限公司 | Vanadium produces the processing method of equipment surface fouling |
| CN106987732A (en) * | 2017-04-17 | 2017-07-28 | 攀钢集团研究院有限公司 | A kind of method for separating and recovering vanadium chromium |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112808689A (en) * | 2021-01-06 | 2021-05-18 | 龙岩烟草工业有限责任公司 | Cleaning method of cigarette feeding equipment |
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Application publication date: 20180320 |
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