CN104532009A - Vanadium extraction method of high-calcium and high-phosphor vanadium slag clinker - Google Patents

Vanadium extraction method of high-calcium and high-phosphor vanadium slag clinker Download PDF

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CN104532009A
CN104532009A CN201410789986.5A CN201410789986A CN104532009A CN 104532009 A CN104532009 A CN 104532009A CN 201410789986 A CN201410789986 A CN 201410789986A CN 104532009 A CN104532009 A CN 104532009A
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vanadium
phosphor
calcium
leaching
grog
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宋文臣
李宏
王艳南
王耀
冯佳
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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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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Abstract

The invention provides a vanadium extraction method of a high-calcium and high-phosphor vanadium slag clinker. The method comprises the following steps: crushing, grinding and screening the high-calcium and high-phosphor vanadium slag clinker with greater than 7wt% of CaO and greater than 0.6wt% of P2O5 until the particle size is 0.050-0.154mm, wherein the mass ratio of CaO to V2O5 is greater than 0.7, then carrying out carbonation leaching in a Na2O3 solution with a concentration of 3-20wt% or a NaHCO3 solution with a concentration of 4-25wt%, wherein a solid-liquid ratio is 1:1mL/g-1:15mL/g, the leaching temperature is 50-99 DEG C, the leaching time is 30-120 minutes and the stirring rate is higher than 150 revolutions per minute during leaching; carrying out solid-liquid separation to obtain a vanadium-containing leaching liquid; and then preparing a vanadium product by using the existing mature process of precipitating vanadium and deaminizing. According to the method, the leaching operation process is simple; a leaching agent is low in cost; a high vanadium leaching rate can be achieved; the leaching of phosphor in the vanadium slag clinker can be avoided; and the effective vanadium extraction of the high-calcium and high-phosphor vanadium slag clinker can be implemented.

Description

A kind of extraction vanadium method of vanadium-bearing slag of high calcium and high phosphor grog
Technical field
The invention belongs to rare metal wet underwater welding field, particularly relate to a kind of method of vanadium extraction from vanadium-bearing slag of high calcium and high phosphor grog.
Background technology
Phosphorus is containing the harmful element in vanadium leachate acid ammonium salt precipitation, and it can form stable and complicated complex compound phosphorus vanadium system's heteropolyacid and their salt with vanadium in acidic medium, in addition, also can form FePO with the iron ion in solution and aluminum ion 4, AlPO 4precipitation, these all can pollute ammonium vanadate precipitation, have a strong impact on the carrying out of acid ammonium salt precipitation.Conventional dephosphorization means be regulator solution pH between 9.5 ~ 11.0, then add appropriate calcium salt or magnesium salts forms calcium phosphate precipitation, the leach liquor P concentration <0.015g/L after general requirement dephosphorization.
Vanadium-bearing hot metal obtains vanadium slag and half steel through bessemerizing.In order to alleviate the burden of semi-steel dephosphorizing, can add lime carries out pre-dephosphorization to vanadium-bearing hot metal blowing vanadium slag simultaneously, obtains the special vanadium slag of low-phosphorous half steel and high calcium high phosphorus.This vanadium slag obtains vanadium-bearing slag of high calcium and high phosphor grog after pyrogenic process oxide treatment.If carry out acidic solution leaching to grog, a large amount of calcium and phosphorus can be made together to enter into leach liquor along with vanadium, owing to there being the existence of a large amount of calcium ion in solution, regulator solution pH can again form calcium vanadate precipitation between 9.5 ~ 11.0, so can not adopt the dephosphorizing method under traditional alkaline condition, and the dephosphorization problem under acid system is not yet captured.
Though have the carbonating mentioning vanadium-bearing slag of high calcium and high phosphor to leach in the production method of a patent documentation CN103914611 barium oxide, but it does not do clear description to phosphorus content, unclear to the concept understanding of vanadium-bearing slag of high calcium and high phosphor.The vanadium-bearing slag of high calcium and high phosphor grog of its research is obtained by roasting after common vanadium slag and lime or Wingdale mixing, above says it is a kind of high calcium vanadium slag or the low-phosphorous vanadium slag of high calcium so strict.
Patent documentation CN103397209 provides a kind of extraction vanadium method of vanadium-bearing slag of high calcium and high phosphor, first activated by concentrated hydrochloric acid and remove most calcium and phosphorus, again calcification baking-acid-leaching vanadium-extracted is carried out to low-phosphorous low calcium vanadium slag after solid-liquid separation, ironic hydroxide and calcium chloride can also be reclaimed from liquid phase.But concentrated hydrochloric acid activation is equivalent to adds additional a procedure, and has harsh requirement to equipment and operating environment.
Summary of the invention
For the deficiency that prior art exists, the object of this invention is to provide the extraction vanadium method that a kind of vanadium-bearing slag of high calcium and high phosphor grog carbonating leaches, present method makes the vanadium in vanadium-bearing slag of high calcium and high phosphor grog enter into solution comparatively completely, control that phosphorus is as far as possible few enters solution simultaneously, thus reaching the Selectively leaching of vanadium and phosphorus, the leach liquor obtained is conducive to preparing highly purified vanadium product.
Technical solution of the present invention is: a kind of extraction vanadium method of vanadium-bearing slag of high calcium and high phosphor grog, joins in carbonic acid soln and leaches, utilize the concentration of three kinds of calcium salts to amass Ca after being divided by vanadium-bearing slag of high calcium and high phosphor chamotte crushing mill dusting cover 3(VO 4) 2> CaCO 3>Ca 3(PO 4) 2character, selectively vanadium is leached into solution from grog and stops phosphorus to enter solution, leach and terminate rear solid-liquid separation and obtain containing vanadium leachate, then obtain vanadium product after precipitation and deamination process.
Further, described vanadium-bearing slag of high calcium and high phosphor grog can be obtained by vanadium-bearing slag of high calcium and high phosphor sinter process, also can obtain the direct high temperature oxidation of molten state vanadium-bearing slag of high calcium and high phosphor just going out converter;
Further, in described vanadium-bearing slag of high calcium and high phosphor grog w(CaO) >7%, CaO/V 2o 5mass ratio >0.7, w(P 2o 5) >0.6%, granularity is between 0.050 mm ~ 0.154 mm.
Further, described carbonic acid soln is concentration is 3 wt% ~ 20 wthe Na of t% 2cO 3solution or concentration are 4 wt% ~ 25 wt% NaHCO 3solution, solid-to-liquid ratio is 1:1-15mL/g, extraction temperature 50 DEG C ~ 99 DEG C, extraction time 30 ~ 120min, stirring velocity >150 r/ min;
Further, leach and terminate filtered while hot, the residue temperature after filtration is the concentration of 50 DEG C ~ 99 DEG C is 1 wt% ~ 10 wthe Na of t% 2cO 3or NaHCO 3solution washing 1 ~ 3 time, washings joins in leach liquor.
Compared with prior art, the invention provides a kind of extraction vanadium method of vanadium-bearing slag of high calcium and high phosphor grog, can realize the Selectively leaching of vanadium and phosphorus in vanadium-bearing slag of high calcium and high phosphor grog, the leaching yield of vanadium is greater than 85%, and the leaching yield of phosphorus is less than 10%.Carbonic acid leaching agent Na of the present invention 2cO 3and NaHCO 3low price, environmental pollution is little, is a kind of vanadium extraction means of low cost.
Embodiment
The present invention proposes a kind of extraction vanadium method of vanadium-bearing slag of high calcium and high phosphor grog, the basis of being intended to ensure that vanadium leaches controls the leaching of impurity element particularly phosphorus.
The present invention adopts Na to vanadium-bearing slag of high calcium and high phosphor grog 2cO 3or NaHCO 3solution leaches, and comprises the following steps:
a. will w(CaO) >7%, CaO/V 2o 5mass ratio >0.7, w(P 2o 5) the vanadium-bearing slag of high calcium and high phosphor chamotte crushing of >0.6% is levigate and sieve.
b. the vanadium-bearing slag of high calcium and high phosphor grog after screening is joined Na 2cO 3or NaHCO 3solution leaches.
c. leach and terminate rear filtered while hot, residue Na 2cO 3or NaHCO 3solution washing 1 ~ 3 time, wash water joins in leach liquor.
d. leach liquor is by obtaining vanadium product after purification, precipitation and deamination.
Wherein, aforesaid operations step adescribed in vanadium-bearing slag of high calcium and high phosphor grog, can be obtained by vanadium-bearing slag of high calcium and high phosphor sinter process, also can the direct high temperature oxidation of molten state vanadium-bearing slag of high calcium and high phosphor just going out converter be obtained.
Wherein, aforesaid operations step agranularity after middle vanadium-bearing slag of high calcium and high phosphor chamotte crushing is at 0.050 mm ~ 0.154 mm, and within the scope of this, the leaching yield of the less vanadium of granularity is higher.
Wherein, aforesaid operations step bin, leaching process control carbonic acid soln is concentration is 3 wt% ~ 20 wthe Na of t% 2cO 3solution or concentration are 4 wt% ~ 25 wt% NaHCO 3solution, preferred solid-to-liquid ratio is 1:1mL/g ~ 1:15 mL/g, extraction temperature 50 DEG C ~ 99 DEG C, extraction time 30 min ~ 120min, stirring velocity >150 r/ min.Preferably 10 wthe Na of t% 2cO 3solution lives 12.5 wthe NaHCO of t% 3solution, solid-to-liquid ratio 1:5mL/g, extraction temperature 95 DEG C, extraction time 90min, stirring velocity 150 r/ min.
Wherein, aforesaid operations step cin, leaching after terminating will filtered while hot as early as possible, and residue is with 50 DEG C ~ 99 DEG C 1 wt% ~ 10 wthe Na of t% 2cO 3or NaHCO 3solution washing 1 ~ 3 time, wash water joins in leach liquor.Preferably 90 DEG C 5 wt% Na 2cO 3or NaHCO 3solution washing 2 times.
Wherein, aforesaid operations step ddescribed in purification, the technology such as precipitation and deamination be all this research field technology known by the technical staff.
Be described further the specific embodiment of the present invention below by embodiment, example is only used to help and understands the present invention, and should not be considered as limitation of the present invention.
embodiment 1
The vanadium-bearing slag of high calcium and high phosphor grog produced by certain vanadium extraction steelworks domestic is (containing CaO13.71 wt%, V 2o 513.93 wt %, P 2o 50.80 wt%) pulverizing and jevigating, get the following screen underflow 10g of 100 order, granularity meets 100% <0.15mm.
The Na that 100mL concentration is 10wt% is added in 250mL Erlenmeyer flask 2cO 3solution, joins in solution by 10g vanadium-bearing slag of high calcium and high phosphor grog, and bottleneck puts rubber plug and not jam-pack, and then put in the water bath with thermostatic control magnetic agitation water-bath of 95 DEG C, setting stirring velocity is 200 r/ min, the time is 30min.
Reaction terminates rear horse back while hot by filtration devices, and residue is with 5 wthe Na of t% concentration 2cO 3solution carries out washing 2 times, joins in 250mL volumetric flask, use deionized water constant volume after wash water and leach liquor mixing.Detect the content of vanadium and phosphorus in constant volume liquid.The leaching yield of vanadium is 90.15%, and the leaching yield of phosphorus is 5.50%.
embodiment 2
The vanadium-bearing slag of high calcium and high phosphor grog produced by certain vanadium extraction steelworks domestic is (containing CaO 13.71 wt%, V 2o 513.93 wt%, P 2o 50.80 wt%) pulverizing and jevigating, get the following screen underflow 10g of 100 order, granularity meets 100% <0.15mm.
In 250mL Erlenmeyer flask, add 100mL concentration is 12.5 wthe NaHCO of t% 3solution, joins in solution by 10g vanadium-bearing slag of high calcium and high phosphor grog, and bottleneck puts rubber plug and not jam-pack, and then put in the water bath with thermostatic control magnetic agitation water-bath of 95 DEG C, setting stirring velocity is 150 r/ min, the time is 60min.
Reaction terminates rear horse back while hot by filtration devices, the residue NaHCO of 5wt% concentration 3solution carries out washing 2 times, joins in 250mL volumetric flask, use deionized water constant volume after wash water and leach liquor mixing.Detect the content of vanadium and phosphorus in constant volume liquid.The leaching yield of vanadium is 91.23%, and the leaching yield of phosphorus is 5.78%.
embodiment 3
By chemical reagent autogamy vanadium-bearing slag of high calcium and high phosphor, be obtained by reacting vanadium-bearing slag of high calcium and high phosphor grog through melt oxidation (containing CaO 20.12 wt%, V 2o 511.44 wt%, P 2o 50.52 wt%).
After chamotte crushing is levigate, get the following screen underflow 10g of 100 order, granularity meets 100%<0.15mm.In 250mL Erlenmeyer flask, add 100mL concentration is 12.5 wthe NaHCO of t% 3solution, joins in solution by 10g vanadium-bearing slag of high calcium and high phosphor grog, and bottleneck puts rubber plug and not jam-pack, and then put in the water bath with thermostatic control magnetic agitation water-bath of 95 DEG C, setting stirring velocity is 250 r/ min, starts clock reaction 90min.
Reaction terminates rear horse back while hot by filtration devices, and residue is with 5 wthe NaHCO of t% concentration 3solution carries out washing 2 times, joins in 250mL volumetric flask, use deionized water constant volume after wash water and leach liquor mixing.Detect the content of vanadium and phosphorus in constant volume liquid.The leaching yield of vanadium is 88.64%, and the leaching yield of phosphorus is 7.56%.
Leach liquor adds 1g/LCaCl 2carry out acid ammonium salt precipitation after the further dephosphorization of solution, silica removal and obtain ammonium poly-vanadate, ammonium poly-vanadate obtains Vanadium Pentoxide in FLAKES product after 500 DEG C of deaminations, grade 98.62%.
embodiment 4
The vanadium-bearing slag of high calcium and high phosphor grog produced by certain vanadium extraction steelworks domestic is (containing CaO 11.59 wt%, V 2o 514.02 wt%, P 2o 50.65 wt%) pulverizing and jevigating, get the following screen underflow 10g of 100 order, granularity meets 100% <0.15mm.
In 250mL Erlenmeyer flask, add 100mL concentration is 20 wthe NaHCO of t% 3solution, joins in solution by 10g vanadium-bearing slag of high calcium and high phosphor grog, and bottleneck puts rubber plug and not jam-pack, and then put in the water bath with thermostatic control magnetic agitation water-bath of 95 DEG C, setting stirring velocity is 200 r/ min, the time is 120.
Reaction terminates rear horse back while hot by filtration devices, the residue NaHCO of 20wt% concentration 3solution carries out washing 2 times, joins in 250mL volumetric flask, use deionized water constant volume after wash water and leach liquor mixing.Detect the content of vanadium and phosphorus in constant volume liquid.The leaching yield of vanadium is 93.45%, and the leaching yield of phosphorus is 4.94%.
embodiment 5
By chemical reagent autogamy vanadium-bearing slag of high calcium and high phosphor, be obtained by reacting vanadium-bearing slag of high calcium and high phosphor grog through melt oxidation (containing CaO18.75 wt%, V 2o 512.55 wt%, P 2o 50.72 wt%).
After chamotte crushing is levigate, get the following screen underflow 10g of 100 order, granularity meets 100%<0.15mm.In 250mL Erlenmeyer flask, add 100mL concentration is 20 wthe NaCO of t% 3solution, joins in solution by 10g vanadium-bearing slag of high calcium and high phosphor grog, and bottleneck puts rubber plug and not jam-pack, and then put in the water bath with thermostatic control magnetic agitation water-bath of 95 DEG C, setting stirring velocity is 300 r/ min, starts clock reaction 50min.
Reaction terminates rear horse back while hot by filtration devices, and residue is with 10 wthe NaHCO of t% concentration 3solution carries out washing 2 times, joins in 250mL volumetric flask, use deionized water constant volume after wash water and leach liquor mixing.Detect the content of vanadium and phosphorus in constant volume liquid.The leaching yield of vanadium is 89.98%, and the leaching yield of phosphorus is 6.36%.

Claims (4)

1. an extraction vanadium method for vanadium-bearing slag of high calcium and high phosphor grog, is characterized in that: specifically comprise the following steps:
Step 1: by thin for vanadium-bearing slag of high calcium and high phosphor chamotte crushing mill sieve size 0.050 mm ~ 0.154 mm, for subsequent use;
Step 2: leach adding a certain amount of carbonic acid soln in grog after fragmentation, extraction temperature is 50 DEG C ~ 99 DEG C, time 30 ~ 120min, stirring velocity >150 r/ min, leaches and terminates filtered while hot, obtains containing vanadium leachate after solid-liquid separation; Wherein, the solid-to-liquid ratio of described vanadium-bearing slag of high calcium and high phosphor grog and carbonic acid soln is 1:1-15mL/g;
Step 3: leach liquor is obtained vanadium product by precipitation and deamination technique, the leaching yield of vanadium is more than 88%, and the leaching yield of phosphorus is more than 5%.
2. the extraction vanadium method of vanadium-bearing slag of high calcium and high phosphor grog according to claim 1, is characterized in that: in the vanadium-bearing slag of high calcium and high phosphor grog in described step 1 w(CaO) >7%, CaO/V 2o 5mass ratio >0.7, w(P 2o 5) >0.6%.
3. the extraction vanadium method of vanadium-bearing slag of high calcium and high phosphor grog according to claim 1, is characterized in that: the carbonic acid soln in described step 2 is concentration is 3 wt% ~ 20 wthe Na of t% 2cO 3solution or concentration are 4 wt% ~ 25 wt% NaHCO 3solution.
4. the extraction vanadium method of vanadium-bearing slag of high calcium and high phosphor grog according to claim 1, is characterized in that: the method following steps: the concentration being 50 DEG C ~ 99 DEG C by the residue temperature after filtration is 1 wt% ~ 10 wthe Na of t% 2cO 3or NaHCO 3solution washing 1 ~ 3 time, washings joins in leach liquor.
CN201410789986.5A 2014-12-19 2014-12-19 Vanadium extraction method of high-calcium and high-phosphor vanadium slag clinker Pending CN104532009A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106834725A (en) * 2017-03-31 2017-06-13 江苏省冶金设计院有限公司 The system and method for processing vanadium chromium slag
CN106868312A (en) * 2017-03-31 2017-06-20 江苏省冶金设计院有限公司 The system and method for processing converter vanadium chromium slag
CN106868311A (en) * 2017-03-31 2017-06-20 江苏省冶金设计院有限公司 The system and method for processing converter vanadium chromium slag
CN106978544A (en) * 2017-03-31 2017-07-25 江苏省冶金设计院有限公司 The system and method for handling converter vanadium chromium slag
CN110106344A (en) * 2019-06-24 2019-08-09 攀钢集团研究院有限公司 Vanadium slag carbonating leaches cleaning extraction vanadium method
CN111647758A (en) * 2020-06-12 2020-09-11 攀钢集团研究院有限公司 Method for pretreating and dephosphorizing high-phosphorus vanadium slag

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106834725A (en) * 2017-03-31 2017-06-13 江苏省冶金设计院有限公司 The system and method for processing vanadium chromium slag
CN106868312A (en) * 2017-03-31 2017-06-20 江苏省冶金设计院有限公司 The system and method for processing converter vanadium chromium slag
CN106868311A (en) * 2017-03-31 2017-06-20 江苏省冶金设计院有限公司 The system and method for processing converter vanadium chromium slag
CN106978544A (en) * 2017-03-31 2017-07-25 江苏省冶金设计院有限公司 The system and method for handling converter vanadium chromium slag
CN110106344A (en) * 2019-06-24 2019-08-09 攀钢集团研究院有限公司 Vanadium slag carbonating leaches cleaning extraction vanadium method
WO2020259500A1 (en) * 2019-06-24 2020-12-30 攀钢集团研究院有限公司 Method for clean vanadium extraction by carbonation leaching of vanadium slag
CN111647758A (en) * 2020-06-12 2020-09-11 攀钢集团研究院有限公司 Method for pretreating and dephosphorizing high-phosphorus vanadium slag
CN111647758B (en) * 2020-06-12 2022-06-03 攀钢集团研究院有限公司 Method for pretreating and dephosphorizing high-phosphorus vanadium slag

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