CN101709377A - Purifying and impurity-removing method of leaching solution containing vanadium - Google Patents

Purifying and impurity-removing method of leaching solution containing vanadium Download PDF

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Publication number
CN101709377A
CN101709377A CN200910250444A CN200910250444A CN101709377A CN 101709377 A CN101709377 A CN 101709377A CN 200910250444 A CN200910250444 A CN 200910250444A CN 200910250444 A CN200910250444 A CN 200910250444A CN 101709377 A CN101709377 A CN 101709377A
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vanadium
alum
impurity
vanadium leachate
purifying
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CN200910250444A
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CN101709377B (en
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邓孝伯
李大标
顾计勇
王永钢
王宗海
邓杰博
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Pangang Group Panzhihua Steel and Vanadium Co Ltd
Panzhihua New Steel and Vanadium Co Ltd
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Pangang Group Panzhihua Steel and Vanadium Co Ltd
Panzhihua New Steel and Vanadium Co Ltd
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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
    • 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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  • Manufacture And Refinement Of Metals (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention provides a purifying and impurity-removing method of a leaching solution containing vanadium, which comprises the following steps: leaching a material containing vanadium to obtain the leaching solution containing vanadium; according to the phosphorus content and the silicon content in the leaching solution containing vanadium, respectively determining the addition of magnesium sulfate and the addition of alum; heating the leaching solution containing vanadium to a certain temperature; first adding part of the alum while stirring the leaching solution containing vanadium; after a first period of time, adding the magnesium sulfate to the mixture; after a second period of time, adding the residual alum to the mixture; after reaction for a period of time, standing and precipitating the mixture; and after precipitating the mixture after reaction for a period of time, delivering the clear solution to a subsequent process of precipitation, and delivering the bottom flow to a plate frame for pressing filtration. The method can effectively control the content of silicon and phosphorus in the solution containing vanadium to below relatively low values, reduces the loss of vanadium and greatly increases the purifying yield.

Description

A kind of vanadium leachate purifying and impurity-removing method that contains
Technical field
The present invention relates to wet method vanadium extraction field, specifically, the present invention relates to a kind of vanadium leachate purifying and impurity-removing method that contains.
Background technology
Generally adopt sodium roasting-leaching-depositing technology to produce vanadium oxide both at home and abroad, in this technology, because precipitation process is had relatively high expectations to containing in the vanadium leachate foreign matter content, and is particularly higher to wherein silicon, phosphorus impurities content requirement, therefore need carry out the purification and impurity removal process to containing vanadium leachate.
Most wet method vanadium extraction producer all adopts calcium chloride to purify to contain vanadium leachate, adopt the advantage of this method to be that phosphor-removing effect is better, and the dephosphorization agent cost is low.But adopt this method exist the loss of dephosphorization underflow content of vanadium height, vanadium big, contain in the vanadium leachate shortcomings such as the silicon clearance is lower, suspended substance sedimentation difficulty.Steel is climbed by the vanadium manufacturer of domestic maximum, and to climb the vanadous oxide production technique of grand vanadium products factory be sodium roasting-water logging-acid precipitation-drying-reduction.Vanadium bearing slag behind the sodium roasting through the continuous water logging of band filter obtain to contain in the vanadium leachate suspended contamination higher, this factory adopts calcium chloride to reduce suspended substance wherein and purifies wherein phosphorus, sila matter, the calcium chloride consumption is 50～60kg/t V 2O 3, containing P＜0.015g/l in the vanadium leachate after the purification, Si is 0.5～1.8g/l, meanwhile, produce a large amount of vanadium underflow slags that contain, according to statistics, 1 ton of vanadous oxide of every production produces the 100kg underflow, the underflow slag vanadiumcontent is 10%～12%, and the process vanadium is lost in 1.4%～1.7%, and this part contains the vanadium underflow slag and adopts prior art to handle, the rate of recovery is lower, even adopt the acidleach method to reclaim, the foreign matter content in the pickling liquor is also higher, influences follow-up vanadium extraction operation.Therefore, a kind of new purifying method is adopted in expectation, with when guaranteeing decontamination effect improving and not influencing follow-up vanadium extraction operation, improves the scavenging process yield.
Summary of the invention
The objective of the invention is to solve above-mentioned problems of the prior art, and a kind of vanadium leachate purifying and impurity-removing method that contains is provided, this method can be carried out purification and impurity removal effectively to containing vanadium leachate, reduces the vanadium loss simultaneously.
The vanadium leachate purifying and impurity-removing method that contains according to the present invention may further comprise the steps: (a), the leaching contain the vanadium material, obtain containing vanadium leachate; (b), phosphorus content and silicone content come to determine respectively sal epsom add-on and alum add-on in the vanadium leachate according to containing; (c), will contain vanadium leachate and be heated to certain temperature, under agitation condition, add a part of alum earlier, after first period, add sal epsom again, after second period, add remaining alum again, staticly settle behind the reaction certain hour; (d), will behind the reacted solution sedimentation certain hour clear liquid be delivered to the precipitation subsequent handling, underflow send filter press.
In step (a), use ammonium ion concentration to leach and contain the vanadium material as the industrial water of condensation of 150mg/l～200mg/l.And the resulting vanadium concentration that contains vanadium leachate is 25g/l～30g/l, and the pH value is 8～10.
In step (b), according to containing phosphorus content in the vanadium leachate, be 2.0～2.5 to determine the sal epsom add-on, and according to containing silicone content in the vanadium leachate according to the Mg/P mass ratio, be 8～10 to determine the alum add-on according to alum/silicon mass ratio.
In step (c), will contain 80 ℃～85 ℃ of vanadium leachate heating.And described first period is 10min～20min, and described second period is 10min～20min.In addition, the amount of a part of alum that adds is about 90% (weight) earlier, and the amount of the remaining alum that the back adds is about 10% (weight).
In step (d), with reacted solution sedimentation 10min～15min.
Compared with prior art, the present invention has the following advantages:
(1) because utilize alum to purify silicon in the basic solution earlier, utilizes again to contain finite concentration NH 4 +Industrial water of condensation and magnesium salts purify dephosphorization, so avoided the loss of bigger vanadium.And then utilize alum flocculation dephosphorization postprecipitation thing, and the solution settling time is short, good purification, and this process has been avoided the introducing of chlorion, has alleviated the system pipeline corrosion phenomenon to a certain extent.
(2) silicone content and the phosphorus content in the vanadium solution of containing after purifying can be controlled at 0.05g/l respectively effectively, below the 0.015g/l, and in scavenging process the vanadium loss be reduced to below 0.8% (weight), improved the purification yield greatly.
Advantages such as (3) the present invention contains vanadium leachate applicable to the water logging behind sodium roasting, and goes for phosphorus, the silicon of different concns, and it is simple to have a technological operation, and purification process is stable, and the clarification time is short.
Embodiment
Below with reference to embodiment the present invention is done to describe in further detail, but the invention is not restricted to the description of following examples.
Specifically, the vanadium leachate purifying and impurity-removing method that contains of the present invention may further comprise the steps:
(a), use ammonium ion concentration to leach to contain the vanadium material as the industrial water of condensation of 150mg/l～200mg/l, obtain vanadium concentration and be 25g/l～30g/l and pH value and be 8～10 and contain vanadium leachate;
(b), according to containing phosphorus content in the vanadium leachate, be 2.0～2.5 to determine the sal epsom add-on according to the Mg/P mass ratio, and according to containing silicone content in the vanadium leachate, be 8～10 to determine the alum add-on according to alum/silicon mass ratio;
(c), will contain vanadium leachate and be heated to 80 ℃～85 ℃, under agitation condition, add the alum of about 90% (weight) earlier, through behind 10min～15min, add sal epsom again, through behind 10min～15min, add remaining alum again, staticly settle behind reaction 15min～20min;
(d), will behind reacted solution sedimentation 10min～15min clear liquid be delivered to the precipitation subsequent handling, underflow send filter press.
In step step (c), the chemical equation that relates to is as follows:
KAl(SO 4) 2·12H 2O+Na 2SiO 3→Al 2(SiO 3) 3↓+K 2SO 4+Na 2SO 4+12H 2O
Mg 2++NH 4 ++PO 4 3++6H 2O→Mg?NH 4PO 4·6H 2O↓
Be exemplary embodiment of the present invention below.
Embodiment 1
Get 1000ml by NH 4 +Concentration be 156mg/l the leaching of industrial water of condensation contain vanadium leachate, vanadium concentration is 28.05g/l, pH value 9.5, P content is 0.065g/l, Si content is 1.06g/l, and the sal epsom consumption is 0.81g (a Mg/P mass ratio 2.5), and the alum consumption is 9.54g (alum/Si mass ratio 9), after being heated to 85 ℃, under agitation condition, add 8.59g alum, add 0.81g sal epsom behind the reaction 15min, add 0.95g alum behind the 15min, stop to stir behind the reaction 15min, leave standstill 13min, the throw out natural subsidence, with underflow (promptly, throw out) send filter press, obtain V content and be 27.84g/l, P content is 0.009g/l, Si content be 0.03g/l contain the vanadium clear liquid, the loss of process vanadium is 0.75%, and purifying yield is 99.25%.
Embodiment 2
Get 1000ml by NH 4 +Concentration be 186mg/l the leaching of industrial water of condensation contain vanadium leachate, vanadium concentration is 26.82g/l, pH value 9, P content is 0.059g/l, Si content is 1.42g/l, the sal epsom consumption is 0.64g (a Mg/P mass ratio 2.2), and the alum consumption is 11.36g (alum/Si mass ratio 8), be heated to 80 ℃ after, under agitation condition, add 10.22g alum, add 0.64g sal epsom behind the 12min, add 1.14g alum behind the 10min, stop to stir behind the reaction 10min, leave standstill 15min, the throw out natural subsidence is sent filter press with underflow, and obtaining V content is 26.68g/l, P content is 0.008g/l, Si content be 0.04g/l contain the vanadium clear liquid, the loss of process vanadium is 0.52%, purifying yield is 99.48%.
Embodiment 3
Get 1000ml by NH 4 +Concentration is the vanadium leachate that contains of 179mg/l industry water of condensation leaching, vanadium concentration is 29.42g/l, pH value 10, P content is 0.061g/l, Si content is 0.98g/l, the sal epsom consumption is 0.61g (a Mg/P mass ratio 2), and the alum consumption is 9.80g (alum/Si mass ratio 10), be heated to 83 ℃ after, under agitation condition, add 8.82g alum, add 0.61g sal epsom behind the 10min, add 0.98g alum behind the 13min, stop to stir behind the reaction 13min, leave standstill 10min, the throw out natural subsidence is sent filter press with underflow, and obtaining V content is 29.22g/l, P content is 0.011g/l, Si content be 0.03g/l contain the vanadium clear liquid, the loss of process vanadium is 0.68%, purifying yield is 99.32%.
Embodiment 4
Get 1000ml by NH 4 +Concentration is the vanadium leachate that contains of 150mg/l industry water of condensation leaching, vanadium concentration is 25g/l, pH value 10, P content is 0.063g/l, Si content is 1.03g/l, the sal epsom consumption is 0.63g (a Mg/P mass ratio 2), and the alum consumption is 10.30g (alum/Si mass ratio 10), be heated to 85 ℃ after, under agitation condition, add 9.27g alum, add 0.63g sal epsom behind the 13min, add 1.03g alum behind the 15min, stop to stir behind the reaction 10min, leave standstill 15min, the throw out natural subsidence is sent filter press with underflow, and obtaining V content is 24.85g/l, P content is 0.012g/l, Si content be 0.04g/l contain the vanadium clear liquid, the loss of process vanadium is 0.6%, purifying yield is 99.4%.
Embodiment 5
Getting 1000ml is the vanadium leachate that contains of 200mg/l industry water of condensation leaching by NH4+ concentration, vanadium concentration is 30g/l, pH value 10, P content is 0.058g/l, Si content is 0.95g/l, the sal epsom consumption is 0.67g (a Mg/P mass ratio 2.3), and the alum consumption is 8.55g (alum/Si mass ratio 9), be heated to 80 ℃ after, under agitation condition, add 7.70g alum, add 0.67g sal epsom behind the 10min, add 0.85g alum behind the 15min, stop to stir behind the reaction 10min, leave standstill 10min, the throw out natural subsidence is sent filter press with underflow, and obtaining V content is 29.78g/l, P content is 0.007g/l, Si content be 0.05g/l contain the vanadium clear liquid, the loss of process vanadium is 0.73%, purifying yield is 99.27%.
Advantage of the present invention is the vanadium loss that can avoid bigger, and avoids introducing chlorion in decontamination process, thereby has alleviated the system pipeline corrosion phenomenon. The advantages such as in addition, it is simple that the present invention has technological operation, and stable and clarification time of process for purifying is short.

Claims (10)

1. one kind contains the vanadium leachate purifying and impurity-removing method, it is characterized in that may further comprise the steps:
A, leaching contain the vanadium material, obtain containing vanadium leachate;
B, phosphorus content and silicone content come to determine respectively sal epsom add-on and alum add-on in the vanadium leachate according to containing;
C, will contain vanadium leachate and be heated to certain temperature, under agitation condition, add a part of alum earlier, after first period, add sal epsom again, after second period, add remaining alum again, staticly settle behind the reaction certain hour.
D, with behind the reacted solution sedimentation certain hour clear liquid being delivered to the precipitation subsequent handling, underflow is carried out press filtration.
2. the vanadium leachate purifying and impurity-removing method that contains according to claim 1 is characterized in that, uses ammonium ion concentration to leach as the industrial water of condensation of 150mg/l～200mg/l and contains the vanadium material.
3. the vanadium leachate purifying and impurity-removing method that contains according to claim 2 is characterized in that, the described vanadium concentration that contains vanadium leachate is 25g/l～30g/l, and the pH value is 8～10.
4. the vanadium leachate purifying and impurity-removing method that contains according to claim 1 is characterized in that, according to containing phosphorus content in the vanadium leachate, is 2.0～2.5 to determine the sal epsom add-on according to the Mg/P mass ratio.
5. the vanadium leachate purifying and impurity-removing method that contains according to claim 1 is characterized in that, according to the silicone content that contains in the vanadium leachate, is 8～10 to determine the alum add-on according to alum/silicon mass ratio.
6. the vanadium leachate purifying and impurity-removing method that contains according to claim 1 is characterized in that, in step c, will contain 80 ℃～85 ℃ of vanadium leachate heating.
7. the vanadium leachate purifying and impurity-removing method that contains according to claim 1 is characterized in that, described first period is 10min～20min, and described second period is 10min～20min.
8. the vanadium leachate purifying and impurity-removing method that contains according to claim 1 is characterized in that, the amount of a part of alum that adds is 90% (weight) earlier, and the amount of the remaining alum that the back adds is 10% (weight).
9. the vanadium leachate purifying and impurity-removing method that contains according to claim 1 is characterized in that, in step c, the reaction times is 15min～20min.
10. the vanadium leachate purifying and impurity-removing method that contains according to claim 1 is characterized in that, with reacted solution sedimentation 10min～15min.
CN200910250444XA 2009-12-09 2009-12-09 Purifying and impurity-removing method of leaching solution containing vanadium Active CN101709377B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102242282A (en) * 2011-07-05 2011-11-16 舒宏庆 Alkaline reduction smelting method for vanadium polymetallic ore
CN102337410A (en) * 2011-10-19 2012-02-01 攀钢集团攀枝花钢铁研究院有限公司 Method for recycling vanadium from dephosphorization base flow residues
CN103014378A (en) * 2011-09-21 2013-04-03 攀钢集团攀枝花钢铁研究院有限公司 Vanadium liquid purification method
CN103014377A (en) * 2011-09-21 2013-04-03 攀钢集团攀枝花钢铁研究院有限公司 Vanadium liquid purification method

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102242282A (en) * 2011-07-05 2011-11-16 舒宏庆 Alkaline reduction smelting method for vanadium polymetallic ore
CN102242282B (en) * 2011-07-05 2014-01-22 舒宏庆 Alkaline reduction smelting method for vanadium polymetallic ore
CN103014378A (en) * 2011-09-21 2013-04-03 攀钢集团攀枝花钢铁研究院有限公司 Vanadium liquid purification method
CN103014377A (en) * 2011-09-21 2013-04-03 攀钢集团攀枝花钢铁研究院有限公司 Vanadium liquid purification method
CN102337410A (en) * 2011-10-19 2012-02-01 攀钢集团攀枝花钢铁研究院有限公司 Method for recycling vanadium from dephosphorization base flow residues

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