CN103290219A - Impurity removing method of leached solution of mixing roasted stone coal vanadium ore - Google Patents
Impurity removing method of leached solution of mixing roasted stone coal vanadium ore Download PDFInfo
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- CN103290219A CN103290219A CN2012100406213A CN201210040621A CN103290219A CN 103290219 A CN103290219 A CN 103290219A CN 2012100406213 A CN2012100406213 A CN 2012100406213A CN 201210040621 A CN201210040621 A CN 201210040621A CN 103290219 A CN103290219 A CN 103290219A
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Abstract
The invention discloses an impurity removing method of leached solution of mixing roasted stone coal vanadium ore. The method comprises the following steps: a mixture of the stone coal vanadium ore and clay vanadium ore is taken as raw material; the mixture is roasted and leached to obtain the leached solution containing vanadium; the leached solution containing vanadium and hydrogen peroxide are added into a container with a molar ratio of the vanadium of the leachedsolution to the hydrogen peroxide at a range of 1:2 to 1:9, and are stirred; an auxiliary agent is added to adjust the pH value to 5 or more after stirring; the solution is stirred again after the adjustment of the pH value; and then slag and water are separated after stirring. The auxiliary agent is ammonium bicarbonate or sodium bicarbonate or a mixture of them. Hydrogen peroxide and ammonium bicarbonate (or sodium bicarbonate ) which are relatively cheap are employed in the method to remove cations, such as iron and aluminium ions, from the solution. The advantages of the method of the invention are that: the agents are easy to obtain, and are relatively cheap, so that the impurity removing method is low in cost; the method is easy to operate, and the loss of the vanadium is easy to control; energy consumption is decreased because that the impurity is removed at normal temperature; the loss rate of the vanadium of the vanadium-contained solution is relatively low, and the loss rate can be reduced to 1.5 to 2.5%.
Description
Technical field
The invention belongs to the bone coal navajoite field of smelting, particularly bone coal navajoite torrefaction ore deposit infusion solution removal of impurities.
Background technology
The technology of current extracting vanadium from stone coal mainly is: raw ore pulverizing-balling-up-roasting-leaching-vanadium enrichment-precipitation.Wherein, the mixing ore deposit of bone coal navajoite and clay navajoite is through roasting, leaching operation, and gained contains has a lot of metallic impurity (as Fe in the vanadium infusion solution
3+, Al
3+), the removal of impurities that contains the vanadium infusion solution just becomes an important procedure of vanadium extraction.At present, the method for bone coal navajoite torrefaction ore deposit infusion solution removal of impurities is a lot, but the rate of loss of vanadium is generally higher in the technology removal of impurities process of prior art.The method of utilizing hydrogen peroxide and cupferron associating removal of impurities that people such as professor Zhang Yiming of Wuhan University of Technology propose, the low energy of rate of loss reaches 10%; The soda ash removal of impurities is used in the vanadium solution removal of impurities that contains of Flos Bombacis Malabarici iron and steel group vanadium smelting project, and its rate of loss reaches more than 15%; Hunan nonferrous metallurgy research institute uses soda ash, the removal of impurities of sodium hydroxide pyrosol, and the primary purification slag is through the high temperature alkali dissolution liquid drip washing more than three times, and the vanadium rate of loss can reach about 2%.There is following deficiency in the impurity-removing method that above-mentioned three tame units propose:
1) the removal of impurities cost is higher, and cupferron is relatively more expensive;
2) use the soda ash removal of impurities merely, its rate of loss is higher;
3) high temperature alkali dissolution liquid need provide heat, and energy consumption is higher;
4) the closed cycle impurity removal process is complicated, needs large-scale equipment in the actual production.
Summary of the invention
The object of the present invention is to provide a kind of simple, production cost is lower, the vanadium rate of loss is lower impurity-removing method that contains the vanadium infusion solution.
With hereinafter except indicating all concentration of mentioning and ratio be concentration expressed in percentage by weight or weight ratio.
Technical program of the present invention lies in: be raw material with bone coal navajoite, clay navajoite mixture, through roasting, leaching, must contain the vanadium infusion solution, in container, add and contain vanadium infusion solution and hydrogen peroxide, containing in the vanadium infusion solution vanadium is 1:2 ~ 1:9 with adding hydrogen peroxide molar weight ratio, stirs 10min ~ 2h; Stir and finish back adding auxiliary agent regulator solution pH 〉=5; Solution stirring 10min ~ 2h behind the adjusting pH; Leave standstill 10min ~ 3h after stirring end, separate pulp water.
Described auxiliary agent is bicarbonate of ammonia or sodium bicarbonate, or its mixture of two kinds.
The described temperature of reaction that contains vanadium infusion solution and hydrogen peroxide is: 2 ~ 90 ℃.
The method of described separation pulp water is filtration, ion-exchange absorption, realizes that pulp water separates.
Design philosophy of the present invention is to precipitate according to process for extracting vanadium a large amount of quadrivalent ion in the removal of impurities process, thereby caused the bigger situation of vanadium loss in the removal of impurities process, adopted the combination of the cheap hydrogen peroxide of price comparison and bicarbonate of ammonia (or sodium bicarbonate) to remove positively charged ions such as iron, aluminium in the infusion solution of bone coal navajoite torrefaction ore deposit.Namely add the lower ion of valence state in this solution of hydrogen peroxide oxidation in the vanadium infusion solution to containing; Vanadic acid radical ion complexing in negative oxygen ion and the solution has stoped the vanadic acid radical ion to precipitate in the pH change procedure simultaneously.Stirred two effects among the present invention: the one, make the abundant oxidation of ion at a low price, the 2nd, reduce because precipitating throwing out to containing the sedimentation of sweeping along of vanadium ion.The impurity that the present invention mainly removes is cation impurity and ultrafine particle, as Fe
3+, Al
3+Deng.
Compared with prior art, advantage of the present invention is:
(1) medicament is obtained easily, and price is relatively cheap, and whole removal of impurities cost is lower;
(2) simple to operate, be easy to control the vanadium loss;
(3) carry out removal of impurities at normal temperatures, cut down the consumption of energy;
(4) it is lower to contain in the vanadium solution rate of loss of vanadium, and its rate of loss can be reduced to 1.5 ~ 2.5%.
Embodiment
Use somewhere, Hubei Province bone coal navajoite and clay navajoite baking mixed, the roasted ore extract technology is: the leaching solid-to-liquid ratio is 1:1 ~ 1.8, adds 1 ~ 2% the vitriol oil (it is 2 ~ 2.5 that assurance contains vanadium infusion solution pH).Get and contain the vanadium infusion solution and test.
Embodiment 1
Get 13.73L and contain the vanadium infusion solution and test, the vanadium concentration that contains that contains the vanadium infusion solution is 3.10g/L; Add the 210ml hydrogen peroxide in this infusion solution, the concentration of hydrogen peroxide is 30%, contains that vanadium is 1:5 with the hydrogen peroxide molar weight ratio that adds hydrogen peroxide in the vanadium infusion solution, stirs 20min; Stir finishing the back and slowly add bicarbonate of ammonia in solution, measure the pH value of solution value while stirring, is 7 to stop to add to pH; Continue to stir 30min; Leave standstill 30min after stirring end; Filter, make solution 13.75L, concentration is 3.02g/L; Carry out ion-exchange absorption, precipitation, deamination get V2O5.Experimental result sees Table 1.
Embodiment 2
Get 5.1L and contain vanadium leachate and test, the vanadium concentration that contains that contains the vanadium infusion solution is 2.69g/L; Add 27ml hydrogen peroxide (concentration is 30%) in this solution, contain that vanadium is 1:2 with the hydrogen peroxide molar weight ratio that adds hydrogen peroxide in the vanadium infusion solution, stir 20min; Stir finishing the back and slowly add bicarbonate of ammonia in solution, measure the pH value of solution value while stirring, is 7 to stop to add to pH; Continue to stir 30min; Leave standstill 30min after stirring end; Filter, make solution 5.04L, concentration is 2.678g/L; Carry out ion-exchange absorption, precipitation, deamination get V2O5.Experimental result sees Table 1.
Embodiment 3
Get 5.05L and contain vanadium leachate and test, the vanadium concentration that contains that contains the vanadium infusion solution is 2.87g/L; Add 99.8ml hydrogen peroxide (concentration is 30%) in this solution, contain that vanadium is 1:7 with the hydrogen peroxide molar weight ratio that adds hydrogen peroxide in the vanadium infusion solution, stir 20min; Stir finishing the back and slowly add bicarbonate of ammonia in solution, measure the pH value of solution value while stirring, is 7 to stop to add to pH; Continue to stir 30min; Leave standstill 30min after stirring end; Filter, make solution 5.11L, concentration is 2.84g/L; Carry out ion-exchange absorption, precipitation, deamination get V2O5.Experimental result sees Table 1.
Embodiment 4
Get 3.64L and contain vanadium leachate and test, the vanadium concentration that contains that contains the vanadium infusion solution is 3.26g/L; Add 58.4ml hydrogen peroxide (concentration is 30%) in this solution, contain that vanadium is 1:5 with the hydrogen peroxide molar weight ratio that adds hydrogen peroxide in the vanadium infusion solution, stir 20min; Stir finishing the back and slowly add sodium bicarbonate in solution, measure the pH value of solution value while stirring, is 7 to stop to add to pH; Continue to stir 30min; Leave standstill 30min after stirring end; Filter, make solution 3.62L, concentration is 3.28g/L; Carry out ion-exchange absorption, precipitation, deamination get V2O5.Experimental result sees Table 1.
Table 1 testing data
Can be known that by the data in the table 1 take method removal of impurities of the present invention, the rate of loss of vanadium can be controlled between 1.5 ~ 2.5% in the vanadium solution.Wherein the add-on of hydrogen peroxide according to bone coal and the baking mixed mineral reductibility of clay navajoite compound what and in the data area of claim, fluctuate: it is more big to mix in the ore deposit bone coal ratio, and the hydrogen peroxide add-on is more big.
Claims (4)
1. the impurity-removing method of the infusion solution of a bone coal navajoite after baking mixed is characterized in that: get and contain vanadium infusion solution and hydrogen peroxide, contain that vanadium and hydrogen peroxide molar weight ratio are 1:2 ~ 1:9 in the vanadium infusion solution, stir 10min ~ 2h; Stir and finish back adding auxiliary agent regulator solution pH 〉=5; Solution stirring 10min ~ 2h behind the adjusting pH; Leave standstill 10min ~ 3h after stirring end, separate pulp water.
2. the impurity-removing method of the infusion solution after baking mixed according to the described bone coal navajoite of claim 1, it is characterized in that: described auxiliary agent is bicarbonate of ammonia or sodium bicarbonate, or its mixture of two kinds.
3. the impurity-removing method of the infusion solution after baking mixed according to the described bone coal navajoite of claim 1, it is characterized in that: the described temperature of reaction that contains vanadium infusion solution and hydrogen peroxide is: 2 ~ 90 ℃.
4. the impurity-removing method of the infusion solution after baking mixed according to the described bone coal navajoite of claim 1 is characterized in that: the method for described separation pulp water for filter, ion-exchange absorption.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103484673A (en) * | 2013-09-13 | 2014-01-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for vadaium precipitation from balck acid leaching vanadium liquid |
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|---|---|---|---|---|
| WO2001062989A1 (en) * | 2000-02-22 | 2001-08-30 | Anaconda Nickel Ltd | Method for the recovery of nickel and/or cobalt |
| US20070007878A1 (en) * | 2003-12-17 | 2007-01-11 | Outokumpu Technology Oy | Method of recycling an exhausted selenium filter mass |
| CN101050014A (en) * | 2007-04-27 | 2007-10-10 | 遵义钛业股份有限公司 | Method for treating wastewater containing copper and vanadium |
| CN101838749A (en) * | 2010-06-10 | 2010-09-22 | 中南大学 | Ion exchange extraction vanadium method of vanadium-containing solution |
| CN101760651B (en) * | 2010-03-04 | 2011-04-27 | 中南大学 | Process for extracting vanadium by acid leaching of stone coal |
-
2012
- 2012-02-22 CN CN2012100406213A patent/CN103290219A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001062989A1 (en) * | 2000-02-22 | 2001-08-30 | Anaconda Nickel Ltd | Method for the recovery of nickel and/or cobalt |
| US20070007878A1 (en) * | 2003-12-17 | 2007-01-11 | Outokumpu Technology Oy | Method of recycling an exhausted selenium filter mass |
| CN101050014A (en) * | 2007-04-27 | 2007-10-10 | 遵义钛业股份有限公司 | Method for treating wastewater containing copper and vanadium |
| CN101760651B (en) * | 2010-03-04 | 2011-04-27 | 中南大学 | Process for extracting vanadium by acid leaching of stone coal |
| CN101838749A (en) * | 2010-06-10 | 2010-09-22 | 中南大学 | Ion exchange extraction vanadium method of vanadium-containing solution |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103484673A (en) * | 2013-09-13 | 2014-01-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for vadaium precipitation from balck acid leaching vanadium liquid |
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Application publication date: 20130911 |