CN102191388B - Process for extracting vanadium from stone coal through two-section curing with concentrated acid - Google Patents
Process for extracting vanadium from stone coal through two-section curing with concentrated acid Download PDFInfo
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- CN102191388B CN102191388B CN2011100512364A CN201110051236A CN102191388B CN 102191388 B CN102191388 B CN 102191388B CN 2011100512364 A CN2011100512364 A CN 2011100512364A CN 201110051236 A CN201110051236 A CN 201110051236A CN 102191388 B CN102191388 B CN 102191388B
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Abstract
The invention relates to a process for extracting vanadium from stone coal through two-section curing with concentrated acid. The process flow mainly comprises the following steps of: a), adding concentrated sulfuric acid into the vanadium-containing stone coal, and uniformly stirring; b), performing one-section curing on the mixture of the concentrated sulfuric acid and the vanadium-containing stone coal at the temperature of at least 50 DEG C; and c), performing second-section curing on the mixture subjected to the one-section curing at the temperature of at least 100 DEG C. The process has high conversion rate, saves mineral resources and has high adaptability.
Description
Technical field
The present invention relates to extraction process of vanadium in a kind of bone coal, particularly relate to a kind of employing vitriol oil two-stage curing technique and extract Vanadium Pentoxide in FLAKES from bone coal.
Background technology
Bone coal is a kind of high rotten sapropelinite or algal coal.Be formed at the early proterozoic era and Eopaleozoic, mostly have high ash, high-sulfur, lower calorific value and the large characteristics of hardness.Its composition also has silicon oxide, calcium oxide and a small amount of ferric oxide, aluminum oxide and magnesium oxide etc. except containing organic carbon.
Bone coal has various classification.Press ash content and thermal value, can be divided into general bone coal and high-quality bone coal: the ash content of general bone coal is 40%～90%, and thermal value is below 16.7 thousand J/gs; The ash content of high-quality bone coal is 20%～40%, and thermal value is 16.7～27.1 thousand J/gs.By structure, structure, can be divided into lump stone coal, granular bone coal, flakey bone coal and powdery bone coal.Press the primary and secondary of bone coal Minerals impurity, be divided into siliceous bone coal, calcareous bone coal etc.
Because the Rock coal containing alum resource reserve is huge, the technique of extracting Vanadium Pentoxide in FLAKES from bone coal is the emphasis of present extracting vanadium from stone coal industry common concern.Domestic extracting vanadium from stone coal adopts salt adding Roasting And Leaching technique for a long time, valuable metal low conversion rate (generally being no more than 55%), and energy consumption is high, and environmental pollution is serious; Since the last century the nineties, many enterprises explore direct acidleach, alkali soaking technology, but V
2O
5The rate of recovery is not high (generally only having 40%～60%), and the transformation efficiency that difficulty is soaked the ore deposit is lower, and the problem of the wasting of resources, environmental pollution still fundamentally is not resolved.
This shows, existing process for extracting vanadium from stone coal obviously exists obvious technological deficiency and environmental pollution, demands urgently being improved.The problem that exists in order to solve extracting vanadium from stone coal, many relevant enterprises fall over each other to develop the extracting vanadium from stone coal novel process, but up to the present have no real clean environment firendly, extracting vanadium from stone coal novel process that the valuable metal transformation efficiency is high is used for suitability for industrialized production.Therefore, developing a kind of energy-conserving and environment-protective, the valuable metal transformation efficiency is high, resource can be fully used extracting vanadium from stone coal novel process, is common aspiration and the task of top priority of extracting vanadium from stone coal industry.
Summary of the invention
Main purpose of the present invention is, overcome the technological deficiency that the extracting vanadium from stone coal traditional technology exists, for the extracting vanadium from stone coal industry provides a kind of brand-new technique, novel process technical problem to be solved guarantees the extracting vanadium from stone coal clean environment firendly exactly, the valuable metal transformation efficiency is high, energy consumption is low, and resource can be fully used, and novel process should have stronger adaptability.
The approach of the object of the invention to solve the technical problems is achieved by the following technical solution.According to a kind of concentrated acid two-stage curing process for extracting vanadium from stone coal that the present invention proposes, this technical process mainly comprises step: a, and the vitriol oil is joined in Rock coal containing alum, stirs; B, with the vitriol oil and Rock coal containing alum mixture at least 50 ℃ of next section slakings; C carries out two-stage curing under the material after one section slaking is placed at least 100 ℃.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal also will add entry in wherein said a step, controls liquid-solid ratio and is at least 0.5.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal also comprises in wherein said a step adding leaching agent.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal, wherein said leaching agent are that strong oxide compound and ammonium salt class material form by cooperation in 1: 1.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal, wherein said strong oxide compound is potassium permanganate, sodium chlorate, hydrogen peroxide, potassium bichromate, cobaltic fluoride.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal, wherein said ammonium salt are ammonium sulfate, ammonium persulphate, ammonium nitrate, volatile salt, ammonium iodide.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal, wherein said leaching agent add-on are 0.1%～3% of a step gained ore pulp weight.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal, the temperature of wherein said one section slaking are 50-70 ℃, and the curing time is 0.5-10 hour.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal, the temperature of wherein said two-stage curing are 100-150 ℃, and the curing time is at least 0.5 hour.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal also comprises c step gained being contained the vanadium solid moltenly soaks, solid-liquid separation, obtains to contain the step of vanadium leachate.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal, the described molten step of soaking is to add water-soluble soaking in c step gained contains the vanadium solid, stirs at least 1 hour more than 50 ℃.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal comprises that also vanadium leachate is purified, settling step with containing.
Aforesaid concentrated acid two-stage curing process for extracting vanadium from stone coal also comprises the step of precipitated solid being calcined pyrolysis.
The present invention compared with prior art has obvious advantage and unusual effect.By technique scheme, the present invention has following advantages and effect at least:
1, certain temperature and humidity are controlled in one section slaking, make acid accumulator penetration mineral aggregate particle deep by etch and internal diffusion effect, allow ore particle be moistened by acidleach fully, participate in oxidizing reaction.
2, two-stage curing makes system reach needed temperature, strengthens the oxidizing reaction of concentrated acid, impels Low Valent Vanadium transform and finally leached to the high price vanadium, improves leaching effect, and the leaching yield of difficult navajoite stone is reached more than 80%.The leaching yield of general ore can reach more than 90%, and is even higher.
3, the use of leaching agent can reduce leaching condition, further improves the transformation efficiency of valuable metal.
In sum, concentrated acid two-stage curing process for extracting vanadium from stone coal of the present invention has significant progress technically, has obvious positively effect, is really a new and innovative, progressive, practical new design.
Above-mentioned explanation is only the general introduction of technical solution of the present invention, for can clearer understanding technique means of the present invention, and can be implemented according to the content of specification sheets, and for above and other purpose of the present invention, feature and advantage can be become apparent, below especially exemplified by preferred embodiment, and the cooperation accompanying drawing, be described in detail as follows.
Description of drawings
The schematic flow sheet of Fig. 1 concentrated acid two-stage curing process for extracting vanadium from stone coal of the present invention.
Embodiment
Reach for further setting forth the present invention technique means and the effect that predetermined goal of the invention is taked, below in conjunction with accompanying drawing and preferred embodiment, to its embodiment of concentrated acid two-stage curing process for extracting vanadium from stone coal, method, step, feature and effect thereof, be described in detail as follows.
Accompanying drawing 1 is the present invention's's " concentrated acid two-stage curing process for extracting vanadium from stone coal " schematic flow sheet.This technical process mainly comprises:
A joins the vitriol oil in Rock coal containing alum, stirs;
B, the vitriol oil and Rock coal containing alum mixture is standing under at least 50 ℃, complete one section slaking;
C, the mixture after one section slaking is standing under at least 100 ℃, complete two-stage curing, obtain containing the vanadium solid.
In above-mentioned a step, the described vitriol oil refers to concentration greater than the sulfuric acid of 3mol/L, and its add-on is with H
2SO
4Meter is at least 17% of bone coal weight.This step also will add entry, controls liquid-solid ratio and is at least 0.5.Liquid-solid ratio of the present invention refers to the ratio of the weight of the volume of liquid and solid.
The present invention adopts with V (II), V (III) valence state and composes the long-pending bone coal that contains of depositing, and adopts conventional Ginding process, is ground into greater than 20 purpose fineves as pulverizer, ball mill etc., and preferred size is between the 20-200 order.
Also comprise the step that adds leaching agent in above-mentioned a step.This leaching agent is that strong oxide compound and ammonium salt class material coordinate by weight and form at 1: 1.Strong oxide compound used can be but be not limited to potassium permanganate, sodium chlorate, hydrogen peroxide, potassium bichromate, cobaltic fluoride, and ammonium salt class material used can be but be not limited to ammonium sulfate, ammonium persulphate, ammonium nitrate, volatile salt, ammonium iodide.The add-on of this leaching agent is 0.1%～3% of ore pulp weight, preferred 0.1%～1%.The use of this leaching agent can reduce leaching condition, further improves the transformation efficiency of valuable metal.
In above-mentioned b step, one section slaking will be completed under higher than the condition of 50 ℃ in temperature, and preferred temperature range is 50-70 ℃.The humidity of this section slaking preferably remains at least 60%, and preferred humidity range is 60-90%.Adopt in the present invention conventional temperature, the temperature and humidity in humidity measuring apparatus detection reaction process, and adopt ordinary method to control temperature and humidity.
The time of one section slaking remains on 0.5-10 hour, and different according to temperature, the time of one section slaking can change.Along with temperature raises, the time of required one section slaking decreases.The effect of one section slaking is by etch and internal diffusion, makes acid accumulator penetration mineral aggregate particle deep, allows ore particle be moistened by acidleach fully, is conducive to mineral and all participates in oxidizing reaction.
In above-mentioned c step, two-stage curing will be completed under higher than the condition of 100 ℃ in temperature, and preferred temperature range is 100-150 ℃.Adopt in the present invention the temperature in conventional temperature measuring set detection reaction process, and adopt conventional method to control temperature.
The time of two-stage curing is wanted more than 0.5 hour at least, and different according to temperature, the time of two-stage curing can change.Along with temperature raises, the time of required two-stage curing decreases.The effect of this two-stage curing is the oxidizing reaction of strengthening concentrated acid, impels Low Valent Vanadium transform and finally leached to the high price vanadium, improves leaching effect.
The use of leaching agent can reduce leaching condition, further improves the transformation efficiency of valuable metal.
Concentrated acid two-stage curing process for extracting vanadium from stone coal of the present invention also comprises:
D contains c step gained that the vanadium solid moltenly soaks, solid-liquid separation, obtains to contain vanadium leachate;
E will contain vanadium leachate and purify, precipitates, and obtain many vanadic acid ammonia;
F obtains V with many vanadic acid ammonia calcining pyrolysis
2O
5Product.
In above-mentioned d step, adopt water will contain vanadium solid molten soaking more than 50 ℃, standing, preferred more than 1 hour, obtain being dissolved with blue solution and the solid residue of vanadium sulfate acyl this moment.Adopt conventional solid-liquid separation means as filtering, obtain leach liquor.
In the e step, the method such as to take to extract the leach liquor that obtains is purified, extraction liquid used can be P204, then adds oxygenant such as hydrogen peroxide in the solution after extraction, through oxidation precipitation, obtains many vanadic acid ammonia.In the f step, the many vanadic acid ammonia that obtains more than 0.5 hour, is obtained V in calcining more than 400 ℃
2O
5Product.V
2O
5The quality of product can adopt conventional X fluorescent instrument to measure and obtain.
Below in conjunction with preferred embodiment, concrete technology parameter of the present invention is made a detailed description.
Embodiment 1
Adopt the normal experiment method, record as X fluorescent instrument that in the present embodiment bone coal used, the vanadium grade is 0.89%.
Above-mentioned bone coal 100g is levigate to greater than 60 orders, admix consumption and be 23% concentration and be 98% sulfuric acid.Add entry, controlling liquid-solid ratio is 0.5, stirs.50 ℃ of next section slakings 1 hour; 120 ℃ of lower two-stage curings 1.5 hours.Adding solid-to-liquid ratio in the solid that obtains after two-stage curing is the water of 2: 1, and then molten soaking 1 hour under 70 ℃, filter, and acid warm water washing obtains to contain vanadium leachate and soak slag.
Titration concentration is the l ferrous ammonium sulfate solution of 4g/L in containing vanadium leachate, according to the routine analysis chemical calculation method, records V leaching rate, and acquired results sees Table 1.
Embodiment 2
Bone coal 100g that will be identical with embodiment 1 is levigate to greater than 60 orders, admixes consumption and be 17% concentration and be 98% sulfuric acid.Add entry, controlling liquid-solid ratio is 0.5, stirs.50 ℃ of next section slakings 1 hour; 120 ℃ of lower two-stage curings 1.5 hours.Adding solid-to-liquid ratio in the solid that obtains after two-stage curing is the water of 2: 1, and then molten soaking 1 hour under 70 ℃, filter, and acid warm water washing obtains to contain vanadium leachate and soak slag.
Adopt the ferrous ammonium sulfate titration as embodiment 1, record V leaching rate, acquired results sees Table 1.
Embodiment 3
Bone coal 100g that will be identical with embodiment 1 is levigate to greater than 60 orders, admixes consumption and be 23% concentration and be 98% sulfuric acid.Add entry, controlling liquid-solid ratio is 0.5, stirs.70 ℃ of next section slakings 1 hour; 100 ℃ of lower two-stage curings 3 hours.Adding solid-to-liquid ratio in the solid that obtains after two-stage curing is the water of 2: 1, and then molten soaking 1 hour under 70 ℃, filter, and acid warm water washing obtains to contain vanadium leachate and soak slag.
Adopt the ferrous ammonium sulfate titration as embodiment 1, record V leaching rate, acquired results sees Table 1.
Embodiment 4
Bone coal 100g that will be identical with embodiment 1 is levigate to greater than 60 orders, admixes consumption and be 23% concentration and be 98% sulfuric acid.Add entry, controlling liquid-solid ratio is 0.5, stirs.70 ℃ of next section slakings 1 hour; 150 ℃ of lower two-stage curings 1.5 hours.Adding solid-to-liquid ratio in the solid that obtains after two-stage curing is the water of 2: 1, and then molten soaking 1 hour under 70 ℃, filter, and acid warm water washing obtains to contain vanadium leachate and soak slag.
Adopt the ferrous ammonium sulfate titration as embodiment 1, record V leaching rate, acquired results sees Table 1.
Table 1
Comparative example 1 and 2 can find out the increase along with sour consumption, and the leaching yield of vanadium improves greatly.Comparative example 1, embodiment 3 and embodiment 4 can find out the raising along with curing temperature, can greatly shorten the curing time, improve the leaching yield of vanadium.
Embodiment 5
The present embodiment adopts and rams the husky ore deposit of mixing, and adopting the normal experiment method to record the vanadium grade is 1.02%.The present embodiment is divided into three groups of experiments A, B and C, only investigates the variation that adds V leaching rate after leaching agent.
A organizes experiment: above-mentioned bone coal 500g is levigate to greater than 60 orders, admix consumption and be 23% concentration and be 98% sulfuric acid.Add entry, controlling liquid-solid ratio is 0.86.Molten soaking 12 hours and 21 hours respectively under 95 ℃ filtered, and acid warm water washing obtains to contain vanadium leachate and soak slag.
B organizes experiment: above-mentioned bone coal 500g is levigate to greater than 60 orders, admix consumption and be 23% concentration and be 98% sulfuric acid.Add entry, controlling liquid-solid ratio is 0.86, adds the leaching agent 1 (potassium permanganate and ammonium sulfate join at 1: 1 according to weight) of ore pulp volume 1%.Molten soaking 12 hours and 21 hours respectively under 95 ℃ filtered, and acid warm water washing obtains to contain vanadium leachate and soak slag.
C organizes experiment: above-mentioned bone coal 500g is levigate to greater than 60 orders, admix consumption and be 23% sulfuric acid.Add entry, controlling liquid-solid ratio is 0.86, adds the leaching agent 2 (sodium chlorate and ammonium persulphate join at 1: 1 according to weight) of ore pulp volume 1%.Molten soaking 12 hours and 21 hours respectively under 95 ℃ filtered, and acid warm water washing obtains to contain vanadium leachate and soak slag.
Adopt the ferrous ammonium sulfate titration as above-mentioned embodiment, can record the V leaching rate in leach liquor, the results are shown in Table 2.
Table 2
Can be found out by above data, after adding leaching agent, V leaching rate significantly improves.
the above, it is only preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, although the present invention discloses as above with preferred embodiment, yet be not to limit the present invention, any those skilled in the art, within not breaking away from the technical solution of the present invention scope, when the technology contents that can utilize above-mentioned announcement is made a little change or is modified to the equivalent embodiment of equivalent variations, in every case be not break away from the technical solution of the present invention content, any simple modification that foundation technical spirit of the present invention is done above embodiment, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (13)
1. concentrated acid two-stage curing process for extracting vanadium from stone coal, this technical process mainly comprises step:
A joins the vitriol oil in Rock coal containing alum, stirs;
B, with the vitriol oil and Rock coal containing alum mixture 50 ℃～70 ℃ next section slakings;
C carries out two-stage curing with the mixture after one section slaking under 100 ℃～150 ℃.
2. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 1, is characterized in that also will adding entry in wherein said a step, controls liquid-solid ratio and be at least 0.5.
3. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 1, is characterized in that also comprising in wherein said a step adding leaching agent.
4. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 3 is characterized in that wherein said leaching agent is that strong oxide compound and ammonium salt class material coordinate by weight and form at 1: 1.
5. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 4, is characterized in that wherein said strong oxide compound is potassium permanganate, sodium chlorate, hydrogen peroxide, potassium bichromate, cobaltic fluoride.
6. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 4, is characterized in that wherein said ammonium salt is ammonium sulfate, ammonium persulphate, ammonium nitrate, volatile salt, ammonium iodide.
7. the described concentrated acid two-stage curing process for extracting vanadium from stone coal of any one claim according to claim 3-4, is characterized in that wherein said leaching agent add-on is 0.1%～3% of a step gained ore pulp weight.
8. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 1, is characterized in that wherein said one period curing time is 0.5-10 hour.
9. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 1, is characterized in that the wherein said two-stage curing time is at least 0.5 hour.
10. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 1 characterized by further comprising and c step gained contained the vanadium solid moltenly soaks, solid-liquid separation, obtains to contain the step of vanadium leachate.
11. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 10 is characterized in that the described molten step of soaking is to add entry in c step gained contains the vanadium solid, stirs at least 1 hour more than 50 ℃.
12. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 1 characterized by further comprising and will contain vanadium leachate purification, settling step.
13. concentrated acid two-stage curing process for extracting vanadium from stone coal according to claim 1 characterized by further comprising the step of precipitated solid being calcined pyrolysis.
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| CN201010117557.5 | 2010-03-04 | ||
| CN2010101175575A CN101921912A (en) | 2010-03-04 | 2010-03-04 | Concentrated acid two-stage curing-gas liquid cyclic vanadium extraction process from stone coal |
| CN2011100512364A CN102191388B (en) | 2010-03-04 | 2011-03-03 | Process for extracting vanadium from stone coal through two-section curing with concentrated acid |
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| CN102391904A (en) * | 2011-10-10 | 2012-03-28 | 郑峰 | Technology for increasing value of stone coal and extracting valuable metal elements |
| CN102732736B (en) * | 2012-07-23 | 2015-01-14 | 中南大学 | Method for extracting vanadium from burning slag of stone coal vanadium mine fluidized bed |
| CN102912144A (en) * | 2012-09-12 | 2013-02-06 | 北京矿冶研究总院 | Method for leaching vanadium pentoxide from vanadium-containing soot |
| CN103290215B (en) * | 2013-06-17 | 2015-05-20 | 长沙矿冶研究院有限责任公司 | Method for curing and leaching reinforced stone coal navajoite concentrated acid |
| CN104451202B (en) * | 2014-11-21 | 2017-04-12 | 长沙矿冶研究院有限责任公司 | Two-stage curing vanadium extraction method of stone coal vanadium ores |
| CN104451201B (en) * | 2014-11-21 | 2017-04-12 | 长沙矿冶研究院有限责任公司 | Two-grade curing vanadium extraction method for stone coal vanadium ores |
| CN104388683B (en) * | 2014-12-08 | 2017-02-22 | 中南大学 | Method for separating and recycling vanadium and chromium from vanadium and chromium-containing material |
| CN104911357A (en) * | 2015-05-05 | 2015-09-16 | 徐强富 | Method for normal temperature and pressure whole-wet leaching of toxic elements in mining and metallurgical solid waste |
| CN105039746A (en) * | 2015-08-28 | 2015-11-11 | 长沙矿冶研究院有限责任公司 | Method for directly extracting high-purity vanadium pentoxide from stone coal vanadium ore |
| CN106350668B (en) * | 2016-09-13 | 2017-12-08 | 武汉轻工大学 | A kind of Rock coal containing alum water vapour charing pretreatment prepares V2O5Method |
| CN106435177A (en) * | 2016-12-05 | 2017-02-22 | 武汉科技大学 | Method for leaching vanadium from vanadium-containing stone coal |
| CN109112324A (en) * | 2018-09-03 | 2019-01-01 | 四川省有色冶金研究院有限公司 | It is a kind of to leach the method for efficiently strengthening V leaching rate in bone coal in activation |
| CN109207720B (en) * | 2018-11-14 | 2019-12-24 | 南华大学 | Leaching method for extracting vanadium from stone coal |
| CN110284013B (en) * | 2019-07-30 | 2023-08-29 | 中国科学院过程工程研究所 | Stone coal vanadium ore curing production equipment and stone coal vanadium ore curing production method |
| CN115354173A (en) * | 2022-08-08 | 2022-11-18 | 北京天瑞利达投资发展有限公司 | Stone coal concentrated acid two-stage curing vanadium extraction process |
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| CN101921912A (en) | 2010-12-22 |
| CN102191388A (en) | 2011-09-21 |
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