CN103276227A - Method for extracting vanadium from vanadium-titanium magnetite concentrates - Google Patents
Method for extracting vanadium from vanadium-titanium magnetite concentrates Download PDFInfo
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Abstract
The invention belongs to the field of hydrometallurgy and in particular relates to a method for extracting vanadium from vanadium-titanium magnetite concentrates. The method comprises the following steps of: 1) carrying out acid dissolution and leaching on vanadium-titanium magnetite concentrates and hydrochloric acid at 100-150 DEG C, and filtering the solution to obtain an acid leaching solution; 2) calcining the acid leaching solution obtained in the step 1) to obtain an iron-vanadium solid material and hydrochloric acid; 3) putting the iron-vanadium solid material obtained in the step 2) in an alkali solution, and stirring, filtering and washing to obtain an iron-containing solid material and a vanadium-containing alkali solution; and 4) evaporating and concentrating the vanadium-containing alkali solution obtained in the step 3), then repeating the step 3), and carrying out cooling crystallization to extract a vanadate crystal when the concentration of vanadate in the alkali solution is 10-30g/L. The method has the advantages that the problems of high energy consumption caused by multiple high-temperature roasting in a method for extracting vanadium through sodium (calcium) roasting, three-waste pollution caused in the roasting processes and the like are avoided; and the recovery rate of vanadium is greatly increased.
Description
Technical field
The invention belongs to the hydrometallurgy field, particularly, the present invention relates to a kind of method of from v-ti magnetite concentrate, extracting vanadium.
Background technology
Vanadium titano-magnetite is that the great characteristic polymetallic ore of China produces resource, and reserves are huge, and many metals symbiosis such as vanadium, titanium, iron, chromium, and comprehensive utilization of resources is worth very high.China's proven reserve surpasses 10,000,000,000 tons, and prospective reserves reaches more than 30,000,000,000 tons, mainly is distributed in Sichuan Panxi Diqu, Chengde and area, Chaoyang.Pan Xi is China's vanadium and titanium resources area of enrichment the most, and existing explored vanadium titano-magnetite prospective reserves surpasses 10,000,000,000 tons, and retained reserve is 67.3 hundred million tons, wherein contains vanadium (V
2O
5) 1,475 ten thousand tons, titanium (TiO
2) 5.93 hundred million tons, account for 63% and 90.5% of national vanadium, titanium reserves respectively, apportion third place in the world and first.The Chengde has been verified 3.57 hundred million tons of vanadium titano-magnetite resource reserves, 75.59 hundred million tons of ultra-poor vanadium titano-magnetite stock numbers.
Obtain iron ore concentrate and ilmenite concentrate after the vanadium titano-magnetite ore dressing separates, the v-ti magnetite iron ore concentrate adopts blast-furnace smelting to carry iron and vanadium, and existing with the iron and steel be the tradition of guiding smelt and the processing technology resource utilization on the low side, the rate of recovery of vanadium≤47%, serious waste of resources.In existing blast furnace ironmaking-converter steelmaking process for extracting vanadium, vanadium enters iron phase, and the spinel structure that forms vanadium iron in the vanadium extraction by converter blowing process enters slag and forms vanadium slag mutually.At present, the existing sodium roasting technology of vanadium slag is comparatively ripe, but the vanadium extraction process needs 850 ℃ of repeatedly roastings of high temperature, the energy consumption height, and the three-waste pollution that produces in the roasting process is serious.Calcification baking-acid-leaching vanadium-extracted as a kind of process for extracting vanadium of cleaning has been subjected to extensive concern.Different with the sodium vanadium extraction, vanadium slag calcareous raw material lime, Wingdale, rhombspar etc. are as the additive roasting, making vanadium be converted into vanadic acid calcium leaches with diluted acid or alkaline solution again, vanadium in the leach liquor reclaims with hydrolysis precipitation method or ion exchange method, calcification baking can be avoided the chlorine pollution of traditional sodium roasting, but vanadium transformation efficiency less than 80% still under the prior art condition, the total yield that causes vanadium is less than 50% still.Can find out that to sum up the existing method of extracting vanadium from v-ti magnetite concentrate is based on high temperature pyrogenic process process, energy consumption is higher, and the rate of recovery of vanadium is lower.
The present invention utilizes Wet-process metallurgy method to handle v-ti magnetite concentrate, adopts salt acid treatment vanadium titano-magnetite concentrate, makes vanadium iron separate with titanium, uses alkaline purification to separate vanadium and iron then.
Summary of the invention
The objective of the invention is at extracting the technology of vanadium from v-ti magnetite concentrate at present, there are shortcomings such as vanadium recovery is low, energy consumption is high, environmental pollution is serious, a kind of cleaning-efficient method of extracting vanadium from v-ti magnetite concentrate is provided, has industrial operation, advantages of environment protection simultaneously.
The method of extracting vanadium from v-ti magnetite concentrate of the present invention may further comprise the steps:
1) v-ti magnetite concentrate and hydrochloric acid are carried out sour molten leaching under 100～150 ℃, filter and obtain pickling liquor, wherein, 1～10 hour reaction times;
2) pickling liquor that step 1) is obtained is calcined, and obtains ferrovanadium solid material and hydrochloric acid;
3) with step 2) the ferrovanadium solid material that obtains places alkaline solution, is 80～160 ℃ of following insulated and stirred 0.5～5 hour in temperature, filters, washing, and obtain iron content solid material and contain the vanadium alkaline solution;
4) step 3) is obtained to contain the evaporation of vanadium alkaline solution, concentrate after, repeating step 3), when treating that vanadate concentration is 10～30g/L in the alkaline solution, crystallisation by cooling is isolated vanadate crystal, further Processing of Preparation ammonium meta-vanadate or Vanadium Pentoxide in FLAKES.
The present invention proposes the direct leaching vanadium titanium magnet ore concentrate of hydrochloric acid separation of iron, vanadium and titanium, re-uses the method that the molten technology of calcining, alkali is extracted vanadium, and hydrochloric acid acid-leaching reaction efficient height can efficiently leach iron, vanadium, and pickling liquor calcining, alkali are molten, obtain the vanadium product after the aftertreatment.The Wet-process metallurgy method of working conditions gentleness of the present invention is handled v-ti magnetite concentrate and is extracted vanadium, flow process is short, energy consumption is low, and the vanadium recovery height has solved traditional blast furnace-converter process energy consumption height, facility investment greatly and vanadium slag sodium roasting technology vanadium extraction yield is low, energy consumption big, pollution heavily waits a difficult problem.
According to the method for extracting vanadium from v-ti magnetite concentrate of the present invention, the liquid-solid ratio of the molten leaching reaction of the described acid of step 1) is 1:1～10:1.
According to the method for extracting vanadium from v-ti magnetite concentrate of the present invention, the mass percent concentration of the described hydrochloric acid of step 1) is 10%～36%.
According to the method for from v-ti magnetite concentrate, extracting vanadium of the present invention, it is characterized in that step 2) 200～800 ℃ of preferred temperature of described calcining, calcination time is 1～5 hour.
According to the method for from v-ti magnetite concentrate, extracting vanadium of the present invention, step 2) hydrochloric acid that obtains can be used for the leaching of the v-ti magnetite concentrate of step 1).
According to the method for extracting vanadium from v-ti magnetite concentrate of the present invention, the liquid-solid ratio of the described alkaline solution of step 3) and ferrovanadium solid material is 0.5:1～20:1.
According to the method for extracting vanadium from v-ti magnetite concentrate of the present invention, the described alkaline solution of step 3) is preferably sodium hydroxide or potassium hydroxide solution.Therefore, be that the vanadate of step 4) gained is vanadic acid sodium or potassium vanadate when alkaline solution uses sodium hydroxide or potassium hydroxide solution.
According to the method for from v-ti magnetite concentrate, extracting vanadium of the present invention, above-mentioned steps 3) described alkaline solution mass percent concentration is 20%～80%.
According to the method for extracting vanadium from v-ti magnetite concentrate of the present invention, the iron content solid material that step 3) obtains can be used as iron-smelting raw material and carries out subsequent disposal.
According to the method for extracting vanadium from v-ti magnetite concentrate of the present invention, the described method for preparing ammonium meta-vanadate or Vanadium Pentoxide in FLAKES of step 4) is preferably the conventional precipitator method.Namely vanadate is dissolved in water, utilizes ammonium salt precipitation preparation ammonium meta-vanadate, then calcining preparation Vanadium Pentoxide in FLAKES.
The invention has the advantages that:
(1) the present invention extracts the method for vanadium from v-ti magnetite concentrate, has avoided the repeatedly roasting of sodium (calcium) roasting vanadium-extracting method high temperature, the energy consumption height, and problems such as the three-waste pollution that produces in the roasting process, the rate of recovery of vanadium increases greatly.
(2) alkali circulation of the present invention and sour circulating technology greatly reduce production energy consumption, do not add any auxiliary material, and no dust waste gas can not cause the pollution of environment.
(3) rate of recovery of vanadium in the v-ti magnetite concentrate of the present invention〉85%.
(4) method of the present invention is not only applicable to v-ti magnetite concentrate, more is applicable to the v-ti magnetite concentrate of high vanadium titanium low iron content.
Embodiment
Embodiment 1
(1) mass content of raw material v-ti magnetite concentrate main component: TFe is 42.97%, TiO
2Mass content be 28.74%, V
2O
5Mass content be 1.23%, v-ti magnetite concentrate is levigate to-200 orders 80%;
(2) with levigate v-ti magnetite concentrate and 10% mixed in hydrochloric acid, liquid-solid ratio is 10:1, leaches 5 hours down at 150 ℃, obtains pickling liquor;
(3) pickling liquor that step (2) is obtained obtains ferrovanadium solid material and hydrochloric acid 300 ℃ of calcinings down, and hydrochloric acid returns the leaching for v-ti magnetite concentrate;
(4) to place mass concentration be 20% sodium hydroxide solution to the ferrovanadium solid material that step (3) is obtained, liquid-solid ratio is 20:1, be 150 ℃ of following insulated and stirred 5 hours in temperature, filter, washing, obtain Vanadium Pentoxide in FLAKES mass content＜0.05% iron content solid material and contain the alkaline solution of vanadium;
(5) step (4) is obtained contain vanadium the alkaline solution evaporation, to be concentrated into the sodium hydroxide mass concentration be 20%, repeating step (4), when treating that vanadic acid sodium concentration is 10～30g/L in the alkaline solution, crystallisation by cooling is isolated the vanadic acid sodium crystal;
(6) the vanadic acid sodium crystal that step (8) is obtained is further handled (being specially the conventional precipitator method), can obtain purity and be 99.5% Vanadium Pentoxide in FLAKES, and the rate of recovery of vanadium is 88.5% in the v-ti magnetite concentrate.
Embodiment 2
(1) mass content of raw material v-ti magnetite concentrate main component: TFe is 43.15%, TiO
2Mass content be 25.14%, V
2O
5Mass content be 1.05%, v-ti magnetite concentrate is levigate to-200 orders 80%;
(2) with levigate v-ti magnetite concentrate and 25% mixed in hydrochloric acid, liquid-solid ratio is 5:1, leaches 3 hours down at 120 ℃, obtains pickling liquor;
(3) pickling liquor that step (2) is obtained 500 ℃ of calcinings down, obtains ferrovanadium solid material and hydrochloric acid, and hydrochloric acid returns the leaching for v-ti magnetite concentrate;
(4) to place mass concentration be 50% sodium hydroxide solution to the ferrovanadium solid material that step (3) is obtained, liquid-solid ratio is 10:1, be 130 ℃ of following insulated and stirred 3 hours in temperature, filter, washing, obtain Vanadium Pentoxide in FLAKES mass content＜0.04% iron content solid material and contain the alkaline solution of vanadium;
(5) step (4) is obtained contain vanadium the alkaline solution evaporation, to be concentrated into mass concentration be 50%, repeating step (4), when treating that vanadic acid sodium concentration is 10～30g/L in the alkaline solution, crystallisation by cooling is isolated the vanadic acid sodium crystal;
(6) the vanadic acid sodium crystal that step (8) is obtained is handled with the precipitator method, can obtain purity and be 98.9% Vanadium Pentoxide in FLAKES, and the rate of recovery of vanadium is 87.4% in the v-ti magnetite concentrate.
Embodiment 3
(1) mass content of raw material v-ti magnetite concentrate main component: TFe is 40.15%, TiO
2Mass content be 24.35%, V
2O
5Mass content be 0.95%, v-ti magnetite concentrate is levigate to-200 orders 80%;
(2) with levigate v-ti magnetite concentrate and 36% mixed in hydrochloric acid, liquid-solid ratio is 1:1, leaches 1 hour down at 100 ℃, obtains pickling liquor;
(3) pickling liquor that step (2) is obtained 800 ℃ of calcinings down, obtains ferrovanadium solid material and hydrochloric acid, and hydrochloric acid returns the leaching for v-ti magnetite concentrate;
(4) to place mass concentration be 80% sodium hydroxide solution to the ferrovanadium solid material that step (3) is obtained, liquid-solid ratio is 0.5:1, be 160 ℃ of following insulated and stirred 0.5 hour in temperature, filter, wash, obtain the iron content solid material and the alkaline solution that contains vanadium of mass content＜0.03% of Vanadium Pentoxide in FLAKES;
(5) step (4) is obtained contain vanadium the alkaline solution evaporation, to be concentrated into mass concentration be 80%, repeating step (4), when treating that vanadic acid sodium concentration is 10～30g/L in the alkaline solution, crystallisation by cooling is isolated the vanadic acid sodium crystal;
(6) the vanadic acid sodium crystal that step (8) is obtained is further handled, and can obtain purity and be 99.1% Vanadium Pentoxide in FLAKES, and the rate of recovery of vanadium is 89.1% in the v-ti magnetite concentrate.
Embodiment 4
(1) mass content of raw material v-ti magnetite concentrate main component: TFe is 35.97%, TiO
2Mass content be 28.74%, V
2O
5Mass content be 1.34%, v-ti magnetite concentrate is levigate to-200 orders 80%;
(2) with levigate v-ti magnetite concentrate and 30% mixed in hydrochloric acid, liquid-solid ratio is 2:1, leaches 1 hour down at 130 ℃, obtains acid dip solution;
(3) pickling liquor that step (2) is obtained 600 ℃ of calcinings down, obtains ferrovanadium solid material and hydrochloric acid, and hydrochloric acid returns the leaching for v-ti magnetite concentrate;
(4) to place mass concentration be 60% sodium hydroxide solution to the ferrovanadium solid material that step (3) is obtained, liquid-solid ratio is 2:1, be 150 ℃ of following insulated and stirred 3 hours in temperature, filter, washing, obtain Vanadium Pentoxide in FLAKES mass content＜0.05% iron content solid material and contain the alkaline solution of vanadium;
(5) step (4) is obtained contain vanadium the alkaline solution evaporation, to be concentrated into mass concentration be 60%, repeating step (4), when treating that vanadic acid sodium concentration is 10～30g/L in the alkaline solution, crystallisation by cooling is isolated the vanadic acid sodium crystal;
(6) the vanadic acid sodium crystal that step (8) is obtained is further handled, and can obtain purity and be 99.0% Vanadium Pentoxide in FLAKES, and the rate of recovery of vanadium is 89.2% in the v-ti magnetite concentrate.
Embodiment 5
(1) mass content of raw material v-ti magnetite concentrate main component: TFe is 39.65%, TiO
2Mass content be 25.39%, V
2O
5Mass content be 1.33%, v-ti magnetite concentrate is levigate to-200 orders 80%;
(2) with levigate v-ti magnetite concentrate and 10% mixed in hydrochloric acid, liquid-solid ratio is 2:1, leaches 10 hours down at 120 ℃, obtains acid dip solution;
(3) pickling liquor that step (2) is obtained 200 ℃ of calcinings down, obtains ferrovanadium solid material and hydrochloric acid, and hydrochloric acid returns the leaching for v-ti magnetite concentrate;
(4) to place mass concentration be 40% potassium hydroxide solution to the ferrovanadium solid material that step (3) is obtained, liquid-solid ratio is 5:1, be 80 ℃ of following insulated and stirred 5 hours in temperature, filter, washing, obtain Vanadium Pentoxide in FLAKES mass content＜0.05% iron content solid material and contain the alkaline solution of vanadium;
(5) step (4) is obtained contain vanadium the alkaline solution evaporation, to be concentrated into mass concentration be 40%, repeating step (4), when treating that vanadic acid sodium concentration is 10～30g/L in the alkaline solution, crystallisation by cooling is isolated the potassium vanadate crystal;
(6) the potassium vanadate crystal that step (8) is obtained is further handled, and can obtain purity and be 98.3% Vanadium Pentoxide in FLAKES, and the rate of recovery of vanadium is 88.1% in the v-ti magnetite concentrate.
Certainly; the present invention can also have various embodiments; under the situation that does not deviate from spirit of the present invention and essence thereof; those of ordinary skill in the art can be according to various corresponding changes and the modification openly made of the present invention, but these corresponding change and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (10)
1. method of extracting vanadium from v-ti magnetite concentrate may further comprise the steps:
1) v-ti magnetite concentrate and hydrochloric acid are carried out sour molten leaching under 100～150 ℃, filter and obtain pickling liquor, wherein, 1～10 hour reaction times;
2) pickling liquor that step 1) is obtained is calcined, and obtains ferrovanadium solid material and hydrochloric acid;
3) with step 2) the ferrovanadium solid material that obtains places alkaline solution, is 80～160 ℃ of following insulated and stirred 0.5～5 hour in temperature, filters, washing, and obtain iron content solid material and contain the vanadium alkaline solution;
4) step 3) is obtained to contain the evaporation of vanadium alkaline solution, concentrate after, repeating step 3), when treating that vanadate concentration is 10～30g/L in the alkaline solution, crystallisation by cooling is isolated vanadate crystal, further Processing of Preparation ammonium meta-vanadate or Vanadium Pentoxide in FLAKES.
2. the method for extracting vanadium from v-ti magnetite concentrate according to claim 1 is characterized in that, the liquid-solid ratio of the molten leaching reaction of the described acid of step 1) is 1:1～10:1.
3. the method for extracting vanadium from v-ti magnetite concentrate according to claim 1 and 2 is characterized in that the mass percent concentration of the described hydrochloric acid of step 1) is 10%～36%.
4. the method for extracting vanadium from v-ti magnetite concentrate according to claim 1 is characterized in that step 2) 200～800 ℃ of described calcining temperatures, calcination time is 1～5 hour.
5. the method for extracting vanadium from v-ti magnetite concentrate according to claim 1 is characterized in that step 2) hydrochloric acid that obtains is used for the leaching of the v-ti magnetite concentrate of step 1).
6. the method for extracting vanadium from v-ti magnetite concentrate according to claim 1 is characterized in that the liquid-solid ratio of the described alkaline solution of step 3) and ferrovanadium solid material is 0.5:1～20:1.
7. according to claim 1 or the 6 described methods of from v-ti magnetite concentrate, extracting vanadium, it is characterized in that the described alkaline solution of step 3) is sodium hydroxide or potassium hydroxide solution.
8. according to claim 1 or the 6 described methods of from v-ti magnetite concentrate, extracting vanadium, it is characterized in that the described alkaline solution mass percent concentration of step 3) is 20%～80%.
9. the method for extracting vanadium from v-ti magnetite concentrate according to claim 1 is characterized in that, the iron content solid material that step 3) obtains is as iron-smelting raw material.
10. the method for extracting vanadium from v-ti magnetite concentrate according to claim 1 is characterized in that the described method for preparing ammonium meta-vanadate or Vanadium Pentoxide in FLAKES of step 4) is the precipitator method.
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| CN103962225A (en) * | 2014-04-23 | 2014-08-06 | 鞍钢集团矿业公司 | Vanadium-titanium magnetite concentrate recleaning method realized through alkaline leaching, classification and gravity separation |
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| CN104689902A (en) * | 2014-04-23 | 2015-06-10 | 鞍钢集团矿业公司 | Method for recleaning vanadium-titanium magnetite concentrates by utilizing alkaline leaching, acid pickling, desliming and reverse flotation |
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| CN106756006A (en) * | 2016-10-12 | 2017-05-31 | 攀枝花学院 | The method of v-ti magnetite concentrate comprehensive utilization |
| CN106756006B (en) * | 2016-10-12 | 2019-04-23 | 攀枝花学院 | The method of v-ti magnetite concentrate comprehensive utilization |
| CN109174398A (en) * | 2018-08-02 | 2019-01-11 | 汤铁 | A kind of comprehensive utilization process of vanadium titano-magnetite |
| US11247270B2 (en) | 2019-01-31 | 2022-02-15 | Na Wang | Method for preparing vanadium and vanadium alloy powder from vanadium-containing materials through shortened process |
| CN114480882A (en) * | 2022-01-18 | 2022-05-13 | 龙佰集团股份有限公司 | Method for fully utilizing ferrotitanium vanadium resources in vanadium-titanium magnetite |
| CN114480882B (en) * | 2022-01-18 | 2023-10-13 | 龙佰集团股份有限公司 | Method for fully utilizing ferrotitanium and vanadium resources in vanadium titano-magnetite |
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