CN102134649B - Comprehensive utilization method for vanadium slag - Google Patents
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Abstract
The invention provides a comprehensive utilization method for vanadium slag, which is characterized by comprising the following steps of: (1) crushing and grinding; (2) mixing materials; (3) melting; (4) dissolving and filtering; (5) settling vanadium; and (6) preparing ferric oxide. Raw materials are wide in sources, the vanadium slag is utilized integrally at one time, immediate products are recycled, the consumption of the raw materials and water is reduced, secondary pollution is avoided, the process is simple, operating conditions are mild, the cost is low, the added value of the product is high, and the economic benefit is high. Iron is effectively removed in the process of producing high-purity vanadium pentoxide, resources such as vanadium and iron are reasonably utilized, and the invention provides a new way for comprehensively utilizing the vanadium slag.
Description
Technical field
The present invention relates to a kind of method of comprehensive utilization of vanadium slag, belong to metallurgical technology field.
Background technology
South Africa, Russia and China are that the world produces vanadium big country and big export country, and European Union, Japan and the U.S. are main body entrance states.It is predicted, the whole world can provide the market space of 100,000 ton/years of vanadium (amounting to Vanadium Pentoxide in FLAKES) between coming 10 years.Expectation from 2011 to the year two thousand twenty, world's vanadium demand will keep sustainable growth trend, annual growth about 4.3%.Vanadium exists with the form that contains vanadium minerals or class matter homophase usually, this makes the vanadium can not be as non-ferrous metals such as copper-lead zinc, method by mechanical beneficiation obtains the vanadium concentrate, therefore in the existing process for extracting vanadium, ore and/or the waste residue grade processed are all lower, therefore find one to be fit to the treatment process of low grade vanadium ore and/or waste residue is had more realistic meaning.
There is a large amount of discarded vanadium slags on the ground such as Sichuan, Chengde and Anhui Maanshan, nearly 1,200,000 tons of annual discharging, these Vanadium in Vanadium Residue content are generally lower, be generally about 2%, major part is present in the vanadium calcium titanate, be the main object of vanadium extraction, be difficult to extract than other navajoite owing to containing nearly 40% CaO.
Number of patent application is technology employing calcification baking-sulfuric acid leaching technique of 200710202445.8, with CaCO
3As the calcium source additive, vanadium slag is carried out roasting, and with the vanadium in the sulfuric acid leaching roasting after product.But this technique exists following shortcoming: ⑴ that new discarded and new pollution is arranged, and has caused the loss of part mineral wealth; ⑵ extraction time is long, and acid consumption is larger, and every output 1t Vanadium Pentoxide in FLAKES will consume 81t sulfuric acid, and the method that there is no is at present recycled; ⑶ the sulfurous gas volatilization is arranged in the technological process, can produce the problems such as more serious atmospheric pollution and operator poisoning; ⑷ sulphuric acid is a strong corrosive under the heating condition, serious to equipment corrosion, dangerous in the production.
Sodium roasting vanadium-extracting is to contain the vanadium raw materials vanadium extraction to use more technique, and its ultimate principle is: take sodium salts such as salt or soda as additive, the vanadium of multivalence attitude is converted into the sodium salt of water-soluble pentavalent vanadium: 4NaCl+2V by roasting
2O
5+ O
2=4NaVO
3+ Cl
2
To the direct water logging of sodium roasting product, can obtain containing the leaching liquid of vanadium and a small amount of aluminium impurity again, rear adding ammonium salt (acid ammonium salt precipitation method) makes the ammonium meta-vanadate precipitation, obtains thick Vanadium Pentoxide in FLAKES through roasting.Again, removal of impurities molten through alkali and get ammonium meta-vanadate with the precipitation of ammonium salt secondary can obtain purity greater than 98% V after the roasting
2O
5Also available sulfuric acid impregnation-calcination product:
2NaVO
3+H
2SO
4=Na
2SO
4+H
2O+?V
2O
5
Separate and obtain thick V
2O
5,, removal of impurities molten by alkali also gets ammonium meta-vanadate with the precipitation of ammonium salt secondary, can get high purity vanadic anhydride through roasting.Sodium roasting vanadium-extracting method technique is relatively ripe, simple to operate, drop in early days little, because of strong to the vanadium selectivity, the rate of recovery is high, is the main method of China's vanadium extraction from raw ore always.But produce a large amount of Cl during owing to sodium roasting
2, HCl and SO
2Deng toxic gas, along with the whole world to the protection of environment and the attention that improves utilization of resources, seek new low pollution, high efficiency process for extracting vanadium has become problem demanding prompt solution in the global vanadium smelting industry.
Summary of the invention
Goal of the invention: the invention provides a kind of method of comprehensive utilization of vanadium slag, its objective is that solution utilized existing high pollution in the Leaching of Vanadium from Vanadium slag method, poor efficiency and unsafe problem in the past; The present invention obtains Vanadium Pentoxide in FLAKES and ferric oxide from vanadium slag.
Technical scheme: the present invention is achieved through the following technical solutions:
A kind of method of comprehensive utilization of vanadium slag is characterized in that carrying out according to the following steps:
⑴ fragmentation and grinding: the powder that vanadium slag is obtained diameter 70～170 μ m through broken and grinding;
⑵ batch mixing: vanadium slag powder and ammonium sulfate and ammonium-potassium sulfate are mixed, and mixing of materials is the vanadium slag powder by weight percentage: ammonium sulfate: ammonium-potassium sulfate=1:5～12:2～5;
⑶ melting: the material of above-mentioned mixing is warming up to 270～440 ℃ and be incubated 10～45min, obtains blocks of solid and ammonia;
⑷ dissolving and filtering: obtain blocks of solid to place concentration be that the aqueous solution of the EDTA of 0.1～0.3mol/L dissolves above-mentioned, make iron and EDTA in the blocks of solid that chelatropic reaction occur, form stable inner complex, and the mol ratio of the iron in EDTA and the blocks of solid is 0.5～1.1:1, then filter and obtain filtrate and residue, residue is iron cement;
⑸ the precipitation of vanadium: pass into the ammonia that step ⑶ obtains in above-mentioned filtrate, and control pH is 1.3～2.7, temperature is 40～80 ℃, makes the vanadium precipitation in the filtrate, and at 220～360 ℃ of calcination 30～150min, obtains Vanadium Pentoxide in FLAKES;
⑹ the preparation of ferric oxide: pass into the ammonia that step ⑶ obtains in the mother liquor of vanadium precipitation, regulating pH is 6.8～7.5, and with mother liquor at 400～520 ℃ of calcination 30～60min, obtain ferric oxide; Gaseous substance cooling with producing in the calcination process obtains ammonium sulfate and ammonium-potassium sulfate mixture, and this mixture is recycled to step ⑵ and recycles.
Vanadium slag described in " ⑴ " step, the weight percent of iron are 20%～30%, and the weight percent of vanadium is 0.8%～3.0%.
In the filtrate of described step ⑷, water-soluble vanadium accounts for the per-cent of the gross weight of Vanadium in Vanadium Residue 〉=93%, and water-soluble iron accounts for the per-cent of the gross weight of iron in the vanadium slag≤30%.
Account for the per-cent of vanadium gross weight in the filtrate 〉=99% with the vanadium of Vanadium Pentoxide in FLAKES form precipitation among the described step ⑸; Account for the per-cent of iron gross weight in the filtrate≤0.0005% with the iron of form of iron oxide precipitation.
Described product Vanadium Pentoxide in FLAKES weight purity 〉=98%; Ferric oxide weight purity 〉=99%, its crystal formation are nano-sized iron oxide.
Advantage and effect:
Compared with prior art, characteristics of the present invention and beneficial effect thereof are:
Vanadium slag powder and ammonium sulfate, ammonium-potassium sulfate are mixed, it is the chemical property of having utilized ammonium-potassium sulfate special, make frit reaction have more selectivity: to make more vanadium be converted into water-soluble vanadium by chemical reaction, and make iron still less be converted into water-soluble iron, carry out the initial gross separation of iron and vanadium (generally, a selectivity is not had in frit reaction, is 201010576256.9 technology such as number of patent application).Water-soluble vanadium accounts for the per-cent of the gross weight of Vanadium in Vanadium Residue 〉=93%, illustrates that its transformation efficiency is high, is that prior art can't realize.
Directly place the aqueous solution of EDTA to dissolve blocks of solid that frit reaction obtains, and in the precipitation process of vanadium control pH and temperature, optionally make the vanadium precipitation, and iron does not precipitate, thereby product Vanadium Pentoxide in FLAKES and ferric oxide purity are high, having realized that Vanadium in Vanadium Residue and the thorough of iron separate, is that prior art can't realize.Simultaneously, blocks of solid that frit reaction obtains is used as iron cement---novel high-performance special cement through the residue of dissolving and filtration generation.
To contain the ferric oxide that the Fe mother liquor obtains behind 400～520 ℃ of calcination 30～60min, its crystal formation is nano-sized iron oxide, is different from common ferric oxide, therefore have special physicochemical property and purposes, greatly having improved value-added content of product, is that prior art can't realize.
At 220～360 ℃ of calcination 30～150min, the Vanadium Pentoxide in FLAKES that obtains has higher crystallization degree with the throw out of vanadium.It is generally acknowledged, the throw out crystallization degree that obtains from the aqueous solution is low, even is amorphous, but the present invention has improved the crystallization degree of Vanadium Pentoxide in FLAKES greatly by calcination.
For separating of iron and vanadium, the percentage composition of iron is higher, and the difficulty of its separation is larger.Therefore, be 20%～30% raw material to the weight percent of iron, be the blank of research such as the iron of vanadium slag and the separating technology of vanadium always, the present invention has realized that well Vanadium in Vanadium Residue and the thorough of iron separate, and is technical significant progress.
In sum, raw material sources of the present invention are extensive, and disposable integral utilizes vanadium slag, and realize the intermediate product recycle, reduced the consumption of starting material and water, non-secondary pollution, technique is simple, and operational condition is gentle, cost is low, and added value of product is high, and economic benefit is high.Both solved the problem of effectively removing iron in the process of producing high-purity vanadium pentoxide, the resources such as vanadium and iron have rationally been utilized again, provide the new way of comprehensive utilization for vanadium slag, and the inventive method is easy to realize suitability for industrialized production, has considerable environmental benefit, a Social benefit and economic benefit.
Description of drawings:
Fig. 1 is process flow diagram of the present invention.
Embodiment:The present invention is described further below in conjunction with accompanying drawing:
Below in conjunction with embodiment the present invention is elaborated, but protection scope of the present invention is not limited only to following embodiment.
Embodiment 1:
⑴ fragmentation and grinding: be 29% with the weight percent of iron content, the weight percent of vanadium is 1.0% vanadium slag obtains diameter 80 μ m through broken and grinding powder;
⑵ batch mixing: by weight the vanadium slag powder: ammonium sulfate: ammonium-potassium sulfate=1:7:3 takes by weighing raw material, and vanadium slag powder and ammonium sulfate, ammonium-potassium sulfate are mixed;
⑶ melting: the material of above-mentioned mixing is warming up to 300 ℃ and be incubated 15min, obtains blocks of solid and ammonia;
⑷ dissolving and filtering: obtain blocks of solid to place concentration be that the aqueous solution of the EDTA of 0.15mol/L dissolves above-mentioned, and the mol ratio of EDTA and iron is 0.6:1, then filter and obtain filtrate and residue, residue is iron cement, the per-cent that filtrate water dissolubility vanadium accounts for the gross weight of Vanadium in Vanadium Residue is 94%, and the per-cent that water-soluble iron accounts for the gross weight of iron in the vanadium slag is 27%;
⑸ the precipitation of vanadium: pass into the ammonia that step ⑶ obtains in above-mentioned filtrate, and control pH is 1.5, temperature is 45 ℃, makes the vanadium precipitation in the filtrate, and at 240 ℃ of calcination 50min, obtains Vanadium Pentoxide in FLAKES; Account for the per-cent 99.2% of vanadium gross weight in the filtrate in this step with the vanadium of Vanadium Pentoxide in FLAKES form precipitation; Account for the per-cent 0.0004% of iron gross weight in the filtrate with the iron of form of iron oxide precipitation.
⑹ the preparation of ferric oxide: pass into the ammonia that step ⑶ obtains in the mother liquor of vanadium precipitation, regulating pH is 7.0, and with mother liquor at 500 ℃ of calcination 60min, obtain ferric oxide; Gaseous substance cooling with producing in the calcination process obtains ammonium sulfate and ammonium-potassium sulfate mixture, and this mixture is recycled to step ⑵ and recycles.
After testing, described product Vanadium Pentoxide in FLAKES weight purity 99.2%; Ferric oxide weight purity 99.3%, its crystal formation are nano-sized iron oxide.
Embodiment 2:
⑴ fragmentation and grinding: be 20% with the weight percent of iron content, the weight percent of vanadium is 3.0% vanadium slag obtains diameter 70 μ m through broken and grinding powder;
⑵ batch mixing: by weight the vanadium slag powder: ammonium sulfate: ammonium-potassium sulfate=1:5:5 takes by weighing raw material, and vanadium slag powder and ammonium sulfate, ammonium-potassium sulfate are mixed;
⑶ melting: the material of above-mentioned mixing is warming up to 270 ℃ and be incubated 30min, obtains blocks of solid and ammonia;
⑷ dissolving and filtering: obtain blocks of solid to place concentration be that the aqueous solution of the EDTA of 0.18mol/L dissolves above-mentioned, and the mol ratio of EDTA and iron is 1.1:1, then filter and obtain filtrate and residue, residue is iron cement, the per-cent that filtrate water dissolubility vanadium accounts for the gross weight of Vanadium in Vanadium Residue is 96%, and the per-cent that water-soluble iron accounts for the gross weight of iron in the vanadium slag is 27%;
⑸ the precipitation of vanadium: pass into the ammonia that step ⑶ obtains in above-mentioned filtrate, and control pH is 1.3, temperature is 40 ℃, makes the vanadium precipitation in the filtrate, and at 220 ℃ of calcination 70min, obtains Vanadium Pentoxide in FLAKES; Account for the per-cent 99% of vanadium gross weight in the filtrate in this step with the vanadium of Vanadium Pentoxide in FLAKES form precipitation; Account for the per-cent 0.0005% of iron gross weight in the filtrate with the iron of form of iron oxide precipitation.
⑹ the preparation of ferric oxide: pass into the ammonia that step ⑶ obtains in the mother liquor of vanadium precipitation, regulating pH is 6.8, and with mother liquor at 520 ℃ of calcination 40min, obtain ferric oxide; Gaseous substance cooling with producing in the calcination process obtains ammonium sulfate and ammonium-potassium sulfate mixture, and this mixture is recycled to step ⑵ and recycles.
After testing, described product Vanadium Pentoxide in FLAKES weight purity 98.7%; Ferric oxide weight purity 99.1%, its crystal formation are nano-sized iron oxide.
Embodiment 3:
⑴ fragmentation and grinding: be 30% with the weight percent of iron content, the weight percent of vanadium is 0.8% vanadium slag obtains diameter 100 μ m through broken and grinding powder;
⑵ batch mixing: by weight the vanadium slag powder: ammonium sulfate: ammonium-potassium sulfate=1:12:2 takes by weighing raw material, and vanadium slag powder and ammonium sulfate, ammonium-potassium sulfate are mixed;
⑶ melting: the material of above-mentioned mixing is warming up to 400 ℃ and be incubated 10min, obtains blocks of solid and ammonia;
⑷ dissolving and filtering: obtain blocks of solid to place concentration be that the aqueous solution of the EDTA of 0.1mol/L dissolves above-mentioned, and the mol ratio of EDTA and iron is 0.8:1, then filter and obtain filtrate and residue, residue is iron cement, the per-cent that filtrate water dissolubility vanadium accounts for the gross weight of Vanadium in Vanadium Residue is 93%, and the per-cent that water-soluble iron accounts for the gross weight of iron in the vanadium slag is 15%;
⑸ the precipitation of vanadium: pass into the ammonia that step ⑶ obtains in above-mentioned filtrate, and control pH is 2.7, temperature is 70 ℃, makes the vanadium precipitation in the filtrate, and at 360 ℃ of calcination 30min, obtains Vanadium Pentoxide in FLAKES; Account for the per-cent 99.8% of vanadium gross weight in the filtrate in this step with the vanadium of Vanadium Pentoxide in FLAKES form precipitation; Account for the per-cent 0.0001% of iron gross weight in the filtrate with the iron of form of iron oxide precipitation.
⑹ the preparation of ferric oxide: pass into the ammonia that step ⑶ obtains in the mother liquor of vanadium precipitation, regulating pH is 7.5, and with mother liquor at 400 ℃ of calcination 50min, obtain ferric oxide; Gaseous substance cooling with producing in the calcination process obtains ammonium sulfate and ammonium-potassium sulfate mixture, and this mixture is recycled to step ⑵ and recycles.
After testing, described product Vanadium Pentoxide in FLAKES weight purity 99%; Ferric oxide weight purity 99.2%, its crystal formation are nano-sized iron oxide.
Embodiment 4:
⑴ fragmentation and grinding: be 26% with the weight percent of iron content, the weight percent of vanadium is 1.5% vanadium slag obtains diameter 100 μ m through broken and grinding powder;
⑵ batch mixing: by weight the vanadium slag powder: ammonium sulfate: ammonium-potassium sulfate=1:8:4 takes by weighing raw material, and vanadium slag powder and ammonium sulfate, ammonium-potassium sulfate are mixed;
⑶ melting: the material of above-mentioned mixing is warming up to 440 ℃ and be incubated 30min, obtains blocks of solid and ammonia;
⑷ dissolving and filtering: obtain blocks of solid to place concentration be that the aqueous solution of the EDTA of 0.3mol/L dissolves above-mentioned, and the mol ratio of EDTA and iron is 0.5:1, then filter and obtain filtrate and residue, residue is iron cement, the per-cent that filtrate water dissolubility vanadium accounts for the gross weight of Vanadium in Vanadium Residue is 98%, and the per-cent that water-soluble iron accounts for the gross weight of iron in the vanadium slag is 8%;
⑸ the precipitation of vanadium: pass into the ammonia that step ⑶ obtains in above-mentioned filtrate, and control pH is 1.6, temperature is 80 ℃, makes the vanadium precipitation in the filtrate, and at 230 ℃ of calcination 150min, obtains Vanadium Pentoxide in FLAKES; Account for the per-cent 99.1% of vanadium gross weight in the filtrate in this step with the vanadium of Vanadium Pentoxide in FLAKES form precipitation; Account for the per-cent 0.0003% of iron gross weight in the filtrate with the iron of form of iron oxide precipitation;
⑹ the preparation of ferric oxide: pass into the ammonia that step ⑶ obtains in the mother liquor of vanadium precipitation, regulating pH is 7.0, and with mother liquor at 450 ℃ of calcination 30min, obtain ferric oxide; Gaseous substance cooling with producing in the calcination process obtains ammonium sulfate and ammonium-potassium sulfate mixture, and this mixture is recycled to step ⑵ and recycles.
After testing, described product Vanadium Pentoxide in FLAKES weight purity 98.3%; Ferric oxide weight purity 99.7%, its crystal formation are nano-sized iron oxide.
Embodiment 5:
⑴ fragmentation and grinding: be 21% with the weight percent of iron content, the weight percent of vanadium is 2.0% vanadium slag obtains diameter 170 μ m through broken and grinding powder;
⑵ batch mixing: by weight the vanadium slag powder: ammonium sulfate: ammonium-potassium sulfate=1:5:2 takes by weighing raw material, and vanadium slag powder and ammonium sulfate, ammonium-potassium sulfate are mixed;
⑶ melting: the material of above-mentioned mixing is warming up to 320 ℃ and be incubated 45min, obtains blocks of solid and ammonia;
⑷ dissolving and filtering: obtain blocks of solid to place concentration be that the aqueous solution of the EDTA of 0.24mol/L dissolves above-mentioned, and the mol ratio of EDTA and iron is 1:1, then filter and obtain filtrate and residue, residue is iron cement, the per-cent that filtrate water dissolubility vanadium accounts for the gross weight of Vanadium in Vanadium Residue is 98%, and the per-cent that water-soluble iron accounts for the gross weight of iron in the vanadium slag is 30%;
⑸ the precipitation of vanadium: pass into the ammonia that step ⑶ obtains in above-mentioned filtrate, and control pH is 2.0, temperature is 50 ℃, makes the vanadium precipitation in the filtrate, and at 300 ℃ of calcination 60min, obtains Vanadium Pentoxide in FLAKES; Account for the per-cent 99.9% of vanadium gross weight in the filtrate in this step with the vanadium of Vanadium Pentoxide in FLAKES form precipitation; Account for the per-cent 0.0002% of iron gross weight in the filtrate with the iron of form of iron oxide precipitation;
⑹ the preparation of ferric oxide: pass into the ammonia that step ⑶ obtains in the mother liquor of vanadium precipitation, regulating pH is 7.0, and with mother liquor at 420 ℃ of calcination 45min, obtain ferric oxide; Gaseous substance cooling with producing in the calcination process obtains ammonium sulfate and ammonium-potassium sulfate mixture, and this mixture is recycled to step ⑵ and recycles.
After testing, described product Vanadium Pentoxide in FLAKES weight purity 99.8%; Ferric oxide weight purity 99%, its crystal formation are nano-sized iron oxide.
Embodiment 6:
⑴ fragmentation and grinding: be 27% with the weight percent of iron content, the weight percent of vanadium is 2.8% vanadium slag obtains diameter 160 μ m through broken and grinding powder;
⑵ batch mixing: by weight the vanadium slag powder: ammonium sulfate: ammonium-potassium sulfate=1:5:2 takes by weighing raw material, and vanadium slag powder and ammonium sulfate, ammonium-potassium sulfate are mixed;
⑶ melting: the material of above-mentioned mixing is warming up to 420 ℃ and be incubated 45min, obtains blocks of solid and ammonia;
⑷ dissolving and filtering: obtain blocks of solid to place concentration be that the aqueous solution of the EDTA of 0.26mol/L dissolves above-mentioned, and the mol ratio of EDTA and iron is 1:1, then filter and obtain filtrate and residue, residue is iron cement, the per-cent that filtrate water dissolubility vanadium accounts for the gross weight of Vanadium in Vanadium Residue is 99%, and the per-cent that water-soluble iron accounts for the gross weight of iron in the vanadium slag is 1.5%;
⑸ the precipitation of vanadium: pass into the ammonia that step ⑶ obtains in above-mentioned filtrate, and control pH is 2.0, temperature is 75 ℃, makes the vanadium precipitation in the filtrate, and at 300 ℃ of calcination 100min, obtains Vanadium Pentoxide in FLAKES; Account for the per-cent 99.3% of vanadium gross weight in the filtrate in this step with the vanadium of Vanadium Pentoxide in FLAKES form precipitation; Account for the per-cent 0.0002% of iron gross weight in the filtrate with the iron of form of iron oxide precipitation;
⑹ the preparation of ferric oxide: pass into the ammonia that step ⑶ obtains in the mother liquor of vanadium precipitation, regulating pH is 7.0, and with mother liquor at 420 ℃ of calcination 45min, obtain ferric oxide; Gaseous substance cooling with producing in the calcination process obtains ammonium sulfate and ammonium-potassium sulfate mixture, and this mixture is recycled to step ⑵ and recycles.
After testing, described product Vanadium Pentoxide in FLAKES weight purity 99.8%; Ferric oxide weight purity 99%, its crystal formation are nano-sized iron oxide.
EDTA is ethylenediamine tetraacetic acid (EDTA) or its disodium salt.
The present invention carries out high efficiency process for extracting vanadium by oligosaprobic approach, and successful has well solved existing high pollution in the process for extracting vanadium in the past, inefficient problem, is beneficial to and applies.
Claims (5)
1. the method for comprehensive utilization of a vanadium slag is characterized in that carrying out according to the following steps:
⑴ fragmentation and grinding: the powder that vanadium slag is obtained diameter 70～170 μ m through broken and grinding;
⑵ batch mixing: vanadium slag powder and ammonium sulfate and ammonium-potassium sulfate are mixed, and mixing of materials is the vanadium slag powder by weight percentage: ammonium sulfate: ammonium-potassium sulfate=1:5～12:2～5;
⑶ melting: the material of above-mentioned mixing is warming up to 270～440 ℃ and be incubated 10～45min, obtains blocks of solid and ammonia;
⑷ dissolving and filtering: obtain blocks of solid to place concentration be that the aqueous solution of the EDTA of 0.1～0.3mol/L dissolves above-mentioned, make iron and EDTA in the blocks of solid that chelatropic reaction occur, form stable inner complex, and the mol ratio of the iron in EDTA and the blocks of solid is 0.5～1.1:1, then filter and obtain filtrate and residue, residue is iron cement;
⑸ the precipitation of vanadium: pass into the ammonia that step ⑶ obtains in above-mentioned filtrate, and control pH is 1.3～2.7, temperature is 40～80 ℃, makes the vanadium precipitation in the filtrate, and at 220～360 ℃ of calcination 30～150min, obtains Vanadium Pentoxide in FLAKES;
⑹ the preparation of ferric oxide: pass into the ammonia that step ⑶ obtains in the mother liquor of vanadium precipitation, regulating pH is 6.8～7.5, and with mother liquor at 400～520 ℃ of calcination 30～60min, obtain ferric oxide; Gaseous substance cooling with producing in the calcination process obtains ammonium sulfate and ammonium-potassium sulfate mixture, and this mixture is recycled to step ⑵ and recycles.
2. the method for comprehensive utilization of a kind of vanadium slag according to claim 1, it is characterized in that: the vanadium slag described in " ⑴ step ", the weight percent of iron are 20%～30%, the weight percent of vanadium is 0.8%～3.0%.
3. the method for comprehensive utilization of a kind of vanadium slag according to claim 1, it is characterized in that: in the filtrate of described step ⑷, water-soluble vanadium accounts for the per-cent of the gross weight of Vanadium in Vanadium Residue 〉=93%, and water-soluble iron accounts for the per-cent of the gross weight of iron in the vanadium slag≤30%.
4. the method for comprehensive utilization of a kind of vanadium slag according to claim 1 is characterized in that: account for the per-cent of vanadium gross weight in the filtrate 〉=99% with the vanadium of Vanadium Pentoxide in FLAKES form precipitation among the described step ⑸; Account for the per-cent of iron gross weight in the filtrate≤0.0005% with the iron of form of iron oxide precipitation.
5. the method for comprehensive utilization of a kind of vanadium slag according to claim 1 is characterized in that: Vanadium Pentoxide in FLAKES weight purity 〉=98%; Ferric oxide weight purity 〉=99%, its crystal formation are nano-sized iron oxide.
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| CN107267766B (en) * | 2017-08-28 | 2019-02-26 | 四川大学 | A method of Selective Separation vanadium, titanium, iron from modified vanadium slag |
| CN110055417B (en) * | 2018-01-17 | 2020-12-29 | 四川大学 | Method for efficiently separating vanadium and titanium from vanadium slag mixed material |
| CN110408790A (en) * | 2018-04-27 | 2019-11-05 | 中国科学院过程工程研究所 | A kind of method that pressure leaching v-bearing steel slag produces vanadium product |
| CN109437341B (en) * | 2018-12-17 | 2020-06-16 | 深圳先进技术研究院 | Preparation method of metal oxide or composite material thereof, application and battery |
| KR102386449B1 (en) * | 2021-12-27 | 2022-04-15 | 한국지질자원연구원 | Method for producing high purity vanadium compounds |
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| CN101381818A (en) * | 2008-09-29 | 2009-03-11 | 浙江大学 | Method for preparing intermediate salt during acid leaching and extraction of vanadium pentoxide from vanadium-containing stone coal ash |
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| CN101265524A (en) * | 2008-04-17 | 2008-09-17 | 武汉科技大学 | Method for extracting V2O5 from stone coal |
| CN101381818A (en) * | 2008-09-29 | 2009-03-11 | 浙江大学 | Method for preparing intermediate salt during acid leaching and extraction of vanadium pentoxide from vanadium-containing stone coal ash |
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