CN105316479A - Red mud vanadium extracting and ore-blending sintering method - Google Patents
Red mud vanadium extracting and ore-blending sintering method Download PDFInfo
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- CN105316479A CN105316479A CN201410368976.4A CN201410368976A CN105316479A CN 105316479 A CN105316479 A CN 105316479A CN 201410368976 A CN201410368976 A CN 201410368976A CN 105316479 A CN105316479 A CN 105316479A
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- red mud
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Abstract
The invention discloses a red mud vanadium extracting and ore-blending sintering method and belongs to the technical field of nonferrous metallurgy and ferrous metallurgy. The red mud comprehensive utilizing method which is high in efficiency, economical and reasonable is provided. The method includes the following steps that (1) red mud is dried and then finely ground; (2) the red mud treated in the step (1) enters a proportioning bin, and sodium carbonate, sodium chloride and sodium sulfate are added; (3) uniformly mixed materials are delivered into a rotary kiln to be roasted; (4) clinker obtained through the roasting is leached out under the normal pressure through a sulfuric acid solution; (5) leachate is kept still, and liquid supernatant is delivered into a precipitation tank in a precipitation process; (6) the tank is opened for stirring, sulfuric acid is added for neutralizing, ammonium sulfate is added, sulfuric acid is used for adjusting, and orange ammonium polyorthovanadate precipitation can be crystallized out under the heating and stirring conditions; (7) ammonium polyorthovanadate obtained through precipitation is delivered to a fuse piece process, and a finished product is obtained through melting after dehydration and deamination; and (8) leached slags are dried in drying equipment and then subjected to pelletizing with refined iron powder.
Description
Technical field
The present invention relates to Non-ferrous Metallurgy and technical field of ferrous metallurgy, particularly relate to the method for vanadium extraction in the waste material red mud of alumina industry, the pelletizing ironmaking processed of batching sintering.The method effectively can process pentoxide content in red mud at 0.2%-5%, all iron content at the red mud of 20%-45%.
Background technology
China is the big country of alumina producing.Alumina laterite is the waste in aluminum oxide production process, the every annual meeting of alumina industry produces the red mud of tens million of tons.A large amount of red muds can not fully effectively utilize, and large-area stockyard can only be relied on to stack, occupy a large amount of soil, also cause serious pollution to environment.Red mud is accompanied with a large amount of industrial alkali, fluorochemical and other metal etc.Very easily cause the pollution to earth's surface, air, underground water and destruction, and the potential safety hazard that the red mud that lies dormant leaks.The production of the mankind, life are caused directly many-sided and indirectly affected, so reduce output and the harm of red mud to greatest extent, realizes by all kinds of means, the resource utilization of large quantity is extremely urgent.Three kinds of metallic elements that in red mud, content is the highest are respectively iron, aluminium, vanadium.Vanadium is a kind of rare metal, and on market, the value of vanadium product is very high, the metallic element therefore in necessary recovery red mud.New raw material sources can be provided for metal smelting.Make up the deficiency of nature Mineral resources and reduce environmental pollution.Significant to building a resource-conserving society.
Current expert both domestic and external, scholar are doing a lot of work in the comprehensive utilization recovery valuable metal of red mud.But the technique that existing red mud reclaims all is carried out efficiently red mud, comprehensive reutilization.Mainly there are following three problems in the scheme of red mud process now: 1, current most of red mud extract technology is all directly use Ore Leaching red mud, with in and red mud in alkali, and the valuable metals such as extracting directly iron wherein, aluminium, but the content of alkali is very high in red mud, if directly leached with acid, the consumption of acid can be very large, and processing cost can improve.2, the iron that only consideration content is higher, the recovery of aluminium element extract, and this kind of method is less economical, and comprehensive utilization is thorough, and the rate of recovery is lower, infeasible in actual production.3, utilize red mud to make binding agent or batching is baked bricks, though this kind of method make use of red mud, do not develop the valuable metal in the middle of red mud.
The method of Chinese invention patent application number to be the disclosure of the invention of 201410084910.2 a kind of carbothermy reduction aluminium metallurgy red mud direct production ferroaluminium, the method comprises red mud by a certain percentage, iron ore is raw material, melting in electric furnace, striking is heated to molten metal liquid, adds appropriate reductive agent carbon, needs if desired to add certain aluminium ingot, efficient acquisition ferroaluminium, its institute's alloy composition that obtains (quality %) is: C1-5%, Al35-60%, Fe35-60%.Its deficiency existed is: the equipment of use is electric furnace, and energy consumption is high.Real reaction is not thorough, causes the rate of recovery low, and well cannot control the composition of ferro-aluminium.
The method of Chinese invention patent application number a kind of valuable metal such as comprehensive recovery of iron, aluminium, scandium, titanium, vanadium from red mud that has been the disclosure of the invention of 201410121083.X, it is characterized in that, comprise the following steps: red mud mixes with reductive agent and carries out reducing roasting, makes Fe by (1)
2o
3change into Fe
3o
4; (2) Armco magnetic iron concentrate and non-magnetic product is obtained by magnetic separation; (3) non-magnetic product is through ammoniacal liquor stripping aluminum oxide; (4) washed-residue and water are made into ore pulp, as absorption agent, absorb the SO in coal-fired flue-gas
2.Alkali in this process in washed-residue is by SO
2neutralization is dissolved, and pH can drop between 5 to 7; (5) in washed-residue, high density H is added
2sO
4carry out acidolysis, stripping scandium, titanium are in acid hydrolysis solution, and acid hydrolysis residue contains SiO
2, the production of cement and refractory materials can be directly used in; (6) acid hydrolysis solution is heated between 90 DEG C to 100 DEG C, adds metatitanic acid crystal seed, titanium with the form of metatitanic acid by hydrolysis separate out, metatitanic acid through filtration washing again through calcining obtained titanium dioxide; (7) the acid hydrolysis solution 13%P that titanium is later is extracted
20
4, 7%TBP and 80% kerosene as extraction agent, the scandium in extraction solution; (8) solution after extracting scandium, adds in ammoniacal liquor and closes, until the pH value of solution is between 1.8 to 2.2, finally uses 19%P
20
4, 8%TBP and 73% kerosene does extraction agent extraction and obtains vanadium, the remaining liquid cycle applications after extraction is in the alumina leaching of step (3).Its deficiency existed is: the required condition of reaction is harsh, is difficult to accurately control reaction conditions, cannot reaches desirable effect in actual production process.Production process is loaded down with trivial details, and in actual production process, the production cycle is oversize, inefficiencies.The rate of recovery of various metal is low, does not reach the object of comprehensive reutilization.
Summary of the invention
The present invention is exactly for the problems referred to above, makes up the deficiencies in the prior art, provide one efficiently, red mud method of comprehensive utilization economically and reasonably.
For realizing above-mentioned purpose of the present invention, the present invention adopts following technical scheme.
The present invention includes following steps.
Step one: red mud is dried 1h in the drying plant of 110 DEG C, the red mud after oven dry enters ball mill feed bin and carries out fine grinding, the Armco magnetic iron of going out with tramp iron separator in red mud.
Step 2: the red mud after deironing sends into batch bin, and add a certain proportion of sodium carbonate, sodium-chlor, sodium sulfate in batch bin, additional proportion is material: sodium carbonate: sodium-chlor: sodium sulfate=10:1:0.05:0.01, is that mixing of materials is even in batch bin.
Step 3: the material after mixing is delivered to revolution roasting in kilns, and maturing temperature controls at 900 DEG C-1050 DEG C, and roasting time is 1.5h-2h.
Step 4: the sulphuric acid soln being 5.5-6.5 by the grog pH value after roasting leaches at ambient pressure, leaching plant is rubber belt type vacuum filter.
Step 5: by static for leach liquor 15h-20h, delivers to supernatant liquor in the setting tank of precipitation operation.
Step 6: open and stir, adds sulfuric acid neutralization, when solution ph is about 4-5, adds ammonium sulfate, then use sulfuric acid adjust ph to 2-2.5, heating, under agitation condition crystallizable go out orange ammonium poly-vanadate (APV) precipitation.Below the mass concentration 0.10g/L of mother liquor vanadium after precipitation.Wherein acid adding coefficient is 0.9-1.1, and adding ammonium coefficient is 1.0-1.2.
Step 7: gained ammonium poly-vanadate will be precipitated and send into fuse piece operation, and melt film-making after dehydration, deamination, both obtain finished product.
Step 8: dry 2h by the drying plant of leached mud 110 DEG C, dry after and Iron concentrate prepare burden in 1:1 ratio, be pelletizing under the ratio of 7.5%-8.5% in moisture atmosphere, make pellet according to iron making and sintering processing requirement afterwards, gained pellet can be directly used in blast furnace ironmaking.
Compared with prior art beneficial effect of the present invention.
(1) efficient: to adopt a kind of red mud vanadium extraction of the present invention, join the method for ore deposit sintering and effectively can process pentoxide content at 0.2%-5%, all iron content at the red mud of 20%-45%.In leach liquor, P content has reached precipitation standard without the need to carrying out dephosphorization operation again, shortens the production cycle, improves production efficiency.
(2) economical: to adopt a kind of red mud vanadium extraction of the present invention, join the method for ore deposit sintering and can fully utilize red mud to greatest extent, obtain maximum economic benefit.
(3) reasonable: a kind of red mud vanadium extraction of the present invention, what join that the method for ore deposit sintering adopts is the production method of smelting iron after first vanadium extraction, the transformation efficiency of the vanadium of guarantee.
Embodiment
Choose the red mud of three kinds of different grades, use the inventive method process respectively.
Embodiment 1: test with the red mud of the inventive method to Henan factory, in this red mud pentoxide content 4.6%, all iron content is 32.5%.
Step one: red mud is dried 1h in the drying plant of 110 DEG C, the red mud after oven dry enters ball mill feed bin and carries out fine grinding, the Armco magnetic iron of going out with tramp iron separator in red mud.
Step 2: the red mud after deironing sends into batch bin, and add a certain proportion of sodium carbonate, sodium-chlor, sodium sulfate in batch bin, additional proportion is material: sodium carbonate: sodium-chlor: sodium sulfate=10:1:0.05:0.01, is that mixing of materials is even in batch bin.
Step 3: the material after mixing is delivered to revolution roasting in kilns, and maturing temperature controls at 950 DEG C, and roasting time is 2h.
Step 4: the sulphuric acid soln being 6.5 by the grog pH value after roasting leaches at ambient pressure, leaching plant is rubber belt type vacuum filter.
Step 5: by static for leach liquor 18h, delivers to supernatant liquor in the setting tank of precipitation operation.
Step 6: open and stir, adds sulfuric acid neutralization, when solution ph is about 4-5, adds ammonium sulfate, then use sulfuric acid adjust ph to 2-2.5, heating, under agitation condition crystallizable go out orange ammonium poly-vanadate (APV) precipitation.Below the mass concentration 0.10g/L of mother liquor vanadium after precipitation.Wherein acid adding coefficient is 1.1, and adding ammonium coefficient is 1.2.
Step 7: gained ammonium poly-vanadate will be precipitated and send into fuse piece operation, and melt film-making after dehydration, deamination, both obtain finished product.
Step 8: dry 2h by the drying plant of leached mud 110 DEG C, dry after and Iron concentrate prepare burden in 1:1 ratio, be pelletizing under the ratio of 8.5% in moisture atmosphere, make pellet according to iron making and sintering processing requirement afterwards, gained pellet can be directly used in blast furnace ironmaking.
Embodiment 2: test with the red mud of the inventive method to Shandong factory, in this red mud pentoxide content 1.8%, all iron content is 41.3%.
Step one: red mud is dried 1h in the drying plant of 110 DEG C, the red mud after oven dry enters ball mill feed bin and carries out fine grinding, the Armco magnetic iron of going out with tramp iron separator in red mud.
Step 2: the red mud after deironing sends into batch bin, and add a certain proportion of sodium carbonate, sodium-chlor, sodium sulfate in batch bin, additional proportion is material: sodium carbonate: sodium-chlor: sodium sulfate=10:1:0.05:0.01, is that mixing of materials is even in batch bin.
Step 3: the material after mixing is delivered to revolution roasting in kilns, and maturing temperature controls at 1000 DEG C, and roasting time is 1.5h.
Step 4: the sulphuric acid soln being 6.5 by the grog pH value after roasting leaches at ambient pressure, leaching plant is rubber belt type vacuum filter.
Step 5: by static for leach liquor 16h, delivers to supernatant liquor in the setting tank of precipitation operation.
Step 6: open and stir, adds sulfuric acid neutralization, when solution ph is about 4-5, adds ammonium sulfate, then use sulfuric acid adjust ph to 2-2.5, heating, under agitation condition crystallizable go out orange ammonium poly-vanadate (APV) precipitation.Below the mass concentration 0.10g/L of mother liquor vanadium after precipitation.Wherein acid adding coefficient is 0.9, and adding ammonium coefficient is 1.2.
Step 7: gained ammonium poly-vanadate will be precipitated and send into fuse piece operation, and melt film-making after dehydration, deamination, both obtain finished product.
Step 8: dry 2h by the drying plant of leached mud 110 DEG C, dry after and Iron concentrate prepare burden in 1:1 ratio, be pelletizing under the ratio of 7.5% in moisture atmosphere, make pellet according to iron making and sintering processing requirement afterwards, gained pellet can be directly used in blast furnace ironmaking.
Embodiment 3: test with the red mud of the inventive method to Shanxi factory, in this red mud pentoxide content 1.1%, all iron content is 39.4%.
Step one: red mud is dried 1h in the drying plant of 110 DEG C, the red mud after oven dry enters ball mill feed bin and carries out fine grinding, the Armco magnetic iron of going out with tramp iron separator in red mud.
Step 2: the red mud after deironing sends into batch bin, and add a certain proportion of sodium carbonate, sodium-chlor, sodium sulfate in batch bin, additional proportion is material: sodium carbonate: sodium-chlor: sodium sulfate=10:1:0.05:0.01, is that mixing of materials is even in batch bin.
Step 3: the material after mixing is delivered to revolution roasting in kilns, and maturing temperature controls at 1050 DEG C, and roasting time is 2h.
Step 4: the sulphuric acid soln being 6.5 by the grog pH value after roasting leaches at ambient pressure, leaching plant is rubber belt type vacuum filter.
Step 5: by static for leach liquor 20h, delivers to supernatant liquor in the setting tank of precipitation operation.
Step 6: open and stir, adds sulfuric acid neutralization, when solution ph is about 4-5, adds ammonium sulfate, then use sulfuric acid adjust ph to 2-2.5, heating, under agitation condition crystallizable go out orange ammonium poly-vanadate (APV) precipitation.Below the mass concentration 0.10g/L of mother liquor vanadium after precipitation.Wherein acid adding coefficient is 1.1, and adding ammonium coefficient is 1.0.
Step 7: gained ammonium poly-vanadate will be precipitated and send into fuse piece operation, and melt film-making after dehydration, deamination, both obtain finished product.
Step 8: dry 2h by the drying plant of leached mud 110 DEG C, dry after and Iron concentrate prepare burden in 1:1 ratio, be pelletizing under the ratio of 8.5% in moisture atmosphere, make pellet according to iron making and sintering processing requirement afterwards, gained pellet can be directly used in blast furnace ironmaking.
Claims (4)
1. red mud vanadium extraction, join ore deposit sintering a method, it is characterized in that:
Step one: red mud is dried 1h in the drying plant of 110 DEG C, the red mud after oven dry enters ball mill feed bin and carries out fine grinding, the Armco magnetic iron of going out with tramp iron separator in red mud;
Step 2: the red mud after deironing sends into batch bin, and add a certain proportion of sodium carbonate, sodium-chlor, sodium sulfate in batch bin, additional proportion is material: sodium carbonate: sodium-chlor: sodium sulfate=10:1:0.05:0.01, is that mixing of materials is even in batch bin;
Step 3: the material after mixing is delivered to revolution roasting in kilns, and maturing temperature controls at 900 DEG C-1050 DEG C, and roasting time is 1.5h-2h;
Step 4: the sulphuric acid soln being 5.5-6.5 by the grog pH value after roasting leaches at ambient pressure, leaching plant is rubber belt type vacuum filter;
Step 5: by static for leach liquor 15h-20h, delivers in the setting tank of precipitation operation by supernatant liquor;
Step 6: open and stir, add sulfuric acid neutralization, when solution ph is about 4-5, add ammonium sulfate, use sulfuric acid adjust ph to 2-2.5 again, heating, under agitation condition crystallizable go out orange ammonium poly-vanadate (APV) precipitation, below the mass concentration 0.10g/L of mother liquor vanadium after precipitation, wherein acid adding coefficient is 0.9-1.1, and adding ammonium coefficient is 1.0-1.2;
Step 7: gained ammonium poly-vanadate will be precipitated and send into fuse piece operation, and melt film-making after dehydration, deamination, both obtain finished product;
Step 8: dry 2h by the drying plant of leached mud 110 DEG C, dry after and Iron concentrate prepare burden in 1:1 ratio, be pelletizing under the ratio of 7.5%-8.5% in moisture atmosphere, make pellet according to iron making and sintering processing requirement afterwards, gained pellet can be directly used in blast furnace ironmaking.
2. a kind of red mud vanadium extraction as claimed in claim 1, join the method for ore deposit sintering, it is characterized in that: use the alkali in Vanadium Pentoxide in FLAKES trade effluent and in red mud.
3. a kind of red mud vanadium extraction as claimed in claim 1, join ore deposit sintering method, it is characterized in that: ratio of components is material: sodium carbonate: sodium-chlor: sodium sulfate=10:1:0.05:0.01.
4. a kind of red mud vanadium extraction as claimed in claim 1, join the method for ore deposit sintering, it is characterized in that: grog leaches and adopts subacidity normal pressure leaching, to leach solution used be pH value is the sulphuric acid soln of 5.5-6.5.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110331289A (en) * | 2019-07-02 | 2019-10-15 | 广西大学 | A method of recycling scandium and sodium sulphate from Bayer process red mud |
| CN110878388A (en) * | 2019-11-29 | 2020-03-13 | 四川大裂谷钒业有限公司 | Method for roasting vanadium-containing material by using chain grate and rotary kiln |
| CN113122720A (en) * | 2019-12-31 | 2021-07-16 | 中国科学院过程工程研究所 | Method for synchronously extracting aluminum, titanium, iron and sodium from red mud |
| CN116024443A (en) * | 2023-03-30 | 2023-04-28 | 湖南东方钪业股份有限公司 | Recovery method of scandium metal |
-
2014
- 2014-07-31 CN CN201410368976.4A patent/CN105316479A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110331289A (en) * | 2019-07-02 | 2019-10-15 | 广西大学 | A method of recycling scandium and sodium sulphate from Bayer process red mud |
| CN110878388A (en) * | 2019-11-29 | 2020-03-13 | 四川大裂谷钒业有限公司 | Method for roasting vanadium-containing material by using chain grate and rotary kiln |
| CN113122720A (en) * | 2019-12-31 | 2021-07-16 | 中国科学院过程工程研究所 | Method for synchronously extracting aluminum, titanium, iron and sodium from red mud |
| CN113122720B (en) * | 2019-12-31 | 2022-09-06 | 中国科学院过程工程研究所 | Method for synchronously extracting aluminum, titanium, iron and sodium from red mud |
| CN116024443A (en) * | 2023-03-30 | 2023-04-28 | 湖南东方钪业股份有限公司 | Recovery method of scandium metal |
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Application publication date: 20160210 |