CN106868308A - The extracting method of iron in a kind of autunezite slag - Google Patents
The extracting method of iron in a kind of autunezite slag Download PDFInfo
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- CN106868308A CN106868308A CN201710091764.XA CN201710091764A CN106868308A CN 106868308 A CN106868308 A CN 106868308A CN 201710091764 A CN201710091764 A CN 201710091764A CN 106868308 A CN106868308 A CN 106868308A
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- iron
- ore pulp
- autunezite
- extracting method
- slag
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C—MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03C1/00—Magnetic separation
- B03C1/02—Magnetic separation acting directly on the substance being separated
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The present invention relates to a kind of extracting method of iron in autunezite slag, the extracting method of iron in a kind of autunezite slag, Jarosite Residues are after broken, fine grinding plus caustic solution is made certain density ore pulp, and the liquid-solid ratio of ore pulp is 0.8~4:1;Ore pulp is mixed with carbohydrate biomass in reactor, Jarosite Residues and carbohydrate biomass ratio are 1.2~3.5 in ore pulp:1;Under 200~450 DEG C of hydrothermal condition, 2~8h is reacted;Reacted solid-liquid separation on ore pulp, the liquid after separation obtains organic acid, polyalcohol through UF membrane;Solid product after separation isolates Fe through magnetic separation process3O4, Fe3O4The rate of recovery is not less than 80%.The present invention proposes full technical strategies for the resource reclaim comprehensive utilization of Jarosite Residues.After solid product carries out magnetic separation, the interference of ferro element is eliminated, other valuable metals create advantage to Jarosite Residues high efficiente callback, realize the high-efficiency comprehensive utilization of Jarosite Residues.
Description
Technical field
The present invention relates to a kind of method that low-grade difficulty selects the comprehensive utilization of Jarosite Residues resource reclaim, belong to green metallurgical
Technical field, the method that iron is extracted in more particularly to a kind of utilization biomass by hydro-thermal reduction Jarosite Residues.
Background technology
China is zinc production and consumption big country, and more than 80% zinc abstraction factory selects zinc hydrometallurgy, and wherein more than half is adopted
Iron is removed with jarosite process, the half that the quantity of slag is about zinc yield is often produced per year.The general iron content of Jarosite Residues is 20~27%, but
Iron cost recovery is too high, and many factories are not handled by, and directly store up.The loss of a large amount of metals is not only caused, while also right
Surrounding enviroment cause huge harm.
Current autunezite Slag treatment essentially consists in the recovery and harmless treatment of valuable metal.The siderotil commonly used at present
Slag decomposition method has two kinds of pyrogenic process and wet processing:Pyrogenic process is mainly the Roasting Decomposition of siderotil;Wet method includes that acid is decomposed and alkali point
Solution.Pyrogenic attack technique is mainly used in volatilization recovery of extraction, ammonium and the sulfur dioxide of indium etc.;Wet processing process lays particular emphasis on iron
Extraction after alum decomposition to metals such as silver, iron is reclaimed.But because investment and operating cost are high, energy consumption is big, secondary environmental pollution
The problems such as, these technologies are all no can be used widely.As environmental protection and low-carbon (LC) idea are goed deep into, people are to metallic zinc smelting
The high energy consumption of refining process and high pollution are increasingly paid close attention to, in the urgent need to efficient, low-carbon (LC), the smelting process of environmental protection.In view of a variety of existing
Shape problem, it is necessary to develop the handling process of a kind of low energy consumption, high yield, solves the accumulation pollution problem of Jarosite Residues, with
Realize the green smelting of metal.
Biomass refer generally to agricultural and forest trimmings, such as wood chip, rice chaff, bagasse, peanut shell, coconut husk, stalk.Biomass
Mainly it is made up of glucide, they are the aldehydes or ketones of polyhydroxy.Under hydrothermal condition more than 250 DEG C, biomass decomposable asymmetric choice net
It is the materials such as the rudimentary organic carboxyl acid such as formic acid, acetic acid, ethanol and acetone, aldehyde, ketone and alcohol, aldehyde radical, ketone group, hydroxyl all have
The functional group of good reducing activity.Meanwhile, extensively, low cost is environment-friendly, therefore can serve as metal compound for biomass source
The reducing agent of thing.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of extracting method of iron in autunezite slag, solve low product
Position difficulty selects Jarosite Residues resource reclaim problem of complex utilization.
To achieve the above object, the present invention is realized using following technical scheme:
A kind of extracting method of iron in autunezite slag, Jarosite Residues add caustic solution system after broken, fine grinding
Into certain density ore pulp, the liquid-solid ratio of ore pulp is 0.8~4:1;Ore pulp and carbohydrate biomass are mixed in reactor
Close, Jarosite Residues and carbohydrate biomass ratio are 1.2~3.5 in ore pulp:1;In 200~450 DEG C of hydrothermal condition
Under, react 2~8h;Reacted solid-liquid separation on ore pulp, the liquid after separation obtains organic acid, polyalcohol through UF membrane;Separate
Solid product afterwards isolates Fe through magnetic separation process3O4, Fe3O4The rate of recovery is not less than 80%.
Described magnetic separation process, solid product is separated after drying, fine grinding into wet magnetic separator magnetic separation.
All iron content is not less than 20% in described Jarosite Residues.
The Jarosite Residues grinding particle size is 100~600 mesh.
The sodium hydroxide solution that described caustic solution is deployed into for industrial sodium hydroxide, concentration of lye is with [Na2O] meter
It is 8~50g/L.
Described carbohydrate biomass, selected from glucose, fructose, sucrose, maltose, cellulose or rich in fiber
Element material in one or more.
The described material rich in cellulose, selected from agricultural and/or forest trimmings in wood chip, rice chaff, bagasse, peanut shell,
One or more in coconut husk, stalk.
When carbohydrate biomass for agricultural and/or during forest trimmings, it is necessary to by they be crushed to particle diameter 0.1~
10mm。
Compared with prior art, the beneficial effects of the invention are as follows:
(1) after solid product carries out magnetic separation, the interference of ferro element is eliminated, other are valuable to Jarosite Residues high efficiente callback
Metal (such as silver, indium) creates advantage, realizes the high-efficiency comprehensive utilization of Jarosite Residues.
(2) compared with reduction roasting technique, with reducing agent wide material sources, low cost, environment-friendly advantage was produced
Journey avoids the high energy consumption of pyrometallurgy, and without SO2The discharge of flue gas and dust, is a kind of metal smelt technique of green.Should
Method is that the exploitation of low-carbon (LC) smelting technique Green reducing agent and biomass recycling use provide new approaches.
(3) Fe is being obtained3O4While, organic acid, the chemicals of polyalcohol high added value are obtained, realize the money of biomass
Sourceization is utilized.
Brief description of the drawings
Fig. 1 is flow chart of the invention.
Specific embodiment
With reference to embodiment, the present invention is further described:
The present invention will be described in detail for following examples.These embodiments are only that preferred embodiment of the invention is entered
Row description, does not limit the scope of the present invention.
Such as Fig. 1:A kind of extracting method of iron in autunezite slag, Jarosite Residues add caustic alkali after broken, fine grinding
Solution is made certain density ore pulp, and ore pulp is mixed with carbohydrate biomass in reactor, at 200~450 DEG C
Under hydrothermal condition, 2~8h is reacted;Reacted solid-liquid separation on ore pulp, liquid after separation goes out organic acid, polynary through UF membrane
Alcohol;Solid product isolates Fe through magnetic separation process after after separation3O4。
Embodiment 1
By 18g Jarosite Residues through crushing, being finely ground to 100 mesh (150 μm), with concentration of lye with [Na2O] it is calculated as 13.5g/
The caustic solution of L is mixed and made into the ore pulp that liquid-solid ratio is 2.0, and all iron content is not less than 20% in Jarosite Residues.By ore pulp
It is mixed to join in autoclave with cellulose, the autunezite quantity of slag in ore pulp is 5 with biomass thing ratio:2;245
DEG C leaching condition under, dissolution pressure be 4MPa, dissolution time is 5h, and the iron ion in Jarosite Residues in ore pulp is by fiber
Element is efficiently reduced to ferromagnetic Fe3O4, reacted solid-liquid separation on ore pulp, the liquid after separation obtains organic acid through UF membrane
And polyalcohol;Solid product after separation isolates Fe after drying, fine grinding into wet magnetic separator magnetic separation3O4, Fe3O4Return
Yield is up to 85.3%.
Embodiment 2
By 28g Jarosite Residues through crushing, being finely ground to 200 mesh (74 μm), with concentration of lye with [Na2O] it is calculated as 15g/L's
It is 4 that caustic solution is mixed and made into liquid-solid ratio:1 ore pulp, ore pulp and cellulose is mixed to join in autoclave, ore pulp
In the autunezite quantity of slag and biological quality ratio be 7:2;Under 260 DEG C of leaching condition, dissolution pressure is 5MPa, during dissolution
Between be 3h, the iron ion in Jarosite Residues in ore pulp is efficiently reduced to ferromagnetic Fe by cellulose3O4, reacted ore deposit
Slurry separation of solid and liquid, the liquid after separation obtains organic acid and polyalcohol through UF membrane;Solid product after separation is through drying, fine grinding
Afterwards Fe is isolated into wet magnetic separator magnetic separation3O4, the rate of recovery of iron is up to 81.8%
Embodiment 3
By 20g Jarosite Residues through crushing, being finely ground to 140 mesh (105 μm), with concentration of lye with [Na2O] it is calculated as 14.3g/
It is 3 that the caustic solution of L is mixed and made into liquid-solid ratio:1 ore pulp, all iron content is not less than 20% in Jarosite Residues.By stalk
Below particle diameter 1mm is crushed to, stalk after crushed is mixed to join in autoclave with ore pulp, the autunezite in ore pulp
The quantity of slag is 5 with biological quality ratio:4;Under 275 DEG C of leaching condition, dissolution pressure is 5MPa, and dissolution time is 4h, ore pulp
In Jarosite Residues in iron ion ferromagnetic Fe is reduced to by biomass efficient3O4, reacted solid-liquid separation on ore pulp,
Liquid after separation obtains organic acid and polyalcohol through UF membrane;Solid product after separation enters wet type after drying, fine grinding
Fe is isolated in magnetic separator magnetic separation3O4, the rate of recovery of iron reaches 80.1%.
Embodiment 4
By 15g Jarosite Residues through crushing, being finely ground to 200 mesh (74 μm), with concentration of lye with [Na2O] it is calculated as 20g/L's
It is 2 that caustic solution is mixed and made into liquid-solid ratio:1 ore pulp, ore pulp and sucrose is mixed to join in autoclave, in ore pulp
The autunezite quantity of slag and biological quality ratio be 3:1;Under 260 DEG C of leaching condition, dissolution pressure is 5MPa, dissolution time
It is 6h, the iron ion in Jarosite Residues in ore pulp is efficiently reduced to ferromagnetic Fe by sucrose3O4, reacted ore pulp consolidate
Liquid is separated, and the liquid after separation obtains organic acid and polyalcohol through UF membrane;Solid product after separation is laggard through drying, fine grinding
Enter wet magnetic separator magnetic separation and isolate Fe3O4, the rate of recovery of iron is up to 82.5%
Embodiment 5
By 15g Jarosite Residues through crushing, being finely ground to 180 mesh (88 μm), with concentration of lye with [Na2O] it is calculated as 25.5g/L
Caustic solution be mixed and made into liquid-solid ratio for 2.5:1 ore pulp, all iron content is not less than 20% in Jarosite Residues.By peanut
Shell and crushed stalk to below particle diameter 1mm, peanut shell after crushed and stalk are mixed to join in autoclave with ore pulp,
The autunezite quantity of slag and biological quality ratio in ore pulp are 2:1;Under 275 DEG C of leaching condition, dissolution pressure is 5MPa, molten
Go out the time for 6h, the iron ion in Jarosite Residues in ore pulp is reduced to ferromagnetic Fe by biomass efficient3O4, after reaction
Solid-liquid separation on ore pulp, the liquid after separation obtains organic acid and polyalcohol through UF membrane;Solid product after separation through drying,
After fine grinding Fe is isolated into wet magnetic separator magnetic separation3O4, the rate of recovery of iron reaches 82.6%.
Claims (8)
1. in a kind of autunezite slag iron extracting method, it is characterised in that Jarosite Residues are after broken, fine grinding plus causticity
Aqueous slkali is made certain density ore pulp, and the liquid-solid ratio of ore pulp is 0.8~4:1;By ore pulp with carbohydrate biomass anti-
Mixing in kettle is answered, Jarosite Residues and carbohydrate biomass ratio are 1.2~3.5 in ore pulp:1;At 200~450 DEG C
Under hydrothermal condition, 2~8h is reacted;Reacted solid-liquid separation on ore pulp, liquid after separation obtains organic acid, polynary through UF membrane
Alcohol;Solid product after separation isolates Fe through magnetic separation process3O4, Fe3O4The rate of recovery is not less than 80%.
2. in a kind of autunezite slag according to claim 1 iron extracting method, it is characterised in that described magnetic separation
Technique is that solid product is separated after drying, fine grinding into wet magnetic separator magnetic separation.
3. in a kind of autunezite slag according to claim 1 iron extracting method, it is characterised in that described yellow potassium
All iron content is not less than 20% in iron vitriol slag.
4. in a kind of autunezite slag according to claim 1 iron extracting method, it is characterised in that the yellow potassium iron
Alum slag grinding particle size is 100~600 mesh.
5. in a kind of autunezite slag according to claim 1 iron extracting method, it is characterised in that described causticity
The sodium hydroxide solution that aqueous slkali is deployed into for industrial sodium hydroxide, concentration of lye is with [Na2O] it is calculated as 8~50g/L.
6. in a kind of autunezite slag according to claim 1 iron extracting method, it is characterised in that described carbon water
Compound biomass, selected from the one kind in glucose, fructose, sucrose, maltose, cellulose or material rich in cellulose or
It is several.
7. in a kind of autunezite slag according to claim 6 iron extracting method, it is characterised in that described is rich in
The material of cellulose, selected from the one kind in agricultural and/or forest trimmings in wood chip, rice chaff, bagasse, peanut shell, coconut husk, stalk or
It is several.
8. in a kind of autunezite slag according to claim 1-7 any one iron extracting method, it is characterised in that
When carbohydrate biomass are for agricultural and/or forest trimmings, it is necessary to they are crushed into 0.1~10mm of particle diameter.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107779597A (en) * | 2017-10-11 | 2018-03-09 | 大连理工大学 | A kind of method using biomass solution iron purification |
CN110040784A (en) * | 2019-04-25 | 2019-07-23 | 兰州理工大学 | A kind of method that Jarosite Residues prepare magnetic iron oxide micro mist |
CN115094240A (en) * | 2022-07-25 | 2022-09-23 | 中南大学 | Method for separating iron and lead and enriching iron element in iron-containing waste residue |
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CN102888515A (en) * | 2012-10-12 | 2013-01-23 | 金川集团股份有限公司 | Comprehensive utilization method of amarillite slag |
CN103993182A (en) * | 2014-05-07 | 2014-08-20 | 西安建筑科技大学 | Comprehensive recovery method for secondary resources in iron vitriol slag |
CN105238924A (en) * | 2015-10-23 | 2016-01-13 | 辽宁科技大学 | Method for extracting aluminum and iron from high-iron diasporic bauxite |
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2017
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Patent Citations (3)
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CN102888515A (en) * | 2012-10-12 | 2013-01-23 | 金川集团股份有限公司 | Comprehensive utilization method of amarillite slag |
CN103993182A (en) * | 2014-05-07 | 2014-08-20 | 西安建筑科技大学 | Comprehensive recovery method for secondary resources in iron vitriol slag |
CN105238924A (en) * | 2015-10-23 | 2016-01-13 | 辽宁科技大学 | Method for extracting aluminum and iron from high-iron diasporic bauxite |
Non-Patent Citations (1)
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107779597A (en) * | 2017-10-11 | 2018-03-09 | 大连理工大学 | A kind of method using biomass solution iron purification |
CN110040784A (en) * | 2019-04-25 | 2019-07-23 | 兰州理工大学 | A kind of method that Jarosite Residues prepare magnetic iron oxide micro mist |
CN110040784B (en) * | 2019-04-25 | 2021-09-21 | 兰州理工大学 | Method for preparing magnetic iron oxide micro powder from jarosite slag |
CN115094240A (en) * | 2022-07-25 | 2022-09-23 | 中南大学 | Method for separating iron and lead and enriching iron element in iron-containing waste residue |
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Application publication date: 20170620 |