CN103088208A - Method for treating manganese-containing and phosphorus-containing hematite - Google Patents
Method for treating manganese-containing and phosphorus-containing hematite Download PDFInfo
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- CN103088208A CN103088208A CN2013100156867A CN201310015686A CN103088208A CN 103088208 A CN103088208 A CN 103088208A CN 2013100156867 A CN2013100156867 A CN 2013100156867A CN 201310015686 A CN201310015686 A CN 201310015686A CN 103088208 A CN103088208 A CN 103088208A
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Abstract
A method for treating manganese-containing and phosphorus-containing hematite relates to a method for comprehensively recovering iron and manganese in the manganese-containing and phosphorus-containing hematite. The method is characterized in that the treatment process sequentially comprises the following steps: crushing raw hematite ore containing manganese and phosphorus, and then uniformly mixing the crushed raw hematite ore and powdered coal to prepare granules; carrying out reduction roasting on the granules; performing high-temperature water quenching and ball milling; performing magnetic separation to obtain concentrate iron powder and tailings; carrying out sulfuric acid leaching and filtering on the tailings, and purifying and removing impurities from filtrate; concentrating and crystallizing the purified solution to prepare manganese sulfate. The method has wide applicability, the raw ore does not need to be finely ground, coke and coking coal are not needed in the metallization roasting process, and the separation effect of Fe, Mn and P after the roasted sand is subjected to ball milling and magnetic separation is good; the magnetic separation tailings have good manganese enrichment effect, and a refined manganese sulfate product is prepared by adopting a conventional leaching agent for sulfuric acid leaching, impurity removal, concentration and crystallization; the equipment used in the process is mature, the automation degree is high, the control is easy, the environmental pollution is low, and the product output value is high.
Description
Technical field
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese relates to a kind of comprehensive iron that contains in the phosphorous rhombohedral iron ore of manganese and method of manganese of reclaiming of the phosphorous rhombohedral iron ore of manganese that contain.
Background technology
At present, production capacity continuous rise due to China's steel products, the iron alloy demand is also increased severely, but the consequent energy, resource, blowdown presssure are huge, along with the pay attention to day by day of international community to environmental protection, the shortage of the resource such as manganese ore, iron ore, people constantly seek the method for comprehensive utilization of the lean ores such as low-grade manganese, jacobsite, phosphorous oolitic hematite.
Contain manganese rhombohedral iron ore reserves both at home and abroad large, but because these mineral contain manganese, phosphorous, the iron grade is low, the Yi Cainan choosing, and manganese, iron, phosphorus is not easily separated etc., and reason is not used appropriately so far.In this type of ore deposit, iron is mainly with Fe
2O
3Form exist, contain Fe 30～46%, MnO 5～10%, P
2O
50.3～1.5%, Al
2O
33～10%, SiO
210～20% etc.This type of ore grade is low, the difficult smelting, the mechanical beneficiation method can not be with the separation between iron and manganese in this type of ore deposit and enrichment, so that this class ore can not be smelted iron, can not be the raw material of iron alloy as manganese, be regarded as the rubbish ore deposit always and abandon, how economical research is, reasonably utilize the low-grade manganese rhombohedral iron ore that contains, to alleviating China's manganese, contradiction that iron ore deposit is in short supply, guaranteeing that the Sustainable development of ferromanganese industry has very important strategic importance.
The prior art processing contains the manganese low-grade iron ore or poor manganese ore mainly adopts: magnetizing roasting-magnetic method, rich manganese slag method.
Magnetizing roasting-magnetic method: allocate jacobsite into the reducing agent low temperature magnetizing roasting, calcining is levigate carries out weak magnetic separation iron after dissociating to mineral monomer, the strong magnetic of weakly magnetic tailings recycling improves the grade of manganese, can obtain the iron ore concentrate of iron grade～50%, the rate of recovery～60% and the mine tailing of manganese grade 5～20%, it is low that the method is processed iron concentrate grade, the rate of recovery is low, and the mine tailing iron content is high, it is low to contain Mn.
Rich manganese slag method: take blast furnace as major equipment, control suitable furnace temperature, make Fe, P reduction as far as possible, and Mn few reduction as far as possible is enriched in Mn in slag, obtains high manganese slag.Comparatively advanced is blast furnace two step method poor manganese ore ferromanganese smelting novel process, the first step of this technique is to the poor manganese ore selective reduction in blast furnace, obtain rich manganese slag, second step is in another blast furnace, with rich manganese slag collocation part high alkalinity magnesium oxide agglomerate, produce carbon element ferromanganese, but the method is high to the manganese content requirement, is only limited to and processes the ferrous manganese ore that contains manganese 23～30%.The treatment process of patent CN88104767.8 is the improvement of blast furnace two step method, can process and contain manganese 10～28%, iron content is more than 20%, the poor manganese ore of Mn/Fe=0.2～2.0, its fs is take rotary kiln as reduction apparatus, adopt coal to make reductive agent, obtain solid-state Fe and Mn, subordinate phase utilizes smelting furnace that the solid product of fs is melted minute, obtain rich manganese slag and molten iron, yet these class methods all can't process contain MnO 5～10% contain the manganese rhombohedral iron ore, and energy consumption is high, cost is high.
In recent years a large amount of research has been done to the sorting of ferromanganese ore by the U.S., result shows: process the including Mn-Fe ore and should adopt Chemical Leaching to process, mainly comprise: ammonium carbamate extraction process, sulphate process, reducing roasting-lixiviation process, reducing roasting-sulfuric acid leaching, Bioleaching method and chlorination process etc.But not yet work out a kind of scale operation that is suitable for, treatment process with certain economic benefit.
Summary of the invention
The objective of the invention is the deficiency for above-mentioned technology existence, a kind of energy high efficiency separation ferromanganese is provided, obtain low-phosphorous high-quality molten iron and POV manganese, good product quality, the ferrimanganic rate of recovery is high, cost is low, and environmental pollution is little, and that easily realizes suitability for industrialized production can comprehensively reclaim the treatment process that contains the phosphorous rhombohedral iron ore of manganese.
The objective of the invention is to be achieved through the following technical solutions.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese is characterized in that the step of its treating processes comprises successively:
(1) will contain after the phosphorous rhombohedral iron ore crushing raw ore of manganese and the fine coal mixing, make pellet;
(2) pellet is carried out reducing roasting;
(3) carry out the high-temperature water quenching ball milling;
(4) carry out the magnetic separation separation and obtain concentrate iron powder and mine tailing;
(5) mine tailing is carried out sulfuric acid leaching, filtration, the filtrate purification and impurity removal;
(6) purify rear liquid condensing crystal and prepare manganous sulfate.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention, it is characterized in that the particle size after cracking that will contain the phosphorous rhombohedral iron ore crushing raw ore of manganese process of step (1) is for surpassing 85% less than 3mm, after the fine coal mixing that accounts for raw ore weight 15%～30%, an ore deposit diameter of making is 10～30mm.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention is characterized in that described fine coal is one or more in bituminous coal, hard coal, brown coal.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention, what it is characterized in that step (2) carries out reducing roasting process with pellet, reducing roasting equipment adopts a kind of in rotary kiln, rotary hearth furnace, multiple hearth furnace, thermal source is coal gas or coal, combustion-supporting gas is air, the high-temperature zone temperature is 900～1050 ℃, and the high-temperature zone residence time is 0.5～3h, controls out kiln gas CO/CO
2Be 3.5～4.5.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention, what it is characterized in that step (3) carries out the shrend mechanical milling process with the high temperature calcining, through sealing after cooling cylinder is cooled to 400～750 ℃ with calcining, carry out shrend chilling, ball milling, after ball milling, the ore particle degree is for to account for 85%～95% less than 0.074mm.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention, it is characterized in that the magnetic separation sepn process of step (4), that ball milling ore pulp with step (3) carries out magnetic separation, advance ore deposit pulp solids mass concentration and be controlled at 15%～25%, magneticstrength is controlled at 800～1500 oersteds, obtains concentrate iron powder and mine tailing.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention, molten minute of the iron powder that step (4) obtains adds 0.1～2% slag former, and described slag former is CaO, CaCO
3In one or both; Temperature is controlled 1550～1650 ℃, and time 0.5～3h can make low-phosphorous high-quality molten iron.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention, the concentration that it is characterized in that the sulphuric acid soln that the sulfuric acid leaching process that mine tailing is carried out of step (5) adopts is 0.8～1.5mol/L, liquid-solid ratio is 2～5:1,50～90 ℃ of extraction temperatures, extraction time 1～4h leaches endpoint pH and controls 1～1.5.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention is characterized in that the filtrate purification and impurity removal process of step (5) is that filtrate is adjusted pH value to 2.5～5.0, after filtration, washing is purified rear manganese sulfate solution.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention, the filtrate purification and impurity removal process that it is characterized in that step (5) is to add CaO, CaCO in filtrate
3, one or more in Wingdale adjust pH.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention is characterized in that described step (6) is the manganese sulfate solution condensing crystal that step (5) is obtained, and after centrifuging, gained manganous sulfate crystal grain is dry, makes POV manganese; Described condensing crystal process adopts triple-effect evaporator, enamel still or whizzer.
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese of the present invention, allocating fine coal after crushing raw ore into granulates, pellet metallization reducing roasting-magnetic separation can be phosphorous less than 0.01% high-quality molten iron with concentrate preparation in molten minute, and mine tailing dilute sulphuric acid leaching-removal of impurities-condensing crystal prepares POV manganese.Compare with traditional processing poor manganese ore, the method for jacobsite, the method suitability is wide, to manganese content without particular requirement; Raw ore need not fine grinding, directly be crushed to less than 3mm and get final product, the metallization roasting process need not coke and coking coal, Fe, Mn, P good separating effect after the magnetic separation of calcining ball milling, molten minute output of gained concentrate iron powder electric furnace is phosphorous less than 0.01% low-phosphorous molten iron, can be used as the high quality raw material of steel-making; The magnetic tailing rich manganese is effective, adopts conventional leaching agent sulfuric acid leaching, makes the POV manganese product after removal of impurities, condensing crystal; The technological process equipment used is ripe, and level of automation is high, is easy to control, and environmental pollution is little, and product value is high.
Method of the present invention is processed and is contained the phosphorous rhombohedral iron ore of manganese, metallization roasting-magnetic separation process, and iron elimination factor 90～95%, phosphorus decreasing ratio 88～95%, in the concentrate iron powder: Fe 85～95%, and P 0.05～0.15%, and Mn 0.5～1.0%, Al
2O
3＜2%, SiO
2＜4%; A molten minute preparation high-quality molten iron process: iron recovery is greater than 98%, phosphorus decreasing ratio 95～99%, P in molten iron～0.005%; Preparation POV manganese process: manganese recovery ratio is greater than 85%, manganous sulfate (MnSO in the product purification manganous sulfate
4H
2O) content is greater than 98%.
Description of drawings
The process flow sheet of Fig. 1 the inventive method.
Embodiment
A kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese to contain the phosphorous rhombohedral iron ore of manganese as raw material, is allocated reductive agent into after fragmentation, mixed pelletization, pellet metallization reducing roasting-magnetic separation, molten minute preparation high-quality molten iron of concentrate, mine tailing sulfuric acid leaching-purification-condensing crystal prepares POV manganese.The method mainly comprises the steps:
1, contain the phosphorous rhombohedral iron ore crushing raw ore of manganese, garrulous ore granularity surpasses 85% less than 3mm, and particle is allocated 15～30% fine coal into, granulates after mixing, and pellet diameter is 10～30mm.
2, with step 1 an ore deposit metallization reducing roasting, control 950～1050 ℃ of temperature, recovery time 0.5～3h, inner flue gas of the stove CO/CO
2Be 3.5～4.5.
3, the high temperature calcining that step 2 is obtained is the shrend chilling behind sealing bore slow cooling to 400～750 ℃, shrend calcining ball milling, and granularity is for to account for 85～95% less than 0.074mm.
4, the ball milling ore pulp that step 3 is obtained carries out magnetic separation, and the ore pulp mass concentration is controlled at 15～25%, and magneticstrength is controlled at 500～2000 oersteds, obtains concentrate pulp and mine tailing ore pulp, obtains iron powder and mine tailing through dense filtration.
5, molten minute of the iron powder that step 4 is obtained, 1550～1600 ℃ of temperature, time 0.5～3h obtains phosphorous less than 0.01% high-quality molten iron.
6, the mine tailing that step 4 is obtained leaches with dilute sulphuric acid, and sulfuric acid concentration is 0.8～1.5mol/L, and liquid-solid ratio is 2～5:1,50～90 ℃ of extraction temperatures, and extraction time 1～4h leaches endpoint pH and controls 1～1.5, soaks after rolling and filters, and filtrate is used CaO, CaCO
3, one or more in Wingdale regulate pH value to 2.5～5.0 removal of impurities, filtration washing obtains the high-purity sulphuric acid manganese solution.
7, the high-purity sulphuric acid manganese solution condensing crystal that obtains of step 6, make POV manganese.
Embodiment 1
(Fe 40%, and MnO 5%, P to contain the phosphorous rhombohedral iron ore raw ore of manganese
2O
51%, Al
2O
35%, SiO
220%) be crushed to less than 3mm and account for 88%, allocate 22% bituminous coal into, granulate (granularity 30mm) after mixing, pellet is 1000 ℃ of constant temperature calcining 2h in rotary kiln, flue gas CO/CO
2Be 4; Calcining slow cooling to 500 ℃ shrend chilling, shrend calcining ball milling, grinding particle size accounts for 87% less than 0.074mm; Control ore pulp mass concentration 20%, magneticstrength 1000 oersted magnetic separation obtain the class iron sponge powder, and (Fe 90%, and P 0.1%, Al
2O
31.5%, SiO
23.2%) and rich manganese mine tailing (Mn 8%, and Fe 6%); 1550 ℃ of molten minute 2h of class iron sponge powder obtain high-quality molten iron (P 0.005%, and Mn 0.3%); Rich manganese mine tailing adopts the 1mol/L dilute sulphuric acid to leach, liquid-solid ratio 4:1, and 80 ℃ of extraction temperatures, extraction time 3h leaches endpoint pH 1.2, and after filtering, filtrate is regulated the removal of impurities of pH value to 3 with CaO, and after filtering, the high-purity sulphuric acid manganese solution obtains POV manganese through condensing crystal.
Embodiment 2
(Fe 35%, and MnO 10%, P to contain the phosphorous rhombohedral iron ore raw ore of manganese
2O
51%, Al
2O
39%, SiO
220%) be crushed to less than 3mm and account for 90%, allocate 20% bituminous coal into, granulate (granularity 25mm) after mixing, pellet is 980 ℃ of constant temperature calcining 3h in rotary kiln, flue gas CO/CO
2Be 3.9; Calcining slow cooling to 550 ℃ shrend chilling, shrend calcining ball milling, grinding particle size accounts for 93% less than 0.074mm; Control ore pulp mass concentration 20%, magneticstrength 1000 oersted magnetic separation obtain the class iron sponge powder, and (Fe 91%, and P 0.08%, Al
2O
31.6%, SiO
23.3%) and rich manganese mine tailing (Mn 9%, and Fe 7%); 1580 ℃ of molten minute 1.5h of class iron sponge powder obtain high-quality molten iron (P 0.005%, and Mn 0.2%); Rich manganese mine tailing adopts the 1.2mol/L dilute sulphuric acid to leach, liquid-solid ratio 3:1, and 90 ℃ of extraction temperatures, extraction time 4h leaches endpoint pH 1.0, and after filtering, filtrate is used CaCO
3Regulate the removal of impurities of pH value to 3.5, after filtering, the high-purity sulphuric acid manganese solution obtains POV manganese through condensing crystal.
Claims (10)
1. treatment process that contains the phosphorous rhombohedral iron ore of manganese is characterized in that the step of its treating processes comprises successively:
(1) will contain after the phosphorous rhombohedral iron ore crushing raw ore of manganese and the fine coal mixing, make pellet;
(2) pellet is carried out reducing roasting;
(3) carry out the high-temperature water quenching ball milling;
(4) carry out the magnetic separation separation and obtain concentrate iron powder and mine tailing;
(5) mine tailing is carried out sulfuric acid leaching, filtration, the filtrate purification and impurity removal;
(5) purify rear liquid condensing crystal and prepare manganous sulfate.
2. a kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese according to claim 1, it is characterized in that the particle size after cracking that will contain the phosphorous rhombohedral iron ore crushing raw ore of manganese process of step (1) is for surpassing 85% less than 3mm, after the fine coal mixing that accounts for raw ore weight 15%～30%, an ore deposit diameter of making is 10～30mm.
3. a kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese according to claim 1, is characterized in that described fine coal is one or more in bituminous coal, hard coal, brown coal.
4. a kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese according to claim 1, what it is characterized in that step (2) carries out reducing roasting process with pellet, reducing roasting equipment adopts a kind of in rotary kiln, rotary hearth furnace, multiple hearth furnace, thermal source is coal gas or coal, combustion-supporting gas is air, the high-temperature zone temperature is 900～1050 ℃, and the high-temperature zone residence time is 0.5～3h, controls out kiln gas CO/CO
2Be 3.5～4.5.
5. a kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese according to claim 1, what it is characterized in that step (3) carries out the shrend mechanical milling process with the high temperature calcining, through sealing after cooling cylinder is cooled to 400～750 ℃ with calcining, carry out shrend chilling, ball milling, after ball milling, the ore particle degree is for to account for 85%～95% less than 0.074mm.
6. a kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese according to claim 1, it is characterized in that the magnetic separation sepn process of step (4), that ball milling ore pulp with step (3) carries out magnetic separation, advance ore deposit pulp solids mass concentration and be controlled at 15%～25%, magneticstrength is controlled at 800～1500 oersteds, obtains concentrate iron powder and mine tailing.
7. a kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese according to claim 1, the concentration that it is characterized in that the sulphuric acid soln that the sulfuric acid leaching process that mine tailing is carried out of step (5) adopts is 0.8～1.5mol/L, liquid-solid ratio is 2～5:1,50～90 ℃ of extraction temperatures, extraction time 1～4h leaches endpoint pH and controls 1～1.5.
8. a kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese according to claim 1, is characterized in that the filtrate purification and impurity removal process of step (5) is that filtrate is adjusted pH value to 2.5～5.0, after filtration, washing is purified rear manganese sulfate solution.
9. a kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese according to claim 1, the filtrate purification and impurity removal process that it is characterized in that step (5) is to add CaO, CaCO in filtrate
3, one or more in Wingdale adjust pH.
10. a kind for the treatment of process that contains the phosphorous rhombohedral iron ore of manganese according to claim 1, is characterized in that described step (6) is the manganese sulfate solution condensing crystal that step (5) is obtained, and after centrifuging, gained manganous sulfate crystal grain is dry, makes POV manganese.
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Cited By (12)
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| CN104263908A (en) * | 2014-10-11 | 2015-01-07 | 陈小众 | Reduction roasting method of siderite in rotary kiln |
| CN105296745A (en) * | 2015-12-01 | 2016-02-03 | 湖南长拓高科冶金有限公司 | Separation and recovery method of manganese and iron in poor ferrous manganese ore |
| CN105671311A (en) * | 2016-01-21 | 2016-06-15 | 昆明理工大学 | Processing method of iron ore |
| CN105886781A (en) * | 2016-06-29 | 2016-08-24 | 广西桂柳化工有限责任公司 | Method for recovering manganese dioxide from electrolytic manganese anode mud |
| CN106902957A (en) * | 2015-12-23 | 2017-06-30 | 本钢板材股份有限公司 | A kind of method that wet magnetic separation processes molten iron pretreatment slag |
| CN107574299A (en) * | 2017-09-11 | 2018-01-12 | 中南大学 | A kind of low-grade Ferromanganese Ore pyrogenic process beneficiation method |
| CN110420726A (en) * | 2019-08-28 | 2019-11-08 | 王宗宝 | A kind of magnetite separation device |
| CN110629054A (en) * | 2019-10-30 | 2019-12-31 | 中国恩菲工程技术有限公司 | Preparation device of manganese-rich slag |
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| CN115020659A (en) * | 2022-01-21 | 2022-09-06 | 昆明理工大学 | LiFePO 4 Preparation method of/C composite positive electrode material |
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| CN103397176A (en) * | 2013-07-26 | 2013-11-20 | 辽宁博联特冶金科技有限公司 | Combined ore-dressing method of extracting iron and removing phosphorus from low-lean, high-phosphorous and refractory iron ore |
| CN104263908A (en) * | 2014-10-11 | 2015-01-07 | 陈小众 | Reduction roasting method of siderite in rotary kiln |
| CN105296745A (en) * | 2015-12-01 | 2016-02-03 | 湖南长拓高科冶金有限公司 | Separation and recovery method of manganese and iron in poor ferrous manganese ore |
| CN106902957A (en) * | 2015-12-23 | 2017-06-30 | 本钢板材股份有限公司 | A kind of method that wet magnetic separation processes molten iron pretreatment slag |
| CN105671311A (en) * | 2016-01-21 | 2016-06-15 | 昆明理工大学 | Processing method of iron ore |
| CN105886781A (en) * | 2016-06-29 | 2016-08-24 | 广西桂柳化工有限责任公司 | Method for recovering manganese dioxide from electrolytic manganese anode mud |
| CN105886781B (en) * | 2016-06-29 | 2018-01-02 | 广西桂柳化工有限责任公司 | Method for recovering manganese dioxide from electrolytic manganese anode mud |
| CN107574299A (en) * | 2017-09-11 | 2018-01-12 | 中南大学 | A kind of low-grade Ferromanganese Ore pyrogenic process beneficiation method |
| CN110420726A (en) * | 2019-08-28 | 2019-11-08 | 王宗宝 | A kind of magnetite separation device |
| CN110420726B (en) * | 2019-08-28 | 2021-05-25 | 山东域潇锆钛矿业股份有限公司 | Magnetite ore dressing device |
| CN110629054A (en) * | 2019-10-30 | 2019-12-31 | 中国恩菲工程技术有限公司 | Preparation device of manganese-rich slag |
| CN110629054B (en) * | 2019-10-30 | 2024-03-22 | 中国恩菲工程技术有限公司 | Preparation device of manganese-rich slag |
| CN113735179A (en) * | 2021-08-24 | 2021-12-03 | 广西锰华新能源科技发展有限公司 | Method for preparing high-purity ferric sulfate by using ferro-manganese |
| CN115020659A (en) * | 2022-01-21 | 2022-09-06 | 昆明理工大学 | LiFePO 4 Preparation method of/C composite positive electrode material |
| CN115020659B (en) * | 2022-01-21 | 2023-04-18 | 昆明理工大学 | LiFePO 4 Preparation method of/C composite positive electrode material |
| CN114230260A (en) * | 2022-01-24 | 2022-03-25 | 广西旭阳环保建材有限公司 | Manganese tailing slag concrete and preparation method thereof |
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