CN103937999A - Method and device for extracting metal manganese from ferromanganese through vacuum distillation - Google Patents
Method and device for extracting metal manganese from ferromanganese through vacuum distillation Download PDFInfo
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- CN103937999A CN103937999A CN201410165638.0A CN201410165638A CN103937999A CN 103937999 A CN103937999 A CN 103937999A CN 201410165638 A CN201410165638 A CN 201410165638A CN 103937999 A CN103937999 A CN 103937999A
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Abstract
The invention provides a method and a device for extracting metal manganese from ferromanganese through vacuum distillation and belongs to the technical field of metal smelting. According to the method, the ferromanganese is distilled under a vacuum condition so as to separate manganese and iron, so that the metal manganese in the ferromanganese is extracted. Raw materials are continuously fed to a furnace by using a feeding system in a distillation process so as to ensure the continuity and high efficiency of the distillation process, and distilled manganese steam is conveyed to a crystallization collecting chamber by using a pipeline so as to be cooled, crystallized and collected. The device for extracting the manganese metal from the ferromanganese through vacuum distillation comprises a vacuum distillation furnace body, a smelting chamber, a matched heating system, a vacuum system, an airtight furnace cover, the feeding system, the steam conveying pipeline, a heating device and the crystallization collecting chamber, wherein the smelting chamber and the matched heating system are arranged in the furnace body, the outer part of the furnace body is connected to the vacuum system, the airtight furnace cover is arranged above the furnace body, the upper part of the furnace cover is connected to the heating system and the steam conveying pipeline, the pipeline is provided with the heating device, the crystallization collecting chamber is arranged at the other end of the pipeline, an air extracting system is arranged on the collecting chamber, and a filter plate is arranged in the collecting chamber and can be used for filtering out gas so as to remain small manganese metal particles. The method and the device have the advantages of high production efficiency, fast pace, relatively high product purity, low content of detrimental impurities and good working environments in production process and hardly causes environment pollution.
Description
Technical field
The invention belongs to Metal smelting technical field, relate to manganeseirom melting, particularly a kind of vacuum distilling ferromanganese extracts method and the device of manganese metal.
Background technology
Manganese is that in alloy production, most important alloy adds element, is the important source material of stainless steel, high strength alloy steel and non-ferrous metal alloy, is also the base mateiral of electron trade.Manganese adds intensity, hardness, elastic limit, wear resistance and the erosion resistance that in steel, can effectively improve steel.According to user, to product demand difference, the manganese that adds different content in steel can make steel show different characteristics.Current global manganese metal is produced and is formed three megatrend: the one, and increasing to its demand; The 2nd, more and more higher to its purity requirement; The 3rd, its production should be fewer and feweri to the harm of environment.The method of traditional mode of production manganese metal comprises thermite process, electro-silicothermic process and electrolytic process.Wherein thermite process is to make manganese metal with the oxide compound of metallic aluminium reduction manganese, and this method not only cost is high, and can not get pure manganese.Even if select the extra high raw material of manganese content to smelt, gained manganese metal still has the detrimental impurity such as phosphorus, aluminium.Electro-silicothermic process complex process, first will smelt low-phosphorous rich manganese slag, then smelt silicon-manganese alloy, last metal smelting manganese, and the manganese metal purity that this method is produced is approximately 97.1%～96.8%, and power consumption is in 9450kwh/tMn left and right, and Xian Cifa various countries are few use all.Electrolytic process starts test in nineteen thirty by mineral bureau of the U.S., and nineteen thirty-five succeeds substantially, and nineteen thirty-nine is dropped into industrial production, after this in succession developed at English, moral, Deng state, now universal various countries.This genealogy of law becomes manganese ore the manganese oxide that dissolves in sulfuric acid through reducing roasting, then leaches and obtain manganese sulphate solution with the mixed solution of sulfuric acid and sulfate of ammoniac, and manganese metal is obtained in last electrolysis.Its product is pure, can reach more than 99.7% containing manganese, and the content of the impurity such as sulphur, phosphorus, carbon is extremely low, and can utilize poor manganese ore to produce.But it is that resource, energy consumption are high that electrolytic process is prepared manganese metal, a kind of technique that pollutent output is large, because current efficiency in all factor electrolytic processes is only 60%～70%, ton manganese is produced power consumption up to 9000～11000kwh, and surface water, underground water and the soil etc. of the pollutent discharging in production process to factory's periphery can cause severe contamination.At present because China's electrolytic manganese production equipment enlarging is inadequate, Automation of Manufacturing Process level is not high causes that labor strength is large, labor condition is poor, and process parameter control is unstable.Unfavorable factor in these productions is seriously restricting the development of electrolytic manganese industry for a long time above.
Vacuum metallurgy technology is a kind of new technology of nonferrous production, and the thirties in 20th century, this technology was applied to industrial production, and this type of process characteristic is: can improve raw material availability, save energy, reduce costs, improve workman's operating environment, and pollute little to surrounding enviroment.Vacuum metallurgy technology is developed so far, and forefathers are studied and have accumulated a large amount of experiences to aspects such as its basic theories, technology and equipment, and nowadays vacuum metallurgy is a kind of comparatively ripe metallurgical technology.Consider the deficiency of above-mentioned Process of Electrolytic Manganese, in conjunction with the feature of vacuum metallurgy technology, through a large amount of theoretical investigationes and experimental analysis checking, proposed a kind of utilize vacuum distilling ferromanganese purify metals the method for manganese and for its technological design water distilling apparatus.
Summary of the invention
The object of the present invention is to provide a kind of vacuum distilling ferromanganese to extract the method for manganese metal, its principle is that the pure substance steam of iron and manganese is pressed with very big difference, certain temperature with under vacuum degree condition, can they be separated by distilling, thereby extract manganese metal.
To achieve these goals, the present invention analyzes and researches theoretically.The pure substance saturated vapor pressure difference of manganese and iron is very large, and wherein the vapour pressure of manganese and the pass of temperature are:
The pure substance vapour pressure that can find out manganese from formula is more much bigger than iron.Under differing temps, the steaming pressure ratio of manganese and iron is more as shown in table 1, below 1000 DEG C
ratio
large 10
5～10
7doubly, more than 1000 DEG C
ratio
large 10
4～10
3doubly, therefore can be according to this characteristic by distilling these two separating substances.In addition, be that the thermodynamic datas such as constituent element concentration and activity quotient are by calculating the gas-liquid two-phase equilibrium relationship that can obtain Fe in Mn-Fe system according to Mn-Fe, as shown in table 2, the weight of iron mark while showing 1200 DEG C in ferromanganese increases in the manganese distilling out iron content at 0.9 o'clock by 4.47 × 10 by 0.3
-5increase to 5.74 × 10
-4, 1550 DEG C time, distill in manganese iron content by 4.06 × 10
-4increase to 5.97 × 10
-3.In lower distillation temperature and alloy, higher manganese content more easily obtains pure distillation manganese as can be seen here.
Table 1
and
relation with temperature t
Table 2Mn-Fe is Fe
l-Fe
gthe equilibrium relationship of (massfraction)
Above from thermodynamics analytic explanation distillation ferromanganese separate the feasibility of manganese, below from kinetics angle analysis manganese distillation dynamic process.Element rate of volatilization in a vacuum adopts Lang Gemiaoer formula to calculate:
A in formula
bfor the pure substance standard activity of B; P
bfor saturated vapor pressure/mmHg of B.By can be calculated the maximum evaporation rate v of manganese
mn=4.03kgm
-2s
-1, such distillation rate be traditional mode of production can not be than.In addition, resistance in still-process is mainly from the gas molecule above liquid level, when manganese molecule moves upward, can run into the collision of top air molecule and hinder distillation when just distilling out, can make liquid level top atmospheric molecular concentration reduce the resistance that reduces evaporative process thereby distill vacuum tightness by raising, be conducive to distillation.
Because having purposes greatly, manganese metal product is available to iron and steel enterprise as adding alloy, as IF steel, therefore user is very harsh to the P content requirement in product, and all can contain a certain amount of P (0.2%～0.3%) in general ferromanganese, so must consider the volatilization problem of P in still-process.P at high temperature (1500 DEG C) saturated vapor pressure is very large, is 7.8 × 10
7pa.But the activity of P is very low, be only 3.9 × 10
-7.Can calculate its vaporator rate v according to Lang Gemiaoer formula like this
p=3.9 × 10
-4kgm
-2s
-1, only illustrate in the manganese distilling out containing trace P extremely.Above theoretical analysis has ensured feasibility of the present invention.
Utilize vacuum distilling technique distillation ferromanganese to extract a method for manganese metal, it is characterized in that: utilize iron and manganese pure substance vapour pressure in the time of 900～1400 DEG C
be 1.74 × 10
5～2.73 × 10
3feature, separate manganese and iron by vacuum distilling, and utilize distillation collection device the manganese distilling is collected, thereby obtain manganese metal.
Concrete extraction step is: first pack raw material ferromanganese into working chamber and carry out cloth, and in the time of cloth, evenly sneak into account for and expect to weigh the carbon granule that 20%～30% granularity is greater than 0.5mm, add the object of carbon granule to be that carbon granule does not melt in the time that raw material just starts to melt, the effect that carbon granule just plays support frame is like this to prevent the distillation of material grain adhesion crust obstruction; After cloth finishes, close charging opening and be evacuated to 10～50Pa; Open heating unit, by the heating schedule of setting, furnace temperature is risen to target temperature, after arrival target temperature, be incubated; In still-process, constantly add ferromanganese from charging opening according to steam output and ensure carrying out continuously of still-process; After distillation for some time, manganese content is reduced to and to a certain degree stops afterwards distillation in stove, falls stove cloth again.The collection of manganese steam: first opening conduits heating system is pipeline heating to 800 DEG C～1000 DEG C, can prevent like this manganese steam contact with the inner-walls of duct of low temperature after rapid crystallization, reduce the condensation bonding of manganese metal in pipeline, improve collection rate; Then open the air extractor of collecting chamber, drive steam to enter collecting chamber by air extractor, manganese steam is condensed into solid granule after entering collecting chamber, is deposited on collecting chamber bottom and is collected under action of gravity, and gas is drawn out of by screen plate.
To achieve these goals, the present invention also provides a kind of vacuum distilling ferromanganese to extract the device of manganese metal, it comprises vacuum distilling body of heater, in body of heater, be provided with working chamber and Heating System Supporting, the outside pumped vacuum systems that connects of body of heater, closed bell is equipped with in body of heater top, bell top connects feed hopper and vapor transport pipeline, on feed hopper, establish charging valve, vapor transport pipeline is furnished with heating unit, the vapor transport pipeline the other end is crystallization collecting chamber, collecting chamber is equipped with air-bleed system and provides power for collecting manganese metal steam, in collecting chamber, being provided with filter plate can filter gas and leave manganese metal small-particle.When apparatus of the present invention distillation, continuity is strong, easy to operate, and environmental pollution is little.
The invention has the advantages that a kind of new method of producing manganese metal that adopted, the electrolytic process that method that this vacuum distilling ferromanganese is prepared manganese metal is more traditional is more efficient, and rhythm of production is fast; The utilization ratio of alloy raw material and the energy is higher, and operating environment is better, and the pollution of environment is obviously reduced.
Four, brief description of the drawings
Fig. 1 vacuum distilling ferromanganese extracts the schematic diagram of manganese metal device, wherein: 1-vacuum distilling body of heater, 2-working chamber heating unit, 3-working chamber, 4-vapor transport pipeline, 5-vacuum distilling bell, 6-crystallization collecting chamber, 7-collecting chamber air extractor, 8-collecting chamber filter plate, 9-pipe heating device, 10-pipeline valve, 11-feed hopper, 12-charging valve, 13-pumped vacuum systems, 14-working chamber base.
Five, embodiment
The present invention's application vacuum distilling ferromanganese extracts the working method of manganese metal device:
1) high carbon ferromanganese (cost is low) that is broken into fritter removed to surperficial grease, dried after internal steam and pack working chamber 3 into, when cloth, evenly add some carbon granules (expecting heavy by 20%～30%);
2) close vacuum distilling bell 5, start pumped vacuum systems 13 and vacuumize, reach after predetermined vacuum tightness, open heating unit 2 and start heating by the target temperature of setting, be incubated after reaching target temperature;
3) in still-process, pipeline is preheated to certain temperature by opening conduits heating unit 9;
4) open collecting chamber air extractor 7 and pipeline valve 10 carries out the collection of manganese steam;
5) in still-process according to the amount of steaming of Time Calculation manganese, by feed hopper 8 regularly to feed supplement in stove;
6) in the time that manganese content is reduced to a certain degree in stove, stop distillation, the stove that falls is again reinforced to be distilled next time.
Embodiment 1: raw material adopts trade mark high carbon ferromanganese (GB/T3795-96) composition that is FeMn74C7.5 is in table 3:
Table 3 high carbon ferromanganese composition and content
Weight is 5kg, raw material stoving and remove surperficial grease after pack working chamber 3 into, sneak into the carbon granule 1kg of granularity 1mm simultaneously, close vacuum distilling bell 5, starting pumped vacuum systems 13 vacuumizes, control vacuum tightness at 5～10Pa, unlatching working chamber heating unit 2 target setting temperature are 1300 DEG C and start to heat 2h, insulation 2h, when intensification to raw material, opening conduits heating unit 9 is preheating to 900 DEG C of left and right, opening collecting chamber air extractor 7 makes the manganese steam distilling out enter into crystallization collecting chamber 6 by transport pipeline 4, in still-process, be total to 9.5kg 15 times by feed hopper 11 to furnace charge, after finishing, one stove distillation closes heating unit 2, close pipeline valve 10, in crystallization collecting chamber 6, obtain manganese metal.
Through assay, manganese metal purity is 95.4%, and all the other proportions are mainly Fe.The product of this purity meets the requirement of iron and steel enterprise to manganese alloy raw material completely.
Claims (5)
1. utilize vacuum distilling technique distillation ferromanganese to extract a method for manganese metal, it is characterized in that: utilize iron and manganese pure substance vapour pressure in the time of 900～1400 DEG C
be 1.74 × 10
5～2.73 × 10
3feature, separate manganese and iron by vacuum distilling, and utilize distillation collection device the manganese distilling is collected, thereby obtain manganese metal.
2. the method for utilizing vacuum distilling technique distillation ferromanganese to extract manganese metal according to claim 1, is characterized in that:
Concrete extraction step is as follows: first pack raw material ferromanganese into working chamber and carry out cloth, and in the time of cloth, evenly sneak into account for and expect to weigh the carbon granule that 20%～30% granularity is greater than 0.5mm, add the object of carbon granule to be that carbon granule does not melt in the time that raw material just starts to melt, the effect that carbon granule just plays support frame is like this to prevent the distillation of material grain adhesion crust obstruction; After cloth finishes, close charging opening and be evacuated to 10～50Pa; Open heating unit, by the heating schedule of setting, furnace temperature is risen to target temperature, after arrival target temperature, be incubated; In still-process, constantly add ferromanganese from charging opening according to steam output and ensure carrying out continuously of still-process; After distillation for some time, manganese content is reduced to and to a certain degree stops afterwards distillation in stove, falls stove cloth again; The collection of manganese steam: first opening conduits heating system is pipeline heating to 800 DEG C～1000 DEG C, can prevent like this manganese steam contact with the inner-walls of duct of low temperature after rapid crystallization, reduce the condensation bonding of manganese metal in pipeline, improve collection rate; Then open the air extractor of collecting chamber, drive steam to enter collecting chamber by air extractor, manganese steam is condensed into solid granule after entering collecting chamber, is deposited on collecting chamber bottom and is collected under action of gravity, and gas is drawn out of by screen plate.
3. the method for utilizing vacuum distilling technique distillation ferromanganese to extract manganese metal according to claim 1, it is characterized in that: charging system has been installed on water distilling apparatus, in still-process, in stove, continue to add ferromanganese raw material by feed hopper, realize continuity and the high efficiency of distillation.
4. the method for utilizing vacuum distilling technique distillation ferromanganese to extract manganese metal according to claim 1, it is characterized in that: vapor transport pipeline is equipped with heating system, collect in the process of manganese steam and pipeline to be heated to reduce manganese steam contacts with cryogenic piping inwall and crystallization bonds.
5. a device that utilizes vacuum distilling technique distillation ferromanganese to extract manganese metal as claimed in claim 1, it is characterized in that: it comprises vacuum distilling body of heater (1), body of heater Nei You working chamber (3) and heating system (2), body of heater outside is connecting pumped vacuum systems (13), closed bell (5) is equipped with in body of heater top, the closed vessel furnace portion of covering connects feed hopper (11) and vapor transport pipeline (4), on feed hopper, establish charging valve (12), it is vapor transport pipeline heating that vapor transport pipeline is furnished with heating unit (9), the vapor transport pipeline the other end is crystallization collecting chamber (6), crystallization collecting chamber is equipped with collecting chamber air extractor (7) and provides power for transferring metal manganese steam, in crystallization collecting chamber, being provided with filter plate (8) can filter gas and leave manganese metal small-particle.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105369041A (en) * | 2015-12-15 | 2016-03-02 | 中国原子能科学研究院 | Sodium-potassium alloy vacuum distillation device |
| CN106382818A (en) * | 2016-09-20 | 2017-02-08 | 广东先导稀材股份有限公司 | Vacuum smelting furnace |
| CN113249573A (en) * | 2021-07-13 | 2021-08-13 | 赣州中新矿业有限公司 | Recovery unit of tungsten and cobalt in cobalt alloy waste material |
| CN113897501A (en) * | 2021-09-30 | 2022-01-07 | 宁波创致超纯新材料有限公司 | Method for purifying manganese metal by vacuum distillation |
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| CN101886168A (en) * | 2010-07-14 | 2010-11-17 | 广西大学 | Extract technology of semi-manganese oxide ore |
| CN101988154A (en) * | 2010-11-09 | 2011-03-23 | 湖南科技大学 | New technology for preparing electrolytic manganese metal solution and recycling iron by reducing pyrolusite with iron scraps |
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| CN1215761A (en) * | 1997-10-27 | 1999-05-05 | 中国石化扬子石油化工公司 | Method for recovery of Co-Mn metal from p-phthalic acid residual liquid |
| JPH11152528A (en) * | 1997-11-18 | 1999-06-08 | Japan Energy Corp | Production of high purity mn material, and high purity mn material for thin film formation |
| CN1560288A (en) * | 2004-03-03 | 2005-01-05 | 武汉理工大学 | Process of recoverying lithium and manganese from their oxide |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105369041A (en) * | 2015-12-15 | 2016-03-02 | 中国原子能科学研究院 | Sodium-potassium alloy vacuum distillation device |
| CN106382818A (en) * | 2016-09-20 | 2017-02-08 | 广东先导稀材股份有限公司 | Vacuum smelting furnace |
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