CN103937999B - A kind of vacuum distilling ferromanganese extracts method and the device of manganese metal - Google Patents
A kind of vacuum distilling ferromanganese extracts method and the device of manganese metal Download PDFInfo
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Abstract
Vacuum distilling ferromanganese extracts method and the device of manganese metal, belongs to Metal smelting technical field.The present invention distills ferromanganese to be separated manganese and iron to extract manganese metal in ferromanganese under taking vacuum condition, in stove, supplement raw material continuously by charging system in still-process and ensure the continuity of still-process and high efficiency, the manganese steam distilled out is collected to the crystallization that is cooled of crystallization collecting chamber by Cemented filling.Vacuum distilling ferromanganese extract the device of manganese metal comprise in vacuum distilling body of heater, body of heater be provided with working chamber and Heating System Supporting, body of heater outside connect closed bell is housed above vacuum system, body of heater, bell top connects charging system and vapor transport pipeline, pipeline is furnished with heating unit, the pipeline the other end is crystallization collecting chamber, collecting chamber is equipped with air-bleed system, is provided with filter plate and can filters gas and leave manganese metal small-particle in collecting chamber.Production efficiency of the present invention is high, rhythm fast, and product purity is higher, detrimental impurity content is low, and production process operating environment is good, and environmental pollution is little.
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 most important alloy Addition ofelements in alloy production, 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 effectively can improve steel in steel.Different to product demand according to user, the manganese adding different content in steel can make steel show different characteristics.Current global manganese metal production formation three megatrend: one is increasing to its demand; Two is more and more higher to its purity requirement; Three is that 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 carrys out obtained 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 Mn-rich 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 at about 9450kwh/tMn, and this method existing is all few in various countries to be used.Electrolytic process was tested by U.S. Bureau in nineteen thirty, and nineteen thirty-five succeeds substantially, and nineteen thirty-nine drops into industrial production, is after this in succession developed in English, moral, Deng state, now universal various countries.Manganese ore is become the manganese oxide dissolving in sulfuric acid by this genealogy of law through reducing roasting, then obtains manganese sulphate solution with the mixed solution leaching of sulfuric acid and sulfate of ammoniac, and last electrolysis obtains manganese metal.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 poor manganese ore can be utilized to produce.But it is that resource, energy consumption are high that electrolytic process prepares manganese metal, a kind of technique that pollutent output is large, because in all factor electrolytic processes, current efficiency is only 60% ~ 70%, ton manganese produces power consumption up to 9000 ~ 11000kwh, and the pollutent discharged in production process can cause severe contamination to the surface water of factory's periphery, underground water and soil etc.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 above in these productions seriously governs the development of electrolytic manganese industry for a long time.
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 aspects such as its basic theories, technology and equipment and have accumulated a large amount of experience, 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 investigation and experimental analysis checking, propose a kind of utilize vacuum distilling ferromanganese purify metals manganese method 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, and they can be separated by distillation with under vacuum degree condition by certain temperature, thus 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:
Can find out that the pure substance vapour pressure of manganese is more much bigger than iron from formula.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 according to this characteristic by distilling these two separating substances.In addition, according to thermodynamic datas such as Mn-Fe system constituent element concentration and activity quotients by calculating the gas-liquid two-phase equilibrium relationship that can obtain Fe in Mn-Fe system, as shown in table 2, in the manganese distilled out when weight of iron mark when showing 1200 DEG C in ferromanganese increases to 0.9 by 0.3, iron content is by 4.47 × 10
-5increase to 5.74 × 10
-4, to distill in manganese iron content when 1550 DEG C by 4.06 × 10
-4increase to 5.97 × 10
-3.In distillation temperature lower as can be seen here and alloy, higher Fe content more easily obtains pure distillation manganese.
Table 1
and
with the relation of temperature t
Table 2Mn-Fe system Fe
l-Fe
gthe equilibrium relationship of (massfraction)
Distillation ferromanganese is separated the feasibility of manganese from thermodynamics analytic explanation above, analyzes manganese distillation dynamic process below from aerodynamic point.Element rate of volatilization in a vacuum adopts Lang Gemiaoer formulae discovery:
A in formula
bfor the pure substance standard activity of B; P
bfor the 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 is that traditional mode of production institute can not be than.In addition, resistance in still-process is mainly from the gas molecule of ullage, distill out when just and can run into the collision of upper air molecule when manganese molecule moves upward and hinder distillation, ullage atmospheric molecular concentration can be made to reduce by improving distillation vacuum tightness thus reduce the resistance of evaporative process, being conducive to distillation.
Because manganese metal product has purposes to be greatly available to iron and steel enterprise as interpolation 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%), so the volatilization problems of P in still-process must be considered in general ferromanganese.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, is only 3.9 × 10
-7.Its vaporator rate v can be calculated like this according to Lang Gemiaoer formula
p=3.9 × 10
-4kgm
-2s
-1, illustrate in the manganese distilled out and only contain extremely trace P.Above theoretical analysis ensure that feasibility of the present invention.
Utilize vacuum distilling technique to distill a method for ferromanganese extraction manganese metal, it is characterized in that: utilize iron and manganese pure substance vapour pressure 900 ~ 1400 DEG C time
be 1.74 × 10
5~ 2.73 × 10
3feature, be separated manganese and iron by vacuum distilling, and utilize distillation collection device to be collected by the manganese distilled, thus obtain manganese metal.
Concrete extraction step is: first raw material ferromanganese is loaded working chamber and carry out cloth, and be evenly mixed into when cloth and account for material and weigh the carbon granule that 20% ~ 30% granularity is greater than 0.5mm, the object adding carbon granule is that carbon granule is non-fusible when raw material has just started to melt, and the effect that such carbon granule just plays support frame hinders distillation to prevent material grain adhesion crust; Cloth terminates rear closedown charging opening and is evacuated to 10 ~ 50Pa; Open heating unit, by the heating schedule of setting, furnace temperature is risen to target temperature, be incubated after arriving target temperature; Constantly add ferromanganese from charging opening according to steam output in still-process and ensure carrying out continuously of still-process; After distillation for some time, Fe content is reduced to and to a certain degree stops distillation afterwards in stove, falls stove cloth again.The collection of manganese steam: first opening conduits heating system is by pipeline heating to 800 DEG C ~ 1000 DEG C, and rapid crystallization after can preventing manganese steam from contacting with the inner-walls of duct of low temperature like this, reduces 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, and be deposited under gravity bottom collecting chamber and be collected, gas is then drawn out of by screen plate.
To achieve these goals, present invention also offers the device that a kind of vacuum distilling ferromanganese extracts manganese metal, it comprises vacuum distilling body of heater, working chamber and Heating System Supporting is provided with in body of heater, body of heater outside connects pumped vacuum systems, closed bell is housed above body of heater, bell top connects feed hopper and vapor transport pipeline, feed hopper establishes 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, be provided with filter plate in collecting chamber can filter gas and leave manganese metal small-particle.During apparatus of the present invention distillation, continuity is strong, and easy to operate, environmental pollution is little.
The invention has the advantages that and have employed a kind of method producing manganese metal newly, the electrolytic process that this vacuum distilling ferromanganese method of preparing 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 obviously reduces the pollution of environment.
Four, accompanying drawing explanation
Fig. 1 vacuum distilling ferromanganese extracts the schematic diagram of manganese metal device, wherein: 1-vacuum distilling body of heater, and 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) load working chamber 3 after the high carbon ferromanganese (cost is low) being broken into fritter being removed the grease on surface, oven dry internal steam, during cloth, evenly add some carbon granules (expecting heavy by 20% ~ 30%);
2) close vacuum distilling bell 5, start pumped vacuum systems 13 and vacuumize, after reaching 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) collection that collecting chamber air extractor 7 and pipeline valve 10 carry out manganese steam is opened;
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) stop distillation when Fe content is reduced to a certain degree in stove, the stove that falls is again reinforced to be distilled next time.
Embodiment 1: raw material adopt the trade mark be high carbon ferromanganese (GB/T3795-96) composition of FeMn74C7.5 in table 3:
Table 3 high carbon ferromanganese composition and content
Weight is 5kg, raw material stoving also loads working chamber 3 after removing surperficial grease, be mixed into the carbon granule 1kg of granularity 1mm simultaneously, close vacuum distilling bell 5, start pumped vacuum systems 13 to vacuumize, control vacuum tightness at 5 ~ 10Pa, unlatching working chamber heating unit 2 target setting temperature is 1300 DEG C and starts to heat 2h, insulation 2h, while heating up to raw material, opening conduits heating unit 9 is preheating to about 900 DEG C, opening collecting chamber air extractor 7 makes the manganese steam distilled out enter into crystallization collecting chamber 6 by transport pipeline 4, 9.5kg is total to 15 times by feed hopper 11 to furnace charge in still-process, one stove distillation terminates rear closedown heating unit 2, closing duct valve 10, manganese metal is obtained in crystallization collecting chamber 6.
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 (4)
1. vacuum distilling ferromanganese extracts a method for manganese metal, it is characterized in that: utilize iron and manganese pure substance vapour pressure 900 ~ 1400 DEG C time
be 1.74 × 10
5~ 2.73 × 10
3feature, be separated manganese and iron by vacuum distilling, and utilize distillation collection device to be collected by the manganese distilled, thus obtain manganese metal;
Concrete extraction step is as follows: first raw material ferromanganese is loaded working chamber and carry out cloth, and be evenly mixed into when cloth and account for material and weigh the carbon granule that 20% ~ 30% granularity is greater than 0.5mm, the object adding carbon granule is that carbon granule is non-fusible when raw material has just started to melt, and the effect that such carbon granule just plays support frame hinders distillation to prevent material grain adhesion crust; Cloth terminates rear closedown charging opening and is evacuated to 10 ~ 50Pa; Open heating unit, by the heating schedule of setting, furnace temperature is risen to target temperature, be incubated after arriving target temperature; Constantly add ferromanganese from charging opening according to steam output in still-process and ensure carrying out continuously of still-process; After distillation for some time, Fe content is reduced to and to a certain degree stops distillation afterwards in stove, falls stove cloth again; The collection of manganese steam: first opening conduits heating system is by pipeline heating to 800 DEG C ~ 1000 DEG C, and rapid crystallization after can preventing manganese steam from contacting with the inner-walls of duct of low temperature like this, reduces 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, and be deposited under gravity bottom collecting chamber and be collected, gas is then drawn out of by screen plate.
2. a kind of vacuum distilling ferromanganese according to claim 1 extracts the method for manganese metal, it is characterized in that: water distilling apparatus has been installed charging system, continue to add ferromanganese raw material in stove by feed hopper in still-process, realize continuity and the high efficiency of distillation.
3. a kind of vacuum distilling ferromanganese according to claim 1 extracts the method for manganese metal, it is characterized in that: vapor transport pipeline is equipped with heating system, collect and in the process of manganese steam, pipeline is heated to reduce manganese steam and cryogenic piping contact internal walls and crystallization bonds.
4. an application rights requires that the vacuum distilling ferromanganese described in 1 extracts the device of the method for manganese metal, 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 connected to pumped vacuum systems (13), closed bell (5) is housed above body of heater, the closed vessel furnace portion of covering connects feed hopper (11) and vapor transport pipeline (4), feed hopper is established charging valve (12), vapor transport pipeline is furnished with heating unit (9) for vapor transport pipeline heating, the vapor transport pipeline the other end is crystallization collecting chamber (6), crystallization collecting chamber is equipped with collecting chamber air extractor (7) for transferring metal manganese steam provides power, be provided with filter plate (8) in crystallization collecting chamber can filter gas and leave manganese metal small-particle.
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| CN105369041B (en) * | 2015-12-15 | 2017-12-26 | 中国原子能科学研究院 | A kind of Na-K alloy vacuum distillation plant |
| CN106382818B (en) * | 2016-09-20 | 2019-04-30 | 广东先导稀材股份有限公司 | A kind of vacuum smelting furnace |
| CN113249573B (en) * | 2021-07-13 | 2022-08-09 | 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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| 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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Patent Citations (5)
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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 |
| CN101886168A (en) * | 2010-07-14 | 2010-11-17 | 广西大学 | Extract technology of semi-manganese oxide ore |
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