CN101302586A - Microwave heating, solid state reduction and gaseous dephosphorization method for manganese ore powder - Google Patents
Microwave heating, solid state reduction and gaseous dephosphorization method for manganese ore powder Download PDFInfo
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Abstract
The invention provides a method of microwave heating, solid-state reduction and gasification dephosphorization for manganese ore powder. The invention adopts a novel method of microwave heating, solid-state reduction and gasification dephosphorization against the characteristic of the manganese ore powder with high content of phosphorus. The method uses the manganese ore powder as a raw material, coal powder as reducing agent, and nitrogen as reduction and dephosphorization protecting gas to perform solid reduction and gasification dephosphorization in a reduction dephosphorization crucible, through raw material selecting, thinning, mixing, stirring and distributing, in an airtight microwave reduction dephosphorization furnace, in the nitrogen atmosphere, at a high temperature of 1390 DEG C, for 20 minutes to preserve heat and keep stand at constant temperature, so that the manganese ore powder can react with the coal powder and lime powder to prepare sponge ferromanganese powder; and manganese powder can be separated from phosphorus and hazardous substances via cooling, fine grinding and dry magnetic separation purifying. The yield of the sponge ferromanganese can reach 95 percent, the dephosphorization rate can reach 60 to 70 percent, and the phosphorus-containing rate is less than or equal to 0.15 percent. The manganese ore powder has the advantages of good reduction effect, high dephosphorization rate, short process flow and no environmental protection, and can be reused after phosphorus is collected.
Description
Technical field
The present invention relates to a kind of microwave heating, solid state reduction and gaseous dephosphorization method of manganese ore powder, belong to the manganese metal breeze and remove objectionable impurities---the method for phosphoric.
Background technology
The abundance of manganese in the earth's crust is 0.13%, comes the 15, and the abundance of phosphorus in the earth's crust is 0.142%, ranked tenth one, and the relative abundance that can draw phosphorus and manganese thus is that P/Mn is 1.092.
The manganese ore deposit type of China is more, based on the appositional pattern mineral deposit, account for 80%, the characteristics of its manganese ore are that phosphorus manganese is than higher, mostly more than 0.01%, and the phosphorus manganese of manganese ore used in metallurgy requires＜0.003% than P/Mn to phosphorus manganese in the manganese ore than P/Mn, and the manganese ore of state belongs to the high phosphorus type still, phosphoric is mostly with phosphoric acid salt, and promptly the form of phosphatic rock is present in the manganese ore.
Phosphatic chemical general formula is A
5[PO
4]
3(F, Cl OH), belongs to hexagonal system phosphoric acid salt, phosphorus in the manganese ore is mainly with phosphatic form and the tight symbiosis of manganese ore, manganese element is the large alloy addition in the Iron and Steel Production, and phosphoric is harmful element in steel products, and the existence of phosphorus can reduce the mechanical property of steel, the alloy property of coupling is reduced, the fragility of steel and steel alloy is increased, and intensity reduces, so must remove phosphoric in the manganese ore fusion process.
The dephosphorizing method of manganese ore also has various ways, and for example: oxidation liquid reduction dephosphorization method, solid state reduction dephosphorization method, oxidation liquid reduction dephosphorization method is under the condition of hypoxemia position, relies on dephosphorizing agent CaSi-CaF
2, CaAl-CaF
2Or CaC
2-CaF
2In calcium metal carry out dephosphorization because the dephosphorization under reducing atmosphere slag contains a large amount of dephosphorization product C a
3P
2, run into airborne moisture and can generate hypertoxic gas phosphine PH3, both polluted environment, also increased the difficulty of slag subsequent disposal, be not used widely always; Solid state reduction dephosphorization method, dephosphorizing agent are MAGNESIUM METAL, or the solution dephosphorization formed of Ca, Mg, Ba, Sr etc. and halogen, at a certain temperature, solid-state ferromanganese powder is carried out dephosphorization under reducing atmosphere, but because phosphorus mass transfer velocity in solid-state ferromanganese is little, the dephosphorization time is long, can not suitable for mass production; Other dephosphorizing methods, for example: the strong anti-float glass process of magnetic, strong magnetic smelting process, microbial method, reducing roasting ammonia leaching process, extra furnace dephosphorization method etc. also exist many deficiencies and shortcoming, are still waiting further research technically.
Summary of the invention
Goal of the invention
Purpose of the present invention is exactly at the deficiencies in the prior art, adopt microwave heating, solid state reduction, gasification dephosphorization method, reduction, dephosphorization one-time continuous to the manganese ore powder are finished, both can reduce to the manganese ore powder, can in reduction process, carry out dephosphorization again, make manganese ore powder product---the phosphorus content of sponge manganese iron powder reaches minimum or less than the alloying requirement of manganese.
Technical scheme
The raw chemical material that the present invention uses is: manganese ore powder, reductive agent coal dust, dephosphorization slag former lime powder, dephosphorization under reducing atmosphere shielding gas nitrogen, its combination consumption is: with kilogram, centimetre
3Be measure unit
Manganese ore powder: MnO
2620kg ± 20kg
Coal dust: C 180kg ± 20kg
Lime powder: CaO 200kg ± 20kg
Nitrogen: N
2100000cm
3± 100cm
3
Reduction, dephosphorizing method is as follows:
(1) selected raw chemical material carries out purity, content control
Manganese ore powder: manganese content: 25-40%
Phosphorus content: 0.2-1%
Coal dust: carbon content 65-80%
Water-content 3-5%
Lime powder: calcium contents 〉=65%
Nitrogen: purity 99.99%
(2) pulverizing, fine grinding, sieve
To selected raw chemical material, carry out ball milling, sieve with dry ball respectively, each raw material becomes finely powdered, repeatedly ball milling, sieve repeatedly;
Dry ball: revolution 400r/min ball milling steel ball Ф 30mm, Ф 20mm
Sieve number: 200 orders
Fine powder particle diameter :≤0.074mm
(3) preparation of raw material, mixing, stirring
Raw material fine powder after sieving is prepared in stainless steel vessel, is mixed by the combination matching consumption, stirs time 20min ± 2min with stirrer;
Manganese ore powder: 620kg ± 20kg
Coal dust: 180kg ± 20kg
Lime powder: 200kg ± 20kg
(4) microwave heating, solid state reduction, gasification dephosphorization
1. carry out in vertical microwave heating crucible dephosphorization under reducing atmosphere stove, the dephosphorization under reducing atmosphere stove is made up of body of heater, bell, stove seat, furnace chamber, reduction mould, thermocouple thermometer, microwave generator, electric control box, liquid crystal display, nitrogengas cylinder;
2. clear up reduction furnace
Open reduction furnace, with dust and hazard residue material in the suction cleaner suction furnace chamber, suction time 6min ± 1min makes in the reduction furnace chamber clean;
3. clear up, clean the dephosphorization under reducing atmosphere crucible
Remove residue and objectionable impurities in the crucible with metal slice, brush, make in the crucible clean;
With dust and objectionable impurities in the suction cleaner suction crucible, suction time 6min ± 1min;
4. preheating dephosphorization under reducing atmosphere crucible
The dephosphorization under reducing atmosphere crucible is placed the drying baker preheating, 400 ℃ ± 10 ℃ of preheating temperatures, time 400min ± 10min;
5. preheating mixing raw material
Mixing raw material is placed stainless steel vessel, preheating in drying baker, 400 ℃ ± 10 ℃ of preheating temperatures, time 40min ± 3min;
6. loose naturally cloth
With the mixing fine powders of manganese ore powder+coal dust+lime powder of mixing, stirring, loose naturally placing in the dephosphorization under reducing atmosphere crucible, cloth is even, loose;
7. the dephosphorization under reducing atmosphere crucible is placed on the middle crucible holder in the microwave reduction furnace chamber, close sealing cover, nitrogengas cylinder is imported nitrogen in furnace chamber, nitrogen input speed 10cm
3/ min makes in furnace chamber and the crucible to be in the nitrogen atmosphere;
8. open electric control box, microwave generator, microwave controller, thermocouple thermometer, liquid crystal display shows microwave heating restore information and temperature information;
Microwave heating heat-up rate: 20-50 ℃/min, accelerate gradually by low temperature to high temperature
Microwave heating reduction temperature: 1390 ℃ ± 10 ℃
Microwave heating power: 100KW
Constant temperature insulation time of repose: 20min ± 2min
Manganese ore powder+coal dust+lime powder absorbs the heat that microwave produces in reduction mould, carry out the hot autoreduction of carbon, generates solid-state sponge ferromanganese;
In airtight reduction furnace chamber, in reduction mould, produce solid carbon reduction, lime powder slag making, nitrogen atmosphere dephosphorisation reaction, reaction formula is as follows:
In the formula:
MnO
2-2SiO
2: manganous silicate
Ca
5[PO
4]
3F: contain calcium monofluorophosphate
Mn: manganese
P: phosphorus
CO: carbon monoxide
CaOSiO
2: Calucium Silicate powder
CaF
2: fluorite
9. handle phosphorous furnace gas
The CO furnace gas that contains phosphorous vapor that to be discharged by pore feeds airtight water cycle cooling tank, and phosphorous vapor is met cold one-tenth solid-state phosphorus, and deposits to the cooling tank bottom, regularly collects solid-state phosphorus and CO gas;
10. nitrogen atmosphere cooling
Turn-off the electric control box power supply, stop microwave heating, reduction, dephosphorization product cool off under nitrogen protection, are cooled to 20 ℃ ± 3 ℃ of normal temperature, and be 120min cooling time, nitrogen input speed 10cm
3/ min, the cooling back becomes sponge manganese iron powder product;
(5) fine grinding sponge manganese iron powder
With ball mill fine grinding sponge manganese iron powder, become finely powdered, sieve with 250 eye mesh screens, fine grinding, sieve and carry out repeatedly, make that powder is even, refinement, powder diameter≤0.057mm;
(6) dry type magnetic separation is purified
To the sponge manganese iron powder of reduction, dephosphorization treatment, purify with dry-type magnetic extractor, remove phosphorus slag and other impurity deviate from the sponge manganese iron powder;
1. with fine grinding, the sponge manganese iron powder that obtains that sieves places in the dry-type magnetic extractor, magnetic separation is purified under high-intensity magnetic field, the magneticstrength in the magnetic separator is 1-2 ten thousand Gausses;
2. after magnetic separation is purified, remove slag and objectionable impurities, get the dephosphorization after product: the sponge manganese iron powder;
(7) detect, chemically examine, analyze
Sponge manganese iron powder after dephosphorization, the purification is detected, chemically examines, analyzes its composition, phosphorus content, gloss, pattern;
Manganese content: 60-70%
Iron level: 20-30%
Phosphorus content :≤0.15%
(8) store
Sponge manganese iron powder to dephosphorization, after purifying will be stored in drying, clean environment with stainless steel vessel, waterproof, protection against the tide, anti-oxidation, acid-proof, alkali, salt corrosion, 20 ℃ ± 3 ℃ of storing temps, relative temperature≤20%.
Described microwave heating crucible dephosphorization under reducing atmosphere stove, primary structure by: stove seat, bell, body of heater, furnace chamber, movable rack, thermocouple thermometer, dephosphorization under reducing atmosphere crucible, microwave generator, microwave controller, liquid crystal display, nitrogengas cylinder are formed; In the bottom of microwave oven body 1 is that stove seat 2, top are sealing cover 4, bell 3, and by movable rack 5 control foldings, on bell 3, sealing cover 4, be provided with thermocouple thermometer 13, pore 10, on the furnace wall of microwave oven body 1, be provided with microwave generator 6, being furnace chamber 9 in microwave oven body 1, is crucible holder 7 in the middle lower portion of furnace chamber 9, the top of crucible holder 7 be dephosphorization under reducing atmosphere crucible 8 and on handle 11, being manganese ore powder+coal dust+lime powder 12 in dephosphorization under reducing atmosphere crucible 8, is nitrogen 24 in the furnace chamber 9; The nitrogengas cylinder of establishing at the sidepiece of microwave oven body 1 21, and by nitrogen valve 22, nitrogen tube 23 and furnace chamber 9 UNICOMs; Sidepiece at body of heater 1 is provided with electric control box 14, and electric control box 14 is provided with pilot lamp 16, liquid crystal display 15, microwave controller 17, power switch 20; Electric control box 14 connects with microwave generator 6 on the body of heater 1 by lead 19, electric control box 14 connects with thermocouple thermometer 13 on the body of heater 1 by lead 18, pore 10 connects furnace gas pipe 38, furnace gas pipe 38 UNICOM's water-cooled casees 35, have water inlet pipe 36, rising pipe 37 on water-cooled case 35 right sides, water-cooled case 35 internal upper parts are phosphorous furnace gas 39, and the middle part is a water coolant 40, and the bottom is a solid-state phosphorus 41.
Described microwave heating, solid state reduction, gasification dephosphorization, temperature are 1390 ℃ ± 10 ℃, and constant temperature, insulation, time of repose are 20min ± 2min, and microwave generator power is 100KW ± 2KW.
Described microwave heating, solid state reduction, gasification dephosphorization, cooling are finished under nitrogen atmosphere, and the nitrogen input speed is 10cm
3/ min.
Described microwave heating, solid state reduction, gasification dephosphorization, the solid state reduction rate of manganese ore powder is 95%, the dephosphorization rate of manganese is 60-70%, phosphorous rate≤0.15% of manganese.
Beneficial effect
The present invention compares with background technology has tangible advance; it is at the high characteristics of China's manganese ore powder phosphorus content and the deficiency of dephosphorizing technology; adopted a kind of brand-new microwave heating; solid state reduction; the gasification dephosphorizing method; in microwave heating dephosphorization under reducing atmosphere stove, reduce; dephosphorization treatment; it is to be raw material with the manganese ore powder; with the coal dust is reductive agent; with the lime powder is the dephosphorization slag former; with nitrogen is gasification dephosphorization shielding gas; selected by to the raw material breeze; refinement; mix; stir; cloth; in airtight microwave heating reduction furnace; under the nitrogen atmosphere protection; in the dephosphorization under reducing atmosphere crucible, carry out solid state reduction; the gasification dephosphorization; under 1390 ℃ of temperature of microwave heating; at constant temperature; insulation; leave standstill 20min in the time; make manganese ore powder and coal dust; lime powder generation chemical reaction; make the manganese element reduction; phosphoric separates; make the sponge manganese iron powder; again through cooling; fine grinding; doing magnetic separation purifies; the low-phosphorous sponge manganese iron powder of purifying out; phosphorus and objectionable impurities are separated; the production yield rate of manganese can reach 95%; the dephosphorization rate of manganese can reach 60-70%; phosphorous rate≤0.15% of manganese, the reduction effect of manganese is good, the dephosphorization rate height; technical process is short; free from environmental pollution, also can collect again after phosphorous furnace gas is discharged and utilize, be the reduction of very good manganese ore powder; dephosphorizing method.
Description of drawings
Fig. 1 is the reduction of manganese ore powder, dephosphorization technology schema
Fig. 2 is microwave heating, solid state reduction, the state graph of gasification dephosphorization
Fig. 3 is the dry type magnetic separation state graph
Fig. 4 is reduction, dephosphorization temperature and time coordinate graph of a relation
Fig. 5 is temperature, time and reduction ratio, dephosphorization rate contrast table
Shown in the figure, list of numerals is as follows:
1, the microwave reduction body of heater, 2, the stove seat, 3, bell, 4, sealing cover, 5, movable rack, 6, microwave generator, 7, crucible holder, 8, the dephosphorization under reducing atmosphere crucible, 9, furnace chamber, 10, pore, 11, handle, 12, manganese ore powder+coal dust+lime powder, 13, thermocouple thermometer, 14, electric control box, 15, liquid crystal display, 16, pilot lamp, 17, the microwave trip switch, 18, lead, 19, lead, 20, power switch, 21, nitrogengas cylinder, 22, nitrogen valve, 23, nitrogen tube, 24, nitrogen, 25, the magnetic separation electric control box, 26, hopper, 27, passage, 28, the control lid, 29, passage, 30, separator box, 31, blower fan, 32, magnetic separator, 33, phosphorus and impurity case, 34, sponge manganese iron powder product case, 35, the water-cooled case, 36, water inlet pipe, 37, rising pipe, 38, the furnace gas pipe, 39, phosphorous furnace gas, 40, water coolant, 41, solid-state phosphorus.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, be microwave heating, solid state reduction, the gasification dephosphorization technology schema of manganese ore powder, strict and undertaken, according to the order of sequence operation by technical process.
The raw chemical material that uses is wanted strict selected, and carry out fine grinding respectively, sieve, circulation is carried out repeatedly, want strict its fine powder particle diameter of control, because of the carbon monoxide reduction and the gasification dephosphorization treatment of in preparation process, carrying out the manganese ore powder simultaneously, so raw material powder must refinement, sieve number is advisable with the 200-250 order, helps the solid state reduction and the gasification dephosphorization treatment of manganese.
Microwave heating dephosphorization under reducing atmosphere stove is wanted strict seal, and leaves pore, is beneficial to input, output and the safety control of nitrogen, and the nitrogen input wants whole process to carry out, must not be intermittently, and input speed is 10cm
3/ min, nitrogen atmosphere both can protect manganese ore powder reduction, again can with dephosphorization slag former lime powder chemical combination, carry out the dephosphorization of manganese ore powder, also can drive away the harmful element in the furnace chamber simultaneously.
The reduction of manganese ore powder is at high temperature to mix with coal dust, carries out the carbon monoxide solid state reduction.
The dephosphorization of manganese ore powder is at high temperature to fit into the promoting the circulation of qi dephosphorization by nitrogen protection and dephosphorization slag former lime powder.
Microwave heating is to be realized by the microwave controller of electric control box and the microwave heater in the stove, its power is 100KW, temperature is shown by thermocouple thermometer and liquid-crystal display in its value and the stove, and regulates and control, to guarantee accuracy, continuity and the controllability of Heating temperature.
Shown in Figure 2, be microwave heating dephosphorization under reducing atmosphere furnace structure and working state figure, this equipment is to design for the solid state reduction of manganese ore powder, the dephosphorization that gasifies specially, its structure is imported three parts by body of heater, automatically controlled and nitrogen and is formed, middle by lead and pipeline UNICOM, the use of working in coordination, note each parameter, strict control, the phosphorous gas that pore 10 is discharged enters airtight water cycle cooling tank, and phosphorous vapor is met water cooling and become solid-state, collects then, be the effective way of handling phosphorous furnace gas, also can go utilization after phosphorus is collected again.
Shown in Figure 3, be manganese ore dried bean noodles formula magnetic separation state graph, magnetic separator is a vertical structure, after the sponge manganese iron powder is entered by hopper 26, through passage 27, control cover 28, passage 29 enters separator box 30,30 fens left and right sides two portions of separator box, left part is that blower fan 31, right part are magnetic separator 32, after the sponge manganese iron powder enters separator box 30, contain phosphorus impurities suction impurity case 33 to what deviate from by blower fan 31, the sponge manganese iron powder by magnetic separator 32 under the magnetic line of force the action of a magnetic field in the suction product case 34.
Shown in Figure 4, be microwave heating, solid state reduction, gasification dephosphorization temperature and time coordinate graph of a relation, ordinate zou is a temperature ℃, X-coordinate is time min, when temperature by 20 ℃ ± 3 ℃ of normal temperature, promptly the A point begins to heat up, the slow earlier back of heat-up rate is fast, heat-up rate is 20-50 ℃/min, when temperature rises to 1390 ℃ ± 10 ℃, i.e. and B point, at this temperature constant temperature, be incubated, leave standstill 20min ± 2min, be the B-C section, begin to be cooled to the D point by the C point then, promptly revert back 20 ℃ ± 3 ℃.
Shown in Figure 5, be reduction ratio, the dephosphorization rate contrast table of microwave heating temperature, constant temperature insulation time of repose and manganese ore powder, in the table as can be known: microwave heating temperature is high more, constant temperature insulation time of repose is long more, and the reduction ratio of manganese ore powder is high more, is directly proportional, the dephosphorization rate of its manganese ore powder is low more, is inversely proportional to.
Claims (6)
1, a kind of microwave heating, solid state reduction and gaseous dephosphorization method of manganese ore powder; it is characterized in that: the raw chemical material of use is: manganese ore powder, reductive agent coal dust, dephosphorization slag former lime powder, dephosphorization under reducing atmosphere shielding gas nitrogen, its combination consumption be: with kilogram, centimetre
3Be measure unit
Manganese ore powder: MnO
2620kg ± 20kg
Coal. powder: C 180kg ± 20kg
Lime powder: CaO 200kg ± 20kg
Nitrogen: N
2100000cm
3± 100cm
3
Reduction, dephosphorizing method is as follows:
(1) selected raw chemical material carries out purity, content control
Manganese ore powder: manganese content: 25-40%
Phosphorus content: 0.2-1%
Coal dust: carbon content 65-80%
Water-content 3-5%
Lime powder: calcium contents 〉=65%
Nitrogen: purity 99.99%
(2) pulverizing, fine grinding, sieve
To selected raw chemical material, carry out ball milling, sieve with dry ball respectively, each raw material becomes finely powdered, repeatedly ball milling, sieve repeatedly;
Dry ball: revolution 400r/min ball milling steel ball Φ 30mm, Φ 20mm
Sieve number: 200 orders
Fine powder particle diameter :≤0.074mm
(3) preparation of raw material, mixing, stirring
Raw material fine powder after sieving is prepared in stainless steel vessel, is mixed by the combination matching consumption, stirs time 20min ± 2min with stirrer;
Manganese ore powder: 620kg ± 20kg
Coal dust: 180kg ± 20kg
Lime powder: 200kg ± 20kg
(4) microwave heating, solid state reduction, gasification dephosphorization
1. carry out in vertical microwave heating crucible dephosphorization under reducing atmosphere stove, the dephosphorization under reducing atmosphere stove is made up of body of heater, bell, stove seat, furnace chamber, reduction mould, thermocouple thermometer, microwave generator, electric control box, liquid crystal display, nitrogengas cylinder;
2. clear up reduction furnace
Open reduction furnace, with dust and hazard residue material in the suction cleaner suction furnace chamber, suction time 6min ± 1min makes in the reduction furnace chamber clean;
3. clear up, clean the dephosphorization under reducing atmosphere crucible
Remove residue and objectionable impurities in the crucible with metal slice, brush, make in the crucible clean;
With dust and objectionable impurities in the suction cleaner suction crucible, suction time 6min ± 1min;
4. preheating dephosphorization under reducing atmosphere crucible
The dephosphorization under reducing atmosphere crucible is placed the drying baker preheating, 400 ℃ ± 10 ℃ of preheating temperatures, time 400min ± 10min;
5. preheating mixing raw material
Mixing raw material is placed stainless steel vessel, preheating in drying baker, 400 ℃ ± 10 ℃ of preheating temperatures, time 40min ± 3min;
6. loose naturally cloth
With the mixing fine powders of manganese ore powder+coal dust+lime powder of mixing, stirring, loose naturally placing in the dephosphorization under reducing atmosphere crucible, cloth is even, loose;
7. the dephosphorization under reducing atmosphere crucible is placed on the middle crucible holder in the microwave reduction furnace chamber, close sealing cover, nitrogengas cylinder is imported nitrogen in furnace chamber, nitrogen input speed 10cm
3/ min makes in furnace chamber and the crucible to be in the nitrogen atmosphere;
8. open electric control box, microwave generator, microwave controller, thermocouple thermometer, liquid crystal display shows microwave heating restore information and temperature information;
Microwave heating heat-up rate: 20-50 ℃/min, accelerate gradually by low temperature to high temperature
Microwave heating reduction temperature: 1390 ℃ ± 10 ℃
Microwave heating power: 100KW
Constant temperature insulation time of repose: 20min ± 2min
Manganese ore powder+coal dust+lime powder absorbs the heat that microwave produces in reduction mould, carry out the hot autoreduction of carbon, generates solid-state sponge ferromanganese;
In airtight reduction furnace chamber, in reduction mould, produce solid carbon reduction, lime powder slag making, nitrogen atmosphere dephosphorisation reaction, reaction formula is as follows:
In the formula:
MnO
2-2SiO
2: manganous silicate
Ca
5[PO
4]
3F: contain calcium monofluorophosphate
Mn: manganese
P: phosphorus
CO: carbon monoxide
CaOSiO
2: Calucium Silicate powder
CaF
2: fluorite
9. handle phosphorous furnace gas
The CO furnace gas that contains phosphorous vapor that to be discharged by pore feeds airtight water cycle cooling tank, and phosphorous vapor is met cold one-tenth solid-state phosphorus, and deposits to the cooling tank bottom, regularly collects solid-state phosphorus and CO gas;
10. nitrogen atmosphere cooling
Turn-off the electric control box power supply, stop microwave heating, reduction, dephosphorization product cool off under nitrogen protection, are cooled to 20 ℃ ± 3 ℃ of normal temperature, and be 120min cooling time, nitrogen input speed 10cm
3/ min, the cooling back becomes sponge manganese iron powder product;
(5) fine grinding sponge manganese iron powder
With ball mill fine grinding sponge manganese iron powder, become finely powdered, sieve with 250 eye mesh screens, fine grinding, sieve and carry out repeatedly, make that powder is even, refinement, powder diameter≤0.057mm;
(6) dry type magnetic separation is purified
To the sponge manganese iron powder of reduction, dephosphorization treatment, purify with dry-type magnetic extractor, remove phosphorus slag and other impurity deviate from the sponge manganese iron powder;
1. with fine grinding, the sponge manganese iron powder that obtains that sieves places in the dry-type magnetic extractor, magnetic separation is purified under high-intensity magnetic field, the magneticstrength in the magnetic separator is 1-2 ten thousand Gausses;
2. after magnetic separation is purified, remove slag and objectionable impurities, get the dephosphorization after product: the sponge manganese iron powder;
(7) detect, chemically examine, analyze
Sponge manganese iron powder after dephosphorization, the purification is detected, chemically examines, analyzes its composition, phosphorus content, gloss, pattern;
Manganese content: 60-70%
Iron level: 20-30%
Phosphorus content :≤0.15%
(8) store
Sponge manganese iron powder to dephosphorization, after purifying will be stored in drying, clean environment with stainless steel vessel, waterproof, protection against the tide, anti-oxidation, acid-proof, alkali, salt corrosion, 20 ℃ ± 3 ℃ of storing temps, relative temperature≤20%.
2, the microwave heating, solid state reduction and gaseous dephosphorization method of a kind of manganese ore powder according to claim 1, it is characterized in that: described microwave heating crucible dephosphorization under reducing atmosphere stove, primary structure by: stove seat, bell, body of heater, furnace chamber, movable rack, thermocouple thermometer, dephosphorization under reducing atmosphere crucible, microwave generator, microwave controller, liquid crystal display, nitrogengas cylinder are formed; In the bottom of microwave oven body (1) is stove seat (2), top is sealing cover (4), bell (3), and by movable rack (5) control folding, in bell (3), sealing cover (4) is provided with thermocouple thermometer (13), pore (10), on the furnace wall of microwave oven body (1), be provided with microwave generator (6), in microwave oven body (1) furnace chamber (9), middle lower portion at furnace chamber (9) is crucible holder (7), the top of crucible holder (7) be dephosphorization under reducing atmosphere crucible (8) and on handle (11), being manganese ore powder+coal dust+lime powder (12) in dephosphorization under reducing atmosphere crucible (8), is nitrogen (24) in the furnace chamber (9); The nitrogengas cylinder of establishing at the sidepiece of microwave oven body (1) (21), and by nitrogen valve (22), nitrogen tube (23) and furnace chamber (9) UNICOM; Sidepiece at body of heater (1) is provided with electric control box (14), and electric control box (14) is provided with pilot lamp (16), liquid crystal display (15), microwave controller (17), power switch (20); Electric control box (14) connects with microwave generator (6) on the body of heater (1) by lead (19), electric control box (14) connects with thermocouple thermometer (13) on the body of heater (1) by lead (18), pore (10) connects furnace gas pipe (38), furnace gas pipe (38) UNICOM's water-cooled case (35), have water inlet pipe (36), rising pipe (37) on water-cooled case (35) right side, water-cooled case (35) internal upper part is phosphorous furnace gas (39), and the middle part is water coolant (40), and the bottom is solid-state phosphorus (41).
3, the microwave heating, solid state reduction and gaseous dephosphorization method of a kind of manganese ore powder according to claim 1, it is characterized in that: described microwave heating, solid state reduction, gasification dephosphorization, temperature is 1390 ℃ ± 10 ℃, constant temperature, insulation, time of repose are 20min ± 2min, and microwave generator power is 100KW ± 2KW.
4, the microwave heating, solid state reduction and gaseous dephosphorization method of a kind of manganese ore powder according to claim 1 is characterized in that: described microwave heating, solid state reduction, gasification dephosphorization, cooling, under nitrogen atmosphere, to finish, and the nitrogen input speed is 10cm
3/ min.
5, the microwave heating, solid state reduction and gaseous dephosphorization method of a kind of manganese ore powder according to claim 1, it is characterized in that: described microwave heating, solid state reduction, gasification dephosphorization, the solid state reduction rate of manganese ore powder is 95%, and the dephosphorization rate of manganese is 60-70%, phosphorous rate≤0.15% of manganese.
6, the microwave heating, solid state reduction and gaseous dephosphorization method of a kind of manganese ore powder according to claim 1, it is characterized in that: the processing of described phosphorous furnace gas, it is the phosphorous carbon monoxide furnace gas of will discharge in the microwave heating reduction furnace, feed airtight water cycle cooling tank, phosphorous vapor is met cold one-tenth solid-state phosphorus, and deposit to the cooling tank bottom, regularly collect solid-state phosphorus and CO (carbon monoxide converter) gas.
Priority Applications (1)
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| CN102230075A (en) * | 2011-06-20 | 2011-11-02 | 江苏大学 | Dephosphorizing process of molybdenum nickel ore |
| CN106906356A (en) * | 2017-03-17 | 2017-06-30 | 攀钢集团攀枝花钢铁研究院有限公司 | The processing unit and processing method of a kind of vanadium titano-magnetite |
| CN107513624A (en) * | 2016-06-16 | 2017-12-26 | 陕西盛华冶化有限公司 | The method that a kind of microwave treatment low-grade manganese reactor and microwave smelt low-grade manganese |
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| JP2021004382A (en) * | 2019-06-25 | 2021-01-14 | Ｊｆｅスチール株式会社 | Dephosphorization method of manganese oxide-containing substance, low phosphorus-containing manganese oxide-containing substance, and method for manufacturing steel using manganese oxide-containing substance |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4311520A (en) * | 1980-02-28 | 1982-01-19 | Cato Research Corporation | Process for the recovery of nickel, cobalt and manganese from their oxides and silicates |
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| CN114026041A (en) * | 2019-06-25 | 2022-02-08 | 杰富意钢铁株式会社 | Method for removing phosphorus from phosphorus-containing substance, method for producing raw material for metal smelting or metal refining, and method for producing metal |
| JP7067532B2 (en) | 2019-06-25 | 2022-05-16 | Ｊｆｅスチール株式会社 | A method for dephosphorizing a manganese oxide-containing substance, a method for producing a low-phosphorus-containing manganese oxide-containing substance, and a method for producing steel using the manganese oxide-containing substance. |
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