CN108080649A - A kind of method that hydrocarbon duplex reduction of low temperature prepares superfine iron powder - Google Patents
A kind of method that hydrocarbon duplex reduction of low temperature prepares superfine iron powder Download PDFInfo
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- CN108080649A CN108080649A CN201711340876.0A CN201711340876A CN108080649A CN 108080649 A CN108080649 A CN 108080649A CN 201711340876 A CN201711340876 A CN 201711340876A CN 108080649 A CN108080649 A CN 108080649A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
A kind of method that hydrocarbon duplex reduction of low temperature prepares superfine iron powder, Step 1: the fine iron breeze, carbon dust and catalyst of certain purity are distinguished ball milling；Step 2: the material after ball milling in the step 1 is uniformly mixed according to a certain percentage；Heating reduction is carried out Step 3: material after mixing is placed under protective atmosphere, a reduced iron is obtained after cooling；Step 4: a reduced iron described in step 3 is subjected to ball milling；Whole reduction is carried out Step 5: a reduced iron after ball milling in step 4 is placed under hydrogen atmosphere, comes out of the stove after cooling, obtains reduced iron powder；Step 6: reduced iron powder described in step 5 is carried out ball milling, superfine iron powder is obtained.The present invention has the advantages that reaction temperature is low, low energy consumption, hydrogen consumption is low etc. compared with prior art, is easy to get high-quality ultrafine iron powder, and preparation process is simple, low energy consumption, production cost is low.
Description
Technical field
The present invention relates to field of powder metallurgy preparation more particularly to a kind of prepare micron order, submicron-grade superfine iron powder
The hydrocarbon duplex reducing preparation method of low temperature.
Background technology
In the prior art, micron order iron powder is one of basic material of powder metallurgy industry, and granularity is 1~10 micron.
Micron order iron powder has larger specific surface area and activity, is mainly used for powder metallurgy, manufacture machine components, production friction material
The fields such as material, antifriction material, superhard material, magnetic material, lubricant and its product.In recent years, in electromagnetism, biology, medicine, light
Etc. numerous areas also have broad application prospects.Particularly the development of 3D printing technique will promote the market of superfine iron powder into
One step expands.
Traditional iron powder is most of to be produced by two stage reduction methods, i.e., the first step uses tunnel kiln reduction, obtains reduction rate about
For 97~98% ingot iron, become the iron powder of 100~200 mesh by broken and ball milling, then contained the oxygen of iron powder by hydrogen reduction
Amount is reduced to 0.5% or so.Due to tunnel kiln reduction temperature high (1150 DEG C), smelting cycle length (72h), so the first step obtains
To product be only ingot iron.Due to the ductility of iron in itself, it is difficult to which low cost is milled down to less than 40 microns, this iron powder is sold
Valency is low.Also the superfine iron powder technique having adds multi-level hierarchical, then the method for hydrogen reduction, the production of this technique using ball milling common iron powder
Measure that low, power consumption is high, recovery rate is low, economy is bad.
A small amount of iron powder technique uses atomization, melts ingot iron, then the atomization in rotation with intermediate frequency furnace first
The iron powder of the mesh of 100 mesh~200 is prepared on equipment, and cannot get superfine iron powder.Atomization is suitble to do alloyed powder.
Following several method can prepare superfine iron powder：
1) carbonyl process
The preparation method of carbonyl iron dust is generally common thermal decomposition method, that is, allows Fe (CO)5It directly decomposes at a certain temperature
Producing iron powder.The principle of laser pyrolysis processes is using continuous laser current system, by carbonyls Fe (CO)5It cracks to prepare
Superfine iron powder.But since carbonyl process system cost is higher, and Fe (CO)5For toxic explosive substance, the operation of entire technological process
Complicated, high processing costs, can produce in batches at present, form large-scale production.
2) gas phase reduction process
Gas phase reduction process is usually by FeCl2Molysite is waited to evaporate at high temperature, use H in the gas phase2Or NH3The reducing agent system of doing
Standby superfine iron powder.Reaction process is divided into molysite dehydration, evaporation and three steps of vapour phase reduction.A-Fe moments in gas phase reduction process
Nucleation, nucleation temperature is relatively low, and iron powder grain size is small, size distribution is concentrated；But because it is reacted in gas phase, reaction process is fine, holds
It is easily influenced by device etc., stability is bad, has not yet to see mass production.
3) solid phase reduction method
Solid phase reduction method is generally referred to as in H2Under atmosphere, by FeC2O4·2H2The presomas such as O or FeOOH decompose, reduction
To prepare superfine iron powder.Reduction temperature is proper at 510 DEG C.This method requires the preparation of presoma high, is also difficult at present
It is extensive to be made.
4) vacuum vapor deposition method and sputtering method
Vacuum vapor deposition method refers to make evaporation of metal in a vacuum, then its steam is cooled down and condensed, and obtains metal and surpass
The method of fine powder.Sputtering method is using sputtering phenomenon evaporation to be replaced to prepare dystectic super-fine metal powder, available for metallic iron
The preparation of powder.The advantages of this kind of method be the superfine powder size distribution for preparing concentrate, particle it is uniform, it is true when shortcoming is industrial production
Altitude is difficult to realize.
5) high-energy ball milling method
High-energy ball milling method is the rotation or vibration using ball mill, and hard sphere is made to carry out strong shock to metallic iron, mill
And stirring, powder is crushed the method for ultrafine dust.Since metallic iron has metal ductility, micron order, sub-micron are prepared
Grade iron powder difficulty is big, high energy consumption.
6) iron oxide high energy ball mill hydrogen reduction simultaneously
Pure raw iron oxide material is placed in ball mill ball milling to refine, and is obtained in 200~350 DEG C of logical hydrogen reducings ultra-fine
Iron powder.This method can obtain superfine iron powder, but the conversion ratio due to hydrogen at low temperature is relatively low, cause hydrogen usage amount inclined
It is high.
The content of the invention
In view of above-mentioned analysis, the present invention provides one kind, and low energy consumption, is easy to get high-quality ultrafine iron powder, and preparation process
Simply, the low superfine iron powder preparation method of production cost.
The purpose of the present invention is mainly achieved through the following technical solutions：
A kind of method that hydrocarbon duplex reduction of low temperature prepares superfine iron powder, the described method comprises the following steps：
Step 1: the fine iron breeze, carbon dust and catalyst of certain purity are distinguished into ball milling；
Step 2: the material after ball milling in the step 1 is uniformly mixed according to a certain percentage；
Heating reduction is carried out Step 3: material after mixing is placed under protective atmosphere, is obtained after cooling once also
Former iron；
Step 4: a reduced iron described in step 3 is subjected to ball milling；
Whole reduction is carried out Step 5: a reduced iron after ball milling in step 4 is placed under hydrogen atmosphere, after cooling
It comes out of the stove, obtains reduced iron powder；
Step 6: reduced iron powder described in step 5 is carried out ball milling, superfine iron powder is obtained.
Further, the step 1 by fine iron breeze specifically, be milled down to d50For 6 microns and d90<10 microns；By carbon
Powder is milled down to d50<10 microns and d90<20 microns；It is to be milled down to below 325 mesh by catalyst.
Further, the fine iron breeze is less than 0.2% containing full iron more than 71.0% and sour insoluble matter；The carbon dust
Ash content is less than 3%, and the sum of fugitive constituent and moisture are less than 8%.
Because preparing straight iron powder, the impurity content in carbon powder of reducing agent is unsuitable excessively high, and otherwise metal iron powder grade is subject to
It influences.Research shows that ash content is less than 3% in carbon dust, and the sum of content of water and fugitive constituent in carbon dust is less than 8%, because containing
Measure excessively high, the carbon dust total amount for being equivalent to addition becomes higher, and makes impurity content exceeding index.
Further, the catalyst is the mixture of potassium carbonate, sodium carbonate or the two.
Further, in the step 2, the mass ratio of fine iron breeze, carbon dust and catalyst is 100:15~20:0.5
~1.5.
A small amount of alkaline carbonic acid salt catalyst is added, can speed up the low-temp reaction performance of iron oxide, but excessive add in can make
Iron powder grade reduces, and it is the efficient additive of comparison that research, which shows that catalyst selects potassium carbonate, sodium carbonate or their mixture,
Addition is advisable with the 0.5~1.5% of fine iron breeze quality.
Carbon dust main purpose is to reduce the consumption of hydrogen reduction hydrogen.Carbon addition is very few, and hydrogen is reduced to technical process
Amount has little significance, and adds a process, adds cost；Carbon addition is excessively high, easily makes carbon content in iron powder exceeded,
Research shows that the addition of carbon is the 15~20% of Iron concentrate quality to be advisable.
Further, the temperature of reduction is heated in the step 3 as 800~850 DEG C, heating time is 2~3h, material
Layer thickness for 10mm~30mm, protective atmosphere is nitrogen or argon gas.
From dynamics, granularity is thinner, and reaction speed is faster or required reaction temperature is lower, therefore the present invention
Ultra-fine fine iron breeze carbon thermal reduction temperature is only 800~850 DEG C, and at this temperature, reaction iron crystal grain is not easy to grow up.Reaction temperature
Excessively high, iron powder easily sinters lump into, cannot get superfine iron powder.Recovery time, 2~3h was more suitable, when material thickness is relatively thin,
Recovery time selection is shorter, and vice versa.Long recovery time, iron powder are easily sintered.
The material thickness of reduction furnace is unsuitable blocked up, because the hybrid reactors density such as ultra-fine fine iron breeze, carbon dust is small, poor heat transfer,
Blocked up heat should not pass to material center.Research shows that 10~30mm material ratios are convenient.
Further, the step 4 by a reduced iron described in step 3 specifically, be milled to 325 mesh.
Iron powder by carbon reduction has been equivalent to material and mixing once, after levigate convenient for subsequent hydrogen reduction
Product quality is evenly.
Further, in the step 5, reduction temperature is 750 DEG C~800 DEG C, and material thickness is 10mm in reduction process
~30mm, recovery time are 1~3h.
Iron particle size is thin due to one time for hydrogen reduction, and unsuitable excessively high, excessively high, the iron powder easy-sintering of reduction temperature crosses low reaction not
Thoroughly.
Further, superfine iron powder described in step 6 is d50<7 microns, d90<12 microns of superfine iron powder.
Iron powder after hydrogen reduction forms magma, and heap density is about 0.5~0.7g/cm3It will, it is necessary to be milled down to the product specified
It asks.
Further, the atmosphere heating furnace used in reduction process is steel band atmosphere heating furnace or pushes away boat atmosphere heating furnace；
Heating process uses electrical heating or gas heating.
The present invention has the beneficial effect that：
The present invention for deficiency of the prior art, provide it is a kind of prepare micron order, submicron-grade superfine iron powder it is low
The hydrocarbon duplex reducing preparation method of temperature, by controlling the technological parameter of each step, obtains d50<7 microns and d90<12 microns
Superfine iron powder.
The present invention overcomes deficiencies of the prior art, if High Temperature Gas base and coal base reduction method reduction temperature are high, iron powder grain
Degree is big；High-energy ball milling method is extremely difficult, power consumption pole since the distinctive ductility of iron powder is milled down to micron order or submicron order
It is high.The present invention has the advantages that reaction temperature is low, low energy consumption, hydrogen consumption is low etc. compared with prior art, is easy to get high-quality
Superfine iron powder, and preparation process is simple, low energy consumption, production cost is low.
Compared with existing tunnel oven technique, 1150 DEG C of the reduction temperature of tunnel oven is reduced to 800~850 by the present invention
DEG C, heating time is reduced to 2~3h from 48h, it is often more important that the present invention can ensure once to reduce using such smelting condition
Iron particle size is subtle, and tunnel kiln reduction is then sintered seriously, becomes ingot iron.Work is prepared by the low temperature duplex of this superfine iron powder
Skill can reduce by 80% or so hydrogen gas consumption, and superfine iron powder manufacturing cost is greatly lowered.
Other features and advantages of the present invention will illustrate in the following description, also, part can become from specification
It obtains it is clear that being understood by implementing the present invention.The purpose of the present invention and other advantages can be by the explanations write
Specifically noted structure is realized and obtained in book, claims and attached drawing.
Description of the drawings
Attached drawing is only used for showing the purpose of specific embodiment, and is not considered as limitation of the present invention, in entire attached drawing
In, identical reference symbol represents identical component.
Fig. 1 is the process flow chart that the hydrocarbon duplex restoring method of low temperature of the present invention prepares superfine iron powder.
Fig. 2 is the particle size distribution figure for the superfine iron powder product that the present invention obtains.
Specific embodiment
The preferred embodiment of the present invention is specifically described below in conjunction with the accompanying drawings, wherein, attached drawing forms the application part, and
It is used to illustrate the principle of the present invention together with embodiments of the present invention.
For the deficiency in existing technology of preparing, for example, High Temperature Gas base and coal base reduction method reduction temperature are high, iron particle size
Greatly；High-energy ball milling method is extremely difficult since the distinctive ductility of iron powder is milled down to micron order or submicron order, and power consumption is high,
In order to prepare high pure and ultra-fine iron powder, the present invention develops the method that a kind of hydrocarbon duplex reduction of low temperature prepares superfine iron powder, including
Following steps：
The pure iron concentrate powder (sour insoluble matter is less than 0.2%) of full iron more than 71.0% is passed through ball by the first step, ball milling
Grinding machine is milled down to d50About 6 microns, d90<10 microns, (ash content is less than 3% to pure carbon powder, and fugitive constituent+moisture is less than 8%) levigate
To d50<10 microns, d90<20 microns, catalyst is potassium carbonate (analysis is pure), sodium carbonate (analysis is pure) or combination are levigate
To below 325 mesh.
A small amount of alkaline carbonic acid salt catalyst is added, can speed up the low-temp reaction performance of iron oxide, but excessive add in can make
Iron powder grade reduces, and it is the efficient additive of comparison that research, which shows that catalyst selects potassium carbonate, sodium carbonate or their mixture,
Addition is advisable with the 0.5~1.5% of fine iron breeze quality.
Second step, dispensing, mixing, by levigate fine iron breeze, carbon dust, catalyst according to mass ratio 100:15~20:0.5
~1.5 dispensings, then mixing.
3rd step, carbon reduction, the material after mixing is placed in atmosphere protection heating furnace and heats reduction, protective atmosphere is nitrogen
Gas or argon gas, 800~850 DEG C, 2~3h of heating time, layer thickness 10mm~30mm of temperature obtain once after reduction cooling
Reduced iron.
The preparation method of superfine iron powder proposed by the invention combines the excellent of gas-based reduction method, carbon thermal reduction and ball-milling method
Gesture, iron oxide belongs to brittle substance, and iron powder belongs to ductile material, therefore iron oxide is easier to be crushed to micrometer level.By
Dynamics understands that granularity is thinner, and reaction speed is faster or required reaction temperature is lower, therefore the ultra-fine iron ore concentrate of the present invention
Powder carbon thermal reduction temperature is only 800~850 DEG C, and at this temperature, reaction iron crystal grain is not easy to grow up.Reaction temperature is excessively high, iron powder
It easily sinters lump into, cannot get superfine iron powder.Recovery time, 2~3h was more suitable, when material thickness is relatively thin, recovery time choosing
Select shorter, vice versa.Long recovery time, iron powder are easily sintered.
Because preparing straight iron powder, the impurity content in carbon powder of reducing agent is unsuitable excessively high, and otherwise metal iron powder grade is subject to
It influences.Research shows that ash content is less than 3% in carbon dust, and the sum of content of water and fugitive constituent in carbon dust is less than 8%, because containing
Measure excessively high, the carbon dust total amount for being equivalent to addition becomes higher, and makes impurity content exceeding index.Carbon dust main purpose is to reduce hydrogen reduction hydrogen
Consumption.Carbon addition is very few, and reducing amounts of hydrogen to technical process has little significance, and adds a process, adds into
This；Carbon addition is excessively high, easily makes carbon content in iron powder exceeded, research show carbon addition be Iron concentrate quality 15~
20% is advisable.
The material thickness of reduction furnace is unsuitable blocked up, because the hybrid reactors density such as ultra-fine fine iron breeze, carbon dust is small, poor heat transfer,
Blocked up heat should not pass to material center.Research shows that 10~30mm material ratios are convenient.
Reduced iron powder is milled down to 325 mesh by the 4th step, a reduced iron ball milling in ball mill.
Iron powder by carbon reduction has been equivalent to material and mixing once, after levigate convenient for subsequent hydrogen reduction
Product quality is evenly.
5th step, hydrogen reduction, will be levigate after a reduced iron powder be put into atmosphere protection heating furnace with hydrogen carry out eventually
Reduction, 750 DEG C~800 DEG C, material thickness 10mm~30mm, 1~3h of recovery time of reduction temperature, iron powder is by heating after reduction
It comes out of the stove after the cooling section cooling of stove.
Iron particle size is thin due to one time for hydrogen reduction, and unsuitable excessively high, excessively high, the iron powder easy-sintering of reduction temperature crosses low reaction not
Thoroughly.Research shows that the hydrogen reduction condition that originally a reduced iron powder is suitable is：10~30mm of reduced iron powder thickness, a heating
750 DEG C~800 DEG C of 1~3h of time, heating temperature.
Iron powder after hydrogen reduction is milled down to d by the 6th step, H-iron ball milling by ball mill50<7 microns, d90<
12 microns of superfine iron powder.
Iron powder after hydrogen reduction forms magma, and heap density is about 0.5~0.7g/cm3It will, it is necessary to be milled down to the product specified
It asks.
In the present invention, carbon reduction heating furnace and hydrogen reduction heating hotplate body can be used steel band atmosphere heating furnace or push away boat atmosphere
Heating furnace, they can realize atmosphere protection and be passed through the function of hydrogen reducing.Electrical heating or gas heating can be used in heating.
Various raw materials and product can be milled down to designated size by the present invention using existing levigate equipment, such as high pressure roller+gas
Flow point grade, airflow milling+air current classifying, impact grinding+air current classifying, Ball-stirring mill etc., but it is not limited to above equipment.
Compared with tunnel oven technique, 1150 DEG C of the reduction temperature of tunnel oven is reduced to 800~850 DEG C by the present invention, heating
Time is reduced to 2~3h from 48h, it is often more important that the present invention can ensure a reduced iron powder granularity using such smelting condition
It is subtle, and tunnel kiln reduction is then sintered seriously, becomes ingot iron.It, can be with by the low temperature duplex preparation process of this superfine iron powder
80% or so hydrogen gas consumption is reduced, superfine iron powder manufacturing cost is greatly lowered.
Embodiment explanation
Embodiment 1-3 prepares superfine iron powder according to the hydrocarbon duplex reduction of low temperature of the present invention, iron ore concentrate in embodiment
Meal component is shown in Table 1, and carbon dust ingredient is shown in Table 2, and sodium carbonate, potassium carbonate are using analysis pure raw material.
1 pure iron concentrate meal component of table/wt%
| TFe | Moisture content | Acid non-soluble substance |
| 71.3 | <1.0 | 0.1 |
2 carbon dust ingredient of table/wt%
| Fugitive constituent | Ash | Fixed carbon | Moisture content |
| 4.25 | 1.44 | 91.91 | 2.40 |
Pure iron oxide is milled down to d50About 6 microns, d90<10 microns, pure carbon powder is milled down to d50<10 microns, d90<
20 microns, catalyst is milled down to below 325 mesh.
In embodiment, carried out in a manner that high pressure roller mill is combined with gas flow sizing machine levigate to fine iron breeze；Using punching
It hits the mode that mill is combined with air current classifying and Ultrafine Grinding is carried out to carbon dust；Using general milling machine to catalyst and a reduced iron into
Row is levigate；Fine grinding is carried out to the iron powder after hydrogen reduction in a manner that impact grinding is combined with gas flow sizing machine.
Embodiment 1-3 is tested according to the proportioning of table 3, and the heating furnace in embodiment is steel strip heating furnace, according to the carbon of table 3
Reducing condition is reduced, and reduction process is protected using nitrogen, it is milled down to 325 mesh water by ball mill after product cooling
It is flat.Then hydrogen reduction is carried out according to the hydrogen reduction condition of table 3, by ball milling to d after product cooling50<7 microns, d90<12 microns
Superfine iron powder.
3 implementation condition of table and result
Embodiment 1
Fine iron breeze, carbon dust and catalyst K2CO3Dispensing mass ratio be 100:16.5:0.6；Carry out the temperature of carbon reduction
For 820 DEG C, heating time 1.5h, layer thickness 20mm；The temperature of hydrogen reduction is carried out as 790 DEG C, heating time 2.0h, paving
Expect thickness 20mm；The content that all iron content is 98.5%, C in final superfine iron powder product is 0.02%, and residual oxygen content is
0.25%, acid non-soluble substance content is 0.1%.
Embodiment 2
Fine iron breeze, carbon dust and catalyst n a2CO3Dispensing mass ratio be 100:18.2:1.2；Carry out the temperature of carbon reduction
For 840 DEG C, heating time 2.5h, layer thickness 25mm；The temperature of hydrogen reduction is carried out as 760 DEG C, heating time 2.5h, paving
Expect thickness 25mm；The content that all iron content is 98.3%, C in final superfine iron powder product is 0.03%, and residual oxygen content is
0.26%, acid non-soluble substance content is 0.09%.
Embodiment 3
The dispensing mass ratio of fine iron breeze, carbon dust and catalyst is 100:16.5:1.3, catalyst K2CO3And Na2CO3
Mixture, wherein K2CO3For 0.5%, Na2CO3For 0.8%；The temperature of carbon reduction is carried out as 820 DEG C, heating time is
1.5h, layer thickness 20mm；The temperature for carrying out hydrogen reduction is 790 DEG C, heating time 2.0h, layer thickness 20mm；Final
The content that all iron content is 98.5%, C in superfine iron powder product is 0.02%, and residual oxygen content is 0.25%, acid non-soluble substance content
For 0.1%.
The chemical composition that product is obtained in embodiment 1-3 meets national Powder Metallurgy Industry requirement, and wherein carbon residue, acid is insoluble
Object, residual oxygen etc. are below similar other superfine iron powders, and final products size distribution is shown in Fig. 2, d50For 5.76 microns, d90For
10.98 microns, all by 21.21 microns, the apparent density of this product is in 1.2~1.5g/cm3。
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto,
Any one skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in,
It should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of method that hydrocarbon duplex reduction of low temperature prepares superfine iron powder, which is characterized in that the described method comprises the following steps：
Step 1: the fine iron breeze, carbon dust and catalyst of certain purity are distinguished into ball milling；
Step 2: the material after ball milling in the step 1 is uniformly mixed according to a certain percentage；
Heating reduction is carried out Step 3: material after mixing is placed under protective atmosphere, a reduced iron is obtained after cooling；
Step 4: a reduced iron described in step 3 is subjected to ball milling；
Whole reduction is carried out Step 5: a reduced iron after ball milling in step 4 is placed under hydrogen atmosphere, is come out of the stove after cooling,
Obtain reduced iron powder；
Step 6: reduced iron powder described in step 5 is carried out ball milling, superfine iron powder is obtained.
2. the method that the hydrocarbon duplex reduction of low temperature prepares superfine iron powder according to claim 1, which is characterized in that the step
One by fine iron breeze specifically, be milled down to d50For 6 microns and d90<10 microns；Carbon dust is milled down to d50<10 microns and d90<20 is micro-
Rice；It is to be milled down to below 325 mesh by catalyst.
3. the method that the hydrocarbon duplex reduction of low temperature prepares superfine iron powder according to claim 1, which is characterized in that the iron essence
Miberal powder is less than 0.2% containing full iron more than 71.0% and sour insoluble matter；The ash content of the carbon dust is less than 3%, fugitive constituent and moisture
The sum of be less than 8%.
4. the method that the hydrocarbon duplex reduction of low temperature prepares superfine iron powder according to claim 1, which is characterized in that the catalysis
Agent is the mixture of potassium carbonate, sodium carbonate or the two.
5. the method that the hydrocarbon duplex reduction of low temperature prepares superfine iron powder according to claim 1, which is characterized in that the step
In two, the mass ratio of fine iron breeze, carbon dust and catalyst is 100:15~20:0.5~1.5.
6. the method that the hydrocarbon duplex reduction of low temperature prepares superfine iron powder according to claim 1, which is characterized in that the step
The temperature of reduction is heated in three as 800~850 DEG C, heating time is 2~3h, and the layer thickness of material is 10mm~30mm, is protected
It is nitrogen or argon gas to protect atmosphere.
7. the method that the hydrocarbon duplex reduction of low temperature prepares superfine iron powder according to claim 1, which is characterized in that the step
Four by a reduced iron described in step 3 specifically, be milled to 325 mesh.
8. the method that the hydrocarbon duplex reduction of low temperature prepares superfine iron powder according to claim 1, which is characterized in that the step
In five, reduction temperature is 750 DEG C~800 DEG C, and material thickness is 10mm~30mm in reduction process, and the recovery time is 1~3h.
9. according to the method that the hydrocarbon duplex reduction of low temperature any one of claim 1-8 prepares superfine iron powder, feature exists
In superfine iron powder described in step 6 is d50<7 microns, d90<12 microns of superfine iron powder.
10. according to the method that the hydrocarbon duplex reduction of low temperature any one of claim 1-9 prepares superfine iron powder, feature exists
In the atmosphere heating furnace used in reduction process is steel band atmosphere heating furnace or pushes away boat atmosphere heating furnace；Heating process is using electricity
Heating or gas heating.
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| CN110029200A (en) * | 2019-03-28 | 2019-07-19 | 钢铁研究总院 | The iron powder preparation method of acid non-soluble substance content in a kind of reduction iron material |
| CN110170646A (en) * | 2019-07-01 | 2019-08-27 | 重庆有研重冶新材料有限公司 | Superfine iron powder and its production method |
| CN110900822A (en) * | 2019-11-08 | 2020-03-24 | 南京赛诺特斯材料科技有限公司 | Composite additive for improving ceramic performance of zirconia powder |
| CN111872412A (en) * | 2020-07-30 | 2020-11-03 | 钢研晟华科技股份有限公司 | Preparation method of metal iron powder for powder metallurgy |
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| CN112267003A (en) * | 2020-09-24 | 2021-01-26 | 山东鲁银新材料科技有限公司 | Preparation method of water atomized pure iron powder with ultrahigh cleanliness, low oxygen and high performance |
| CN112410493A (en) * | 2020-11-02 | 2021-02-26 | 钢研晟华科技股份有限公司 | Method for preparing metal powder by hydrogen reduction |
| CN113265507A (en) * | 2021-06-28 | 2021-08-17 | 王恩礼 | Oxygen-free reduction process for iron oxide ore and closed reduction converter thereof |
| CN113462842A (en) * | 2021-05-31 | 2021-10-01 | 钢研晟华科技股份有限公司 | Method for preparing high-titanium slag powder and metal iron powder by reducing ilmenite concentrate powder at low temperature |
| WO2023067497A1 (en) * | 2021-10-19 | 2023-04-27 | Pometon Spa | Process and plant for obtaining metal powders for burners |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1641053A (en) * | 2005-01-07 | 2005-07-20 | 梅卫东 | Composite additive for vanadium-titanium magnetite reduction |
| CN101586172A (en) * | 2009-07-06 | 2009-11-25 | 何德武 | Method for preparing metallized pellet and reduced iron powder |
| US20110300062A1 (en) * | 2010-02-05 | 2011-12-08 | Di Luca Carla D | Environmentally friendly system and method for manufacturing iron powder |
| CN104190950A (en) * | 2014-07-25 | 2014-12-10 | 玉溪大红山矿业有限公司 | Iron powder production process |
| CN106238745A (en) * | 2016-08-19 | 2016-12-21 | 朝阳金河粉末冶金材料有限公司 | The method utilizing strip stove temperature production reduced iron powder |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR970002097B1 (en) * | 1994-12-20 | 1997-02-22 | 김만제 | Method of iron powder |
-
2017
- 2017-12-14 CN CN201711340876.0A patent/CN108080649B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1641053A (en) * | 2005-01-07 | 2005-07-20 | 梅卫东 | Composite additive for vanadium-titanium magnetite reduction |
| CN101586172A (en) * | 2009-07-06 | 2009-11-25 | 何德武 | Method for preparing metallized pellet and reduced iron powder |
| US20110300062A1 (en) * | 2010-02-05 | 2011-12-08 | Di Luca Carla D | Environmentally friendly system and method for manufacturing iron powder |
| CN104190950A (en) * | 2014-07-25 | 2014-12-10 | 玉溪大红山矿业有限公司 | Iron powder production process |
| CN106238745A (en) * | 2016-08-19 | 2016-12-21 | 朝阳金河粉末冶金材料有限公司 | The method utilizing strip stove temperature production reduced iron powder |
Non-Patent Citations (2)
| Title |
|---|
| 赵沛等: "利用粉体纳米晶化促进低温冶金反应的研究", 《钢铁》 * |
| 郭培民等: "低温下碳还原氧化铁的催化机理研究", 《钢铁钒钛》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110029200A (en) * | 2019-03-28 | 2019-07-19 | 钢铁研究总院 | The iron powder preparation method of acid non-soluble substance content in a kind of reduction iron material |
| CN110170646B (en) * | 2019-07-01 | 2021-08-24 | 重庆有研重冶新材料有限公司 | Superfine iron powder and its production process |
| CN110170646A (en) * | 2019-07-01 | 2019-08-27 | 重庆有研重冶新材料有限公司 | Superfine iron powder and its production method |
| CN110900822A (en) * | 2019-11-08 | 2020-03-24 | 南京赛诺特斯材料科技有限公司 | Composite additive for improving ceramic performance of zirconia powder |
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| CN112410493A (en) * | 2020-11-02 | 2021-02-26 | 钢研晟华科技股份有限公司 | Method for preparing metal powder by hydrogen reduction |
| CN112222418A (en) * | 2020-12-07 | 2021-01-15 | 西安稀有金属材料研究院有限公司 | Method for preparing nano tungsten powder by regulating nucleation and growth processes and application |
| CN113462842A (en) * | 2021-05-31 | 2021-10-01 | 钢研晟华科技股份有限公司 | Method for preparing high-titanium slag powder and metal iron powder by reducing ilmenite concentrate powder at low temperature |
| CN113265507A (en) * | 2021-06-28 | 2021-08-17 | 王恩礼 | Oxygen-free reduction process for iron oxide ore and closed reduction converter thereof |
| WO2023067497A1 (en) * | 2021-10-19 | 2023-04-27 | Pometon Spa | Process and plant for obtaining metal powders for burners |
| WO2023067498A1 (en) * | 2021-10-19 | 2023-04-27 | Pometon Spa | Plant and use of a plant for obtaining metal powders for burners |
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