CN104308170A - Superfine iron powder preparation method - Google Patents
Superfine iron powder preparation method Download PDFInfo
- Publication number
- CN104308170A CN104308170A CN201410606384.1A CN201410606384A CN104308170A CN 104308170 A CN104308170 A CN 104308170A CN 201410606384 A CN201410606384 A CN 201410606384A CN 104308170 A CN104308170 A CN 104308170A
- Authority
- CN
- China
- Prior art keywords
- iron powder
- superfine iron
- fluidized bed
- bed furnace
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
Aiming at solving the problems of production process complexity, large equipment investment and high production cost during superfine iron powder preparation in the prior art, the invention provides a superfine iron powder preparation method and belongs to the field of powder metallurgy. The superfine iron powder preparation method includes: placing ferrous oxalate powder prepared from liquid-phase synthesis into a fluidized bed furnace and feeding gas in the weakly reducing atmosphere into the fluidized bed furnace, so that the ferrous oxalate powder is in fluidized movement in the fluidized bed furnace under the action of gas flow; heating the furnace to 350-500 DEG C, holding and reacting for 1-3 hours, so that superfine iron powder can be obtained. The superfine iron powder preparation method has the advantages that special hydrogen production equipment is unneeded, and the prepared superfine iron powder is more disperse, avoids aftertreatment processes such as crushing and is finer in granularity, larger in specific surface area, good in sphericity degree and more uniform in grain distribution.
Description
Technical field
The invention belongs to field of powder metallurgy, be specifically related to a kind of preparation method of superfine iron powder.
Background technology
Superfine iron powder is one of basic material of powder metallurgy industry, owing to having larger specific area and activity, thus has the performance that electricity, magnetic, light and catalysis, absorption and chemical reactivity etc. are special.Therefore, purposes is very extensive, is mainly used in powder metallurgy, manufacturing machine part, produces friction material, antifriction material, superhard material, magnetic material, lubricant and goods thereof.Secondly iron powder is widely used in chemical industry, cutting, exothermic material, welding rod etc.In recent years, iron powder also has broad application prospects at numerous areas such as electromagnetism, biology, medical science, optics.
As iron powder is applied widely in sulfate process titanium dioxide is produced, be mainly used in ferric reduction.The application of iron powder in powdered metal parts is produced, iron powder output 85% for the manufacture of powdered metal parts, wherein the powdered metal parts of 70% ~ 83% is used for auto industry.The application of iron powder in magnetic material, the iron powder that particle diameter is less than 5nm has good magnetic.Magnetic fluid is a kind of new function material, it can by magnetic control, ring-type magnetic field is produced in rotatory sealing place with ringshaped magnet, magnetic fluid is constrained among magnetic field and form magnetic fluid ring, for nothing wearing and tearing, long-life dynamic seal (packing), after magnetic fluid is magnetized, magnetic pressure increases, object in magnetic fluid can float, and can be used for the development of magnetic liquid densimeter.The application of superfine iron powder in medicine and food, utilizes nanometer technology and advanced biotechnology to combine, with superfine iron powder as carrier, guides to diseased region under can making the effect of medicine outside magnetic field, make it play special medical function.The application of iron powder in welding rod manufacturing industry, iron powder is also the manufacturing primary raw material of development high efficiency electrode, and its consumption accounts for 14% ~ 20% of the total consumption of iron powder.Superfine iron powder can as vehicle maintenance service, chemical industry, metallurgical catalyst, be applied to the manufacturing of superhard material, carbide alloy, heavy alloy, plant equipment, coating, rubber pigment etc., also can be applicable to agricultural-seed preferably, seed purification, soil improvement etc.
The preparation method of superfine iron powder mainly comprises chemical method and Physical.Chemical method comprises: gas phase reduction process, solid phase reduction method, carbonyl process, microemulsion method, electrolysis, freeze-drying.Physical comprises plasma physics chemical method, evaporation, sputtering method, high-energy ball milling method, atomization.From current technical merit, it is all more ripe that reducing process, microemulsion method and ball-milling method prepare superfine iron powder technology.Wherein, gas phase reduction process and microemulsion method can prepare the very thin superfine iron powder of particle diameter, and ball milling rule is only suitable for the thicker product preparation of granularity.Gas phase reduction process and microemulsion method complicated operation, cost is high and higher to the requirement of equipment.
On market, superfine iron powder is mainly based on carbonyl iron dust, particle diameter is at 1-10um, pattern is spherical, the production process of carbonyl iron dust, strict to ingredient requirement, be generally raw material with reducing sponge iron, simultaneously, need the CO device of high-purity, under high temperature, high pressure, complete the reaction of synthetic reaction Sum decomposition.Production process is complicated, equipment investment is large, the high development to carbonyl iron dust of production cost has a significant impact.Current domestic existing part producer adopts reducing process to produce superfine iron powder, mainly pushes away boat stove based on reduction, supporting fragmentation, screening plant, but because of equipment restriction, production cost is higher, and product pattern is irregular simultaneously, and particle diameter is uneven, uses and is subject to also to a definite limitation.Other also comprise hydrogen reducing molysite precursor power superfine iron powder, and the iron powder obtained has good dendroid pattern, and epigranular, production cost is low.But hydrogen needs special product hydrogen storage equipment, the iron powder simultaneously obtained need through operation after fragmentation etc.
Summary of the invention
Goal of the invention of the present invention is: for above-mentioned superfine iron powder preparation method Problems existing, provide a kind of preparation method of superfine iron powder, the method cost is low, iron powder pattern is spherical, even particle size distribution, without the need to special product hydrogen storage equipment, and the iron powder obtained is without the need to rear operations such as fragmentations.
The technical solution used in the present invention is as follows:
A preparation method for superfine iron powder, step is as follows:
The ferrous oxalate powder crossing 150-300 mesh sieve prepared by liquid phase synthesis puts into fluidized bed furnace, co-current flow state stove passes into the gas of the weakly reducing atmosphere be made up of 1-5% reducibility gas and 95-99% inert gas, and ferrous oxalate powder does fluidization campaign under the effect of air-flow in fluidized bed furnace; 350-500 DEG C will be heated in stove and keep this temperature, through reaction in 1-3 hour, can superfine iron powder be obtained;
The chemical equation occurred in this process is as follows:
Wherein, described ferrous oxalate add the 1/6-1/3 that volume is fluidized bed furnace volume;
Described reducibility gas is at least one in hydrogen, carbon monoxide, methane; Described inert gas is at least one in nitrogen, carbon dioxide, argon gas;
The gas of described weakly reducing atmosphere passes into by bottom fluidized bed furnace, and flow velocity is 5-10m/s;
In described stove, heating ramp rate is 5-10 DEG C/h;
Described by mode of heating in stove, by electrical heating, heating using microwave or infrared heating.
Principle of the present invention is: fluidization refers to fluidization of solid, liquefy also known as vacation, be called for short fluidisation, it is the effect utilizing streaming flow, solid particle group is suspended, thus makes solid particle have some fluid appearance features, utilize the way of contact between this fluid and solid to realize the operation of production process, be called fluidization technology, belong to the research category of powder technology.Fluidization technology is the operation of a kind of strengthening fluid (gas or liquid) and solid particle interphase interaction, as added granular solids material off and on or continuously in upright container, control fluid to be passed into by bottom with certain speed, its Pressure Drop is equaled or slightly larger than the weight of solid particle on unit section, the i.e. motion and unlikelyly to be taken away by fluid in suspension of solid particle.
Fluidized bed furnace, Gu it have gas-between heat exchanges that matter exchanges that speed is fast, temperature is average in layer, commercial quality good, heat transfer parameter between fluidize bed and cooler wall is large, the rate of output is high, it is simple and easy to operate, be convenient to realization produces and change in succession and a series of strong point such as automation, so obtain deep application.
The present invention compared with prior art, it is advantageous that:
1, this technique adopts fluidized bed furnace, ferrous oxalate is in suspension and tumbling state, and be in motion and collision status each other, avoid the reunion of product in calcination process, superfine iron powder is disperseed more and avoids product to need broken grade for last handling process, granularity is thinner, specific area is larger, and sphericity is also better, under all ferrous oxalate particles are in identical atmosphere and state, so the superfine iron powder granularity distribution of gained is more even.
2, the iron powder surface-active due to harsh one-tenth is very strong, and in order to avoid oxidation, the gas shield that need pass into weakly reducing atmosphere avoids it oxidized.
3, the gas of weakly reducing atmosphere can adopt some industrial tail gas, comprises water-gas etc., avoid and need special product hydrogen storage equipment, thus cost is lower.
Detailed description of the invention
Embodiment 1
Mistake 200 ~ 250 object ferrous oxalate powder prepared by liquid phase synthesis joins in fluidized bed furnace, add that volume is fluidized bed furnace volume 1/5, bottom fluidized bed furnace, pass into the gas of the weakly reducing atmosphere be made up of 1% hydrogen and 99% nitrogen, gas flow rate is 5m/s; Use heating using microwave fluidized bed furnace, heating rate is 8 DEG C/h, in-furnace temperature is risen to 450 DEG C, and ferrous oxalate powder does fluidization campaign under the effect of gas flow in fluidized bed furnace, can obtain superfine iron powder through reaction in 2 hours.
Obtained superfine iron powder index is as follows:
| Main content (%) | BET(m 2/g) | Granularity (um) | (D90-D10)/D50 |
| 99.85 | 15 | 0.9 | 1.1 |
Embodiment 2
Mistake 150 ~ 200 object ferrous oxalate powder prepared by liquid phase synthesis joins in fluidized bed furnace, add that volume is fluidized bed furnace volume 1/4, bottom fluidized bed furnace, pass into the gas of the weakly reducing atmosphere be made up of 2.5% methane gas and 97.5% argon gas, gas flow rate is 8.5m/s; Use infrared heating fluidized bed furnace, heating rate is 10 DEG C/h, in-furnace temperature is risen to 500 DEG C, and ferrous oxalate powder does fluidization campaign under the effect of gas flow in fluidized bed furnace, can obtain superfine iron powder through reaction in 1 hour.
Obtained superfine iron powder index is as follows:
| Main content (%) | BET(m 2/g) | Granularity (um) | (D90-D10)/D50 |
| 99.81 | 16 | 0.8 | 1.2 |
Embodiment 3
Mistake 250 ~ 300 object ferrous oxalate powder prepared by liquid phase synthesis joins in fluidized bed furnace, add that volume is fluidized bed furnace volume 1/6, bottom fluidized bed furnace, pass into the gas of the weakly reducing atmosphere be made up of 5% carbon monoxide and 95% carbon dioxide, gas flow rate is 10m/s; Use electrical heating fluidized bed furnace, heating rate is 5 DEG C/h, in-furnace temperature is risen to 350 DEG C, and ferrous oxalate powder does fluidization campaign under the effect of gas flow in fluidized bed furnace, can obtain superfine iron powder through reaction in 2 hours.
Obtained superfine iron powder index is as follows:
| Main content (%) | BET(m 2/g) | Granularity (um) | (D90-D10)/D50 |
| 99.89 | 13.5 | 0.89 | 1.0 |
Embodiment 4
The mistake 300 object ferrous oxalate powder prepared by liquid phase synthesis joins in fluidized bed furnace, add that volume is fluidized bed furnace volume 1/3, bottom fluidized bed furnace, pass into the gas of the weakly reducing atmosphere be made up of 0.5% carbon monoxide, 2% hydrogen and 90% carbon dioxide, 7.5% argon gas, gas flow rate is 9m/s; Use infrared heating fluidized bed furnace, heating rate is 8 DEG C/h, in-furnace temperature is risen to 350 DEG C, and ferrous oxalate powder does fluidization campaign under the effect of gas flow in fluidized bed furnace, can obtain superfine iron powder through reaction in 3 hours.
Obtained superfine iron powder index is as follows:
| Main content (%) | BET(m 2/g) | Granularity (um) | (D90-D10)/D50 |
| 99.80 | 14.5 | 0.95 | 1.2 |
Embodiment 5
The mistake 300 object ferrous oxalate powder prepared by liquid phase synthesis joins in fluidized bed furnace, add that volume is fluidized bed furnace volume 1/3, bottom fluidized bed furnace, pass into the gas of the weakly reducing atmosphere be made up of 0.5% carbon monoxide, 1% hydrogen, 1% methane and 10% nitrogen, 80% carbon dioxide, 7.5% argon gas, gas flow rate is 9m/s; Use infrared heating fluidized bed furnace, heating rate is 8 DEG C/h, in-furnace temperature is risen to 350 DEG C, and ferrous oxalate powder does fluidization campaign under the effect of gas flow in fluidized bed furnace, can obtain superfine iron powder through reaction in 3 hours.
Obtained superfine iron powder index is as follows:
| Main content (%) | BET(m 2/g) | Granularity (um) | (D90-D10)/D50 |
| 99.84 | 14.1 | 0.93 | 1.12 |
Embodiment 6
The mistake 300 object ferrous oxalate powder prepared by liquid phase synthesis joins in fluidized bed furnace, add that volume is fluidized bed furnace volume 1/3, bottom fluidized bed furnace, pass into the gas of the weakly reducing atmosphere be made up of 3% carbon monoxide, 1% hydrogen, 1% methane and 75% nitrogen, 10% carbon dioxide, 10% argon gas, gas flow rate is 9m/s; Use infrared heating fluidized bed furnace, heating rate is 8 DEG C/h, in-furnace temperature is risen to 350 DEG C, and ferrous oxalate powder does fluidization campaign under the effect of gas flow in fluidized bed furnace, can obtain superfine iron powder through reaction in 3 hours.
Obtained superfine iron powder index is as follows:
| Main content (%) | BET(m 2/g) | Granularity (um) | (D90-D10)/D50 |
| 99.86 | 13.4 | 0.91 | 1.10 |
Embodiment 7
The mistake 300 object ferrous oxalate powder prepared by liquid phase synthesis joins in fluidized bed furnace, add that volume is fluidized bed furnace volume 1/3, bottom fluidized bed furnace, pass into the gas of the weakly reducing atmosphere be made up of 2% carbon monoxide, 0.5% methane and 90% nitrogen, 7.5% argon gas, gas flow rate is 9m/s; Use infrared heating fluidized bed furnace, heating rate is 8 DEG C/h, in-furnace temperature is risen to 350 DEG C, and ferrous oxalate powder does fluidization campaign under the effect of gas flow in fluidized bed furnace, can obtain superfine iron powder through reaction in 3 hours.
Obtained superfine iron powder index is as follows:
| Main content (%) | BET(m 2/g) | Granularity (um) | (D90-D10)/D50 |
| 99.78 | 12.8 | 1.01 | 1.04 |
Embodiment 8
The mistake 300 object ferrous oxalate powder prepared by liquid phase synthesis joins in fluidized bed furnace, add that volume is fluidized bed furnace volume 1/3, bottom fluidized bed furnace, pass into the gas of the weakly reducing atmosphere be made up of 0.5% methane, 2% hydrogen and 90% nitrogen, 7.5% carbon dioxide, gas flow rate is 9m/s; Use infrared heating fluidized bed furnace, heating rate is 8 DEG C/h, in-furnace temperature is risen to 350 DEG C, and ferrous oxalate powder does fluidization campaign under the effect of gas flow in fluidized bed furnace, can obtain superfine iron powder through reaction in 3 hours.
Obtained superfine iron powder index is as follows:
| Main content (%) | BET(m 2/g) | Granularity (um) | (D90-D10)/D50 |
| 99.87 | 13.2 | 1.02 | 0.99 |
Comparative example 1
When other conditions of embodiment 1 are constant, only furnace temperature is risen to 300 DEG C, the main content of final iron powder only has 92.5%, and iron powder purity obviously reduces.
Comparative example 2
When other conditions of embodiment 2 are constant, only gas flow rate is become 3m/s, the specific area of final iron powder is 7.2m
2/ g, and (D90-D10)/D50 is 3.0, specific area and the uniform particle sizes degree of iron powder are obviously deteriorated.
Claims (8)
1. a preparation method for superfine iron powder, is characterized in that, step is as follows:
The ferrous oxalate powder prepared by liquid phase synthesis puts into fluidized bed furnace, and pass into the gas of weakly reducing atmosphere in co-current flow state stove, ferrous oxalate powder does fluidization campaign under the effect of air-flow in fluidized bed furnace; 350-500 DEG C will be heated in stove simultaneously and keep this temperature, through reaction in 1-3 hour, can superfine iron powder be obtained.
2. the preparation method of a kind of superfine iron powder according to claim 1, is characterized in that, the granularity of described ferrous oxalate powder was 150-300 mesh sieve.
3. the preparation method of a kind of superfine iron powder according to claim 1, is characterized in that, described ferrous oxalate add the 1/6-1/3 that volume is fluidized bed furnace volume.
4. the preparation method of a kind of superfine iron powder according to claim 1, is characterized in that, described weakly reducing atmosphere gas is made up of 1-5% reducibility gas and 95-99% inert gas.
5. the preparation method of a kind of superfine iron powder according to claim 4, is characterized in that, reducibility gas is at least one in hydrogen, carbon monoxide, methane; Described inert gas is at least one in nitrogen, carbon dioxide, argon gas.
6. the preparation method of a kind of superfine iron powder according to claim 1, is characterized in that, the flow velocity of the gas of described weakly reducing atmosphere is 5-10m/s.
7. the preparation method of a kind of superfine iron powder according to claim 1, is characterized in that, in described stove, the rate of heat addition is 5-10 DEG C/h.
8. the preparation method of a kind of superfine iron powder according to claim 1, is characterized in that, in described stove, mode of heating is, by electrical heating, heating using microwave or infrared heating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410606384.1A CN104308170B (en) | 2014-10-31 | 2014-10-31 | Superfine iron powder preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410606384.1A CN104308170B (en) | 2014-10-31 | 2014-10-31 | Superfine iron powder preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104308170A true CN104308170A (en) | 2015-01-28 |
| CN104308170B CN104308170B (en) | 2017-01-11 |
Family
ID=52363557
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410606384.1A Expired - Fee Related CN104308170B (en) | 2014-10-31 | 2014-10-31 | Superfine iron powder preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104308170B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104972134A (en) * | 2015-08-05 | 2015-10-14 | 河南聚鑫超硬材料有限公司 | Method for producing superfine iron powder |
| CN107523662A (en) * | 2017-08-16 | 2017-12-29 | 河钢股份有限公司承德分公司 | A kind of method that metallic iron in rich iron tailings is reclaimed in fluidization |
| CN108907230A (en) * | 2018-07-24 | 2018-11-30 | 安徽工业大学 | A kind of preparation method of threadiness iron powder |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3530385A1 (en) * | 2018-02-26 | 2019-08-28 | Linde Aktiengesellschaft | Method for the production of metallic powders |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850397A (en) * | 2006-03-22 | 2006-10-25 | 成都汉基投资有限公司 | Method for preparing inorganic nano composite powder |
| CN101397606A (en) * | 2007-09-24 | 2009-04-01 | 宝山钢铁股份有限公司 | Fine iron pre-reduction technology suitable for wide grain size distribution and apparatus thereof |
-
2014
- 2014-10-31 CN CN201410606384.1A patent/CN104308170B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1850397A (en) * | 2006-03-22 | 2006-10-25 | 成都汉基投资有限公司 | Method for preparing inorganic nano composite powder |
| CN101397606A (en) * | 2007-09-24 | 2009-04-01 | 宝山钢铁股份有限公司 | Fine iron pre-reduction technology suitable for wide grain size distribution and apparatus thereof |
Non-Patent Citations (1)
| Title |
|---|
| 宋乙峰等: "搅拌流化床中超细氧化铁粉流态化及还原实验研究", 《过程工程学报》, vol. 11, no. 3, 30 June 2011 (2011-06-30), pages 361 - 367 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104972134A (en) * | 2015-08-05 | 2015-10-14 | 河南聚鑫超硬材料有限公司 | Method for producing superfine iron powder |
| CN104972134B (en) * | 2015-08-05 | 2017-02-01 | 河南聚鑫超硬材料有限公司 | Method for producing superfine iron powder |
| CN107523662A (en) * | 2017-08-16 | 2017-12-29 | 河钢股份有限公司承德分公司 | A kind of method that metallic iron in rich iron tailings is reclaimed in fluidization |
| CN108907230A (en) * | 2018-07-24 | 2018-11-30 | 安徽工业大学 | A kind of preparation method of threadiness iron powder |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104308170B (en) | 2017-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104308170B (en) | Superfine iron powder preparation method | |
| CN104801721B (en) | A kind of device and method for preparing nano metal powder | |
| CN102120570B (en) | Device and process method for continuously producing carbon nanotubes | |
| CN102849799B (en) | Device and method for synthesizing fullerene structure nanometer WS2 and application of fullerene structure nanometer WS2 | |
| Chen et al. | The texture evolution of g-C3N4 nanosheets supported Fe catalyst during Fischer-Tropsch synthesis | |
| CN108064214A (en) | For from the method for production of hydrocarbons hydrogen and graphitic carbon | |
| CN100488673C (en) | Method of manufacturing micro and sub-micron iron powder | |
| CN103056381B (en) | A kind of preparation method of nanometer tungsten carbide/Co composite powder | |
| CN103056377B (en) | Method for manufacturing nanometer tungsten/cobalt carbide composite powder | |
| CN103920886A (en) | Method for producing ultra-fine iron powder | |
| CN102794456B (en) | Fluidized bed reactor for preparing ultrafine iron powder | |
| Ying et al. | Preparation of ultrafine nickel powder by polyol method and its oxidation product | |
| CN103922403B (en) | The method of powdery Vanadium Pentoxide in FLAKES is produced in a kind of ammonium poly-vanadate fluidization | |
| CN101176920A (en) | Method for preparing active metal titanium and boron carbide complex spherical hot spraying powder | |
| CN102186583A (en) | Supported catalyst for synthesizing carbon nanotubes, method for preparing thereof and carbon nanotube using the same | |
| CN102078965A (en) | Method for preparing WC-Co (tungsten carbide-cobalt) nano-powder | |
| CN110227826A (en) | A method of preparing high-purity nm molybdenum powder | |
| CN104070173B (en) | The preparation method of globular tungsten powder | |
| CN102528068A (en) | Device and method for preparing superfine nickel powder | |
| CN103420359B (en) | The method of carbon nanotube, reaction unit and application are prepared in red mud catalysis | |
| CN108348901A (en) | A method of control graphite form | |
| CN101821001B (en) | Method for the preparation of hydrocarbon synthesis catalyst and the use thereof in hydrocarbon synthesis process | |
| Sun et al. | Core-shell-like Fe2O3/MgO oxygen carriers matched with fluidized bed reactor for chemical looping reforming | |
| CN103273072A (en) | Process and device for preparing superfine nickel powder | |
| CN103101978B (en) | Preparation method of nano WS2 with fullerene structure, fluidized bed reactor, fluidifying method and applications |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170111 Termination date: 20171031 |