CN108148938A - More gradient vacuum method direct-reduction iron scales prepare high-purity iron powder method off field outside a kind of microwave - Google Patents
More gradient vacuum method direct-reduction iron scales prepare high-purity iron powder method off field outside a kind of microwave Download PDFInfo
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- CN108148938A CN108148938A CN201711210624.6A CN201711210624A CN108148938A CN 108148938 A CN108148938 A CN 108148938A CN 201711210624 A CN201711210624 A CN 201711210624A CN 108148938 A CN108148938 A CN 108148938A
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- microwave
- reduction
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- iron powder
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B13/00—Making spongy iron or liquid steel, by direct processes
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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
Abstract
The present invention relates to a kind of microwave, more gradient vacuum methods direct-reduction iron scales prepare high-purity iron powder method off field outside, can carry out quick carbon thermal reduction to iron scale using microwave under vacuum using this method, produce high-purity iron powder.And the impurity component while raw materials for production of this method are metallurgical waste and regenerative resource in raw material is relatively fewer so that while product is purer after reaction, avoids the harm that convenient source and fossil energy bring environment.The technological process of the present invention is shorter simultaneously, and operation is relatively simple, is easy to actual production use.
Description
Technical field
The present invention relates to field of metallurgy, more particularly to one kind utilizes more gradient vacuum method direct reduced iron off field outside microwave
Squama prepares high-purity iron powder method.
Background technology
At present, in non-blast furnace ironmaking technology both domestic and external, either direct-reduction process or smelting reduction process still rely on
Fossil energy, energy resource structure do not occur to sexually revise at all, are equally also faced with increasingly harsh environmental requirement, this forces people
Seek new fuel pathways.And novel reproducible biomass fuel, have the characteristics that it is widely distributed, using convenient and pollute small
Start to be valued by people, to break away from dependence of traditional steel and iron industry to fossil energy, reduce CO2 emission, realize green
Color, clean manufacturing provide possibility.At present, biomass fuel is constantly being opened in metallurgical processes such as sintering, pelletizing, ironmaking
Hair, application and exploration.
During conventional metallurgical has been broken in microwave heating, the pattern that the energy is provided by combustion of fossil fuels is reacted, there is section
Can be efficient, easily controllable, pollution is low the features such as, there is huge application potential in metallurgical industry.And microwave heating is used
During the carbon thermal reduction of metal, carbon can generate local high temperature, can promote the progress of cloth Dorr reaction and the concentration of raising CO.
In carbothermic reduction process, total reaction rate is controlled by the gasification reaction of carbon, is reacted even with as charcoal
The very strong reducing agent of property is also such.Therefore, when replacing traditional heating with microwave heating, the carbon thermal reduction speed of metal oxide
Rate can significantly improve.
Steel scale of steel rolling (iron scale) is in steel material forging and hot rolling hot-working, due to the steel and air of high temperature
The reaction of middle oxygen, the product necessarily led to.Although each iron and steel enterprise does in terms of the generation for reducing steel scale of steel rolling, raising lumber recovery
A large amount of work, but the iron scale for still having about 1.3% or so generates.At present, the oxygen that the iron and steel enterprise in China generates every year
Change about 10,000,000 t of iron sheet.Its main Land use systems is used as sintered material and steel-making cooling agent or slagging agent, but is used
In production high value added product --- if reduced iron powder and ferromagnetic amount remain unchanged very little, embody instantly industrial level for iron
The limitation that squama utilizes, thus develop it is practicable using iron scale production high value-added product and technique seem more urgent
It cuts.
Invention content
The technical problems to be solved by the invention are to provide outside a kind of microwave more gradient vacuum method direct-reduction iron scales off field
High-purity iron powder method is prepared, promotes the progress of carbothermic reduction reaction, reduces the impurity content that the substances such as conventional coal dust are substituted into,
So that products therefrom is purer after reaction.
To achieve the above object, the present invention is realized using following technical scheme：
More gradient vacuum methods direct-reduction iron scales prepare high-purity iron powder method off field outside a kind of microwave, in the high-purity iron powder
More than 97% all iron content, more than 98% degree of metalization, technological process are：Raw material crushes-batch mixing-briquetting-difference gradient vacuum
Lower microwave carbon thermal reduction-magnetic separation separation；Specifically include following steps：
Step 1：Raw material crushes
Iron scale, reducing agent are crushed respectively, are ground to below 0.1mm；
Step 2：Batch mixing and briquetting
Iron scale, reducing agent are carried out with carbon batch mixing, the fixation carbon content in iron scale in the oxygen content and reducing agent of iron oxide
Than being 1：1.4~1.6, treat that reaction material carries out being pressed into 4~6cm of diameter, the material block of 2~3cm of height, compacting by what is mixed
Power is set as 20MPa；
Step 3：The carbon thermal reduction of microwave outfield
It will treat the hair of the carbothermic reduction reaction, wherein microwave of progress microwave outside off field in reaction material block feeding microwave reactor
Raw power is 1500~2000W, and the reaction time is 25 ± 2min, to carrying out three-stage vacuum processing in stove in reaction process, the
One section starts preceding 2~3min for reaction, and vacuum degree is 20~25KPa in vacuum processing stove；Second segment be after 3~5min,
Stop carrying out vacuum processing in stove, only carry out single microwave reduction；Third section is until reaction terminates, at continuation vacuum later
It manages, vacuum degree is 20~22KPa in stove, is treated after completion of the reaction, and product after reduction is carried out inert gas cooling；
Step 4：Magnetic separation detaches
Product after cooling obtains high-purity iron powder after carrying out second-time breakage grinding 0.1mm hereinafter, carrying out magnetic separation screening.
The reducing agent is activated carbon or bamboo charcoal.
Compared with prior art, the beneficial effects of the invention are as follows：
(1) operating method and technological process of the invention are relatively easy, and highly practical, required material and equipment are relatively
It is few.In production process using a batch mixing briquetting and by the way of once restoring, avoid relatively cumbersome and complicated in traditional approach
Cloth condition and reduction mode.
(2) present invention with it is raw materials used be iron scale, activated carbon etc., the impurity component in raw material is relatively fewer, and then
So that the purity for promoting product after reduction is guaranteed.And the reducing agent in carbon thermal reduction employs the side of activated carbon or bamboo charcoal
Formula is compared compared to common fossil energy, belongs to regenerative resource, contributes to the protection of environment.
(3) it is used as the heating source of carbothermic reduction reaction by microwave, can not only saves the drying ring for initial material
Section, cost-effective and processing step, while microwave heating are also possible that the contact of storeroom in reaction process and react more
Fully and uniformly, during and being reacted using microwave, since microwave can promote to divide in the structure of reactant itself
Connecting key fracture between son or cluster so that the carbothermic reduction reaction process of iron scale can be more quick and be smoothly carried out.Phase
Compared with modes, the reaction rate of microwave reduction process and the microwave utilization rate such as conventional electrical heating and fossil energy heating
Higher.
(4) during microwave reduction, initial reaction stage is heating drying stage, passes through microwave treatment and the side vacuumized
Formula makes reaction material constantly heat up under microwave action, and temperature of charge can rise to 300-350 DEG C from room temperature, while in material
Oxygen in moisture and stove etc. obtains fast eliminating.Second stage is the medium temperature indirect reduction stage, due to stopped lasting pumping
Vacuum is taken, the own temperature of material rises to 850-900 DEG C so that occur between the fixed carbon and iron scale in reducing agent in the process
Indirect reduction is reacted, and biomass carbon (activated carbon or bamboo charcoal) volatilization, cracking generate higher concentration CO and H2, make the Fe in iron scale2O3
Indirect reduction forms Fe step by step3O4Or Fu Shi iron (FexThe objects phase such as O), and gaseous reducing agent is wrapped in around reaction particles and is formed
One layer of local reduction boundary layer promotes indirect reduction reaction and furnace charge heating.Phase III is high-temperature direct reduction and heat preservation rank
Section starts to carrying out vacuum processing again in stove, and temperature of charge is controlled at 900 DEG C to 1250 DEG C, and the carbon in biomass is then opened
Beginning and Fe3O4Or Fu Shi iron (FexO direct reduction reactor) occurs and forms metallic iron (reaction equation Fe3O4+ 4C=Fe3O4+ 4CO,
FexO+xC=xFe+CO), the effect of vacuum causes gas phase CO, CO2Wait gases quickly escape, break it is original under the conditions of reaction put down
Weighing apparatus, so as to which the depth of direct reduction reactor be promoted to carry out.Make that the oxide of iron restores more fully, and due to impurity in material
Less and any reaction does not occur substantially, the slag phase that impurity primarily becomes a small amount of is attached on the sponge iron restored.Straight
During connecing reduction reaction, with infrared temperature measurement apparatus measure its material reaction temperature can reach 1350 DEG C it is even higher.
(5) products therefrom is loose after reacting, the porosity is high, easily broken, need to only pass through simple magnetic separation separation process just
It may be such that metallic iron and slag phase obtain good separation.The metallic iron purity magneticly elected after separation is than sponge that usual manner obtains
Metal Ferrum content taller more than 2% in iron.
(6) the method for the present invention technological process is short, can once restore the metallic iron of high-purity, good slag is reached after magnetic separation
Gold separation.Iron scale is restored using the method, for all iron content in product up to more than 97%, degree of metalization can reach 98%, and
And other impurities content is relatively low.
Description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Specific embodiment
The specific embodiment of the present invention is further illustrated below in conjunction with the accompanying drawings：
For implementer's method of the conciser statement present invention, Fig. 1 provides outside the microwave of the present invention more gradients off field
Vacuum method direct-reduction iron scale prepares the process flow diagram of high-purity iron powder.
Embodiment 1
More gradient vacuum method direct-reduction iron scales prepare high-purity iron powder method off field outside a kind of microwave, and technological process is：It is former
Expect microwave carbon thermal reduction under broken-batch mixing-briquetting-difference gradient vacuum-magnetic separation separation；Specifically include following steps：
Step 1：It will treat that reactant iron scale carries out crushing grinding to below 0.1mm with reducing agent (activated carbon)；Iron scale is main
Chemical composition is as shown in table 1 below；
Table 1：Main chemical compositions/% of iron scale
| Ingredient | TFe | FeO | Fe2O3 |
| Content | 72.88 | 60.95 | 36.5 |
Step 2：By reducing agent (activated carbon) and iron scale by the fixation carbon content in activated carbon and the oxygen of iron oxide in iron scale
Content is than 1.4~1.6：1 carries out with carbon batch mixing.The material mixed is pressed into diameter 4cm, the material block of height 2cm, press power
For 20MPa；
Step 3：It will treat that reaction material block is sent into wave reactor the carbothermic reduction reaction carried out outside microwave off field, wherein micro-
The generation power of wave is 1500~2000W, reaction time 25min.It is and true to carrying out three-stage in stove during the reaction
Vacancy reason is restored, and first segment starts preceding 2~3min for reaction, the stage to carrying out online vacuum processing in stove, in stove
Vacuum degree reaches 20~25KPa；Second segment be after 3~5min, the conversion zone stop carry out vacuum processing, only into
The single microwave reduction of row；Third section terminates until reacting later, at this stage, continues to start vacuum processing, guarantee was reacted
Vacuum degree is 20~22KPa in its stove in journey.It treats after completion of the reaction, product after reduction is subjected to inert gas cooling, prevents height
The metallic iron restored under temperature is again be oxidized.
Step 4：By after cooling product carry out again crushing grinding to 0.1mm hereinafter, magnetic separation sieves to obtain high-purity iron powder.
The iron powder obtained in embodiment is detected to obtain all iron content in its product up to 97.84%, degree of metalization
98.21%, S content 0.01%, C content 2.47%.
Embodiment 2
More gradient vacuum method direct-reduction iron scales prepare high-purity iron powder method off field outside a kind of microwave, and technological process is：It is former
Expect microwave carbon thermal reduction under broken-batch mixing-briquetting-difference gradient vacuum-magnetic separation separation；Specifically include following steps：
Step 1：It will treat that reactant iron scale carries out crushing grinding to below 0.1mm with reducing agent (bamboo charcoal)；Iron scale is mainly changed
It studies point as shown in table 1 below；
Table 1：Main chemical compositions/% of iron scale
| Ingredient | TFe | FeO | Fe2O3 |
| Content | 73.20 | 61.55 | 35.9 |
Step 2：By reducing agent bamboo charcoal and iron scale by the fixation carbon content in activated carbon and the oxygen content of iron oxide in iron scale
Than 1.4~1.6：1 carries out with carbon batch mixing.The material mixed is pressed into diameter 4cm, the material block of height 2cm, press power is
20MPa；
Step 3：It will treat that reaction material block is sent into wave reactor the carbothermic reduction reaction carried out outside microwave off field, wherein micro-
The generation power of wave is 1500~2000W, reaction time 25min.It is and true to carrying out three-stage in stove during the reaction
Vacancy reason is restored, and first segment starts preceding 2~3min for reaction, the stage to carrying out online vacuum processing in stove, in stove
Vacuum degree reaches 20~25KPa；Second segment be after 3~5min, the conversion zone stop carry out vacuum processing, only into
The single microwave reduction of row；Third section terminates until reacting later, at this stage, continues to start vacuum processing, guarantee was reacted
Vacuum degree is 20~22KPa in its stove in journey.It treats after completion of the reaction, product after reduction is subjected to inert gas cooling, prevents height
The metallic iron restored under temperature is again be oxidized.
Step 4：By after cooling product carry out again crushing grinding to 0.1mm hereinafter, magnetic separation sieves to obtain high-purity iron powder.
The iron powder obtained in embodiment is detected to obtain all iron content in its product up to 97.68%, degree of metalization
98.15%, S content 0.009%, C content 2.42%.
Described above is only the basic principle of the present invention, and not the present invention is imposed any restrictions, every right according to the present invention
It carries out equivalent variations and modification, within the scope of the art of this patent protection scheme.
Claims (2)
1. more gradient vacuum method direct-reduction iron scales prepare high-purity iron powder method off field outside a kind of microwave, which is characterized in that described
More than 97% all iron content in high-purity iron powder, more than 98% degree of metalization, technological process are：Raw material crushes-batch mixing-briquetting-no
With microwave carbon thermal reduction under gradient vacuum-magnetic separation separation；Specifically include following steps：
Step 1：Raw material crushes
Iron scale, reducing agent are crushed respectively, are ground to below 0.1mm；
Step 2：Batch mixing and briquetting
Iron scale, reducing agent are carried out with carbon batch mixing, the fixation carbon content ratio in iron scale in the oxygen content and reducing agent of iron oxide is
1：1.4~1.6, treat that reaction material carries out being pressed into 4~6cm of diameter, the material block of 2~3cm of height by what is mixed, press power is set
It is set to 20MPa；
Step 3：The carbon thermal reduction of microwave outfield
It will treat the generation work(of the carbothermic reduction reaction, wherein microwave of progress microwave outside off field in reaction material block feeding microwave reactor
Rate is 1500~2000W, and the reaction time is 25 ± 2min, to carrying out three-stage vacuum processing, first segment in stove in reaction process
Start preceding 2~3min for reaction, vacuum degree is 20~25KPa in vacuum processing stove；Second segment be after 3~5min, in stove
Stop carrying out vacuum processing, only carry out single microwave reduction；Third section terminates until reacting later, continues vacuum processing, stove
Interior vacuum degree is 20~22KPa, is treated after completion of the reaction, and product after reduction is carried out inert gas cooling；
Step 4：Magnetic separation detaches
Product after cooling obtains high-purity iron powder after carrying out second-time breakage grinding 0.1mm hereinafter, carrying out magnetic separation screening.
2. more gradient vacuum method direct-reduction iron scales prepare high-purity iron powder side off field outside a kind of microwave according to claim 1
Method, which is characterized in that the reducing agent is activated carbon or bamboo charcoal.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110804A (en) * | 2018-11-09 | 2019-01-01 | 攀枝花学院 | Sub- titanium oxide of high-purity Magn é li phase and preparation method thereof |
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| US5958156A (en) * | 1996-03-15 | 1999-09-28 | Kemp Development Corporation | Process for treating a particulate material within a rotating retort |
| CN1539024A (en) * | 2001-05-31 | 2004-10-20 | 黄小第 | Method for direct metal making by microwave energy |
| CN102839250A (en) * | 2012-09-28 | 2012-12-26 | 昆明理工大学 | Method for collecting high-quality coal gas in process of producing reduced iron powder by means of microwave heating |
| CN104498734A (en) * | 2015-01-09 | 2015-04-08 | 重庆大学 | Titanium recovery treatment method for titanium-bearing blast furnace slag based on vacuum carbothermal reduction |
| CN107745132A (en) * | 2017-10-20 | 2018-03-02 | 酒泉钢铁(集团)有限责任公司 | A kind of method that iron oxide red prepares high-purity iron powder |
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2017
- 2017-11-28 CN CN201711210624.6A patent/CN108148938B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5958156A (en) * | 1996-03-15 | 1999-09-28 | Kemp Development Corporation | Process for treating a particulate material within a rotating retort |
| CN1539024A (en) * | 2001-05-31 | 2004-10-20 | 黄小第 | Method for direct metal making by microwave energy |
| CN102839250A (en) * | 2012-09-28 | 2012-12-26 | 昆明理工大学 | Method for collecting high-quality coal gas in process of producing reduced iron powder by means of microwave heating |
| CN104498734A (en) * | 2015-01-09 | 2015-04-08 | 重庆大学 | Titanium recovery treatment method for titanium-bearing blast furnace slag based on vacuum carbothermal reduction |
| CN107745132A (en) * | 2017-10-20 | 2018-03-02 | 酒泉钢铁(集团)有限责任公司 | A kind of method that iron oxide red prepares high-purity iron powder |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110804A (en) * | 2018-11-09 | 2019-01-01 | 攀枝花学院 | Sub- titanium oxide of high-purity Magn é li phase and preparation method thereof |
| CN109110804B (en) * | 2018-11-09 | 2021-01-12 | 攀枝花学院 | High-purity magneli phase titanium suboxide and preparation method thereof |
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| CN108148938B (en) | 2019-07-26 |
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