CN113736945B - Vacuum iron smelting method without reducing agent - Google Patents
Vacuum iron smelting method without reducing agent Download PDFInfo
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Abstract
The invention discloses a method for smelting iron in vacuum without reducing agent. By a method of between 10 and 10 ‑9 Under Pa vacuum condition, adopting power density of 10-10 4 W/cm 2 Irradiating an iron-containing oxide (ore) sample at an angle of 0.5-90 deg., decomposing gaseous substances producing elemental iron and oxygen; placing a circulating cooling collector at a position 1-500 cm away from the upper part of the sample, and depositing and collecting a product containing metal iron; and finally, separating by mineral separation to obtain metal iron powder, thereby realizing the purpose of zero-carbon clean iron smelting without reducing agent. The reducing agent-free vacuum iron smelting method provided by the invention is simple, easy to operate, zero in carbon and emission, green and environment-friendly, has the potential of large-scale continuous production, and is expected to be applied to the technical field of intelligent clean and efficient iron production in the future and on-site metallurgy of iron-containing mineral resources outside the ground.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a vacuum metallurgy method of iron-containing oxidized ore without reducing agent by taking photons as energy sources. The method can be used for future intelligent clean iron making and moon iron-bearing mineral in-situ metallurgy.
Background
Carbon reduction iron smelting is the most mature iron making technology developed by human beings so far and is the main stream technology of the world industry iron making at present. The carbon reduction ironmaking needs to consume a large amount of carbon energy sources such as coal, coke, natural gas and the like, and is a carbon dioxide discharging household. Compared with the traditional carbon reduction iron making, the hydrogen reduction and electrochemical reduction technology is in principle free from consuming carbon energy; however, the above-mentioned technology is a low-carbon or zero-carbon clean iron-making technology in a true sense only on the premise of "green hydrogen" and "green electricity" which do not consume carbon energy. More importantly, the chemical nature of the method is that the separation of iron and oxygen in iron oxide ores is realized through electron loss and transfer, so that a reducing agent or electric energy is consumed; and more directly, the high-energy light beam acts on the iron oxide ore, and the chemical bond between iron and oxygen is broken by the energy of photons, so that the separation of metal and oxygen can be realized.
Laser is a high-energy beam heat source widely used in the current intelligent metallurgical industry production, and comprises laser cutting, laser drilling, laser cladding, laser welding, laser hardening and the like. The energy sources of the laser include electric energy and solar energy, which are all clean and sustainable energy sources in the future. In 2006, yabe et al conducted a study of laser pyrolysis of MgO under vacuum and an inert atmosphere, and a small amount of elemental Mg was detected in the pyrolysis product [ Yabe, T., et al, applied Physics Letters,2006.89 (26): p.261107 ]. In 2011, liao et al developed laser pyrolysis of SiO in a vacuum environment 2 A small amount of elemental Si was detected in the pyrolysis product [ Liao, s.h., et al, journal of Applied Physics,2011.109 (1): p.0133103 ]. In 2019, tanaka et Al developed laser pyrolysis of Al under vacuum 2 O 3 But no Al simple substance was collected [ Tanaka, s., et Al, vacuum,2019.167:p.495-499 ]. In the early stage, the adoption of pulse laser to irradiate iron-containing oxidized ores such as olivine, pyroxene and anorthite has been reported in literature, and trace amounts of nano-grade elementary Fe particles are prepared in a micro area of a sample [ Sasaki, S., et al, nature,2001.410 (6828): p.555-7; sasaki, s., et al, advances in Space Research,2002.29 (5): p.783-788; sasaki, S., et al, advances in Space Research,2003.31 (12): p.2537-42 ]. However, no published report on the preparation of micron-sized Fe particles by directly decomposing iron-containing minerals by laser or solar energy focused light is currently seen.
Furthermore, with the continuous progress of lunar exploration technology, future lunar mineral resource utilization has become one of the key targets for deep space exploration of humans. Due to extreme environmental characteristics such as microgravity on the lunar surface, strong solar radiation, ultra-high vacuum, large day and night temperature difference and the like, the existing mature metallurgical technology of the earth is developed based on the characteristics of earth resources and environment, and is difficult to be directly applied to lunar mineral smelting. Currently, both NASA and ESA publications in the united states report the electrochemical extraction of metals and oxygen from lunar soil. Dan Zhongning et al, university of northeast in China, also disclose a method for extracting metals and oxygen from lunar soil and rocks by molten salt electrolysis [ CN201911172554.9 ]. However, the electrochemical methods all require additional chemical reagent and electrode consumption, and the design and the improvement of the electrolysis efficiency of the large-scale electrolysis device in the microgravity and ultra-vacuum environment severely limit the application prospect of the technology on the moon. The iron-containing oxidized ore on the lunar surface is directly decomposed by laser or solar laser, so that metal iron and oxygen can be prepared and obtained for future lunar base construction and human life activities; and moreover, the metallurgy can be effectively extracted from lunar soil minerals without chemical reagents, so that the ground and moon transport cost is greatly reduced, and the method has a huge application prospect in future lunar mineral in-situ utilization.
Accordingly, those skilled in the art have focused on developing a reductant-free vacuum metallurgical process with a laser or solar focused beam as the energy input.
Disclosure of Invention
Aiming at the inherent defects existing in the prior art of iron making and the application background of future intelligent clean iron making and in-situ utilization of moon surface iron-containing minerals, the invention provides a vacuum iron smelting method using laser or solar energy focused light beams as energy input, which is used for preparing large-particle-size (more than micron-sized) metallic iron and oxygen from iron-containing oxides (ores) under the condition of no reducing agent. And under the vacuum condition, the high-power laser or solar energy focusing light beam is adopted to irradiate the massive sample, so that iron oxide in the massive sample is decomposed into elemental iron and oxygen, a product containing metal iron is obtained through deposition of a cooling device, and the oxygen is collected after being pumped out by a vacuum pump set, thereby realizing the purpose of reducing-agent-free vacuum iron smelting.
In order to achieve the above purpose, the invention provides a method for vacuum smelting iron without reducing agent, which comprises the following steps:
(1) Placing a movable object stage in the vacuum cavity, placing an iron-containing mineral sample in a high-temperature-resistant crucible, and respectively fixing the high-temperature-resistant crucible filled with the sample and a product collector on the object stage;
(2) Setting the incident angle and the output power of a high-power laser or solar energy focusing beam; controlling the power density of the light beam in the action area by adjusting the focal length of the light beam and the defocusing amount of the sample; adjusting the angle of the objective table to irradiate the light beam to the surface of the sample; adjusting the relative positions of the product collector and the sample;
(3) Closing the vacuum cavity, starting a vacuum pump source, enabling the vacuum degree in the cavity to reach a preset value, and connecting a gas collecting bag to a tail gas pipeline of the vacuum pump source;
(4) Starting a collector cooling system, and starting a light beam to irradiate a sample; after the reaction of the sample is finished, the beam control system is closed, the collector cooling system is closed, and the gas collection bag is taken out; closing a vacuum pump source, breaking vacuum by adopting inert gas, taking out a product collector, and collecting a deposition product;
and (3) fully grinding the sediment product collected in the step (4), and then carrying out mineral separation to obtain pure iron powder.
Further, the movable stage of step (1) is a multi-axis linear motion platform or a gimbaled robot platform.
Further, the iron-containing mineral sample of step (1) refers to a powder or lump ore of an iron oxide-containing mineral selected from one or more of the following groups: hematite, magnetite, siderite, limonite, goethite, specularite, ilmenite, fayalite, chromite, red mud, siderite and lunar soil minerals.
Further, the high temperature resistant crucible of step (1) is a high melting point metal or ceramic material, or a copper crucible with a built-in circulating cooling medium.
Further, the product collector of step (1) refers to a copper collector with a circulating cooling medium therein, the cooling medium comprising water, argon or liquid nitrogen, and the physical shape of the copper collector comprises a square, cylindrical, conical, helical blade, other shaped or a combination thereof.
Further, the wavelength range of the high-power laser or solar energy focused beam in the step (2) is from visible light to infrared light, the incident angle refers to the acute angle formed by the beam line and the surface of the sample, the angle is 0.5-90 degrees, the beam power density refers to the ratio of the beam output power to the area of the action area, and the ratio is 10-10 4 W/cm 2 。
Further, the relative position of the product collector and the sample in the step (2) refers to the distance from the center of the sample in the laser action area to the surface of the collector, and the distance is 1-500 cm.
Further, the vacuum degree in the cavity in the step (3) reaches a preset value of 10 to 10 -9 Pa。
Further, the sample is irradiated by the opening light beam in the step (4), the sample is preheated by lower power irradiation until the sample is melted, and then the sample is irradiated by higher power laser until the sample is completely decomposed; inert gas refers to any gas that does not react with metallic iron, including nitrogen and argon.
Further, the beneficiation separation in the step (5) refers to the process of carrying out magnetic separation, flotation and reselection on metal iron particles in the sediment product and other material particles.
Compared with the prior art, the invention has the following obvious prominent substantive features and obvious advantages:
1. the traditional iron production method using iron-containing oxidized ore as raw material is to add additional reducing agent and other chemical reagents, especially the carbon dioxide emission in the current industrial carbon reduction iron production process is nearly 2 times as high as the iron yield; the invention provides a method for preparing iron by adopting clean and high-efficiency high-energy light beams as energy sources and under the high vacuum condition, which realizes the zero-carbon pollution-free high-efficiency iron preparation.
2. The existing electrochemical reduction low-carbon iron production technology needs to be electrified in a high-temperature molten oxide or molten salt system for reduction, has the technical defects of low current efficiency, easy corrosion of electrode materials and the like, and is difficult to industrially apply; the invention directly acts on the mineral sample by high-energy light beams, and can obtain the metallic iron through vacuum decomposition reaction, thereby being easy to realize intelligent industrial production.
3. The existing technical scheme of in-situ metallurgy of the iron-containing minerals outside the earth, especially the moon is improved on the basis of the existing earth metallurgy technology, the ultra-high vacuum environment of the moon is fully utilized, high-energy light beams are directly adopted to heat the minerals on the surface of the moon to prepare metal iron and oxygen, no chemical reagent is needed, the high cost of ground and moon transportation is greatly reduced, and the technical support is hopefully provided for the construction of the moon base and the human life activities.
4. The existing metallic iron prepared by the action of pulse laser on iron-containing minerals is only visible in a tiny area of the action of the laser, is trace nano-scale particles, and does not have the capability of industrial production at all; the high-power continuous wave laser and the solar energy focusing beam adopted by the invention can obtain a large amount of metal iron particles with the size of more than microns, and the high-power continuous wave laser and the solar energy focusing beam have the capability of high-efficiency continuous production.
5. The laser power density in the existing laser heat source metal oxide deoxidation method should be more than 10 5 W/cm 2 In contrast, the invention reduces the power density of the light beam to 10-10 by improving the included angle between the light beam line and the surface of the sample and adopting the low-power preheating process 4 W/cm 2 The beam energy utilization efficiency is greatly improved, the power index of the beam equipment is reduced, and the beam can be expanded to a solar energy focusing beam.
The conception, specific structure, and technical effects of the present invention will be further described with reference to the accompanying drawings to fully understand the objects, features, and effects of the present invention.
Drawings
FIG. 1 is a graph of XRD data analysis and fitting quantitative calculations of deposition products collected in a preferred embodiment of the invention;
FIG. 2 is a scanning electron microscope image of the received deposition output in a preferred embodiment of the invention;
FIG. 3 is a scanning electron microscope image of the collected product in a preferred embodiment of the invention;
FIG. 4 is a scanning electron microscope image and spectral surface scan element distribution diagram of the collected product in a preferred embodiment of the invention.
Fig. 5 is a scanning electron microscope image of the collected product of fig. 4.
Detailed Description
The following description of the preferred embodiments of the present invention refers to the accompanying drawings, which make the technical contents thereof more clear and easy to understand. The present invention may be embodied in many different forms of embodiments and the scope of the present invention is not limited to only the embodiments described herein.
Example 1
Step 1: using iron-bearing mineral sample as ferric oxide powder (analytically pure, 99.0%), 1g of the powder sample was placed in a water-cooled copper crucible with a hemispherical cavity of 8mm diameter, and the crucible was mounted on a stage within the vacuum chamber.
Step 2: a cylindrical red copper collector with a central through hole (with the diameter of 5 mm) and built-in through type circulating water cooling is placed at the position 50mm above the sample, and the diameter of the collector is 80mm and the thickness of the collector is 40mm.
Step 3: the height of the objective table is adjusted to enable the surface of the sample to be located at a positive defocusing position, the defocusing amount is 50cm, and the size of a light spot of a laser action area is close to the size of the sample.
Step 4: setting two-section laser irradiation parameters: the first section laser output power is 300W, the action time is 60s, the second section laser output power is 3000W, and the action time is 20s.
Step 5: closing the vacuum cavity, starting the vacuum pump source to make the vacuum degree in the cavity reach 10 -3 Pa, and then connecting a gas collecting bag into a tail gas pipeline of the vacuum pump source.
Step 6: opening a collector cooling system, starting laser, closing a beam control system after the reaction is finished, closing the collector cooling system, taking out a gas collection bag, closing a vacuum pump source, breaking vacuum by adopting high-purity Ar gas, taking out a product collector, and collecting a deposition product.
Step 7: and directly using a small part of the collected sediment product for component analysis, grinding the rest part to a particle size of less than 2um, and then carrying out magnetic separation to obtain pure iron powder.
Fig. 1 is a graph of XRD data analysis and fitting quantitative calculations of the deposition output in this example. As can be seen from the figure, the product has obvious diffraction peaks of elemental iron, and part of ferrous oxide. The mass percentage of the simple substance iron phase in the sediment product is 27.1 percent through phase quantitative calculation.
Fig. 2 is a scanning electron microscope image of the deposition product received in this example, wherein the white irregular particles are elemental iron, and the size of the particles can reach the order of tens of micrometers. The mole fractions of iron and oxygen in the elemental iron particles were 98.5% and 1.5%, respectively.
The purity of the oxygen in the gas collection bag in this example was 99.5%; the purity of iron in the powder sample obtained after magnetic separation was 90%.
Example 2
This embodiment is substantially the same as embodiment 1, except that:
(1) In the step 1, an iron-containing mineral sample is adopted as ilmenite concentrate powder, and the chemical components of the ilmenite concentrate powder contain FeTiO according to mass percent 3 74.9％，Fe 2 O 3 14.2％，SiO 2 7.9%, the balance being impurities.
(2) In the step 2, the distance between the lower surface of the collector and the surface of the sample is 30mm, and the included angle between the lower surface of the red copper collector and the central line of the laser beam is 45 degrees.
(3) Setting two-section laser irradiation parameters in the step 4: the first section laser output power is 500W, the action time is 20s, the second section laser output power is 2000W, and the action time is 10s.
(4) In step 5, the vacuum cavity is closed, and a vacuum pump source is started to enable the vacuum degree in the cavity to reach 10 -3 Pa, and then connecting a gas collecting bag into a tail gas pipeline of the vacuum pump source.
(5) The main phase in the deposition product collected in this example was Fe, feO, feTiO 3 、FeSiO 4 And SiO 2 Wherein the mass percentage of the simple substance iron is 30 percent.
(6) Fig. 3 is a scanning electron microscope image of the product collected in this example, wherein white irregular particles are elemental iron, and the particle size of the elemental iron in the product can reach tens of micrometers at maximum.
(7) The elemental mole percentages of elemental iron particles collected in the product in this example are: fe90.5%, O7.2%, si1.3%, ti1.0%.
(8) The purity of the oxygen in the gas collection bag in this example was 99.0%; the powder sample obtained after magnetic separation had an iron purity of 85%.
Example 3
This embodiment is substantially the same as embodiment 1, except that:
(1) In the step 1, the iron-containing mineral sample is adopted as the simulated lunar soil mineral mixed by the volcanic cinders and basalt in the mass ratio of 1:1, and the chemical components of the simulated lunar soil mineral contain SiO according to the mass percentage 2 45.5％，Al 2 O 3 17.3％，FeO13.2％，CaO8.3％，MgO5.6％，Na 2 O2.7％，TiO 2 2.6％，K 2 O1.9％，P 2 O 5 0.5 percent of MnO0.3 and the balance of impurities.
(2) The collector in step 2 was 35mm from the sample surface. The included angle between the lower surface of the red copper collector and the central line of the laser beam is 60 degrees.
(3) Setting two-section laser irradiation parameters in the step 4: the first section laser output power is 500W, the action time is 20s, the second section laser output power is 5000W, and the action time is 5s.
(4) In step 5, the vacuum cavity is closed, and a vacuum pump source is started to enable the vacuum degree in the cavity to reach 10 -4 Pa, and then connecting a gas collecting bag into a tail gas pipeline of the vacuum pump source.
(4) The main crystal phases in the deposition product collected in this example are Fe, siO 2 And (Mg, fe) SiO 4 There are also partially amorphous materials.
(5) Fig. 4 is a scanning electron microscope image and a spectrum surface scanning element distribution diagram of the product collected in this example, wherein white pellet particles are elemental iron, and the particle size of the white pellet particles is not only in micro-scale but also in nano-scale.
(6) The elemental mole percentages of elemental iron particles collected in the product in this example are: fe92.2%, O2.4%, si3.9%, ti1.5%.
(7) The purity of the oxygen in the gas collection bag in this example was 98.5%; in this embodiment, the raw material has a low iron content, the collected product has a low content of elemental iron, the nano-sized particles are more, the magnetic separation effect is poor, and the purity of iron in the obtained powder sample is 45%.
In the embodiment of the invention, the combination of the mechanical pump and the molecular pump is adopted, so that the maximum vacuum degree in the vacuum cavity can reach 10 -5 Pa。
The high-energy beam adopted in the embodiment of the invention is commercial high-power continuous wave laser, the central wavelength is 1080+/-5 um, the maximum output power is 6000W, the focal length is 400mm, and the spot diameter at the focal point is 200um.
The crucible in the embodiment of the invention is a water-cooled copper crucible, and the water cooling temperature is set to 25 ℃.
The product collector cooling medium in the examples of the present invention was water, and the water cooling temperature was set at 5 ℃.
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention without requiring creative effort by one of ordinary skill in the art. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by the person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (7)
1. A method for vacuum smelting iron without reducing agent, which is characterized by comprising the following steps:
placing a movable object stage in the vacuum cavity, placing an iron-containing mineral sample in a high-temperature-resistant crucible, and respectively fixing the high-temperature-resistant crucible filled with the sample and a product collector on the object stage;
setting the incident angle and the output power of a high-power laser or solar energy focusing beam; controlling the power density of the light beam in the action area by adjusting the focal length of the light beam and the defocusing amount of the sample; adjusting the angle of the objective table to irradiate the light beam to the surface of the sample; adjusting the relative positions of the product collector and the sample;
closing the vacuum cavity, starting a vacuum pump source, enabling the vacuum degree in the cavity to reach a preset value, and connecting a gas collecting bag to a tail gas pipeline of the vacuum pump source;
starting a collector cooling system, and starting a light beam to irradiate a sample; after the reaction of the sample is finished, the beam control system is closed, the collector cooling system is closed, and the gas collection bag is taken out; closing a vacuum pump source, breaking vacuum by adopting inert gas, taking out a product collector, and collecting a deposition product;
fully grinding the sediment product collected in the step (4), and then carrying out mineral separation to obtain pure iron powder;
the wavelength range of the high-power laser or solar energy focused beam in the step (2) is from visible light to infrared light, the incident angle refers to an acute angle formed by a beam line and the surface of a sample, the angle is more than 0.5 degree and less than 90 degrees, the beam power density refers to the ratio of the output power of the beam to the area of an action area, and the ratio is 10-10 4 W/cm 2 The method comprises the steps of carrying out a first treatment on the surface of the The relative position of the product collector and the sample in the step (2) means that the distance from the center of the sample in the laser action area to the surface of the collector is 1-500 cm; the sample is irradiated by the open light beam in the step (4), the sample is preheated by irradiation with lower power until the sample is melted, and then the sample is irradiated by laser with higher power until the sample is completely decomposed; inert gas refers to any gas that does not react with metallic iron, including nitrogen and argon.
2. The method of reducing agent-free vacuum metallurgical iron of claim 1, wherein the movable stage of step (1) is a multi-axis linear motion stage or a gimbaled robotic stage.
3. The reductant-free vacuum process for smelting iron according to claim 1, wherein the iron-containing mineral sample of step (1) is a powder or lump ore of an iron oxide-containing mineral selected from one or more of the group consisting of: hematite, magnetite, siderite, limonite, goethite, specularite, ilmenite, fayalite, chromite, red mud, siderite and lunar soil minerals.
4. The method of reducing agent-free vacuum iron smelting as defined in claim 1, wherein the refractory crucible of step (1) is a refractory metal or ceramic material or a copper crucible with a built-in circulating cooling medium.
5. The reducing agent-free vacuum metallurgical iron process of claim 1, wherein the product collector of step (1) is a copper collector with a circulating cooling medium therein, the cooling medium comprising water, argon or liquid nitrogen, and the physical shape of the copper collector comprises a square, cylindrical, conical, or spiral vane shape.
6. The method for reducing agent-free vacuum iron smelting according to claim 1, wherein the vacuum degree in the cavity of the step (3) reaches a predetermined value of 10-10 -9 Pa。
7. The method for reducing agent-free vacuum iron smelting according to claim 1, wherein the beneficiation separation in the step (5) means magnetic separation, flotation and reselection of metallic iron particles in the deposit product from other material particles.
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| CN202111102513.XA CN113736945B (en) | 2021-09-20 | 2021-09-20 | Vacuum iron smelting method without reducing agent |
| PCT/CN2022/116019 WO2023040660A1 (en) | 2021-09-20 | 2022-08-31 | Reducing agent-free vacuum iron production method |
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| CN114480746A (en) * | 2022-03-04 | 2022-05-13 | 上海大学 | Method for reconstructing ore phase of ilmenite and separating ferrotitanium |
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| AR011079A1 (en) * | 1998-01-19 | 2000-08-02 | Armco Inc | METHOD AND APPARATUS FOR REMOVING OXIDE FROM A METALLIC SURFACE |
| CN106544695A (en) * | 2015-09-17 | 2017-03-29 | 鞍钢股份有限公司 | A kind of carbon-free iron method and device processed |
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| CN101163639A (en) * | 2005-03-18 | 2008-04-16 | 国立大学法人东京工业大学 | Hydrogen forming apparatus, laser reduction apparatus, energy transformation apparatus method for forming hydrogen and electricity generation system |
| US10400309B2 (en) * | 2013-08-29 | 2019-09-03 | The Regents Of The University Of Colorado, A Body Corporate | Carbothermal reduction reactor system, components thereof, and methods of using same |
| CN105695767B (en) * | 2014-11-28 | 2017-09-26 | 鞍钢股份有限公司 | A kind of semicontinuous magnesium-smelting reduction device of vacuum and method |
| CN104482663B (en) * | 2014-12-12 | 2016-04-27 | 浙江大学 | A kind of solar energy bicavate metal oxide particle heat collection, energy storage method and device thereof |
| CN205062101U (en) * | 2015-09-17 | 2016-03-02 | 鞍钢股份有限公司 | Carbon -free system iron device |
| CN109355108B (en) * | 2018-09-18 | 2020-02-21 | 华中科技大学 | Concentrating solar gasification biomass system for synthesis gas preparation and metal smelting |
| CN111004883B (en) * | 2019-12-27 | 2021-09-17 | 周斌 | Solar energy molten reduced iron device and process |
| CN113736945B (en) * | 2021-09-20 | 2023-06-23 | 上海大学 | Vacuum iron smelting method without reducing agent |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AR011079A1 (en) * | 1998-01-19 | 2000-08-02 | Armco Inc | METHOD AND APPARATUS FOR REMOVING OXIDE FROM A METALLIC SURFACE |
| CN106544695A (en) * | 2015-09-17 | 2017-03-29 | 鞍钢股份有限公司 | A kind of carbon-free iron method and device processed |
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| Title |
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| Iron Metallurgy via Concentrated Solar Energy;Daniel Fernández-González等;Metals;第8卷(第873期);第1-25页 * |
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