CN113932615A - Supergravity high-temperature metallurgy device and method - Google Patents

Supergravity high-temperature metallurgy device and method Download PDF

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CN113932615A
CN113932615A CN202111208841.8A CN202111208841A CN113932615A CN 113932615 A CN113932615 A CN 113932615A CN 202111208841 A CN202111208841 A CN 202111208841A CN 113932615 A CN113932615 A CN 113932615A
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temperature
temperature resistance
resistance furnace
pyrometallurgical
supergravity
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郭占成
高金涛
兰茜
郭磊
王哲
钟怡玮
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University of Science and Technology Beijing USTB
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D19/00—Arrangements of controlling devices
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B13/00—Making spongy iron or liquid steel, by direct processes
    • C21B13/0006—Making spongy iron or liquid steel, by direct processes obtaining iron or steel in a molten state
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B13/00—Making spongy iron or liquid steel, by direct processes
    • C21B13/006—Starting from ores containing non ferrous metallic oxides
    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21B—MANUFACTURE OF IRON OR STEEL
    • C21B13/00—Making spongy iron or liquid steel, by direct processes
    • C21B13/12—Making spongy iron or liquid steel, by direct processes in electric furnaces
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00—Obtaining lead
    • C22B13/02—Obtaining lead by dry processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B13/00—Obtaining lead
    • C22B13/06—Refining
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/10—Obtaining titanium, zirconium or hafnium
    • C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
    • C22B34/1218—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry processes
    • C22B34/1227—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by dry processes using an oxygen containing agent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/04—Heavy metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B4/00—Electrothermal treatment of ores or metallurgical products for obtaining metals or alloys
    • C22B4/08—Apparatus
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/001—Dry processes
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
    • C22B7/04—Working-up slag
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
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    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
    • F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

The invention provides a supergravity high-temperature metallurgical device which comprises a high-temperature reactor box body, wherein the high-temperature reactor box body is divided into a high-temperature metallurgical area and a driving area, the high-temperature metallurgical area is positioned above the driving area, a centrifugal machine rotating shaft penetrates through the high-temperature metallurgical area in the vertical direction, a high-temperature resistance furnace and a balancing device are symmetrically arranged on two sides of the centrifugal machine rotating shaft, a driving component is fixedly connected in the driving area and positioned below the high-temperature metallurgical area, the driving component is in transmission connection with the centrifugal machine rotating shaft, a rotary guide ring sealed by magnetofluid in the high-temperature resistance furnace is communicated with a gas source assembly, a heating component and a thermocouple are arranged in the high-temperature resistance furnace, the heating component and the thermocouple are electrically connected with a measurement and control system through sliding conducting rings, and the measurement and control system is fixedly arranged at the top of the outer side of the high-temperature reactor box body. The invention provides a technical and equipment foundation for scientific research and technical development of a novel supergravity high-temperature metallurgy technology.

Description

Supergravity high-temperature metallurgy device and method
Technical Field
The invention belongs to the field of new high-temperature metallurgy technology, and particularly relates to a supergravity high-temperature metallurgy device and method.
Background
It is well known that the nature of pyrometallurgical processes is the separation of chemical reactions from substances. From the standpoint of the rate of thermochemical reactions, chemical reactions are generally not the limiting links of a pyrometallurgical process, and the rates of mass transfer and interphase separation are often the primary factors that determine the production efficiency of a pyrometallurgical process. Under the action of gravity, the density difference DeltaP between phases is the basis for generating natural convection and relative motion, and the gravity difference is the determining factor of the driving force DeltaPg (DeltaPc, density difference; g, gravity acceleration) of phase separation. Under the supergravity field, the gravity coefficient is increased, and the relative motion between phases caused by density difference can be intensified, so that the material transfer and the interphase transfer are obviously strengthened. Therefore, the reasonable application of the supergravity technology can greatly improve the high-temperature metallurgical efficiency. Particularly for the high-temperature metallurgy fields of high-efficiency separation of slag/gold in DRI of complex iron ores, high-efficiency separation of valuable components in metallurgical slag, purification and purification of metal melts and the like in China, the supergravity technology is expected to break through the bottleneck problem of high-temperature metallurgy phase separation and make breakthrough progress.
The development of the hypergravity technology started in the 80 th 20 th century, the hypergravity was first introduced into the operation of a rectification unit in the chemical field by professor Ramashaw of ICI corporation in uk, and then relevant research work was carried out in the english, american and middle countries successively. At present, the hypergravity technology is mainly applied to the chemical field under the conditions of room temperature and low temperature, and the molecular mixing and mass transfer processes of gas-liquid, gas-liquid-solid and liquid-liquid reactions in unit operations such as rectification, degassing, dust removal and the like are enhanced by utilizing a hypergravity field.
On the ground, the hypergravity can be generated under the rotating conditions of the reactor. However, due to the limitations of the technologies such as heating, temperature measurement and control, atmosphere control, etc. of the high-temperature reactor in the high-speed rotation state, researches and developments on the supergravity pyrometallurgical technology and devices have been reported. At present, in the reports on centrifugal separation and casting of melts, because the technical problems of heating, temperature measurement and control, atmosphere control and the like of a high-temperature reactor in a high-speed rotation state cannot be solved, the reports are only limited to research and application of a natural cooling process of melts, and a supergravity high-temperature metallurgy device and a supergravity high-temperature metallurgy method are urgently needed.
Disclosure of Invention
The invention aims to provide a supergravity pyrometallurgical device, which comprises a high-temperature reactor box body, wherein the high-temperature reactor box body is divided into a pyrometallurgical area and a driving area, the pyrometallurgical area is positioned above the driving area, a centrifuge rotating shaft penetrates through the pyrometallurgical area in the vertical direction, a high-temperature resistance furnace and a balancing device are symmetrically arranged on two sides of the centrifuge rotating shaft, a driving component is fixedly connected in the driving area and positioned below the pyrometallurgical area, the driving component is in transmission connection with the centrifuge rotating shaft, a rotary diversion ring sealed by magnetofluid is communicated with a gas source assembly in the high-temperature resistance furnace, a heating component and a thermocouple are arranged in the high-temperature resistance furnace, the heating component and the thermocouple are electrically connected with a measurement and control system through sliding, and the driving component is electrically connected with the measurement and control system, the measurement and control system is fixedly arranged at the top of the outer side of the high-temperature reactor box body.
Preferably, the bottom fixedly connected with in pyrometallurgical area the slip conducting ring, the slip conducting ring cup joints the outside of centrifuge pivot, inside the high temperature resistance stove heating element with the thermocouple passes through respectively the slip conducting ring with observe and control system electric connection.
Preferably, the top of the centrifuge rotating shaft is sleeved with a magnetic fluid sealed rotating flow guide ring, and the gas source assembly is communicated with the high-temperature resistance furnace through the magnetic fluid sealed rotating flow guide ring.
Preferably, the two sides of the rotating shaft of the centrifuge are symmetrically and fixedly connected with a balance frame, the high-temperature resistance furnace is fixedly connected to the inner side of one of the balance frames, and the balance device is fixedly connected to the inner side of the other balance frame.
Preferably, the temperature in the high-temperature resistance furnace is set to be 25-1700 ℃, and the gravity coefficient in the high-temperature resistance furnace is 1-5000.
Preferably, the heating assembly comprises a metal wire resistor and an anti-vibration ceramic resistor heating body, the metal wire resistor is used for heating the inside of the high-temperature resistance furnace to 25-1300 ℃, and the anti-vibration ceramic resistor heating body is used for heating the inside of the high-temperature resistance furnace to 1300-1700 ℃.
A super-gravity high-temperature metallurgy method comprises the following steps:
the method comprises the following steps: loading a metallurgical material into the high-temperature resistance furnace of the supergravity high-temperature metallurgical device;
step two: controlling the reducing, oxidizing or inert atmosphere of the supergravity high-temperature metallurgical device, and heating the metallurgical material in the step one to a melt heterogeneous phase separation temperature interval;
step three: and starting the driving assembly to realize melt heterogeneous phase separation.
Preferably, in the third step, the measurement and control system acquires a temperature signal actually measured by the thermocouple inside the high-temperature resistance furnace, and the measurement and control system sends a heating or temperature control instruction to the heating component and the thermocouple, and controls the temperature inside the high-temperature resistance furnace in real time according to the melt heterogeneous phase separation condition.
Preferably, in the third step, the gas source assembly continuously inputs gas into the high-temperature resistance furnace, and selectively controls the internal atmosphere of the high-temperature resistance furnace according to the requirement of the melt atmosphere; and continuously generating a gas phase in the high-temperature resistance furnace, and monitoring the components of the gas phase discharged from the high-temperature resistance furnace in real time on line.
The invention has the following technical effects: under the action of the driving assembly and the centrifuge rotating shaft, the high-temperature resistance furnace and the balancing device are driven to realize high-gravity centrifugal rotation, and the stability of centrifugal rotation motion is realized by adjusting the balance weight and the gravity center of the balancing device; the interior of the high-temperature resistance furnace in a high-speed rotation state is continuously heated through the heating assembly, and real-time temperature measurement and control are carried out through a measurement and control system; the gas source assembly can provide selective atmosphere for the interior of the high-temperature resistance furnace, and the measurement and control system can carry out real-time measurement and control; the magnetic fluid sealing rotary guide ring is communicated with the gas source assembly and the interior of the high-temperature resistance furnace; the temperature signal of the high-temperature resistance furnace is transmitted to the measurement and control system through the sliding conducting ring, and the heating or temperature control instruction is transmitted to the heating component inside the high-temperature resistance furnace through the sliding conducting ring.
The invention solves the core technical problem restricting the application of the hypergravity technology to the field of high-temperature metallurgy, develops the technologies of continuous heating, real-time temperature measurement and control, selective atmosphere control and the like in the high-temperature resistance furnace in a high-speed rotating state, develops the hypergravity high-temperature metallurgy device and the hypergravity high-temperature metallurgy method, and provides a technical and equipment foundation for scientific research and technical development of a new hypergravity high-temperature metallurgy technology.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a macro-topography and SEM image of a slag/gold separation sample in the DRI of iron ore of example 1;
FIG. 3 is an XRD pattern of a slag/gold separation sample of the DRI of iron ore of example 1;
FIG. 4 is a macro-morphology and SEM image of a separated sample of valuable components in metallurgical slag of example 3;
FIG. 5 is an XRD pattern of a separated sample of valuable components in metallurgical slag of example 3;
FIG. 6 is a macro-topography and SEM image of a sample of a metal purification clean up separation of example 5;
FIG. 7 is an XRD pattern of a sample of the metal purification and separation apparatus of example 5;
wherein, 1, a high-temperature reactor box body; 2. the magnetic fluid seals the rotary guide ring; 3. an air source static end interface; 4. a high temperature resistance furnace; 5. a thermocouple; 6. a balancing stand; 7. a centrifuge shaft; 8. controlling the temperature of a static end; 9. a drive assembly; 10. controlling the temperature of the movable end; 11. sliding the conducting ring; 12. a balancing device; 13. an air source dynamic end interface; 14. an interlayer; 15. and (5) a measurement and control system.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Referring to fig. 1, the invention provides a supergravity pyrometallurgical device, which comprises a high-temperature reactor box body 1, wherein the interior of the high-temperature reactor box body 1 is divided into a pyrometallurgical area and a driving area, the pyrometallurgical area is positioned above the driving area, a centrifuge rotating shaft 7 penetrates through the pyrometallurgical area in the vertical direction, a high-temperature resistance furnace 4 and a balancing device 12 are symmetrically arranged on two sides of the centrifuge rotating shaft 7, a driving component 9 is fixedly connected in the driving area, the driving component 9 is positioned below the pyrometallurgical area, the driving component 9 is in transmission connection with the centrifuge rotating shaft 7, a rotary diversion ring 2 sealed by a magnetic fluid in the high-temperature resistance furnace 4 is communicated with a gas source assembly, a heating component and a thermocouple 5 are arranged in the high-temperature resistance furnace 4 in an annular manner, the heating component and the thermocouple 5 are electrically connected with a measurement and control system 15 through a sliding conducting ring 11, the driving component 9 is electrically connected with the measurement and control system 15, the measurement and control system 15 is fixedly arranged at the top of the outer side of the high-temperature reactor box body 1.
Under the action of the driving component 9 and the centrifuge rotating shaft 7, the high-temperature resistance furnace 4 and the balancing device 12 are driven to realize supergravity centrifugal rotation, and the stability of centrifugal rotation motion is realized by adjusting the balance weight and the gravity center of the balancing device 12; the interior of the high-temperature resistance furnace 4 in a high-speed rotation state is continuously heated through the heating assembly, and real-time temperature measurement and control are carried out through a measurement and control system; the selective atmosphere can be provided for the interior of the high-temperature resistance furnace 4 through the gas source assembly, and real-time measurement and control are carried out through the measurement and control system; the magnetic fluid sealing rotary guide ring 2 is communicated with the gas source assembly and the interior of the high-temperature resistance furnace 4; the temperature signal of the high-temperature resistance furnace 4 is transmitted to the measurement and control system through the sliding conducting ring 11, and the heating or temperature control instruction is transmitted to the heating component and the thermocouple 5 in the high-temperature resistance furnace 4 through the sliding conducting ring 11.
According to the further optimization scheme, the bottom of the pyrometallurgical area is fixedly connected with a sliding conducting ring 11, the sliding conducting ring 11 is sleeved on the outer side of the centrifuge rotating shaft 7, and the heating assembly and the thermocouple 5 inside the high-temperature resistance furnace 4 are electrically connected with the measurement and control system 15 through the sliding conducting ring 11 respectively. The sliding conducting ring 11 can transmit electric signals, temperature signals inside the high-temperature resistance furnace 4 are transmitted to the measurement and control system 15 through the temperature control static end 8, and heating or temperature control instructions are sent to the heating assembly and the thermocouple 5 through the temperature control movable end 10.
According to the further optimized scheme, the top of a centrifuge rotating shaft 7 is sleeved with a magnetic fluid sealing rotary guide ring 2, and a gas source assembly is communicated with the inside of a high-temperature resistance furnace 4 through the magnetic fluid sealing rotary guide ring 2; an air source static end interface 3 and an air source dynamic end interface 13 are arranged on the outer side of the magnetic fluid sealing rotary guide ring 2, the air source static end interface 3 is communicated with an air source assembly, and the air source dynamic end interface 13 is communicated with the inside of the high-temperature resistance furnace 4.
Further optimize the scheme, centrifuge pivot 7 bilateral symmetry fixedly connected with balancing stand 6, high temperature resistance furnace 4 fixed connection is in the inboard of one of them balancing stand 6, balancing unit 12 fixed connection is in the inboard of another balancing stand 6. The balance with different metallurgical materials in the high-temperature resistance furnace 4 is realized by adjusting the balance weight and the gravity center of the balance device 12.
Further optimizing the scheme, the temperature in the high-temperature resistance furnace 4 is set to be 25-1700 ℃; the gravity coefficient in the high-temperature resistance furnace 4 is 1-5000. Aiming at different melt separation stages, the corresponding gravity coefficient is set under the high-speed rotation state of the high-temperature resistance furnace 4, so that the separation efficiency can be improved.
In a further optimized scheme, the heating assembly comprises a metal wire resistor and an anti-vibration ceramic resistor heating body, the metal wire resistor is used for heating the interior of the high-temperature resistance furnace 4 to 25-1700 ℃, and the anti-vibration ceramic resistor heating body is used for heating the interior of the high-temperature resistance furnace 4 to 1300-1700 ℃. Different melting temperatures are set according to different metallurgical materials.
In a further optimized scheme, the balancing device 12 adopts an existing centrifugal rotation balancing adjusting structure, and details are not repeated.
Further optimize the scheme, pyrometallurgical zone bottom is provided with interlayer 14, and interlayer 14 fixed connection is on the inside wall of high temperature reactor box 1, and interlayer 14 is run through to the vertical direction of centrifuge pivot 7, and the drive area is located the below of interlayer 14 for the heat transfer in isolated pyrometallurgical zone is to the drive area.
A super-gravity high-temperature metallurgy method comprises the following steps:
the method comprises the following steps: loading metallurgical materials such as ore, slag, metal and the like into a high-temperature resistance furnace 4 of a supergravity high-temperature metallurgical device;
step two: controlling the reducing, oxidizing or inert atmosphere of the supergravity high-temperature metallurgical device, and heating the metallurgical materials such as the ore, the slag, the metal and the like in the step one to a heterogeneous phase separation temperature interval in the ore, the slag and the metal melt;
step three: and starting the driving component 9 to drive the centrifuge rotating shaft 7 to rotate, controlling the temperature, the gravity coefficient and the atmosphere in the high-temperature resistance furnace 4 rotating at a high speed in real time, and separating heterogeneous phases in the ore, slag and metal melt in the step two by utilizing the supergravity to realize separation under the conditions of real-time controllable temperature, gravity and atmosphere.
In the third step, the measurement and control system 15 acquires a temperature signal inside the high-temperature resistance furnace 4, the measurement and control system 15 sends a heating or temperature control instruction to the heating component and the thermocouple 5, and the temperature inside the high-temperature resistance furnace is controlled in real time according to the melt heterogeneous phase separation condition.
And in the third step, the gas source assembly inputs gas into the high-temperature resistance furnace 4, and the atmosphere in the high-temperature resistance furnace is selectively controlled according to the requirement of the melt atmosphere.
In the third step, the heterogeneous phase separation in the melt comprises any one of phase transfer and filtration separation.
Further optimizing the scheme, the control mode of the measurement and control system adopts the prior art.
In a further optimized scheme, the magnetic fluid sealing rotary guide ring 2 and the sliding conducting ring 11 adopt the existing structures.
The working process of the embodiment is as follows:
starting the driving component 9 to drive the centrifuge rotating shaft 7 to rotate at a high speed, controlling the temperature, the gravity coefficient and the atmosphere in the high-temperature resistance furnace 4 in real time in the high-speed rotating process, and realizing interphase transfer or filtering separation under the conditions of real-time controllable temperature, gravity and atmosphere by utilizing heterogeneous phases in the ore, slag and metal melt in the supergravity driving step two; according to the condition of heterogeneous phase separation in the melt in the high-temperature resistance furnace 4, the balance device 12 is adjusted to ensure that the whole centrifugal motion runs stably. The core technical problem restricting the application of the hypergravity technology to the field of high-temperature metallurgy is solved, the technologies of continuous heating, real-time temperature measurement and control, selective atmosphere control and the like in the high-temperature resistance furnace 4 in a high-speed rotating state are developed, the hypergravity high-temperature metallurgy device and the hypergravity high-temperature metallurgy phase separation method are developed, and a technology and equipment basis is provided for scientific research and technical development of a novel hypergravity high-temperature metallurgy technology.
Example one
Referring to fig. 2 and 3, the separation process of this example consists in slag/gold separation in a typical complex iron ore DRI under a reducing atmosphere:
step 1, 100kg of typical complex iron ore DRI (taking ludwigite DRI as an example, the main technical indexes are TFe 67.34%, MFe 67.30% and B)2O36.76 percent of MgO24.50 percent) is loaded into a high-temperature resistance furnace 4 of a supergravity high-temperature metallurgical device.
And 2, controlling the interior of the high-temperature resistance furnace 4 to be a reducing atmosphere, heating the ludwigite to 1250 ℃ under the reducing atmosphere, realizing the melting of slag/gold, and simultaneously effectively avoiding the oxidation of a metal phase.
Step 3, starting a driving assembly 9 to drive a centrifuge rotating shaft 7 to rotate, and controlling the internal gravity coefficient of the high-temperature resistance furnace 4 to be G equal to 2000; the sliding conducting ring 11 is adopted to connect the high-temperature resistance furnace 4 and the movable end and the static end of the measurement and control system 15, and the internal temperature of the high-speed rotating high-temperature resistance furnace 4 is controlled to 1250 ℃ in real time; the magnetofluid sealed rotary guide ring 2 is connected with the high-temperature resistance furnace 4 and the movable end and the static end of an air source, and the interior of the high-speed rotary high-temperature resistance furnace 4 is selectively controlled to be in a reducing atmosphere; separating at constant temperature for 5min until the residue/gold is sufficiently separated; then the centrifugal rotation is closed, the sample is taken for analysis, and the macro morphology, SEM and XRD patterns of the slag/gold sample are respectively shown in figures 2 and 3. As can be seen from fig. 2 and 3, under the driving of the high gravity field, the metal phase and the slag phase are separated efficiently and rapidly at a lower melting temperature; moreover, because the separation temperature is low and the separation rate is high, the infiltration of impurity elements into the metal phase can be effectively avoided, the purity of the separated metal phase is very high, the XRD spectrum only has a single MFe diffraction peak, and the microstructure of the metal phase does not contain any impurities; moreover, the recovery rate of the separated metal phase is very high, and any metal phase is not included in the residual slag phase.
In the embodiment, under a real-time reducing atmosphere and at a lower melting temperature, the slag phase and the metal phase in typical complex iron ore (ludwigite) DRI are driven by supergravity to realize high-efficiency and rapid separation, the content of Fe (iron) in the separated metal phase reaches 99.96%, and the content of Fe in the slag phase is as low as 0.06%.
Example two
The separation process of this example differs from that of the first example only in that in step 3, the separation temperature is controlled to 1350 ℃, the gravity coefficient is controlled to be 1000, and the separation time is controlled to be 3 min:
the Fe (iron) content in the separated metal phase reaches up to 99.97 percent, and the Fe content in the slag phase is as low as 0.04 percent.
EXAMPLE III
Referring to fig. 4 and 5, the separation process of the present embodiment is different from that of the first embodiment only in that the valuable components in the typical metallurgical slag are separated under the oxidizing atmosphere:
step 1, 200kg of typical metallurgical slag (taking titanium-containing blast furnace slag as an example, the main technical index is TiO)222% -29% and alkalinity of 0.3-0.5) are loaded into a high-temperature resistance furnace 4 of the supergravity high-temperature metallurgical device.
And 2, controlling the inside of the high-temperature resistance furnace 4 to be an oxidizing atmosphere, and heating the titanium-containing blast furnace slag to 1320 ℃ under the oxidizing atmosphere to realize the efficient conversion of valuable element Ti (titanium) in the slag to TiO2 (rutile).
Step 3, starting a driving assembly 9 to drive a centrifuge rotating shaft 7 to rotate, and controlling the gravity coefficient in the high-speed rotating high-temperature resistance furnace 4 to be G500; the sliding conducting ring 11 is adopted to connect the high-temperature resistance furnace 4 and the movable end and the static end of the measurement and control system 15, the temperature in the high-speed rotating high-temperature resistance furnace 4 is controlled in real time to be slowly reduced at a constant rate at the temperature of 1320-1180 ℃, and the full separation and growth of rutile are realized; the magnetofluid sealed rotary guide ring 2 is connected with the high-temperature resistance furnace 4 and the movable end and the static end of an air source, and the inside of the high-speed rotary high-temperature resistance furnace 4 is selectively controlled to be an oxidizing atmosphere; continuously separating for 10min until rutile and slag are fully separated; after that, the centrifugal rotation is turned off, and the sample is sampled and analyzed, and the macro morphology, the SEM and the XRD pattern of the sample are respectively shown in figures 4 and 5. As can be seen from fig. 4 and 5, the rutile crystal is efficiently separated from the slag under the driving of the high gravity field; moreover, the oxidation atmosphere can promote the Ti to be fully converted into the rutile, the rutile obtained by separation is columnar crystal with developed dendrite, the crystal purity is very high, the XRD pattern of the rutile is only a single diffraction peak of TiO2, and the microstructure of the rutile does not contain any slag inclusion; furthermore, the recovery of Ti from the separated rutile is also very high, and the residual slag phase is free of any rutile particles.
In the embodiment, the slag is controlled to slowly cool at a constant rate in a liquating and crystallizing temperature interval of valuable element Ti (titanium) under a real-time oxidizing atmosphere, so that the sufficient transformation from Ti to rutile and the sufficient precipitation and growth of rutile are realized, the rutile phase and the slag phase in typical metallurgical slag (titanium-containing blast furnace slag) are driven by supergravity to realize high-efficiency separation, the content of TiO2 in the separated rutile phase reaches 98.04%, and the recovery rate of Ti in the rutile phase reaches 99.89%.
Example four
The separation process of this embodiment differs from the third embodiment only in that in step 3, the temperature is controlled at 1320-:
the content of TiO2 in the separated rutile phase reaches 99.17 percent, and the recovery rate of Ti in the rutile phase reaches 98.25 percent.
EXAMPLE five
Referring to fig. 6 and 7, the separation process of this example differs from that of example one only in that the typical metal purification is carried out under an inert atmosphere:
step 1, 300kg of typical metal (taking lead bullion as an example, the main technical indexes of the lead bullion are Pb 96.5-97.7 percent and Cu 1-2 percent) is loaded into a high-temperature resistance furnace 4 of a supergravity high-temperature metallurgical device.
Step 2, controlling the interior of the high-temperature resistance furnace 4 to be inert atmosphere, and heating the crude lead to 550 ℃ under the protection of the inert atmosphere until the metal lead is fully melted; then slowly cooling to 450 ℃, realizing the full liquation of impurity element Cu (copper), and simultaneously effectively avoiding the oxidation of the metal lead liquid.
Step 3, starting a driving assembly 9 to drive a centrifuge rotating shaft 7 to rotate, and controlling the internal gravity coefficient of the high-speed rotating high-temperature resistance furnace 4 to be G-300; the sliding conducting ring 11 is adopted to connect the high-temperature resistance furnace 4 and the movable end and the static end of the measurement and control system 15, and the internal temperature of the high-temperature resistance furnace 4 rotating at a high speed is controlled to be 450 ℃ in real time; the magnetofluid sealed rotary guide ring 2 is connected with the high-temperature resistance furnace 4 and the movable end and the static end of an air source, and the inert atmosphere in the high-speed rotary high-temperature resistance furnace 4 is selectively controlled; separating at constant temperature for 6min until lead liquid and Cu particles are fully separated; after that, the centrifugal rotation is turned off, and the sample is sampled and analyzed, and the macro morphology, SEM and XRD pattern of the sample are shown in FIG. 6 and FIG. 7 respectively. As can be seen from fig. 6 and 7, under the driving of the high gravity field, the metal lead liquid and the copper crystal grains are separated efficiently, the purity of the separated metal lead liquid and the purity of the separated copper crystal grains are both very high, the XRD patterns of the two metal lead liquid and the separated copper crystal grains respectively only have a single diffraction peak of Pb or Cu, and no impurity phase is mixed in the microstructures of the two metal lead liquid and the separated copper crystal grains.
In the embodiment, the lead liquid is controlled to be slowly cooled in the liquation interval of Cu under the protection of real-time inert atmosphere, the sufficient liquation of Cu is realized, the impurity Cu in typical metal (crude lead) is driven by the supergravity to realize high-efficiency separation, the Cu content in the separated metal lead liquid is reduced to 0.07%, and the Cu removal rate in the metal lead liquid is as high as 99.50%.
EXAMPLE six
The separation process of this example differs from that of the fifth example only in that in step 3, the separation temperature is controlled to 350 ℃, the gravity coefficient is 600, and the separation time is 2 min:
the Cu content in the separated metal lead liquid is reduced to 0.03%, and the Cu removal rate in the metal lead liquid is as high as 99.79%.
In the description of the present invention, it is to be understood that the terms "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, are merely for convenience of description of the present invention, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (9)

1. A hypergravity pyrometallurgical device which characterized in that: including high temperature reactor box (1), divide into pyrometallurgical zone and drive area in high temperature reactor box (1), just pyrometallurgical zone is located the top of drive area, pyrometallurgical zone vertical direction runs through there is centrifuge pivot (7), centrifuge pivot (7) bilateral symmetry is provided with high temperature resistance stove (4) and balancing unit (12), the rigid coupling has drive assembly (9) in the drive area, drive assembly (9) are located high temperature metallurgical zone below, drive assembly (9) with centrifuge pivot (7) transmission is connected, sealed rotatory water conservancy diversion ring (2) and air supply assembly intercommunication through the magnetic current body in high temperature resistance stove (4), be provided with heating element and thermocouple (5) in high temperature resistance stove (4), heating element with thermocouple (5) observe and control through slip conducting ring (11) and observe and control system (15) electric connection, the driving assembly (9) is electrically connected with the measurement and control system (15), and the measurement and control system (15) is fixedly arranged at the top of the outer side of the high-temperature reactor box body (1).
2. A supergravity pyrometallurgical apparatus in accordance with claim 1, wherein: the bottom fixedly connected with in pyrometallurgical area slip conducting ring (11), slip conducting ring (11) cup joint the outside of centrifuge pivot (7), inside high temperature resistance stove (4) heating element with thermocouple (5) pass through respectively slip conducting ring (11) with observe and control system (15) electric connection.
3. A supergravity pyrometallurgical apparatus in accordance with claim 1, wherein: the top of the centrifuge rotating shaft (7) is sleeved with a magnetic fluid seal rotating guide ring (2), and the gas source assembly is communicated with the high-temperature resistance furnace (4) through the magnetic fluid seal rotating guide ring (2).
4. A supergravity pyrometallurgical apparatus in accordance with claim 1, wherein: the centrifuge rotating shaft (7) is symmetrically and fixedly connected with balancing frames (6) on two sides, the high-temperature resistance furnace (4) is fixedly connected to the inner side of one of the balancing frames (6), and the balancing device (12) is fixedly connected to the inner side of the other balancing frame (6).
5. A supergravity pyrometallurgical apparatus in accordance with claim 1, wherein: the temperature in the high-temperature resistance furnace (4) is set to be 25-1700 ℃, and the gravity coefficient in the high-temperature resistance furnace (4) is G1-5000.
6. A hypergravity pyrometallurgical apparatus according to claim 5 wherein: the heating assembly comprises a metal wire resistor and a vibration-proof ceramic resistor heating body, the metal wire resistor is used for heating the inside of the high-temperature resistance furnace (4) to 25-1300 ℃, and the vibration-proof ceramic resistor heating body is used for heating the inside of the high-temperature resistance furnace (4) to 1300 DEG C
-1700℃。
7. A supergravity high-temperature metallurgy method is characterized in that: a hypergravity pyrometallurgical apparatus according to claims 1 to 6 which comprises the steps of:
the method comprises the following steps: charging a metallurgical material into the high temperature resistance furnace (4) of the hypergravity pyrometallurgical apparatus;
step two: controlling the reducing, oxidizing or inert atmosphere of the supergravity high-temperature metallurgical device, and heating the metallurgical material in the step one to a melt heterogeneous phase separation temperature interval;
step three: and starting the driving assembly (9) to realize melt heterogeneous phase separation.
8. The hypergravity pyrometallurgical method in accordance with claim 7 wherein: in the third step, the measurement and control system (15) acquires the temperature signal actually measured by the thermocouple (5) inside the high-temperature resistance furnace (4), the measurement and control system (15) sends heating or temperature control instructions to the heating component and the thermocouple (5), and the internal temperature of the high-temperature resistance furnace (4) is controlled in real time according to the melt heterogeneous phase separation condition.
9. The hypergravity pyrometallurgical method in accordance with claim 7 wherein: in the third step, the gas source assembly continuously inputs gas into the high-temperature resistance furnace (4), and the internal atmosphere of the high-temperature resistance furnace (4) is selectively controlled according to the requirement of the melt atmosphere; and continuously generating a gas phase in the high-temperature resistance furnace (4), and monitoring the components of the gas phase discharged from the high-temperature resistance furnace (4) in real time on line.
CN202111208841.8A 2021-10-18 2021-10-18 Supergravity high-temperature metallurgy device and method Pending CN113932615A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102181888A (en) * 2011-04-07 2011-09-14 北京化工大学 Super-gravity device used for electrochemical deposition in ionic liquid
CN102825539A (en) * 2012-09-25 2012-12-19 郑州大地机械制造有限公司 Hydraulic counter weight device applied to high-speed reciprocating motion component
CN103290443A (en) * 2013-05-15 2013-09-11 北京化工大学 Method for synchronizing high preferred orientation aluminum coating by using supergravity technology
CN105154716A (en) * 2015-09-29 2015-12-16 攀枝花学院 Preparation method and preparation device of titanium-aluminum alloy
CN109358087A (en) * 2018-11-26 2019-02-19 中国科学院上海硅酸盐研究所 Material at high temperature directional solidification experimental provision and experimental method under a kind of Elevated Gravity

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102181888A (en) * 2011-04-07 2011-09-14 北京化工大学 Super-gravity device used for electrochemical deposition in ionic liquid
CN102825539A (en) * 2012-09-25 2012-12-19 郑州大地机械制造有限公司 Hydraulic counter weight device applied to high-speed reciprocating motion component
CN103290443A (en) * 2013-05-15 2013-09-11 北京化工大学 Method for synchronizing high preferred orientation aluminum coating by using supergravity technology
CN105154716A (en) * 2015-09-29 2015-12-16 攀枝花学院 Preparation method and preparation device of titanium-aluminum alloy
CN109358087A (en) * 2018-11-26 2019-02-19 中国科学院上海硅酸盐研究所 Material at high temperature directional solidification experimental provision and experimental method under a kind of Elevated Gravity

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