CN112077333A - Method for preparing metal powder and energy-saving push boat type hydrogen reduction furnace for preparing metal powder - Google Patents

Method for preparing metal powder and energy-saving push boat type hydrogen reduction furnace for preparing metal powder Download PDF

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CN112077333A
CN112077333A CN202010989640.5A CN202010989640A CN112077333A CN 112077333 A CN112077333 A CN 112077333A CN 202010989640 A CN202010989640 A CN 202010989640A CN 112077333 A CN112077333 A CN 112077333A
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furnace tube
furnace
metal powder
temperature
reduction
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CN112077333B (en
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赵景学
毕琨
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Chengdu Shijia Huanjing Technology Co ltd
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Chengdu Shijia Huanjing Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B22F9/22Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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  • General Chemical & Material Sciences (AREA)
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Abstract

The invention discloses a method for preparing metal powder and an energy-saving push boat type hydrogen reduction furnace for preparing the metal powder, wherein metal oxide powder in the method sequentially passes through a first heating section and a second heating section, and the metal oxide powder and residual hydrogen in high-temperature reduction reaction are subjected to pre-reduction reaction in the first heating section to form the metal oxide powder in a sub-metallic state; and continuously carrying out high-temperature reduction reaction on the metal oxide powder subjected to the pre-reduction reaction in a second heating section to obtain metal powder after the high-temperature reduction reaction is finished. On one hand, the utilization rate of hydrogen is improved, and the hydrogen consumption of the metal powder prepared by the energy-saving push boat type hydrogen reducing furnace is 2/3 of that of the traditional hydrogen reducing furnace; on the other hand, the metal oxide powder is pre-reduced to form the metal oxide powder in a sub-metallic state, so that the difficulty of high-temperature reduction reaction of the metal powder is reduced.

Description

Method for preparing metal powder and energy-saving push boat type hydrogen reduction furnace for preparing metal powder
Technical Field
The invention belongs to metal powder preparation, and particularly relates to a method for preparing metal powder and an energy-saving push boat type hydrogen reduction furnace for preparing the metal powder.
Background
Since most of metal oxides are more stable than elemental metals, metals exist in oxide form in nature, and with the development demand of modern industry, especially the high-speed development of modern powder metallurgy technology, since high-purity metal powder which was developed in the last 30 centuries was discovered, the high-purity metal powder is applied to various fields due to its special properties, increasing the market demand for the high-purity metal powder. However, how to prepare high-purity metal powder in large quantities becomes a difficult problem for manufacturers.
In view of the above problems, the production of metal powder by reducing metal oxide powder in a high temperature state using hydrogen gas based on the conventional hydrogen reducing furnace as shown in fig. 6 has the following problems:
(1) when the metal powder is prepared using the metal oxide powder for the conventional hydrogen reducing furnace as shown in fig. 6, the conventional preparation method is to directly reduce the metal oxide powder with hydrogen at a high temperature to obtain the metal powder. However, not all hydrogen and metal oxide powder are reduced at high temperature in the whole high-temperature reduction process, so that part of hydrogen which does not participate in the reaction is discharged, which causes waste of energy and increases the preparation cost of metal powder.
(2) If the prepared metal powder is micron-sized, the high-temperature metal powder can generate spontaneous combustion in the cooling process and after cooling, on one hand, certain potential safety hazards are caused, on the other hand, micron-sized metal powder is difficult to obtain, especially when the metal powder below 25 microns is required to be prepared, spontaneous combustion is easy to generate in the cooling process, and the possibility of obtaining the metal powder below 25 microns is almost eliminated.
Disclosure of Invention
Based on the above problems, it is an object of the present invention to provide a method for producing a metal powder having a particle size of 1 to 25 μm at a low production cost.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing metal powder, metal oxide powder takes place prereduction and high-temperature reduction with reducing gas at first sequentially and get the metal powder of high temperature state, then get the metal powder comprising average particle size 1-25 μm after cooling the metal powder of high temperature state; the high-temperature metal powder is passivated with passivation gas at the beginning of cooling so as to generate a protective layer on the surface of the high-temperature metal powder; the residual reducing gas after high-temperature reduction and the metal oxide powder are subjected to pre-reduction.
Preferably, the reducing gas is H2(ii) a The temperature of the pre-reduction is 450-800 ℃; the temperature of the high-temperature reduction is 500-850 ℃; the time of the pre-reduction and the high-temperature reduction of the metal oxide powder is 8-18h in total.
Another object of the present invention is to provide an energy-saving push boat type hydrogen reduction furnace for preparing metal powder, which comprises an upper layer furnace tube, a lower layer furnace tube, a transfer mechanism, and a heating element;
the upper layer furnace tube comprises a first heating section, wherein the upper layer furnace tube is used for feeding and is used for pre-reducing metal oxide powder in the first heating section under the matching of a heating element;
the lower furnace tube comprises a second heating section and a cooling section, wherein the lower furnace tube is used for discharging cooled metal powder and passivating and cooling high-temperature metal powder in the cooling section; the metal oxide powder is subjected to high-temperature reduction in a second heating section by matching with the heating element; wherein, the heating element directly heats the second heating section of the lower furnace tube;
the transfer mechanism is used for transferring the pre-reduced metal oxide powder to the lower furnace tube;
wherein the temperature of the second heating section is 10-50 ℃ higher than the temperature of the first heating section.
Preferably, the energy-saving push boat type hydrogen reduction furnace further comprises a furnace body for placing the tube bodies of the upper layer furnace tube and the lower layer furnace tube, wherein the furnace body is used for containing metal oxide powder and can move the material boat in the upper layer furnace tube and the lower layer furnace tube, so that H is provided for pre-reduction and high-temperature reduction2And an air inlet pipe connected with the lower furnace tube for discharging gas and unreacted H generated in the high-temperature reduction and pre-reduction processes2The exhaust pipe is connected with the upper layer furnace tube, and the cooling device is arranged on the lower layer furnace tube; wherein, the material boat for containing the metal oxide powder is transferred to the lower furnace tube from the upper furnace tube by the transfer mechanism.
Preferably, when the cooling device is located outside the furnace body, a first heating section for pre-reducing the metal oxide powder and a second heating section for high-temperature reducing the metal oxide powder are located in the furnace body, and the air inlet pipe and the air outlet pipe are located outside the furnace body.
Preferably, the cooling device is a water cooling device arranged on the cooling section of the lower furnace tube.
Preferably, the cooling device comprises an air cooling device and a water cooling device which are sequentially arranged along the moving direction of the material boat in the tube of the lower furnace tube and used for cooling the high-temperature metal powder moving to the cooling section; wherein, the water cooling device is arranged on the cooling section of the lower furnace tube.
Preferably, the transfer mechanism is including connecting the transfer chamber that is in the other end of upper boiler tube and lower floor's boiler tube and with upper boiler tube and lower floor's boiler tube U type intercommunication sets up in the transfer chamber and be used for placing the platform of material boat sets up on the bottom plate of transfer chamber and with the third thrust machine that the platform is connected, and set up and be in on the lateral wall of transfer chamber and be used for pushing the material boat that is located on the platform the intraductal second thrust machine of lower floor's boiler tube.
Preferably, the furnace body comprises a furnace liner for placing the first heating section of the upper layer furnace tube and the second heating section of the lower layer furnace tube, and a heat preservation and insulation layer coated outside the furnace liner.
Preferably, the energy-saving push boat type hydrogen reduction furnace further comprises a temperature detector arranged on the heat preservation and insulation layer and used for monitoring the temperature of the upper layer furnace tube and the lower layer furnace tube, a first thrust machine which is matched with the feeding hole and used for pushing the material boat into the upper layer furnace tube, guide rails which are arranged in the tubes of the upper layer furnace tube and the lower layer furnace tube and used for moving the material boat, and a cooling device arranged on the upper layer furnace tube.
Compared with the prior art, the invention has the following beneficial effects:
(1) in the preparation method of the metal powder, the metal oxide powder is subjected to pre-reduction and high-temperature reduction in sequence. Firstly, the metal oxide powder is partially reduced or reduced into a sub-metallic oxide during pre-reduction; then, the pre-reduced metal oxide powder is subjected to high temperature reduction with a reducing gas. Because the pre-reduction leads the metal oxide powder to form the sub-metallic oxide or partially reduce, on one hand, the difficulty of the high-temperature reduction of the metal powder is reduced, and on the other hand, the high-temperature reduction time is shortened, thereby reducing the difficulty coefficient of preparing the metal powder with the average grain diameter of 1-25 mu m. In addition, after the pre-reduction and the high-temperature reduction are started, the residual reducing gas after the high-temperature reduction and the metal oxide powder are subjected to pre-reduction, and compared with the method for preparing the metal powder by adopting the traditional hydrogen reduction furnace through a high-temperature reduction method, the method disclosed by the invention has the advantages that the hydrogen which does not participate in the high-temperature reduction is fully utilized by utilizing the pre-reduction, and the consumption of the hydrogen is reduced. Therefore, the preparation cost of the metal powder is reduced, and the market competitiveness of the metal powder prepared by the method is improved.
In addition, in order to prepare the metal powder with the particle size of less than 25 microns, on the basis of reducing the difficulty system of the preparation process of the metal powder with the particle size of 1-25 microns by combining pre-reduction and high-temperature reduction, the invention leads the high-temperature metal powder obtained by pre-reduction and high-temperature reduction to be passivated with air, thereby forming a layer of protective film on the surface of the metal, so that the protective film can isolate the further contact between the metal powder and the air on one hand and avoid the spontaneous combustion easily caused by preparing the metal powder with the particle size of less than 25 microns; on the other hand, the protective film can improve the heat resistance of the metal powder, thereby further inhibiting spontaneous combustion of the prepared metal powder with the particle size of less than 25 mu m. And simultaneously, the safety in the metal powder preparation process is also improved.
(2) The energy-saving push boat type hydrogen reduction furnace is provided with an upper layer of furnace tube and a lower layer of furnace tube, metal oxide powder is pre-reduced in a first heating section of the upper layer of furnace tube, and high-temperature reduction is performed in a second heating section of the lower layer of furnace tube, and the pre-reduction and the high-temperature reduction of the metal oxide powder are simultaneously performed when the energy-saving push boat type hydrogen reduction furnace is adopted to prepare the metal powder, so that the time for preparing the metal powder with the particle size of 1-25 mu m is shortened, and the preparation cost of the metal powder with the particle size of 1-25 mu m is reduced. In addition, because the upper-layer furnace tube and the lower-layer furnace tube in the energy-saving push boat type hydrogen reduction furnace are connected through the transfer mechanism, hydrogen which does not participate in high-temperature reduction of the second heating section enters the upper-layer furnace tube through the transfer mechanism and is subjected to pre-reduction with metal powder placed in the first heating section of the upper-layer furnace tube; the practice of the applicant proves that when the same amount of metal oxide powder is used for preparing the metal powder, the consumption of the hydrogen gas of the energy-saving push boat type hydrogen reducing furnace is only 2/3 of the consumption of the hydrogen gas of the traditional hydrogen reducing furnace, so that the preparation cost of the metal powder is further reduced, and the market competitiveness of the metal powder prepared by the invention is further improved.
(3) The energy-saving push boat type hydrogen reduction furnace is provided with an upper layer of furnace tube and a lower layer of furnace tube, the heating element directly heats the second heating section, the temperature of the second heating section is 10-50 ℃ higher than that of the first heating section, namely the second heating section directly heats the first heating section in a heat transfer mode. In addition, the temperature of the pre-reduction in the first heating section is 450-800 ℃ and the temperature of the high-temperature reduction in the second heating section is 500-850 ℃ in the invention, which means that as long as the high-temperature reduction in the second heating section can be carried out, the second heating section has enough heat to transfer to the first heating section to ensure the pre-reduction reaction to be carried out. And practices show that compared with the traditional hydrogen reduction furnace, the energy-saving push boat type hydrogen reduction furnace has the advantages that the consumption of electric energy is reduced by 1/2, so that the preparation cost of metal powder is further reduced, and the market competitiveness of the metal powder prepared by the invention is improved.
(4) Compared with the traditional hydrogen reduction furnace, the length of the tube bodies of the upper layer of the furnace tube and the lower layer of the furnace tube and the length of the heating section in the energy-saving push boat type hydrogen reduction furnace are respectively shortened by half, so that the energy-saving push boat type hydrogen reduction furnace is more compact compared with the traditional hydrogen reduction furnace, and the floor area and the preparation cost of the energy-saving push boat type hydrogen reduction furnace are reduced.
(5) According to the invention, the cooling device is arranged on the lower layer furnace tube, and the obtained high-temperature metal powder is cooled by the cooling device, so that the cooling time of the metal powder prepared by the energy-saving push boat type hydrogen reduction furnace is shortened. On one hand, the problem that the metal powder is spontaneously combusted in the air due to the over-short cooling time and over-high temperature of the metal powder is avoided; on the other hand, the efficiency of producing metal powder by the energy-saving push boat type hydrogen reduction furnace is improved, and the preparation cost of the product metal powder is reduced. In addition, the air cooling device in the cooling device avoids the problem of safety generation caused by spontaneous combustion of the metal powder due to sudden cooling of the high-temperature metal powder; on the other hand, the method avoids the over-high oxygen content in the obtained metal powder and reduces the performance of the product.
Drawings
FIG. 1 is a first schematic structural diagram of the present invention;
FIG. 2 is a schematic diagram of a second embodiment of the present invention;
FIG. 3 is a third schematic structural view of the present invention;
FIG. 4 is a schematic structural view of a furnace body according to the present invention;
FIG. 5 is a schematic view of the transfer mechanism of the present invention;
FIG. 6 is a schematic structural view of a conventional hydrogen reduction furnace;
fig. 7 is an SEM image of iron powder prepared according to the present invention at different magnification ratios;
1-a first thrust machine, 2-a feed inlet, 3-an exhaust pipe, 4-an upper layer furnace tube, 5-a furnace body, 6-a heating element, 7-an air inlet tube, 8-a water cooling device, 9-a discharge port, 10-a material boat, 11-a second thrust machine, 12-a third thrust machine, 13-a platform, 14-a lower layer furnace tube, 15-a furnace pipe, 16-a heat preservation and insulation layer, 17-a transfer chamber, 18-a temperature detector, 19-a guide rail, 20-a heat insulation plate and 21-an air cooling device.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail and completely with reference to the accompanying drawings and embodiments of the present invention.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. The use of "first," "second," and similar terms in the description and claims of the present application do not denote any order, quantity, or importance, but rather are used to distinguish one element from another in various locations of the energy efficient hydrogen pushed boat reduction furnace of the present invention.
Example 1
As shown in fig. 1, the energy-saving hydrogen push boat type reduction furnace comprises a material boat 10, an upper layer furnace tube 4, a lower layer furnace tube 14, a furnace body 5, a transfer mechanism, an air inlet pipe 7, an air outlet pipe 3, a feed inlet 2, a discharge outlet 9, a heating element 6 and a cooling device. Specifically, an upper layer furnace tube 4 and a lower layer furnace tube 14 are arranged in parallel up and down and are positioned in a furnace body 5, wherein the upper layer furnace tube 4 comprises a first heating section, the lower layer furnace tube 14 comprises a second heating section and a cooling section, and the temperature of the second heating section is 10-50 ℃ higher than that of the first heating section; in practice, the upper furnace tube 4 and the lower furnace tube 14 each include at least one tube. The exhaust pipe 3 is connected to the upper layer furnace tube 4, the gas inlet pipe 7 is connected to the lower layer furnace tube 14, the gas introduced into the gas inlet pipe 7 in the actual production can be any gas with reducibility, in the embodiment, the gas introduced into the gas inlet pipe 7 is reduction H2. The feeding port 2 is arranged at one end of the upper layer furnace tube 4, the discharging port 9 is arranged on the lower layer furnace tube 14 and is positioned at the same end as the feeding port 2, and the feeding port 2 and the discharging port 9 are both positioned outside the furnace body 5; wherein, the material boat 10 containing the metal oxide enters the upper layer furnace tube 4 through the feeding hole 2 and is unloaded from the lower layer furnace tube 14 through the discharging hole 9. The transfer mechanism is connected with the other ends of the upper layer furnace tube 4 and the lower layer furnace tube 14 and is used for transferring the material boat in the upper layer furnace tube to the lower layer furnace tube and simultaneously forming a U-shaped material route for the upper layer furnace tube 4 and the lower layer furnace tube 14. The heating element 6 is arranged on the lower furnace tube 14 and directly heats the second heating section, and the second heating section heats the first heating section in a heat transfer mode, so that two different temperature ranges are formed on the upper furnace tube 4 and the lower furnace tube 14Enclosing a place for the metal oxide powder to carry out reduction reaction. In this embodiment, the heating element 6 is disposed at the bottom of the outer sidewall of the lower furnace tube 14 as the second heating section tube, and in addition, the heating element in this embodiment is a resistance heating element, and in practice, may also be other devices, combinations of devices, or other heating manners, such as a gas heating manner, which can play the same role; in addition, in practice, the heating element 6 can provide heat for the upper furnace tube and the lower furnace tube in other forms, such as being uniformly wound on the lower furnace tube 14 and the upper furnace tube 4, instead of being directly disposed at the bottom of the outer sidewall of the lower furnace tube 14.
As shown in fig. 1, in order to shorten the cooling time of the ultra-fine metal powder prepared by the energy-saving hydrogen push boat type reduction furnace and avoid the problem that the ultra-fine metal powder is self-ignited in the air due to the over-short cooling time and the over-high temperature of the ultra-fine metal powder, the energy-saving hydrogen push boat type reduction furnace in the embodiment is provided with a cooling device in the cooling section of the lower furnace tube 14, and the cooling device is located in the furnace body 5. The cooling device in this embodiment is a water cooling device 8, and preferably, the water cooling device 8 is a water cooling tank, and may be other devices, combinations of devices, or other cooling methods that perform the same function in an actual application process.
As shown in fig. 4, the furnace body 5 includes a furnace pipe 15 and a heat insulating layer 16. As shown in fig. 1, in order to prevent the heat supplied from the heating element 6 from affecting the cooling effect of the water cooling device 8 on the ultra-fine metal powder, a heat insulating plate 20 for dividing the furnace 15 into a heating zone and a cooling zone is provided in the furnace 15. Specifically, the upper layer furnace tube 4 and the lower layer furnace tube 14 are arranged in the furnace pipe 15 through the heat insulation plate 20, and heat insulation treatment is performed on gaps formed by the upper layer furnace tube 4, the lower layer furnace tube 14 and the heat insulation plate 20; the heating element 6 is positioned in the heating area, the air inlet pipe 7, the exhaust pipe 3 and the water cooling device 8 are positioned in the cooling area, the air inlet pipe 7 is connected to the pipe body of the lower-layer furnace pipe 14 positioned in the cooling area, and the exhaust pipe 3 is connected to the pipe body of the upper-layer furnace pipe 4 positioned in the cooling area; the discharge port 9 and the feed port 2 are both positioned outside the furnace pipe 15. Wherein, the first heating section of the upper layer furnace tube 4 and the second heating section of the lower layer furnace tube 14 are both located in the heating zone, and the cooling section of the lower layer furnace tube is located in the cooling zone.
As shown in fig. 1, in order to avoid thermal deformation of the upper furnace tube 4 outside the heating section, the cooling device is disposed on the upper furnace tube 4 in this embodiment, the cooling device in this embodiment is a water cooling device 8, preferably, the water cooling device 8 is a water cooling tank, and in an actual application process, other devices, combinations of devices, or other cooling methods that perform the same function may also be used.
As shown in fig. 1, in order to push the material boat 10 into the upper furnace tube 4 more conveniently, the energy-saving hydrogen boat-pushing reduction furnace in this embodiment further includes a first thrust machine 1 disposed to match the feeding port 2. The first thrust machine 1 in this embodiment is a hydraulic cylinder, a pneumatic cylinder or an electric screw thrust machine, and in practice, may be other devices or combinations of devices that perform the same function.
As shown in fig. 4, in order to facilitate monitoring of the temperatures in the upper layer furnace tube 4 and the lower layer furnace tube 14, a temperature detector 18 for monitoring the temperatures of the upper layer furnace tube 4 and the lower layer furnace tube 14 is provided on the heat insulating layer 16. In addition, in order to facilitate the movement of the material boat 10 in the tubes of the upper layer furnace tube 4 and the lower layer furnace tube 14, guide rails 19 for moving the material boat 10 are arranged in the tubes of the upper layer furnace tube 4 and the lower layer furnace tube 14.
As shown in fig. 5, the transfer mechanism in this embodiment includes a transfer chamber 17, a stage 13, a third thrust machine 12, and a second thrust machine 11. Specifically, the transfer chamber 17 is connected with the other ends of the upper layer furnace tube 4 and the lower layer furnace tube 14 and communicates the upper layer furnace tube 4 with the lower layer furnace tube 14 in a U shape, the platform 13 is arranged in the transfer chamber 17, the third thrust machine 12 is arranged on the bottom plate of the transfer chamber 17 and connected with the platform 13, and the second thrust machine 11 is arranged on the side wall of the transfer chamber 17. In this example, the third thrust unit 12 and the second thrust unit 11 are hydraulic cylinders, pneumatic cylinders or electric screw thrust units, and may be other devices or combinations of devices that can perform the same function. In the practical use process of the embodiment, the third thrust machine 12 drives the platform 13 to move upward to be parallel to the upper layer furnace tube 4, and the first thrust machine 1 simultaneously pushes the material boat 10 out of the upper layer furnace tube 4 and pushes the material boat 10 to the platform 13; then, the third thrust machine 12 drives the platform 13 to move downward to be parallel to the lower furnace tube 14, the second thrust machine 11 starts to extend, and simultaneously pushes the material boat positioned on the platform 13 into the tube of the lower furnace tube 14, thereby completing the transfer of the material boat 10 from the upper furnace tube 4 to the lower furnace tube 14, and simultaneously forming a U-shaped material route for the upper furnace tube 4 and the lower furnace tube 14.
Example 2
As shown in fig. 2, the energy-saving hydrogen push boat type reduction furnace includes a material boat 10, an upper layer furnace tube 4, a lower layer furnace tube 14, a furnace body 5, a transfer mechanism, an air inlet pipe 7, an air outlet pipe 3, a feed inlet 2, a discharge outlet 9, a heating element 6, and a cooling device. Specifically, the upper layer furnace tube 4 and the lower layer furnace tube 14 are arranged in parallel up and down, and part of tube bodies of the upper layer furnace tube 4 and the lower layer furnace tube 14 are arranged in the furnace body 5, wherein the upper layer furnace tube 4 comprises a first heating section, the lower layer furnace tube 14 comprises a second heating section and a cooling section, and the temperature of the second heating section is 10-50 ℃ higher than that of the first heating section; in practice, the upper furnace tube 4 and the lower furnace tube 14 each include at least one tube. The feeding port 2 is arranged at one end of the upper layer furnace tube 4, the discharging port 9 is arranged on the lower layer furnace tube 14 and is positioned at the same end as the feeding port 2, and the feeding port 2 and the discharging port 9 are both positioned outside the furnace body 5; wherein, the material boat 10 for containing metal oxide powder enters the upper layer furnace tube 4 through the feeding hole 2 and is unloaded from the lower layer furnace tube 14 through the discharging hole 9. The transfer mechanism is connected to the other ends of the upper layer furnace tube 4 and the lower layer furnace tube 14 and is used for transferring the material boat 10 in the upper layer furnace tube 4 to the lower layer furnace tube 14 and simultaneously forming a U-shaped material route for the upper layer furnace tube 4 and the lower layer furnace tube 14. The air inlet pipe 7 is connected to the lower layer furnace tube 14, and the exhaust pipe 3 is connected to the upper layer furnace tube 4; wherein, the air inlet pipe 7 and the air outlet pipe 3 are both positioned outside the furnace body 5; the gas introduced into the gas inlet pipe 7 in the actual production can be any gas with reducibility, and in the embodiment, the gas introduced into the gas inlet pipe 7 is reduction H2. The heating element 6 is arranged on the lower furnace tube 14 and directly heats the second heating section, and the second heating section heats the first heating section in a heat transfer mode, so that two places with different temperature ranges for the metal oxide powder to perform reduction reaction are formed. In the present embodiment, the heating elements 6 are disposed on the lower furnace tube 14A bottom portion of the outer sidewall; the heating element in this embodiment is a resistance heating element, and may be other devices, combinations of devices, or other heating methods, such as a gas heating method, which can perform the same function; in addition, in practice, the heating element 6 can provide heat for the upper furnace tube and the lower furnace tube in other forms, such as being uniformly wound on the lower furnace tube and the upper furnace tube, instead of being directly disposed on the outer sidewall of the lower furnace tube 14.
As shown in fig. 2, in order to shorten the cooling time of the ultrafine metal powder prepared by the energy-saving hydrogen push boat type reduction furnace and avoid the problem that the temperature of the ultrafine metal powder is too high and causes the ultrafine metal powder to self-ignite in the air due to too short cooling time, the energy-saving hydrogen push boat type reduction furnace in the embodiment is provided with a cooling device on the cooling section of the lower furnace tube 14, and the cooling device is located outside the furnace body 5; at this time, the first heating section of the upper layer furnace tube 4 and the second heating section of the lower layer furnace tube 14 are both located in the furnace body 5, and the cooling section of the lower layer furnace tube 14 is located outside the furnace body. The air inlet pipe 7 and the air outlet pipe 3 are both positioned between the cooling device and the furnace body 5. In addition, in order to avoid the upper furnace tube 4 outside the furnace body 5 from being deformed by heat, the cooling device is provided on the upper furnace tube 4 in the present embodiment.
The cooling device in this embodiment is a water cooling device 8, and preferably, the water cooling device 8 is a water cooling tank, and may be other devices, combinations of devices, or other cooling methods that perform the same function in an actual application process.
As shown in fig. 2, in order to push the material boat 10 into the upper furnace tube 4 more conveniently, the energy-saving hydrogen boat-pushing reduction furnace in this embodiment further includes a first thrust machine 1 disposed to match the feeding port 2. The first thrust machine 1 in this embodiment is a hydraulic cylinder, a pneumatic cylinder or an electric screw thrust machine, and in practice, may be other devices or combinations of devices that perform the same function.
As shown in fig. 4, the furnace body 5 in the energy-saving hydrogen push boat type reduction furnace includes a furnace pipe 15 and a heat insulating layer 16. Specifically, the first heating section and the second heating section are located in the furnace pipe 15, and the cooling section is located outside the furnace pipe 15; in order to reduce the heat loss provided by the heating element 6, the furnace pipe 15 is coated with a heat insulation layer 16. As shown in fig. 4, in order to facilitate monitoring of the temperatures in the upper layer furnace tube 4 and the lower layer furnace tube 14, a temperature detector 18 for monitoring the temperatures of the upper layer furnace tube 4 and the lower layer furnace tube 14 is provided on the heat insulating layer 16. In addition, in order to facilitate the movement of the material boat 10 in the tubes of the upper layer furnace tube 4 and the lower layer furnace tube 14, guide rails 19 for moving the material boat 10 are arranged in the tubes of the upper layer furnace tube 4 and the lower layer furnace tube 14.
As shown in fig. 5, the transfer mechanism in this embodiment includes a transfer chamber 17, a stage 13, a third thrust machine 12, and a second thrust machine 11. Specifically, the transfer chamber 17 is connected to the other ends of the upper layer furnace tube 4 and the lower layer furnace tube 14 and communicates the upper layer furnace tube 4 with the lower layer furnace tube 14 in a U shape, the platform 13 is arranged in the transfer chamber 17, the third thrust machine 12 is arranged on the bottom plate of the transfer chamber 17 and connected with the platform 13, and the second thrust machine 11 is arranged on the side wall of the transfer chamber 17. In this example, the third thrust machine 12 and the second thrust machine 11 are all hydraulic cylinders, pneumatic cylinders or electric screw thrust machines, and in practice, other devices and combinations of devices may also be used to perform the same function. In the actual use process, the third thrust machine 12 drives the platform 13 to move upwards to be parallel to the upper layer furnace tube 4, and the first thrust machine 1 simultaneously pushes the material boat 10 out of the upper layer furnace tube 4 and pushes the material boat 10 to the platform 13; then, the third thrust machine 12 drives the platform 13 to move downward to be parallel to the lower furnace tube 14, the second thrust machine 11 starts to extend, and simultaneously pushes the material boat positioned on the platform 13 into the tube of the lower furnace tube 14, thereby completing the transfer of the material boat 10 from the upper furnace tube 4 to the lower furnace tube 14, and simultaneously forming a U-shaped material route for the upper furnace tube 4 and the lower furnace tube 14.
Example 3
As shown in fig. 3, the energy-saving hydrogen push boat type reduction furnace includes a material boat 10, an upper layer furnace tube 4, a lower layer furnace tube 14, a furnace body 5, a transfer mechanism, an air inlet pipe 7, an air outlet pipe 3, a feed inlet 2, a discharge outlet 9, a heating element 6, and a cooling device. Specifically, the upper layer furnace tube 4 and the lower layer furnace tube 14 are arranged in parallel up and down, and part of the tube bodies of the upper layer furnace tube 4 and the lower layer furnace tube 14 are arranged in the furnace body 5, wherein the upper layer furnace tube 4 comprises a first heating section, and the lower layer furnace is arranged in parallelThe tube 14 comprises a second heating section and a cooling section, and the temperature of the second heating section is 10-50 ℃ higher than the temperature of the first heating section; in practice, the upper furnace tube 4 and the lower furnace tube 14 each include at least one tube. The feeding port 2 is arranged at one end of the upper layer furnace tube 4, the discharging port 9 is arranged on the lower layer furnace tube 14 and is positioned at the same end as the feeding port 2, and the feeding port 2 and the discharging port 9 are both positioned outside the furnace body 5; wherein, the material boat 10 for containing metal oxide enters the upper layer furnace tube 4 through the feeding hole 2 and is unloaded from the lower layer furnace tube 14 through the discharging hole 9. The transfer mechanism is connected to the other ends of the upper layer furnace tube 4 and the lower layer furnace tube 14 and is used for transferring the material boat 10 in the upper layer furnace tube 4 to the lower layer furnace tube 14 and simultaneously forming a U-shaped material route for the upper layer furnace tube 4 and the lower layer furnace tube 14. The air inlet pipe 7 is connected to the lower layer furnace tube 14, and the exhaust pipe 3 is connected to the upper layer furnace tube 4; wherein, the air inlet pipe 7 and the air outlet pipe 3 are both positioned outside the furnace body 5; the gas introduced into the gas inlet pipe 7 in the actual production can be any gas with reducibility, and in the embodiment, the gas introduced into the gas inlet pipe 7 is reduction H2. The heating element 6 is arranged on the lower furnace tube 14 and directly heats the second heating section, and the second heating section heats the first heating section in a heat transfer mode, so that two places with different temperature ranges for the metal oxide powder to perform reduction reaction are formed. In the present embodiment, the heating element 6 is disposed at the bottom of the outer sidewall of the lower furnace tube 14; the heating element in this embodiment is a resistance heating element, and may be other devices, combinations of devices, or other heating methods, such as a gas heating method, which can perform the same function; in addition, in practice, the heating element 6 can provide heat for the upper furnace tube and the lower furnace tube in other forms, such as being uniformly wound on the lower furnace tube and the upper furnace tube, instead of being directly disposed on the outer sidewall of the lower furnace tube 14.
As shown in fig. 3, in order to shorten the cooling time of the ultrafine metal powder prepared by the energy-saving hydrogen push boat type reduction furnace and avoid the problem that the temperature of the ultrafine metal powder is too high and causes the ultrafine metal powder to self-ignite in the air due to too short cooling time, the energy-saving hydrogen push boat type reduction furnace in the embodiment is sleeved with a cooling device in the cooling section of the lower furnace tube 14, and the cooling device is located outside the furnace body 5; the first heating section of the upper layer furnace tube 4 and the second heating section of the lower layer furnace tube 14 are both located in the furnace body 5, and the cooling section of the lower layer furnace tube 14 is located outside the furnace body. The cooling device in the embodiment includes an air cooling device 21 and a water cooling device 8, which are sequentially arranged along the moving direction of the material boat 10 in the lower furnace tube 14 and used for cooling the cooling section of the lower furnace tube 14, wherein the water cooling device 8 is arranged on the lower furnace tube 14. In this embodiment, the water cooling device 8 is preferably a water cooling tank; the air cooling device 21 is preferably an electric fan, and in the embodiment, the electric fan accelerates the air flow around the tube body of the lower furnace tube 14 between the furnace body 5 and the water cooling device 8, so as to cool the high-temperature ultrafine metal powder coming out of the second heating section; in the actual production process, the air cooling device 21 can be deactivated along with the change of the external environment temperature, and the tube body of the lower furnace tube 14 between the furnace body 5 and the water cooling device 8 is directly cooled by the external environment. But in practice it may be other devices, combinations of devices or other cooling means that serve the same purpose.
In addition, in order to avoid the upper furnace tube 4 outside the furnace body 5 from being deformed by heat, the cooling device is provided on the upper furnace tube 4 in this embodiment, the cooling device in this embodiment is a water cooling device 8, preferably, the water cooling device 8 is a water cooling tank, and in an actual application process, other devices, combinations of devices, or other cooling methods that play the same role may also be used.
As shown in fig. 3, in order to push the material boat 10 into the upper furnace tube 4 more conveniently, the energy-saving hydrogen boat-pushing reduction furnace in this embodiment further includes a first pushing machine 1 disposed to match the feeding port 2. The first thrust machine 1 in this embodiment is a hydraulic cylinder, a pneumatic cylinder or an electric screw thrust machine, and in practice, may be other devices or combinations of devices that perform the same function.
As shown in fig. 4, the furnace body 5 in the energy-saving hydrogen push boat type reduction furnace includes a furnace pipe 15 and a heat insulating layer 16. Specifically, the first heating section and the second heating section are located in the furnace pipe 15, and the cooling section is located outside the furnace pipe 15; in order to reduce the heat loss provided by the heating element 6, the furnace pipe 15 is coated with a heat insulation layer 16. As shown in fig. 4, in order to facilitate monitoring of the temperatures in the upper layer furnace tube 4 and the lower layer furnace tube 14, a temperature detector 18 for monitoring the temperatures of the upper layer furnace tube 4 and the lower layer furnace tube 14 is provided on the heat insulating layer 16. In addition, in order to facilitate the movement of the material boat in the tubes of the upper furnace tube 4 and the lower furnace tube 14, guide rails 19 are arranged in the tubes of the upper furnace tube 4 and the lower furnace tube 14.
As shown in fig. 5, the transfer mechanism in this embodiment includes a transfer chamber 17, a stage 13, a third thrust machine 12, and a second thrust machine 11. Specifically, the transfer chamber 17 is connected to the other ends of the upper layer furnace tube 4 and the lower layer furnace tube 14 and communicates the upper layer furnace tube 4 with the lower layer furnace tube 14 in a U shape, the platform 13 is arranged in the transfer chamber 17, the third thrust machine 12 is arranged on the bottom plate of the transfer chamber 17 and connected with the platform 13, and the second thrust machine 11 is arranged on the side wall of the transfer chamber 17. In this example, the third thrust machine 12 and the second thrust machine 11 are all hydraulic cylinders, pneumatic cylinders or electric screw thrust machines, and in practice, other devices and combinations of devices may also be used to perform the same function. In the actual use process, the third thrust machine 12 drives the platform 13 to move upwards to be parallel to the upper layer furnace tube 4, and the first thrust machine 1 simultaneously pushes the material boat 10 out of the upper layer furnace tube 4 and pushes the material boat 10 to the platform 13; then, the third thrust machine 12 drives the platform 13 to move downward to be parallel to the lower furnace tube 14, the second thrust machine 11 starts to extend, and simultaneously pushes the material boat positioned on the platform 13 into the tube of the lower furnace tube 14, thereby completing the transfer of the material boat 10 from the upper furnace tube 4 to the lower furnace tube 14, and simultaneously forming a U-shaped material route for the upper furnace tube 4 and the lower furnace tube 14.
Example 4
On the basis of embodiment 1, embodiment 2 or embodiment 3, this embodiment further illustrates a method for using the energy-saving hydrogen push boat reduction furnace to prepare ultrafine metal powder, which specifically includes the following steps:
step 1: firstly, metal oxide powder is placed in a material boat, the material boat is pushed into an upper layer furnace tube by starting a first pushing machine, and the metal oxide powder in the material boat and hydrogen from a lower layer furnace tube generate pre-reduction reaction in a first heating section.
Step 2: and when the material boat is pushed out from the first heating section, starting a third thrust machine to lift the platform to be parallel to the upper-layer furnace tube, pushing the material boat to the platform by the first thrust machine, then lowering the platform to be parallel to the lower-layer furnace tube under the action of the third thrust machine, and simultaneously starting a second thrust machine to push the material boat into the second heating section of the lower-layer furnace tube.
And step 3: after entering the second heating section, the material boat and the hydrogen entering from the air inlet pipe are subjected to high-temperature reduction reaction to obtain high-temperature ultrafine metal powder after full reaction, and unreacted hydrogen and water vapor generated by the reduction reaction enter the upper furnace tube through the transfer chamber.
And 4, step 4: and (3) pushing the superfine metal powder with higher temperature obtained in the step (3) out of the second heating section by a second pushing machine, cooling the reduced metal powder by a cooling device to obtain the superfine metal powder, and unloading the obtained superfine metal powder from a discharge port along with the material boat.
Example 5
The energy-saving push boat type hydrogen reduction furnace described in example 3 is used to prepare metal powder, and the preparation method of the metal powder specifically includes the following steps:
step 1:
placing the metal oxide powder in a first heating zone, and reducing the metal oxide powder in the first heating zone2Pre-reduction takes place. Wherein the particle size of the metal oxide powder is 1-2 μm, and the pre-reduction temperature is 450-800 ℃.
Step 2
Placing the metal oxide powder pre-reduced in the step 1 in a second heating section, and reducing H in the second heating section2And carrying out high-temperature reduction to obtain high-temperature metal powder after the reaction is finished. Wherein after the initial reaction, the remaining reduced H is reduced at a high temperature2And carrying out pre-reduction reaction with the metal oxide powder in the first heating section, wherein the high-temperature reduction temperature is 500-850 ℃.
Step 3
And (3) placing the high-temperature metal powder obtained by the high-temperature reduction in the step (2) in a cooling section to cool the high-temperature metal powder, contacting the high-temperature metal powder with passivation gas in the initial cooling section to passivate the surface of the high-temperature metal powder, and further cooling and separating the passivated metal powder to obtain the metal powder with the particle size of 1-25 mu m. Wherein the passivation gas is air.
Iron powder was prepared by the method described in this example, and the unseparated iron powder was scanned by a Scanning Electron Microscope (SEM), and the results are shown in fig. 7.
The foregoing is only a partial embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A method for preparing metal powder is characterized in that metal oxide powder is firstly subjected to pre-reduction and high-temperature reduction with reducing gas in sequence to obtain high-temperature metal powder, and then the high-temperature metal powder is cooled to obtain metal powder with the average particle size of 1-25 mu m; the high-temperature metal powder is passivated with passivation gas at the beginning of cooling so as to generate a protective layer on the surface of the high-temperature metal powder; the residual reducing gas after high-temperature reduction and the metal oxide powder are subjected to pre-reduction.
2. The method of claim 1, wherein the reducing gas is H2(ii) a The temperature of the pre-reduction is 450-800 ℃; the temperature of the high-temperature reduction is 500-850 ℃; the time of the pre-reduction and the high-temperature reduction of the metal oxide powder is 8-18h in total.
3. An energy-saving push boat type hydrogen reduction furnace for producing the metal powder according to claim 1 or 2, characterized by comprising an upper layer furnace tube (4), a lower layer furnace tube (14), a transfer mechanism, a heating element (6);
the upper layer furnace tube (4) comprises a first heating section, wherein the upper layer furnace tube (4) is used for feeding and is used for pre-reducing metal oxide powder in the first heating section under the cooperation of the heating element (6);
the lower furnace tube (14) comprises a second heating section and a cooling section, wherein the lower furnace tube (14) is used for discharging the cooled metal powder and passivating and cooling the high-temperature metal powder in the cooling section; the metal oxide powder is subjected to high-temperature reduction in a second heating section by matching with the heating element (6); wherein, the heating element (6) directly heats the second heating section of the lower furnace tube (14);
the transfer mechanism is used for transferring the pre-reduced metal oxide powder into the lower furnace tube (14);
wherein the temperature of the second heating section is 10-50 ℃ higher than the temperature of the first heating section.
4. The energy-saving push boat type hydrogen reduction furnace for producing metal powder as claimed in claim 3, further comprising a furnace body (5) for placing the tube bodies of the upper furnace tube (4) and the lower furnace tube (14), wherein the boat (10) is movable in the upper furnace tube (4) and the lower furnace tube (14) for holding metal oxide powder and providing H for pre-reduction and high temperature reduction2And an inlet pipe (7) connected to the lower furnace tube (14) for discharging gas and unreacted H generated during the high-temperature reduction and pre-reduction processes2The exhaust pipe (3) is connected with the upper layer furnace tube (4), and the cooling device is arranged on the lower layer furnace tube (14); wherein, the material boat (10) containing the metal oxide powder is transferred to the lower furnace tube (14) from the upper furnace tube (4) by the transfer mechanism.
5. The push boat type hydrogen reducing furnace of claim 4, wherein when the cooling means is located outside the furnace body (5), a first heating section for pre-reducing the metal oxide powder and a second heating section for high-temperature reducing the metal oxide powder are located in the furnace body (5), and the gas inlet pipe (7) and the gas outlet pipe (3) are located outside the furnace body (5).
6. An energy-saving push boat type hydrogen reducing furnace for producing metal powder according to claim 5, wherein said cooling means is a water cooling means (8) provided on a cooling section of said lower furnace tube (14).
7. An energy-saving push boat type hydrogen reducing furnace for producing metal powder according to claim 5, wherein the cooling means comprises an air cooling means (21) and a water cooling means (8) which are provided in this order along the direction of movement of the material boat (10) in the lower furnace tube (14) and which are used for cooling the metal powder in a high temperature state which has moved to the cooling zone; wherein, the water cooling device (8) is arranged on the cooling section of the lower furnace tube (14).
8. The energy-saving push boat type hydrogen reduction furnace for preparing metal powder according to claim 6 or 7, wherein the transfer mechanism comprises a transfer chamber (17) connected to the other end of the upper layer furnace tube (4) and the lower layer furnace tube (14) and communicating the upper layer furnace tube (4) and the lower layer furnace tube (14) in a U shape, a platform (13) arranged in the transfer chamber (17) and used for placing the material boat (10), a third thrust machine (12) arranged on the bottom plate of the transfer chamber (17) and connected with the platform (13), and a second thrust machine (11) arranged on the side wall of the transfer chamber (17) and used for pushing the material boat (10) on the platform (13) into the lower layer furnace tube (14).
9. An energy-saving push boat type hydrogen reducing furnace for producing metal powder according to claim 8, wherein said furnace body (5) comprises a furnace pipe (15) for placing a first heating section of said upper layer furnace tube (4) and a second heating section of said lower layer furnace tube (14), and a heat insulating layer (16) covering said furnace pipe (15).
10. The energy-saving push boat type hydrogen reduction furnace for preparing metal powder according to claim 9, further comprising a temperature detector (18) disposed on the heat insulating layer (16) for monitoring the temperature of the upper layer furnace tube (4) and the lower layer furnace tube (14), a first pusher (1) disposed in match with the feed port (2) for pushing the material boat (10) into the upper layer furnace tube (4), a guide rail (19) disposed in the tubes of the upper layer furnace tube (4) and the lower layer furnace tube (14) for moving the material boat (10), and a cooling device disposed on the upper layer furnace tube (4).
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