CN114672818A - Method for preparing iron-aluminum-silicon carbide composite material by utilizing red mud - Google Patents

Method for preparing iron-aluminum-silicon carbide composite material by utilizing red mud Download PDF

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CN114672818A
CN114672818A CN202210304321.5A CN202210304321A CN114672818A CN 114672818 A CN114672818 A CN 114672818A CN 202210304321 A CN202210304321 A CN 202210304321A CN 114672818 A CN114672818 A CN 114672818A
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electrolysis
red mud
cathode
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李慧
梁精龙
付玉田
李昊天
杨宇
刘畅
严红燕
曹卫刚
张利芳
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North China University of Science and Technology
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Abstract

The invention belongs to the technical field of fused salt electrolysis, and particularly discloses a method for preparing an iron-aluminum-silicon carbide composite material by using red mudThe method comprises the following steps which are carried out in sequence: preparation of NaCl-CaCl2Melting a salt; preparing red mud cathode, preparing graphite anode, putting the red mud cathode and the graphite anode into NaCl-CaCl2Carrying out molten salt electrolysis on the molten salt; and after the electrolysis is finished, quickly taking out the electrolysis product, cooling, cleaning and drying to obtain the iron-aluminum-silicon carbide composite material. The preparation method of the invention does not need acid-base solution, has simple process equipment, lower energy consumption and production cost, is environment-friendly and has little harm to human body. The preparation method is suitable for preparing the iron-aluminum-silicon carbide composite material.

Description

Method for preparing iron-aluminum-silicon carbide composite material by utilizing red mud
Technical Field
The invention belongs to the technical field of fused salt electrolysis, and particularly relates to a method for preparing an iron-aluminum-silicon carbide composite material by utilizing red mud.
Background
Red mud is industrial solid waste discharged during extraction of alumina in the aluminum industry, and is called red mud because of its large iron oxide content and appearance similar to red clay. Red mud is an insoluble residue that can be divided into sintering process red mud, bayer process red mud, and combination process red mud.
China can generate a large amount of red mud every year, but the utilization rate of the red mud is low, and hundreds of millions of tons of red mud are accumulated. A large amount of red mud is stored in a damming way, land resources are occupied, and alkaline exudate and dust can pollute surrounding water sources and air and become a great potential safety hazard for the health of nearby residents. At present, the method for largely utilizing the red mud mainly utilizes the red mud integrally, such as the method for integrally preparing building materials, the method for using the red mud as an adsorbent and the like. However, in the process of integrally utilizing the red mud, a large amount of components containing valuable elements in the red mud are not utilized. Therefore, with the continuous development of metallurgical technology, a process technology for recovering and extracting valuable elements in the red mud is continuously provided in order to make the best use of the red mud. The technical difficulty and the treatment cost of valuable metal recovery are increased due to complex components of the red mud and high impurity content, and the conventional extraction process of valuable elements in the red mud mainly focuses on the enrichment of single metal, so that systematic recovery of various elements in the red mud is difficult to realize, and the recovery of the valuable metals in the red mud is incomplete, and the low-grade metal recovery economy is poor. Therefore, the development of a technology for recovering valuable metals more efficiently and the enhancement of the related research on the systematic extraction of various valuable metals in the red mud are the key to realizing the resource utilization of the red mud in the future.
Disclosure of Invention
The invention aims to provide a method for preparing an iron-aluminum-silicon carbide composite material by utilizing red mud, which realizes the recycling of valuable metals in the red mud by a molten salt electro-deoxidation technology.
In order to achieve the purpose, the technical method comprises the following steps:
s1, adding NaCl and CaCl2Mixing according to a molar ratio of 1:1, drying, transferring into a tube furnace, keeping the temperature, raising the temperature in the tube furnace, and adding CaCl2Melting the NaCl mixed salt to obtain NaCl-CaCl2Melting a salt;
s2, preparing a cathode from the red mud, preparing an anode from the graphite, connecting the cathode and the anode through a stainless steel rod, and placing the red mud cathode and the graphite anode into NaCl-CaCl in a reactor2Electrolysis is carried out in molten salt;
and S3, after the electrolysis is finished, quickly taking out the electrolysis product, immersing the electrolysis product and the conductor bar into deionized water to quickly cool the electrolysis product and the conductor bar, continuously washing off residual salt on the surface of the electrode by using the deionized water, taking down the electrolysis product from the stainless steel bar, washing and drying to obtain the iron-aluminum-silicon-carbide composite material.
As a limitation: in the step S1, the drying temperature is 150-250 ℃, the drying time is more than 8h, the heat preservation temperature is 300-500 ℃, the heat preservation time is more than 4h, and the temperature in the tubular furnace is increased to 800-900 ℃.
As a further limitation: step S1 obtaining NaCl-CaCl2After melting the salt, NaCl-CaCl is needed2Pre-electrolyzing fused salt, specifically: using a stainless steel rod as a cathode, graphite as an anode, connecting the cathode and the anode through the stainless steel rod, and inserting NaCl-CaCl into the cathode and the anode2Pre-electrolysis is carried out in molten salt for more than 6h under the electrolysis voltage of 2.8V, and then the stainless steel bar cathode and the graphite anode are taken out.
As yet a further limitation: in the step S2, the reactor is sealed by a plug with a rubber tube, and the distance between the red mud cathode and the graphite anode is 1.8 cm; the electrolytic process is as follows: under the condition of 800-900 ℃, the electrolysis is carried out by adopting constant voltage electrolysis or adopting a staged voltage electrolysis mode, the voltage of the constant voltage electrolysis is 3.1-3.2V, and the electrolysis time is 10-12 h; carrying out first-stage electrolysis by adopting staged voltage electrolysis, and then carrying out second-stage electrolysis, wherein the voltage of the first-stage electrolysis is 2.4V, the electrolysis time is 4h, the voltage of the second-stage electrolysis is 3.1V-3.2V, and the electrolysis time is 8 h; and continuously introducing argon into the closed reactor in the electrolysis process, and discharging carbon monoxide or carbon dioxide generated in the electrolysis process along with the argon through the rubber tube.
As another limitation: the red mud cathode preparation process in the step S2 is as follows: ball-milling and crushing the red mud, pressing by using a press to obtain a cylindrical sample with the diameter of 15mm and the thickness of 2mm, sintering the cylindrical sample in a tubular furnace, taking out the sintered cylindrical sample, and connecting the sintered cylindrical sample with a lead collector to obtain a red mud cathode;
the preparation process of the graphite anode comprises the following steps: polishing 10mm × 5mm × 100mm graphite flakes on 1000#, 1500# and 2000# abrasive paper in sequence, cleaning the surfaces of the graphite flakes with deionized water and ethanol for more than 3 times in ultrasonic waves to remove graphite powder and grease adsorbed on the surfaces of the graphite flakes, then placing the graphite flakes in a vacuum drying oven to dry for more than 4 hours at the temperature of 150 ℃, drilling holes with the diameter of 1mm at one end of the graphite flakes, and connecting the graphite flakes with stainless steel conductor bars with the diameter of 5mm by passing nickel wires with the diameter of 1mm through the holes at one end of the graphite flakes to obtain the graphite anode.
As a further limitation: the pressure of the pressing machine is 8-10 Mpa, the pressing time is 150-250 s, the heating rate of the tube furnace is 3-5 ℃/min, the sintering temperature is 900-1100 ℃, and the sintering time is 2-4 h.
As a final definition: in the step S3, the cleaning mode is to clean for 1h in ultrasonic wave by adopting deionized water, the drying temperature is 150-250 ℃, and the drying time is more than 4 h.
Due to the adoption of the scheme, compared with the prior art, the invention has the beneficial effects that:
according to the method for preparing the iron-aluminum-silicon carbide composite material by using the red mud, the mechanical strength of the red mud is increased by sintering the red mud, and the sintered red mud is used as a cathode, so that the collection of a cathode product after the electrolysis is finished is facilitated; the contact area of the reaction can be increased in the electrolytic process, which is beneficial to the rapid reaction; after sintering, the red mud phase is changed, which is beneficial to electrochemical reduction; the sintered red mud cathode solid has certain porosity, and has positive influence on the electrolysis process and the current efficiency; in addition, the method does not need to use acid-base solution, has simple process equipment, lower energy consumption and production cost, is environment-friendly and has little harm to human bodies.
The preparation method is suitable for preparing the iron-aluminum-silicon carbide composite material.
Drawings
The invention is described in further detail below with reference to the figures and the embodiments.
FIG. 1 is a physical diagram of sintered red mud of examples 1 to 6 of the present invention;
FIG. 2 is an XRD spectrum of red mud before sintering in example 3 of the present invention;
FIG. 3 is an XRD spectrum of the red mud after sintering in example 3 of the present invention;
FIG. 4 is SEM images of red mud before and after sintering in example 3 of the present invention;
FIG. 5 is a graph showing the change in potential during electrolysis with a stepwise voltage in example 3 of the present invention;
FIG. 6 is an XRD spectrum of the iron-aluminum-silicon carbide composite material obtained in example 3 of the present invention;
FIG. 7 is an XRD spectrum of the Fe-Al-Si-SiC composite material obtained in example 2 of the present invention.
Detailed Description
The present invention is further described with reference to the following examples, but it should be understood by those skilled in the art that the present invention is not limited to the following examples, and any modifications and equivalent changes based on the specific examples of the present invention are within the scope of the claims of the present invention.
Examples 1 to 6A method for preparing an iron-aluminum-silicon carbide composite material from red mud
A method for preparing an iron-aluminum-silicon carbide composite material by utilizing red mud is disclosed, wherein the technological parameters in the preparation process are shown in Table 1, and the preparation method comprises the following steps of:
s1, adding NaCl and CaCl2Mixing the components according to the molar ratio of 1:1, placing the mixture into a clean and dry corundum crucible, drying the mixture in a vacuum drying oven at the temperature of between 150 and 250 ℃ for more than 8 hours, taking the dried mixture out, quickly transferring the dried mixture into a tubular furnace, preserving the heat at the temperature of between 300 and 500 ℃ for more than 4 hours, raising the temperature in the tubular furnace, and when the temperature in the tubular furnace reaches between 800 and 900 ℃, adding CaCl2Fully melting the NaCl mixed salt to obtain NaCl-CaCl2Melting a salt; for NaCl-CaCl2Pre-electrolyzing the molten salt, specifically: using a stainless steel rod as a cathode, graphite as an anode, connecting the cathode and the anode through the stainless steel rod, and inserting NaCl-CaCl into the cathode and the anode2Pre-electrolyzing for more than 6h in molten salt under the electrolytic voltage of 2.8V, and taking out the stainless steel rod cathode and the graphite anode;
s2, preparing a cathode from the red mud, preparing an anode from the graphite, connecting the cathode and the anode through a stainless steel rod, and placing the red mud cathode and the graphite anode into NaCl-CaCl in a reactor2In molten salt, the reactor is sealed by a plug with a rubber tube, the distance between the red mud cathode and the graphite anode is 1.8cm, electrolysis is carried out by adopting constant voltage electrolysis or by adopting a staged voltage electrolysis mode at the temperature of 800-900 ℃, the voltage of the constant voltage electrolysis is 3.1-3.2V, and the electrolysis time is 3.1-3.2V10h-12 h; carrying out first-stage electrolysis by adopting staged voltage electrolysis, and then carrying out second-stage electrolysis, wherein the voltage of the first-stage electrolysis is 2.4V, the electrolysis time is 4h, the voltage of the second-stage electrolysis is 3.1V-3.2V, and the electrolysis time is 8 h; continuously introducing argon into the closed reactor in the electrolysis process, and discharging carbon monoxide or carbon dioxide generated in the electrolysis process through a rubber tube along with the argon;
and S3, after the electrolysis is finished, quickly taking out the electrolysis product, immersing the electrolysis product and the conductor bar into deionized water to quickly cool the electrolysis product, continuously washing the residual salt on the surface of the electrode by using the deionized water, taking down the electrolysis product from the stainless steel bar, washing the electrolysis product for 1h by using the deionized water in ultrasonic waves, and drying the electrolysis product for more than 4h at the temperature of 150-250 ℃ to obtain the iron-aluminum-silicon carbide composite material.
The specific process for manufacturing the red mud cathode comprises the following steps: ball-milling and crushing the red mud, pressing the crushed red mud for 150-250 s by a press machine under the pressure of 8-10 Mpa to obtain a cylindrical sample with the diameter of 15mm and the thickness of 2mm, putting the cylindrical sample into a tubular furnace, heating the cylindrical sample to 900-1100 ℃ at the heating rate of 3-5 ℃/min, sintering the cylindrical sample for 2-4 h, taking out the cylindrical sample, and connecting the cylindrical sample with a lead current collector to obtain a red mud cathode;
the specific process for manufacturing the graphite anode comprises the following steps: sequentially polishing 10mm multiplied by 5mm multiplied by 100mm graphite flakes through 1000#, 1500# and 2000# abrasive paper, cleaning the surfaces of the graphite flakes with deionized water and ethanol for more than 3 times in ultrasonic waves to remove graphite powder and grease adsorbed on the surfaces of the graphite flakes, then placing the graphite flakes in a vacuum drying oven to be dried for more than 4 hours at the temperature of 150 ℃, drilling holes with the diameter of 1mm at one end of the graphite flakes, and connecting the graphite flakes with stainless steel conductor bars with the diameter of 5mm by passing nickel wires with the diameter of 1mm through the holes at one end of the graphite flakes to obtain the graphite anode.
Table 1 examples 1-6 process parameters during the preparation of iron-aluminum-silicon-carbide composites
Figure BDA0003564260590000051
Table 2 examples 1-6 process parameters in the preparation of red mud cathodes
Figure BDA0003564260590000052
Figure BDA0003564260590000061
The red mud after sintering in examples 1 to 6 is shown in fig. 1, the red mud before sintering in example 3 is shown in fig. 2, the red mud after sintering is shown in fig. 3, the red mud before sintering in example 3 is shown in fig. 4(a), the red mud after sintering is shown in fig. 4(b), the red mud before sintering and the red mud after sintering in other examples are similar to those in example 3, and are not repeated herein, surface water and bound water after sintering the red mud can be completely removed, so that the red mud phase is changed, the phase composition is stable, the mechanical strength of the red mud is increased, and the collection of cathode products after electrochemical reduction and electrolysis is facilitated; the sintered red mud has certain porosity, has positive influence on the electrolysis process and the current efficiency, can increase the contact area of the reaction in the electrolysis process, and is beneficial to the rapid reaction.
Example 3 the potential change in the stepwise voltage electrolysis process is shown in fig. 5, and the physical properties of the obtained fe-al-si-sic composite material were analyzed by an X-ray diffractometer to obtain the XRD pattern shown in fig. 6. Example 2 electrolysis was performed by constant voltage electrolysis, and physical properties of the obtained iron-aluminum-silicon carbide composite material were analyzed by an X-ray diffractometer, so as to obtain an XRD spectrum shown in fig. 7. The XRD patterns of the iron-aluminum-silicon carbide composite materials prepared in examples 1 and 5 are similar to those of the iron-aluminum-silicon carbide composite material prepared in example 2, and the XRD patterns of the iron-aluminum-silicon carbide composite materials prepared in examples 4 and 6 are similar to those of the iron-aluminum-silicon carbide composite material prepared in example 3, which are not repeated herein.

Claims (8)

1. A method for preparing an iron-aluminum-silicon carbide composite material by utilizing red mud is characterized by comprising the following steps of:
s1, adding NaCl and CaCl2Mixing according to a molar ratio of 1:1, drying, transferring into a tube furnace, keeping the temperature, raising the temperature in the tube furnace, and adding CaCl2Melting the NaCl mixed salt to obtain NaCl-CaCl2Melting a salt;
s2, preparing a cathode from the red mud, preparing an anode from the graphite, connecting the cathode and the anode through a stainless steel rod, and placing the red mud cathode and the graphite anode into NaCl-CaCl in a reactor2Electrolysis is carried out in molten salt;
and S3, after the electrolysis is finished, quickly taking out the electrolysis product, immersing the electrolysis product and the conductor bar into deionized water to quickly cool the electrolysis product and the conductor bar, continuously washing off residual salt on the surface of the electrode by using the deionized water, taking down the electrolysis product from the stainless steel bar, washing and drying to obtain the iron-aluminum-silicon-carbide composite material.
2. The method for preparing the iron-aluminum-silicon carbide composite material by using the red mud as claimed in claim 1, wherein the drying temperature in the step S1 is 150 ℃ to 250 ℃, the drying time is more than 8h, the heat preservation temperature is 300 ℃ to 500 ℃, the heat preservation time is more than 4h, and the temperature in the tubular furnace is raised to 800 ℃ to 900 ℃.
3. The method for preparing iron-aluminum-silicon-carbide composite material by using red mud as claimed in claim 1 or 2, wherein the NaCl-CaCl obtained in step S12After melting the salt, NaCl-CaCl is needed2Pre-electrolyzing fused salt, specifically: using a stainless steel rod as a cathode, graphite as an anode, connecting the cathode and the anode through the stainless steel rod, and inserting NaCl-CaCl into the cathode and the anode2Pre-electrolysis is carried out in molten salt for more than 6h under the electrolysis voltage of 2.8V, and then the stainless steel bar cathode and the graphite anode are taken out.
4. The method for preparing the iron-aluminum-silicon carbide composite material by using the red mud as claimed in claim 1 or 2, wherein the reactor is sealed by a plug with a rubber tube in step S2, and the distance between the red mud cathode and the graphite anode is 1.8 cm; the electrolytic process is as follows: under the condition of 800-900 ℃, the electrolysis is carried out by adopting constant voltage electrolysis or adopting a staged voltage electrolysis mode, the voltage of the constant voltage electrolysis is 3.1-3.2V, and the electrolysis time is 10-12 h; carrying out first-stage electrolysis by adopting staged voltage electrolysis, and then carrying out second-stage electrolysis, wherein the voltage of the first-stage electrolysis is 2.4V, the electrolysis time is 4h, the voltage of the second-stage electrolysis is 3.1V-3.2V, and the electrolysis time is 8 h; and continuously introducing argon into the closed reactor in the electrolysis process, and discharging carbon monoxide or carbon dioxide generated in the electrolysis process along with the argon through the rubber tube.
5. The method for preparing the iron-aluminum-silicon carbide composite material by using the red mud as claimed in claim 3, wherein the reactor is sealed by a plug with a rubber tube in the step S2, and the distance between the red mud cathode and the graphite anode is 1.8 cm; the electrolytic process is as follows: under the condition of 800-900 ℃, the electrolysis is carried out by adopting constant voltage electrolysis or adopting a staged voltage electrolysis mode, the voltage of the constant voltage electrolysis is 3.1-3.2V, and the electrolysis time is 10-12 h; carrying out first-stage electrolysis by adopting staged voltage electrolysis, and then carrying out second-stage electrolysis, wherein the voltage of the first-stage electrolysis is 2.4V, the electrolysis time is 4h, the voltage of the second-stage electrolysis is 3.1V-3.2V, and the electrolysis time is 8 h; and continuously introducing argon into the closed reactor in the electrolysis process, and discharging carbon monoxide or carbon dioxide generated in the electrolysis process along with the argon through the rubber tube.
6. The method for preparing the iron-aluminum-silicon carbide composite material by using the red mud according to any one of claims 1, 2 and 5, wherein the red mud cathode preparation process in the step S2 is as follows: ball-milling and crushing the red mud, pressing by using a press to obtain a cylindrical sample with the diameter of 15mm and the thickness of 2mm, sintering the cylindrical sample in a tubular furnace, taking out the sintered cylindrical sample, and connecting the sintered cylindrical sample with a lead collector to obtain a red mud cathode;
the preparation process of the graphite anode comprises the following steps: polishing 10mm × 5mm × 100mm graphite flakes on 1000#, 1500# and 2000# abrasive paper in sequence, cleaning the surfaces of the graphite flakes with deionized water and ethanol for more than 3 times in ultrasonic waves to remove graphite powder and grease adsorbed on the surfaces of the graphite flakes, then placing the graphite flakes in a vacuum drying oven to dry for more than 4 hours at the temperature of 150 ℃, drilling holes with the diameter of 1mm at one end of the graphite flakes, and connecting the graphite flakes with stainless steel conductor bars with the diameter of 5mm by passing nickel wires with the diameter of 1mm through the holes at one end of the graphite flakes to obtain the graphite anode.
7. The method for preparing the iron-aluminum-silicon carbide composite material by utilizing the red mud as claimed in claim 6, wherein the pressure of a pressing machine is 8MPa-10MPa, the pressing time is 150s-250s, the temperature rising rate of a tube furnace is 3 ℃/min-5 ℃/min, the sintering temperature is 900 ℃ -1100 ℃, and the sintering time is 2h-4 h.
8. The method for preparing the iron-aluminum-silicon carbide composite material from the red mud according to any one of claims 1, 2, 5 and 7, wherein the cleaning manner in the step S3 is to clean the red mud with deionized water in ultrasonic waves for 1 hour, the drying temperature is 150-250 ℃, and the drying time is more than 4 hours.
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