CN110592377A - Metal magnesium carbon thermal reduction process and device - Google Patents
Metal magnesium carbon thermal reduction process and device Download PDFInfo
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- CN110592377A CN110592377A CN201910711119.2A CN201910711119A CN110592377A CN 110592377 A CN110592377 A CN 110592377A CN 201910711119 A CN201910711119 A CN 201910711119A CN 110592377 A CN110592377 A CN 110592377A
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- 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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/20—Obtaining alkaline earth metals or magnesium
- C22B26/22—Obtaining magnesium
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- 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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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Abstract
The invention discloses a metal magnesium carbothermic reduction process and a device. The process comprises the steps of taking a magnesium-containing raw material, a carbon-containing reducing agent and a catalyst as raw materials, uniformly mixing and forming, directly electrifying two ends of a formed sample under the conditions of certain temperature and vacuum degree, controlling the current to carry out electrifying reduction reaction, and cooling after the reaction is finished to obtain the metal magnesium. The apparatus of the present invention comprises: a reactor for carrying out a magnesium metal reduction reaction; a positive electrode and a negative electrode for directly applying current to the reaction raw material molded member; a buffer part for adjusting and controlling the position of the positive electrode and the negative electrode and a sealing cover for sealing the reactor. The method overcomes the series problems of high reduction temperature, long reduction time, reversible reaction and the like of the metal magnesium by the existing carbothermic method, greatly reduces the temperature of the reduction device, can start to reduce the metal magnesium at room temperature, greatly improves the reduction speed of the metal magnesium, and is green and environment-friendly.
Description
Technical Field
The invention belongs to the field of metallurgical industry, and particularly relates to a magnesium metal carbon thermal reduction process and a magnesium metal carbon thermal reduction device.
Background
Magnesium metal and its alloy are the lightest metal structure materials at present, have good mechanical properties and physical properties, and gradually become popular metal materials in wide application. At present, the production process of magnesium smelting mainly adopts an electrolytic method and a silicothermic method. Compared with the prior widely applied process, the carbothermic magnesium-smelting process has the characteristics of short production flow, low energy consumption, low cost, high production efficiency, small pollution and the like. With the global attention and concern on the efficient utilization of resources and the ecological protection of the environment, the magnesium smelting by the carbothermic method has very important practical significance.
Researchers at home and abroad have carried out a lot of researches on the magnesium smelting process technology by the carbothermic method, but the inhibition of Mg-CO reverse reaction in the condensation process of magnesium vapor in the carbothermic reduction reaction is not effectively solved.
Although the carbothermic reduction process is applied in the second war period, the reaction temperature is high, the problems of reduction heating and high-temperature resistant materials of a vacuum sealing device are not easy to solve, the energy consumption in the heating process is high, and the requirements of modern clean production cannot be met. The microwave heating is adopted and reported, but a series of technologies such as microwave energy conversion efficiency, microwave thermal runaway, microwave penetration depth of materials and the like need to be solved by feeding microwaves into a vacuum device, and the problems of high heating cost exist, and the problems of high power consumption, easy damage of electrodes, high production cost and the like exist in an electric heating carbothermic reduction process by utilizing joule heat.
Disclosure of Invention
Aiming at the defects or shortcomings of the prior art, the invention provides a novel magnesium metal carbothermic reduction process and a device.
The magnesium metal carbothermic reduction process provided by the invention comprises the following steps: the carbon-containing reducing agent with proper granularity, the magnesium-containing raw material and the catalyst are reasonably proportioned and uniformly mixed, then are molded, and then are directly electrified on the molded part under the conditions of room temperature and proper vacuum to carry out reduction reaction, and then are cooled to obtain the metal magnesium.
In some embodiments, the inventive metal magnesium carbothermic reduction process comprises: proportionally and uniformly mixing carbon-containing reducing agent with proper granularity, magnesium-containing raw material and catalyst, molding, and directly introducing 50-2000mA/mm on the molded part under the conditions of room temperature and vacuum of 100-2000Pa2The reduction reaction is carried out for 1 to 60 minutes by current, and then the magnesium is cooled to obtain magnesium metal,/mm2Is the unit area of the radial cross section of the shaped part. In the scheme, further optional, the vacuum degree: 1000-2000Pa, current: 1000-,The reaction time is as follows: 5-15 minutes.
In another scheme, the metal magnesium carbon thermal reduction process comprises the following steps: the method comprises the steps of reasonably proportioning and uniformly mixing a carbon-containing reducing agent with a proper granularity, a magnesium-containing raw material and a catalyst, forming, heating to a proper temperature, directly electrifying the formed piece under the conditions of the proper temperature and the proper vacuum to carry out reduction reaction, and cooling to obtain the metal magnesium.
In some embodiments, the magnesium-carbon thermal reduction process of the invention comprises reasonably proportioning, uniformly mixing and molding a carbon-containing reducing agent with a proper particle size, a magnesium-containing raw material and a catalyst, and then directly introducing 1000mA/mm of 100-plus-1000 mA/mm on the molded piece under the conditions of 600-plus-1300 ℃ and 100-plus-2000 Pa vacuum2The reduction reaction is carried out for 60 to 1200 seconds by current, and then the magnesium is cooled to obtain magnesium metal,/mm2Is the unit area of the radial cross section of the shaped part.
Optionally, the molar ratio of Mg to C in the reasonable proportion is 1: 1.5-5. Further optionally, the molar ratio of Mg to C is 1: 2.5-3.
Further, the process comprises the step of respectively collecting the gas and the reducing slag generated in the reduction reaction process for resource utilization. In some embodiments, collecting the gas produced during the reduction reaction comprises collecting carbon dioxide and carbon monoxide separately in two stages.
In another aspect, the present invention provides a magnesium-carbon metal thermal reduction apparatus comprising:
the reactor is used for carrying out metal magnesium reduction reaction, and a feed inlet and a discharge outlet are arranged on the reactor;
the positive electrode and the negative electrode are used for directly applying current to the reaction raw material formed part, the positive electrode and the negative electrode are positioned in the reactor, and the raw material formed part is arranged between the positive electrode and the negative electrode;
the buffer piece is used for adjusting and controlling the positions of the positive electrode and the negative electrode and ensuring that the positive electrode and the negative electrode are always contacted with the raw material forming piece in the reduction reaction process;
and the sealing cover is arranged at the material inlet and the material outlet and used for sealing the reactor.
In some embodiments, the apparatus of the present invention further comprises a heating device for heating the reactor.
In some schemes, the two opposite end parts of the reactor are provided with a material inlet and a material outlet; the device comprises:
the two sealing covers are respectively arranged at the two material inlet and outlet openings, both the two sealing covers can conduct electricity, both the two sealing covers are provided with an electric connection structure connected with a power supply, and one sealing cover is provided with a gas outlet;
the two buffer parts can be both conductive and are respectively and electrically connected with the two sealing covers, and the two buffer parts are positioned in the reactor;
and the positive electrode and the negative electrode are positioned in the reactor and are respectively and electrically connected with the two buffering parts.
Optionally, the sealing cover of the invention adopts a flange structure.
Optionally, the buffer of the present invention is a metal spring structure.
Compared with the prior art, the method for reducing the metal magnesium has the beneficial effects that:
(1) the traditional carbon reduction magnesium smelting needs high temperature of more than 1500 ℃, but the existing metal magnesium reduction tank can only resist the high temperature within the range of 1200 ℃, thus greatly limiting the popularization and application of the carbon reduction magnesium smelting method in the industry. Also, due to the high reduction temperatures required, a "reverse reaction" can occur during the carbon reduction process. The invention leads the temperature in the sample to be high and the temperature of the furnace body to be low by directly electrifying the sample, thereby reducing the occurrence of reverse reaction in the prior art.
(2) After the press-formed sample is electrified and heated, the raw materials are activated under the action of current, the activation energy of the reduction reaction is reduced, and compared with the existing carbothermic reduction reaction, the reduction reaction rate is greatly improved, and the reaction temperature is greatly reduced.
(3) The pressed sample is electrified to generate heat, the electrothermal conversion rate is high, the heat utilization rate is high, and the energy consumption is low.
(4) In other embodiments, the invention can first raise the temperature of the raw materials in a traditional manner, and then perform the electric reaction, so that the furnace temperature is far lower than the tolerance temperature limit, and the occurrence of reverse reaction is reduced. Further, the invention ensures the conductivity and the reduction rate of the formed part by submitting the dosage of the carbon reducing agent.
(5) The raw material product can shrink in the reduction process, and the buffer piece in the device can ensure that the sample is always contacted with the electrode in the reduction reaction process. The feed inlets are arranged at two ends of the furnace, end sealing is adopted, and direct electrification is carried out on the end sealing covers, so that the problem of difficulty in sealing the furnace can be solved, and the electrification process can be realized.
(6) The current reduction process of the sample has a sintering compact phenomenon, and the reduced sample is a sintered product which can be used as a building material and can realize solid waste-free output.
(7) Decomposing carbon dioxide at high temperature (about 1100 ℃ is required for dolomite) under normal pressure in the traditional calcination to obtain calcined dolomite, and then adding a reducing agent to reduce at 1550 ℃ in vacuum to obtain metal magnesium; in some embodiments of the invention (i.e. dolomite or magnesia is selected as the raw material containing magnesium, and the electrifying time is longer), calcination and reduction are carried out simultaneously, so that the reduction temperature can be greatly reduced (by 300 ℃ to 400 ℃), and carbon dioxide generated during calcination and carbon monoxide generated during reduction can be recycled; meanwhile, the calcined dolomite enters a reduction stage after sintering, and is carried out in one reactor without replacing a reaction device, so that the traditional dolomite calcining large-scale equipment is omitted.
Generally, the magnesium metal reduction method has the advantages of high reduction speed, low furnace temperature and environmental energy conservation, and belongs to a new green technology and a new process for reducing magnesium metal.
Drawings
FIG. 1 is a schematic view of the apparatus according to the present invention;
FIG. 2 is a schematic process flow diagram according to an embodiment of the present invention.
Detailed Description
The raw materials used in the invention comprise carbonaceous reducing agent, magnesium-containing raw material, catalyst and the like which are all used for reducing metal magnesium by the existing carbothermic method. For example, the carbonaceous reductant can be selected from graphite, semi coke, coal, calcium carbide, and the like; the magnesium-containing raw material can be dolomite, calcined dolomite (calcined dolomite) or magnesite or calcined magnesite, etc., the catalyst is fluorite, etc., and the proportion of each raw material is similar to or the same as that of the existing carbothermic reduction method. The proper particle size of the raw material is determined according to specific process requirements, and a 100-mesh sieve can be selected generally.
When calcined dolomite or calcined magnesite is selected as a magnesium-containing raw material, the calcined dolomite can be obtained by ordinary calcination, namely, calcination is carried out at normal pressure and high temperature, for example, carbon dioxide is decomposed from dolomite at about 1100 ℃ under normal pressure to obtain the calcined dolomite.
The raw materials are uniformly mixed and molded by a method commonly used in the field, such as ball milling, uniform mixing, pressure molding and the like. The molded sample piece is cylindrical, a three-dimensional column or brick-shaped, the size and the shape of the molded sample piece are determined according to the structure and the size of the production device, and the reduction effect can be achieved by controlling other process conditions according to the sizes and the shapes of different samples. When the molded sample is installed in the device, the two electrodes are positioned at the two axial ends of the sample.
The current used in the process can be direct current or alternating current. The room temperature according to the present invention is conventionally understood to be in the range of 20 to 40 c depending on seasons.
Example 1:
mixing calcined dolomite with the magnesium oxide content of 36 wt%, coke and fluorite according to the mass ratio of 60:13:10, ball-milling and sieving with a 100-mesh sieve, pressure-forming into a cylindrical sample with the diameter of 6mm and the length of 12mm, placing the cylindrical sample between an upper electrode and a lower electrode in a vacuum reduction furnace, vacuumizing, controlling the applied current of the sample to be 0.8 ampere under the pressure of the vacuum degree of 1000Pa, carrying out an electrifying reaction for 30 minutes, cooling, and measuring the reduction rate of the magnesium oxide in the sample to be 61%.
Example 2:
mixing calcined dolomite with the magnesium oxide content of 36 wt%, coke and fluorite according to the mass ratio of 60:30:10, ball-milling and sieving with a 100-mesh sieve, pressure-forming into a cylindrical sample with the diameter of 6mm and the length of 12mm, placing the cylindrical sample between an upper electrode and a lower electrode in a vacuum reduction furnace, vacuumizing, controlling the applied current of the sample to be 0.8 ampere under the pressure of the vacuum degree of 100Pa, carrying out an electrifying reaction for 23 minutes, cooling, and measuring the reduction rate of the magnesium oxide in the sample to be 65%.
Example 3:
mixing calcined dolomite with the magnesium oxide content of 36 wt%, coke and fluorite according to the mass ratio of 60:35:10, ball-milling and sieving by a 200-mesh sieve, forming into a cylindrical sample with the diameter of 6mm and the length of 12mm under the pressure of 25MPa, placing the cylindrical sample between an upper electrode and a lower electrode in a vacuum reduction furnace, vacuumizing, applying current to the sample under the pressure of 2000Pa of vacuum degree to control the current to be 0.8 ampere, carrying out an electrifying reaction for 10 minutes, cooling, and measuring the reduction rate of the magnesium oxide in the sample to be 67%.
Example 4:
the difference of the embodiment from the embodiment 1 is that the calcined dolomite is replaced by dolomite with the magnesium oxide content of 36 wt%, the dolomite, the coke and the fluorite are proportioned according to the mass ratio of 120:13:10, and the electrifying time is prolonged by one time. The reduction rate of magnesium oxide in the obtained sample was 65%.
Example 5:
the difference of the embodiment from the embodiment 2 is that the calcined dolomite is replaced by dolomite with the magnesium oxide content of 36 wt%, the dolomite, the coke and the fluorite are proportioned according to the mass ratio of 120:30:17, and the electrifying time is prolonged by 1.5 times. The reduction ratio of magnesium oxide in the obtained sample was 64%.
Example 6:
the difference of the embodiment from the embodiment 3 is that the calcined dolomite is replaced by dolomite with the magnesium oxide content of 36 wt%, the dolomite, the coke and the fluorite are proportioned according to the mass ratio of 120:35:9, and the electrifying time is prolonged by one time. The reduction rate of magnesium oxide in the obtained sample was 69%.
Example 7:
mixing calcined dolomite with the magnesium oxide content of 36 wt%, coke and fluorite according to the mass ratio of 70:16:8, ball-milling and sieving with a 100-mesh sieve, pressure forming to obtain a cylindrical sample with the diameter of 6mm and the length of 12mm, placing the cylindrical sample between an upper electrode and a lower electrode in a vacuum reduction furnace, vacuumizing, keeping the temperature for half an hour after the temperature of the furnace is raised to 600 ℃, applying current to the sample under the pressure of 1000Pa to control the current to be 0.8 ampere, carrying out an electrifying reaction for 5 minutes, cooling, and measuring the reduction rate of the magnesium oxide in the sample to be 83%.
Example 8:
mixing calcined dolomite with the magnesium oxide content of 36 wt%, coke and fluorite according to the mass ratio of 70:38:8, ball-milling and sieving by a 100-mesh sieve, forming into a cylindrical sample with the diameter of 6mm and the length of 12mm under the pressure of 30MPa, placing the cylindrical sample between an upper electrode and a lower electrode in a vacuum reduction furnace, vacuumizing, keeping the temperature for half an hour after the temperature of the furnace rises to 1000 ℃, controlling the current applied to the sample to be 0.8 ampere under the pressure of 100Pa, carrying out an electrifying reaction for 1 minute, cooling, and measuring the reduction rate of the magnesium oxide in the sample to be 87%.
Example 9:
mixing calcined dolomite with the magnesium oxide content of 36 wt%, coke and fluorite according to the mass ratio of 70:22:8, ball-milling and sieving with a 100-mesh sieve, pressure-forming to obtain a cylindrical sample with the diameter of 6mm and the length of 12mm, placing the cylindrical sample between an upper electrode and a lower electrode in a vacuum reduction furnace, vacuumizing, keeping the temperature for half an hour after the furnace temperature is increased to 800 ℃, applying current to the sample under the pressure of 2000Pa, controlling the current to be 0.8 ampere, carrying out an electrifying reaction for 10 minutes, cooling, and measuring the reduction rate of the magnesium oxide in the sample to be 85%.
Example 10:
the difference of the embodiment from the embodiment 7 is that the calcined dolomite is replaced by dolomite with the magnesia content of 36 wt%, the dolomite, the coke and the fluorite are proportioned according to the mass ratio of 140:16:9, and the electrifying time is prolonged by 1.5 times. The reduction ratio of magnesium oxide in the obtained sample was 82%.
Example 11:
the difference of the embodiment from the embodiment 8 is that the calcined dolomite is replaced by dolomite with the magnesium oxide content of 36 wt%, the dolomite, the coke and the fluorite are proportioned according to the mass ratio of 140:38:20, and the electrifying time is prolonged by 1.5 times. The reduction rate of magnesium oxide in the obtained sample was 86%.
Example 12:
the difference of the embodiment and the embodiment 9 is that the calcined dolomite is replaced by dolomite with the magnesia content of 36 wt%, the dolomite, the coke and the fluorite are proportioned according to the mass ratio of 140:22:15, and the electrifying time is prolonged by 1.5 times. The reduction rate of magnesium oxide in the obtained sample was 85%.
Example 13:
in this example, gases and final reducing slag in the calcining and/or reducing reaction process are recovered, carbon dioxide is recovered in the calcining, and carbon monoxide is recovered in the reducing reaction process, and the specific process is shown in fig. 2.
Example 14:
the embodiment provides a magnesium smelting device, as shown in fig. 1, the device of the embodiment is horizontally arranged, the device comprises a reduction reactor 8, the two ends of the reactor in the preferred scheme are provided with a feeding and discharging port, the two feeding and discharging ports are provided with sealing covers 9, and the sealing covers can be metal flanges 9; the sealing cover is provided with an electric connection structure connected with a power supply, and the power supply directly supplies power to the sealing cover; the two sealing covers 9 are electrically connected with the buffer parts 3 on the wall facing the inside of the reactor, the two buffer parts can be conductive, and the buffer parts can be metal springs; a left positive electrode and a right positive electrode 4 are arranged in the reactor 8, the two electrodes are positioned between the two buffer parts and are respectively and electrically connected with the corresponding buffer parts, and a mounting position of a formed part to be reduced is arranged between the two electrodes; the controller 2 controls the current generated from the power source to be applied to the reduced sample 5 through the sealing cap 9, the buffer 3 and the electrode 4. The device may be supplied with either direct current or alternating current.
Further, an electric heating device 6 is arranged outside the reactor 8, and the electric heating device 6 is heated and temperature-controlled by a furnace temperature controller 7 according to a thermocouple 12.
The integral device also comprises a vacuum pump 1 which is communicated with an air outlet hole arranged on the sealing cover 9 at one end to vacuumize the reactor. The specific implementation mode is that a vacuum tube 10 is connected to a sealing cover on one side, the vacuum tube 10 is communicated with a vacuum pump, and a vacuum meter 11 is arranged on a gas path to control the vacuum condition. The entire device of this embodiment is in a bedroom arrangement.
The process gas is output through the vacuum pump 1 while being collected.
When the device is used, the raw materials are subjected to reduction reaction in the reactor of the device according to the process of the invention, the controller is closed after the reaction is finished, the magnesium metal is taken out after the reactor is directly cooled, and the magnesium metal reducing slag is removed for the next production.
Claims (10)
1. A magnesium carbon thermal reduction process of metal, characterized by, comprising: the carbon-containing reducing agent with proper granularity, the magnesium-containing raw material and the catalyst are reasonably proportioned and uniformly mixed, then are molded, and then are directly electrified on the molded part under the conditions of room temperature and proper vacuum to carry out reduction reaction, and then are cooled to obtain the metal magnesium.
2. A process for carbothermic reduction of magnesium metal as defined in claim 1, comprising: proportionally and uniformly mixing carbon-containing reducing agent with proper granularity, magnesium-containing raw material and catalyst, molding, and directly introducing 50-2000mA/mm on the molded part under the conditions of room temperature and vacuum of 100-2000Pa2The reduction reaction is carried out for 1 to 60 minutes by current, and then the magnesium is cooled to obtain magnesium metal,/mm2Is the unit area of the radial cross section of the shaped part.
3. A magnesium carbon thermal reduction process of metal, characterized by, comprising: the method comprises the steps of reasonably proportioning and uniformly mixing a carbon-containing reducing agent with a proper granularity, a magnesium-containing raw material and a catalyst, forming, heating to a proper temperature, directly electrifying the formed piece under the conditions of the proper temperature and the proper vacuum to carry out reduction reaction, and cooling to obtain the metal magnesium.
4. The magnesium carbothermic reduction process as set forth in claim 3, wherein the carbonaceous reducing agent with suitable particle size, the magnesium-containing raw material and the catalyst are mixed in a reasonable proportion, molded, and then directly charged with 1000mA/mm of 100 mA/mm on the molded part under the conditions of 600-1300 ℃ and 100-2000Pa vacuum2The reduction reaction is carried out for 60 to 1200 seconds by current, and then the magnesium is cooled to obtain magnesium metal,/mm2Is the unit area of the radial cross section of the shaped part.
5. A process for the carbothermic reduction of magnesium metal as in claim 1, 2, 3 or 4 wherein the molar ratio of Mg to C in said stoichiometric ratio is 1:1.5 to 5.
6. A carbothermic process to produce magnesium metal as recited in claim 1, 2, 3 or 4 wherein the gases and reducing slag produced during the reduction reaction are collected separately for resource utilization.
7. A magnesium carbon thermal reduction apparatus, comprising:
the reactor is used for carrying out metal magnesium reduction reaction, and a feed inlet and a discharge outlet are arranged on the reactor;
the positive electrode and the negative electrode are used for directly applying current to the reaction raw material formed part, the positive electrode and the negative electrode are positioned in the reactor, and the raw material formed part is arranged between the positive electrode and the negative electrode;
the buffer piece is used for adjusting and controlling the positions of the positive electrode and the negative electrode and ensuring that the positive electrode and the negative electrode are always contacted with the raw material forming piece in the reduction reaction process;
the sealing cover is arranged at the material inlet and the material outlet and used for sealing the reactor;
the apparatus further comprises a heating device for heating the reactor.
8. The magnesium-carbon thermal reduction device of claim 7, wherein the reactor is provided with a feed inlet and a discharge outlet at two opposite ends; the device comprises:
the two sealing covers are respectively arranged at the two material inlet and outlet openings, both the two sealing covers can conduct electricity, both the two sealing covers are provided with an electric connection structure connected with a power supply, and one sealing cover is provided with a gas outlet;
the two buffer parts can be both conductive and are respectively and electrically connected with the two sealing covers, and the two buffer parts are positioned in the reactor;
and the positive electrode and the negative electrode are positioned in the reactor and are respectively and electrically connected with the two buffering parts.
9. The metal magnesium carbon thermal reduction device of claim 8, wherein the sealing cover is a flange structure.
10. The metal magnesium carbon thermal reduction device of claim 8, wherein the buffer is a metal spring structure.
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Application publication date: 20191220 |