CN1827808A - Inner resistance heating metallothermic reduction furnace for melting magnesium - Google Patents
Inner resistance heating metallothermic reduction furnace for melting magnesium Download PDFInfo
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Abstract
The invention relates internal resistance heating metal thermal reduction magnesium furnace. The furnace body is barrel or rectangle, and it has two chambers, one of which is high temperature vacuum reduction reaction chamber, and the other of which is magnesium crystallization chamber. In the crystallization chamber there is Na-K drip catcher, at the port of crystallization chamber is covered by furnace lid, on the outer of crystallization chamber there is cooling-jacket, and in the crystallization chamber there is crystallizer. Between chambers there is hot baffle, heat-resisting alloy steel furnace inner wall is out of the furnace inside lining, between heat-resisting alloy steel furnace inner wall and furnace outer wall there is heat-insulating material, in high temperature vacuum reduction reaction chamber there is metal resistance heater connected with receiving terminal. The reaction mass is between two vertical metal resistance heater. The furnace lid seals the port of high temperature vacuum reduction reaction chamber. The furnace not only suits to produce magnesium metal with metallothermic reduction process, but also is used to produce calcium, strontium, lithium and other metals. The furnace can be used to metal vacuum distillation and sublimation purification, or reclamation of the twice metal.
Description
Technical Field
The invention relates to non-ferrous metal vacuum reduction smelting equipment, in particular to an internal resistance heating metallothermic reduction magnesium smelting furnace.
Background
In general, alkali metals and alkaline earth metals can be produced by molten salt electrolysis, but some of the higher vapor pressure alkali metals and alkaline earth metals, such as strontium, magnesium, calcium, etc., can be produced by metallothermic reduction of silicon, aluminum or their alloys under vacuum conditions. Among these metal thermal reduction methods, the metallothermic reduction of magnesium is mainly the silicothermic or aluminothermic reduction which is most widely used, the reducing agent is mostly used in the form of ferrosilicon and silicon-aluminum alloy, the reduced raw material is mostly calcined dolomite, and the calcined product of the mixture of magnesite and limestone can also be used. But most commonly used is the ferrosilicon reductant known as silicothermic magnesium production. According to different heating methods, the prior silicothermic magnesium smelting method can be divided into three types: one is Pidgeon Process (The Pidgeon Process), one is French semi-continuous Process (The Magnetherm Process), and The other is Italy Pilgano Process (The Bolgano Process). The former belongs to external heating silicothermic method forsmelting magnesium, and the latter two methods are internal resistance heating silicothermic method for smelting magnesium. However, the two kinds of silicothermic smelting of magnesium by internal resistance heating are not completely the same. The main equipment of the French semi-continuous process is similar to a vacuum ore-smelting furnace, the mixture of calcined magnesite ore, dolomite and bauxite is used as raw material, the melt produced in the smelting process of a vacuum electric arc furnace is used as a heating element of a resistor, the smelting temperature is above 1600 ℃, and the French semi-continuous process has the advantages of high reaction temperature, high reaction speed, large single-furnace yield, unstable process and low product purity. Therefore, the method is not popularized and applied. The Italy pilgarno method is another internal resistance heating silicothermic magnesium-smelting technique, and is characterized by that the internal resistance heating in the vacuum furnace is implemented by means of resistance heat of sheet metal electric heating body in the furnace. The method has the disadvantages that the reaction materials are directly arranged on the sheet-shaped metal electric heating body, and the resistance heating body is easily corroded by the reaction materials under the high-temperature condition, so that the electric heating parameters of the electric heating body are unstable, the service life is short, and the production cost is high. For smelting magnesium by the Pidgeon process with external heating, solid fuel, liquid fuel and external resistance can be used for heating, but the heating efficiency is not high, the furnace body is limited by heat transfer and furnace body materials, the space of the furnace body is small, the output of a single furnace is low, the service life of the furnace body is short, the production rate is low and the cost is high.
Disclosure of Invention
Aiming at the defects of the existing magnesium smelting furnace, the invention provides an internal resistance heating metal thermal reduction magnesium smelting furnace.
The invention provides a novel vacuum smelting furnace for reducing and smelting magnesium by metal through internal resistance heating, wherein a furnace body is in a barrel shape or a rectangular barrel shape, refractory material or carbon material is used as a lining for the furnace, the inner wall of a heat-resistant alloy steel furnace body is arranged outside the lining, heat insulation material is filled between the inner wall of the heat-resistant alloy steel furnace body and the outer wall of the furnace, the furnace can be vacuumized, and the deformation of the heat-resistant alloy steel metal furnace body caused by negative pressure in a furnace chamber under the high-temperature condition can be ensured and the heat insulation effect can be enhanced. The metal resistance heating body is arranged in the furnace chamber, the temperature in the furnace chamber can be ensured to reach 1200-1300 ℃, and the reaction materials are placed between two rows of vertically arranged electric heating bodies in the furnace chamber. This furnace has two chambers, one of which is a reduction reaction chamber, and a resistance heating element and a charge material are placed in this chamber. And the other chamber is a crystallization chamber for gaseous reaction products, the outer wall of the chamber is provided with a cooling water jacket, and the inner wall is provided with a crystallizer made of stainless steel and used for condensing the reaction products. The crystallizer is tightly attached to the inner wall of the crystallization chamber and is a cylinder which is made of stainless steel, one end of the cylinder is bottomless, the other end of the cylinder is bottomless and the bottom of the cylinder is provided with a hole.
The furnace body of the furnace is in a barrel shape or a rectangular barrel shape, one side of the furnace body is a high-temperature vacuum reduction reaction furnace chamber, the other end of the furnace body is a crystallization chamber of gaseous metal products, the high-temperature vacuum reduction reaction furnace body is made of high-temperature heat-resistant alloy steel, and a refractory material or a carbon material is lined in the high-temperature vacuum reduction reaction furnace body. The reaction furnace chamber is internally provided with a plurality of rows of vertically arranged high-resistance heating elements, two ends of the resistance heating elements are connected with metal conductors, and the metal conductors are connected with an external power supply. Reaction materials are placed between two vertical rows of resistance heating bodies in the reaction furnace chamber. Light refractory materials or heat insulating materials are filled between the inner wall of the high-temperature reduction reaction furnace body and the outer shell and between the inner wall of the furnace cover of the reaction furnace chamber and the outer shell, and the high-temperature reduction reaction furnace body and the outer shell are vacuumized.
The method for producing the magnesium metal by adopting the furnace is as follows.
Firstly, the calcined dolomite or magnesite and limestone are mixed with ferrosilicon or silicon-aluminum reducing agent according to the stoichiometric ratio, and the mixture is pressed into a dough shape, and the dough-shaped material is placed between two rows of vertical resistance heating elements in a reaction furnace chamber. Then closing a furnace cover of a reaction furnace chamber and a furnace cover of a crystallization chamber, vacuumizing the reaction furnace chamber, the crystallization chamber, the space between the inner wall of a furnace body and a furnace outer shell, and the space between the inner wall of the furnace cover and the furnace outer shell, electrifying, heating the reaction materials to 1200-1300 ℃ by means of a resistance heating element in the reaction furnace body, and carrying out oxidation-reduction reaction under the vacuum condition (the residual pressure of the system is 1-13 Pa), wherein the main reaction equation is as follows:
the magnesium metal of the reaction product is crystallized on the inner wall of the crystallizer, and the potassium and sodium metal impurities with higher vapor pressure in the product are crystallized on the sodium-potassium catcher. After the reaction is finished, argon is filled into the furnace, a cover at the end part of the crystallization chamber is opened, the crystallized magnesium and the crystallizer are taken out of the furnace together, the crystallized magnesium is physically separated and taken out, the cover of the reaction furnace chamber is opened, and residues after the reaction are taken out. The purity of the prepared magnesium metal is more than 98 percent.
The magnesium smelting furnace of the invention is not only suitable for producing metal magnesium by a metallothermic reduction method, but also can be used for producing other alkali metals, alkaline earth metals or other metals with high vapor pressure, such as strontium, calcium, lithium and the like by the metallothermic reduction method. It can also be used for vacuum distillation or sublimation purification of the above metals, or recovery purification of the above secondary metals. The method for smelting magnesium by adopting the magnesium smelting furnace is different from the Pidgeon method, the semi-continuous method of France and the pilgarno method of Italy. The method realizes the built-in resistance heating element for the vacuum reduction reaction furnace, the heating element is not in direct contact with reaction materials, the service life of the resistance heating element is long, frequent maintenance is not needed, the production cost is low, and no environmental pollution is caused.
Drawings
FIG. 1 is a schematic front view of an internal resistance heating magnesium-making furnace for metallothermic reduction of the present invention.
FIG. 2 is a schematic top view of an internal resistance heating type metallothermic magnesium-making furnace.
In fig. 1 and 2: the furnace comprises a furnace cover 1, a furnace cover vacuumizing tube 2, a furnace body outer wall 3, a heat-resistant alloy steel furnace body inner wall 4, a furnace body inner lining 5, a crystallization chamber 10, a heat shield plate 11, a crystallizer 12, a cooling water jacket 13, a vacuumizing tube 14, a sodium-potassium catcher 15, a vacuum gasket 16, a crystallization chamber furnace cover 17 and a furnace body heat-insulating layer vacuumizing tube 18, wherein the furnace body inner lining is made of a high-temperature-resistant high-density refractory material, the heat-insulating material 6, a metal resistance heating body 7, an external terminal 8, the high-temperature vacuum reduction.
Detailed Description
As shown in figures 1 and 2, the furnace body of the magnesium smelting furnace is in a barrel shape, the furnace is provided with two chambers, one end of the furnace body is a high-temperature vacuum reduction reaction furnace chamber 9, and the other end is a crystallization chamber 10 of gaseous metal products. An evacuation tube 14 is provided on the side wall of the crystallization chamber 10, and a sodium potassium trap 15 is provided in the crystallization chamber 10. The port of the crystallization chamber 10 is sealed by a crystallization chamber lid 17 (flange) pressing a vacuum gasket 16. The outer wall of the crystallization chamber 10 is provided with a cooling water jacket 13, the inner wall of the crystallization chamber 10 is provided with a crystallizer 12 which is made of stainless steel and is used for condensing reaction products, and the crystallizer 12 is tightly attached to the inner wall of the crystallization chamber 10 and is a cylinder which is made of stainless steel, has no bottom at one end and has a bottom at the other end and a hole at the bottom. A heat shield 11 is provided between the high-temperature vacuum reduction reaction furnace chamber 9 and the crystallization chamber 10. The furnace uses refractory material or carbon material as furnace body lining 5, the heat-resisting alloy steel furnace body inner wall 4 is arranged outside the furnace body lining 5, and heat-insulating material 6 is filled between the heat-resisting alloy steel furnace body inner wall 4 and the furnace body outer wall 3, and is vacuumized, thereby ensuring the deformation of the heat-resisting alloy steel metal furnace body caused by negative pressure in the furnace chamber under the high-temperature condition. The vacuum-pumping pipe 18 of the furnace body heat-insulating layer is arranged on the side wall of the furnace body outer wall 3 for vacuum pumping. The high-temperature vacuum reduction reaction furnace chamber 9 is internally provided with a metal resistance heating body 7, the temperature in the furnace chamber can be ensured to reach 1200-1300 ℃, two ends of the metal resistance heating body 7 are connected with a metal conductor, and the metal conductor is connected with a terminal 8 outside the furnace and can be connected with an external power supply. The reaction materials are placed between two rows of vertically arranged metal resistance heating bodies 7 in a high-temperature vacuum reduction reaction furnace chamber 9. The metal resistance heating elements 7 are arranged in a vertical manner in a plurality of rows. The port of the high-temperature vacuum reduction reaction furnace chamber 9 is sealed by a furnace cover 1 pressing a vacuum gasket 16, and a furnace cover vacuum-pumping pipe 2 is arranged on the side wall of the furnace cover 1 for vacuum pumping. The furnace has the characteristics of long service life of the furnace body, large volume of the furnace chamber, large output of a single furnace, high thermal efficiency and low energy consumption.
The method for producing the magnesium metal by adopting the furnace is as follows.
Firstly, mixing calcined dolomite or magnesite and calcined limestone with a ferrosilicon or silicon-aluminum reducing agent according to a stoichiometric ratio, pressing the materials into a dough, and placing the dough-like materials between two rows of vertical metal resistance heating elements 7 in a high-temperature vacuum reduction reaction furnace chamber 9. Then closing the furnace cover 1 and the crystallizing chamber furnace cover 17, vacuumizing the high-temperature vacuum reduction reaction furnace chamber 9, the crystallizing chamber 10, the space between the outer wall 3 of the furnace body and the inner wall 4 of the heat-resistant alloy steel furnace body and the space between the inner wall of the furnace cover 1 and the shell, electrifying, heating the reaction materials to 1200-1300 ℃ by virtue of a metal resistance heating body 7 in the reaction furnace body, and carrying out oxidation-reduction reaction under the vacuum condition (the residual pressure of the system is 1-13 Pa), wherein the main reaction equation is as follows:
the magnesium metal of the reaction product crystallizes on the inner wall of the crystallizer 12, while the potassium and sodium metal impurities with higher vapor pressure in the product crystallize on the sodium-potassium catcher 15. After the reaction is finished, argon is filled into the furnace, the furnace cover 17 of the crystallization chamber is opened, the crystallized magnesium and the crystallizer 12 are taken out of the furnace together, the crystallized magnesium is physically separated and taken out, the furnace cover 1 is opened, and residues after the reaction are taken out. The purity of the prepared magnesium metal is more than 98 percent.
Claims (5)
1. An internal resistance heating metal thermal reduction magnesium smelting furnace is characterized in that a furnace body is in a barrel shape or a rectangular barrel shape and is provided with two chambers, one end of the furnace body is a high-temperature vacuum reduction reaction furnace chamber (9), the other end of the furnace body is a crystallization chamber (10) of a gaseous metal product, a vacuumizing pipe (14) is arranged on the side wall of the crystallization chamber (10), a sodium-potassium catcher (15) is arranged in the crystallization chamber (10), the port of the crystallization chamber (10) is sealed by a vacuum gasket (16) pressed by a crystallization chamber furnace cover (17), the outer wall of the crystallization chamber (10) is provided with a cooling water jacket (13), the inner wall of the crystallization chamber (10) is provided with a crystallizer (12), a heat baffle plate (11) is arranged between the high-temperature vacuum reduction reaction furnace chamber (9) and the crystallization chamber (10), a heat-resistant alloy steel furnace body inner wall (4) is arranged outside a furnace body lining (5), and an alloy steel heat, and vacuumizing, wherein a vacuumizing pipe (18) of a furnace body heat-insulating layer is arranged on the side wall of the outer wall (3) of the furnace body, a metal resistance heating body (7) is arranged in a high-temperature vacuum reduction reaction furnace chamber (9), two ends of the metal resistance heating body (7) are connected with a metal conductor, the metal conductor is connected with an external terminal (8), the port of the high-temperature vacuum reduction reaction furnace chamber (9) is sealed by a furnace cover (1) pressing a vacuum gasket (16), and a furnace cover vacuumizing pipe (2) is arranged on the side wall of the furnace cover (1).
2. The internal resistance-heated metallothermic reduction magnesium-making furnace according to claim 1, wherein the metallic resistance heating elements (7) built in the vacuum reduction reaction furnace chamber (9) are arranged vertically.
3. An internally resistance-heated metallothermic reduction magnesium-making furnace according to claim 1, wherein the mold (12) is closely attached to the inner wall of the crystallization chamber (10) and is a cylinder made of stainless steel having one end bottomless, the other end bottomed and a hole in the bottom.
4. The internal resistance heating metallothermic reduction magnesium-making furnace according to claim 1, wherein the reaction materials are placed between two rows of vertically arranged metallic resistance heating elements (7) in the high temperature vacuum reduction reaction furnace chamber (9).
5. The method for smelting magnesium by adopting the internal resistance heating metallothermic reduction magnesium smelting furnace of claim 1 is characterized by comprising the following process steps:
firstly, preparing a calcined dolomite or magnesite and a calcined limestone product and a ferrosilicon or silicon-aluminum reducing agent according to a stoichiometric ratio, pressing the materials into a bulk, placing the bulk material between two rows of vertical metal resistance heating elements (7) in a high-temperature vacuum reduction reaction furnace chamber (9), then closing a furnace cover (1) and a crystallization chamber furnace cover (17), vacuumizing the high-temperature vacuum reduction reaction furnace chamber (9), the crystallization chamber (10), a space between an outer wall (3) of a furnace body and an inner wall (4) of a heat-resistant alloy steel furnace body, and a space between the inner wall of the furnace cover (1) and a shell, electrifying, heating the reaction materials to 1200-1300 ℃ by virtue of the metal resistance heating elements (7) in the reaction furnace body, reacting under the vacuum condition of the residual pressure of the system being 1-13 Pa, crystallizing metal magnesium of a reaction product on the inner wall of a crystallizer (12), and obtaining potassium in the product, Sodium metal impurities are crystallized on a sodium-potassium trap (15), after the reaction is finished, argon is filled into the furnace, a furnace cover (17) of a crystallization chamber is opened, crystallized magnesium and a crystallizer (12) are taken out of the furnace together, the crystallized magnesium is physically separated and taken out, a furnace cover (1) is opened, and residues after the reaction are taken out.
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| CNB2006100461499A CN100342045C (en) | 2006-03-24 | 2006-03-24 | Inner resistance heating metallothermic reduction furnace for melting magnesium |
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| CNB2006100461499A CN100342045C (en) | 2006-03-24 | 2006-03-24 | Inner resistance heating metallothermic reduction furnace for melting magnesium |
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| CN102131942A (en) * | 2008-07-31 | 2011-07-20 | 澳大利亚联邦科学与工业研究组织 | Production process |
| CN102816938A (en) * | 2012-08-22 | 2012-12-12 | 刘海永 | Reducing furnace for smelting magnesium by electrothermal method |
| CN103397204A (en) * | 2013-07-03 | 2013-11-20 | 宁夏鹏程致远自动化技术有限公司 | Novel insulation baffle of magnesium crystallizer |
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| US5782952A (en) * | 1996-08-30 | 1998-07-21 | Massachusetts Institute Of Technology | Method for production of magnesium |
| CN2443004Y (en) * | 2000-09-30 | 2001-08-15 | 于洪喜 | Internal heating magnesium smelting furnace |
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2006
- 2006-03-24 CN CNB2006100461499A patent/CN100342045C/en not_active Expired - Fee Related
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