CN100342045C - 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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- CN100342045C CN100342045C CNB2006100461499A CN200610046149A CN100342045C CN 100342045 C CN100342045 C CN 100342045C CN B2006100461499 A CNB2006100461499 A CN B2006100461499A CN 200610046149 A CN200610046149 A CN 200610046149A CN 100342045 C CN100342045 C CN 100342045C
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Abstract
The present invention relates to an inner resistance heating metallothermic reduction furnace for melting magnesium. A furnace body forms a drum shape or a rectangular drum shape, and is provided with two chambers. One end of the furnace body is a high-temperature vacuum reduction reaction furnace chamber, and the other end of the furnace body is a magnesium crystallization chamber. A natrium and kalium catcher is arranged in the crystallization chamber, and the end opening of the crystallization chamber is sealed by a furnace cover of the crystallization chamber. The outer wall of the crystallization chamber is provided with a cooling water jacket, and a crystallizer is arranged in the cooling water jacket. A heat baffle plate is arranged between the high-temperature vacuum reduction reaction furnace chamber and the magnesium crystallization chamber. The inner wall of a heat resistant alloy steel furnace body is arranged outside an inner lining of the furnace body, heat insulating materials are filled between the inner wall of the heat resistant alloy steel furnace body and the outer wall of the furnace and are vacuated. Metallic resistor heaters are arranged in the high-temperature vacuum reduction reaction furnace chamber, and are connected with a terminal outside the furnace. Reaction materials are placed between the metallic resistor heaters which are arranged vertically in two rows. The end opening of the high-temperature vacuum reduction reaction furnace chamber is sealed by a furnace cover. The present invention can be suitable for a metallothermic reduction method to produce magnesium, and suitable for a metallothermic reduction method to produce metals, such as strontium, calcium, lithium, etc. Besides, the present invention can also be applied to the vacuum distillation or the sublimation and purification of the metals, or the secondary recovery and purification of the metals.
Description
Technical field
The present invention relates to a kind of non-ferrous metal vacuum reduction smelting equipment, be specifically related to a kind of inner resistance heating metallothermic reduction furnace for melting magnesium.
Background technology
In general, basic metal and alkaline-earth metal can be used fused salt electrolysis process production, but some vapour pressure higher alkali metal and alkaline-earth metal as strontium, magnesium, calcium etc., can make with metallothermics under the condition of vacuum with silicon, aluminium or their alloy.And in the hot reducing method of these metals, the metallothermic reduction of magnesium mainly is that silicon heat or aluminothermy metallothermic reduction obtain using the most widely, the many forms with ferrosilicon and silumin of its reductive agent are used, and the raw material that is reduced mostly is the rhombspar after the calcining, also can be with the after product of forging of magnesite and Wingdale mixture.But use maximum ferrosilicon reductive agents that are to use, be called magnesium-smelting silicothermic process.Difference according to heating means, present magnesium-smelting silicothermic process can be divided into three kinds: a kind of is production of magnesium by pidgeonprocess (The PidgeonProcess), a kind of is the semi-continuous process refining magnesium (The Magnetherm Process) of France, and another kind is gondola Pierre Jia Nuofa refining magnesium (The Bolgano Process).The former belongs to the magnesium-smelting silicothermic process of outer heating, and then two kinds of methods are internal resistance heating magnesium-smelting silicothermic process.But the magnesium-smelting silicothermic process of these two kinds of internal resistance heating is incomplete same again.The semi-continuous process of France, its main equipment is similar to a hot stove in vacuum ore deposit, use the compound of giobertite, rhombspar and bauxite after forging to be raw material, the melt that produces when vacuum arc furnace melting is as the heating element of resistance, and its smelting temperature is more than 1600 ℃, and the advantage of this method is the temperature of reaction height, speed of response is fast, single furnace output is big, and shortcoming is the technology instability, and the purity of product is not high.Therefore this method is not applied.Gondola Pierre Jia Nuofa is another kind of internal resistance heating magnesium-smelting silicothermic process technology, and the characteristics of this technology are that the internal resistance heating in the vacuum oven is to realize by the resistance heat of the sheet metal electric heating element in the stove.Reaction mass directly places on the flaky metal electric heating body, and the shortcoming of this method is because reaction mass directly places on the electric heating element, under hot conditions, resistance heater is corroded by reaction mass easily, cause the electric heating parameter instability of electric heating element, the life-span is short, the production cost height.For the production of magnesium by pidgeonprocess of outer heating, can use solid fuel, liquid fuel heat also can be used the external resistance heating, but heating efficiency is not high, is conducted heat and the restriction of body of heater material, and furnace space is little, and single furnace output is low, converter life is short, and productivity is low, the cost height.
Summary of the invention
Weak point at existing Mg-smelting furnace the invention provides a kind of inner resistance heating metallothermic reduction furnace for melting magnesium.
The present invention is to provide a kind of novel internal resistance heating of metal reduction refining magnesium vacuum smelting furnace, body of heater is that drum shape or square are barrel-shaped, this stove is made liner with refractory materials or carbonaceous material, it outside liner the heat-resisting alloy steel inboard wall of furnace body, fill insulant material between heat-resisting alloy steel inboard wall of furnace body and the furnace outer wall, and can be evacuated, can guarantee the distortion that heat-resisting alloy steel metal body of heater causes owing to the negative pressure in the furnace chamber and strengthen heat insulation effect under hot conditions.Furnace chamber built-in metal resistance heater can guarantee that the temperature in the furnace chamber reaches 1200～1300 ℃, and reaction mass is positioned between the electric heating element of the vertical arrangement of two rows in the furnace chamber, this stove has converter life long, and the furnace chamber volume is big, and single furnace output is big, the thermo-efficiency height, characteristic of low energy consumption.This stove has two chambers, and one is reduction reaction chamber, and resistance heater and furnace charge place this indoor.And another chamber is the crystallisation chamber of gaseous reaction products, and this chamber outer wall has watercooling jacket, and inwall has a crystallizer that is used for the congealing reaction product of being made by stainless steel.This crystallizer is close to the crystallisation chamber inwall, is that an end of being made by stainless steel does not have the end, the other end has foraminous cylinder at the end and the end.
The body of heater of this stove is that drum shape or square are barrel-shaped, one side body of heater is high-temperature vacuum reduction reaction furnace chamber, the other end is the crystallisation chamber of gaseous metal product, and the high-temperature vacuum reacting furnace-e/or is made by the high temperature heat-resisting steel, in be lined with refractory materials or carbonaceous material.The indoor high resistant resistance heater that the vertical arrangement of number row is arranged of Reaktionsofen, these resistance heater two ends are connected with metallic conductor, and metallic conductor is connected with external power.Put reaction mass between the indoor two vertical row's resistance heaters of Reaktionsofen.Between the inwall of high temperature reduction reacting furnace-e/or and the stove outer covering and between reaction furnace chamber bell inwall and the shell, light filling refractory materials or lagging material, and be evacuated.
Adopt the method for this stove production MAGNESIUM METAL as follows.
Rhombspar after at first will calcining or the product behind giobertite and the limestone calcination and ferrosilicon or sial reductive agent prepare material by stoichiometric ratio, and material is pressed into bulk, and the bulk material is placed between the vertical resistance heater of indoor two rows of Reaktionsofen.To react the furnace chamber bell then and the crystallisation chamber bell is closed, to reaction furnace chamber, crystallisation chamber, and between inboard wall of furnace body and the stove outer covering, vacuumize between bell inwall and the shell after, energising, by reacting furnace-e/or internal resistance heating element reaction mass is heated to 1200～1300 ℃, under vacuum condition (oxidation-reduction reaction takes place in system surplus pressure 1～13Pa), and the principal reaction equation is as follows:
2MgOCaO (Gu)+Si (Gu)=2Mg (gas)+2CaOSiO
2(Gu or liquid)
The crystallization of reaction product MAGNESIUM METAL is to the inwall of crystallizer, and the potassium that vapour pressure is higher in the product, the crystallization of sodium metallic impurity are on sodium potassium trap.Reaction charges into argon gas after finishing in stove, open the lid of crystallisation chamber end, and crystallization magnesium and crystallizer are together taken out outside the stove, and its physical sepn is taken out crystallization magnesium, opens the lid of reaction furnace chamber, takes out reacted residuum.Prepared MAGNESIUM METAL purity＞98%.
Mg-smelting furnace of the present invention not only is suitable for metallothermics production MAGNESIUM METAL, also can be used for basic metal and alkaline-earth metal or other metal that metallothermics is produced other high vapour pressures such as strontium, calcium, lithium.The vacuum distilling or the distillation that also can be used for above-mentioned metal are purified, or the recovery of above-mentioned secondary metals is purified.Adopt the method for Mg-smelting furnace refining magnesium of the present invention both to be different from Pidgeon process, also be different from the semi-continuous process and the gondola Pierre Jia Nuofa of France.This method realizes is the vacuum reducing Reaktionsofen with built-in resistance heater, and heating element does not directly contact with reaction mass, and the resistance heating body life time is long, does not need frequent maintenance, and production cost is low, does not have environmental pollution.
Description of drawings
Fig. 1 is the front view sketch of inner resistance heating metallothermic reduction furnace for melting magnesium of the present invention.
Fig. 2 is an inner resistance heating metallothermic reduction furnace for melting magnesium vertical view sketch.
Among Fig. 1, Fig. 2: 1 bell, 2 bell vacuum-pumping tubes, 3 furnace body outer walls, 4 heat-resisting alloy steel inboard wall of furnace body, 5 furnace linings are made 6 lagging materials by resistant to elevated temperatures Monofrax, 7 metal resistance heater, 8 stove external terminal, 9 high-temperature vacuum reduction reaction furnace chambers, 10 crystallisation chamber, 11 hot baffles, 12 crystallizers, 13 watercooling jackets, 14 vacuum-pumping tubes, 15 sodium potassium traps, 16 vacuum packing rings, 17 crystallisation chamber bells, 18 insulating layer of furnace body vacuum-pumping tubes.
Embodiment
As shown in Figure 1 and Figure 2, Mg-smelting furnace body of heater of the present invention is a drum shape, and this stove has two chambers, and an end of body of heater is a high-temperature vacuum reduction reaction furnace chamber 9, and the other end is the crystallisation chamber 10 of gaseous metal product.At crystallisation chamber 10 sidewalls vacuum-pumping tube 14 is set, sodium potassium trap 15 is set in crystallisation chamber 10.Crystallisation chamber 10 ports are pushed down 16 sealings of vacuum packing ring with crystallisation chamber bell 17 (flange).Crystallisation chamber 10 outer walls have watercooling jacket 13, crystallisation chamber 10 inwalls are provided with a crystallizer that is used for the congealing reaction product 12 of being made by stainless steel, crystallizer 12 is close to crystallisation chamber 10 inwalls, is that an end of being made by stainless steel does not have the end, the other end has foraminous cylinder at the end and the end.Between high-temperature vacuum reduction reaction furnace chamber 9 and crystallisation chamber 10, hot baffle 11 is set.This stove is made furnace lining 5 with refractory materials or carbonaceous material, it outside furnace lining 5 heat-resisting alloy steel inboard wall of furnace body 4, fill insulant material 6 between heat-resisting alloy steel inboard wall of furnace body 4 and the furnace body outer wall 3, and be evacuated, can guarantee the distortion that heat-resisting alloy steel metal body of heater causes owing to the negative pressure in the furnace chamber under hot conditions.Insulating layer of furnace body vacuum-pumping tube 18 is arranged on furnace body outer wall 3 sidewalls and is used to vacuumize.High-temperature vacuum reduction reaction furnace chamber 9 built-in metal resistance heaters 7 can guarantee that the temperature in the furnace chamber reaches 1200～1300 ℃, and metal resistance heater 7 two ends are connected with metallic conductor, and metallic conductor is connected with stove external terminal 8, can be connected with external power.Reaction mass is positioned between the metal resistance heater 7 of the vertical arrangement of two rows in the high-temperature vacuum reduction reaction furnace chamber 9.Metal resistance heater 7 marks are arranged vertical arrangement.Port at high-temperature vacuum reduction reaction furnace chamber 9 is pushed down 16 sealings of vacuum packing ring with bell 1, at bell 1 sidewall bell vacuum-pumping tube 2 is set and is used to vacuumize.This stove has converter life length, big, the single furnace output of furnace chamber volume is big, thermo-efficiency is high, characteristic of low energy consumption.
Adopt the method for this stove production MAGNESIUM METAL as follows.
Rhombspar after at first will calcining or the product behind giobertite and the limestone calcination and ferrosilicon or sial reductive agent prepare material by stoichiometric ratio, and material is pressed into bulk, the bulk material is placed between the vertical metal resistance heater 7 of two rows in the high-temperature vacuum reduction reaction furnace chamber 9.Then bell 1 and crystallisation chamber bell 17 are closed, to high-temperature vacuum reduction reaction furnace chamber 9, crystallisation chamber 10, and between furnace body outer wall 3 and the heat-resisting alloy steel inboard wall of furnace body 4, vacuumize between bell 1 inwall and the shell after, energising, by metal resistance heater in the reacting furnace-e/or 7 reaction mass is heated to 1200～1300 ℃, under vacuum condition (oxidation-reduction reaction takes place in system surplus pressure 1～13Pa), and the principal reaction equation is as follows:
2MgOCaO (Gu)+Si (Gu)=2Mg (gas)+2CaOSiO
2(Gu or liquid)
The crystallization of reaction product MAGNESIUM METAL is to the inwall of crystallizer 12, and the potassium that vapour pressure is higher in the product, the crystallization of sodium metallic impurity are on sodium potassium trap 15.Reaction charges into argon gas after finishing in stove, open crystallisation chamber bell 17, and crystallization magnesium and crystallizer 12 are together taken out outside the stove, and its physical sepn is taken out crystallization magnesium, opens bell 1, takes out reacted residuum.Prepared MAGNESIUM METAL purity＞98%.
Claims (5)
1, a kind of inner resistance heating metallothermic reduction furnace for melting magnesium, it is characterized in that body of heater is that drum shape or square are barrel-shaped, two chambers are arranged, one end of body of heater is a high-temperature vacuum reduction reaction furnace chamber (9), the other end is the crystallisation chamber (10) of gaseous metal product, at crystallisation chamber (10) sidewall vacuum-pumping tube (14) is set, sodium potassium trap (15) is set in crystallisation chamber (10), crystallisation chamber (10) port is pushed down vacuum packing ring (16) sealing with crystallisation chamber bell (17), crystallisation chamber (10) outer wall has watercooling jacket (13), crystallisation chamber (10) inwall is provided with a crystallizer (12), between high-temperature vacuum reduction reaction furnace chamber (9) and crystallisation chamber (10), hot baffle (11) is set, outside furnace lining (5) heat-resisting alloy steel inboard wall of furnace body (4), fill insulant material (6) between heat-resisting alloy steel inboard wall of furnace body (4) and the furnace body outer wall (3), and be evacuated, insulating layer of furnace body vacuum-pumping tube (18) is arranged on furnace body outer wall (3) sidewall, high-temperature vacuum reduction reaction furnace chamber (9) built-in metal resistance heater (7), metal resistance heater (7) two ends are connected with metallic conductor, metallic conductor is connected with stove external terminal (8), the port of high-temperature vacuum reduction reaction furnace chamber (9) is pushed down vacuum packing ring (16) sealing with bell (1), at bell (1) sidewall bell vacuum-pumping tube (2) is set.
2,, it is characterized in that the built-in vertical arrangement of metal resistance heater (7) of vacuum reducing reaction furnace chamber (9) according to the described inner resistance heating metallothermic reduction furnace for melting magnesium of claim 1.
3, according to the described inner resistance heating metallothermic reduction furnace for melting magnesium of claim 1, it is characterized in that crystallizer (12) is close to crystallisation chamber (10) inwall, be that an end of being made by stainless steel does not have the end, the other end has foraminous cylinder at the end and the end.
4,, it is characterized in that in high-temperature vacuum reduction reaction furnace chamber (9) placing response material between the metal resistance heater (7) of the vertical arrangement of two rows according to the described inner resistance heating metallothermic reduction furnace for melting magnesium of claim 1.
5, adopt the method for the described inner resistance heating metallothermic reduction furnace for melting magnesium refining of claim 1 magnesium, it is characterized in that processing step is as follows:
Rhombspar after at first will calcining or the product behind giobertite and the limestone calcination and ferrosilicon or sial reductive agent prepare material by stoichiometric ratio, and material is pressed into bulk, the bulk material is placed between the vertical metal resistance heater (7) of interior two rows of high-temperature vacuum reduction reaction furnace chamber (9), then bell (1) and crystallisation chamber bell (17) are closed, to high-temperature vacuum reduction reaction furnace chamber (9), crystallisation chamber (10), and between furnace body outer wall (3) and the heat-resisting alloy steel inboard wall of furnace body (4), after vacuumizing between bell (1) inwall and the shell, energising, by metal resistance heater in the reacting furnace-e/or (7) reaction mass is heated to 1200～1300 ℃, under system surplus pressure 1～13Pa vacuum condition, react, the crystallization of reaction product MAGNESIUM METAL is to the inwall of crystallizer (12), potassium in the product, the crystallization of sodium metallic impurity is on sodium potassium trap (15), after reaction finishes, in stove, charge into argon gas, open crystallisation chamber bell (17), together take out crystallization magnesium and crystallizer (12) outside the stove, its physical sepn is taken out crystallization magnesium, open bell (1), take out reacted residuum.
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN100342045C true CN100342045C (en) | 2007-10-10 |
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| 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 |
| CN104344715A (en) * | 2013-08-06 | 2015-02-11 | 宁夏鹏程致远自动化技术有限公司 | Vacuum leakage detecting method of magnesium metal smelting reduction furnace |
| CN108070727A (en) * | 2016-11-15 | 2018-05-25 | 镇江市润州金山金属粉末厂 | A kind of preparation facilities of Preparation of Metallic Strontium |
| CN109022826B (en) * | 2018-10-19 | 2023-11-24 | 西安银研镁业装备有限公司 | Reduction and refining integrated smelting system |
| CN109536709A (en) * | 2019-01-02 | 2019-03-29 | 北京科技大学 | A kind of improved metal magnesium, calcium smelt the cooling section for using reductive jar |
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| CN111057850B (en) * | 2020-01-03 | 2020-12-25 | 四川万邦胜辉新能源科技有限公司 | Method for preparing high-purity lithium metal by vacuum thermal reduction method |
| CN111097920B (en) * | 2020-01-03 | 2021-02-02 | 四川万邦胜辉新能源科技有限公司 | Method for producing magnesium-lithium alloy by gaseous co-condensation method |
| CN111495294A (en) * | 2020-04-24 | 2020-08-07 | 广东电网有限责任公司东莞供电局 | Reaction kettle device for bioengineering and use method thereof |
| CN114485148A (en) * | 2022-01-14 | 2022-05-13 | 中南大学 | High-temperature reaction-evaporative crystallization integrated smelting equipment and smelting method based on smelting equipment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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