CN101289708A - Semi-continuous metallothermic reduction process - Google Patents

Semi-continuous metallothermic reduction process Download PDF

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Publication number
CN101289708A
CN101289708A CNA2008101063820A CN200810106382A CN101289708A CN 101289708 A CN101289708 A CN 101289708A CN A2008101063820 A CNA2008101063820 A CN A2008101063820A CN 200810106382 A CN200810106382 A CN 200810106382A CN 101289708 A CN101289708 A CN 101289708A
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liquid
crystallizer
reduction
tundish
jar
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CN101289708B (en
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辛卫亚
唐贤军
李文胜
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Abstract

The invention provides a method for semi continuous metallothermic reduction. In the method, a reduction pot is communicated with a liquid crystallizer arranged outside the reduction pot by a diversion device, therefore metal steams in the reduction pot enter the liquid crystallizer through the diversion device and are converted to liquid state and kept as the liquid state; liquid metal in the liquid crystallizer periodically and quantificationally flows into liquid pouring baskets; when a liquid pouring basket is filled up, another liquid pouring basket replaces the original liquid pouring basket to connect the liquid crystallizer so as to continuously collecting the liquid metal in the liquid crystallizer; after complete separation of the metal in the reduction pot, slag is removed, and new palletized feed stock is put in the reduction pot for starting a new reduction. The method has the advantages of realizing the semi continuous production of metal vacuum metallurgy, improving production efficiency and lowering production cost.

Description

Semicontinuous metallothermic reduction method
Technical field
The present invention relates to a kind of reduction jar for vacuum metal smelting, particularly a kind of vacuum melting and reducing tank that is used for smelting magnesium or calcium.
Background technology
Some vapour pressure higher alkali metal and alkaline-earth metal as clang, inscription, magnesium, calcium etc., can make with metallothermics under the condition of vacuum with silicon, aluminium or their alloy.Silicon heat or aluminothermy metallothermic reduction then obtain using the most widely among the metallothermic reduction preparation method of magnesium, but the many forms with ferro-silicon of its reductive agent are used, and the raw material that is reduced mostly is the rhombspar after the calcination, also can be with the forging after product of magnesite and Wingdale mixture.Use the ferrosilicon reductive agent, be called magnesium-smelting silicothermic process and use at most.
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 Pidgeon Process), 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.
Wherein most popular both at home and abroad is Pidgeon process, be raw material promptly and be that reductive agent refines magnesium with ferrosilicon (si-Fe) with calcination rhombspar (Mgo, Cao), raw material and reductive agent are mixed in proportion the back pressure to be rolled into a ball into pelletizing feed, then pelletizing feed is put into the reduction jar, jar adding reduction furnace high-temperature (1200 ℃) that will reduce again (reacts under 1~23.3Pa) environment with vacuum.After for some time, magnesium vapor is separated out from pelletizing feed, and is collected by crystallizer behind the arrival reduction tank top.General through after 11~12 hours recovery time, the magnesium metal base of a reduction jar originally could be separated out.Separate out finish after, also need reduction jar is removed, in the reduction jar of having removed, crystallizer is taken out again.At last, behind replacing reduction jar interior pelletizing feed and crystallizer, be reentered in the reduction furnace, so circulate and carry out.
Adopting the advantage of production of magnesium by pidgeonprocess is that method is simple, prolongs usefulness for a long time always, but the weak point of its existence pollutes except the energy consumption height, to environment, also has:
1, traditional reduction jar and crystallizer are to make that the magnesium vapor condensation-crystallization is solid-state the recovery, solid metal magnesium is put into carried out refining after refining furnace melts then.In also original production and refining are produced, all have the process that an intensification reaches phase transformation, not only production process is many, energy consumption is high, and causes production efficiency low, also some loss of magnesium metal output.
2, traditional production method, the production of MAGNESIUM METAL are to be the cycle with reduction cycle (general 11~12 hours), belong to be interrupted and produce, and go out the magnesium poor continuity, are unsuitable for big industrial production.
3, traditional production method, hand labor dependency height, poor working environment, job security is low, is unsuitable for big industrial production.
Therefore, also be necessary the apparatus and method of existing production of magnesium by pidgeonprocess are improved, to meet the needs that modern industry is produced.
Summary of the invention
At the deficiencies in the prior art, the objective of the invention is to: a kind of semicontinuous metallothermic reduction method is provided, solves the low problem of poor continuity, production efficiency that conventional metals vacuum metling exists.
For achieving the above object, the technical solution used in the present invention is:
A kind of semicontinuous metallothermic reduction method is characterized in that, may further comprise the steps:
(1) will reduce and jar be fixed in the reduction furnace, then pelletizing feed be joined in the reduction jar;
(2) will reduce jar sealing and vacuumize and reach production requirement, and then start reduction furnace reduction jar is heated, and reach and remain on working temperature;
(3) described reduction jar is communicated with by a guiding device and jar outside liquid crystallizer that reduces, and the metal vapors in the feasible reduction jar enters in the described liquid crystallizer by described guiding device;
(4) described liquid crystallizer comprises a crystallizer housing, described crystallizer housing has accommodation space, described liquid crystallizer is provided with the crystallizer vacuum extractor that is used for controlling the crystallizer heating control apparatus of accommodation space temperature and is used for controlling vacuum tightness in the accommodation space, the metal vapors temperature that enters in the liquid crystallizer reduces, be converted into liquid state, and remain on liquid state;
(5) described crystallizer housing also is provided with intermediate conduit, is used for being communicated with a liquid tundish; Liquid metal in the liquid crystallizer regularly, flow in the described liquid tundish quantitatively;
(6) after a liquid tundish is filled, change a liquid tundish and link to each other, to collect the liquid metal in the liquid crystallizer incessantly with liquid crystallizer;
(7) after to be restored jar of interior metal separated out and finished, will expect the slag removing, then put into new pelletizing feed, begin new reduction work.
In the preferable technical scheme, can also add following technical characterictic: described reduction jar vertically is arranged in the reduction furnace, all stretch out outside the described reduction furnace upper end, the lower end of reduction jar, a reduction jar upper end is provided with the mechanical charging mouth, the lower end is provided with mechanical discharge port, and described upper end or lower end are connected with described guiding device.
In the preferable technical scheme, can also add following technical characterictic: be installed with a guide shell in the described reduction jar, described guide shell is hollow tube-shape, its stack shell is provided with a plurality of holes that run through wall thickness, inside and external communications with guide shell, have the gap between the inwall of described guide shell and reduction jar, described gap can be placed for pelletizing feed.
In the preferable technical scheme, can also add following technical characterictic: also be provided with a plurality of air channels on the outer side wall of described guide shell, described air channel is interconnected described a plurality of holes.
In the preferable technical scheme, can also add following technical characterictic: described liquid crystallizer and guiding device junction are provided with crystallizer control valve group, and switch the connected state of accommodation space and guiding device by described crystallizer control valve group.
In the preferable technical scheme, can also add following technical characterictic: described liquid tundish comprises a tundish main body, has article containing space in the described tundish main body, described article containing space is connected by the accommodation space of described intermediate conduit with described crystallizer housing, described tundish main body is provided with the tundish heating control apparatus that is used for controlling the article containing space temperature and is used for controlling the tundish vacuum extractor of vacuum tightness in the article containing space, and described tundish main body also is provided with a liquid outlet that is used for discharge opeing.
In the preferable technical scheme, can also add following technical characterictic: described tundish main body external packets is covered with heat preserving and insulating material.
In the preferable technical scheme, can also add following technical characterictic: described intermediate conduit is provided with tundish control valve group, is used for controlling the connected state of liquid tundish and liquid crystallizer.
In the preferable technical scheme, can also add following technical characterictic: the material of described tundish main body is the Cr18Ni9Ti stainless material.
In the preferable technical scheme, can also add following technical characterictic: the material of described crystallizer housing is the Cr18Ni9Ti stainless material.
In the preferable technical scheme, can also add following technical characterictic: described crystallizer hull outside is coated with the heat insulating fiber.
Compared with prior art, the beneficial effect that has of the present invention is:
1, magnesium vapor liquid crystals in crystallizer maintains it liquid state and transports to refining in the refining furnace by tundish again, has saved solid metal magnesium phase transformation energy needed in refining furnace, has both reduced operation, has saved the energy again, has reduced production cost;
2, the charging of reduction jar, slagging tap does not influence the work of liquid crystallizer, has guaranteed the continuity of liquid crystallizer work, is the important assurance that realizes semicontinuous production;
3, the control by tundish control valve group, liquid magnesium are the essential condition that realizes semicontinuous production regularly, flow in the liquid tundish quantitatively.
4, the existence of guide shell makes that the circulation of magnesium vapor is more smooth and easy, has shortened the recovery time (reducing to 9~10 hours), has saved fuel, has shortened the work period, has improved production efficiency.
Description of drawings
Fig. 1 is the structural representation of the semicontinuous metallothermic reduction method of the present invention;
Fig. 2 is the structural representation of liquid crystallizer of the present invention;
Fig. 3 is the structural representation of liquid tundish of the present invention;
Fig. 4 is the structural representation after guide shell of the present invention is cut open from the centre;
Fig. 5 is the another kind of structural representation after guide shell of the present invention is cut open from the centre;
Fig. 6 is another structural representation after guide shell of the present invention is cut open from the centre.
Embodiment
For structure of the present invention and characteristics can be understood better, below will the present invention is described in detail by preferred embodiment and accompanying drawing bonded mode.In order to make structure of the present invention more clear, described accompanying drawing might change actual proportionlity in drawing process, and this is not appreciated that the qualification to present patent application.
As shown in Figure 1, be the structural representation of the semicontinuous metallothermic reduction method of the present invention, comprise reduction furnace 1, reduction jar 4, liquid crystallizer 8 and liquid tundish 20, wherein:
Described reduction furnace 1 adopts regenerative combustion technology, and is provided with body of heater 3 and burner 2, all is prior aries, will not give unnecessary details.
Described reduction jar 4 vertically is arranged in the body of heater 3 of reduction furnace 1, and stretch out outside the body of heater 3 at two ends.Wherein, reduction jar 4 upper ends are provided with mechanical charging mouth 5, and the lower end is provided with mechanical discharge port 6, can realize mechanize ground pan feeding and discharging.(in fact, also can be the upper end) sidepiece is connected with a piped guiding device 7 in reduction jar 4 lower ends, is used for the magnesium vapor in the reduction jar 4 is derived.Middle part in reduction jar 4 is installed with a guide shell 11, described guide shell 11 is that the heating resisting metal material (can anti-1300 ℃ of high temperature, as Cr25Ni20Si2 heat-resistance stainless steel material), and as shown in Figure 4, described guide shell 11 is hollow tube-shape, also has the gap between described guide shell 11 and reduction jar 4 inwalls, for placing pelletizing feed, guide shell 11 bottoms are provided with block body 12, avoid pelletizing feed to spill; On the stack shell of guide shell 11, be provided with a plurality of holes 14 that run through wall thickness, inside and external communications with guide shell 11, accelerate the speed of separating out of magnesium vapor, also be provided with a plurality of air channels 15 on the outer side wall of described guide shell 11 along its length, flow to described guiding device 7 along guide shell 11 for magnesium vapor.Described hole 14 does not need concrete restriction with shape, the size of air channel 15, and can ventilate gets final product, and certainly, spills in order to prevent pelletizing feed, and the width of hole 14 should be less than the diameter of pelletizing feed.And the setting of air channel 15 also can be increased and decreased according to actual needs, if the circulation speed of magnesium vapor can reach design requirements, just there is no need to offer described air channel 15; Circulation speed at magnesium vapor does not reach under the situation of design requirements, just is necessary to offer described air channel 15.
Wherein, in the present embodiment, described hole 14 is oval-shaped through holes, and described hole 14 also can be circular hole, polygonal hole or slotted hole.
What need replenish is that above-mentioned guiding device 7 is connected with described guide shell 11 inside after stretching into reduction jar 4, has good water conservancy diversion effect.In the present embodiment, described guiding device 7 is heating resisting metal material (can anti-1300 ℃ of high temperature, as Cr25Ni20Si2 heat-resistance stainless steel material), is shaped as pipe shape or square tube type and all can.
Described guiding device 7 overhanging ends connect described liquid crystallizer 8, and described liquid crystallizer 8 is provided with crystallizer control valve group 84 with guiding device 7 junctions.The internal structure of described liquid crystallizer 8, as shown in Figure 2, comprise crystallizer housing 81, crystallizer housing 81 materials preferably adopt the Cr18Ni9Ti stainless material, adopt the thick stainless steel plate punching press welding of 12mm to make, the crystallizer housing 81 outside heat insulating staplings of using are incubated (for simplicity, described heat insulating fiber does not give diagram, its material is an aluminium sesquioxide), described crystallizer housing 81 has accommodation space, and switches the connected state of accommodation space and guiding device 7 by described crystallizer control valve group 84.Also be provided with crystallizer heating control apparatus 82 and crystallizer vacuum extractor 83 on the described liquid crystallizer, described crystallizer heating control apparatus 82 (preferably adopting electric heater unit) makes crystallizer housing 81 interior temperature remain on certain limit, and (temperature controlling system belongs to prior art, do not repeat them here), thereby transform and remain on liquid state after making magnesium vapor enter liquid crystallizer 8, described crystallizer vacuum extractor 83 makes in the accommodation space of housing 81 of crystallizer 8 and remains on predetermined vacuum tightness.
Described liquid tundish 20 communicates by the accommodation space of intermediate conduit 21 with described liquid crystallizer 8, and described intermediate conduit 21 is provided with tundish control valve group 22, to switch the connected state of liquid tundish 20 and liquid crystallizer.The concrete structure of described liquid tundish 20, as shown in Figure 3, comprise one tundish main body 23, the material of tundish main body 23 is the Cr18Ni9Ti stainless material, adopt the thick stainless steel plate punching press welding of 8mm to make, tundish main body 23 external packets are covered with heat preserving and insulating material (for simplicity, described heat preserving and insulating material does not give diagram, its material is an aluminium sesquioxide), has article containing space in the tundish main body 23, described tundish main body 23 is provided with tundish heating control apparatus 24 and tundish vacuum extractor 25, described tundish heating control apparatus 24 (preferably adopting electric heater unit) makes liquid tundish 20 interior temperature remain on certain limit, and (temperature controlling system belongs to prior art, do not repeat them here), thereby remain on liquid state after making liquid magnesium enter liquid tundish 8, described tundish vacuum extractor 25 makes in the article containing space of tundish main body 23 and remains on predetermined vacuum tightness.Described tundish main body 23 also is provided with a liquid outlet 26, is used for the liquid magnesium in the article containing space is discharged, to descend refining procedure one.
Below introduce how to use above-mentioned semicontinuous metallothermic reduction method, may further comprise the steps:
(1) guide shell 11 is fixed in the reduction jars 4, and will reduce and jars 4 be fixed in the reduction furnace 1, pelletizing feed is joined inside and outside the interior guide shell 11 of reduction jars 4;
(2) will reduce jars 4 sealings and vacuumize and reach production requirement, then starting 1 pair of reduction jar 4 of reduction furnace heats, after reaching working temperature, magnesium vapor is separated out from pelletizing feed, and the hole 14 by guide shell 11 and air channel 15 arrive described guiding device 7, enters the liquid crystallizer 8 from guiding device 7 then;
(3) the magnesium vapor temperature that enters in the liquid crystallizer 8 reduces, and is converted into liquid state, and remains on liquid state;
(4) control by described tundish control valve group 22, the liquid magnesium in the liquid crystallizer 8 regularly, flow in the liquid tundish 20 quantitatively, to realize semicontinuous production;
(5) after liquid tundish 20 is filled, transport to refining in the refining furnace; Simultaneously, changing a liquid tundish 20 links to each other with liquid crystallizer 8; So, do not stop to change and transport liquid tundish 20;
(6) after to be restored jar 4 interior MAGNESIUM METAL separated out and finished, close described crystallizer control valve group 84, jar 4 bottom mechanical discharge ports 6 that will reduce are then opened, and will expect the slag removing, then, close mechanical discharge port 6, open power feed mouth 5, put into new pelletizing feed, vacuumize, open described crystallizer control valve group 84, begin new reduction work.
Use the metal vacuum smelting reduction device and the method for reducing of semi-continuous production of the present invention, compared with prior art, have following advantage:
1, magnesium vapor liquid crystals in crystallizer maintains it liquid state and transports to refining in the refining furnace by tundish again, has saved solid metal magnesium phase transformation energy needed in refining furnace, has both reduced operation, has saved the energy again, has reduced production cost;
2, the charging of reduction jar, slagging tap does not influence the work of liquid crystallizer, has guaranteed the continuity of liquid crystallizer work, is the important assurance that realizes semicontinuous production;
3, the control by tundish control valve group, liquid magnesium are the essential condition that realizes semicontinuous production regularly, flow in the liquid tundish quantitatively.
4, the existence of guide shell makes that the circulation of magnesium vapor is more smooth and easy, has shortened the recovery time (reducing to 9~10 hours), has saved fuel, has shortened the work period, has improved production efficiency.
As shown in Figure 5, be another structure formation of guide shell, it is compared with Fig. 4, and difference is: air channel 15 is the circumferential settings along guide shell 11, so the air channel 15 that is provided with can be communicated with each hole 14 get up equally, promotes the circulation speed of magnesium vapor.
And as shown in Figure 6, be again another structure formation of guide shell, compare with previous embodiment, its difference is: part air channel 15 is provided with along its length, a part of in addition air channel 15 is along circumferentially being provided with, so the air channel 15 that is provided with can further be promoted the contact between each hole 14, improves the circulation speed of magnesium vapor again, thereby improves the production efficiency of MAGNESIUM METAL.In addition, in the present embodiment, hole 14 and air channel 15 have used polygonal shape, also are different places.
In fact, under the prerequisite of the structural strength that does not influence guide shell 11, the bearing of trend of air channel 15 can also be changed, for example be arranged to volution or arachnoid, all be fine.
In the foregoing description, be that smelting with MAGNESIUM METAL is example explanation the application's structure and characteristics, and in fact, the inventive method and device are equally applicable to smelt vapour pressure higher alkali metal and alkaline-earth metal such as clang, inscription, calcium, difference wherein to those skilled in the art, belong to common practise, do not repeat them here.
More than explanation is just illustrative for the purpose of the present invention; and nonrestrictive, those of ordinary skills understand, under the situation of the spirit and scope that do not break away from claim and limited; can make many modifications, variation or equivalence, but all will fall within protection scope of the present invention.

Claims (11)

1, a kind of semicontinuous metallothermic reduction method is characterized in that, may further comprise the steps:
(1) will reduce and jar be fixed in the reduction furnace, then pelletizing feed be joined in the reduction jar;
(2) will reduce jar sealing and vacuumize and reach production requirement, and then start reduction furnace reduction jar is heated, and reach and remain on working temperature;
(3) described reduction jar is communicated with by a guiding device and jar outside liquid crystallizer that reduces, and the metal vapors in the feasible reduction jar enters in the described liquid crystallizer by described guiding device;
(4) described liquid crystallizer comprises a crystallizer housing, described crystallizer housing has accommodation space, described liquid crystallizer is provided with the crystallizer vacuum extractor that is used for controlling the crystallizer heating control apparatus of accommodation space temperature and is used for controlling vacuum tightness in the accommodation space, the metal vapors temperature that enters in the liquid crystallizer reduces, be converted into liquid state, and remain on liquid state;
(5) described crystallizer housing also is provided with intermediate conduit, is used for being communicated with a liquid tundish; Liquid metal in the liquid crystallizer regularly, flow in the described liquid tundish quantitatively;
(6) after a liquid tundish is filled, change a liquid tundish and link to each other, to collect the liquid metal in the liquid crystallizer incessantly with liquid crystallizer;
(7) after to be restored jar of interior metal separated out and finished, will expect the slag removing, then put into new pelletizing feed, begin new reduction work.
2, semicontinuous metallothermic reduction method according to claim 1, it is characterized in that: described reduction jar vertically is arranged in the reduction furnace, all stretch out outside the described reduction furnace upper end, the lower end of reduction jar, a reduction jar upper end is provided with the mechanical charging mouth, the lower end is provided with mechanical discharge port, and described upper end or lower end are connected with described guiding device.
3, semicontinuous metallothermic reduction method according to claim 1 and 2, it is characterized in that: be installed with a guide shell in the described reduction jar, described guide shell is hollow tube-shape, its stack shell is provided with a plurality of holes that run through wall thickness, inside and external communications with guide shell, have the gap between the inwall of described guide shell and reduction jar, described gap can be placed for pelletizing feed.
4, semicontinuous metallothermic reduction method according to claim 1 is characterized in that: also be provided with a plurality of air channels on the outer side wall of described guide shell, described air channel is interconnected described a plurality of holes.
5, semicontinuous metallothermic reduction method according to claim 1, it is characterized in that: described liquid crystallizer and guiding device junction are provided with crystallizer control valve group, and switch the connected state of accommodation space and guiding device by described crystallizer control valve group.
6, semicontinuous metallothermic reduction method according to claim 1, it is characterized in that: described liquid tundish comprises a tundish main body, has article containing space in the described tundish main body, described article containing space is connected by the accommodation space of described intermediate conduit with described crystallizer housing, described tundish main body is provided with the tundish heating control apparatus that is used for controlling the article containing space temperature and is used for controlling the tundish vacuum extractor of vacuum tightness in the article containing space, and described tundish main body also is provided with a liquid outlet that is used for discharge opeing.
7, semicontinuous metallothermic reduction method according to claim 6 is characterized in that: described tundish main body external packets is covered with heat preserving and insulating material.
8, semicontinuous metallothermic reduction method according to claim 6, it is characterized in that: described intermediate conduit is provided with tundish control valve group, is used for controlling the connected state of liquid tundish and liquid crystallizer.
9, semicontinuous metallothermic reduction method according to claim 6, it is characterized in that: the material of described tundish main body is the Cr18Ni9Ti stainless material.
10, semicontinuous metallothermic reduction method according to claim 1, it is characterized in that: the material of described crystallizer housing is the Cr18Ni9Ti stainless material.
11, semicontinuous metallothermic reduction method according to claim 1, it is characterized in that: described crystallizer hull outside is coated with the heat insulating fiber.
CN2008101063820A 2008-05-13 2008-05-13 Semi-continuous metallothermic reduction process Expired - Fee Related CN101289708B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102286668A (en) * 2008-12-15 2011-12-21 辛卫亚 Tilting charge and discharge type reducing furnace and reducing method thereof
CN105039744A (en) * 2015-07-28 2015-11-11 宋开泉 Method for preparing solid carbon dioxide and calcium metal through calcite
CN105525108A (en) * 2015-12-16 2016-04-27 东北大学 Method for preparing magnesium-calcium alloy through aluminothermic reduction
CN113737019A (en) * 2021-08-25 2021-12-03 西安交通大学 Method and device for continuously extracting crystallized magnesium in Pidgeon magnesium smelting process at high temperature

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2713751B1 (en) * 1993-12-15 1996-01-19 Pechiney Electrometallurgie Method and device for condensing metallic vapors in the liquid state.
CN2265379Y (en) * 1996-12-21 1997-10-22 蒋黎民 Device for obtaining mangesium by induction heating reduction
CN2701875Y (en) * 2004-06-16 2005-05-25 罗希文 Vacuum reduction magnesium continuously making equipment using electrothermal furnace

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102286668A (en) * 2008-12-15 2011-12-21 辛卫亚 Tilting charge and discharge type reducing furnace and reducing method thereof
CN105039744A (en) * 2015-07-28 2015-11-11 宋开泉 Method for preparing solid carbon dioxide and calcium metal through calcite
CN105525108A (en) * 2015-12-16 2016-04-27 东北大学 Method for preparing magnesium-calcium alloy through aluminothermic reduction
CN113737019A (en) * 2021-08-25 2021-12-03 西安交通大学 Method and device for continuously extracting crystallized magnesium in Pidgeon magnesium smelting process at high temperature

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Assignee: Hengtuo Energy & Environment Engineering Tech Co., Ltd., Beijing

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