CN107523701A - A kind of method of normal pressure silicothermic reduction magnesium metal - Google Patents
A kind of method of normal pressure silicothermic reduction magnesium metal Download PDFInfo
- Publication number
- CN107523701A CN107523701A CN201710725825.3A CN201710725825A CN107523701A CN 107523701 A CN107523701 A CN 107523701A CN 201710725825 A CN201710725825 A CN 201710725825A CN 107523701 A CN107523701 A CN 107523701A
- Authority
- CN
- China
- Prior art keywords
- magnesium
- normal pressure
- gas
- silicothermic reduction
- silicothermic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
- C22B5/04—Dry methods smelting of sulfides or formation of mattes by aluminium, other metals or silicon
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention discloses a kind of method of normal pressure silicothermic reduction magnesium metal, realizes reducing metal magnesium under normal pressure, specifically reduces the magnesium partial pressure around pellet using flowing gas, reaction is occurred continuously and healthily.This method has overturned conventional metals magnesium silicothermic reduction technique, solves the vacuum problem of traditional handicraft, and automatic continuous production can be achieved, increase heat transfer medium and heat transfer type simultaneously, the heat transfer efficiency between pellet is improved, production efficiency can be increased substantially, reduces production cost.Once this method Realizing Achievement converts, subversive impetus will be carried out to Smelting magnesium process bands.
Description
Technical field
The present invention relates to metal smelt field, and in particular to a kind of protective gas using high-speed circulating flowing reduces magnesium
The method of the silicothermic reduction reaction of partial pressure, can be promoted for reforming traditional magnesium metal smelting technique.
Background technology
Magnesium and magnesium alloy have that in light weight, specific strength is high, good toughness, damping performance are strong, thermal conductivity is good, electromagnetic shielding
Property many good characteristics such as good, easy processing and easy recycling, can be widely applied to Aero-Space, defence and military, traffic (bag
Include automobile, bullet train, track traffic, aircraft, motorcycle, electric bicycle etc.), 3C (computer, communication, household electrical appliances, electrical equipment and
Electronic product), sports equipment, the field such as medical material.Magnesium alloy has the potentiality for meeting any of the above industry requirement, is development
The extremely considerable light alloy material of prospect.
The conventional mode of the magnesium of industry refining at present has the methods of electrolytic chlorination magnesium and silicothermic process (also known as Pidgeon process), wherein
Most widely used method is silicothermic process.Smelting magnesium by silicothermic process is with dolime (CaOMgO), ferrosilicon and firefly
Stone flour is raw material, and walnut shape or jujube core shape raw material pelletizing (composition Si+MgO+CaF are prepared into by ball milling, dispensing2), lead to
Cross Si reduction MgO generation magnesium vapors (CaF2Mineralizer is used as in the reaction), it is condensed to obtain Crystalline Magnesium.Main reaction formula is：2
(MgO·CaO)+Si→2Mg(g)+2CaO·SiO2, vacuum needed for reaction is 13Pa (integral pressure), and temperature is 1200 DEG C
Left and right, reaction time are 10h or so.This method is high to vacuum level requirements, and heat transfer efficiency is low, causes production cycle length, energy
Consume height, low production efficiency, environmental pollution is big, labor intensity is high.
In recent years, traditional silicothermic reduction technique has obtained a certain degree of improvement.As patent No. CN204421605U is carried
Heat storage formula reduction furnace inside and outside a kind of perpendicular tank has been supplied, has improved heat transfer efficiency；Patent No. CN101698907A proposes a kind of base
In the raw material that preparing salt by working up seawater accessory substance (waste material) (bischofite) is silicothermic reduction reaction, cost of material is reduced；The patent No.
CN105420516A proposes a kind of new technology of continuity method electric furnace smelting magnesium metal, realize expect in production process it is not liftoff；Patent
Number CN102409185A proposes that a kind of rotation reductive jar prepares pure magnesium technique, shortening pelletizing heat transfer time；The patent No.
CN101376928A proposes a kind of smelting magnesium by microwave heating Pidgeon process technique, is heated using microwave heating uniformity feature；Specially
Profit CN104611563A and CN1664135A propose that carbon heat and aluminothermic process realize silicothermic reduction respectively.It is however, above-mentioned various new
Method does not have from the substantial reaction condition for changing silicothermic process：Reaction is still needed under higher vacuum (being less than 13Pa)
Carry out, heat transfer type is only radiant heat transfer, can not thoroughly solve smelting magnesium by silicothermic process high energy consumption, it is inefficient the problems such as.
The content of the invention
The present invention realizes prepared by the pure magnesium under normal pressure in view of the above-mentioned problems, propose a kind of method of normal pressure smelting magnesium,
This method substitutes the method vacuumized from the reaction condition for substantially changing silicothermic process, using gas as heat transfer medium and
Its strong heat convection improves the heat transfer efficiency between pellet, fundamentally thoroughly solves the high energy of smelting magnesium by silicothermic process
The problems such as consuming, be inefficient.
The present invention is achieved by the steps of：
(1) feed.The raw material pelletizing reacted for silicothermic reduction is placed in graphite material boat, is fitted into quartz ampoule, by stone
English pipe is put into three sections of temperature control furnaces.
(2) gas washing.By one end of quartz ampoule gas flow optimized valve closure, the other end is connected to vavuum pump, be evacuated to-
0.1MPa, then it is 0.1MPa to be passed through high purity inert gas to the integral pressure that purity is 99.99% by control valve, that is, completes 1
Secondary " gas washing ".So gas washing 2-6 times.High purity inert gas is continually fed into after completing gas washing.
(3) reaction and collection of products.It is 1100~1300 by one section temperature setting of three sections of temperature control furnaces close to gas access
DEG C, realize the heating to inert gas.It it is 1100~1300 DEG C by second segment temperature setting, this section is the portion of placing graphite material boat
Position, that is, the position of silicothermic reduction reaction occurs.It it is 200~700 DEG C by the 3rd section of (close to gas vent) temperature setting, in the section
Place magnesium collection of products device.After pelletizing fully reacts, it is set to be cooled to room temperature in the inert gas environment of flowing.
Described silicothermic reduction reaction is carried out at ambient pressure, and provides heat transfer medium by inert gas.
By the present invention in that the magnesium vapor molecule caused by the inert gas of flowing takes away reaction makes reactant (pellet) attached
Near magnesium partial pressure reduces, and reaches with vacuumizing identical effect in traditional silicothermic process.
The inert gas includes all not gases with magnesium vapor reaction, including but not limited to helium, neon, argon
Gas, Krypton, xenon or radon gas etc..
The inert gas heating-up temperature is 1100~1300 DEG C (preferably 1200~1250 DEG C).
The silicothermic reduction reaction zone temperature is 1100~1300 DEG C (preferably 1200~1250 DEG C).
The product collection zone temperature is 200~700 DEG C, and (it is preferably 200~400 DEG C of powder to collect product, and product is
Preferably 500~700 DEG C of Crystalline Magnesium).
The flow rates for being passed through inert gas are 0.5~5000LPM (preferably 10~500LPM).
The present invention is tested using only three sections of temperature control furnaces, it is not limited to three sections of temperature control furnaces.
Product prepared by the present invention includes but is not limited to Crystalline Magnesium, magnesium powder, magnesium ingot or magnesium ribbon etc..
Compared with traditional production method, the invention has the advantages that：
(1) inherently change the condition of silicothermic reduction, realize the progress that silicothermic reduction is reacted under normal pressure, solve silicon heat
The condition of high vacuum that needs is reduced, technique is simple.
(2) change its heat transfer medium and increase gaseous exchange heat exchange, improve the heat transfer efficiency between pellet, reduce reaction
Time, solve smelting magnesium by silicothermic process high energy consumption, it is inefficient the problems such as.
(3) this method possesses the potentiality of automation and large-scale production, can solve the problems such as millworker's labor intensity is big,
Fundamentally solves the heavy-polluted problem of the environment of plant.
In summary, the present invention have developed a kind of normal pressure magnesium-smelting silicothermic process technology, party's genealogy of law domestic initiation, have extremely strong
Novelty, and possess automation and large-scale production potentiality, once successfully realizing technical transform, magnesium industry will be reformed comprehensively
Labor intensity is high, reduction cycle is long, the present situation of high energy consumption high pollution, and brings considerable economic benefit.
Brief description of the drawings
Fig. 1 is the SEM pictures and EDS results that the present invention prepares Crystalline Magnesium.
Fig. 2 is the SEM pictures and EDS results that the present invention prepares Crystalline Magnesium.
Embodiment
The present invention is described in further detail with reference to embodiments：
Embodiment one：
(1) feed.The raw material pelletizing 180g reacted for silicothermic reduction is placed in graphite material boat, is fitted into quartz ampoule,
Quartz ampoule is put into three sections of temperature control furnaces.
(2) gas washing.By one end of quartz ampoule gas flow optimized valve closure, the other end of quartz ampoule is connected to vavuum pump,
- 0.1MPa is evacuated to, then it is 0.1MPa to be passed through high-purity argon gas to the integral pressure that purity is 99.99% by control valve, i.e.,
Complete 1 time " gas washing ".So gas washing 5 times.Argon gas, flow control 3LPM are continually fed into after completing gas washing.
(3) reaction and collection of products.It is 1100~1300 by one section temperature setting of three sections of temperature control furnaces close to gas access
DEG C (preferably 1200 DEG C), realize the heating to inert gas.It it is 1100~1300 DEG C (preferably 1200 by second segment temperature setting
DEG C), this section is the position of placing graphite material boat, that is, the position of silicothermic reduction reaction occurs.By the 3rd section (close to gas vent)
Temperature setting is 200~700 DEG C (preferably 500~700 DEG C), and magnesium collection of products device is placed in the section.Half an hour is incubated, when
After pelletizing fully reacts, it is set to be cooled to room temperature in the inert gas environment of flowing, magnesium collection of products area is collected into product and is
Pure magnesium.
Embodiment two：
(1) feed.The raw material pelletizing 180g reacted for silicothermic reduction is placed in graphite material boat, is fitted into quartz ampoule,
Quartz ampoule is put into three sections of temperature control furnaces.
(2) gas washing.By one end of quartz ampoule gas flow optimized valve closure, the other end of quartz ampoule is connected to vavuum pump,
- 0.1MPa is evacuated to, then it is 0.1MPa to be passed through high-purity argon gas to the integral pressure that purity is 99.99% by control valve, i.e.,
Complete 1 time " gas washing ".So gas washing 5 times.Argon gas, flow control 10LPM are continually fed into after completing gas washing.
(3) reaction and collection of products.It is 1100~1300 by one section temperature setting of three sections of temperature control furnaces close to gas access
DEG C (preferably 1200 DEG C), realize the heating to inert gas.It it is 1100~1300 DEG C (preferably 1200 by second segment temperature setting
DEG C), this section is the position of placing graphite material boat, that is, the position of silicothermic reduction reaction occurs.By the 3rd section (close to gas vent)
Temperature setting is 200~700 DEG C (preferably 500~700 DEG C), and magnesium collection of products device is placed in the section.Half an hour is incubated, when
After pelletizing fully reacts, it is set to be cooled to room temperature in the inert gas environment of flowing, magnesium collection of products area is collected into product and is
Pure magnesium.
Claims (9)
- A kind of 1. method of normal pressure silicothermic reduction magnesium metal, it is characterised in that comprise the following steps：(1) feed：The raw material pelletizing reacted for silicothermic reduction is placed in graphite material boat, is fitted into quartz ampoule, by quartz ampoule It is put into three sections of temperature control furnaces；(2) gas washing：By one end of quartz ampoule gas flow optimized valve closure, the other end of quartz ampoule is connected to vavuum pump, taken out true Empty extremely -0.1MPa, then it is 0.1MPa to be passed through high purity inert gas to the integral pressure that purity is 99.99% by control valve, i.e., Complete 1 gas washing, such gas washing 2-6 time, be continually fed into high purity inert gas after completion gas washing；(3) reaction and collection of products：It is 1100~1300 DEG C by one section temperature setting of three sections of temperature control furnaces close to gas access, it is real It it is 1100~1300 DEG C by second segment temperature setting now to the heating of inert gas, this section is the position of placing graphite material boat, i.e., The position of silicothermic reduction reaction occurs, 200~700 DEG C are arranged to close to gas outlet temperature by the 3rd section, magnesium is placed in the section Collection of products device, after pelletizing fully reacts, it is set to be cooled to room temperature in the inert gas environment of flowing.
- 2. the method for a kind of normal pressure silicothermic reduction magnesium metal according to claim 1, it is characterised in that silicothermic reduction is reacted Carry out at ambient pressure, and heat transfer medium is provided by inert gas.
- A kind of 3. method of normal pressure silicothermic reduction magnesium metal according to claim 1, it is characterised in that protective gas bag Include all not gases with magnesium vapor reaction, including but not limited to helium, neon, argon gas, Krypton, xenon or radon gas.
- 4. the method for a kind of normal pressure silicothermic reduction magnesium metal according to claim 1, it is characterised in that inert gas heats Temperature is 1100~1300 DEG C, preferably 1200~1250 DEG C.
- 5. the method for a kind of normal pressure silicothermic reduction magnesium metal according to claim 1, it is characterised in that silicothermic reduction is reacted Area's temperature is 1100~1300 DEG C, preferably 1200~1250 DEG C.
- A kind of 6. method of normal pressure silicothermic reduction magnesium metal according to claim 1, it is characterised in that product collection zone Temperature is 200~700 DEG C, and collection product is preferably 200~400 DEG C of powder, and product is preferably 500~700 DEG C of Crystalline Magnesium.
- A kind of 7. method of normal pressure silicothermic reduction magnesium metal according to claim 1, it is characterised in that the step (3) In to be passed through the flow rates of inert gas be 0.5~5000LPM, preferably 10~500LPM.
- A kind of 8. method of normal pressure silicothermic reduction magnesium metal according to claim 1, it is characterised in that the step (3) Tested using three sections of temperature control furnaces, it is not limited to three sections of temperature control furnaces.
- A kind of 9. method of normal pressure silicothermic reduction magnesium metal according to claim 1, it is characterised in that the product bag of preparation Include but be not limited to Crystalline Magnesium, magnesium powder, magnesium ingot or magnesium ribbon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710725825.3A CN107523701A (en) | 2017-08-22 | 2017-08-22 | A kind of method of normal pressure silicothermic reduction magnesium metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710725825.3A CN107523701A (en) | 2017-08-22 | 2017-08-22 | A kind of method of normal pressure silicothermic reduction magnesium metal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107523701A true CN107523701A (en) | 2017-12-29 |
Family
ID=60681830
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710725825.3A Pending CN107523701A (en) | 2017-08-22 | 2017-08-22 | A kind of method of normal pressure silicothermic reduction magnesium metal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107523701A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109930001A (en) * | 2019-04-28 | 2019-06-25 | 府谷县泰达煤化有限责任公司 | Mg9995B and the above primary magnesium ingot production technology |
| CN110273071A (en) * | 2019-07-19 | 2019-09-24 | 华西能源工业股份有限公司 | It is a kind of using inert gas blow and inside and outside combined heat the continuous magnesium smelting reducing furnace system of minute-pressure |
| CN113073211A (en) * | 2021-03-17 | 2021-07-06 | 西安交通大学 | Method for directly reducing powder into magnesium metal under inert gas carrying |
| CN113278821A (en) * | 2021-04-30 | 2021-08-20 | 西安交通大学 | Method for directly reducing metal magnesium by taking pure silicon powder as reducing agent |
| 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 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3918959A (en) * | 1973-12-28 | 1975-11-11 | Showa Denko Kk | Process for production of magnesium |
| WO2005103309A1 (en) * | 2004-04-26 | 2005-11-03 | Fos International S.A. | Metallothermic process for magnesium production and vacuum-induction furnace thereto |
| CN101967566A (en) * | 2010-11-04 | 2011-02-09 | 北京科技大学 | Process for preparing metal magnesium by normal pressure thermal reduction method |
| CN101985701A (en) * | 2010-11-11 | 2011-03-16 | 北京科技大学 | Method for reducing calcined magnesite by using calcium carbide under normal pressure |
| CN106191467A (en) * | 2016-07-12 | 2016-12-07 | 吉林市润成膜科技有限公司 | A kind of method that former Smelting magnesium prepares porous silicon simultaneously |
-
2017
- 2017-08-22 CN CN201710725825.3A patent/CN107523701A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3918959A (en) * | 1973-12-28 | 1975-11-11 | Showa Denko Kk | Process for production of magnesium |
| WO2005103309A1 (en) * | 2004-04-26 | 2005-11-03 | Fos International S.A. | Metallothermic process for magnesium production and vacuum-induction furnace thereto |
| CN101967566A (en) * | 2010-11-04 | 2011-02-09 | 北京科技大学 | Process for preparing metal magnesium by normal pressure thermal reduction method |
| CN101985701A (en) * | 2010-11-11 | 2011-03-16 | 北京科技大学 | Method for reducing calcined magnesite by using calcium carbide under normal pressure |
| CN106191467A (en) * | 2016-07-12 | 2016-12-07 | 吉林市润成膜科技有限公司 | A kind of method that former Smelting magnesium prepares porous silicon simultaneously |
Non-Patent Citations (1)
| Title |
|---|
| 唐祁峰等: "真空热还原氧化镁的理论分析与实验研究", 《真空科学与技术学报》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109930001A (en) * | 2019-04-28 | 2019-06-25 | 府谷县泰达煤化有限责任公司 | Mg9995B and the above primary magnesium ingot production technology |
| CN110273071A (en) * | 2019-07-19 | 2019-09-24 | 华西能源工业股份有限公司 | It is a kind of using inert gas blow and inside and outside combined heat the continuous magnesium smelting reducing furnace system of minute-pressure |
| CN113073211A (en) * | 2021-03-17 | 2021-07-06 | 西安交通大学 | Method for directly reducing powder into magnesium metal under inert gas carrying |
| CN113278821A (en) * | 2021-04-30 | 2021-08-20 | 西安交通大学 | Method for directly reducing metal magnesium by taking pure silicon powder as reducing agent |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107523701A (en) | A kind of method of normal pressure silicothermic reduction magnesium metal | |
| CN106498185B (en) | A kind of method of vacuum microwave refining magnesium | |
| CN105506318B (en) | A kind of production technology of extra super duralumin alloy | |
| CN103614593B (en) | A kind of refractory alloy with good thermal processability and preparation method thereof | |
| WO2018228141A1 (en) | Aluminum thermal self-propagation gradient reduction and slag washing and refining-based method for preparing tungsten-iron alloy | |
| CN109280781A (en) | A kind of method of decomposition and inversion Rare Earth Mine | |
| CN109941993A (en) | A kind of method of high vacuum low temperature purification graphite | |
| CN103773968B (en) | Method and system for removing gas and slag in aluminum melt by three-phase combination | |
| CN106591566B (en) | A kind of method that tungsten associated minerals smelt W metallurgy | |
| CN103938002B (en) | A kind of Cu-Cr-Zr alloy casting rod reduces the vacuum melting technique of segregation | |
| WO2024056108A1 (en) | Environmentally-friendly device for producing magnesium by means of aluminothermic reduction | |
| WO2024056107A1 (en) | Green and environmentally friendly method for producing magnesium by means of aluminothermic reduction | |
| CN105399106B (en) | The preparation method and device of a kind of high purity boron powder | |
| CN105460926A (en) | Boat-free natural graphite purification process | |
| CN102432020B (en) | Manufacturing method of solar grade polysilicon | |
| CN102808091B (en) | A kind of preparation method of high purity titanium | |
| CN104726738A (en) | Crystalline silicon waste treatment method | |
| CN102534221A (en) | Technology for recycling scrap copper in high-temperature vacuum nitrogen-charging cycle smelting manner | |
| CN103924103A (en) | Production technology of metal molybdenum | |
| CN101545042A (en) | Method for producing microalloy ferro-silicon by using a ferrous metasilicate electric stove integral deoxidation and reduction | |
| CN101805921B (en) | Preparation method of polycrystalline silicon | |
| CN102071271B (en) | Blast-furnace ironmaking raw material hot delivery and hot charging process and equipment | |
| CN102191344A (en) | Hot delivery and hot charging process of blast furnace iron making raw material and device thereof | |
| CN101545044B (en) | Method for producing ferro-silicon by using a ferrous metasilicate electric stove integral deoxidation and reduction | |
| CN104282355B (en) | A kind of copper-coated magnesium alloy wire rod and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171229 |