CN101376928B - Process for smelting magnesium by microwave heating Pidgeon process - Google Patents

Process for smelting magnesium by microwave heating Pidgeon process Download PDF

Info

Publication number
CN101376928B
CN101376928B CN2008102328551A CN200810232855A CN101376928B CN 101376928 B CN101376928 B CN 101376928B CN 2008102328551 A CN2008102328551 A CN 2008102328551A CN 200810232855 A CN200810232855 A CN 200810232855A CN 101376928 B CN101376928 B CN 101376928B
Authority
CN
China
Prior art keywords
magnesium
heating
reduction jar
pelletizing
microwave
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.)
Expired - Fee Related
Application number
CN2008102328551A
Other languages
Chinese (zh)
Other versions
CN101376928A (en
Inventor
李万绪
郝建学
帅林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chongqing Kejian Metallurgy Material Co., Ltd.
Original Assignee
Chongqing Gaoling Investment (Group) Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Chongqing Gaoling Investment (Group) Co Ltd filed Critical Chongqing Gaoling Investment (Group) Co Ltd
Priority to CN2008102328551A priority Critical patent/CN101376928B/en
Publication of CN101376928A publication Critical patent/CN101376928A/en
Application granted granted Critical
Publication of CN101376928B publication Critical patent/CN101376928B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Manufacture And Refinement Of Metals (AREA)
  • Furnace Details (AREA)

Abstract

The invention discloses a magnesium reduction process through a micro-wave heating silicothermic method; the process comprises the following steps: 1. dolomite calcinations: the dolomite is heated to 1100 DEG C to 1200 DEG C and becomes calcined dolomite; 2. the calcined dolomite, silicon nitride powder and fluorite powder are weighed, mixed, milled and then pressed into a ball which meets technological requirements; 3. the ball is put into a closed non-metal reduction tank of a micro-wave heating oven to be heated under 1000 DEG C to 1200 DEG C, so that the magnesium compound in the ball reacts with the silicon nitride powder; 4. the vacuum degree of the closed non-metal reduction tank is kept to be 13.3Pa or higher for 4h to 6h; magnesium vapor is condensed in a condenser and becomes crude magnesium; 5. the crude magnesium is heated, melted and refined by solvent, to obtain refined magnesium; 6. acid washing and the like. The method evenly and quickly heats in the principle of micro-wave heating with high heating efficiency, is easy to be controlled, saves production cost, is safe, environment protective and harmless.

Description

The technology of smelting magnesium by microwave heating Pidgeon process
Technical field
The present invention relates to a kind of processing method of production of magnesium by pidgeonprocess, especially microwave heating technique is applied to the processing method of Pidgeon process (also being silicothermic process) refining magnesium.
Background technology
Pidgeon process production MAGNESIUM METAL is to be that raw material, ferrosilicon are that reductive agent, fluorite are catalyzer with the calcined dolomite, carries out batching, proportionally mixes after the batching.Suppress balling-up behind the grinding, be called pelletizing.With pelletizing pack into the reduction jar in, be heated to 1200 ℃, inside is evacuated to 13.3Pa or higher, then produces magnesium vapor.Magnesium vapor forms crystallization magnesium in the condenser of reduction jar front end, also claim crude magnesium.Again through flux-refining, output commodity magnesium ingot, promptly smart magnesium.Production of magnesium by pidgeonprocess main chemical reactions formula is:
(1) rhombspar is calcined in rotary kiln, shaft furnace or sleeve kiln:
Figure G2008102328551D00011
(2) reduction reaction in the reduction jar
Figure G2008102328551D00012
Traditional technology is to the type of heating of reduction jar, be heating unit to be set in the outside of reduction jar, the heating of employing external heating, by thermal conduction add the thermal reduction jar with and interior pelletizing material, its deficiency is mainly reflected in following several aspect: 1, energy consumption is big, the heat energy utilization rate is low, approximately have only about 24%, normally directly adopt coal-fired or fire coal is converted into the heating that acts as a fuel behind the coal gas and use, 1 ton of MAGNESIUM METAL of every production approximately needs 10 tons of fat coals, calculate if press the coal power generation coal consumption of 2.5kwh/kg, being equivalent to power consumption is 25000kwh, has consumed a large amount of resources.2, the refining magnesium cycle long, needs 8~12 hours.3, owing to adopt indirect heating, inside vacuumizes, and now is easy to oxidizedly with heating resisting metal reduction jar, produces distortion etc., and work-ing life is short, the longest use 2 months.Need to change continually the reduction jar that burns out, increase cost, reduce work efficiency.4, in the smelting reducing operation, produced environmentally harmful effluent discharge such as a large amount of carbonic acid gas and flue dust, polluted environment.
Summary of the invention
The present invention is directed to the above-mentioned deficiency of prior art production of magnesium by pidgeonprocess technology, the technology of the smelting magnesium by microwave heating Pidgeon process of a kind of thermo-efficiency height, save energy, low, the no carbonic acid gas of smelting cost and soot emissions is provided.
Technical scheme of the present invention: the technology of smelting magnesium by microwave heating Pidgeon process comprises the steps:
1, dolomite calcination: rhombspar is heated to 1100~1200 ℃ in rotary kiln, shaft furnace or sleeve kiln, burns till and forge white (MgOCaO);
2, batching system ball: will forge white, ferrosilicon powder and fluorite powder batching, grinding, and be pressed into the pelletizing that meets processing requirement then;
3, pelletizing is placed in the airtight nonmetal reduction jar in the microwave oven, starting microwave oven heats pelletizing, Heating temperature reacts magnesium compound and ferrosilicon powder in the pelletizing between 1000 ℃~1200 ℃, and the MAGNESIUM METAL that reaction generates exists with the form of magnesium vapor;
4, the vacuum tightness that keeps airtight nonmetal reduction jar is to 13.3Pa or higher, and the time length is at 4~6 hours, and magnesium vapor becomes crude magnesium after the condensation being connected, being arranged in the condenser of microwave oven outside with airtight nonmetal reduction jar front end;
5, with the crude magnesium heat fused, under 680 ℃~750 ℃ temperature, after solvent refined, cast magnesium ingot, obtain smart magnesium.
The technology of smelting magnesium by microwave heating Pidgeon process of the present invention with respect to prior art, has following characteristics:
1, utilize the principle of microwave heating, in a single day heated object puts into microwave electric field, and polar molecule wherein and non-polar molecule just cause polarization, become even molecule.According to the direction of an electric field orientation, because this electric field belongs to alternating electric field, so dipole just causes rotation and vibrations along with electric field change, for example frequency is 2.45GHz, rotation and vibrations with per second 2,400,000,000 5 thousand ten thousand times, produced the effect that is similar to phase mutual friction between the molecule, thereby absorbed the energy of electric field and generate heat, made object itself become heating element.Do not need heat conducting process, therefore can reach even rapid heating at short notice, the heating efficiency height makes heating object can reach required temperature fast.Reduce the reduction reaction time, thereby shorten the whole refining magnesium cycle, can shorten to 4~6 hours from original 8~12 hours.
2, microwave has different effects to different substances, contains the polar material and absorbs microwave energy easily and generate heat.Therefore do not contain polarity and then seldom absorb microwave heating, heat with strong pointsly, the ineffectivity of other dielectric material heating is improved greatly.Heat utilization efficiency significantly improves, and makes reduction reaction finish fully fast, reduces production energy consumption.
3, be easy to control; Only to object heating itself, air heats hardly in body of heater, the furnace chamber, so thermal inertia is minimum when heating, and appliance computer control is suitable for the standard and the automatization control of heat-processed and heating process especially.
4, substituted original heat-resistance stainless steel reduction jar with nonmetal reduction jar, improve the work-ing life of reduction jar, reduced the consumption of reduction jar, saves production cost.
5, safe, environmentally friendly; Usually micro-wave energy is to work in metal closed heating He in the waveguide, so the leakage of energy is minimum, the microwave leakage amount is all in the safety standards scope that country formulates.Adopt microwave heating, do not produce environmentally harmful effluent discharge such as carbonic acid gas, cinder and flue dust, free from environmental pollution, environment protection is had outstanding effect.
Embodiment
The technology of smelting magnesium by microwave heating Pidgeon process of the present invention comprises the steps:
1, dolomite calcination: rhombspar is heated to 1100~1200 ℃ in rotary kiln, shaft furnace or sleeve kiln, burns till and forge white (MgOCaO);
2, batching system ball: will forge white, ferrosilicon powder and fluorite powder batching, grinding, and be pressed into the pelletizing that meets processing requirement then; The above-mentioned proportion scale of forging white, ferrosilicon powder and fluorite powder adopts the proportion scale of prior art;
3, pelletizing is placed in the airtight nonmetal reduction jar in the microwave oven, starting microwave oven heats pelletizing, Heating temperature reacts magnesium compound and ferrosilicon powder in the pelletizing between 1000 ℃~1200 ℃, and the MAGNESIUM METAL that reaction generates exists with the form of magnesium vapor; Available temperature is 1000 ℃, 1050 ℃, 1100 ℃, 1130 ℃, 1150 ℃, 1180 ℃, 1200 ℃ etc.
4, the vacuum tightness that keeps airtight nonmetal reduction jar is to 13.3Pa or higher, and the time length is at 4~6 hours, and magnesium vapor becomes crude magnesium after the condensation being connected, being arranged in the condenser of microwave oven outside with airtight nonmetal reduction jar front end; The available time period is 4 hours, 4.5 hours, 5 hours, 5.5 hours equal times;
5, with the crude magnesium heat fused, under 680 ℃~750 ℃ temperature, after solvent refined, cast magnesium ingot, obtain smart magnesium.Available temperature is 680 ℃, 700 ℃, 720 ℃, 740 ℃, 750 ℃ etc.
6, pickling: magnesium ingot with sulfuric acid or nitric acid clean surface, is removed the surface and is mingled with, make surface aesthetic.
7, other explanation: airtight reduction jar is a nonmetallic ceramics class container, and refractoriness is greater than 1350 ℃, and intensity can satisfy the following vacuum tightness service requirements of 13.3Pa, has good microwave penetration performance, suitable microwave heating technique requirement.The reduction jar adopts the flangeseal mode of connection with condenser, reaches the vacuum tightness service requirements.The microwave frequency range that microwave heating is used is: 915 megahertzes and 2450 megahertzes.

Claims (3)

1. the technology of smelting magnesium by microwave heating Pidgeon process is characterized in that comprising the steps:
(1), dolomite calcination: rhombspar is heated to 1100~1200 ℃ in rotary kiln or shaft furnace, burns till and forge white (MgOCaO);
(2), batching system ball: will forge white, ferrosilicon powder and fluorite powder batching, grinding, and be pressed into the pelletizing that meets processing requirement then;
(3), pelletizing is placed in the airtight nonmetal reduction jar in the microwave oven, starting microwave oven heats pelletizing, Heating temperature reacts magnesium compound and ferrosilicon powder in the pelletizing between 1000 ℃~1130 ℃, and the MAGNESIUM METAL that reaction generates exists with the form of magnesium vapor;
(4), the vacuum tightness that keeps airtight nonmetal reduction jar is to 13.3Pa or higher, the time length is at 4~6 hours, magnesium vapor becomes crude magnesium after the condensation being connected, being arranged in the condensing works of microwave oven outside with airtight nonmetal reduction jar front end;
(5), with the crude magnesium heat fused, under 680 ℃~750 ℃ temperature, after solvent refined, cast magnesium ingot, obtain smart magnesium.
2. the technology of smelting magnesium by microwave heating Pidgeon process according to claim 1 is characterized in that: the microwave frequency range that described microwave oven uses is: 915 megahertzes and 2450 megahertzes.
3. the technology of smelting magnesium by microwave heating Pidgeon process according to claim 1 and 2 is characterized in that: described reduction jar is a nonmetallic ceramics class container, and reduction jar is connected with condenser employing flangeseal.
CN2008102328551A 2008-10-10 2008-10-10 Process for smelting magnesium by microwave heating Pidgeon process Expired - Fee Related CN101376928B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2008102328551A CN101376928B (en) 2008-10-10 2008-10-10 Process for smelting magnesium by microwave heating Pidgeon process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2008102328551A CN101376928B (en) 2008-10-10 2008-10-10 Process for smelting magnesium by microwave heating Pidgeon process

Publications (2)

Publication Number Publication Date
CN101376928A CN101376928A (en) 2009-03-04
CN101376928B true CN101376928B (en) 2011-01-12

Family

ID=40420667

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2008102328551A Expired - Fee Related CN101376928B (en) 2008-10-10 2008-10-10 Process for smelting magnesium by microwave heating Pidgeon process

Country Status (1)

Country Link
CN (1) CN101376928B (en)

Families Citing this family (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101892395B (en) * 2010-06-12 2013-01-09 安泰科技股份有限公司 Method for smelting magnesium by decomposition in vacuum through microwaves
CN102409185A (en) * 2011-11-14 2012-04-11 宁夏华亿镁业股份有限公司 Novel reduction method in Pidgeon magnesium smelting process
CN102534254A (en) * 2012-03-28 2012-07-04 瓮福(集团)有限责任公司 Method with high magnesium phosphorus gangue as raw materials to prepare metal magnesium
CN102534253A (en) * 2012-03-28 2012-07-04 瓮福(集团)有限责任公司 Method using high magnesium phosphorus gangue smelting reduction to prepare metal magnesium
CN103602833B (en) * 2013-11-15 2015-02-25 吴永 Improved pidgeon-process magnesium refining process
CN103589879A (en) * 2013-11-20 2014-02-19 北京环宇冠川等离子技术有限公司 Magnesium metal smelting method and device employing plasma torch heating technology
CN103882247B (en) * 2014-04-10 2015-09-02 于洪喜 Microwave heating refining magnesium technology
CN105420516B (en) * 2015-11-09 2017-11-21 孙克本 The new process of continuity method electric furnace smelting magnesium metal
JP2017088974A (en) * 2015-11-13 2017-05-25 オリコン・エナジー株式会社 Magnesium smelting apparatus and smelting method using microwaves
CN105567969B (en) * 2015-12-17 2018-06-08 于洪喜 Microwave carbon method process for smelting magnesium
JP5945373B1 (en) * 2016-01-13 2016-07-05 オリコン・エナジー株式会社 Magnesium smelting apparatus and smelting method using microwaves
JP6077164B1 (en) * 2016-06-10 2017-02-08 オリコン・エナジー株式会社 Smelting raw material pellet having resonance structure and smelting raw material using the same
CN106282605A (en) * 2016-09-14 2017-01-04 李华梅 Magnesium oxide produces magnesium metal with carbon with vacuum microwave heating
CN106498185B (en) * 2016-11-01 2018-08-31 深圳市中启新材料有限公司 A kind of method of vacuum microwave refining magnesium
CN107400789A (en) * 2017-01-18 2017-11-28 青海丰瑞镁业有限公司 A kind of magnesium crystal filter and crude magnesium reduction filtering purifying technique
CN107058762A (en) * 2017-05-09 2017-08-18 安徽工业大学 It is a kind of for pelletizing of smelting magnesium and preparation method thereof
CN107090547A (en) * 2017-05-17 2017-08-25 西安建筑科技大学 It is a kind of to reduce the method that magnesium process prepares AL-Si-Fe alloy and reduces magnesium in Pidgeon process
CN109055779A (en) * 2018-09-19 2018-12-21 成都先进金属材料产业技术研究院有限公司 The method of refining of magnesium refining agent and preparation method thereof and high purity magnesium
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
CN112267018A (en) * 2020-09-29 2021-01-26 朱广东 Aluminum magnesium co-production process
CN113737019B (en) * 2021-08-25 2022-06-21 西安交通大学 Method and device for continuous extraction of crystalline magnesium in Pidgeon magnesium smelting process at high temperature
CN113774235B (en) * 2021-08-25 2022-06-21 西安交通大学 Method and device for intermittently and continuously extracting crystallized magnesium in Pidgeon magnesium smelting
CN114892026B (en) * 2022-04-22 2024-06-11 五台云海镁业有限公司 Improved Pidgeon process magnesium smelting production process

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2457173Y (en) * 2000-10-30 2001-10-31 祁孙成 Vacuum smelting furnace for high-purity metal magnesium

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN2457173Y (en) * 2000-10-30 2001-10-31 祁孙成 Vacuum smelting furnace for high-purity metal magnesium

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
徐日瑶.硅热法炼镁生产工艺学.《硅热法炼镁生产工艺学》.中南大学出版社,2003,54-57,109,101,120-124. *
朱祖武等.国内皮江法炼镁技术的缺陷与改进途径.南昌高专学报 2.2007,(2),92-94.
朱祖武等.国内皮江法炼镁技术的缺陷与改进途径.南昌高专学报 2.2007,(2),92-94. *
郑英等.微波在矿物处理过程中的应用.铀冶金21 3.2002,21(3),151-153.
郑英等.微波在矿物处理过程中的应用.铀冶金21 3.2002,21(3),151-153. *

Also Published As

Publication number Publication date
CN101376928A (en) 2009-03-04

Similar Documents

Publication Publication Date Title
CN101376928B (en) Process for smelting magnesium by microwave heating Pidgeon process
CN102320806B (en) Micronano superfine powder high-temperature high-radiance paint and preparation method thereof
CN106498185B (en) A kind of method of vacuum microwave refining magnesium
Wu et al. Preparation and thermal shock resistance of cordierite-spodumene composite ceramics for solar heat transmission pipeline
CN103708455A (en) Method for preparing calcium carbide
CN101967566B (en) Process for preparing metal magnesium by normal pressure thermal reduction method
WO2020057094A1 (en) Silicon carbide closed-cell ceramic prepared by using industrial silicon-based waste residue and preparation method therefor
CN101985701B (en) Method for reducing calcined magnesite by using calcium carbide under normal pressure
CN101016590A (en) Method of preparing lithium from spodumene concentrate
CN107285778B (en) Preparation method of high-temperature-resistant forsterite type refractory material
CN102689882B (en) Method for producing yellow phosphorus by virtue of low grade phosphate rotary hearth furnace method
CN103896605B (en) A kind of method of kyanite synthesis of dichroite-mullite composite
CN101892395B (en) Method for smelting magnesium by decomposition in vacuum through microwaves
CN103352128A (en) Direct zinc-coal mixing cyclone burning type zinc oxide production system
CN101602609B (en) A kind of method for preparing Fe-Si3N4 refractory material
CN106756107A (en) A kind of vacuum microwave magnesium smelting device
CN104477862A (en) Method and raw material for producing yellow phosphorus or phosphoric acid by adopting rotary kiln
CN109748281A (en) A method for preparing high-quality silicon carbide by using waste silicon micropowder
CN105567969A (en) Magnesium smelting process with microwave carbon method
CN101857439A (en) A method for synthesizing SiC powder from gold ore tailings
CN103708459A (en) Method for preparing calcium carbide
JP2014084501A (en) Magnesium vapor condensation device
CN102776389A (en) Method for using thermal-state magnesium slag afterheat and moving bed
WO2024056107A1 (en) Green and environmentally friendly method for producing magnesium by means of aluminothermic reduction
CN101654373A (en) Method for preparing Fe-Sialon spinel complex phase fire-proof material

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
ASS Succession or assignment of patent right

Owner name: CHONGQING KEJIAN METALLURGY MATERIAL CO., LTD.

Free format text: FORMER OWNER: CHONGQING GAOLING INVESTMENT (GROUP) CO., LTD.

Effective date: 20140724

C41 Transfer of patent application or patent right or utility model
COR Change of bibliographic data

Free format text: CORRECT: ADDRESS; FROM: 400080 DADUKOU, CHONGQING TO: 401258 CHANGSHOU, CHONGQING

TR01 Transfer of patent right

Effective date of registration: 20140724

Address after: 401258, Changshou District, Chongqing City Jiangnan District Street, steel auxiliary road three, No. 2

Patentee after: Chongqing Kejian Metallurgy Material Co., Ltd.

Address before: Eight town 400080 Dadukou District of Chongqing

Patentee before: Chongqing Gaoling Investment (Group) Co., Ltd.

CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20110112

Termination date: 20151010

EXPY Termination of patent right or utility model