CN101386919B - High-pure magnesium preparation method and apparatus - Google Patents
High-pure magnesium preparation method and apparatus Download PDFInfo
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- CN101386919B CN101386919B CN2008103051334A CN200810305133A CN101386919B CN 101386919 B CN101386919 B CN 101386919B CN 2008103051334 A CN2008103051334 A CN 2008103051334A CN 200810305133 A CN200810305133 A CN 200810305133A CN 101386919 B CN101386919 B CN 101386919B
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Abstract
The invention discloses a method and a device for preparing high-purity magnesium. The method is to use magnesium ingot as a raw material to produce the high-purity magnesium with the purity of 99.98 percent. The device comprises a vacuum distilling furnace (1), an inner wall of the vacuum distilling furnace is provided with a heating element (2), and the vacuum distilling furnace is provided with a vacuumizing interface (3); the inside of the vacuum distilling furnace is provided with a vacuum distiller (4), the upper side of the vacuum distiller is provided with an annular water jacket (5), and the annular water jacket is provided with a circulating water interface (6); the upper side of the vacuum distiller is provided with a large flange (7), the large flange is provided with an annular water jacket (8), and the annular water jacket is provided with the circulating water interface; and the large flange is provided with the vacuumizing interface and a condenser (9). The method improves the high-purity magnesium with the purity up to 99.98 percent by using the apparatus with simple operation and no pollution so as to meet the requirements on development of national defense industry technology and nuclear industry technology. The device has the advantages of long service life, simple structure, less investment in the apparatus, and safe and reliable use.
Description
Technical field
The present invention relates to a kind of producing magnesium method and device, particularly a kind of vacuum distilling prepares the method and the device of high-purity magnesium.
Background technology
Industrial, the production method of magnesium has two kinds, and the one, electrolytic process, the MgCl2 electrolysis is carried out in no partition board electrolytic cell, contains Fe, Si, Ni, Cu, Mn, Al, Ca, CL in the crude magnesium of production
2, N
2, O
2Deng impurity.Another kind is a silicothermic process, and chemical reaction is heated in Chou Zhen Kong And 1200 ℃ the reduction jar and carries out, and contains metallic impurity such as Si, Mn, Zn, Cu, K, Na, Ca and CaO, MgO, SiO in the crude magnesium of condensation
2, AlO
3, Fe
2O
3Deng nonmetallic impurity.
The crude magnesium of two kinds of method productions all will carry out refining, removes the impurity in the magnesium.Smart magnesium purity after the refining can reach more than 99.90 foreign matter content≤0.1.
The commodity magnesium of this quality can satisfy car hub, and engine and aircraft industry magnesium alloy replace partly steel plate or aluminium, produces extensive needs the such as nodulizing agent of spheroidal graphite cast iron.
But development along with national defense industry and nuclear industry technology, metal purities such as the metallic beryllium that uses in these industry, zirconium, hafnium, uranium, plutonium require high, produce the reductive agent magnesium of these metals, require to use purity to be equal to or higher than high-purity magnesium of 99.98%, and prior art still can not satisfy the needs of producing and using.
Summary of the invention
The objective of the invention is to, a kind of preparation method and device of high-purity magnesium is provided.Be equal to or higher than high-purity magnesium of 99.98% with simple to operate, free of contamination device dna purity, to overcome the deficiencies in the prior art and the development need that satisfies national defense industry and nuclear industry technology.
Technical scheme of the present invention.A kind of preparation method of high-purity magnesium is that to adopt magnesium ingot be that raw material is made purity and is equal to or higher than high-purity magnesium of 99.98%; Step is as follows:
A), φ 300 * 130mm magnesium ingot that will be placed in the plumbago crucible divides three layers every layer 5 to be placed in the vacuum distilling apparatus, places an aluminium sheet above every layer of magnesium ingot; Then vacuum distilling apparatus is put into vacuum distillation furnace;
B), will vacuumize between vacuum distilling apparatus and the condenser and between vacuum distilling apparatus and the vacuum distillation furnace;
C), to vacuum distillation furnace heating 2 hours, the Heating temperature of epimere is 650 ℃, the Heating temperature of hypomere is 660 ℃;
D), feed in the ring-type water jacket above the sealing rubber ring of the ring-shaped water jacket of condenser and vacuum distilling apparatus cooling water circulationly, make the condensation 3 hours on condenser of magnesium steam;
E), stop to vacuumize, and in vacuum distilling apparatus, charge into argon gas, remove vacuum cooling after, open high-purity magnesium that vacuum distilling apparatus takes out condensation; Every stove can produce high-purity magnesium 100Kg, and a production cycle is 13～15 hours.
The preparation facilities of a kind of high-purity magnesium that the preparation method of above-mentioned high-purity magnesium is used comprises vacuum distillation furnace, and the vacuum distillation furnace inwall is provided with heating unit, and vacuum distillation furnace is provided with and vacuumizes interface; Be provided with vacuum distilling apparatus in the vacuum distillation furnace, the top of vacuum distilling apparatus is provided with the ring-type water jacket, and the ring-type water jacket is provided with the recirculated water interface; The vacuum distilling apparatus top is provided with big flange, and big flange is provided with ring-shaped water jacket, and ring-shaped water jacket is provided with the recirculated water interface; Big flange is provided with and vacuumizes interface and condenser
In the preparation facilities of aforesaid high-purity magnesium, be provided with sealing rubber ring in the junction of described vacuum distillation furnace and vacuum distilling apparatus and the junction of vacuum distilling apparatus and condenser.
In the preparation facilities of aforesaid high-purity magnesium, the heating unit total power in the described vacuum distillation furnace is 100KW.
In the preparation facilities of aforesaid high-purity magnesium, described vacuum distillation furnace one side is provided with three thermopairs along short transverse.
Compared with prior art, the present invention adopts, and simple to operate, free of contamination equipment dna purity is equal to or higher than high-purity magnesium of 99.98%, thereby can satisfy the development need of national defense industry and nuclear industry technology.Device long service life of the present invention, simple in structure, facility investment is little, and is safe and reliable.
Description of drawings
Fig. 1 is the used preparation facilities structural representation of the present invention.
Being labeled as in the accompanying drawing: the 1-vacuum distillation furnace, the 2-heating unit, 3-vacuumizes interface, 4-vacuum distilling apparatus, 5-ring-type water jacket, 6-recirculated water interface, the big flange of 7-, 8-ring-shaped water jacket, 9-condenser, 10-sealing rubber ring, the 11-thermopair, 12-magnesium ingot, 13-aluminium sheet, 14-plumbago crucible.
Embodiment
The present invention is described in further detail below in conjunction with embodiment, but not as limitation of the present invention.
Embodiments of the invention.A kind of preparation method of high-purity magnesium.As shown in Figure 1.A kind of preparation method of high-purity magnesium.This method adopts magnesium ingot 12 to make purity for raw material and is equal to or higher than high-purity magnesium of 99.98%; Step is as follows:
A), φ 300 * 130mm magnesium ingot that will be placed on 14 li of plumbago crucible divides three layers every layer 5 to be placed in the vacuum distilling apparatus 4, places an aluminium sheet 13 above every layer of magnesium ingot; Then vacuum distilling apparatus is put into vacuum distillation furnace 1;
B), will vacuumize between vacuum distilling apparatus 4 and the condenser 9 and between vacuum distilling apparatus 4 and the vacuum distillation furnace 1;
C), to vacuum distillation furnace 1 heating 2 hours, the Heating temperature of epimere is 650 ℃, the Heating temperature of hypomere is 660 ℃;
D), feed in the ring-type water jacket above the sealing rubber ring 10 of the ring-shaped water jacket of condenser 9 and vacuum distilling apparatus 4 cooling water circulationly, make the condensation 3 hours on condenser 9 of magnesium steam;
E), stop to vacuumize, and in vacuum distilling apparatus 4, charge into argon gas, remove vacuum cooling after, open vacuum distilling apparatus 4 and take out high-purity magnesium of condensations; Every stove can produce high-purity magnesium 100Kg, and a production cycle is 13～15 hours.
When making the preparation facilities of the used high-purity magnesium of the preparation method of above-mentioned high-purity magnesium, install heating unit 2 on existing vacuum distillation furnace 1 inwall, the total power of heating unit 2 is 100KW, is provided with to vacuumize interface 3 on vacuum distillation furnace 1; Be provided with vacuum distilling apparatus 4 in the vacuum distillation furnace 1, above vacuum distilling apparatus 4, install ring-type water jacket 5, on ring-type water jacket 5, be provided with recirculated water interface 6; Above vacuum distilling apparatus 4, install big flange 7, on big flange 7, be provided with ring-shaped water jacket 8, on ring-shaped water jacket 8, be provided with recirculated water interface 6; On big flange 7, be provided with and vacuumize interface 3 and condenser 9; All install sealing rubber ring 10 at described vacuum distillation furnace 1 and the junction and the vacuum distilling apparatus 4 of vacuum distilling apparatus 4 with the junction of condenser 7.During work, will vacuumize between vacuum distilling apparatus 4 and the condenser 9 and between vacuum distilling apparatus 4 and the vacuum distillation furnace 1; Make vacuum distilling apparatus 4 internal and external pressure balances, alleviate suffered external pressure of distiller and reduction oxidation corrosion, the preparation facilities work-ing life of improving high-purity magnesium vacuum distilling apparatus 4.Vacuum distillation furnace 1 one sides are provided with three thermopairs 11 along the different heights of short transverse.Be used to measure the temperature of vacuum distillation furnace 1 different heights.
Claims (2)
1. the preparation method of high-purity magnesium is characterized in that: it is that raw material is made purity and is equal to or higher than high-purity magnesium of 99.98% that this method adopts magnesium ingot; Step is as follows:
A), φ 300 * 130mm magnesium ingot that will be placed in the plumbago crucible divides three layers every layer 5 to be placed in the vacuum distilling apparatus, places an aluminium sheet above every layer of magnesium ingot; Then vacuum distilling apparatus is put into vacuum distillation furnace;
B), will vacuumize between vacuum distilling apparatus and the condenser and between vacuum distilling apparatus and the vacuum distillation furnace;
C), to vacuum distillation furnace heating 2 hours, the Heating temperature of epimere is 650 ℃, the Heating temperature of hypomere is 660 ℃;
D), feed in the ring-type water jacket above the sealing rubber ring of the ring-shaped water jacket of condenser and vacuum distilling apparatus cooling water circulationly, make the condensation 3 hours on condenser of magnesium steam;
E), stop to vacuumize, and in vacuum distilling apparatus, charge into argon gas, remove vacuum cooling after, open high-purity magnesium that vacuum distilling apparatus takes out condensation; Every stove can produce high-purity magnesium 100Kg, and a production cycle is 13～15 hours.
2. the preparation facilities of the used high-purity magnesium of the preparation method of high-purity magnesium according to claim 1, it is characterized in that: comprise vacuum distillation furnace (1), vacuum distillation furnace (1) inwall is provided with heating unit (2), and vacuum distillation furnace (1) is provided with and vacuumizes interface (3); Be provided with vacuum distilling apparatus (4) in the vacuum distillation furnace (1), the top of vacuum distilling apparatus (4) is provided with ring-type water jacket (5), and ring-type water jacket (5) is provided with recirculated water interface (6); Vacuum distilling apparatus (4) top is provided with big flange (7), and big flange (7) is provided with ring-shaped water jacket (8), and ring-shaped water jacket (8) is provided with recirculated water interface (6); Big flange (7) is provided with and vacuumizes interface (3) and condenser (9); Be provided with sealing rubber ring (10) in vacuum distillation furnace (1) and the junction of vacuum distilling apparatus (4) and the junction of vacuum distilling apparatus (4) and condenser (7); Heating unit (2) total power in the vacuum distillation furnace (1) is 100KW; Vacuum distillation furnace (1) one side is provided with three thermopairs (11) along short transverse.
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| CN2008103051334A CN101386919B (en) | 2008-10-24 | 2008-10-24 | High-pure magnesium preparation method and apparatus |
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| CN2008103051334A CN101386919B (en) | 2008-10-24 | 2008-10-24 | High-pure magnesium preparation method and apparatus |
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| CN101386919A CN101386919A (en) | 2009-03-18 |
| CN101386919B true CN101386919B (en) | 2011-12-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609777A (en) * | 2019-01-10 | 2019-04-12 | 西安理工大学 | A kind of device and method purifying high purity magnesium |
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| CN101948957B (en) * | 2010-10-14 | 2012-07-04 | 宁波翔博机械有限公司 | Vacuum distillation method for magnesium alloy |
| CN102296184B (en) * | 2011-09-15 | 2012-10-03 | 重庆大学 | Solvent-free magnesium alloy purification method |
| JP5290387B2 (en) | 2011-12-07 | 2013-09-18 | Ｊｘ日鉱日石金属株式会社 | Method for producing high purity calcium |
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| CN103253703A (en) * | 2013-06-06 | 2013-08-21 | 江西海宸光电科技有限公司 | Preparation method and equipment of high-purity arsenic oxide |
| CN103740949B (en) * | 2013-12-31 | 2015-02-04 | 深圳市华星光电技术有限公司 | Device and method for pre-treating magnesium metal |
| CN104164563B (en) * | 2014-06-27 | 2016-08-24 | 宁夏太阳镁业有限公司 | A kind of metal reducing jar |
| CN104313579B (en) * | 2014-11-11 | 2017-01-18 | 武汉钢铁(集团)公司 | Production method of zinc-magnesium galvanized alloy steel plate |
| CN106811607A (en) * | 2015-12-02 | 2017-06-09 | 镇江市润州金山金属粉末厂 | A kind of vacuum aluminothermic process produces strontium reacting furnace |
| CN107574319B (en) * | 2017-10-24 | 2022-11-18 | 山西宝盛远华新材料股份有限公司 | Semi-continuous distillation production method of high-purity magnesium |
| CN108130450A (en) * | 2018-02-05 | 2018-06-08 | 南通鑫祥锌业有限公司 | A kind of alloy zinc belt and preparation method thereof |
| CN108149072A (en) * | 2018-02-05 | 2018-06-12 | 南通鑫祥锌业有限公司 | A kind of zinc foil material and preparation process |
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| CN1202529A (en) * | 1998-05-12 | 1998-12-23 | 周广文 | Purifying process for producing high purity metal magnesium |
| CN2335976Y (en) * | 1998-05-12 | 1999-09-01 | 周广文 | High purity metallic magnesium distillator |
| CN1740352A (en) * | 2005-09-28 | 2006-03-01 | 中国科学院物理研究所 | A kind of high vacuum in-situ two-step refining process of high-purity material |
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| US5698158A (en) * | 1995-02-21 | 1997-12-16 | Sony Corporation | Vacuum distillation apparatus for producing ultra high purity material |
| CN1202529A (en) * | 1998-05-12 | 1998-12-23 | 周广文 | Purifying process for producing high purity metal magnesium |
| CN2335976Y (en) * | 1998-05-12 | 1999-09-01 | 周广文 | High purity metallic magnesium distillator |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109609777A (en) * | 2019-01-10 | 2019-04-12 | 西安理工大学 | A kind of device and method purifying high purity magnesium |
| CN109609777B (en) * | 2019-01-10 | 2020-05-22 | 西安理工大学 | Device and method for purifying high-purity magnesium |
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| CN101386919A (en) | 2009-03-18 |
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