CN100398679C - Method of preparing Mg, Sr alloy by vacuum heat reduction - Google Patents
Method of preparing Mg, Sr alloy by vacuum heat reduction Download PDFInfo
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- CN100398679C CN100398679C CNB2006100542161A CN200610054216A CN100398679C CN 100398679 C CN100398679 C CN 100398679C CN B2006100542161 A CNB2006100542161 A CN B2006100542161A CN 200610054216 A CN200610054216 A CN 200610054216A CN 100398679 C CN100398679 C CN 100398679C
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Abstract
The present invention relates to a method for preparing Mg-Sr alloy by vacuum thermal reduction, which belongs to the field of non-ferrous metal metallurgy. The present invention comprises the technological processes: after raw materials such as calcined magnesium ore, strontia or the precursor of strontia, calcia, silicon iron (or other silicon alloy, aluminium and aluminium alloy), fluorite, etc. are taken according to a certain proportion, the raw materials are pulverized and uniformly mixed; then the raw materials are pressed into pellets to be packed into a reaction tank to carry out vacuum thermal reduction, and generated metal Mg vapour and metal Sr vapour are collected and reduced to be cooled to form the condensed-state Mg-Sr alloy. Compared with the prior art of smelting magnesium by a vacuum silicothermic process, and the prior art of smelting strontium by a vacuum aluminothermic process, the method can directly prepare the Mg-Sr alloy having low cost and high efficiency by simultaneously adding magnesium oxide and strontium oxide, or the precursor of magnesium oxide, and the precursor of strontium oxide to auxiliary materials via the synchronous vacuum thermal reduction of magnesium and strontium.
Description
Technical field
The present invention relates to a kind of method of preparing Mg, Sr alloy by vacuum heat reduction, belong to smelting field of nonferrous metal.
Background technology
Strontium is important industrial production starting material, but resource is very limited, strontium conservation of resources and efficiently be utilized as the universe and pay close attention to.
Strontium (Sr) and alloy thereof are widely used in deoxidation, desulfurization, dephosphorization, purification and the aluminium of alloy smeltings such as steel, iron, copper, the grain refining and the alloying of magnesium alloy.Compare with Preparation of Metallic Strontium, magnesium strontium (Mg-Sr) is when alloy is used for Metal Melting, the strontium utilization ratio is higher, effects such as deoxidation, desulfurization, dephosphorization, purification, refinement, alloying are better, deposit and use safer and convenient, its preparation and use increasingly extensive, especially along with the great development of global magnesium alloy industry, contain the strontium heat resistance magnesium alloy and paid much attention to and be large scale application trend, be used to produce the Mg-Sr master alloy that contains the strontium heat resistance magnesium alloy and contain the strontium magnesium ingot market requirement very vigorous.
Existing Mg-Sr alloy preparation method is mainly method of mixing and infiltration reduction method.
Preparation Mg-Sr alloy to the method for mixing be with MAGNESIUM METAL and Preparation of Metallic Strontium under molten state to mixing, form the Mg-Sr alloy after the condensation.This method need be used the higher Preparation of Metallic Strontium of price, and because the chemical property of strontium is very active, the vapour pressure of molten state is big, and is bigger to oxidation in the process of mixing, vaporization losses.The utilization ratio of strontium has only 50-60% usually in the Preparation of Metallic Strontium preparation process, the utilization ratio of strontium has only 50-85% usually in the Mg-Sr alloy preparation process, experience after two flow processs only 25-51% of strontium utilization ratio, not only the strontium wasting of resources is big, and long flow path, the secondary remelting consumes energy, the manufacturing cost height, less economical.
The infiltration reduction method is that strontium compound is added the magnesium melt, adds strontium by the infiltration reduction in the magnesium melt.Because the melt temperature of magnesium alloy only needs 600-800 ℃ usually, under this temperature, the infiltration reduction kinetics motivating force of strontium is less, the reduction ratio of strontium compound is lower, and when temperature raise, strontium infiltration reduction kinetics motivating force increased, but strontium vaporization losses also becomes greatly, and the utilization ratio of strontium is also lower.The common less than 30% of the strontium utilization ratio of infiltration reduction method.Therefore, infiltration reduction method strontium utilization ratio is low, less economical, is only necessarily used when adding very micro-strontium in metal melt.
Vacuum-thermal method is extensive with its heat energy source, material use efficiency is high, production efficiency is high, low cost of manufacture, comparatively significant Technological Economy such as be easy to realize to produce in enormous quantities, easily is being used widely in the evaporated metal production.But vacuum-thermal method is used for the preparation of Mg-Sr alloy does not appear in the newspapers as yet.
Summary of the invention
The objective of the invention is: overcome existingly, a kind of novel method of preparing Mg, Sr alloy by vacuum heat reduction is provided the low deficiency of strontium utilization ratio in method of mixing and the infiltration reduction method.
Technical scheme of the present invention is:
(1) get the raw materials ready, starting material comprise calcined magnesium ore, strontium oxide, calcium oxide, 75 ferrosilicon, fluorite, and its component and mass percent are controlled at: MgO and SrO add up to 30-55%, CaO 30-50%, 75 ferrosilicon 12-18%, fluorite 2-4%;
(2) starting material are crushed to particle diameter less than 0.15mm, and mix;
(3) starting material that will pulverize and mix are pressed into pelletizing;
(4) pelletizing is packed into retort, at temperature 1000-1250 ℃, vacuum tightness 1-20Pa reduction 1-10 hour down;
(5) collect the metallic vapor that reduction generates and be condensed into condensed state Mg-Sr alloy.
Wherein: the mass ratio of strontium element and magnesium elements is 0.001-2 in the starting material, adjusts this ratio and can prepare the various Mg-Sr alloys of strontium content 0.08-56%; Strontium oxide in the starting material can be used on the strontium compound that can form strontium oxide under the vacuum-thermal reduction condition and partly or entirely replaces; Magnesium ore is rhombspar, magnesite, when using rhombspar, because of wherein having contained calcium oxide, can not add or add less calcium oxide in getting the raw materials ready; Si in the ferrosilicon is as reductive agent, and available aluminium, aluminium alloy partly or entirely replace.
Beneficial effect of the present invention is mainly reflected in: compare with vacuum aluminothermy refining strontium technology with existing vacuum silicon heat refining magnesium, oxide compound or its presoma of magnesium to be restored, strontium in batching, have been added simultaneously, by the synchronous vacuum-thermal reduction of magnesium, strontium, directly realize low cost, the high-level efficiency preparation of Mg-Sr alloy.Manufacturing process of the present invention is short, the material use efficiency height, and Technological Economy is good; Can realize the high-level efficiency of the Mg-Sr alloy of various content, produce low-costly and in high volume; Can use primary energy source such as coal, fuel oil, combustion gas to use the energy as heating, capacity usage ratio is higher, also can use under the not abundant condition of electric power resource.
Embodiment
Further specify below in conjunction with embodiment and to carry out the present invention.
Embodiment 1:
Implementation process is:
(1) get the raw materials ready, starting material are: the calcined dolomite of MgO content 40%, the SrO of purity 99%, the ferrosilicon of Si content 75%, the fluorite of purity 97%.The batching mass ratio is: forge white: SrO: ferrosilicon: fluorite=100: 56: 28: 4;
(2) all raw material is crushed to particle diameter less than 0.15mm, and mixes;
(3) starting material that will pulverize and mix are pressed into pelletizing;
(4) pelletizing is packed into retort, 1200 ± 50 ℃ of temperature, vacuum tightness 1-20Pa reduction 1 hour down;
(5) collect the metallic vapor that reduction generates and be condensed into condensed state Mg-Sr master alloy.
Implementation result: the Mg-Sr alloy contains Sr amount 56%.Strontium utilization ratio 60%.
Embodiment 2:
Implementation process is:
(1) get the raw materials ready, starting material are: the calcined magnesite of MgO content 95%, the Sr of purity 99% (OH)
2, the CaO of purity 98%, the ferrosilicon of Si content 75%, purity is 99% aluminium powder, Al, each Al-Si alloy of 49% of Si content, the fluorite of purity 97%.The batching mass ratio is: calcined magnesite: Sr (OH)
2: CaO: ferrosilicon: aluminium powder: Al-Si alloy: fluorite=100: 0.08: 145.4: 53.2: 0.005: 0.005: 9.5;
(2) all raw material is crushed to particle diameter less than 0.15mm, and mixes;
(3) starting material that will pulverize and mix are pressed into pelletizing;
(4) pelletizing is packed into retort, 1050 ± 50 ℃ of temperature, vacuum tightness 1-20Pa reduction 10 hours down;
(5) collect the metallic vapor that reduction generates and be condensed into condensed state Mg-Sr alloy.
Implementation result: the Mg-Sr alloy contains Sr amount 0.08%.Strontium utilization ratio 60%.
Claims (1)
1. the method for a preparing Mg, Sr alloy by vacuum heat reduction is characterized in that, processing step is:
(1) gets the raw materials ready, starting material are made up of calcined magnesium ore, strontium oxide, calcium oxide, 75 ferrosilicon, fluorite, its component and mass percent are controlled at: the mass ratio of MgO total 30-55% and strontium element and magnesium elements is 0.001-2 in SrO and the calcined magnesium ore, CaO 30-50%, 75 ferrosilicon 12-18%, fluorite 2-4%;
(2) starting material are crushed to particle diameter less than 0.15mm, and mix;
(3) starting material that will pulverize and mix are pressed into pelletizing;
(4) pelletizing is packed into retort, at temperature 1000-1250 ℃, vacuum tightness 1-20Pa reduction 1-10 hour down;
(5) collect the metallic vapor that reduction generates and be condensed into condensed state Mg-Sr alloy.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100542161A CN100398679C (en) | 2006-04-17 | 2006-04-17 | Method of preparing Mg, Sr alloy by vacuum heat reduction |
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| CNB2006100542161A CN100398679C (en) | 2006-04-17 | 2006-04-17 | Method of preparing Mg, Sr alloy by vacuum heat reduction |
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| CN100398679C true CN100398679C (en) | 2008-07-02 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101173337B (en) * | 2006-10-31 | 2010-08-11 | 北京有色金属研究总院 | Method for producing creep resistant magnesium alloy |
| CN101781707B (en) * | 2010-03-16 | 2014-03-19 | 重庆大学 | Method for preparing non-ferrous metal by thermal reduction of silicon-copper alloy |
| CN102080164A (en) * | 2010-12-02 | 2011-06-01 | 重庆大学 | Method for preparing Mg-Li alloy by vacuum synchronous thermal reduction |
| CN102011021A (en) * | 2010-12-02 | 2011-04-13 | 重庆大学 | Method for reduction preparation of Mg-Li-Sr alloy by vacuum heat |
| CN102061400B (en) * | 2010-12-08 | 2012-10-10 | 重庆理工大学 | Method for preparing Mg-Sr intermediate alloy by gas-aid SrO smelt thermal reduction |
| CN105803189B (en) * | 2016-05-16 | 2018-06-29 | 贵州大学 | A kind of method of phosphorus in efficient removal high-phosphor oolitic hematite |
| CN106702178B (en) * | 2016-11-21 | 2018-11-06 | 厦门稀纯材料科技有限公司 | A kind of preparation method of high pure metal strontium and a kind of high pure metal strontium prepared with this method |
| CN109295321A (en) * | 2018-11-02 | 2019-02-01 | 中国科学院青海盐湖研究所 | The preparation method of Preparation of Metallic Strontium |
| CN111455207B (en) * | 2020-04-08 | 2021-05-07 | 中国恩菲工程技术有限公司 | Method for preparing magnesium-scandium alloy by precursor process and magnesium-scandium alloy prepared by method |
Citations (4)
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| CN1067071A (en) * | 1991-05-23 | 1992-12-16 | 颜志明 | The industrialized producing technology technology and the equipment thereof of the vacuum-thermal method of non-ferrous metal such as strontium and barium |
| FR2800097A1 (en) * | 1999-10-26 | 2001-04-27 | Ete Etudes Thermiques Et Elect | Fabrication of alkaline earth metals in a mobile cylindrical furnace heated by the Joule effect in graphite bars within the heating container for the relevant metal oxides |
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| WO2005103309A1 (en) * | 2004-04-26 | 2005-11-03 | Fos International S.A. | Metallothermic process for magnesium production and vacuum-induction furnace thereto |
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2006
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1067071A (en) * | 1991-05-23 | 1992-12-16 | 颜志明 | The industrialized producing technology technology and the equipment thereof of the vacuum-thermal method of non-ferrous metal such as strontium and barium |
| FR2800097A1 (en) * | 1999-10-26 | 2001-04-27 | Ete Etudes Thermiques Et Elect | Fabrication of alkaline earth metals in a mobile cylindrical furnace heated by the Joule effect in graphite bars within the heating container for the relevant metal oxides |
| WO2005103309A1 (en) * | 2004-04-26 | 2005-11-03 | Fos International S.A. | Metallothermic process for magnesium production and vacuum-induction furnace thereto |
| CN1594616A (en) * | 2004-07-16 | 2005-03-16 | 东南大学 | Primary vacuum reduction distillation production process by thermit process and metallic strontium |
Non-Patent Citations (4)
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| 真空铝热还原法制备金属Sr的热力学分析及实验研究. 于金等.金属学报，第41卷第8期. 2005 |
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