CN100540752C - A kind of method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide - Google Patents
A kind of method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide Download PDFInfo
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- CN100540752C CN100540752C CNB2007100786264A CN200710078626A CN100540752C CN 100540752 C CN100540752 C CN 100540752C CN B2007100786264 A CNB2007100786264 A CN B2007100786264A CN 200710078626 A CN200710078626 A CN 200710078626A CN 100540752 C CN100540752 C CN 100540752C
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Abstract
A kind of preparation method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide, belong to the magnesium alloy materials preparing technical field, it is characterized in that: adopt electrolytic process that manganese is separated out the formation alloy from manganic compound, step comprises: fusing Mg or metal M g and alloying element thereof in electrolyzer obtain the magnesium melt; The preparation ionogen, wherein the quality of manganese element is the 0.2-10% of MAGNESIUM METAL melt quality in the manganic compound, halide weight be manganic compound weight 0.5-5 doubly, all raw material fully dewatered and mix; The ionogen for preparing is added the magnesium melt, and heat fused becomes the ionogen fused salt; Electrolysis temperature: 700-800 ℃, electrolysis voltage: 1.7-2.7V, electrolysis obtains the Mg-Mn alloy melt, and condensation obtains solid-state Mg-Mn alloy.It is short that the present invention has manufacturing process, resource and energy utilization rate height, product quality and advantages such as good stability, low cost of manufacture thereof.
Description
Technical field
The invention belongs to the magnesium alloy materials preparing technical field, relate to a kind of method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide specifically.
Background technology
The Mg-Mn alloy is of wide application as important industrial sector raw material.Except in ironmaking and steelmaking process, being used as reductor, sweetening agent and the alloy addition, the Mg-Mn alloy is as a kind of deforming alloy, the anti-corrosion part of aviation part and gasoline and lubricating oil system be can make, plate members, baffle plate, fuel tank weldment, stamp work also can be processed into.Along with the great development of global magnesium alloy industry, the Mg-Mn alloy is paid much attention to and application surface and application quantity are quick growing trend.
At present, the method for producing the Mg-Mn alloy both at home and abroad is for to the method for mixing, and this method needs preparation metal M n separately, it is joined in the magnesium of fusing or the magnesium alloy again and obtains the Mg-Mn alloy.During preparation metal M n, adopt the wet processing of " manganese ore-leaching-refining-electrolysis of solutions " usually, this technology greatest problem is that manufacturing process is tediously long, and " three wastes " (waste residue, waste water, waste gas) generation is big, disposes the difficulty height, and environmental pollution is serious.Metal M g and metal M n to the process of mixing in, need seasoning metal, energy consumption is big, and the harmful structure among the metal M n may be genetic in the Mg-Mn alloy, influences the Mg-Mn alloy property.Therefore, to be equipped with the Technological Economy of Mg-Mn alloy relatively poor to mixing legal system.
Summary of the invention
The objective of the invention is:, provide a kind of method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide to mixing the problem and shortage that exists in the smelting method for preparing Mg-Mn alloy technology.
Main contents of the present invention comprise:
A kind of method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide, it is characterized in that this method in the following order step carry out:
(1) deposite metal Mg or metal M g and alloying element thereof in electrolyzer obtain the magnesium melt;
(2) preparation ionogen, starting material comprise manganic compound and halogenide, and wherein, the quality of manganese element is the 0.2-10% of MAGNESIUM METAL melt quality in the manganic compound, halide weight be manganic compound weight 0.5-5 doubly, all raw material fully dewatered and mix;
(3) ionogen with preparation adds the magnesium melt, and heat fused becomes the ionogen fused salt;
(4) magnesium melt and electrolytical temperature are adjusted into 700-800 ℃, with the negative electrode importing magnesium melt of dc electrolysis power supply, anode imports ionogen, and electrolysis voltage is adjusted into 1.7-2.7V, and the energising electrolysis obtains the Mg-Mn alloy melt;
(5) condensation Mg-Mn alloy melt obtains solid-state Mg-Mn alloy.
Manganese oxide among the present invention replaces with manganese ore or the manganic compound that high temperature produces manganese oxide down; Halogenide is halid one or more the mixture of Li, Mg, Ca, Ba in the ionogen; Alloying element in metal M g and the alloying element thereof is: one or both among Al, the Zn.
The electrolyzer that the present invention adopts is conventional fused salt electrolysis device.Mass percent with Mn in the Mg-Mn alloy of the present invention's preparation is: 0.15-6%.
The novel preparation method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide of the present invention, do not need to use traditional sulfuric acid to leach manganese ore to generate the manganese sulfate solution electrolysis and make manganese metal, with respect to having now to mixing smelting technique, manufacturing process significantly shortens, resource and energy utilization rate, product quality and stability thereof all significantly promote, manufacturing cost significantly reduces, and technical economic benefit is significantly improved.
Embodiment
Further specify the specific embodiment of the present invention below in conjunction with embodiment.
Embodiment 1:
Implementation process:
(1) get metal M g2.0kg, add electrolyzer, heat fused also is adjusted into 700 ℃ with temperature, obtains the magnesium melt;
(2) preparation ionogen 0.26kg, wherein: manganese oxide (containing Mn51%) 0.13Kg, CaCl
2: 0.08kg, MgCl
2: 0.05kg, these materials are fully dewatered and pulverize is the powdery of granularity less than 0.075mm, mixes;
(3) ionogen for preparing is added the magnesium melt, heat fused becomes the ionogen fused salt;
(4) negative electrode with the dc electrolysis power supply imports the magnesium melt, and anode imports ionogen, the energising electrolysis.Electrolysis temperature is 700 ℃, and electrolysis voltage is 1.7V, the Mn content in the monitoring Mg melt, reach preset value after, stop electrolysis, obtain the Mg-Mn melt;
(5) condensation Mg-Mn alloy melt obtains solid-state Mg-Mn alloy.
Implementation result: obtain Mg-Mn alloy 2Kg, its Mn content is 2.5wt%.
Embodiment 2:
Implementation process:
(1) get metal M g1.99Kg, add in the electrolyzer, heat fused adds Metal Zn 0.01Kg, and fusing also is adjusted into 750 ℃ with temperature, obtains the magnesium melt;
(2) preparation ionogen 0.12kg, wherein: pyrolusite (containing Mn30%) 0.02Kg, CaF
2: 0.06kg, BaCl
2: 0.04kg, all material is fully dewatered and pulverizes is the powdery of granularity less than 0.075mm, mixes;
(3) ionogen for preparing is added the magnesium melt, heat fused becomes the ionogen fused salt;
(4) negative electrode with the dc electrolysis power supply imports the magnesium melt, and anode imports ionogen, the energising electrolysis.Electrolysis temperature is 750 ℃, and electrolysis voltage is 2.2V, the Mn content in the monitoring Mg-Zn alloy melt, reach preset value after, stop electrolysis, obtain the Mg-Mn-Zn alloy melt;
(5) condensation Mg-Mn-Zn alloy melt obtains solid-state Mg-Mn-Zn alloy.
Implementation result: obtain Mg-Mn-Zn alloy 2Kg, its Mn content is 0.15wt%.
Embodiment 3:
Implementation process:
(1) get metal M g1.85Kg, add electrolyzer, heat fused adds metal A l0.12Kg, Metal Zn 0.03Kg, and fusing also is adjusted into 800 ℃ with temperature, obtains the magnesium melt;
(2) preparation ionogen 0.5kg, wherein: manganous carbonate (industrial one-level) 0.3Kg, BaF
2: 0.1kg, LiF:0.1kg, all material is fully dewatered and pulverizes is the powdery of granularity less than 0.075mm, mixes;
(3) ionogen for preparing is added the magnesium melt, heat fused becomes the ionogen fused salt;
(4) negative electrode with the dc electrolysis power supply imports the magnesium melt, and anode imports ionogen, the energising electrolysis.Electrolysis temperature is 800 ℃, and electrolysis voltage is 2.7V, the Mn content in the monitoring Mg-Al-Zn alloy melt, reach preset value after, stop electrolysis, obtain the Mg-Mn-Al-Zn alloy melt;
(5) condensation Mg-Mn-Al-Zn alloy melt obtains solid-state Mg-Mn-Al-Zn alloy.
Implementation result: obtain Mg-Mn-Al-Zn alloy 2.1Kg, its Mn content is 5wt%.
Claims (5)
1. the method for a preparing Mg-Mn alloy by electrolytic reduction of manganese oxide, it is characterized in that this method in the following order step carry out:
(1) deposite metal Mg or metal M g and alloying element thereof in electrolyzer obtain the magnesium melt;
(2) preparation ionogen, starting material comprise manganic compound and halogenide, and wherein, the quality of manganese element is the 0.2-10% of MAGNESIUM METAL melt quality in the manganic compound, halide weight be manganic compound weight 0.5-5 doubly, all raw material fully dewatered and mix;
(3) ionogen for preparing is added the magnesium melt, heat fused becomes the ionogen fused salt;
(4) magnesium melt and electrolytical temperature are controlled at 700-800 ℃, with the negative electrode importing magnesium melt of dc electrolysis power supply, anode imports ionogen, and electrolysis voltage is adjusted into 1.7-2.7V, and the energising electrolysis obtains the Mg-Mn alloy melt;
(5) condensation Mg-Mn alloy melt obtains solid-state Mg-Mn alloy.
2. the preparation method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide according to claim 1 is characterized in that: described manganese oxide replaces with manganese ore or the manganic compound that high temperature produces manganese oxide down.
3. the preparation method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide according to claim 1 is characterized in that: described halogenide is halid one or more the mixture of Li, Mg, Ca, Ba.
4. the preparation method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide according to claim 1, it is characterized in that: the alloying element in described metal M g and the alloying element thereof is: one or both among Al, the Zn.
5. the preparation method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide according to claim 1 is characterized in that: contain Mn:0.15-6wt% in the Mg-Mn alloy of preparation.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100786264A CN100540752C (en) | 2007-06-15 | 2007-06-15 | A kind of method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide |
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|---|---|---|---|
| CNB2007100786264A CN100540752C (en) | 2007-06-15 | 2007-06-15 | A kind of method of preparing Mg-Mn alloy by electrolytic reduction of manganese oxide |
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| CN101086075A CN101086075A (en) | 2007-12-12 |
| CN100540752C true CN100540752C (en) | 2009-09-16 |
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| CN103060852B (en) * | 2013-01-18 | 2015-02-25 | 哈尔滨工程大学 | Method for preparing Mg-Mn-La ternary alloy through molten salt electrolysis |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5024737A (en) * | 1989-06-09 | 1991-06-18 | The Dow Chemical Company | Process for producing a reactive metal-magnesium alloy |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5024737A (en) * | 1989-06-09 | 1991-06-18 | The Dow Chemical Company | Process for producing a reactive metal-magnesium alloy |
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Granted publication date: 20090916 Termination date: 20100615 |