CN107746968A - The recovery method of residual Re in magnesium-rare earth flux slag - Google Patents
The recovery method of residual Re in magnesium-rare earth flux slag Download PDFInfo
- Publication number
- CN107746968A CN107746968A CN201711001068.1A CN201711001068A CN107746968A CN 107746968 A CN107746968 A CN 107746968A CN 201711001068 A CN201711001068 A CN 201711001068A CN 107746968 A CN107746968 A CN 107746968A
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- China
- Prior art keywords
- magnesium
- rare earth
- slag
- flux
- magnesium alloy
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Classifications
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- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
-
- 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
- C22B59/00—Obtaining rare earth metals
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of recovery method of residual Re in magnesium-rare earth flux slag, comprise the following steps：（1）, magnesium-rare earth flux ground-slag it is broken：Magnesium-rare earth flux slag is in small, broken bits to 30 40mm granularities through jaw crusher, and the coarse grain magnesium alloy flux slag of 30 40mm granularities is sent into chain type pulverizer and is crushed to 60 80 mesh；（2）, water logging：By be crushed to 60 80 mesh magnesium alloy flux slag and water by 1:5 ratio mixes 60 minutes；（3）, the mixture of magnesium alloy flux slag and water added into centrifugal filter with pump, magnesium alloy particles, which are dehydrated to 1 1.5% recovery Mg-alloy particles, on machine is used for producing for high purity magnesium.Magnesium-rare earth flux waste residue is through processes such as broken, water loggings, remaining magnesium alloy particles, chloride, oxide, Fluorspar Powder in slag are proposed respectively, and rare earth oxide is made after sulfuric acid reaction and oxalic acid precipitation make rare earth oxalate roasting and is used for the fields such as Aero-Space, automobile, weaponry, hard-core technology.
Description
Technical field
It is residual in specially a kind of magnesium-rare earth flux waste residue the invention belongs to magnesium alloy smelting solid slag process field
Deposit the recoverying and utilizing method of rare earth element.
Background technology
Magnesium metal is a kind of silvery white light metal, and specific strength is high, activity is strong, has preferable shielding action to electromagnetic wave,
Because density is small, it is expected to turn into most promising structural material from now on and is used for Aero-Space, automobile making, engineering machinery, Dormant oils
The industrial departments such as chemical industry, but it is poor because of the intensity that it is compared with traditional structural materials such as steels, corrosion resistance is poor, hinders again
Hinder its fast development, pass through the application of some new manufacturing technologies, new technique, new material of application, these defects of magnesium
Overcome, magnesium alloy is added using rare earth element, with regard to its many kinds of force word property and high-temperature behavior can be significantly improved.It is so dilute
Native magnesium alloy is developed rapidly.Magnesium-rare earth is largely used to Aero-Space and weaponry and munitions.
Magnesium-rare earth understand in fusion process some oxidizing fire phenomenon appearance, prevent costliness rare earth material from
Product is fully converted to, and stays in smelting slag and discards as residue, rare earth element is a kind of rare strategic resource, extraction
Magnesium-rare earth flux waste residue rare earth elements have greatly politics and economic implications.
Main component is potassium chloride, magnesium chloride, sodium chloride and barium chloride in magnesium-rare earth waste residue；Have 40-50%'s in addition
The metal such as the oxide of magnesium, also aluminium, zinc, manganese, iron and oxide impurity, while also 10% or so fluoride is present, its
Slag middle rare earth is that rare earth alloy smelting process enters in slag, and its recycling has very big potentiality.Due to the comparison of ingredients of slag
Complexity according to the different physicochemical properties of various composition in slag, it is necessary to progressively be recycled.
The content of the invention
It is an object of the present invention to provide a kind of recovery method of remaining rare earth in magnesium-rare earth flux slag, for reclaiming costliness
Rare earth composition, reduce production cost.
The present invention adopts the following technical scheme that realization：
The recovery method of remaining rare earth in a kind of magnesium-rare earth flux slag, there is following process：
1st, magnesium-rare earth flux ground-slag is broken
Magnesium-rare earth flux slag is in small, broken bits to 30-40mm granularities through jaw crusher, and the coarse grain magnesium alloy of 30-40mm granularities is melted
Agent slag is sent into chain type pulverizer and is crushed to 60-80 mesh.
2nd, water logging
By process 1 be crushed to 60-80 mesh magnesium alloy flux slag and water by 1:5 ratio mixes 60 minutes.
3rd, the mixture of the magnesium alloy flux slag of process 2 and water is added into centrifugal filter with pump, magnesium alloy particles on machine
It is dehydrated to 1-1.5% recovery Mg-alloy particles and is used for producing for high purity magnesium.
4th, the mixed solution that the centrifuge of process 3 is isolated is added in belt vacuum filter and filtered.
5th, the belt vacuum filter of process 4 filter out clear liquid send triple effect evaporator extraction chloride produce magnesium alloy flux；Cross
The belt vacuum filter of journey 4 filters out in filter residue addition carburizing reagent equipment and CO2It is added to after reaction in belt vacuum filter
Filtering, for removing the metal oxide impurities such as calcirm-fluoride and iron oxide, aluminum oxide, zinc oxide.
6th, the belt vacuum filter of process 5 filters out filter residue and sulfuric acid reaction, and sour addition presses 1.3 of composition requirements amount in slag
Add again, react 3-4 hours.
7th, 6 reacted reaction solution of process is added in belt vacuum filter and filtered, filter residue, which is cleaned to pH, reaches 6-7, water
Fluorspar Powder finished product is crushed into when part is to less than 1.5%.
8th, by the belt vacuum filter of process 7 filter out filtrate add sedimentation basin in be slowly added into 30% oxalic acid solution, observation
Stop adding oxalic acid when producing without new precipitation.
9th, the oxalate precipitation of process 8 is filtered and cleaned out with centrifugal filter from mixed liquor, clear liquid is used to carry
Magnesium sulfate, ferrous sulfate, aluminum sulfate, zinc sulfate, manganese sulfate etc. are taken, or is produced for multi-elements composite fertilizer.
10th, the filter residue after process 9 is cleaned is calcined, and obtains earth oxide product.
The inventive method is progressively reclaimed according to the different chemistry of each composition in slag, physical property, is had according to chloride
There is good water solubility first to be extracted with flooding.The reaction of magnesia and carbon dioxide is recycled the magnesia for occupying 40-50%
It is proposed, then aluminium, zinc, manganese, metal and its oxide impurity such as iron in slag are proposed with sulfuric acid to leach.Rare earth element is in acidleach process
In also be soluble in acid, recycle oxalic acid and the rare-earth oxalate that easily precipitates of solution middle rare earth class reaction generation to separate out quilt from acid
Extract, finally calcirm-fluoride and a small amount of silica are precipitated as insoluble in common acids, available for cement, glass, ceramics etc.
Industrial production.Generation rare earth oxide can be used for directly smelting rare earth metal, extraordinary conjunction after the rare-earth oxalate roasting extracted
The alloys such as Jin Gang, aluminium, copper and glass, hard-core technology and agricultural.
Brief description of the drawings
Fig. 1 represents the schematic flow sheet of the inventive method.
Embodiment
The specific embodiment of the present invention is described in detail below in conjunction with the accompanying drawings.
The recovery method of residual Re in a kind of magnesium-rare earth flux slag, as shown in figure 1, comprising the following steps：
（1）, magnesium-rare earth flux ground-slag it is broken
Magnesium-rare earth flux slag is in small, broken bits to 30-40mm granularities through jaw crusher, and the coarse grain magnesium alloy of 30-40mm granularities is melted
Agent slag is sent into chain type pulverizer and is crushed to 60-80 mesh；
（2）, water logging
By be crushed to 60-80 mesh magnesium alloy flux slag and water by 1:5 ratio mixes 60 minutes；
（3）, by the mixture of magnesium alloy flux slag and water with pump add sieve aperture be more than 2mm centrifugal filter, filter
Upper magnesium alloy particles, which are dehydrated to 1-1.5% recovery Mg-alloy particles, is used for producing for high purity magnesium；
（4）, by step（3）The solution that centrifuge is isolated is added on the belt vacuum filter that sieve aperture is 60 mesh and carried out
Filter；
（5）, step（4）Belt vacuum filter filters out filtrate and send triple effect evaporator extraction chloride to produce magnesium alloy flux, walks
Suddenly（4）Belt vacuum filter filters out in filter residue addition carburizing reagent equipment and CO2After reaction, belt vacuum filter is added；
（6）, step（5）Belt vacuum filter filters out filter residue and sulfuric acid reaction, reacts 3-4 hours；
（7）, by step（6）Reacted reaction solution is added in belt vacuum filter and filtered, and filter residue, which is cleaned to PH, reaches 6-7, water
Fluorspar Powder finished product is crushed into when part is to less than 1.5%；
（8）, by step（7）Belt vacuum filter filters out the oxalic acid solution that filtrate adds addition 30% in sedimentation basin, and observation is without new
Precipitation, which produces, to be stopped adding oxalic acid；
（9）, by step（8）Oxalate precipitation is filtered and cleaned out with centrifugal filter from mixed liquor, and clear liquid is used to carry
Magnesium sulfate, ferrous sulfate, aluminum sulfate, zinc sulfate, manganese sulfate are taken, or is produced for multi-elements composite fertilizer；
（10）, by step（9）Filter residue after cleaning is calcined, and obtains earth oxide product.
Magnesium-rare earth flux waste residue proposes remaining magnesium alloy particles, chlorination in slag respectively through processes such as broken, water loggings
After thing, oxide, Fluorspar Powder, make after rare earth oxalate is calcined and rare earth oxide is made and uses with oxalic acid precipitation after sulfuric acid reaction
In fields such as Aero-Space, automobile, weaponry, hard-core technologies.
It should be pointed out that for the those skilled in the art of the art, under the premise without departing from the principles of the invention,
Some improvement and application can also be made, these are improved and application is also considered as protection scope of the present invention.
Claims (1)
- A kind of 1. recovery method of residual Re in magnesium-rare earth flux slag, it is characterised in that：Comprise the following steps：（1）, magnesium-rare earth flux ground-slag it is brokenMagnesium-rare earth flux slag is in small, broken bits to 30-40mm granularities through jaw crusher, and the coarse grain magnesium alloy of 30-40mm granularities is melted Agent slag is sent into chain type pulverizer and is crushed to 60-80 mesh；（2）, water loggingBy be crushed to 60-80 mesh magnesium alloy flux slag and water by 1:5 ratio mixes 60 minutes；（3）, the mixture of magnesium alloy flux slag and water added into centrifugal filter with pump, magnesium alloy particles are dehydrated to 1- on machine 1.5% recovery Mg-alloy particles are used for producing for high purity magnesium；（4）, by step（3）The solution that centrifuge is isolated, which is added in belt vacuum filter, to be filtered；（5）, step（4）Extraction chloride produces magnesium alloy flux, step after belt vacuum filter filters out filtrate（4）Belt is true Empty filter filters out in filter residue addition carburizing reagent equipment and CO2After reaction, belt vacuum filter is added；（6）, step（5）Belt vacuum filter filters out filter residue and sulfuric acid reaction, reacts 3-4 hours；（7）, by step（6）Reacted reaction solution is added in belt vacuum filter and filtered, and filter residue, which is cleaned to pH, reaches 6-7, water Fluorspar Powder finished product is crushed into when part is to less than 1.5%；（8）, by step（7）Belt vacuum filter filters out the oxalic acid solution that filtrate adds addition 30% in sedimentation basin, and observation is without new Precipitation, which produces, to be stopped adding oxalic acid；（9）, by step（8）Oxalate precipitation is filtered and cleaned out with centrifugal filter from mixed liquor, and clear liquid is used to carry Magnesium sulfate, ferrous sulfate, aluminum sulfate, zinc sulfate, manganese sulfate are taken, or is produced for multi-elements composite fertilizer；（10）, by step（9）Filter residue after cleaning is calcined, and obtains earth oxide product.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711001068.1A CN107746968A (en) | 2017-10-24 | 2017-10-24 | The recovery method of residual Re in magnesium-rare earth flux slag |
| CN202110471663.1A CN113136490A (en) | 2017-10-24 | 2017-10-24 | Method for recovering residual rare earth in rare earth magnesium alloy flux slag |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711001068.1A CN107746968A (en) | 2017-10-24 | 2017-10-24 | The recovery method of residual Re in magnesium-rare earth flux slag |
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| CN202110471663.1A Division CN113136490A (en) | 2017-10-24 | 2017-10-24 | Method for recovering residual rare earth in rare earth magnesium alloy flux slag |
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| CN107746968A true CN107746968A (en) | 2018-03-02 |
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| CN201711001068.1A Pending CN107746968A (en) | 2017-10-24 | 2017-10-24 | The recovery method of residual Re in magnesium-rare earth flux slag |
| CN202110471663.1A Pending CN113136490A (en) | 2017-10-24 | 2017-10-24 | Method for recovering residual rare earth in rare earth magnesium alloy flux slag |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110468275A (en) * | 2019-09-27 | 2019-11-19 | 中国恩菲工程技术有限公司 | Remove the method for sulfate radical and the product obtained by this method in rare-earth precipitation object |
| CN110484754A (en) * | 2019-09-27 | 2019-11-22 | 中国恩菲工程技术有限公司 | Remove the method for sulfate radical and the product obtained by this method in rare-earth precipitation object |
| CN112279276A (en) * | 2020-10-13 | 2021-01-29 | 宜兴市宏丰化肥有限公司 | Agricultural harmless treatment process for industrial byproduct potassium salt |
| CN114250366A (en) * | 2019-09-10 | 2022-03-29 | 山西宝盛远华新材料股份有限公司 | Method and equipment for recovering magnesium refining flux waste residue by using boiling point difference |
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| CN101353178A (en) * | 2002-06-07 | 2009-01-28 | 昭和电工株式会社 | Process for recovering rare earth oxide, process for producing abrasive containing rare earth oxide and polishing method using abrasive |
| CN103030312A (en) * | 2013-01-10 | 2013-04-10 | 朱广东 | Treatment method of magnesium metal smelting waste slag |
| CN104261703A (en) * | 2014-09-30 | 2015-01-07 | 扬州大学 | Method for recycling rare earth magnesium alloy smelting slag |
| CN105603202A (en) * | 2016-03-22 | 2016-05-25 | 闻喜县远华冶金材料有限公司 | System and method for producing magnesium and magnesium alloy solvent from waste solvent residues |
| CN106241842A (en) * | 2016-08-30 | 2016-12-21 | 闻喜县远华冶金材料有限公司 | The production method of light magnesium carbonate |
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| CA1129798A (en) * | 1980-08-18 | 1982-08-17 | Leroy R. Clavenna | System for the recovery of alkali metal compounds for reuse in a catalytic coal conversion process |
| CN102828053B (en) * | 2012-09-05 | 2013-09-04 | 北方民族大学 | Method for smelting magnesium metal with rare earth waste serving as mineralizing agent |
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2017
- 2017-10-24 CN CN201711001068.1A patent/CN107746968A/en active Pending
- 2017-10-24 CN CN202110471663.1A patent/CN113136490A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353178A (en) * | 2002-06-07 | 2009-01-28 | 昭和电工株式会社 | Process for recovering rare earth oxide, process for producing abrasive containing rare earth oxide and polishing method using abrasive |
| CN103030312A (en) * | 2013-01-10 | 2013-04-10 | 朱广东 | Treatment method of magnesium metal smelting waste slag |
| CN104261703A (en) * | 2014-09-30 | 2015-01-07 | 扬州大学 | Method for recycling rare earth magnesium alloy smelting slag |
| CN105603202A (en) * | 2016-03-22 | 2016-05-25 | 闻喜县远华冶金材料有限公司 | System and method for producing magnesium and magnesium alloy solvent from waste solvent residues |
| CN106241842A (en) * | 2016-08-30 | 2016-12-21 | 闻喜县远华冶金材料有限公司 | The production method of light magnesium carbonate |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114250366A (en) * | 2019-09-10 | 2022-03-29 | 山西宝盛远华新材料股份有限公司 | Method and equipment for recovering magnesium refining flux waste residue by using boiling point difference |
| CN110468275A (en) * | 2019-09-27 | 2019-11-19 | 中国恩菲工程技术有限公司 | Remove the method for sulfate radical and the product obtained by this method in rare-earth precipitation object |
| CN110484754A (en) * | 2019-09-27 | 2019-11-22 | 中国恩菲工程技术有限公司 | Remove the method for sulfate radical and the product obtained by this method in rare-earth precipitation object |
| CN110484754B (en) * | 2019-09-27 | 2021-08-10 | 中国恩菲工程技术有限公司 | Method for removing sulfate radical in rare earth precipitate and product obtained by method |
| CN112279276A (en) * | 2020-10-13 | 2021-01-29 | 宜兴市宏丰化肥有限公司 | Agricultural harmless treatment process for industrial byproduct potassium salt |
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| CN113136490A (en) | 2021-07-20 |
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Address after: 043800 Shanxi city in Yuncheng province Xin Village Wenxi County town of Ao Di Applicant after: Shanxi Baosheng Yuanhua New Material Co., Ltd Applicant after: Zhu Guangdong Address before: 043800 Shanxi city in Yuncheng province Xin Village Wenxi County town of Ao Di Applicant before: WENXI YUANHUA METALLURGICAL MATERIALS Co.,Ltd. Applicant before: Zhu Guangdong |
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Application publication date: 20180302 |