CN102154558B - Method for recovering rare earth by segments from neodymium iron boron waste - Google Patents
Method for recovering rare earth by segments from neodymium iron boron waste Download PDFInfo
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- CN102154558B CN102154558B CN201110070156A CN201110070156A CN102154558B CN 102154558 B CN102154558 B CN 102154558B CN 201110070156 A CN201110070156 A CN 201110070156A CN 201110070156 A CN201110070156 A CN 201110070156A CN 102154558 B CN102154558 B CN 102154558B
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Abstract
The invention discloses a method for recovering rare earth by segments from neodymium iron boron waste. The method comprises the following steps: with a segment extraction separation method, clearly classifying the impurities in rare earth chloride into each rare earth component in a four-segment multilevel extractor; and mutually and independently processing the rare earth element components by the subsequent precipitation roasting technology to obtain high-purity rare earth oxide. With the method, the recovery rate of the valuable rare earth element from the neodymium iron boron waste can be 98%, and the quality of the rare earth product can be guaranteed.
Description
Technical field
The present invention relates to rare earth resources and reclaim and the recycle utilization field, particularly relate to a kind of from neodymium iron boron waste material the method for segmentation recovery rare earth.
Background technology
Nd-Fe-B permanent magnet is a kind of permanent magnet material of superior performance, since nineteen eighty-three comes out, just from numerous permanent magnet materials, has shown one's talent, and is widely used in high-tech every field.Become the outstanding person in the permanent magnet material owing to Nd-Fe-Bo permanent magnet material has high remanent magnetism, high-coercive force, high energy product, be acknowledged as " magnetic king ".China is at the industrial system that has begun to take shape oneself aspect the Nd-Fe-Bo permanent magnet material production, and output accounts for 45% of global total value.In recent years, the output of Chinese sintered NdFeB is with 35% speed increment, and the output of estimation China's neodymium iron boron in 2010 is above 100,000 tons.
In the process of producing the Nd-Fe-B permanent magnetic element, must carry out mechanical workout to it, and make it to become the magnetic spare of rectangle, square, circle, inside and outside circle, watt shape and special shape.In this course of processing, will produce the waste material of many blanks, material cutting and abrasive material class, and add underproof magnetic spare, its amount of waste material is about raw material weight about 30%.With 100,000 tons of neodymium iron boron yield meters of China in 2010, about 30,000 tons of neodymium iron boron leftover bits then and substandard product total amount.
The moity of neodymium iron boron leftover bits is almost completely consistent with finished product, contains about 30% the REE of having an appointment, 60～65% iron, and other has cobalt, aluminium.About about 90% is Nd in the above-mentioned REE, and all the other are Dy, Tb, Gd, Ho etc.; Along with of the employing of permanent magnet material manufacturer, contain Pr toward contact in the neodymium iron boron leftover bits to Pr or Pr-Nd raw material.
The production in the world; In the process that mind-set China shifts in the new material industry; Enjoy as the novel material industry on new high-tech industry basis and to look steadily day, as the rare earth hydromagnetic material of new material industry important component part, on especially neodymium iron boron is produced; Begun to take shape the industrial system of oneself, output has accounted for 45% of world's total value.
About the existing bibliographical information and the patent of neodymium iron boron waste material recoverying and utilizing method, its main method comprises according at present: the fluorochemical precipitator method, sulfuric acid-double salt precipitation technology, employing hydrochloric acid are full method, the oxidizing roasting-dissolving with hydrochloric acid etc. of dissolving of solvent; These methods lack the recovery that comprises different REEs such as Nd, Pr, Dy, Tb, Gd, Ho carries out the specific aim measure of clear minute matter.In concrete production implementation process, have that recovery utilization rate is low, solid-liquid generation of waste materials amount big and the not high situation of rare-earth products quality.
Summary of the invention
The purpose of this invention is to provide a kind of from neodymium iron boron waste material segmentation reclaim the method for rare earth; Its objective is for problem such as solve in the past that neodymium iron boron waste material reclaims that the existing recovery utilization rate of link was low, solid-liquid generation of waste materials amount big and the rare-earth products quality is not high, is the working method that raw material reclaims Praseodymium trioxide neodymium, dysprosium oxide, terbium sesquioxide, Holmium trioxide, gadolinium sesquioxide with the neodymium iron boron waste material thereby provide a kind of.
The objective of the invention is to realize like this: a kind of from neodymium iron boron waste material segmentation reclaim the method for rare earth, this method may further comprise the steps:
(1) pre-treatment: neodymium iron boron waste material is carried out pre-treatment, and the Fe element is converted into Fe in oxidizing roasting link control waste material system
2O
3Transformation efficiency>=99.5%;
(2) hydrochloric acid is excellent dissolves: will pass through the material body and function dissolving with hydrochloric acid after the oxidizing roasting, and filter and obtain filtered liq A and residue A; Detect REO content among the residue A, residue A is repeated to use the dissolving with hydrochloric acid after-filtration, the gained filtered liq merges among the filtered liq A, REO content≤0.5% in residue A;
(3) alkali lye neutralization and oxidation de-iron: A neutralizes with alkali lye with filtered liq, carries out oxidation with oxygenant, filters to obtain filtered liq B and residue B; Detect Fe constituent content among the filtered liq B, Fe constituent content≤0.5% in filtered liq B;
(4) hcl acidifying and degree of depth de-iron: filtered liq B is carried out acidifying with hydrochloric acid, carry out oxidation, filter and obtain filtered liq C and residue C with oxygenant; Detect Fe constituent content among the filtered liq C, Fe constituent content≤0.2% in filtered liq C;
(5) section extracting and separating: after filtered liq C being entered into 1 section of the extraction of 4 segmentation multi-stage solvent extraction devices; At P507-sulfonated kerosene-hydrochloric acid system; Through extracting 1 section extracting and separating; Make Pr, Nd element stay water, and heavy component Gd, Tb, Dy, Ho enter into organic phase, obtain raffinate D and strip liquor E; After strip liquor E entered into 2 sections of extractions,, make Gd, Tb element and a small amount of Dy element stay water, and heavy component Dy, Ho enter into organic phase, obtain raffinate F and strip liquor G through extracting 2 sections extracting and separating; After strip liquor G entered into 3 section 1 district of extraction,, make the Dy element stay water, and heavy component Ho enter into organic phase, obtains raffinate H and strip liquor I through extracting the extracting and separating in 3 section 1 district; After raffinate F entered into 3 section 2 district of extraction,, make Gd, Tb element stay water, and heavy component Dy enter into organic phase, obtains raffinate J and strip liquor K through extracting the extracting and separating in 3 section 2 district; After raffinate J entered into 4 sections of extractions,, make the Gd element stay water, and heavy component Tb enter into organic phase, obtains raffinate L and strip liquor M through extracting 4 sections extracting and separating;
(6) deposition roasting: roasting obtains the Praseodymium trioxide neodymium through deposition with raffinate D; After raffinate H and strip liquor K mixing, roasting obtains dysprosium oxide through deposition; Roasting obtains gadolinium sesquioxide through deposition with raffinate L; Strip liquor M is obtained terbium sesquioxide through the deposition roasting; Roasting obtains Holmium trioxide through deposition with strip liquor I.
4 segmentation multi-stage solvent extraction devices described in the step of method described in the invention (5) comprise 1 section of extraction, 2 sections of extractions, 3 sections of extractions, 4 sections of extractions, wherein extract 3 sections and comprise independently extraction section of two in two 1 districts and 2 districts.
Advantage of the present invention is: the present invention utilizes the method for section extracting and separating; In 4 segmentation multi-stage solvent extraction devices, be each REE component, thereby the separate post precipitation sinter process that passes through obtain the high purity rare earth oxide with the clear score matter of rare earth chloride.Adopt present method, have the valency REE can realize full recovering effect in the neodymium iron boron waste material, the rare earth oxide product quality is fully guaranteed.
Description of drawings
The present invention comprises 1 of Figure of description.
Figure of description for the present invention a kind of from neodymium iron boron waste material segmentation reclaim the process flow sheet of the method for rare earth.
Embodiment
Below in conjunction with embodiment the present invention is further specified.
The present invention a kind of from neodymium iron boron waste material segmentation reclaim the method for rare earth, this method may further comprise the steps:
(1) pre-treatment: neodymium iron boron waste material is carried out pulverization process, and 800 ℃ of following oxidizing roastings 3 hours, the Fe element was converted into Fe in the detection neodymium iron boron waste material system
2O
3Transformation efficiency be 99.7%;
(2) hydrochloric acid is excellent dissolves: will pass through the material body and function dissolving with hydrochloric acid after the oxidizing roasting, and filter and obtain filtered liq A and residue A; REO content is 0.45% among the detection residue A;
(3) alkali lye neutralization and oxidation de-iron: filtered liq A is neutralized with the sodium hydroxid aqueous solution, carry out oxidation, filter and obtain filtered liq B and residue B with ydrogen peroxide 50; The Fe constituent content is 0.4% among the detection filtered liq B;
(4) hcl acidifying and degree of depth de-iron: filtered liq B is carried out acidifying with hydrochloric acid, carry out oxidation, filter and obtain filtered liq C and residue C with ydrogen peroxide 50; Detect Fe constituent content among the filtered liq C, the Fe constituent content is 0.1% in filtered liq C;
(5) section extracting and separating: filtered liq C is entered into 4 segmentation multi-stage solvent extraction devices, and this multi-stage solvent extraction device comprises 1 section of extraction, 2 sections of extractions, 3 sections of extractions, 4 sections of extractions, wherein extracts 3 sections and comprises independently extraction section of two in two 1 districts and 2 districts; After filtered liq C entered into 1 section of extraction,,, make Pr, Nd element stay water, and heavy component Gd, Tb, Dy, Ho enter into organic phase, obtain raffinate D and strip liquor E through extracting 1 section extracting and separating at P507-sulfonated kerosene-hydrochloric acid system; After strip liquor E entered into 2 sections of extractions,, make Gd, Tb element and a small amount of Dy element stay water, and heavy component Dy, Ho enter into organic phase, obtain raffinate F and strip liquor G through extracting 2 sections extracting and separating; After strip liquor G entered into 3 section 1 district of extraction,, make the Dy element stay water, and heavy component Ho enter into organic phase, obtains raffinate H and strip liquor I through extracting the extracting and separating in 3 section 1 district; After raffinate F entered into 3 section 2 district of extraction,, make Gd, Tb element stay water, and heavy component Dy enter into organic phase, obtains raffinate J and strip liquor K through extracting the extracting and separating in 3 section 2 district; After raffinate J entered into 4 sections of extractions,, make the Gd element stay water, and heavy component Tb enter into organic phase, obtains raffinate L and strip liquor M through extracting 4 sections extracting and separating;
(6) deposition roasting: roasting obtains the Praseodymium trioxide neodymium through deposition with raffinate D; After raffinate H and strip liquor K mixing, roasting obtains dysprosium oxide through deposition; Roasting obtains gadolinium sesquioxide through deposition with raffinate L; Strip liquor M is obtained terbium sesquioxide through the deposition roasting; Roasting obtains Holmium trioxide through deposition with strip liquor I.
Detect gained Praseodymium trioxide neodymium, dysprosium oxide, gadolinium sesquioxide, terbium sesquioxide, Holmium trioxide purity all more than 99.5%, gained rare earth oxide product all is up to state standards and the industry standard requirement.
According to calculating, comprise that the total recovery utilization rate of REE of 5 products such as Praseodymium trioxide neodymium, dysprosium oxide, gadolinium sesquioxide, terbium sesquioxide, Holmium trioxide reaches 98.0% (weight ratio of neodymium iron boron waste material middle-weight rare earths element total amount relatively).
Claims (1)
- One kind from neodymium iron boron waste material segmentation reclaim the method for rare earth, it is characterized in that this method may further comprise the steps:(1) pre-treatment: neodymium iron boron waste material is carried out pre-treatment, and the Fe element is converted into Fe in oxidizing roasting link control waste material system 2O 3Transformation efficiency>=99.5%;(2) hydrochloric acid is excellent dissolves: will pass through the material body and function dissolving with hydrochloric acid after the oxidizing roasting, and filter and obtain filtered liq A and residue A; Detect REO content among the residue A, residue A is repeated to use the dissolving with hydrochloric acid after-filtration, the gained filtered liq merges among the filtered liq A, REO content≤0.5% in residue A;(3) alkali lye neutralization and oxidation de-iron: A neutralizes with alkali lye with filtered liq, carries out oxidation with oxygenant, filters to obtain filtered liq B and residue B; Detect Fe constituent content among the filtered liq B, Fe constituent content≤0.5% in filtered liq B;(4) hcl acidifying and degree of depth de-iron: filtered liq B is carried out acidifying with hydrochloric acid, carry out oxidation, filter and obtain filtered liq C and residue C with oxygenant; Detect Fe constituent content among the filtered liq C, Fe constituent content≤0.2% in filtered liq C;(5) section extracting and separating: after filtered liq C being entered into 1 section of the extraction of 4 segmentation multi-stage solvent extraction devices; At P507-sulfonated kerosene-hydrochloric acid system; Through extracting 1 section extracting and separating; Make Pr, Nd element stay water, and heavy component Gd, Tb, Dy, Ho enter into organic phase, obtain raffinate D and strip liquor E; After strip liquor E entered into 2 sections of extractions,, make Gd, Tb element and a small amount of Dy element stay water, and heavy component Dy, Ho enter into organic phase, obtain raffinate F and strip liquor G through extracting 2 sections extracting and separating; After strip liquor G entered into 3 section 1 district of extraction,, make the Dy element stay water, and heavy component Ho enter into organic phase, obtains raffinate H and strip liquor I through extracting the extracting and separating in 3 section 1 district; After raffinate F entered into 3 section 2 district of extraction,, make Gd, Tb element stay water, and heavy component Dy enter into organic phase, obtains raffinate J and strip liquor K through extracting the extracting and separating in 3 section 2 district; After raffinate J entered into 4 sections of extractions,, make the Gd element stay water, and heavy component Tb enter into organic phase, obtains raffinate L and strip liquor M through extracting 4 sections extracting and separating;(6) deposition roasting: roasting obtains the Praseodymium trioxide neodymium through deposition with raffinate D; After raffinate H and strip liquor K mixing, roasting obtains dysprosium oxide through deposition; Roasting obtains gadolinium sesquioxide through deposition with raffinate L; Strip liquor M is obtained terbium sesquioxide through the deposition roasting; Roasting obtains Holmium trioxide through deposition with strip liquor I.
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| CN201110070156A CN102154558B (en) | 2011-03-23 | 2011-03-23 | Method for recovering rare earth by segments from neodymium iron boron waste |
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Families Citing this family (15)
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| JP6017914B2 (en) * | 2012-10-10 | 2016-11-02 | 株式会社日立製作所 | Rare earth element separation method and separation apparatus |
| CN103343234B (en) * | 2013-07-19 | 2015-01-14 | 北京工业大学 | Method for preparing neodymium and iron oxides by using neodymium iron boron oil sludge through regeneration and co-precipitation |
| CN103482670B (en) * | 2013-09-10 | 2014-09-24 | 中铝稀土（常熟）有限公司 | Method for preparing high-purity dysprosium oxide |
| CN104480316B (en) * | 2014-12-24 | 2016-12-07 | 连云港市兆昱新材料实业有限公司 | A kind of simplified industrial method reclaiming Co element from neodymium iron boron magnetic materials waste material |
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| CN105087967A (en) * | 2015-08-30 | 2015-11-25 | 常州市鼎日环保科技有限公司 | Device for recycling rare earth elements in neodymium iron boron waste materials |
| CN106119558A (en) * | 2016-07-27 | 2016-11-16 | 信丰县包钢新利稀土有限责任公司 | The method that three grades of recirculated water solutions reclaim neodymium iron boron waste material filtering residue rare earth elements |
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| CN107794373B (en) * | 2017-11-06 | 2019-01-22 | 孙东江 | The integrated conduct method of the useless magnetic material of neodymium iron boron |
| CN108193051A (en) * | 2017-12-28 | 2018-06-22 | 长春工程学院 | A kind of neodymium iron boron powdered scrap room temperature wet method air, ozone secondary oxidation remove the device and method of iron |
| CN108018430A (en) * | 2017-12-28 | 2018-05-11 | 长春工程学院 | A kind of device and method of neodymium iron boron powdered scrap room temperature wet oxidation iron removaling |
| CN110306071A (en) * | 2018-07-26 | 2019-10-08 | 安徽金三隆再生资源有限公司 | A kind of method for extraction and purification of dysprosia |
| CN109666801B (en) * | 2019-03-07 | 2020-08-25 | 中稀天马新材料科技股份有限公司 | Method for recycling rare earth elements from high-silicon low-content neodymium iron boron waste |
| CN114574717B (en) * | 2022-03-09 | 2022-12-09 | 江苏国源稀土新材料有限公司 | Device and method for recycling praseodymium-neodymium oxide in sections from neodymium-iron-boron waste |
| CN115323164B (en) * | 2022-09-16 | 2024-02-20 | 赣州华卓再生资源回收利用有限公司 | Multistage calcining method for neodymium iron boron waste |
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