CN1119216A - Method for preparing neodymium and neodymium-dysprosium compounds from waste neodymium-iron-boron recovery - Google Patents

Method for preparing neodymium and neodymium-dysprosium compounds from waste neodymium-iron-boron recovery Download PDF

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CN1119216A
CN1119216A CN94111454A CN94111454A CN1119216A CN 1119216 A CN1119216 A CN 1119216A CN 94111454 A CN94111454 A CN 94111454A CN 94111454 A CN94111454 A CN 94111454A CN 1119216 A CN1119216 A CN 1119216A
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neodymium
rare earth
acid
solution
precipitate
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李呙昕
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Juntai Rare Earth Industry Co ltd Taixing City
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Juntai Rare Earth Industry Co ltd Taixing City
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    • 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
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    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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Abstract

The invention relates to a method for preparing neodymium and neodymium dysprosium compounds by recovering waste neodymium iron boron, which selects acid dissolution, precipitation or extraction separation according to the properties of neodymium iron boron and various elements contained in the neodymium iron boron, and gradually removes non-rare earth impurities to prepare rare earth oxides. The rare earth product meets the requirement of making neodymium-dysprosium alloy (total rare earth content is greater than or equal to 98%, Fe is less than 0.2%).

Description

Useless neodymium iron boron reclaims the method for producing neodymium and neodymium dysprosium compound
The present invention relates to hydrometallurgy and produce neodymium and neodymium dysprosium compound.
The production of neodymium compound at present is to adopt various rare-earth mineral, and mixed rare-earth oxide and muriate made through pre-treatment (acid is molten), extracting and separating, three steps of aftertreatment (precipitation, calcination).Annual both at home and abroad production of neodymium-iron-boron magnetic material and consumption are very big, the so just unavoidable NdFeB material that gives up in enormous quantities that produces, according to the retrieval, the useless neodymium iron boron of recycling makes neodymium compound and reaches than higher purity, goes back the both economical rational technology of none at present.
The purpose of this invention is to provide and a kind of wherein rare earth element is handled, reclaimed to useless neodymium iron boron, make the processing method of needed single neodymium compound or neodymium dysprosium compound, to remedy the deficiency of the raw material neodymium compound of producing the required rare earth metal of neodymium-iron-boron magnetic material on the market.
Character and composition situation according to neodymium-iron-boron magnetic material self, rare earth element is different with the characteristic of iron boron, the neodymium iron boron that will give up dissolving (hydrochloric acid, sulfuric acid, nitric acid) obtains waste material acid solution (chlorate solution, sulfate liquor, nitrate solution), the present invention adopts following method to handle, to obtain needed rare-earth products:
(1) waste solution adds Sodium sulfate anhydrous.min(99) (Na 2SO 4) carry out double salt precipitation, adding caustic soda (NaOH) alkali after the throw out washing changes, and precipitation of hydroxide adds hydrochloric acid (sulfuric acid, nitric acid), and to carry out acid molten, adds oxalic acid (H 2C 2O 4) or carbon ammonium (NH 4HCO 3) precipitation, the throw out washing filtering at high temperature carries out calcination, the rare earth oxide that obtains reclaiming with throw out then.
(2) the waste material acid solution adds H 2O 2With Fe 2+Be oxidized to Fe 3+, add HN 3H 2O transfers solution PH=3.5～4.5, forms Fe (OH) 3Precipitation, filtration, supernatant liquor carry out oxalic acid precipitation by method (1), make rare earth oxide.
(3) the waste material acid solution adds H 2O 2With Fe 2+Be oxidized to Fe 3+, adopt neutral extraction agent extracting and separating Fe 2+, the earth solution that obtains adds oxalic acid (or carbon ammonium) precipitation, washing filtering, and throw out at high temperature calcination obtains rare earth oxide.
(4) the waste material acid solution directly adds oxalic acid precipitation, adds H with acid solution 2O 2Washing and filtering, throw out is calcination at high temperature, obtains rare earth oxide.
The rare earth acid solution that obtains by method (1) carries out extracting and separating before oxalic acid precipitation separates different rare earth elements contained in the neodymium iron boron waste material and obtains single Neodymium trichloride and Dysprosium trichloride, and then does oxalic acid precipitation by method (1) and make Neodymium trioxide and dysprosium oxide.
The earth solution that obtains by method (3) extracting and separating can further adopt neodymium and the dysprosium that contains in neutrality or the acidic extractant rare-earth separating solution, obtain single Neodymium trichloride and Dysprosium trichloride, add oxalic acid precipitation, washing filtering, throw out calcination at high temperature obtains Neodymium trioxide and dysprosium oxide.
The present invention recycles neodymium iron boron waste material, makes needed rare-earth products, reaches the comprehensive utilization of waste product, and decontamination cuts the waste, and has good economic benefits and social benefit.
Embodiment: waste material (by material: hydrochloric acid＜industry 〉=1: 3～5) is added the dissolving with hydrochloric acid groove carry out acid and dissolve, obtain the chloride soln of iron and rare earth, and boron is insoluble to hydrochloric acid, treat all to dissolve after-filtration, filter residue is used to reclaim boron, filtrate is squeezed into setting tank, (by oxalic acid: rare earth content=1.2～1.5: (solution acidity is controlled at [H]=0.01～1N) and stirs and precipitate 1) to add oxalic acid to measure liquor capacity and rare earth concentration, after treating that precipitation is fully also clarified, the siphon supernatant liquor is used to reclaim iron, and throw out is with containing 1～3%H 2O 21～3%Hcl1～3% 2C 2O 4Solution washing 3～5 times, after iron level meets the requirements in the mensuration throw out, filtration obtains rare-earth oxalate, the oxalate earthen bowl of packing into is put into chamber type electric resistance furnace or tunnel furnace, under 850～900 ℃, constant temperature calcination 2-3 hour, cooling is come out of the stove and is obtained oxide compound, plastic bag packaging is as the raw material of electrolytic metal.Whole process flow:
Figure A9411145400071

Claims (5)

1、将废钕铁硼溶解(盐酸、硫酸、硝酸)得到废料酸溶液(氯化盐溶液、硫酸盐溶液、硝酸盐溶液)，采用以下方法进行处理，以得到所需要的稀土产品：1. Dissolve waste NdFeB (hydrochloric acid, sulfuric acid, nitric acid) to obtain waste acid solutions (chloride solution, sulfate solution, nitrate solution), and use the following methods to process to obtain the required rare earth products: (1)废料溶液加元明粉(Na2SO4)进行复盐沉淀，沉淀物水洗后加烧碱(NaOH)碱转，氢氧化物沉淀加盐酸(硫酸、硝酸)进行酸溶，加草酸(H2C2O4)或碳铵(NH4HCO3)沉淀，沉淀物水洗过滤，然后将沉淀物在高温下进行灼烧，得到回收的稀土氧化物。(1) Add sodium hydroxide (Na 2 SO 4 ) to the waste solution for double salt precipitation, add caustic soda (NaOH) to the precipitate after washing with water, add hydrochloric acid (sulfuric acid, nitric acid) to the hydroxide precipitate for acid dissolution, add oxalic acid ( H 2 C 2 O 4 ) or ammonium bicarbonate (NH 4 HCO 3 ) is precipitated, the precipitate is washed with water and filtered, and then the precipitate is burned at high temperature to obtain the recovered rare earth oxide. (2)废料酸溶液加H2O2将Fe2+氧化成Fe3+，加HN3H2O调溶液PH＝3.5～4.5，形成Fe(OH)3沉淀、过滤、上清液按方法(1)进行草酸沉淀，制成稀土氧化物。(2) Add H 2 O 2 to the waste acid solution to oxidize Fe 2+ to Fe 3+ , add HN 3 H 2 O to adjust the pH of the solution to 3.5-4.5, form Fe(OH) 3 precipitate, filter, and supernatant according to the method (1) Carry out oxalic acid precipitation to make rare earth oxides. (3)废料酸溶液加H2O2将Fe2+氧化成Fe3+，采用中性萃取剂萃取分离Fe2+，得到的稀土溶液加草酸(或碳铵)沉淀、水洗过滤，沉淀物在高温下灼烧得到稀土氧化物。(3) Add H 2 O 2 to waste acid solution to oxidize Fe 2+ into Fe 3+ , use neutral extractant to extract and separate Fe 2+ , add oxalic acid (or ammonium bicarbonate) to the obtained rare earth solution, wash and filter, and the precipitate Burning at high temperature to obtain rare earth oxides. (4)废料酸溶液直接加草酸沉淀，用酸溶液加H2O2洗涤过滤，沉淀物在高温下灼烧，得到稀土氧化物。(4) Add oxalic acid directly to the waste acid solution for precipitation, wash and filter the acid solution with H 2 O 2 , and burn the precipitate at high temperature to obtain rare earth oxides. 2、根据权利要求1中(1)所述的方法，将得到的稀土酸溶液在草酸沉淀前进行萃取分离将钕铁硼废料中所含的不同稀土元素分离得到单一的氯化钕和氯化镝，然后再按方法(1)做草酸沉淀制成氧化钕和氧化镝。2. According to the method described in (1) in claim 1, the rare earth acid solution obtained is extracted and separated before the oxalic acid precipitation, and the different rare earth elements contained in the NdFeB waste are separated to obtain a single neodymium chloride and chloride Dysprosium, then do oxalic acid precipitation according to method (1) and make neodymium oxide and dysprosium oxide. 3、根据权利要求1中(3)所述的方法，将萃取分离得到的稀土溶液可进一步采用中性或酸性萃取剂分离稀土溶液中含有的钕和镝，得到单一氯化钕和氯化镝，加草酸沉淀、水洗过滤，沉淀物在高温下灼烧得到氧化钕和氧化镝。3. According to the method described in (3) in claim 1, the rare earth solution obtained by extraction and separation can further adopt neutral or acidic extractant to separate neodymium and dysprosium contained in the rare earth solution to obtain single neodymium chloride and dysprosium chloride , add oxalic acid to precipitate, wash and filter with water, and burn the precipitate at high temperature to obtain neodymium oxide and dysprosium oxide. 4、根据权利要求1所述的方法，沉淀物用含有1～3％H2O2、1～3％Hcl、1～3％H2C2O4的水溶液洗涤3～5次。4. The method according to claim 1, wherein the precipitate is washed 3-5 times with an aqueous solution containing 1-3% H 2 O 2 , 1-3% Hcl, and 1-3% H 2 C 2 O 4 . 5、根据权利要求1所述的方法，将水洗过滤后的沉淀物在800～900℃的高温下灼烧2～3小时。5. The method according to claim 1, wherein the washed and filtered precipitate is burned at a high temperature of 800-900°C for 2-3 hours.
CN94111454A 1994-09-22 1994-09-22 Method for preparing neodymium and neodymium-dysprosium compounds from waste neodymium-iron-boron recovery Pending CN1119216A (en)

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Cited By (28)

* Cited by examiner, † Cited by third party
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CN1077603C (en) * 1998-05-12 2002-01-09 住友金属矿山株式会社 Recovering method of valuable composition from rare earth element-containing material and alloy powder obtained therefrom
CN1295357C (en) * 2005-05-08 2007-01-17 西安西骏新材料有限公司 Recovery method of valuable element in neodymium iron boron waste material
CN1321201C (en) * 2004-08-25 2007-06-13 日本磁力选矿株式会社 Method for recovering rear-earth element
CN102583492A (en) * 2012-02-20 2012-07-18 甘肃稀土新材料股份有限公司 Production process of neodymium oxide with small bulk density
WO2012113263A1 (en) * 2011-02-26 2012-08-30 赣州力赛科新技术有限公司 Method for removing iron and aluminum from iron-based waste material containing high-value elements through natural oxidation
CN103093916A (en) * 2013-02-06 2013-05-08 南京信息工程大学 Neodymium iron boron magnetic materials and preparation method of the same
CN103160681A (en) * 2013-02-19 2013-06-19 北京工业大学 Preprocessing method of preparing neodymium iron boron alloy by using neodymium iron boron grinding-material oil sludge
CN103160682A (en) * 2013-02-19 2013-06-19 北京工业大学 Preprocessing method of preparing neodymium iron boron alloy by using neodymium iron boron linear-cutting oil sludge
CN103343233A (en) * 2013-07-19 2013-10-09 北京工业大学 Method for recovering neodymium and iron from neodymium iron boron oil sludge
CN103343234A (en) * 2013-07-19 2013-10-09 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
CN103343235A (en) * 2013-07-19 2013-10-09 北京工业大学 Method for recovering neodymium and iron from neodymium iron boron oil sludge through two-step co-precipitation
CN103667715A (en) * 2013-12-17 2014-03-26 北京工业大学 A method for simultaneously recovering neodymium, praseodymium, dysprosium, cobalt, and iron from NdFeB sludge under C2H2O4-OH system
CN103911516A (en) * 2014-03-27 2014-07-09 全南晶环科技有限责任公司 Process for extracting neodymium from waste electronic ceramic powder
CN103917672A (en) * 2011-11-14 2014-07-09 住友金属矿山株式会社 Recovery method of rare earth elements
CN104388711A (en) * 2014-12-11 2015-03-04 内蒙古科技大学 Method for recovering rare earth by leaching rare earth oxide molten slag
WO2016019044A1 (en) * 2014-07-29 2016-02-04 Trustees Of The University Of Pennsylvania Simple chemical method for the separation of rare earth metals
CN107470640A (en) * 2017-09-26 2017-12-15 北京京磁电工科技有限公司 The waste material of neodymium iron boron magnetic body recycles preparation technology
CN107758679A (en) * 2017-10-10 2018-03-06 北京工业大学 A kind of technique that boron is reclaimed from waste and old NdFeB material
CN107794373A (en) * 2017-11-06 2018-03-13 王志勇 The integrated conduct method of the useless magnetic material of neodymium iron boron
CN108004412A (en) * 2017-12-28 2018-05-08 长春工程学院 A kind of room temperature wet method ozone oxidation goes iron removaling and the equipment and technique of organic matter from neodymium iron boron greasy filth waste material
CN108018429A (en) * 2017-12-28 2018-05-11 长春工程学院 A kind of method that room temperature ultrasound-hydrogen peroxide wet oxidation removes the impurity such as iron removaling and organic matter from neodymium iron boron waste material
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
CN108018427A (en) * 2017-12-28 2018-05-11 长春工程学院 A kind of method of room temperature wet method UV-ozone oxidation organics removal from neodymium iron boron greasy filth waste material
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
CN108559845A (en) * 2017-12-28 2018-09-21 长春工程学院 A kind of method that the oxidation of room temperature wet method ultrasound-ozone removes iron and organic matter from neodymium iron boron greasy filth waste material
CN110607537A (en) * 2019-09-26 2019-12-24 江西理工大学 A method for synchronously and efficiently extracting rare earth and iron from high-value recycled NdFeB waste
CN112301220A (en) * 2020-10-30 2021-02-02 包头市聚峰稀土有限责任公司 Method for reducing iron content in rare earth sulfate water leaching solution
CN116818983A (en) * 2023-06-14 2023-09-29 中国检验认证集团宁波有限公司 Rare earth oxide content determination method for NdFeB waste material

Cited By (38)

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CN1077603C (en) * 1998-05-12 2002-01-09 住友金属矿山株式会社 Recovering method of valuable composition from rare earth element-containing material and alloy powder obtained therefrom
CN1321201C (en) * 2004-08-25 2007-06-13 日本磁力选矿株式会社 Method for recovering rear-earth element
CN1295357C (en) * 2005-05-08 2007-01-17 西安西骏新材料有限公司 Recovery method of valuable element in neodymium iron boron waste material
WO2012113263A1 (en) * 2011-02-26 2012-08-30 赣州力赛科新技术有限公司 Method for removing iron and aluminum from iron-based waste material containing high-value elements through natural oxidation
CN103917672A (en) * 2011-11-14 2014-07-09 住友金属矿山株式会社 Recovery method of rare earth elements
CN103917672B (en) * 2011-11-14 2016-06-22 住友金属矿山株式会社 Recovery method of rare earth elements
CN102583492A (en) * 2012-02-20 2012-07-18 甘肃稀土新材料股份有限公司 Production process of neodymium oxide with small bulk density
CN103093916A (en) * 2013-02-06 2013-05-08 南京信息工程大学 Neodymium iron boron magnetic materials and preparation method of the same
CN103160681A (en) * 2013-02-19 2013-06-19 北京工业大学 Preprocessing method of preparing neodymium iron boron alloy by using neodymium iron boron grinding-material oil sludge
CN103160682A (en) * 2013-02-19 2013-06-19 北京工业大学 Preprocessing method of preparing neodymium iron boron alloy by using neodymium iron boron linear-cutting oil sludge
CN103343233A (en) * 2013-07-19 2013-10-09 北京工业大学 Method for recovering neodymium and iron from neodymium iron boron oil sludge
CN103343235A (en) * 2013-07-19 2013-10-09 北京工业大学 Method for recovering neodymium and iron from neodymium iron boron oil sludge through two-step co-precipitation
CN103343234A (en) * 2013-07-19 2013-10-09 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
CN103343235B (en) * 2013-07-19 2015-03-25 北京工业大学 Method for recovering neodymium and iron from neodymium iron boron oil sludge through two-step co-precipitation
CN103343233B (en) * 2013-07-19 2015-10-28 北京工业大学 A kind of neodymium iron boron greasy filth reclaims the method for neodymium iron
CN103667715A (en) * 2013-12-17 2014-03-26 北京工业大学 A method for simultaneously recovering neodymium, praseodymium, dysprosium, cobalt, and iron from NdFeB sludge under C2H2O4-OH system
CN103667715B (en) * 2013-12-17 2016-05-18 北京工业大学 A kind of at C2H2O4Under-OH system, from neodymium iron boron greasy filth, reclaim the method for neodymium, praseodymium, dysprosium, cobalt, iron simultaneously
CN103911516A (en) * 2014-03-27 2014-07-09 全南晶环科技有限责任公司 Process for extracting neodymium from waste electronic ceramic powder
CN103911516B (en) * 2014-03-27 2015-10-28 全南晶环科技有限责任公司 A kind of technique extracting neodymium from waste electronic ceramics powder
WO2016019044A1 (en) * 2014-07-29 2016-02-04 Trustees Of The University Of Pennsylvania Simple chemical method for the separation of rare earth metals
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CN104388711A (en) * 2014-12-11 2015-03-04 内蒙古科技大学 Method for recovering rare earth by leaching rare earth oxide molten slag
CN107470640A (en) * 2017-09-26 2017-12-15 北京京磁电工科技有限公司 The waste material of neodymium iron boron magnetic body recycles preparation technology
CN107470640B (en) * 2017-09-26 2019-10-01 北京京磁电工科技有限公司 The waste material of neodymium iron boron magnetic body recycles preparation process
CN107758679A (en) * 2017-10-10 2018-03-06 北京工业大学 A kind of technique that boron is reclaimed from waste and old NdFeB material
CN107758679B (en) * 2017-10-10 2020-01-24 北京工业大学 Process for recovering boron from waste neodymium iron boron material
CN107794373A (en) * 2017-11-06 2018-03-13 王志勇 The integrated conduct method of the useless magnetic material of neodymium iron boron
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
CN108559845A (en) * 2017-12-28 2018-09-21 长春工程学院 A kind of method that the oxidation of room temperature wet method ultrasound-ozone removes iron and organic matter from neodymium iron boron greasy filth waste material
CN108018427A (en) * 2017-12-28 2018-05-11 长春工程学院 A kind of method of room temperature wet method UV-ozone oxidation organics removal from neodymium iron boron greasy filth waste material
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
CN108018429A (en) * 2017-12-28 2018-05-11 长春工程学院 A kind of method that room temperature ultrasound-hydrogen peroxide wet oxidation removes the impurity such as iron removaling and organic matter from neodymium iron boron waste material
CN108004412A (en) * 2017-12-28 2018-05-08 长春工程学院 A kind of room temperature wet method ozone oxidation goes iron removaling and the equipment and technique of organic matter from neodymium iron boron greasy filth waste material
CN110607537A (en) * 2019-09-26 2019-12-24 江西理工大学 A method for synchronously and efficiently extracting rare earth and iron from high-value recycled NdFeB waste
CN110607537B (en) * 2019-09-26 2021-02-26 江西理工大学 A method for synchronously and efficiently extracting rare earth and iron in high-value recycled NdFeB waste
CN112301220A (en) * 2020-10-30 2021-02-02 包头市聚峰稀土有限责任公司 Method for reducing iron content in rare earth sulfate water leaching solution
CN116818983A (en) * 2023-06-14 2023-09-29 中国检验认证集团宁波有限公司 Rare earth oxide content determination method for NdFeB waste material

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