CN102719674A - Method for extracting rare earth from oxidized neodymium iron boron waste - Google Patents
Method for extracting rare earth from oxidized neodymium iron boron waste Download PDFInfo
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- CN102719674A CN102719674A CN2012102419951A CN201210241995A CN102719674A CN 102719674 A CN102719674 A CN 102719674A CN 2012102419951 A CN2012102419951 A CN 2012102419951A CN 201210241995 A CN201210241995 A CN 201210241995A CN 102719674 A CN102719674 A CN 102719674A
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Abstract
The invention discloses a method for extracting rare earth from oxidized neodymium iron boron waste. The method comprises the following steps of: mixing the neodymium iron boron waste with water and then grinding; oxidizing the ground neodymium iron boron waste; performing primary grinding of the oxidation product; adding acid and leaching; separating solid from liquid; extracting to remove iron; chloridizing rare earth; extracting and separating rare earth; extracting to remove aluminum; precipitating; and firing. By adopting the method disclosed by the invention to recover the rare earth, the rare earth recovery rate is increased by 5-8%; and moreover, the use value of the recovered rare earth is increased, the production cost of further processing is lowered, the problem of muddy objects of the molten salt when in single rare earth electrolysis is effectively solved, the electrolysis efficiency when in the electrolysis of the rare earth metal is improved, the power consumption can be effectively reduced, and the content of the non-rare earth elements in metal such as C, S, O and the like is reduced.
Description
Technical field
The present invention relates to rare earth resources and reclaim and the recycle utilization field, particularly relate to the method for extracting rare earth a kind of neodymium iron boron waste material after oxidation.
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 money 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 brill, 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 money 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 mouth, as the rare earth permanent-magnetic material of new material industry important component part, on especially neodymium iron boron is produced; Begun to take shape the industrial system of controlling oneself, oneself has accounted for 45 % of the world's total value output.
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 are to comprising Nd, Pr, and Dy, Tb, Gd, the recovery of different REEs such as Ho lacks carries out the specific aim measure of clear minute matter.In concrete production implementation process, exist recovery utilization rate low, the big and not high situation of rare-earth products quality of solid, liquid generation of waste materials amount.
Summary of the invention
The purpose of this invention is to provide the method for extracting rare earth a kind of neodymium iron boron waste material after oxidation.; Its objective is that the existing recovery utilization rate of neodymium iron boron waste material recovery link was low in the past in order to solve; Problems such as the big and rare-earth products quality of solid, liquid generation of waste materials amount is not high are the working method that raw material reclaims oxidation Praseodymium trioxide neodymium, dysprosium oxide, terbium sesquioxide, Holmium trioxide, gadolinium sesquioxide thereby provide a kind of with neodymium boron waste material.
The objective of the invention is to realize like this: extract the method for rare earth a kind of neodymium iron boron waste material after oxidation, this method may further comprise the steps:
A. neodymium iron boron waste material is added the water allotment;
B. will transfer confected materials to filter;
C. the pug after filtering is carried out oxidizing roasting;
D. raw material behind ball milling is carried out the secondary Raymond mill;
E. the product of regrind being added acidleach goes out;
F. carry out solid-liquid separation to adding the product that acidleach goes out, the feed liquid extraction deironing after the separation forms rare earth chloride;
G. adopt P507 kerosene-hydrochloric acid separation system extracting and separating rare earth chloride;
H. in the rare earth chloride after separating, wherein praseodymium chloride neodymium is extracted except that aluminium;
I. the earth solution after separating is precipitated respectively;
J. deposition is carried out calcination.
Wherein, among the step a, the weight ratio of money iron boron waste material and water is preferably 2:3, and its positive negative error is no more than 10%.
Among the step a, be preferably deionized water with neodymium iron boron waste material blended water.
Among the step b, the size range of the pug that preferred control forms is the 90-200 order.
Among the step b, said pug preferably is controlled at 20 %-30% through the water cut after filtering.Its objective is the production efficiency that improves oxidation furnaces, and improve the oxidation efficiency of material, thereby improve the material organic efficiency.
Among the step c, the TR of oxidizing roasting is preferably between 800 degrees centigrade to 950 degrees centigrade.Its objective is the oxidation rate that improves ferrous salt, improve the material organic efficiency.
Step e, the acid of adding is preferably one or more in hydrochloric acid, nitric acid and the sulfuric acid.
Step e also adds oxide compound in the product that regrind obtains, said oxide compound is preferably one or more in potassium permanganate, VAL-DROP, Potcrate and the ydrogen peroxide 50.
Among the step h, adopt naphthenic acid extraction agent extraction aluminum ion earlier; Separate the back and add the oxalic acid precipitation rare earth again, rare earth and aluminium are separated containing aluminum solutions.
In the step I, add bicarbonate of ammonia or yellow soda ash with precipitating rare earth.
In the above-mentioned method that from neodymium iron boron waste material, reclaims REE, increased the technological process that extraction removes aluminium.Its objective is the aluminium element of removing in the reclaimed materials REE, reclaim rare earth oxide in electrolytic process, because contained aluminium element is assembled the negative effect of being brought near electric tank cathode thereby reduce; Comprise the reduction power consumption; Increase electrolytic efficiency, prolong bath life, increase quality of rare earth metal product or the like; Thereby optimized the extended field of rare-earth products, improved the rare earth metal performance of products.
Beneficial effect:
(1) compares and traditional grind operation and need money iron boron leftover bits be ground into 100-800 purpose fine powder or micro mists; The inventive method only need be shredded the neodymium iron boron leftover bits below the 100g/ piece; Stopped injury and the pollution of airborne dust, micro mist, avoided the consumption of a large amount of rare gas element, reduced the consumption of coal, electric energy significantly site operation personnel and surrounding enviroment; There is any danger in that production operation and control process are medium and small; Simultaneously, labour intensity greatly reduces, and shorten dramatically working cycle.
(2) pretreatment process is under normal operation, the 1st shell ring position only in order to the spontaneous combustion heat production of iron boron waste material fragment in rotary kiln of spending money as unique thermal source in the kiln, reach the purpose of oxidizing roasting through its spontaneous heat production, need not external heat source power.So can reduce the consumption of extra powers such as ability coal, electricity significantly.
(3) control between each shell ring through many shell rings internal heating self-combusting rotary kiln and shell ring, can be so that neodymium iron boron waste material be realized abundant oxidizing roasting effect, and can satisfy the quantity-produced requirement, do to imitate effect and production efficiency greatly improves.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Extract the method flow of rare earth a kind of neodymium iron boron waste material after oxidation as shown in Figure 1, the steps include: 1) ball milling: money iron boron waste material is mixed with water and carries out ball milling, the strict granularity of controlling generation pug behind ball milling, size range is the 90-200 order; Its objective is the degree of oxidation that improves ferrous salt, improve the organic efficiency of rare earth.Make money the ratio of iron boron waste material and water at 2:3 in the ball milling time control, and its positive negative error is no more than 10%; Its objective is the raising grinding efficiency, help controlling raw meal particle size, and the degree of oxidation that improves ferrous salt, organic efficiency improved.The ball milling water is the de-ionized pure water, its objective is the non-rare earth impurity that reduces in the product, like Ca
2+, Mg
2+, Si, Mn, B
-Reach even be lower than level Deng, the non-rare earth impurity content that make to reclaim product with the non-rare earth impurity content of the product of conventional raw material production.
2) vacuum filtration: utilize aspiration vacuum to accelerate filtration velocity, the water cut of control raw material to increase the oxidation ratio of material, improves the yield of rare earth at 20%-30%.
3) oxidizing roasting: at high temperature with the oxidizing roasting of ground slip, main purpose is to reduce the solubility rate of iron when adding acidleach and going out.The controlled oxidation temperature is between 800 ℃-950 ℃, and the time is more than 90min, to improve Fe
2+Oxidation rate, thereby the recovery is improved.
4) regrind: the material that oxidation is qualified grinds, and mainly is to improve rare earth yield.
5) adding acidleach goes out: purpose is the whole strippings of the rare earth in the waste material, and carries out solid-liquid separation.
6) extraction deironing: the iron in the feed liquid is effectively separated with rare earth through extraction.
7) rare earth chloride: in adding the process that acidleach goes out because the adding of hydrochloric acid forms the muriate of iron and REE, in the process of extraction iron, neutral extraction agent N235 with the rare earth ion reaction, the iron nature separates with REE, the formation rare earth chloride.
Rare Earth Separation: be separated into single rare earth solution to the rare earth in the earth solution through P507 kerosene-hydrochloric acid separation system.
9) extraction removes aluminium: extraction removes the concrete principle of aluminium and is operating as: aluminium is present in the earth solution as metals ion, can't remove in its operation in front; Because aluminum ions separation factor between praseodymium ion and neodymium ion, adopts naphthenic acid extraction agent extraction aluminum ion earlier, the while is extracting rare-earth slightly, has so just reached separating of aluminium and rare earth; Separate back output high alumina rare earth and two kinds of solution of low aluminium rare earth, high aluminum solutions is added the oxalic acid precipitation rare earth again, rare earth and aluminium are separated.This technological operation is simple, and is stable, on extraction is produced, fully used.
10) deposition, calcination: this workshop section is converted into rare earth oxide with the single rare earth after separating, the raw material that adds as the single rare earth metal.
Through evidence: add acidleach and go out in the step, the acid of adding can be following one or more: hydrochloric acid, nitric acid, sulfuric acid etc.Add acidleach and go out in the step, also can in system, add following oxide compound: one or more in potassium permanganate, VAL-DROP, Potcrate, the ydrogen peroxide 50.
In the settling step, in system, add bicarbonate of ammonia or yellow soda ash with precipitating rare earth.
Claims (1)
1. extract the method for rare earth the neodymium iron boron waste material after oxidation, it is characterized in that: this method may further comprise the steps:
A. neodymium iron boron is given up and carry out oxidizing roasting;
B. the raw material after the roasting is carried out ball-milling processing;
C. raw material behind ball milling is carried out the secondary Raymond mill;
D. the product of regrind being added acidleach goes out;
E. carry out solid-liquid separation to adding the product that acidleach goes out, the feed liquid extraction deironing after the separation forms rare earth chloride;
F. adopt kerosene-hydrochloric acid separation system extracting and separating rare earth chloride;
G. in the rare earth chloride after separating, wherein praseodymium chloride neodymium is extracted except that aluminium;
H. the earth solution after separating is precipitated respectively;
I. deposition is carried out calcination;
J. to the warehouse-in that sieves of the batch mixing after the calcination.
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| CN103146921A (en) * | 2013-04-07 | 2013-06-12 | 内蒙古包钢稀土(集团)高科技股份有限公司 | Method for removing aluminum in rare-earth solution |
| CN103409649A (en) * | 2013-06-05 | 2013-11-27 | 哈尔滨工程大学 | Method and device for reducing, extracting and separating rear earth through fused salt and liquid metal |
| CN104446412A (en) * | 2014-11-14 | 2015-03-25 | 连云港市兆昱新材料实业有限公司 | High-performance permanent-magnet ferrite pre-sintered material prepared based on NdFeB wastes and preparation method thereof |
| CN104446427A (en) * | 2014-11-18 | 2015-03-25 | 连云港市兆昱新材料实业有限公司 | Rare-earth doped spinel type ferrite magnetic powder prepared based on NdFeB wastes and preparation method thereof |
| CN104789773A (en) * | 2015-03-30 | 2015-07-22 | 德庆兴邦稀土新材料有限公司 | Rare-earth liquid impurity removal process |
| CN105002366A (en) * | 2015-07-14 | 2015-10-28 | 山东梁山天马永磁材料有限公司 | Method for recycling rear earth from neutralization dregs generated in process of recycling rear earth from neodymium-iron-boron waste material |
| CN105886801A (en) * | 2016-06-07 | 2016-08-24 | 福建省长汀金龙稀土有限公司 | Method for recovering precious rare earth element dysprosium from abandoned dysprosium-plated molybdenum plate |
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| CN107522222A (en) * | 2017-09-29 | 2017-12-29 | 吉安鑫泰科技股份有限公司 | A kind of new technology for precipitating praseodymium chloride neodymium |
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Application publication date: 20121010 |