CN103343233B - A kind of neodymium iron boron greasy filth reclaims the method for neodymium iron - Google Patents
A kind of neodymium iron boron greasy filth reclaims the method for neodymium iron Download PDFInfo
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Abstract
Neodymium iron boron greasy filth reclaims a method for neodymium iron, belongs to neodymium iron boron greasy filth recovery and utilization technology field.By acid-soluble for neodymium iron boron greasy filth hydrochloric acid and after filtering insolubles, after adding hydrogen peroxide oxidation, control certain pH value, temperature of reaction, add bicarbonate of ammonia and ammoniacal liquor or hydrofluoric acid and ammoniacal liquor successively, the physical properties of rare earth carbonate and rare earth fluorine and ferric hydroxide colloid is utilized to adsorb by being formed, co-precipitation goes out neodymium iron precipitation mixture, and the product roasting under suitable decomposition temperature after filtering respectively is obtained the compound of neodymium iron.Present invention, avoiding the loaded down with trivial details wet process pursuing single high-purity rare-earth in recovery, for follow-up preparation neodymium iron boron regeneration magnetic powder provides favourable condition.
Description
Technical field
The present invention relates to and a kind ofly neodymium iron boron greasy filth is utilized ferric hydroxide colloid adsorption coprecipitation neodymium iron and reclaims the method for neodymium iron, belong to neodymium iron boron greasy filth recovery and utilization technology field.
Background technology
Nowadays, just have in every 6 new technologies one relevant with rare earth, this absolutely proves the role and importance of rare earth in new technology.Rare earth is 21 century important strategic resource, is modern industry " monosodium glutamate ".Why rare earth element is called as " 21 century strategy element ", is because it has other elements and does not possess specific physical character and chemical property.Based on many rare earth new materials that these characteristics are made, excellent performance, of many uses, by a large amount of for fields such as electronic information, mechanics of communication, automobile making, the energy and aerospace.Rare earth was described as once " material VITAMIN " and " 21 century high-tech and the treasure-house of functional materials " etc.
Rare earth element is as the rare and grand strategy resource of costliness, and the valuable element in synthetical recovery waste material is very valuable work; Reasonable recovering rare earth element, can not only save and protect national resource, reduce costs and increase economic efficiency, and is conducive to domestic each field and develops steadily in the long term, also helps the cycling and reutilization of rare earth element and the Sustainable development of country.
And as being rich in the neodymium iron boron of rare earth element didymium, neodymium iron boron reclaiming work is seemed very important naturally.Iron boron magnet magnetic energy product is 240 ~ 440kJ/m
3, being referred to as the present age " king of permanent magnetism ", is the permanent magnet material that over-all properties known is at present the highest.Compared with traditional magnet, the magnetic energy product of rare earth permanent-magnetic material will exceed 4 ~ 10 times, and other magnetic properties also far exceed conventional magnet; And the magnetic energy product of Nd-Fe-Bo permanent magnet material more will exceed 8 ~ 10 times of traditional magnetic material.
The technical process of NdFeB waste recovery has multiple, as acid-soluble depositing technology, double salt conversion process, the excellent molten technique of hydrochloric acid etc.List the recovery method that some are traditional as follows:
Comprehensive above current Rare earth recovery method, although these techniques can regain rare earth, but also there are problems: first finally, the endless chain of above technique formation useless circulation truly, the product that these technique obtains is only rare earth oxide, and does not make the mechanicals that can directly use.And rare-earth oxidation material desire purify for industrial can direct applied high-purity single rare earth, also need to carry out tens grades of extraction process, its extraction agent is very expensive especially, and social benefit obviously reduces.Secondly from economic benefit, except above-mentioned when purification high-purity single rare earth, extraction process by consume a large amount of acid solution, time and costliness extraction agent beyond, the common acid-soluble precipitator method will carry out secondary sedimentation to rare earth when recovering rare earth, not only flow process is longer for it, invest higher, and the rate of recovery is lower, economic benefit is obviously very low; And in the technique of full extraction process Extraction of rare earth, although the purity of this technique rare earth when recovering rare earth is higher, and the cobalt element of higher degree can be obtained, but its numerous and diverse chemical technology and high cost make this method at the very start cannot accept by industrial production.Again, from the angle of energy-conserving and environment-protective, no matter be the excellent molten method of hydrochloric acid, full extraction process or the sulfuric acid double salt precipitator method, they all can form a large amount of acid-base waste fluids and toxic and harmful in rare earth reclaims.Only in extraction process, because need higher liquid liquor ratio and better back extraction effect, the consumption of its acid is all more than 10 times of normal chemical metering, and the acid-base waste fluid that these processes are formed all is difficult to process at technique end; Moreover, the sulfuric acid double salt precipitator method will produce the SO very large to human injury in the process reclaiming iron
2and H
2s gas.
Summary of the invention
The present invention is directed to these problems above-mentioned, generation has toughness, the rare earth fluorine of adsorptivity precipitates and rare earth carbonate precipitation, and utilize the physical properties of precipitation, form co-precipitation with iron ion, we are referred to as " colloid adsorption method ".Be when about 5 ~ 6 in pH value, bicarbonate of ammonia be added in rare earths salt, foundry loam shape rare earth carbonate precipitation RE can be separated out
2(CO
3)
3nH
2o.When these foundry loam shape Precipitations time, a large amount of ion will inevitably be adsorbed in surface.And bicarbonate of ammonia is weakly alkaline, easy and iron ion reacts.These two kinds reaction actings in conjunction, make iron and neodymium together precipitate.Add excessive hydrofluoric acid in earth solution, rare earth element can be converted into the fluorochemical REF of white gum
3nH
2o.The solubleness of rare earth fluorine is also less than rare-earth oxalate, and can obtain very high deposition rate.Its gelatinous precipitate generated can also adsorb iron ion and together precipitate.Neodymium iron reclaims by the method simultaneously, and technical process is short, not wasting of valuable element, and follow-up can be used to synthesizes NdFeB magnetic powder, realizes real recycle, the therefore economic and practical that had of the method.
A kind of neodymium iron boron greasy filth reclaims the method for neodymium iron, it is characterized in that, comprise the following steps: be by acid-soluble for neodymium iron boron greasy filth hydrochloric acid and after filtering insolubles, after adding hydrogen peroxide oxidation, control certain pH value, temperature of reaction, add bicarbonate of ammonia and ammoniacal liquor or hydrofluoric acid and ammoniacal liquor successively, the physical properties of rare earth carbonate and rare earth fluorine and ferric hydroxide colloid is utilized to adsorb by being formed, co-precipitation goes out neodymium iron precipitation mixture, and the product roasting under suitable decomposition temperature after filtering respectively is obtained the compound of neodymium iron.
The technical scheme that the present invention formulates is:
After acid-soluble for neodymium iron boron greasy filth filtration, add excessive mass concentration 30% hydrogen peroxide oxidation and stir, by the solution after oxidation by the pH value of ammoniacal liquor regulator solution to 5 ~ 6, in the hot solution of 35-50 DEG C, first adding mass concentration under continuous stirring is 40% hydrofluoric acid solution, then be placed in 50-70 DEG C of water-bath, intermittent stirring, in solution, form sticky sludge; Under water-bath temperature is 50-70 DEG C of state, be that 1:2 ammoniacal liquor dropwise joins in reactor by excessive volume ratio, intermittent stirring, after precipitation of iron ions is complete, centrifugal and clean solid, oven dry is placed in box-type furnace, roasting 90mins at T=800 DEG C, preferably the corresponding 2-3g hydrofluoric acid solution of every 5g neodymium iron boron greasy filth.
Or after the acid-soluble filtration of neodymium iron boron greasy filth, add excessive mass concentration 30% hydrogen peroxide oxidation and do not stop to stir, by the solution after oxidation by the pH value of ammoniacal liquor regulator solution to 5 ~ 6; In the hot solution of 35-50 DEG C, under constantly stirring, first add the ammonium bicarbonate soln of higher concentration 1mol/L.Then be placed in 50-70 DEG C of water-bath, intermittent stirring, in solution, form sticky sludge.Under water-bath temperature is 50-70 DEG C of state, be that 1:2 ammoniacal liquor dropwise joins in reactor by excessive volume ratio, intermittent stirring, treat that precipitation of iron ions is complete, solution centrifugal is cleaned solid, oven dry is placed in box-type furnace, roasting 90mins at T=800 DEG C, preferably every 5g neodymium iron boron greasy filth correspondence 138 ~ 210ml ammonium bicarbonate soln.
During preparation ammoniacal liquor, ammonia used is the ammoniacal liquor containing ammonia 25% ~ 28%.
In above-mentioned two kinds of methods, when neodymium iron boron greasy filth is acid-soluble, preferred solid-to-liquid ratio 1g:10-15ml.In the final iron neodymium product that the present invention is obtained by colloid adsorption method, iron neodymium mass content is respectively: 69.46% ~ 70.20%, 19.31% ~ 20.35%.
(1) the present invention can effectively reduce in neodymium-iron alloy co-precipitation, ferric hydroxide colloid is to the absorption of foreign ion, wherein the foreign matter content of bicarbonate of ammonia-Ammonia Process is not higher than 4%, and the foreign matter content of hydrofluoric acid-Ammonia Process is not higher than 3%, by adjusting process, the purity of neodymium-iron alloy still has the space of rising.
(2) rare earth carbonate and rare earth fluorine have more ripe technique, more stable to the precipitation of rare earth, are of value to the precipitation at co-precipitation neodymium-iron alloy middle-weight rare earths.
(3) present invention, avoiding the loaded down with trivial details wet process pursuing single high-purity rare-earth in recovery, for follow-up preparation neodymium iron boron regeneration magnetic powder provides favourable condition, is the committed step forming circulation industry.Realize business cycle chain, for " mine, city " lays a good foundation.
Accompanying drawing explanation
The XRD figure spectrum of material after Fig. 1 to be bicarbonate of ammonia-ammoniacal liquor be calcining that precipitation agent obtains;
The XRD figure spectrum of material after Fig. 2 to be hydrofluoric acid-ammoniacal liquor be calcining that precipitation agent obtains.
Embodiment
Below in conjunction with example, the present invention is further described, but the present invention is not limited to following examples.
Embodiment 1:
(1) get 5g neodymium iron boron greasy filth, in waste material, add 4mol/L hydrochloric acid 60ml, fully dissolve in backward filtrate and add 30% hydrogen peroxide oxidation 10mins and do not stop to stir, by the solution after oxidation by the pH value of ammoniacal liquor regulator solution to 5.In hot solution, under constantly stirring, first add mass ratio is at leisure 40% hydrofluoric acid solution 3g.Then place in 50-70 DEG C of water-bath, intermittent stirring, in solution, form sticky sludge.In a heated state, by excess volume than slowly, dropwise joining in reactor for 1:2 ammoniacal liquor, intermittent stirring.Treat that precipitation of iron ions is complete, solution centrifugal is cleaned.Clear liquid and washing lotion are discarded.Being dried by pelleting centrifugation is placed in box-type furnace, roasting 90mins at T=800 DEG C.
Or get 5g neodymium iron boron greasy filth, in waste material, add 4mol/L hydrochloric acid 60ml, fully dissolve in backward filtrate and add 30% hydrogen peroxide oxidation 10mins and do not stop to stir, by the solution after oxidation by the pH value of ammoniacal liquor regulator solution to 5.In hot solution, under constantly stirring, first add the ammonium bicarbonate soln 210ml of 1mol/L at leisure.Then place in water-bath, intermittent stirring, in solution, form sticky sludge.In a heated state, excessive 1:2 ammoniacal liquor slowly, is dropwise joined in reactor, intermittent stirring.Treat that precipitation of iron ions is complete, solution centrifugal is cleaned.Clear liquid and washing lotion are discarded.Being dried by pelleting centrifugation is placed in box-type furnace, roasting 90mins at T=800 DEG C.
Experimental result is as follows:
The XRF outcome quality % of table 1-1 hydrofluoric acid-ammoniacal liquor to be precipitation agent and bicarbonate of ammonia-ammoniacal liquor be material obtained after precipitation agent calcining
As can be seen from Fig. 1 and Fig. 2: be no matter be precipitation agent with hydrofluoric acid-ammoniacal liquor or be precipitation agent with bicarbonate of ammonia-ammoniacal liquor, the halfwidth of XRD spectral line is all very narrow, and the intensity at peak is also higher; But wherein do not have the existence mutually of rare earth oxide.Be that material after precipitation agent roasting is mainly Fe2O3, NdF3, NdOF with hydrofluoric acid-ammoniacal liquor.Bicarbonate of ammonia-ammoniacal liquor is that after the calcining that obtains of precipitation agent, material is mainly Fe2O3, NdClO.
The XRF result display of table 1-1, the iron obtained as precipitation agent with hydrofluoric acid-ammoniacal liquor and the element mass percent of neodymium are 69.46% and 20.35% respectively; The ratio of the iron obtained as precipitation agent with bicarbonate of ammonia-ammoniacal liquor and the element of neodymium is 70.20% and 19.31% respectively.All be comparatively close to original material ratio.The neodymium element recovering effect of hydrofluoric acid-ammoniacal liquor is slightly better than the recovering effect of bicarbonate of ammonia-ammoniacal liquor.The content of the praseodymium that hydrofluoric acid-Ammonia Process reclaims and cobalt is also slightly high, and other foreign matter contents are less.As can be seen from test result, the method for colloid absorption can precipitate recovering rare earth element and iron preferably.
Claims (2)
1. the method for a neodymium iron boron greasy filth recovery neodymium iron, it is characterized in that, after acid-soluble for neodymium iron boron greasy filth filtration, add excessive mass concentration 30% hydrogen peroxide oxidation not stop to stir, by the solution after oxidation by the pH value of ammoniacal liquor regulator solution to 5 ~ 6, in the hot solution of 35-50 DEG C, under constantly stirring, first add mass concentration is 40% hydrofluoric acid solution, then be placed in 50-70 DEG C of water-bath, intermittent stirring, in solution, form sticky sludge; Under control bath temperature is 50-70 DEG C of state, be that 1:2 ammoniacal liquor dropwise joins in reactor by excessive volume ratio, intermittent stirring, after precipitation of iron ions is complete, centrifugal and clean solid, oven dry is placed in box-type furnace, roasting 90mins at T=800 DEG C, the corresponding 2-3g hydrofluoric acid solution of every 5g neodymium iron boron greasy filth.
2. neodymium iron boron greasy filth reclaims a method for neodymium iron, it is characterized in that, after the acid-soluble filtration of neodymium iron boron greasy filth, adds excessive mass concentration 30% hydrogen peroxide oxidation and does not stop to stir, by the solution after oxidation by the pH value of ammoniacal liquor regulator solution to 5 ~ 6; In the hot solution of 35-50 DEG C, under constantly stirring, first add the ammonium bicarbonate soln of 1mol/L; Then place in 50-70 DEG C of water-bath, intermittent stirring, forming sticky sludge in solution, under bath temperature is 50-70 DEG C of state, is that 1:2 ammoniacal liquor dropwise joins in reactor by excessive volume ratio, intermittent stirring, treat that precipitation of iron ions is complete, solution centrifugal is cleaned solid, dries and be placed in box-type furnace, roasting 90mins at T=800 DEG C, every 5g neodymium iron boron greasy filth correspondence 138 ~ 210ml ammonium bicarbonate soln.
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