CN103343233A - Method for recovering neodymium and iron from neodymium iron boron oil sludge - Google Patents
Method for recovering neodymium and iron from neodymium iron boron oil sludge Download PDFInfo
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- CN103343233A CN103343233A CN2013103066222A CN201310306622A CN103343233A CN 103343233 A CN103343233 A CN 103343233A CN 2013103066222 A CN2013103066222 A CN 2013103066222A CN 201310306622 A CN201310306622 A CN 201310306622A CN 103343233 A CN103343233 A CN 103343233A
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Abstract
The invention relates to a method for recovering neodymium and iron from neodymium iron boron oil sludge, belonging to the technical field of recycling of neodymium iron boron oil sludge. The method comprises the following steps of: dissolving the neodymium iron boron oil sludge by using hydrochloric acid and filtering undissolved substances, and then, controlling a certain pH value and reaction temperature after oxidizing through adding hydrogen peroxide; sequentially adding ammonium bicarbonate and ammonium hydroxide or hydrofluoric acid and ammonium hydroxide; co-precipitating a neodymium and iron sediment mixture through adsorption among rare earth carbonate, rare earth fluoride and iron hydroxide colloid according to the physical properties of the rare earth carbonate and the rare earth fluoride; and respectively roasting a filtered product at the proper decomposition temperature to obtain a neodymium and iron compound. A complex wet-method process for obtaining single high-purity rare earth in recovery is avoided, and advantageous conditions are provided for subsequently preparing neodymium iron boron regeneration magnetic powder.
Description
Technical field
The present invention relates to a kind of method of neodymium iron boron greasy filth being utilized ferric hydroxide colloid adsorption coprecipitation neodymium iron and reclaiming neodymium iron, belong to neodymium iron boron greasy filth recovery and utilization technology field.
Background technology
Nowadays, just have in per 6 new technologies one relevant with rare earth, this proves absolutely effect and the status of rare earth in new technology.Rare earth is 21 century important strategic resource, is " monosodium glutamate " of modern industry.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, be used for fields such as electronic information, mechanics of communication, automobile making, the energy and aerospace in a large number.Rare earth was described as " material VITAMIN " and " 21 century high-tech and the treasure-house of functional materials " etc. once.
Rare earth element is as rare and expensive grand strategy resource, and the valuable element that comprehensively reclaims in the waste material is very valuable work; Rationally reclaim rare earth element, can not only save and protect national resource, reduce cost and increase economic efficiency, be conducive to domestic each field and develop steadily in the long term, also help the cycling and reutilization of rare earth element and the Sustainable development of country.
And as the neodymium iron boron that is rich in the rare earth element didymium, neodymium iron boron reclaiming work is seemed very important naturally.The iron boron magnet magnetic energy product is 240～440kJ/m
3, be known as the present age " king of permanent magnetism ", be the present known the highest permanent magnet material of over-all properties.Compare 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 the molten depositing technology of acid, double salt conversion process, the excellent molten technology of hydrochloric acid etc.Following some traditional recovery methods of listing:
Comprehensive above present rare earth recovery method, though these technologies can regain rare earth, but also there are problems: at first finally, the endless chain of above technology and formation useless circulation truly, the product that these technologies obtain only is rare earth oxide, and does not make the mechanicals that can directly use.And the rare-earth oxidation material desire purify for industrial can direct applied high-purity single rare earth, also need carry out tens grades of extraction process, its extraction agent is very expensive especially, social benefit obviously reduces.Secondly on economic benefit, except above-mentioned when the purification high-purity single rare earth, extraction process will consume beyond the extraction agent of a large amount of acid solutions, time and costliness, the common sour molten precipitator method will be carried out secondary sedimentation to rare earth when reclaiming rare earth, not only flow process is longer for it, invest higherly, and the rate of recovery is lower, and economic benefit is obviously very low; And extract in the technology of rare earth at full extraction process, though the purity of this technology rare earth when reclaiming rare earth is higher, and can obtain the cobalt element of higher degree, but its numerous and diverse chemical technology and high cost make this method can't accepted by industrial production at the very start.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, its sour consumption all is normal stoichiometric more than 10 times, and the acid-base waste fluid that these processes form is in technology end intractable all; Moreover, the sulfuric acid double salt precipitator method will produce the SO very big to the human injury in the process that reclaims iron
2And H
2S gas.
Summary of the invention
The present invention is directed to above-mentioned these problems, generate rare earth fluorine precipitation and rare earth carbonate precipitation with toughness, adsorptivity, utilize the physical properties of precipitation, form co-precipitation with iron ion, we are referred to as " colloid adsorption method ".When the pH value is about 5～6, bicarbonate of ammonia is added in the rare earths salt, can separate out foundry loam shape rare earth carbonate precipitation RE
2(CO
3)
3NH
2O.When these foundry loam shape precipitations were separated out, a large amount of ions will inevitably be adsorbed in the surface.And bicarbonate of ammonia is weakly alkaline, and easy and iron ion reacts.These two kinds reaction actings in conjunction make iron and neodymium together precipitate.Add excessive hydrofluoric acid in the earth solution, rare earth element can be converted into the gluey fluorochemical REF of white
3NH
2O.The solubleness of rare earth fluorine is also littler than rare-earth oxalate, and can obtain very high deposition rate.The gelatinous precipitate of its generation can also adsorb iron ion and together precipitate.This method reclaims neodymium iron simultaneously, and technical process is short, not the wasting of valuable element, and follow-uply can be used to synthetic NdFeB magnetic powder, realizes real recycle, so this method has the economic and practical of getting well.
A kind of neodymium iron boron greasy filth reclaims the method for neodymium iron, it is characterized in that, may further comprise the steps: be with neodymium iron boron greasy filth with hydrochloric acid acid molten and filter insolubles after, 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, utilize physical properties and the ferric hydroxide colloid of rare earth carbonate and rare earth fluorine to adsorb by forming, co-precipitation goes out neodymium iron precipitation mixture, the product roasting under suitable decomposition temperature after filtering is respectively obtained the compound of neodymium iron.
The technical scheme that the present invention formulates is:
After the molten filtration of neodymium iron boron greasy filth acid, add excessive mass concentration 30% hydrogen peroxide oxidation and stirring, with pH value to 5～6 of the solution after the oxidation with the ammoniacal liquor regulator solution, in 35-50 ℃ hot solution, constantly stirring down, elder generation's adding mass concentration is 40% hydrofluoric acid solution, be placed on then in the 50-70 ℃ of water-bath, intermittently stir, form foundry loam shape precipitation in the solution; Be under the 50-70 ℃ of state in the water-bath temperature, be that 1:2 ammoniacal liquor dropwise joins in the reactor with excessive volume ratio, intermittently stir, after treating that precipitation of iron ions fully, centrifugal and clean solid, oven dry is placed in the box-type furnace, at T=800 ℃ of following roasting 90mins, and the corresponding 2-3g hydrofluoric acid solution of preferred every 5g neodymium iron boron greasy filth.
Or after the molten filtration of neodymium iron boron greasy filth acid, add excessive mass concentration 30% hydrogen peroxide oxidation and do not stop to stir, with pH value to 5～6 of the solution after the oxidation with the ammoniacal liquor regulator solution; In 35-50 ℃ hot solution, constantly stir the ammonium bicarbonate soln that adds higher concentration 1mol/L down earlier.Be placed on then in the 50-70 ℃ of water-bath, intermittently stir, form foundry loam shape precipitation in the solution.Be under the 50-70 ℃ of state in the water-bath temperature, be that 1:2 ammoniacal liquor dropwise joins in the reactor with excessive volume ratio, intermittently stir, treat that precipitation of iron ions is complete, with solution centrifugal and clean solid, oven dry is placed in the box-type furnace, at T=800 ℃ of following roasting 90mins, and preferred every 5g neodymium iron boron greasy filth correspondence 138～210ml ammonium bicarbonate soln.
Used ammonia is the ammoniacal liquor that contains ammonia 25%～28% during preparation ammoniacal liquor.
In above-mentioned two kinds of methods, when the acid of neodymium iron boron greasy filth is molten, preferred solid-to-liquid ratio 1g:10-15ml.Iron neodymium mass content is respectively in the final iron neodymium product that the present invention obtains by colloid adsorption method: 69.46%～70.20%, 19.31%～20.35%.
(1) the present invention can effectively reduce in the neodymium-iron alloy co-precipitation, ferric hydroxide colloid is to the absorption of foreign ion, wherein the foreign matter content of bicarbonate of ammonia-ammoniacal liquor method is not higher than 4%, and the foreign matter content of hydrofluoric acid-ammoniacal liquor method 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 ripe technology, and be more stable to the precipitation of rare earth, is of value to the precipitation at co-precipitation neodymium-iron alloy middle-weight rare earths.
(3) the present invention has avoided pursuing the loaded down with trivial details wet process of single high-purity rare-earth in recovery, for subsequent preparation neodymium iron boron regeneration magnetic provides favourable condition, is the committed step that forms the circulation industry.Realization industry endless chain is for " mine, city " lays a good foundation.
Description of drawings
Fig. 1 is the XRD figure spectrum of material after the calcining that obtains of precipitation agent for bicarbonate of ammonia-ammoniacal liquor;
Fig. 2 is the XRD figure spectrum of material after the calcining that obtains of precipitation agent for hydrofluoric acid-ammoniacal liquor.
Embodiment
Below in conjunction with example the present invention is further specified, but the present invention is not limited to following examples.
Embodiment 1:
(1) get 5g neodymium iron boron greasy filth, add 4mol/L hydrochloric acid 60ml in the waste material, fully the dissolving back is added 30% hydrogen peroxide oxidation 10mins in the filtrate and is not stopped to stir, with the pH value to 5 of the solution after the oxidation with the ammoniacal liquor regulator solution.In hot solution, adding mass ratio at leisure earlier under constantly stirring is 40% hydrofluoric acid solution 3g.Place then in the 50-70 ℃ of water-bath, intermittently stir, form foundry loam shape precipitation in the solution.Under heated condition, excess volume slowly, is dropwise joined in the reactor than for 1:2 ammoniacal liquor, intermittently stir.Treat that precipitation of iron ions is complete, with solution centrifugal and cleaning.Clear liquid and washing lotion are discarded.To precipitate centrifugal oven dry and be placed in the box-type furnace, at T=800 ℃ of following roasting 90mins.
Or get 5g neodymium iron boron greasy filth, and in waste material, add 4mol/L hydrochloric acid 60ml, fully the dissolving back is added 30% hydrogen peroxide oxidation 10mins in the filtrate and is not stopped to stir, with the pH value to 5 of the solution after the oxidation with the ammoniacal liquor regulator solution.In hot solution, under constantly stirring, add earlier the ammonium bicarbonate soln 210ml of 1mol/L at leisure.Place in water-bath then, intermittently stir, form foundry loam shape precipitation in the solution.Under heated condition, excessive 1:2 ammoniacal liquor slowly, is dropwise joined in the reactor, intermittently stir.Treat that precipitation of iron ions is complete, with solution centrifugal and cleaning.Clear liquid and washing lotion are discarded.To precipitate centrifugal oven dry and be placed in the box-type furnace, at T=800 ℃ of following roasting 90mins.
Experimental result is as follows:
Table 1-1 hydrofluoric acid-ammoniacal liquor is that precipitation agent and bicarbonate of ammonia-ammoniacal liquor are the XRF outcome quality % of the material that obtains after the precipitation agent calcining
By Fig. 1 and Fig. 2 as can be seen: no matter be to be precipitation agent or to be precipitation agent with bicarbonate of ammonia-ammoniacal liquor that with hydrofluoric acid-ammoniacal liquor the halfwidth of XRD spectral line is all very narrow, the intensity at peak is also than higher; But the wherein not existence mutually of rare earth oxide.Be that material after the precipitation agent roasting is mainly Fe2O3, NdF3, NdOF with hydrofluoric acid-ammoniacal liquor.Bicarbonate of ammonia-ammoniacal liquor is that material is mainly Fe2O3, NdClO after the calcining that obtains of precipitation agent.
The XRF result of table 1-1 shows, the iron that obtains as precipitation agent with hydrofluoric acid-ammoniacal liquor and the element mass percent of neodymium are respectively 69.46% and 20.35%; The ratio of the iron that obtains as precipitation agent with bicarbonate of ammonia-ammoniacal liquor and the element of neodymium is respectively 70.20% and 19.31%.All compare close to original material ratio.The neodymium element recovering effect of hydrofluoric acid-ammoniacal liquor slightly is better than the recovering effect of bicarbonate of ammonia-ammoniacal liquor.The praseodymium that hydrofluoric acid-ammoniacal liquor method reclaims and the content of cobalt are also slightly high, and other foreign matter contents are less.By test result as can be seen, the method for colloid absorption can precipitate preferably and reclaim rare earth element and iron.
Claims (5)
1. a neodymium iron boron greasy filth reclaims the method for neodymium iron, it is characterized in that, may further comprise the steps: be with neodymium iron boron greasy filth with hydrochloric acid acid molten and filter insolubles after, after adding hydrogen peroxide oxidation, the control pH value is 5～6, temperature of reaction, adds hydrofluoric acid and ammoniacal liquor, utilizes rare earth carbonate physical properties and ferric hydroxide colloid to adsorb by forming, co-precipitation goes out neodymium iron precipitation mixture, the product after filtering is respectively obtained the compound of neodymium iron at 800 ℃ of roasting temperatures.
2. according to the method for claim 1, it is characterized in that, after the molten filtration of neodymium iron boron greasy filth acid, add excessive mass concentration 30% hydrogen peroxide oxidation and do not stop to stir, with pH value to 5～6 of the solution after the oxidation with the ammoniacal liquor regulator solution, in 35-50 ℃ hot solution, adding mass concentration earlier under constantly stirring is 40% hydrofluoric acid solution, be placed on then in the 50-70 ℃ of water-bath, intermittently stir, form foundry loam shape precipitation in the solution; Control bath temperature be under the 50-70 ℃ of state, be that 1:2 ammoniacal liquor dropwise joins in the reactor with excessive volume ratio, intermittently stir, after treating that precipitation of iron ions fully, centrifugal and clean solid, oven dry is placed in the box-type furnace, at T=800 ℃ of following roasting 90mins, and the corresponding 2-3g hydrofluoric acid solution of preferred every 5g neodymium iron boron greasy filth.
3. a neodymium iron boron greasy filth reclaims the method for neodymium iron, it is characterized in that, may further comprise the steps: be with neodymium iron boron greasy filth with hydrochloric acid acid molten and filter insolubles after, after adding hydrogen peroxide oxidation, the control pH value is 5～6, temperature of reaction, adds bicarbonate of ammonia and ammoniacal liquor, utilizes the physical properties of rare earth carbonate and ferric hydroxide colloid to adsorb by forming, co-precipitation goes out neodymium iron precipitation mixture, the product after filtering is respectively obtained the compound of neodymium iron at 800 ℃ of roasting temperatures.
4. according to the method for claim 3, it is characterized in that, after the molten filtration of neodymium iron boron greasy filth acid, add excessive mass concentration 30% hydrogen peroxide oxidation and do not stop to stir, with pH value to 5～6 of the solution after the oxidation with the ammoniacal liquor regulator solution; In 35-50 ℃ hot solution, constantly stir the ammonium bicarbonate soln that adds 1mol/L down earlier; Place then in the 50-70 ℃ of water-bath, intermittently stir, forming foundry loam shape precipitation in the solution, is under the 50-70 ℃ of state at bath temperature, is that 1:2 ammoniacal liquor dropwise joins in the reactor with excessive volume ratio, intermittently stir, treat that precipitation of iron ions is complete, with solution centrifugal and clean solid, oven dry is placed in the box-type furnace, at T=800 ℃ of following roasting 90mins, preferred every 5g neodymium iron boron greasy filth correspondence 138～210ml ammonium bicarbonate soln.
5. the neodymium iron product that utilizes the described arbitrary method of claim 1-4 to obtain, it is characterized in that: the content of iron neodymium is respectively in the product: 69.46%～70.20%, 19.31%～20.35%, all the other are the content of other elements.
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| CN103667718A (en) * | 2013-12-17 | 2014-03-26 | 北京工业大学 | Method for recovering Nd (neodymium), Pr (praseodymium), Dy (dysprosium), Co (cobalt) and Fe (iron) simultaneously from NdFeB (neodymium iron boron) oil sludge under CO3-NH3 system |
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