CN103911516A - Process for extracting neodymium from waste electronic ceramic powder - Google Patents
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Abstract
The invention relates to a process for extracting neodymium from waste electronic ceramic powder. The process comprises the steps of carrying out raw material pretreatment on waste electronic ceramic elements as raw materials through grinding, soda boiling and water washing processes, and then carrying out deep treatment through twice acid dissolving process, wherein in the first acid dissolving process, a water washing material, oxydol, polyethylene glycol and hydrochloric acid are added to an acid dissolving pot to react so as to generate rare earth feed liquid, and a flocculant is added to the rare earth feed liquid to carry out flocculation reaction to separate most of impurities from the rare earth ion so as to facilitate purification and production of high-purity neodymium oxalate, and hydrochloric acid is utilized for second acid dissolving; carrying out acid dissolving impurity removal on the rare earth feed liquid obtained through separation after twice acid dissolving to further guarantee the purity of the material in the subsequent working procedure, carrying out impurity removal, water washing, carbonate precipitation, circulating acid dissolving and oxalic acid precipitation, and then baking to obtain a neodymium oxide finished product. By adopting the process, wastes can be effectively utilized to produce high-purity neodymium oxide, industrial wastes are reduced and the waste of rare earth resources is avoided; the method has realistic economic value and social value.
Description
Technical field
The present invention relates to the treatment process field of waste material, be specially a kind of technique of extracting neodymium from waste electronic ceramics powder.
Background technology
Neodymium element relies on its unique status in rare earth field, becomes for many years the focus that market is paid close attention to, and is widely used in the industries such as electronics, machinery, aviation, military affairs, communication, medical treatment.Neodymium metal can not only be used for preparing Nd-Fe-Bo permanent magnet material in industrial aspect, can also also there is its special role in non-ferrous metal metallurgy industry, as added 1.5 ~ 2.5% neodymiums in magnesium or aluminium alloy, can put forward heavy alloyed high-temperature behavior, resistance to air loss and erosion resistance, in addition, in the production process of the painted and rubber item of glass and stupalith, can also use to improve as process additive the quality of product; Meanwhile, also can be used as disinfectant for external use at medical field uses.And along with scientific and technical development, the expanding and extending of rare earth sciemtifec and technical sphere, neodymium element will have the more wide space that utilizes.
But neodymium is rare and expensive grand strategy resource as rare earths mineral element, and become more and more precious along with the exploitation of relevant Mineral resources, rationally reclaiming containing the neodymium in neodymium waste is very valuable work.And containing in the various wastes of neodymium, discarded electrode component has accounted for sizable ratio, these discarded electrode components are mainly the waste and old product of eliminating in defect ware and use procedure on production line, and neodymium content is wherein higher.This class waste is thrown away a large amount of wastes that can cause resource on the one hand, has also polluted on the other hand environment.For these reasons; develop one preferably recovery process to this type of waste carry out neodymium reclaim can not only save and protect national resource, reduce costs 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 national Sustainable development.
Summary of the invention
Technical problem solved by the invention is to provide a kind of technique of extracting neodymium from waste electronic ceramics powder, to solve the shortcoming in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
From waste electronic ceramics powder, extract a technique for neodymium, comprise following operation steps:
1. abrasive dust: the waste electronic ceramic material of recovery carried out to fragmentation and grind through ball mill, reaching 100 ~ 200 object standards with the electronic ceramics powder powder order number grinding out and be as the criterion.
2. soda boiling: ceramics powder powder and sheet alkali after grinding are together added to soda boiling pot, carry out through soda boiling pot that high temperature alkali cooking makes the liquid phase of material in soda boiling pot fully and alkali reaction generation oxyhydroxide.
3. washing: well-done alkali material is proceeded to washing and wash in agitation vat, make after soda boiling the soluble impurity ion in material fully clean, must wash material through sheet frame squeezing machine solid-liquid separation after having washed.
4. once acid-soluble: will to wash material, hydrogen peroxide and polyoxyethylene glycol add in acid-soluble pot, hydrogen peroxide is 1:50 ~ 1:100 with the weight ratio of washing material, polyoxyethylene glycol is 1:10 ~ 1:50 with the weight ratio of washing material, and add technical hydrochloric acid that the acid number of acid-soluble pot is controlled to 0.5 ~ 1.5N, open acid-soluble pot temperature controlled switch acid-soluble temperature is controlled to 60 ~ 90 ℃, under lasting agitation condition, reaction continues 3 ~ 4 hours, reacted material is obtained once after sheet frame squeezing machine solid-liquid separation to acid-soluble slag and a neodymium feed liquid, and by a neodymium feed liquid through pump suction feed clarification pond.
Two times acid-soluble: will be once acid-solublely proceed to acid-soluble pot, in acid-soluble pot, utilizing technical hydrochloric acid to adjust acid number is 2 ~ 4N, opening acid-soluble pot lasting stirring reaction at the temperature of 60 ~ 90 ℃ completes acid-soluble in 7 ~ 8 hours, reaction finishes the pH value of acid-soluble pot to be pulled back to 3 ~ 4 with neodymium carbonate afterwards, and in acid-soluble pot in polyoxyethylene glycol: once the ratio of the weight ratio 1:10 ~ 1:50 of acid-soluble slag adds polyoxyethylene glycol, then by material after sheet frame squeezing machine solid-liquid separation quadratic acid molten slag and secondary neodymium feed liquid, by secondary neodymium feed liquid through pump suction feed clarification pond.
6. feed clarification removal of impurities: neodymium feed liquid and secondary neodymium feed liquid are joined to acid-soluble pot, and add polyoxyethylene glycol, acid-soluble pot temperature is controlled to 60 ~ 90 ℃, add flocculation agent flocculation to remove suspension small particle, by the feed liquid after flocculation removal of impurities after sheet frame squeezing machine solid-liquid separation three neodymium feed liquids and slag head.
7. washing slag head: the slag head in quadratic acid molten slag and step 6 is collected, add washing agitation vat, carry out agitator treating with the hot water of 80 ~ 100 ℃, after agitator treating, product pump is entered in sheet frame squeezing machine, reusable heat water squeezes washing in squeezing machine, multi-pass operations reaches 5 ~ 7 until discharge washing water PH, stop washing and by washing water through pump machine suction carbon deep gouge.
8. wash water carbon is heavy, neodymium carbonate is acid-soluble: add sodium bicarbonate to carry out precipitin reaction the washing water in step 7, when arriving 7 ~ 8, reaction rear solution PH reacts, after sheet frame squeezing machine solid-liquid separation, obtain neodymium carbonate, neodymium carbonate is substituted to washing material and carry out according to the process of step 4 acid-soluble, and according to the removal step of step 6 to make the heavy neodymium feed liquid of carbon.
9. oxalic acid precipitation and neodymium oxalate washing, roasting: after three neodymium feed liquids and the heavy neodymium feed liquid of carbon are filtered, squeeze in precipitin reaction still, add oxalic acid solution to prepare neodymium oxalate, and the precipitation material in precipitin reaction still is put into the filtering basin hot water of 80 ~ 100 ℃ and wash, wash while add water, in the time that arriving 5 ~ 6, the pH value of washing water stops, put into whizzer, then in whizzer, wash to wash water PH reach 6 ~ 7 rear dryings, dress wraps to obtain neodymium oxalate; Neodymium oxalate obtains Neodymium trioxide product after roasting kiln roasting.
In an acid dissolution of the present invention, acid-soluble pot adds washing material, hydrogen peroxide and polyoxyethylene glycol reaction to generate neodymium feed liquid, this neodymium feed liquid separates most of impurity by flocculation reaction process adding after flocculation agent with rare earth ion, produce high-purity oxalic acid neodymium to facilitate to purify, this operation material decomposes rare earth yield and arrives more than 70%; Then utilize hydrochloric acid to carry out secondary acid-soluble, the rare earth feed liquid that the separation after acid-soluble by twice obtains carries out acid-soluble removal of impurities, can further guarantee the purity of operation material below.
In the present invention, in the alkali cooking process of described step 2, the mass ratio adding of described electronic ceramics powder material and sheet alkali is 10:3 ~ 10:10, soda boiling temperature requirement is 100 ~ 150 ℃, alkali cooking process maintains 8 ~ 20 hours, reach 98% above required time with the rate of decomposition of neodymium element in electronic ceramics powder and be as the criterion, now, electronic ceramics powder fully reacts with alkali and generates oxyhydroxide in soda boiling pot.
In the present invention, in the water washing process of described step 3, using the hot water of 80 ~ 100 ℃ as wash water, wash 2 ~ 5 times, reach at 8 ~ 9 o'clock and stop washing to discharging wash water PH.Water washing process to soda boiling after the soluble impurity ion such as impurity element Ca, Ba, Na, K in material play removal effect.
In the present invention, in described step 4, the rotating speed of the whipping device of the lasting stirring in acid-soluble pot is that per minute 35 ~ 40 turns.
In the present invention, the neodymium content that the neodymium feed liquid of described step 4 and step 5 gained can be required according to precipitation, returns to it again in described step 4 and step 5 and does end water, carries out repeatedly cyclical operation to adjust in neodymium feed liquid containing neodymium amount.
In the present invention, the polyoxyethylene glycol in described step 5 plays flocculation removal effect to impurity element Ti, Fe in feed liquid, Mg, Al, Si etc.
In the present invention, when in described step 6, the add-on of polyoxyethylene glycol and settling time are with neodymium feed clarification, supernatant liquor is limpid is as the criterion.
In the present invention, in described step 8, after sheet frame squeezing machine solid-liquid separation, obtain neodymium carbonate can be directly in step 5 for the readjustment of acid-soluble pot pH value, to reduce outsourcing raw materials requirement amount.
In the present invention, in the process of described step 9, in oxalic acid solution mesoxalic acid consumption and feed liquid to be precipitated, the weight ratio of neodymium amount of metal is 2:1 ~ 3:1, use excessive oxalic acid as precipitation agent further to remove impurity element, guarantee yield and the purity of neodymium.
Beneficial effect: utilization of the present invention is carried out neodymium extraction containing the electronic ceramics element waste material of neodymium, can Matter Transfer between simple, the multiple step of technological operation, processing cost is low, particle to raw material and neodymium content requirement are low, rare earth yield reaches more than 95%, just can obtain content through primary treatment and reach more than 98% high-purity neodymium oxide, effectively avoid the waste of rare earth resources, reduce the discharge of relative refuse waste material.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
In an embodiment, the waste electronic ceramic material of recovery is carried out to fragmentation and grind through ball mill, electronic ceramics powder powder order number is ground to 100 orders.
The 1000kg tap water that adds water is to soda boiling pot, drop into sheet alkali 1000kg, open stirring, after sheet alkali dissolution, drop into abrasive dust material 1000kg, open the thermal oil switch of soda boiling pot, soda boiling pot starts to heat up, and when soda boiling material temperature degree reaches 100 ℃ and move 8 hours, sampling and measuring rate of decomposition reaches 98% and completes for soda boiling.Add hot water dilution, blowing is to washing bath, add again in the hot water of 80 ℃ and stir and wash, after washing, squeeze to obtain washing material, the squeezing of washing material, and put into washing bath and again wash, so operation 2 times, now extensively test paper survey rinsing solution PH is 9, and washing completes, and after crusher squeezing, must wash material.
In acid-soluble pot, add tap water 1200kg, get 1000kg washing material and drop into acid-soluble pot, adding starts to heat up after hydrogen peroxide 12kg, polyoxyethylene glycol 20kg adds hydrochloric acid acid adjustment value, in the time that acid-soluble pot temperature is stabilized in 90 ℃ and material acid number and is stabilized in 0.5N, under the rotating speed turning at per minute 35, utilize whipping device to continue stirring reaction 3 hours, reacted material is obtained once after sheet frame squeezing machine solid-liquid separation to acid-soluble slag and a neodymium feed liquid, and by a neodymium feed liquid through pump suction feed clarification pond.
To once acid-solublely proceed to acid-soluble pot, in acid-soluble pot, utilizing technical hydrochloric acid to adjust acid number is 2N, opening acid-soluble pot lasting stirring reaction at the temperature of 90 ℃ completes acid-soluble in 8 hours, reaction finishes the pH value of acid-soluble pot to be pulled back to 3 with neodymium carbonate afterwards, and in acid-soluble pot in polyoxyethylene glycol: once the ratio of the weight ratio 1:10 of acid-soluble slag adds polyoxyethylene glycol, then by material after sheet frame squeezing machine solid-liquid separation quadratic acid molten slag and secondary neodymium feed liquid, by secondary neodymium feed liquid through pump suction feed clarification pond.
Neodymium feed liquid and secondary neodymium feed liquid are joined to acid-soluble pot, and add polyoxyethylene glycol, supernatant liquor is limpid during with neodymium feed clarification is as the criterion for the add-on of polyoxyethylene glycol and settling time, acid-soluble pot temperature is controlled to 90 ℃, add flocculation agent flocculation to remove suspension small particle, by the feed liquid after flocculation removal of impurities after sheet frame squeezing machine solid-liquid separation three neodymium feed liquids and slag head.
Quadratic acid molten slag and slag head are collected, add washing agitation vat, carry out agitator treating with the hot water of 100 ℃, after agitator treating, product pump is entered in sheet frame squeezing machine, reusable heat water squeezes washing in squeezing machine, reach 5 until discharge wash water PH, stop washing and by washing water through pump machine suction carbon deep gouge.Add sodium bicarbonate to carry out precipitin reaction the washing water in above-mentioned steps, in the time that arriving 7, reaction rear solution PH reacts, after sheet frame squeezing machine solid-liquid separation, obtain neodymium carbonate, neodymium carbonate is substituted to washing material and carry out according to once acid-soluble process acid-soluble, and according to the removal step of flocculation removal of impurities process to make the heavy neodymium feed liquid of carbon.
After being filtered, three neodymium feed liquids and the heavy neodymium feed liquid of carbon squeeze in precipitin reaction still, add oxalic acid solution to prepare neodymium oxalate, after neodymium oxalate has filtered, adding 80 ℃ of hot water washs, wash while add water, in the time that being 5, washs washing water PH, neodymium oxalate dress bag proceeds to next process and carries out centrifugal washing, in the time that whizzer water outlet PH is 7, centrifugal water washes into, then neodymium oxalate is dried to dress bag and carry out roast through roasting kiln, roasting kiln temperature is 800 ℃, turns over kiln and obtain rare-earth oxidation neodymium product after 12 hours.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (8)
1. a technique of extracting neodymium from waste electronic ceramics powder, is characterized in that, comprises following operation steps:
1., abrasive dust: the waste electronic ceramic material of recovery carried out to fragmentation and grind through ball mill, reaching 100 ~ 200 object standards with the electronic ceramics powder powder order number grinding out and be as the criterion;
2., soda boiling: ceramics powder powder and sheet alkali after grinding are together added to soda boiling pot, carry out through soda boiling pot that high temperature alkali cooking makes the liquid phase of material in soda boiling pot fully and alkali reaction generation oxyhydroxide;
3., washing: well-done alkali material is proceeded to washing and wash in agitation vat, make after soda boiling the soluble impurity ion in material fully clean, must wash material through sheet frame squeezing machine solid-liquid separation after having washed;
4., once acid-soluble: will to wash material, hydrogen peroxide and polyoxyethylene glycol add in acid-soluble pot, hydrogen peroxide is 1:50 ~ 1:100 with the weight ratio of washing material, polyoxyethylene glycol is 1:10 ~ 1:50 with the weight ratio of washing material, and add technical hydrochloric acid that the acid number of acid-soluble pot is controlled to 0.5 ~ 1.5N, open acid-soluble pot temperature controlled switch acid-soluble temperature is controlled to 60 ~ 90 ℃, under lasting agitation condition, reaction continues 3 ~ 4 hours, reacted material is obtained once after sheet frame squeezing machine solid-liquid separation to acid-soluble slag and a neodymium feed liquid, and by a neodymium feed liquid through pump suction feed clarification pond,
5., secondary is acid-soluble: will once acid-solublely proceed to acid-soluble pot, in acid-soluble pot, utilizing technical hydrochloric acid to adjust acid number is 2 ~ 4N, opening acid-soluble pot lasting stirring reaction at the temperature of 60 ~ 90 ℃ completes acid-soluble in 7 ~ 8 hours, reaction finishes the pH value of acid-soluble pot to be pulled back to 3 ~ 4 with neodymium carbonate afterwards, and in acid-soluble pot in polyoxyethylene glycol: once the ratio of the weight ratio 1:10 ~ 1:50 of acid-soluble slag adds polyoxyethylene glycol, then by material after sheet frame squeezing machine solid-liquid separation quadratic acid molten slag and secondary neodymium feed liquid, by secondary neodymium feed liquid through pump suction feed clarification pond;
6., feed clarification removal of impurities: neodymium feed liquid and secondary neodymium feed liquid are joined to acid-soluble pot, and add polyoxyethylene glycol, acid-soluble pot temperature is controlled to 60 ~ 90 ℃, add flocculation agent flocculation to remove suspension small particle, by the feed liquid after flocculation removal of impurities after sheet frame squeezing machine solid-liquid separation three neodymium feed liquids and slag head;
7., washing slag head: the slag head by quadratic acid molten slag and step in is 6. collected, add washing agitation vat, carry out agitator treating with the hot water of 80 ~ 100 ℃, after agitator treating, product pump is entered in sheet frame squeezing machine, reusable heat water squeezes washing in squeezing machine, multi-pass operations reaches 5 ~ 7 until discharge washing water PH, stop washing and by washing water through pump machine suction carbon deep gouge;
8., wash water carbon is heavy, neodymium carbonate is acid-soluble: the washing water by step in 7. add sodium bicarbonate to carry out precipitin reaction, when arriving 7 ~ 8, reaction rear solution PH reacts, after sheet frame squeezing machine solid-liquid separation, obtain neodymium carbonate, neodymium carbonate is substituted to washing material and carry out according to step process 4. acid-soluble, and according to step removal step 6. to make the heavy neodymium feed liquid of carbon;
9., oxalic acid precipitation and neodymium oxalate washing, roasting: after three neodymium feed liquids and the heavy neodymium feed liquid of carbon are filtered, squeeze in precipitin reaction still, add oxalic acid solution to prepare neodymium oxalate, and the precipitation material in precipitin reaction still is put into the filtering basin hot water of 80 ~ 100 ℃ and wash, wash while add water, in the time that arriving 5 ~ 6, the pH value of washing water stops, put into whizzer, then in whizzer, wash to wash water PH reach 6 ~ 7 rear dryings, dress wraps to obtain neodymium oxalate; Neodymium oxalate obtains Neodymium trioxide product after roasting kiln roasting.
2. a kind of technique of extracting neodymium from waste electronic ceramics powder according to claim 1, it is characterized in that, in described step alkali cooking process 2., the mass ratio adding of described electronic ceramics powder material and sheet alkali is 10:3 ~ 10:10, soda boiling temperature requirement is 100 ~ 150 ℃, and alkali cooking process maintains 8 ~ 20 hours, reaches 98% above required time be as the criterion with the rate of decomposition of neodymium element in electronic ceramics powder, now, electronic ceramics powder fully reacts with alkali and generates oxyhydroxide in soda boiling pot.
3. a kind of technique of extracting neodymium from waste electronic ceramics powder according to claim 1, is characterized in that, in described step water washing process 3., using the hot water of 80 ~ 100 ℃ as wash water, washes 2 ~ 5 times, reaches at 8 ~ 9 o'clock and stop washing to discharging wash water PH.
4. a kind of technique of extracting neodymium from waste electronic ceramics powder according to claim 1, is characterized in that, the rotating speed of described step whipping device of the lasting stirring in acid-soluble pot in is 4. that per minute 35 ~ 40 turns.
5. a kind of technique of extracting neodymium from waste electronic ceramics powder according to claim 1, is characterized in that, described step 4. and step 5. in the neodymium feed liquid of gained can do end water, carry out repeatedly cyclical operation to adjust in neodymium feed liquid containing neodymium amount.
6. a kind of technique of extracting neodymium from waste electronic ceramics powder according to claim 1, is characterized in that, described step 6. in the add-on of polyoxyethylene glycol and settling time supernatant liquor is limpid during with neodymium feed clarification is as the criterion.
7. a kind of technique of extracting neodymium from waste electronic ceramics powder according to claim 1, is characterized in that, described step after sheet frame squeezing machine solid-liquid separation, obtain in 8. neodymium carbonate can be directly step 5. in for the readjustment of acid-soluble pot pH value.
8. a kind of technique of extracting neodymium from waste electronic ceramics powder according to claim 1, it is characterized in that, in described step process 9., in oxalic acid solution mesoxalic acid consumption and feed liquid to be precipitated, the weight ratio of neodymium amount of metal is 2:1 ~ 3:1, use excessive oxalic acid as precipitation agent further to remove impurity element, guarantee yield and the purity of neodymium.
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