CN106191446A - A kind of recovering rare earth Yt method of preparing resin surface composite deposite from waste phosphor powder - Google Patents
A kind of recovering rare earth Yt method of preparing resin surface composite deposite from waste phosphor powder Download PDFInfo
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- CN106191446A CN106191446A CN201610525689.9A CN201610525689A CN106191446A CN 106191446 A CN106191446 A CN 106191446A CN 201610525689 A CN201610525689 A CN 201610525689A CN 106191446 A CN106191446 A CN 106191446A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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Abstract
A kind of recovering rare earth Yt method of preparing resin surface composite deposite from waste phosphor powder, belongs to solid waste resource recovery and utilizes field.First by passing through certain mesh number sieved through sieve after discarded CRT fluorescent screen Mechanical Crushing, remove the impurity such as glass, obtain the powder body based on fluorescent material；Then the fluorescent material oxidation acid leaching after screening is processed, fluorescent material rare earth elements is leached；Major part yttrium and small part europium being extracted by multitple extraction method subsequently, then obtain yttrium chloride solution by back extraction, just there is white precipitate to solution in regulation pH value；Yttrium chloride solution is added dropwise in the ammonium bicarbonate soln containing dispersant, prepares presoma；Nano yttrium oxide powder can be prepared after presoma drying, roasting；Finally nano yttrium oxide powder is allocated into and the plating solution containing dispersant is made composite plating solution, electroplate the conductive plastics surface made at resin and carbon system conductor.
Description
Technical field
The invention belongs to solid waste resource recovery and utilize field, be specifically related to a kind of recovering rare earth from waste phosphor powder
Yt the method preparing resin surface composite deposite.
Background technology
China is the country that rare earth resources is the abundantest, and rare earth yield and reserves all occupy first place in the world, and rare-earth mineral kind is neat
Entirely, and production cost is low.But owing to China is ineffective to rare earth mining industry management and control, a large amount of gophers, inexpensively export
And domestic demand quickly increases, China rare earth reserves from 50 years front 74% fall sharply by now 23%, China simultaneously
Also continuing to supply the demand in the world more than 95%.The domestic demand of China rare earth is also sharply increasing in addition, from 2002
It was only for 5 years to 2007 and just increases 3 times more than.The rare earth resources of China is extremely to allow of no optimist, and rare earth resources is possessed
Measure and continuing rapid decrease, for recycling rare earth from garbage, reduce natural resources exploitation, have urgent demand.
The recycling of discarded CRT fluorescent material rare earth elements can solve the realistic problem of a lot of rare-earth trade.First
Being environmental problem, the recovery for fluorescent material rare earth elements can prevent rare earth element to be transferred in nature, in animals and plants
Enrichment, causes poison pathological condition.Recycling to rare earth simultaneously contributes to reducing the exploitation of a rare earth resources, a rare earth
Resource is huge to the destruction on earth's surface and environment, and its needs cut into a mountain and separate smelting, have caused various environment to ask in China
Topic.The recycling of rare earth contributes to solving above environmental problem.
Secondly, the rare earth element in CRT fluorescent material reclaims and has economic interests.The three primary colors fluorescent powder used in a crt
In Hydrargyri Oxydum Rubrum composition be: Y2O3Or Y2O2S:Eu3+.The rare earth element wherein contained is mainly Y and Eu.Averagely every complete CRT
The quality typically containing fluorescent material in panel glass is 1-7g, and its Rare-Earth Content accounts for about the 15% of fluorescent material quality, so often
Platform CRT middle rare earth amount is about 0.15-1g.The discarded rare earth oxide producing more than 4.5t to I haven't seen you for ages in the most only 2013.Right
In the most big city mineral reserve, economic interests are self-evident.
In current research, the technology of waste phosphor powder recovering rare earth is had multiple, is broadly divided into the acid-hatching of young eggs, alkali fusion
Method, extraction and the sedimentation method, but seldom there is the Technology that directly utilize after waste phosphor powder can be reclaimed.Discarded fluorescence
Recycling in powder recycling is also critically important link, how to have certain by easy being transformed into of the rare earth element of recovery
The industrial products of added value are used, cut down the number of intermediate links be current solid wastes recycling utilize important research direction.
Summary of the invention
The invention aims to provide a kind of easy method reclaimed and utilize rare earth element in waste phosphor powder, will
The rare earth element reclaimed is configured to composite plating solution, and electroplates formation composite galvanized coating on resin.It it is a kind of rare earth element
Reclaim and utilize integrated high efficiency, low cost process route.
The technical solution adopted for the present invention to solve the technical problems is: a kind of recovering rare earth element from waste phosphor powder
Yttrium the method preparing resin surface composite deposite, comprise the following steps:
A, utilize sieve method will broken after fluorescent material open with magazins' layout, by 20 mesh, 60 mesh, 100 mesh, 200 mesh nets
After sieve progressively screening, collecting 200 mesh siftage, siftage accounts for and is unscreened more than the 99.9% of front powder body weight；
B, siftage step a obtained join in acid and hydrogen peroxide mixed liquor, react a period of time, then carry out
Filter, containing rare earth element in filtrate；
C, filtrate step b obtained use phosphorus system extractant to extract, and after point three grades of extractions, comprise only in extract
Rare earth element；
D, the extract hydrochloric acid containing rare earth element step c obtained carries out back extraction, is rare earth element in strip liquor
Yttrium, if possibly together with rare-earth europium in extract, then rare-earth europium is in raffinate；
E, strip liquor step d obtained addition ammonia is neutralized to solution has just had a small amount of white precipitate to produce, solution
Main Ingredients and Appearance is Yttrium chloride(Y2Cl6), by yttrium chloride solution evaporation and concentration or after being evaporated and being configured to finite concentration again, is added dropwise to be furnished with
In the ammonium bicarbonate soln of dispersant, generate presoma；
After the filtration of f, the presoma that step e is obtained, drying, calcine, after grinding, obtain nano yttrium oxide powder；
G, nano yttrium oxide powder step f obtained add makes composite plating to the electroplate liquid be furnished with dispersant
Liquid, is electroplated to resin surface.
Further preferred:
Wherein, in said method step b, the kind of acid is hydrochloric acid or sulphuric acid.
Wherein, if using sulphuric acid in said method step b, molar concentration is 1.5～3.5mol/L；If use hydrochloric acid, rub
Your concentration is 2.5～6.5mol/L.
Wherein, the hydrogen peroxide used in said method step b is 0.03～0.1. with the volume ratio of sulphuric acid
Wherein, in said method step b, siftage is 1g:20～40ml with sour and hydrogen peroxide solid-to-liquid ratio.
Wherein, in said method step b, the leaching response time is 30～90min.
Wherein, leaching reaction temperature in said method step b is 35～65 DEG C.
Wherein, in said method step c, extractant is P507, P204, Cyanex272 or PC88A.
Wherein, in said method step c, the volume ratio of filtrate and extractant is 1:2～5.
Wherein, in said method step d, the volume ratio of extract and hydrochloric acid is 1:0.1～0.2.Wherein hydrochloric acid molar concentration
It is 1～4mol/L.
Wherein, the yttrium chloride solution evaporation and concentration that obtains in said method step e or be evaporated and be formulated into molar concentration again and be
The yttrium chloride solution of 0.2～0.4mol/L.
Wherein, in said method step e, the molar concentration of ammonium bicarbonate soln is 1～2mol/L.
Wherein, the dispersant added in ammonium bicarbonate soln in said method step e is PEG-4000, poly-second two
Alcohol-2000 or hexadecyltrimethylammonium chloride.Wherein dispersant addition and Yttrium chloride(Y2Cl6) mass ratio are 0.5～2:10.
Wherein, in said method step e, mixing speed is 200～400r/min.
Wherein, in said method step e, Yttrium chloride(Y2Cl6) rate of titration is 60～100/min.
Wherein, in said method step f, the drying temperature of presoma is 50～90 DEG C.
Wherein, in said method step f, the calcining heat of presoma is 700～900 DEG C, and calcination time is 1～5h.
Wherein, in said method step g, composite plating solution proportioning is: 30～50g/L NiSO4·H2O, 10～20g/
LNiCl2·H2O, 10～20g/LH3BO3, 1～5g/L saccharin, 15～20g/L nano yttrium oxide.
Wherein, in said method step g, dispersant is PEG-4000, Polyethylene glycol-2000 or Triammonium citrate.Its
The concentration that middle dispersant adds is 0.5～2g/L.
Wherein, in said method step g, electroplating current density is 2～3A/dm2, electroplating time 15～30min, plating bath temperature
Spend 40～70 DEG C, mixing speed 200～400r/min.
Wherein, in said method step g, resin is that the carbon system filled-type that resin becomes with carbon series conductive material hybrid process is led
Electricity plastics.
The invention has the beneficial effects as follows: the present invention, by waste phosphor powder first screened process, removes a large amount of impurity.After through
Oxidation acid leaching processes, and can effectively destroy phosphor structure, makes rare earth element leach under optimum process condition, rare earth element yttrium and
The leaching rate of europium can be more than 99.9%, and the response time is shorter, and leaching efficiency is high.Extraction link is by controlling leachate and extraction
Take the ratio of agent, increase the order of reaction, the yttrium of more than 95% can be made to be extracted out, and the most a small amount of europium enters extract,
Making yttrium be reclaimed in a large number by the concentration of stripping process acid with consumption again, europium is then stayed in extract to be entered by other technological processes
Row is collected and is reclaimed.The response rate of whole process yttrium is up to 90.5%.The Yttrium chloride(Y2Cl6) reclaimed back is by chemical precipitation method easily
Produce nano yttrium oxide powder, and addition directly utilizes to the composite plating solution can be used for conductive plastics plating, plating
After form composite galvanized coating on conductive plastics surface, hardness and the anti-wear performance of plastics can be increased substantially, allow discarded fluorescence
Rare earth element in powder creates new value.The nano yttrium oxide that the yttrium simultaneously reclaimed with waste phosphor powder manufactures, it becomes
This most also will the price low 10%～20% of more commercially available yittrium oxide.
Accompanying drawing explanation
Fig. 1 is present invention process schematic flow sheet.
Detailed description of the invention
Below in conjunction with the accompanying drawings and embodiment, the present invention is described in detail, but the present invention is not limited to following example.
As it is shown in figure 1, the present invention a kind of recovering rare earth Yt prepare the side of resin surface composite deposite from waste phosphor powder
Method, including following 7 steps: 1) screening pre-treatment step；2) oxidation acid leaching step；3) extract and separate step；4) back extraction is reclaimed
Step；5) chemical precipitation step；6) high-temperature calcinations step；7) electrodeposited resin step.
Embodiment 1:
A kind of recovering rare earth Yt method of preparing resin surface composite deposite from waste phosphor powder, including as follows
Seven steps:
1) screening pre-treatment step: by tentatively broken waste phosphor powder by 20 mesh, 60 mesh, 100 mesh, 200 mesh mesh screens
Progressively after screening, collecting 200 mesh siftage, siftage accounts for and is unscreened more than the 99.9% of powder body.
2) oxidation acid leaching step: fluorescent material screening processed adds sulphuric acid by solid-to-liquid ratio 1g:30ml and enters with hydrogen peroxide
Row leaches reaction, and the concentration of sulphuric acid is 3mol/L, and hydrogen peroxide is 0.04 with the volume ratio of sulphuric acid, reacts 60min, instead at 50 DEG C
Filter after should, obtain the leachate containing rare earth element.In fluorescent material, the leaching rate of yttrium and europium is above 99.9%.
3) extract and separate step: the filtrate obtained is extracted by the volume ratio of 1:2 with P507, point three grades of extractions.
4) back extraction recycling step: will enter under the extract 1.5mol/L hydrochloric acid 1:0.2 by volume containing rare earth element
Row back extraction, the response rate of rare-earth yttrium is 95%.
5) chemical precipitation step: the strip liquor obtained is added in ammonia and pH value has just had a small amount of white precipitate to produce to solution
Raw, solution Main Ingredients and Appearance is Yttrium chloride(Y2Cl6), by Yttrium chloride(Y2Cl6) evaporation and concentration or be evaporated re-dissolved to 0.2mol/L, by the speed of 80/min
Degree is added dropwise in the ammonium bicarbonate soln that concentration is 1.5mol/L, is furnished with Yttrium chloride(Y2Cl6) mass ratio is in ammonium bicarbonate soln
The PEG-4000 dispersant of 1:10, generates presoma.
6) high-temperature calcinations step: after the presoma filtration obtained, 60 DEG C of drying, calcine 2h at 860 DEG C, after grinding
To nano yttrium oxide powder.
7) electrodeposited resin step: by prepared nano yttrium oxide powder by 15g/L addition to proportioning be: 40g/LNiSO4·
H2O、20g/LNiCl2·H2O、10g/LH3BO3, 2g/L saccharin, dispersant be 1g/L the brush plating liquid of Polyethylene glycol-2000 in,
Make composite plating solution.It is 2A/dm at electroplating current density2, electroplating time 20min, bath temperature 50 DEG C, mixing speed
At graphite-filled type conductive plastics electroplating surface composite galvanized coating under conditions of 250r/min.
Embodiment 2: a kind of recovering rare earth Yt prepare conductive plastics surface composite plating from waste phosphor powder
Method, including following seven steps:
1) screening pre-treatment step: by tentatively broken waste phosphor powder by 20 mesh, 60 mesh, 100 mesh, 200 mesh mesh screens
Progressively after screening, collecting 200 mesh siftage, the content of siftage rare earth elements accounts for and is unscreened more than the 99.9% of powder body.
2) oxidation acid leaching step: fluorescent material screening processed adds hydrochloric acid by solid-to-liquid ratio 1g:35ml and enters with hydrogen peroxide
Row leaches reaction, and the concentration of hydrochloric acid is 6mol/L, and hydrogen peroxide is 0.06 with the volume ratio of hydrochloric acid, reacts 80min, instead at 40 DEG C
Filter after should, obtain the leachate containing rare earth element.In fluorescent material, the leaching rate of yttrium and europium is above 99.9%.
3) extract and separate step: the filtrate obtained extracted by the volume ratio of 1:2.5 with Cyanex272, divides three grades
Extraction.
4) back extraction recycling step: will enter under the extract 1.5mol/L hydrochloric acid 1:0.2 by volume containing rare earth element
Row back extraction, the response rate of rare-earth yttrium is 95%.
5) chemical precipitation step: the strip liquor obtained is added in ammonia and pH value has just had a small amount of white precipitate to produce to solution
Raw, solution Main Ingredients and Appearance is Yttrium chloride(Y2Cl6), by Yttrium chloride(Y2Cl6) evaporation and concentration or be evaporated re-dissolved to 0.2mol/L, by the speed of 90/min
Degree is added dropwise in the ammonium bicarbonate soln that concentration is 1.5mol/L, and ammonium bicarbonate soln is furnished with and with Yttrium chloride(Y2Cl6) mass ratio is
The hexadecyltrimethylammonium chloride dispersant of 1.5:10, generates presoma.
6) high-temperature calcinations step: after the presoma filtration obtained, 80 DEG C of drying, calcine 3h at 800 DEG C, after grinding
To nano yttrium oxide powder.
7) electrodeposited resin step: by prepared nano yttrium oxide powder by 20g/L addition to proportioning be: 40g/LNiSO4·
H2O、15g/LNiCl2·H2O、15/LH3BO3, 3g/L saccharin, dispersant be 1.5g/L the brush plating liquid of Triammonium citrate in, system
Become composite plating solution.It is 2A/dm at electroplating current density2, electroplating time 15min, bath temperature 60 DEG C, mixing speed 350r/
At conductive fiber filled-type frosting brush plating composite galvanized coating under conditions of min.
Through cost accounting, the nano yttrium oxide cost produced from waste phosphor powder has similar finger than market sale
Target nano yttrium oxide low cost 11.8%-17.8%, has certain economic benefit.That makes has leading of composite galvanized coating
Electricity plastics can be applicable to material requirements light weight and wearability are required high mechanical part, and the plating solution using the present invention to obtain enters
Row plating, coating fine uniform, the wearability of resin, heat-resisting quantity and hardness all improve.
Claims (10)
1. recovering rare earth Yt a method of preparing resin surface composite deposite from waste phosphor powder, its feature exists
In, comprise the following steps:
A, utilize sieve method will broken after fluorescent material open with magazins' layout, by 20 mesh, 60 mesh, 100 mesh, 200 mesh mesh screens by
After step screening, collect 200 mesh siftage；
B, siftage step a obtained join in acid and hydrogen peroxide mixed liquor, react a period of time, then filter,
Containing rare earth element in filtrate；
C, filtrate step b obtained use phosphorus system extractant to extract, and after point three grades of extractions, comprise only rare earth in extract
Element；
D, the extract hydrochloric acid containing rare earth element step c obtained carries out back extraction, is rare earth element yttrium in strip liquor, as
Really possibly together with rare-earth europium in extract, then rare-earth europium is in raffinate；
E, strip liquor step d obtained addition ammonia is neutralized to solution has just had a small amount of white precipitate to produce, and solution is main
Composition is Yttrium chloride(Y2Cl6), by yttrium chloride solution evaporation and concentration or after being evaporated and being configured to finite concentration again, is added dropwise to be furnished with dispersion
In the ammonium bicarbonate soln of agent, generate presoma；
After the filtration of f, the presoma that step e is obtained, drying, calcine, after grinding, obtain nano yttrium oxide powder；
G, nano yttrium oxide powder step f obtained add makes composite plating solution to the electroplate liquid be furnished with dispersant, electricity
It is plating to resin surface.
2. according to the recovering rare earth Yt prepare resin surface Composite Coatings from waste phosphor powder of the one described in claim 1
The method of layer, it is characterised in that in step b, the kind of acid is hydrochloric acid or sulphuric acid；If use sulphuric acid, molar concentration be 1.5～
3.5mol/L；If use hydrochloric acid, molar concentration is 2.5～6.5mol/L；Hydrogen peroxide is 0.03～0.1 with the volume ratio of sulphuric acid:
1；In step b, siftage is 1g:20～40ml with the solid-to-liquid ratio of acid and hydrogen peroxide cumulative volume.
3. according to the recovering rare earth Yt prepare resin surface Composite Coatings from waste phosphor powder of the one described in claim 1
The method of layer, it is characterised in that in step b, the leaching response time is 30～90min；Leaching reaction temperature is 35～65 DEG C.
4. according to the recovering rare earth Yt prepare resin surface Composite Coatings from waste phosphor powder of the one described in claim 1
The method of layer, it is characterised in that in step c, phosphorus system extractant is P507, P204, Cyanex272 or PC88A.
5. according to the recovering rare earth Yt prepare resin surface Composite Coatings from waste phosphor powder of the one described in claim 1
The method of layer, it is characterised in that in step c, filtrate is 1:2～5 with the volume ratio of phosphorus system extractant.
6. according to the recovering rare earth Yt prepare resin surface Composite Coatings from waste phosphor powder of the one described in claim 1
The method of layer, it is characterised in that in step d, extract is 1:0.1～0.2 with the volume ratio of hydrochloric acid；Wherein hydrochloric acid molar concentration
It is 1～4mol/L.
7. according to the recovering rare earth Yt prepare resin surface Composite Coatings from waste phosphor powder of the one described in claim 1
The method of layer, it is characterised in that the yttrium chloride solution evaporation and concentration that obtains in step e or be evaporated and be formulated into molar concentration again and be
The yttrium chloride solution of 0.2～0.4mol/L；The molar concentration of ammonium bicarbonate soln is 1～2mol/L.
8. according to the recovering rare earth Yt prepare resin surface Composite Coatings from waste phosphor powder of the one described in claim 1
The method of layer, it is characterised in that the dispersant added in ammonium bicarbonate soln in step e be PEG-4000, Polyethylene Glycol-
2000 or hexadecyltrimethylammonium chloride.Wherein dispersant addition and Yttrium chloride(Y2Cl6) mass ratio are 0.5～2:10.
9. according to the recovering rare earth Yt prepare resin surface Composite Coatings from waste phosphor powder of the one described in claim 1
The method of layer, it is characterised in that in step f, the calcining heat of presoma is 700～900 DEG C, and calcination time is 1～5h.
10. according to the one described in claim 1 from waste phosphor powder recovering rare earth Yt and prepare resin surface be combined
The method of coating, it is characterised in that in step g, the composition of electroplate liquid is 30～50g/LNiSO4·H2O, 10～20g/
LNiCl2·H2O, 10～20g/LH3BO3, 1～5g/L saccharin, 15～20g/L nano yttrium oxide, dispersant be Polyethylene Glycol-
400, Polyethylene glycol-2000 or Triammonium citrate, the concentration that wherein dispersant adds is 0.5～2g/L, and electroplating current density is 2
～3A/dm2, electroplating time 15～30min, bath temperature 40～70 DEG C, mixing speed 200～400r/min；Resin is resin
The carbon-filled conductive plastics become with carbon series conductive material hybrid process.
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| CN108060304A (en) * | 2017-11-28 | 2018-05-22 | 曾文生 | A kind of pollution-free recycling and processing device of waste hardware material |
| CN108060304B (en) * | 2017-11-28 | 2019-04-26 | 广西云邦货架有限公司 | A kind of pollution-free recycling and processing device of waste hardware material |
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