CN108359408A - A method of recycling polishing powder from polishing powder from rare earth waste residue - Google Patents
A method of recycling polishing powder from polishing powder from rare earth waste residue Download PDFInfo
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- CN108359408A CN108359408A CN201710057377.4A CN201710057377A CN108359408A CN 108359408 A CN108359408 A CN 108359408A CN 201710057377 A CN201710057377 A CN 201710057377A CN 108359408 A CN108359408 A CN 108359408A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- C09K3/14—Anti-slip materials; Abrasives
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Abstract
A method of recycling polishing powder from polishing powder from rare earth waste residue：Using polishing powder from rare earth waste residue caused by glass polishing industry as raw material, it is activated using acid solution first, then it is neutralized and the technological means such as cyclone classification by medicaments flotation and lye, realize efficiently separating between the invalid component contained in polishing powder from rare earth waste residue and the thinner overground rare earth component of particle and the rare earth component for keeping original polishing characteristic, thus to obtain high-content polishing powder from rare earth, and realizes the highly efficient regeneration of special floating agent by the way of lye neutralization and recycle.Using the method for the present invention, it can effectively realize efficiently separating for impurity and overground rare earth component in polishing powder from rare earth waste residue, not only it is remarkably improved the content of rare earth of recycled polishing powder, effectively maintain the original polishing characteristic of polishing powder from rare earth simultaneously, and it is not necessarily to high-temperature calcination process, energy consumption is effectively reduced, there is good economy and environmental benefit and wide prospects for commercial application.
Description
Technical field
The invention belongs to waste resource utilization technology fields, more particularly to a kind of to be recycled from polishing powder from rare earth waste residue
The method of polishing powder.
Background technology
With the development of science and technology, polishing powder from rare earth is widely used in showing because it is with unique physics and chemical property
The fine grinding of display screen, optical photoconductor glass, ornaments, building materials, mold and precision instrument.Wherein, cerium based relief polishing powder it is moderate with its hardness,
Precision is high in polishing process, polish the epigranular of powder, polishing time is shorter, cutting force is strong, operating environment very wiper ring
The advantages that guarantor and service life are longer is widely used in every field.When polishing powder from rare earth is polished article,
Polishing slurries are injected into article surface, polish repeatedly, and polishing fluid cannot recycle, dilute after polishing ± to throw until failure
Light powder is discharged with polishing fluid, thereby produces largely useless polishing powder from rare earth.There are many factories to polish discarded rare earth
Powder is deposited in as waste product near plant area, this not only pollutes environment, occupies Shangdi, but also is also the waste to rare earth resources.
The polishing performance and CeO of polishing powder from rare earth2Content it is closely related.According to analysis, polishing powder from rare earth fails main
Reason is two aspects：First is to have up to 20% or so glass granules in polishing process to be enriched to rare earth oxide
On surface and greasy dirt and bulky grain foreign matter are mixed into, and are reduced the content of rare earth oxide, are hindered glass surface and polishing
The close contact of powder particle, makes polishing powder in polishing process, reduces frictional heat, and the plasticity for reducing glass surface generation becomes
Thus shape affects the process that glass surface molecule redistributes and forms flat surface；Second be polishing process is a kind of strong
Strong process of lapping causes polishing crystal grain excessively to be refined, reduces polishing effect.Polishing powder from rare earth waste residue is mainly by rare earth
Polishing powder polishes the solid slag of waste liquid precipitation separation, and main component includes the polishing powder from rare earth particle of failure, and throwing chips away
Base material clast, such as glass micro mist, stone material clast, the object under the throwing of polishing pad, such as wool pad, foam bits, and
Artificial mixed precipitating reagent aluminium chloride etc. in waste liquid.With the increase of domestic polishing powder from rare earth output and dosage, not only need
A large amount of Rare-earth Mine mineral products resource is consumed, and is rich in a large amount of rare earth element in polishing powder from rare earth waste residue, there is preciousness
Resource utilization value.Therefore, the high efficiente callback that rare earth resources are carried out from polishing powder from rare earth waste residue is protected to economizing on resources
Retaining ring border has great importance, and has become an important technology and industry project.
At present around polishing powder is recycled from polishing powder from rare earth waste residue, has more patent report both at home and abroad.Chinese invention
A kind of regeneration method of fail rare earth polishing powder is disclosed in patent CN1246407C, mainly first throws the rare earth of failure
Light powder is directly chemically treated using the chemical reagent of the water-soluble alkali of 0.5~3mol/L and soluble fluoride, then right
The solid of recycling carries out high-temperature roasting processing.This method not only needs to consume a large amount of chemical reagent, generates a large amount of waste water, and
High-temperature process high energy consumption, integrated artistic are uneconomical.A kind of discard on dilute is disclosed in Chinese invention patent CN1194060C
The regeneration method of polishing powder, mainly useless polishing powder from rare earth, which is added in acid, for this method dissolves trivalent rare earth oxide, then adds
Enter 30% hydrogen peroxide by undissolved CeO2Then 5~8% light rare earth hydroxide or Ce (OH) is added in further dissolving4
Suspension be made rare-earth hydroxide precipitation, most prepare polishing powder from rare earth through high-temperature calcination afterwards.This dissolving rare earth and oxygen
Change restoring method, although dilute upper polishing powder regeneration may be implemented, also needs to consume a large amount of chemical reagent, generate a large amount of useless
Water, and the solubility of rare earth oxide is very low, thus causes the rate of recovery of polishing powder from rare earth low.Chinese Patent Application No. is
A kind of method regenerating the discarded polishing powder from rare earth applied to crystal glass is disclosed in 201110265136.1, this method is first
Scalping is carried out to polishing powder from rare earth waste residue using screening plant and removes impurity removing and bulky grain, then to dilute upper polishing powder waste residue tune
Slurry carries out gravity treatment using gravitational separation equipment, and isolated recombination is divided into the polishing powder from rare earth waste of high-content, finally uses strong
Acid carries out chemical treatment and dissolves soluble matter therein and the obtained polishing powder of high-temperature roasting.Strong acid used in this method be nitric acid and
Thus hydrofluoric acid generates great amount of soluble metal ion nitrate and fluosilicic acid waste liquid, not only need to consume a large amount of chemistry examination
Agent generates a large amount of waste water, and high-temperature roasting high energy consumption.Chinese Patent Application No. discloses one kind in being 201310148306.7
The regenerated preparation method of polishing powder from rare earth is mainly thrown using the discarded rare earth after the processing gravity treatment of hexafluoro zirconium acid aqueous ammonium
Light powder is achieved in the regeneration of polishing powder from rare earth.This method can effectively avoid the use of strong acid and the discharge of waste water, but need
A large amount of hexafluoro zirconium acid ammonium chemical reagent is consumed, cost is not only increased, and also reduces regeneration polishing powder middle rare earth
Content.Chinese Patent Application No. discloses a kind of reclaiming preparation side of waste and old polishing powder from rare earth in being 201310148306.7
Method prepares polishing powder mainly under the action of ammonium sulfate and silica using the method reclaiming of high-temperature calcination.It should
Method not only generates a large amount of exhaust gas, but also the introducing of silica causes to regenerate recovering rare earth polishing powder Rare-Earth Content drop
Low, polishing characteristic is difficult to restore completely, and needs high-temperature burning process high energy consumption.
Invention content
The technical problem to be solved by the present invention is to：The side that polishing powder is recycled in a kind of waste residue from polishing powder from rare earth is provided
Method, and effectively solve generally existing impurity in existing polishing powder from rare earth reclaiming preparation process and be difficult to effectively remove, regeneration is thrown
The content of light powder middle rare earth is low, and the problems such as need the energy consumption caused by high-temperature calcination process higher.Using the method for the present invention,
It can effectively realize efficiently separating for impurity in polishing powder from rare earth waste residue, thus to obtain the polishing powder of high rare-earth content, and nothing
High-temperature calcination process is needed, energy consumption is not only reduced, and maintains the particle characteristics of regeneration polishing powder very well, so that this hair
There is the polishing powder that bright method is recycled good polishing characteristic, integrated artistic method to have good economy and environmental benefit.
The method that polishing powder is recycled in the waste residue provided by the invention from polishing powder from rare earth, is primarily characterized in that, in acidity
The efficient activation of impurity in polishing powder from rare earth waste residue, and the combination using medicaments flotation and cyclone classification are realized in solution
Phase separation mode is realized efficiently separating for impurity and rare earth component in polishing powder from rare earth waste residue, is thrown thus to obtain high-content rare earth
Light powder, and realize the highly efficient regeneration of special floating agent by the way of lye neutralization and recycle.
Technical scheme of the present invention includes the following steps：
(1) polishing powder from rare earth waste residue is stirred according to certain mass ratio in corrosion-resistant stirred tank with acid solution
It mixes uniformly mixed, obtains polishing powder from rare earth waste residue acid slime；
(2) according to certain mass flotation more special than addition in the polishing powder from rare earth waste residue acid slime obtained to step (1)
Medicament is simultaneously further uniformly mixed；
(3) mixed material that step (2) obtains is delivered to progress first time phase separation in dense slot using noncorrosive pump
Operation is mainly the special floating agent containing impurity above dense slot, is mainly polished containing rare earth below dense slot
The acid slime of powder；
(4) the special floating agent containing impurity for obtaining step (3) is neutralized using lye, and solid-liquid point is carried out after neutralization
From, thus obtain impurity and special floating agent, in the special direct return to step of floating agent (2) with polishing powder from rare earth waste residue acid
Property slurry mixing；
(5) acid slime containing polishing powder from rare earth that step (3) obtains further is delivered to rotation using noncorrosive pump
It flows and carries out second of phase separation operation in clasfficiator, what is overflowed above vortrap is thinner overground containing particle
Rare earth acid slime, in the high-content polishing powder from rare earth acid that the mainly particle characteristics that vortrap bottom comes out are not destroyed
Property slurry；
(6) the high-content polishing powder from rare earth acid slime that step (5) obtains is separated by solid-liquid separation, thus obtains high-content
Polishing powder from rare earth and acid solution are uniformly mixed with polishing powder from rare earth waste residue in the direct return to step of acid solution (1)；
(7) it is separated by solid-liquid separation what step (6) obtained containing the thinner overground rare earth acid slime of particle, thus obtains
Overground rare-earth products and acid solution are uniformly mixed with polishing powder from rare earth waste residue in the direct return to step of acid solution (1).
Preferably, the acid solution is selected from one or more of hydrochloric acid, sulfuric acid, nitric acid, formic acid, acetic acid, propionic acid,
And the composition of acid solution is to be calculated as 0.1~20mol/L with total hydrogen ion molar concentration.
Preferably, the special floating agent is mainly to be made of collecting agent, foaming agent and regulator, wherein collecting
Agent is mainly selected from the organic solvent of phosphoric acid ester, and foaming agent is mainly selected from the organic molten of alkylsulfonate and alkylsurfuric acid salt
Agent, regulator are mainly selected from the organic solvent of alkanes, and collecting agent, foaming agent and regulator three in special floating agent
Mass ratio be 1: 0.001~0.1: 0.01~100.
Preferably, the phosphoric acid ester organic solvent is selected from dimethyl phosphate, diethyl phosphate, dibutylphosphoric acid ester, phosphorus
Sour trimethyl, tributyl phosphate, triphenyl phosphate, trioctyl phosphate, tricresyl phosphate, tricresyl phosphate tert-butyl benzene base ester, first
One or more of base phosphonic acids diisoamyl ester, butyl phosphonic acids diisobutyl ester.
Preferably, the alkyl sulfonates organic solvent be selected from dodecyl sodium sulfate, sodium cetanesulfonate,
One or more of C14-C17 sodium secondary alkyl sulfonate, neopelex, cetyl benzenesulfonic acid sodium.
Preferably, the alkylsurfuric acid salt organic solvent be selected from lauryl sodium sulfate, sodium hexadecyl sulfate,
One or more of C14-C17 Teepols.
Preferably, the alkanes organic solvent be selected from hexane and its isomers, heptane and its isomers, octane and its
One or more of isomers, nonane and its isomers, benzene,toluene,xylene, each model solvent naphtha.
Preferably, it is described for special floating agent neutralize needed for lye be selected from containing sodium hydroxide, potassium hydroxide,
Sodium carbonate, sodium bicarbonate, potassium carbonate, saleratus, calcium oxide, calcium hydroxide, magnesia, magnesium hydroxide, liquefied ammonia, gas ammonia, ammonia
The aqueous solution or slurries of one or more of water, ammonium carbonate, ammonium hydrogen carbonate, and lye additive amount is according to special floating agent
The pH of obtained aqueous solution determines for 6~8 after neutralization.
Preferably, when the polishing powder from rare earth waste residue is mixed with acid solution, polishing powder from rare earth waste residue butt amount and acid
Property solution mass ratio be 0.05~2.
Preferably, when the polishing powder from rare earth waste residue acid slime is mixed with special floating agent, polishing powder from rare earth is useless
Slag butt amount is 0.05~10 with special floating agent mass ratio.
Preferably, system temperature is 20~100 DEG C when the polishing powder from rare earth waste residue is mixed with acid solution, is averagely stopped
It is 10~120 minutes to stay the time.
Preferably, when the polishing powder from rare earth waste residue acid slime is mixed with special floating agent system temperature be 20~
100 DEG C, mean residence time is 10~120 minutes.
Object used in the present invention is polishing powder from rare earth waste residue caused by glass polishing industry.Polishing powder from rare earth is when in use
It is often slurried first with water, solid content is generally in 5~20wt%.As polishing slurries recycle the increasing of number
Add, polishing powder particles can be by continuous abrasion until failure；Meanwhile the base material (such as glass, stone material) of polishing is also with polished
Journey and be constantly enriched in slurry system.Therefore, this kind of polishing powder from rare earth waste residue mainly contains the polishing powder from rare earth of failure
Grain, throws the base material clast chipped away, such as glass micro mist, stone material clast, the object under the throwing of polishing pad, such as wool pad, bubble
Artificial mixed precipitating reagent aluminium chloride etc. in foam bits etc. and waste liquid.It unites according to the analysis of domestic useless polishing powder from rare earth component
It counts, polishing powder Particle Breakage rate is typically in the range of between 7~17% in waste slurry, glass granules, glass chip, organic polymer
Class grinds the solid content accounting of the invalid component such as skin between 3~24%；Simultaneously powder surface can there is a certain proportion of
Wrap up situation in surface.Rare earth component of the polishing powder from rare earth in polishing process contained by it does not chemically react, thus may be used
Know that in polishing powder from rare earth waste residue about 80% rare earth component still maintains the original polishing characteristic of polishing powder from rare earth.Therefore,
The rare earth component for still keeping original polishing characteristic is recycled in the recycling for realizing efficient resource in polishing powder from rare earth waste residue,
Key is how to efficiently separate out the thinner overground rare earth component of particle and glass granules, glass in polishing powder from rare earth waste residue
The invalid components such as clast, organic polymer species mill skin.
Based on this, present invention proposition is stirred using acid solution with polishing powder from rare earth waste residue first, main purpose
It is that the glass granules contained in polishing powder from rare earth waste residue, glass chip, organic polymer species are ground the invalid component such as skin to live
Change, while keeping the physical structural characteristic of rare earth component as possible.Acid solution of the present invention be selected from hydrochloric acid, sulfuric acid, nitric acid,
One or more of formic acid, acetic acid, propionic acid.Polishing powder from rare earth waste residue is after the processing of these acid solutions, its institute of one side
The particles of vitreous surface contained significantly increases-OH groups, on the other hand also promotes between above-mentioned invalid component and rare earth component
Stripping, in favor of later separation.Also, since its main function is CeO in polishing powder from rare earth2, CeO2Hardly with it is above-mentioned
Acid solution chemically reacts, and thus also preferably maintains the polishing characteristic of rare earth component.In addition, the present invention also proposes to adopt
The invalid component after activation is effectively separated with rare earth component with the mode of medicaments flotation.It is of the present invention special
Floating agent is mainly to be made of collecting agent, foaming agent and regulator, and wherein collecting agent is mainly selected from the organic of phosphoric acid ester
Solvent, foaming agent are mainly selected from the organic solvent of alkylsulfonate and alkylsurfuric acid salt, and regulator is mainly selected from alkanes
Organic solvent.Further directed in special floating agent and rare earth component containing impurity contain the thinner overground rare earth of particle
Component, the present invention also proposes to realize efficiently separating for impurity and special floating agent in such a way that lye neutralizes, and uses
The mode of cyclone classification realizes overground rare earth component and keeps efficiently separating for original rare earth component for polishing characteristic.Based on above-mentioned
Separation means, be achieved in from polishing powder from rare earth waste residue high efficiente callback polishing powder from rare earth and special floating agent efficiently again
It gives birth to and recycles.
The beneficial effects of the invention are as follows being raw material using polishing powder from rare earth waste residue caused by glass polishing industry, adopt first
It is activated with acid solution, is then neutralized by medicaments flotation and lye and the technological means such as cyclone classification,
It realizes the invalid component contained in polishing powder from rare earth waste residue and the thinner overground rare earth component of particle and keeps original polishing characteristic
Rare earth component between efficiently separate, thus to obtain high-content polishing powder from rare earth, and using lye neutralization by the way of realize
The highly efficient regeneration of special floating agent with recycle.Using the method for the present invention, can effectively realize in polishing powder from rare earth waste residue
Glass granules, glass chip, the invalid component of organic polymer species mill skin etc. and the thinner overground rare earth component of particle it is efficient
Separation, thus significantly improves the content of rare earth of the recycled polishing powder from polishing powder from rare earth waste residue, while effectively maintaining rare earth
The original polishing characteristic of polishing powder, and it is not necessarily to high-temperature calcination process, energy consumption is effectively reduced, so that the method for the present invention has
There are good economy and environmental benefit and wide prospects for commercial application.
Specific implementation mode
Of the invention for ease of understanding, it is as follows that the present invention enumerates embodiment.Those skilled in the art are it will be clearly understood that the implementation
Example is used only for helping to understand the present invention, should not be regarded as a specific limitation of the invention.
Embodiment 1.
The present embodiment is using the polishing powder from rare earth waste residue after the polishing departement use of optical manufacturing factory as raw material, and specific steps are such as
Under：
1) by polishing powder from rare earth waste residue and total hydrogen ion concentration be 0.1mol/L containing hydrochloric acid, sulfuric acid, nitric acid, formic acid,
The acid solution of one or more of acetic acid, propionic acid is 0.05 to be stirred in corrosion-resistant stirred tank according to mass ratio
It mixes uniformly mixed, obtains polishing powder from rare earth waste residue acid slime, wherein system temperature is 20 DEG C, and mean residence time is 120 points
Clock；
2) special floating agent is added in the polishing powder from rare earth waste residue acid slime obtained to step 1) and futher stirs
It is uniformly mixed, wherein special floating agent is made of collecting agent, foaming agent and regulator, and is caught in special floating agent
The mass ratio for receiving agent, foaming agent and regulator three is 1: 0.1: 100, and special floating agent addition is polishing powder from rare earth waste residue
0.1 times of butt amount, system temperature be 20 DEG C, mean residence time be 120 minutes, and collecting agent be selected from dimethyl phosphate,
Diethyl phosphate, dibutylphosphoric acid ester, trimethyl phosphate, tributyl phosphate, triphenyl phosphate, trioctyl phosphate, phosphate trimethylbenzene
One or more of ester, tricresyl phosphate tert-butyl benzene base ester, diisoamyl methylphosphonate, butyl phosphonic acids diisobutyl ester, foaming agent
Selected from dodecyl sodium sulfate, sodium cetanesulfonate, C14-C17 sodium secondary alkyl sulfonate, neopelex, hexadecane
One or more of base benzene sulfonic acid sodium salt, lauryl sodium sulfate, sodium hexadecyl sulfate, C14-C17 Teepols are adjusted
Whole dose selected from hexane and its isomers, heptane and its isomers, octane and its isomers, nonane and its isomers, benzene, toluene,
One or more of dimethylbenzene, each model solvent naphtha.
3) mixed material that step 2) obtains is delivered to using noncorrosive pump in dense slot and carries out phase separation behaviour for the first time
Make, is mainly the special floating agent containing impurity above dense slot, mainly contains polishing powder from rare earth below dense slot
Acid slime；
4) the special floating agent containing impurity for obtaining step 3) is used containing sodium hydroxide, potassium hydroxide, carbonic acid
Sodium, sodium bicarbonate, potassium carbonate, saleratus, calcium oxide, calcium hydroxide, magnesia, magnesium hydroxide, liquefied ammonia, gas ammonia, ammonium hydroxide, carbon
The aqueous solution or slurries of one or more of sour ammonium, ammonium hydrogen carbonate are neutralized, and so that after the neutralization of special floating agent
The pH of obtained aqueous solution is 8, is separated by solid-liquid separation after neutralization, thus obtains impurity and special floating agent, special floating agent
Direct return to step 2) in mixed with polishing powder from rare earth waste residue acid slime；
5) acid slime containing polishing powder from rare earth that step 3) obtains further is delivered to eddy flow using noncorrosive pump
Second of phase separation operation is carried out in clasfficiator, what is overflowed above vortrap is thinner overground dilute containing particle
Native acid slime, it is acid in the high-content polishing powder from rare earth that the mainly particle characteristics that vortrap bottom comes out are not destroyed
Slurry；
6) the high-content polishing powder from rare earth acid slime that step 5) obtains is separated by solid-liquid separation, it is dilute thus obtains high-content
Native polishing powder and acid solution, the direct return to step of acid solution 1) in uniformly mixed with polishing powder from rare earth waste residue；
7) it is separated by solid-liquid separation what step 5) obtained containing the thinner overground rare earth acid slime of particle, thus obtained
Grind rare-earth products and acid solution, the direct return to step of acid solution 1) in uniformly mixed with polishing powder from rare earth waste residue.
8) it is tested by Weighing and analysis, the results showed that the present embodiment middle rare earth polishing powder rate of recovery is 75%, is thrown
Light powder Rare-Earth Content is 98%.
Embodiment 2.
The present embodiment is using the polishing powder from rare earth waste residue after the polishing departement use of optical manufacturing factory as raw material, and specific steps are such as
Under：
1) polishing powder from rare earth waste residue and total hydrogen ion concentration are contained into hydrochloric acid, sulfuric acid, nitric acid, formic acid, second for 20mol/L
The acid solution of one or more of acid, propionic acid is stirred mixing for 2 according to mass ratio in corrosion-resistant stirred tank
Uniformly, polishing powder from rare earth waste residue acid slime is obtained, wherein system temperature is 100 DEG C, and mean residence time is 10 minutes；
2) special floating agent is added in the polishing powder from rare earth waste residue acid slime obtained to step 1) and futher stirs
It is uniformly mixed, wherein special floating agent is made of collecting agent, foaming agent and regulator, and is caught in special floating agent
The mass ratio for receiving agent, foaming agent and regulator three is 1: 0.001: 0.01, and special floating agent addition is polishing powder from rare earth
20 times of waste residue butt amount, system temperature are 100 DEG C, and mean residence time is 10 minutes, and collecting agent is selected from phosphoric acid diformazan
Ester, diethyl phosphate, dibutylphosphoric acid ester, trimethyl phosphate, tributyl phosphate, triphenyl phosphate, trioctyl phosphate, tripotassium phosphate
One or more of phenyl ester, tricresyl phosphate tert-butyl benzene base ester, diisoamyl methylphosphonate, butyl phosphonic acids diisobutyl ester, blistering
Agent is selected from dodecyl sodium sulfate, sodium cetanesulfonate, C14-C17 sodium secondary alkyl sulfonate, neopelex, 16
One or more of sodium alkyl benzene sulfonate, lauryl sodium sulfate, sodium hexadecyl sulfate, C14-C17 Teepols,
Regulator is selected from hexane and its isomers, heptane and its isomers, octane and its isomers, nonane and its isomers, benzene, first
One or more of benzene, dimethylbenzene, each model solvent naphtha.
3) mixed material that step 2) obtains is delivered to using noncorrosive pump in dense slot and carries out phase separation behaviour for the first time
Make, is mainly the special floating agent containing impurity above dense slot, mainly contains polishing powder from rare earth below dense slot
Acid slime；
4) the special floating agent containing impurity for obtaining step 3) is used containing sodium hydroxide, potassium hydroxide, carbonic acid
Sodium, sodium bicarbonate, potassium carbonate, saleratus, calcium oxide, calcium hydroxide, magnesia, magnesium hydroxide, liquefied ammonia, gas ammonia, ammonium hydroxide, carbon
The aqueous solution or slurries of one or more of sour ammonium, ammonium hydrogen carbonate are neutralized, and so that after the neutralization of special floating agent
The pH of obtained aqueous solution is 6, is separated by solid-liquid separation after neutralization, thus obtains impurity and special floating agent, special floating agent
Direct return to step 2) in mixed with polishing powder from rare earth waste residue acid slime；
5) acid slime containing polishing powder from rare earth that step 3) obtains further is delivered to eddy flow using noncorrosive pump
Second of phase separation operation is carried out in clasfficiator, what is overflowed above vortrap is thinner overground dilute containing particle
Native acid slime, it is acid in the high-content polishing powder from rare earth that the mainly particle characteristics that vortrap bottom comes out are not destroyed
Slurry；
6) the high-content polishing powder from rare earth acid slime that step 5) obtains is separated by solid-liquid separation, it is dilute thus obtains high-content
Native polishing powder and acid solution, the direct return to step of acid solution 1) in uniformly mixed with polishing powder from rare earth waste residue；
7) it is separated by solid-liquid separation what step 5) obtained containing the thinner overground rare earth acid slime of particle, thus obtained
Grind rare-earth products and acid solution, the direct return to step of acid solution 1) in uniformly mixed with polishing powder from rare earth waste residue.
8) it is tested by Weighing and analysis, the results showed that the present embodiment middle rare earth polishing powder rate of recovery is 72%, is thrown
Light powder Rare-Earth Content is 95%.
Embodiment 3.
The present embodiment is using the polishing powder from rare earth waste residue after the polishing departement use of optical manufacturing factory as raw material, and specific steps are such as
Under：
1) polishing powder from rare earth waste residue and total hydrogen ion concentration are contained into hydrochloric acid, sulfuric acid, nitric acid, formic acid, second for 10mol/L
The acid solution of one or more of acid, propionic acid is stirred mixing for 1 according to mass ratio in corrosion-resistant stirred tank
Uniformly, polishing powder from rare earth waste residue acid slime is obtained, wherein system temperature is 50 DEG C, and mean residence time is 60 minutes；
2) special floating agent is added in the polishing powder from rare earth waste residue acid slime obtained to step 1) and futher stirs
It is uniformly mixed, wherein special floating agent is made of collecting agent, foaming agent and regulator, and is caught in special floating agent
The mass ratio for receiving agent, foaming agent and regulator three is 1: 0.1: 50, and special floating agent addition is polishing powder from rare earth waste residue
10 times of butt amount, system temperature are 100 DEG C, and mean residence time is 60 minutes, and collecting agent is selected from dimethyl phosphate, phosphorus
Diethyl phthalate, dibutylphosphoric acid ester, trimethyl phosphate, tributyl phosphate, triphenyl phosphate, trioctyl phosphate, tricresyl phosphate,
One or more of tricresyl phosphate tert-butyl benzene base ester, diisoamyl methylphosphonate, butyl phosphonic acids diisobutyl ester, foaming agent is selected from
Dodecyl sodium sulfate, sodium cetanesulfonate, C14-C17 sodium secondary alkyl sulfonate, neopelex, cetyl benzene
One or more of sodium sulfonate, lauryl sodium sulfate, sodium hexadecyl sulfate, C14-C17 Teepols, regulator
Selected from hexane and its isomers, heptane and its isomers, octane and its isomers, nonane and its isomers, benzene, toluene, diformazan
One or more of benzene, each model solvent naphtha.
3) mixed material that step 2) obtains is delivered to using noncorrosive pump in dense slot and carries out phase separation behaviour for the first time
Make, is mainly the special floating agent containing impurity above dense slot, mainly contains polishing powder from rare earth below dense slot
Acid slime；
4) the special floating agent containing impurity for obtaining step 3) is used containing sodium hydroxide, potassium hydroxide, carbonic acid
Sodium, sodium bicarbonate, potassium carbonate, saleratus, calcium oxide, calcium hydroxide, magnesia, magnesium hydroxide, liquefied ammonia, gas ammonia, ammonium hydroxide, carbon
The aqueous solution or slurries of one or more of sour ammonium, ammonium hydrogen carbonate are neutralized, and so that after the neutralization of special floating agent
The pH of obtained aqueous solution is 7, is separated by solid-liquid separation after neutralization, thus obtains impurity and special floating agent, special floating agent
Direct return to step 2) in mixed with polishing powder from rare earth waste residue acid slime；
5) acid slime containing polishing powder from rare earth that step 3) obtains further is delivered to eddy flow using noncorrosive pump
Second of phase separation operation is carried out in clasfficiator, what is overflowed above vortrap is thinner overground dilute containing particle
Native acid slime, it is acid in the high-content polishing powder from rare earth that the mainly particle characteristics that vortrap bottom comes out are not destroyed
Slurry；
6) the high-content polishing powder from rare earth acid slime that step 5) obtains is separated by solid-liquid separation, it is dilute thus obtains high-content
Native polishing powder and acid solution, the direct return to step of acid solution 1) in uniformly mixed with polishing powder from rare earth waste residue；
7) it is separated by solid-liquid separation what step 5) obtained containing the thinner overground rare earth acid slime of particle, thus obtained
Grind rare-earth products and acid solution, the direct return to step of acid solution 1) in uniformly mixed with polishing powder from rare earth waste residue.
8) it is tested by Weighing and analysis, the results showed that the present embodiment middle rare earth polishing powder rate of recovery is 74%, is thrown
Light powder Rare-Earth Content is 97%.
Embodiment 4.
The present embodiment is using the polishing powder from rare earth waste residue after the polishing departement use of optical manufacturing factory as raw material, and specific steps are such as
Under：
1) polishing powder from rare earth waste residue and total hydrogen ion concentration are contained into hydrochloric acid, sulfuric acid, nitric acid, formic acid, second for 10mol/L
The acid solution of one or more of acid, propionic acid is stirred mixing for 1 according to mass ratio in corrosion-resistant stirred tank
Uniformly, polishing powder from rare earth waste residue acid slime is obtained, wherein system temperature is 60 DEG C, and mean residence time is 60 minutes；
2) special floating agent is added in the polishing powder from rare earth waste residue acid slime obtained to step 1) and futher stirs
It is uniformly mixed, wherein special floating agent is made of collecting agent, foaming agent and regulator, and is caught in special floating agent
The mass ratio for receiving agent, foaming agent and regulator three is 1: 0.001: 0.01, and special floating agent addition is polishing powder from rare earth
10 times of waste residue butt amount, system temperature are 60 DEG C, and mean residence time is 60 minutes, and collecting agent is selected from phosphoric acid diformazan
Ester, diethyl phosphate, dibutylphosphoric acid ester, trimethyl phosphate, tributyl phosphate, triphenyl phosphate, trioctyl phosphate, tripotassium phosphate
One or more of phenyl ester, tricresyl phosphate tert-butyl benzene base ester, diisoamyl methylphosphonate, butyl phosphonic acids diisobutyl ester, blistering
Agent is selected from dodecyl sodium sulfate, sodium cetanesulfonate, C14-C17 sodium secondary alkyl sulfonate, neopelex, 16
One or more of sodium alkyl benzene sulfonate, lauryl sodium sulfate, sodium hexadecyl sulfate, C14-C17 Teepols,
Regulator is selected from hexane and its isomers, heptane and its isomers, octane and its isomers, nonane and its isomers, benzene, first
One or more of benzene, dimethylbenzene, each model solvent naphtha.
3) mixed material that step 2) obtains is delivered to using noncorrosive pump in dense slot and carries out phase separation behaviour for the first time
Make, is mainly the special floating agent containing impurity above dense slot, mainly contains polishing powder from rare earth below dense slot
Acid slime；
4) the special floating agent containing impurity for obtaining step 3) is used containing sodium hydroxide, potassium hydroxide, carbonic acid
Sodium, sodium bicarbonate, potassium carbonate, saleratus, calcium oxide, calcium hydroxide, magnesia, magnesium hydroxide, liquefied ammonia, gas ammonia, ammonium hydroxide, carbon
The aqueous solution or slurries of one or more of sour ammonium, ammonium hydrogen carbonate are neutralized, and so that after the neutralization of special floating agent
The pH of obtained aqueous solution is 7, is separated by solid-liquid separation after neutralization, thus obtains impurity and special floating agent, special floating agent
Direct return to step 2) in mixed with polishing powder from rare earth waste residue acid slime；
5) acid slime containing polishing powder from rare earth that step 3) obtains further is delivered to eddy flow using noncorrosive pump
Second of phase separation operation is carried out in clasfficiator, what is overflowed above vortrap is thinner overground dilute containing particle
Native acid slime, it is acid in the high-content polishing powder from rare earth that the mainly particle characteristics that vortrap bottom comes out are not destroyed
Slurry；
6) the high-content polishing powder from rare earth acid slime that step 5) obtains is separated by solid-liquid separation, it is dilute thus obtains high-content
Native polishing powder and acid solution, the direct return to step of acid solution 1) in uniformly mixed with polishing powder from rare earth waste residue；
7) it is separated by solid-liquid separation what step 5) obtained containing the thinner overground rare earth acid slime of particle, thus obtained
Grind rare-earth products and acid solution, the direct return to step of acid solution 1) in uniformly mixed with polishing powder from rare earth waste residue.
8) it is tested by Weighing and analysis, the results showed that the present embodiment middle rare earth polishing powder rate of recovery is 74%, is thrown
Light powder Rare-Earth Content is 97%.
Embodiment 4.
The present embodiment is using the polishing powder from rare earth waste residue after the polishing departement use of optical manufacturing factory as raw material, and specific steps are such as
Under：
1) polishing powder from rare earth waste residue and total hydrogen ion concentration are contained into hydrochloric acid, sulfuric acid, nitric acid, formic acid, second for 5mol/L
The acid solution of acid, one or more of propionic acid, according to mass ratio be 0.5 be stirred in corrosion-resistant stirred tank it is mixed
It closes uniformly, obtains polishing powder from rare earth waste residue acid slime, wherein system temperature is 60 DEG C, and mean residence time is 60 minutes；
2) special floating agent is added in the polishing powder from rare earth waste residue acid slime obtained to step 1) and futher stirs
It is uniformly mixed, wherein special floating agent is made of collecting agent, foaming agent and regulator, and is caught in special floating agent
The mass ratio for receiving agent, foaming agent and regulator three is 1: 0.05: 5, and special floating agent addition is polishing powder from rare earth waste residue
1 times of butt amount, system temperature are 60 DEG C, and mean residence time is 60 minutes, and collecting agent is selected from dimethyl phosphate, phosphoric acid
Diethylester, dibutylphosphoric acid ester, trimethyl phosphate, tributyl phosphate, triphenyl phosphate, trioctyl phosphate, tricresyl phosphate, phosphorus
One or more of sour tri-tert phenylester, diisoamyl methylphosphonate, butyl phosphonic acids diisobutyl ester, foaming agent are selected from ten
Dialkyl sulfonates, sodium cetanesulfonate, C14-C17 sodium secondary alkyl sulfonate, neopelex, cetyl benzene sulphur
One or more of sour sodium, lauryl sodium sulfate, sodium hexadecyl sulfate, C14-C17 Teepols, regulator choosing
From hexane and its isomers, heptane and its isomers, octane and its isomers, nonane and its isomers, benzene,toluene,xylene,
One or more of each model solvent naphtha.
3) mixed material that step 2) obtains is delivered to using noncorrosive pump in dense slot and carries out phase separation behaviour for the first time
Make, is mainly the special floating agent containing impurity above dense slot, mainly contains polishing powder from rare earth below dense slot
Acid slime；
4) the special floating agent containing impurity for obtaining step 3) is used containing sodium hydroxide, potassium hydroxide, carbonic acid
Sodium, sodium bicarbonate, potassium carbonate, saleratus, calcium oxide, calcium hydroxide, magnesia, magnesium hydroxide, liquefied ammonia, gas ammonia, ammonium hydroxide, carbon
The aqueous solution or slurries of one or more of sour ammonium, ammonium hydrogen carbonate are neutralized, and so that after the neutralization of special floating agent
The pH of obtained aqueous solution is 7, is separated by solid-liquid separation after neutralization, thus obtains impurity and special floating agent, special floating agent
Direct return to step 2) in mixed with polishing powder from rare earth waste residue acid slime；
5) acid slime containing polishing powder from rare earth that step 3) obtains further is delivered to eddy flow using noncorrosive pump
Second of phase separation operation is carried out in clasfficiator, what is overflowed above vortrap is thinner overground dilute containing particle
Native acid slime, it is acid in the high-content polishing powder from rare earth that the mainly particle characteristics that vortrap bottom comes out are not destroyed
Slurry；
6) the high-content polishing powder from rare earth acid slime that step 5) obtains is separated by solid-liquid separation, it is dilute thus obtains high-content
Native polishing powder and acid solution, the direct return to step of acid solution 1) in uniformly mixed with polishing powder from rare earth waste residue；
7) it is separated by solid-liquid separation what step 5) obtained containing the thinner overground rare earth acid slime of particle, thus obtained
Grind rare-earth products and acid solution, the direct return to step of acid solution 1) in uniformly mixed with polishing powder from rare earth waste residue.
8) it is tested by Weighing and analysis, the results showed that the present embodiment middle rare earth polishing powder rate of recovery is 74%, is thrown
Light powder Rare-Earth Content is 97%.
Applicant states that the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological processes, that is, it is above-mentioned detailed not mean that the present invention has to rely on
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The addition of equivalence replacement and auxiliary element to each raw material of product of the present invention, the selection etc. of concrete mode all fall within the present invention's
Within protection domain and the open scope.
Claims (10)
1. a kind of method for recycling polishing powder in waste residue from polishing powder from rare earth, is primarily characterized in that, first in an acidic solution
It realizes the efficient activation of impurity in polishing powder from rare earth waste residue, and is separated using medicaments flotation and the combination of cyclone classification
Mode realizes efficiently separating for impurity and rare earth component in polishing powder from rare earth waste residue, thus to obtain high-content polishing powder from rare earth, and
And realize the highly efficient regeneration of special floating agent by the way of lye neutralization and recycle, specific technical solution includes following
Step：
(1) polishing powder from rare earth waste residue is stirred according to certain mass ratio in corrosion-resistant stirred tank with acid solution mixed
It closes uniformly, obtains polishing powder from rare earth waste residue acid slime；
(2) according to certain mass floating agent more special than addition in the polishing powder from rare earth waste residue acid slime obtained to step (1)
And it is further uniformly mixed；
(3) mixed material that step (2) obtains is delivered to using noncorrosive pump in dense slot and carries out phase separation operation for the first time,
It is mainly the special floating agent containing impurity above dense slot, is mainly the acid containing polishing powder from rare earth below dense slot
Property slurry；
(4) the special floating agent containing impurity for obtaining step (3) is neutralized using lye, is separated by solid-liquid separation after neutralization,
Thus impurity and special floating agent are obtained, it is acid with polishing powder from rare earth waste residue in the special direct return to step of floating agent (2)
Slurry mixes；
(5) acid slime containing polishing powder from rare earth that step (3) obtains further is delivered to eddy flow point using noncorrosive pump
Second of phase separation operation is carried out in grade device, what is overflowed above vortrap is containing the thinner overground rare earth of particle
Acid slime, in the high-content polishing powder from rare earth acidity material that mainly particle characteristics are not destroyed that vortrap bottom comes out
Slurry；
(6) the high-content polishing powder from rare earth acid slime that step (5) obtains is separated by solid-liquid separation, thus obtains high-content rare earth
Polishing powder and acid solution are uniformly mixed with polishing powder from rare earth waste residue in the direct return to step of acid solution (1)；
(7) it is separated by solid-liquid separation, thus obtains overground containing the thinner overground rare earth acid slime of particle by what step (6) obtained
Rare-earth products and acid solution are uniformly mixed with polishing powder from rare earth waste residue in the direct return to step of acid solution (1).
2. the method for recycling polishing powder in the waste residue as described in claim 1 from polishing powder from rare earth, wherein the acid solution
Composition selected from one or more of hydrochloric acid, sulfuric acid, nitric acid, formic acid, acetic acid, propionic acid, and acid solution be with total hydrogen from
Sub- molar concentration is calculated as 0.1~20mol/L.
3. the method for recycling polishing powder in the waste residue as described in claim 1 from polishing powder from rare earth, wherein the special flotation
Medicament is mainly to be made of collecting agent, foaming agent and regulator, and wherein collecting agent is mainly selected from the organic solvent of phosphoric acid ester,
Foaming agent is mainly selected from the organic solvent of alkylsulfonate and alkylsurfuric acid salt, and regulator is mainly selected from the organic molten of alkanes
Agent, and in special floating agent collecting agent, foaming agent and regulator three mass ratio be 1: 0.001~0.1: 0.01~
100。
4. the method for recycling polishing powder in the waste residue as described in claim 1 from polishing powder from rare earth, wherein described being used for is special
Floating agent neutralizes required lye and is selected from containing sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, bicarbonate
One kind or several in potassium, calcium oxide, calcium hydroxide, magnesia, magnesium hydroxide, liquefied ammonia, gas ammonia, ammonium hydroxide, ammonium carbonate, ammonium hydrogen carbonate
The aqueous solution or slurries of kind, and lye additive amount is true for 6~8 according to the pH of obtained aqueous solution after the neutralization of special floating agent
It is fixed.
5. by the method for recycling polishing powder in the slave polishing powder from rare earth waste residue described in claim 1 and 3, the phosphoric acid ester has
Solvent be selected from dimethyl phosphate, diethyl phosphate, dibutylphosphoric acid ester, trimethyl phosphate, tributyl phosphate, triphenyl phosphate,
Trioctyl phosphate, tricresyl phosphate, tricresyl phosphate tert-butyl benzene base ester, diisoamyl methylphosphonate, butyl phosphonic acids diisobutyl ester
One or more of.
6. by the method for recycling polishing powder in the slave polishing powder from rare earth waste residue described in claim 1 and 3, the alkylsulfonate
Class organic solvent is selected from dodecyl sodium sulfate, sodium cetanesulfonate, C14-C17 sodium secondary alkyl sulfonate, detergent alkylate sulphur
One or more of sour sodium, cetyl benzenesulfonic acid sodium.
7. by the method for recycling polishing powder in the slave polishing powder from rare earth waste residue described in claim 1 and 3, the alkyl sulfate
The one kind or several of class organic solvent in lauryl sodium sulfate, sodium hexadecyl sulfate, C14-C17 Teepols
Kind.
8. by the method for recycling polishing powder in the slave polishing powder from rare earth waste residue described in claim 1 and 3, the alkanes are organic
Solvent be selected from hexane and its isomers, heptane and its isomers, octane and its isomers, nonane and its isomers, benzene, toluene,
One or more of dimethylbenzene, each model solvent naphtha.
9. by the method for recycling polishing powder in the slave polishing powder from rare earth waste residue described in claim 1-8, the polishing powder from rare earth
System temperature is 20~100 DEG C when waste residue is mixed with acid solution, the quality of polishing powder from rare earth waste residue butt amount and acid solution
Than being 0.05~2, mean residence time is 10~120 minutes.
10. by the method for recycling polishing powder in the slave polishing powder from rare earth waste residue described in claim 1-8, the polishing powder from rare earth
System temperature is 20~100 DEG C when waste residue acid slime is mixed with special floating agent, polishing powder from rare earth waste residue butt amount and spy
Different floating agent mass ratio is 0.05~10, and mean residence time is 10~120 minutes.
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| CN114700180A (en) * | 2022-03-21 | 2022-07-05 | 中南大学 | Method for recovering rare earth components in waste polishing powder |
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