CN107022681A - A kind of comprehensive recovering process of aluminium scrap silicon middle rare earth, aluminium and silicon - Google Patents
A kind of comprehensive recovering process of aluminium scrap silicon middle rare earth, aluminium and silicon Download PDFInfo
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- CN107022681A CN107022681A CN201710063044.2A CN201710063044A CN107022681A CN 107022681 A CN107022681 A CN 107022681A CN 201710063044 A CN201710063044 A CN 201710063044A CN 107022681 A CN107022681 A CN 107022681A
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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
- C22B21/00—Obtaining aluminium
- C22B21/0015—Obtaining aluminium by wet processes
- C22B21/0023—Obtaining aluminium by wet processes from waste materials
- C22B21/003—Obtaining aluminium by wet processes from waste materials from spent catalysts
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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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Abstract
The invention discloses the comprehensive recovering process of a kind of aluminium scrap silicon middle rare earth, aluminium and silicon, comprise the following steps：S1 aluminium scrap silicon acidleach obtains the pickle liquor containing rare earth and aluminium and Silicon-rich slag；Pickle liquors of the S2 containing rare earth and aluminium adds precipitating reagent and obtains double salt of rare earth precipitation and filtrate containing aluminium；S3 filtrates containing aluminium prepare sodium metaaluminate or aluminum sulfate.Being completely separated for rare earth and aluminium is the method achieve, the two yield and purity greatly improved, while completing being recovered according to a price for silicon, the comprehensive reutilization of essential element in aluminium scrap silicon is truly realized.Whole recovery process flow has alkaline consumption small, and water consume is small, the advantage such as wastewater discharge is small, while the technique also has, fixed investment is few, and production cost is low, the characteristics of easily realizing industrialization production.
Description
Technical field
The invention belongs to solid waste recycling field, and in particular to a kind of to reclaim dilute from the aluminum-silicon materials containing rare earth
The method of soil, aluminium and silicon.
Background technology
Rare earth is widely used as new and high technology element in catalyst field.In the 1960s, rare earth-Y type molecules
Sieve is widely used in RFCC, and rare earth is also applied on other molecular sieve catalysts afterwards.At present, it is domestic
Consumption figure of the rare earth in Effect of Catalysis In Petrochemistry field accounts for more than the 10% of rare earth aggregate consumption, and the whole world is annual for the dilute of petrochemical industry
Native number is with ten thousand tons of calculating.
With the worsening shortages of resource, reclaim valuable dilute from petrochemical catalyst preparation process or in catalyst waste material
Native composition has good social and economic benefit.Chinese patent CN1686813 discloses one kind catalyst of deposed molecular sieve system
The method of standby aluminium polychloride, can enable the aluminium in waste material reclaim, but the patent is not directed to the recovery of high price rare earth element.
Domestic early stage is also sunk to the rare earth chloride filtrate produced in sieve synthesis procedure using extraction, ammoniacal liquor or sodium carbonate
Shallow lake method directly reclaims (Zhang Jiguang；《Extraction reclaims molecular sieve filtrate middle rare earth technology》, Industrial Catalysis, GONGYE CUIHUA
(INDUSTRIALCATALYSIS), phase nineteen ninety-five 01) (Jiao reads a letter,《The recovery profit of rare earth chloride in molecular sieve production waste
With》, Shandong petrochemical industry, Qilu Petrochemical Technology, phase nineteen ninety-five 02), (Lanzhou Oil Refinery,《Molecule
The recovery of screen device rare earth chloride》, petroleum refining and chemical industry, Petroleum Processing and Petrochemicals,
08 phase in 1981), because rare earth chloride filtrate component is relatively single, therefore above-mentioned recovery process is simple, is adopted extensively at home
With.For from system with molecular sieve for preparing it is standby during direct recovering rare earth in the molecular sieve waste material produced or the molecular sieve waste material used
Work do not carry out also both at home and abroad.
Main component is silicon and aluminium in molecular sieve waste material, belongs to typical aluminum-silicon materials, additionally contains rare earth element.Root
According to Chinese patent CN1686813 and experimental study, the aluminium element activity in molecular sieve waste material is high, is easy to during direct Ore Leaching
Dissolving, rare earth and aluminium have the characteristic of co-dissolve, not only consume substantial amounts of leaching and follow-up removal of impurities and single rare earth extraction are returned with acid
Separation is taken to bring great trouble.
For the rare earth waste of the silicon containing aluminium, this kind of rare earth of such as fluorescent powder scrap and the relatively low material of aluminium dissolving activity are domestic
Also there is the technique that Extraction of rare earth is handled using alkaline process, patent CN200810029417.5 is to propose similar method, this method pair
Low activity alumina raw material has applicability, there is long flow path, the problem of rare-earth yield is low.
However, the above method is primarily upon the separation and recovery of rare earth, and substantial amounts of aluminium and silicon materials fail effective utilization.Together
When, the method for prior art is difficult to being completely separated for rare earth and aluminium, and alkaline consumption and water consume are larger in whole technological process, environment
It is seriously polluted.
The content of the invention
A kind of method that the present invention proposes recovering rare earth from the aluminum-silicon materials containing rare earth, aluminium and silicon.This method is realized
Being completely separated for rare earth and aluminium, greatly improved the two yield and purity, while completing being recovered according to a price for silicon, very
Just realizing the comprehensive reutilization of essential element in aluminium scrap silicon.Whole recovery process flow has alkaline consumption small, and water consume is small, gives up
The advantage such as water discharge capacity is small, while the technique also has, fixed investment is few, and production cost is low, easily realizes the spy of industrialization production
Point.
The technical solution adopted by the present invention is：
The comprehensive recovering process of a kind of aluminium scrap silicon middle rare earth, aluminium and silicon, comprises the following steps：S1 aluminium scrap silicon acidleach is obtained
To the pickle liquor containing rare earth and aluminium and Silicon-rich slag；Pickle liquors of the S2 containing rare earth and aluminium add precipitating reagent obtain double salt of rare earth precipitation and
Filtrate containing aluminium, it is characterised in that S3 filtrates containing aluminium prepare sodium metaaluminate or aluminum sulfate.
Method also includes：S4, Silicon-rich slag prepares waterglass；Preferably, method also comprises the following steps：S5, double salt of rare earth
Precipitation obtains rare earth hydrate and waste liquid with being filtered after aqueous slkali reaction.Step S1 process conditions are：Control the temperature of acidleach
For 10~80 DEG C, preferably 15~60 DEG C, more preferably 20-40 DEG C.Course of reaction pH value is 0.1~2.5, is preferably
0.5~2.0, more preferably 0.8~1.5.The endpoint pH of pickle liquor containing rare earth and aluminium is 0.5~2.0, is preferably
0.6~1.8, more preferably 0.8~1.5.Leaching way can take stirring or dump leaching.When taking mixer meanses, stir
The time of mixing is advantageously 3~12 hours；When taking dump leaching means, the dump leaching time is advantageously 24~72 hours.Liquid-solid ratio has
It is 3 sharply:1~6:1, preferably 4:1~5:1.
Step S1 acid is selected from one kind of sulfuric acid solution, hydrochloric acid solution or salpeter solution；Most preferably hydrochloric acid solution.
Step S2 process conditions are：The mol ratio of precipitating reagent and the pickle liquor Rare Earth Ion containing rare earth and aluminium is 1:1
~5:1, preferably 3:1~4:1.Precipitation reaction preferably continues 0.5~4h, preferably at 10~60 DEG C at a temperature of 20~40 DEG C
Continue 1-3h.
Step S2 precipitating reagent is in ammonium sulfate, ammonium hydrogen sulfate, sodium sulphate, niter cake, potassium sulfate or potassium acid sulfate
One kind, preferably ammonium sulfate, sodium sulphate or potassium sulfate one kind, most preferably sodium sulphate.The addition of precipitating reagent be equal to or
More than theoretical amount needed for double salt of rare earth precipitation, 1.0-3.0 times of the latter is advantageously.The temperature control of double salt of rare earth precipitated crystal
System is between 20-90 DEG C.Increase precipitating reagent consumption and improve precipitated crystal temperature be conducive to improve rare-earth yield, this be because
Reduced for the solubility with temperature rise of sulfuric acid rare earth double salt.To avoid being in the solution loss of rare earth element, actual production
The loss of double salt of rare earth precipitation and reduction water consumption are avoided, liquid-solid ratio is unsuitable excessive.
Precipitating reagent in step S2 is sodium sulphate or potassium sulfate, and after double salt of rare earth precipitation is obtained, this method also includes：
S5, double salt of rare earth precipitation obtains rare earth hydrate and waste liquid with being filtered after aqueous slkali reaction, wherein, aqueous slkali is sodium hydroxide
Or potassium hydroxide, the waste liquid that correspondence is obtained is metabisulfite solution or potassium sulfate solution, and this method also includes：Step S5 is obtained
Above-mentioned steps S2 applications are returned after metabisulfite solution or potassium sulfate solution concentration and recovery.
Step S3 is：Filtrate containing aluminium prepares sulfuric acid by alkali precipitation-alkali transformation of ownership for sodium metaaluminate or alkali precipitation-sulfuric acid dissolution
Aluminium.
Step S3 alkali precipitation step is：Alkaline matter is added into filtrate containing aluminium and carries out precipitation reaction, obtains containing hydrogen-oxygen
Change the precipitation of aluminium.Advantageously, precipitation reaction is carried out under agitation.
Alkaline matter is selected from organic basic material and/or inorganic base substance.Organic basic material is quaternary ammonium base, had
Aqueous solution of machine amine etc..Inorganic base substance is soluble carbonate salt, soluble bicarbonate, soluble hydroxide or ammonia
At least one of water, preferably sodium hydroxide, sodium carbonate and sodium acid carbonate.
Precipitation reaction preferably continues 0.5~4h at a temperature of 20~40 DEG C, preferably lasts for 2~3h at 10~60 DEG C；Reaction
The pH value of terminal is 4.5~9.0, preferably 4.5~7.0.
Step S3 alkali go to step for：The precipitation of aluminium hydroxide and sodium hydrate aqueous solution or piece alkali are reacted, reaction
After be filtrated to get sodium aluminate solution and aluminium white residue；Sulfuric acid dissolution step is：The precipitation of aluminium hydroxide and sulfuric acid reaction are obtained
To aluminum sulfate solution.
In alkali is gone to step, the mol ratio of aluminium atom is 1 in the precipitation of sodium hydroxide and aluminium hydroxide:1~3:1, it is excellent
Elect 1.5~2 as:1；Reaction, preferably at 35~100 DEG C, 0.5~8h is continued at a temperature of most preferably 50~80 DEG C at 20~120 DEG C,
1~6h is preferably lasted for, most preferably continues 1~4h；In sulfuric acid dissolution step, in the aluminum sulfate solution of preparation, concentration is with aluminum oxide
70~110g/L, preferably 85~95g/L are calculated as, pH value is 1.5~2.5.
Step S4 is：Silicon-rich slag is reacted with sodium hydrate aqueous solution or piece alkali, and waterglass and waste residue are filtrated to get after reaction.
Wherein, the mol ratio of silicon atom and sodium hydroxide is 1.6 in Silicon-rich slag:1~4.8:1, reaction pressure 0.5~
1.2MPa, reaction continues 2~10h at a temperature of 150~300 DEG C, preferably lasts for 6-8h.
Step S5 process conditions are：The mol ratio of hydroxyl ion and double salt of rare earth middle rare earth atom is 3 in aqueous slkali:1
~5:1；Slurry liquid-solid ratio 2:1~4:1, react at 50~100 DEG C, preferably at 70~100 DEG C, most preferably in 80~95 DEG C of temperature
Under continue 1~5 hour.
When alumina-silica amount ratio is more than 1 in aluminium scrap silicon:When 1, before step S1, increase and the aluminium in aluminium scrap silicon is carried out
The step of step S6 tentatively reclaimed, preliminary recovery, includes：Aluminium scrap silicon and sodium hydroxide are reacted, separation of solid and liquid obtains inclined aluminium
Acid sodium solution and the aluminium white residue containing rare earth.The aluminium white residue containing rare earth that this step is obtained carries out subsequent treatment as aluminium scrap silicon.
The mol ratio of sodium hydroxide and aluminium atom in aluminium scrap silicon is 1:1~3:1, preferably 1.5:1~2:1；Reaction exists
20~120 DEG C, preferably at 35~100 DEG C, continue 0.5~8h at a temperature of most preferably 50~80 DEG C, preferably last for 1~6h, it is optimal
Choosing continues 1~4h.
The above method destroys the structure containing rare earth and aluminium component in aluminium scrap silicon by the way that acid is molten, realizes in aluminium silicon waste residue
The efficient leaching of rare earth and aluminium.The property of the double salt precipitation insoluble in acid solution can be formed using rare earth, it is suitable by addition
The precipitating reagent of amount realizes the Selective Separation of rare earth；Gained double salt of rare earth obtains the smaller hydroxide of solubility after being reacted with alkali dilute
Soil precipitation, while removing the aluminium dissolving of entrained with double salt of rare earth precipitation, gained rare earth hydrate can dissolve to formulate concentration
Rare-earth salt solution reclaimed.The property that can be further hydrolyzed in acid condition using aluminium is from double salt precipitation rare earth
Selecting property water prepares aluminum hydroxide precipitation in solution afterwards, realizes the separation of aluminium.Because aluminium hydroxide has both sexes, acid can be dissolved in
Or alkali, therefore corresponding aluminum salt solution or sodium aluminate solution can be prepared into as needed reclaimed.
Top method not only realizes being completely separated for rare earth and aluminium, and the yield and purity of the two greatly improved, and
Being recovered according to a price for silicon is completed simultaneously, the comprehensive reutilization of essential element in aluminium scrap silicon is truly realized.According to the present invention
The invention thought, the Silicon-rich slag that above-mentioned steps S1 is separated to has been carried out silicon from efficiently separating in waste material, its follow-up tool
Body application, such as, the higher Silicon-rich slag of gained dioxide-containing silica after acidleach is utilized as silicon source, by with liquid caustic soda or
Silica dissolution in Silicon-rich slag can be prepared and reclaimed as waterglass, not by the separation method by the reaction of piece alkali
Limitation.Thus, present invention also offers the comprehensive recovering process of another aluminium scrap silicon middle rare earth, aluminium and silicon, including following step
Suddenly：S1, aluminium scrap silicon acidleach obtains pickle liquor and Silicon-rich slag containing rare earth and aluminium；S2, the pickle liquor containing rare earth and aluminium adds heavy
Shallow lake agent obtains double salt of rare earth precipitation and filtrate containing aluminium, and S3, filtrate containing aluminium prepares sodium metaaluminate or aluminum sulfate.
Compared with prior art, on the one hand, The inventive method achieves being completely separated for rare earth and aluminium, greatly improved
The yield and purity of the two, while complete being recovered according to a price for silicon, are truly realized the comprehensive of essential element in aluminium scrap silicon
Close and recycle.On the other hand, method of the invention has alkaline consumption small, and water consume is small, the advantage such as wastewater discharge is small, while also having
There is fixed investment few, production cost is low, the characteristics of easily realizing industrialization production.
Embodiment
Purpose/or scheme of the present invention will be provided in the form of preferred embodiment.To saying for these embodiments
Bright is to be used for the understanding of the present invention, and unrestricted feasible other modes, and these feasible other embodiments can be by this
The practice of invention is learnt.
The present invention is described in further detail below in conjunction with specific embodiment, these embodiments are it is not intended that limit this
Invent scope claimed.
Embodiment 1 to 12 refers to the aluminium scrap silicon containing rare earth carrying out the step of inorganic acid aqueous solution carries out acidleach,
Aluminium scrap silicon main component such as table 1 below containing rare earth：
Embodiment 1
Liquid-solid ratio is 3 after aluminium scrap silicon containing rare earth is sized mixing:1, add aluminium silicon of the 1mol/L HCl treatments containing rare earth and give up
Material, it is 2.5 to control course of reaction pH value, and mechanical agitation (200rad/min) leaches 12h at 10 DEG C, controls reaction end solution
PH=2.0；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Aluminium in pickle liquor containing rare earth and aluminium, rare earth and
The leaching rate (in terms of oxide) of silicon is respectively 66.9%, 85.3% and 3.5%.
Comparative example 1
Liquid-solid ratio is 3 after aluminium scrap silicon containing rare earth is sized mixing:1.Aluminium silicon of the 1mol/L HCl treatments containing rare earth is added to give up
Material, it is 3.0 to control course of reaction pH value, and mechanical agitation (200rad/min) leaches 12h at 10 DEG C, controls reaction end solution
PH=2.8；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Aluminium in pickle liquor containing rare earth and aluminium, rare earth and
The leaching rate (in terms of oxide) of silicon is respectively 60.3%, 77.8% and 3.3%.
Embodiment 2
First the aluminium scrap silicon containing rare earth is crushed before acid-leaching reaction, ground, sized mixing, liquid-solid ratio is 4 after sizing mixing:1.
Aluminium scrap silicon of the 3mol/L HCl treatments containing rare earth is added, it is 2.0, the mechanical agitation at 20 DEG C to control course of reaction pH value
(180rad/min) leaches 8h, controls the pH=1.8 of reaction end solution；It is filtrated to get pickle liquor and richness containing rare earth and aluminium
White residue.The leaching rate (in terms of oxide) of aluminium, rare earth and silicon is respectively 73.6%, 89.2% in pickle liquor containing rare earth and aluminium
With 4.2%.
Embodiment 3
Liquid-solid ratio is 5 after aluminium scrap silicon containing rare earth is sized mixing:1.Aluminium silicon of the 5mol/L HCl treatments containing rare earth is added to give up
Material, it is 1.8 to control course of reaction pH value, and mechanical agitation (220rad/min) leaches 6h at 40 DEG C, controls reaction end solution
PH=1.5；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Aluminium in pickle liquor containing rare earth and aluminium, rare earth and
The leaching rate (in terms of oxide) of silicon is respectively 77.2%, 91.5% and 4.5%.
Embodiment 4
Liquid-solid ratio is 6 after aluminium scrap silicon containing rare earth is sized mixing:1.Aluminium silicon of the 7mol/L HCl treatments containing rare earth is added to give up
Material, it is 1.5 to control course of reaction pH value, and mechanical agitation (200rad/min) leaches 4h at 80 DEG C, controls reaction end solution
PH=1.2；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Aluminium in pickle liquor containing rare earth and aluminium, rare earth and
The leaching rate (in terms of oxide) of silicon is respectively 82.1%, 93.6% and 5.5%.
Embodiment 5
Liquid-solid ratio is 5 after aluminium scrap silicon containing rare earth is sized mixing:1.Add aluminium silicon of the 9.5mol/L HCl treatments containing rare earth
Waste material, it is 1.5 to control course of reaction pH value, and mechanical agitation (240rad/min) leaches 4h at 25 DEG C, and control reaction end is molten
The pH=1.2 of liquid；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Aluminium, rare earth in pickle liquor containing rare earth and aluminium
Leaching rate (in terms of oxide) with silicon is respectively 80.7%, 92.1% and 5.0%.
Embodiment 6
Aluminium scrap silicon containing rare earth is sized mixing with Silicon-rich wash heat water, and (liquid-solid ratio is 2.5:1).Add at 9.5mol/L hydrochloric acid
The aluminium scrap silicon containing rare earth is managed, it is 1.0 to control course of reaction pH value, mechanical agitation (200rad/min) leaches 4h at 25 DEG C,
Control the pH=0.8 of reaction end solution；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Silicon-rich slag water adverse current
Wash 2 (liquid-solid ratioes 3:1).Leaching rate (in terms of the oxide) difference of aluminium, rare earth and silicon in pickle liquor containing rare earth and aluminium
For 85.8%, 95.9% and 5.8%.
Embodiment 7
Liquid-solid ratio is 5 after aluminium scrap silicon containing rare earth is sized mixing:1.Aluminium silicon of the 12mol/L HCl treatments containing rare earth is added to give up
Material, it is 0.8 to control course of reaction pH value, and mechanical agitation (150rad/min) leaches 4h at 25 DEG C, controls reaction end solution
PH=0.5；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Aluminium in pickle liquor containing rare earth and aluminium, rare earth and
The leaching rate (in terms of oxide) of silicon is respectively 86.7%, 97.5% and 5.9%.
Embodiment 8
Liquid-solid ratio is 4 after aluminium scrap silicon containing rare earth is sized mixing:1.Aluminium silicon of the 10mol/L HCl treatments containing rare earth is added to give up
Material, it is 0.1 to control course of reaction pH value, and mechanical agitation (180rad/min) leaches 4h at 25 DEG C, controls reaction end solution
PH=0.1；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Aluminium in pickle liquor containing rare earth and aluminium, rare earth and
The leaching rate (in terms of oxide) of silicon is respectively 86.9%, 97.6% and 8.2%.
Embodiment 9
Liquid-solid ratio is 4 after aluminium scrap silicon containing rare earth is sized mixing:1.Add aluminium scrap silicon of the HCl treatment containing rare earth, hydrochloric acid
In hydrionic concentration be 6mol/L, control course of reaction pH value be 2.5, the dump leaching 72h at 25 DEG C, control reaction end solution
PH=2.0；It is filtrated to get pickle liquor and Silicon-rich slag.The leaching rate of aluminium, rare earth and silicon in pickle liquor (in terms of oxide)
Respectively 69.4%, 88.2% and 3.2%.
Embodiment 10
Liquid-solid ratio is 5 after aluminium scrap silicon containing rare earth is sized mixing:1.Add aluminium scrap silicon of the HCl treatment containing rare earth, hydrochloric acid
In hydrionic concentration be 8mol/L, control course of reaction pH value be 1.8, the dump leaching 24h at 25 DEG C, control reaction end solution
PH=1.5；It is filtrated to get pickle liquor and Silicon-rich slag.The leaching rate of aluminium, rare earth and silicon in pickle liquor (in terms of oxide)
Respectively 67.7%, 84.6% and 4.0%.
Embodiment 11
Liquid-solid ratio is 5 after aluminium scrap silicon containing rare earth is sized mixing:1.Aluminium silicon of the 6mol/L nitric acid treatments containing rare earth is added to give up
Material, it is 1.5 to control course of reaction pH value, and mechanical agitation (180rad/min) leaches 6h at 30 DEG C, controls reaction end solution
PH=1.2；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Aluminium in pickle liquor containing rare earth and aluminium, rare earth and
The leaching rate (in terms of oxide) of silicon is respectively 85.2%, 96.7% and 7.2%.
Embodiment 12
Liquid-solid ratio is 4 after aluminium scrap silicon containing rare earth is sized mixing:1.Add aluminium silicon of the 8mol/L sulfuric acid acid treatment containing rare earth
Waste material, it is 1.2 to control course of reaction pH value, and mechanical agitation (200rad/min) leaches 4h at 30 DEG C, and control reaction end is molten
The pH=1.0 of liquid；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Aluminium, rare earth in pickle liquor containing rare earth and aluminium
Leaching rate (in terms of oxide) with silicon is respectively 82.6%, 60.4% and 8.1%.
Embodiment 13 refers to another aluminium scrap silicon containing rare earth carrying out the progress acidleach of the inorganic acid aqueous solution
Step, the aluminium scrap silicon main component such as following table containing rare earth：
| Composition | Al2O3 | REO | SiO2 | CaO |
| Content wt% | 22 | 8 | 68 | 0.1 |
Embodiment 13
Liquid-solid ratio is 4 after aluminium scrap silicon containing rare earth is sized mixing:1.Add aluminium silicon of the 9.5mol/L HCl treatments containing rare earth
Waste material, it is 1.8 to control course of reaction pH value, and mechanical agitation (200rad/min) leaches 4h at 30 DEG C, and control reaction end is molten
The pH=1.5 of liquid；It is filtrated to get the pickle liquor containing rare earth and aluminium and Silicon-rich slag.Aluminium, rare earth in pickle liquor containing rare earth and aluminium
Leaching rate (in terms of oxide) with silicon is respectively 98.2%, 99.1% and 1.5%.
Embodiment 14 to 21 refer to by containing rare earth and aluminium pickle liquor add precipitating reagent obtain double salt of rare earth precipitation and
The step of filtrate containing aluminium：
Embodiment 14
The pickle liquor obtained using in embodiment 6 adds sodium sulphate as precipitating reagent, precipitating reagent is with containing rare earth and aluminium as raw material
Pickle liquor Rare Earth Ion mol ratio be 1:1.Precipitation reaction continues 4h at a temperature of 10 DEG C.Al and REO during this
Rate of deposition is respectively 0.1% and 96.8%.
Embodiment 15
The pickle liquor obtained using in embodiment 6 adds sodium sulphate as precipitating reagent, precipitating reagent is with containing rare earth and aluminium as raw material
Pickle liquor Rare Earth Ion mol ratio be 2:1.Precipitation reaction continues 3h at a temperature of 20 DEG C.Al and REO during this
Rate of deposition is respectively 0.12% and 97.2%.
Embodiment 16
The pickle liquor obtained using in embodiment 6 adds sodium sulphate as precipitating reagent, precipitating reagent is with containing rare earth and aluminium as raw material
Pickle liquor Rare Earth Ion mol ratio be 3:1.Precipitation reaction continues 2h at a temperature of 30 DEG C.Al and REO during this
Rate of deposition is respectively 0.15% and 99.5%.
Comparative example 2
The pickle liquor obtained using in embodiment 6 adds sodium sulphate as precipitating reagent, precipitating reagent is with containing rare earth and aluminium as raw material
Pickle liquor Rare Earth Ion mol ratio be 2:1.Precipitation reaction continues 2h at a temperature of 30 DEG C.Al and REO during this
Rate of deposition is respectively 0.11% and 97.1%.
Embodiment 17
The pickle liquor obtained using in embodiment 6 adds sodium sulphate as precipitating reagent, precipitating reagent is with containing rare earth and aluminium as raw material
Pickle liquor Rare Earth Ion mol ratio be 4:1.Precipitation reaction continues 2h at a temperature of 40 DEG C.Al and REO during this
Rate of deposition is respectively 0.18% and 99.6%.
Embodiment 18
The pickle liquor obtained using in embodiment 6 adds sodium sulphate as precipitating reagent, precipitating reagent is with containing rare earth and aluminium as raw material
Pickle liquor Rare Earth Ion mol ratio be 5:1.Precipitation reaction continues 1h at a temperature of 50 DEG C.Al and REO during this
Rate of deposition is respectively 0.2% and 99.7%.
Embodiment 19
The pickle liquor obtained using in embodiment 6 adds sodium sulphate as precipitating reagent, precipitating reagent is with containing rare earth and aluminium as raw material
Pickle liquor Rare Earth Ion mol ratio be 3:1.Precipitation reaction continues 0.5h at a temperature of 60 DEG C.Al and REO during this
Rate of deposition be respectively 0.14% and 99.7%.
Embodiment 20
The pickle liquor obtained using in embodiment 6 adds ammonium sulfate as precipitating reagent, precipitating reagent is with containing rare earth and aluminium as raw material
Pickle liquor Rare Earth Ion mol ratio be 2:1.Precipitation reaction continues 3h at a temperature of 20 DEG C.Al and REO during this
Rate of deposition is respectively 0.11% and 97.1%.
Embodiment 21
The pickle liquor obtained using in embodiment 6 adds potassium sulfate as precipitating reagent, precipitating reagent is with containing rare earth and aluminium as raw material
Pickle liquor Rare Earth Ion mol ratio be 3:1.Precipitation reaction continues 2h at a temperature of 30 DEG C.Al and REO during this
Rate of deposition is respectively 0.16% and 99.4%.
Embodiment 22 to 26 refer to by double salt of rare earth precipitation with aqueous slkali reaction after filter, obtain rare earth hydrate and
The step of waste liquid：
Embodiment 22
Reacted with the double salt of rare earth precipitation obtained in embodiment 16 with aqueous slkali, hydroxyl ion and double salt of rare earth in aqueous slkali
The mol ratio of middle rare earth atom is 3:1；Slurry liquid-solid ratio 2:1, reaction continues 1 hour at a temperature of 100 DEG C.REO during this
Conversion ratio be 95.6%.
Embodiment 23
Reacted with the double salt of rare earth precipitation obtained in embodiment 16 with aqueous slkali, hydroxyl ion and double salt of rare earth in aqueous slkali
The mol ratio of middle rare earth atom is 4:1；Slurry liquid-solid ratio 3:1, reaction continues 4 hours at a temperature of 95 DEG C.REO during this
Conversion ratio is 99.8%.
Embodiment 24
Reacted with the double salt of rare earth precipitation obtained in embodiment 16 with aqueous slkali, hydroxyl ion and double salt of rare earth in aqueous slkali
The mol ratio of middle rare earth atom is 5:1；Slurry liquid-solid ratio 3:1, reaction continues 3 hours at a temperature of 90 DEG C.REO during this
Conversion ratio is 99.4%.
Embodiment 25
Reacted with the double salt of rare earth precipitation obtained in embodiment 16 with aqueous slkali, hydroxyl ion and double salt of rare earth in aqueous slkali
The mol ratio of middle rare earth atom is 5:1；Slurry liquid-solid ratio 4:1, reaction continues 5 hours at a temperature of 80 DEG C.REO during this
Conversion ratio is 99.7%.
Embodiment 26
Reacted with the double salt of rare earth precipitation obtained in embodiment 16 with aqueous slkali, hydroxyl ion and double salt of rare earth in aqueous slkali
The mol ratio of middle rare earth atom is 4:1；Slurry liquid-solid ratio 3:1, reaction continues 4 hours at a temperature of 50 DEG C.REO during this
Conversion ratio is 97.4%.
Embodiment 27 to 32 refers to the step of filtrate containing aluminium prepares the precipitation of aluminium hydroxide by alkali precipitation：
Embodiment 27
Filtrate containing aluminium that precipitating reagent obtains is added as feed liquid using pickle liquor of the embodiment 16 containing rare earth and aluminium, to filtrate containing aluminium
Middle addition sodium hydroxide solution carries out precipitation reaction, and reaction is carried out under agitation；The precipitation reaction is at a temperature of 60 DEG C
Continue 0.5h, the pH value of reaction end is 4.5；The precipitation of aluminium hydroxide is obtained, Al rates of deposition are 99.1% during this.
Embodiment 28
Filtrate containing aluminium that precipitating reagent obtains is added as feed liquid using pickle liquor of the embodiment 16 containing rare earth and aluminium, to filtrate containing aluminium
Middle addition sodium hydroxide solution carries out precipitation reaction, and reaction is carried out under agitation；The precipitation reaction is at a temperature of 40 DEG C
Continue 2h, the pH value of reaction end is 5.0；The precipitation of aluminium hydroxide is obtained, Al rates of deposition are 99.7% during this.
Comparative example 3
Filtrate containing aluminium that precipitating reagent obtains is added as feed liquid using pickle liquor of the embodiment 16 containing rare earth and aluminium, to filtrate containing aluminium
Middle addition sodium hydroxide solution carries out precipitation reaction, and reaction is carried out under agitation；The precipitation reaction is at a temperature of 30 DEG C
Continue 2h, the pH value of reaction end is 4.0；The precipitation of aluminium hydroxide is obtained, Al rates of deposition are 97.8% during this.
Embodiment 29
Filtrate containing aluminium that precipitating reagent obtains is added as feed liquid using pickle liquor of the embodiment 16 containing rare earth and aluminium, to filtrate containing aluminium
Middle addition sodium hydroxide solution carries out precipitation reaction, and reaction is carried out under agitation；The precipitation reaction is at a temperature of 30 DEG C
Continue 3h, the pH value of reaction end is 7.0；The precipitation of aluminium hydroxide is obtained, Al rates of deposition are 99.9% during this.
Embodiment 30
Filtrate containing aluminium that precipitating reagent obtains is added as feed liquid using pickle liquor of the embodiment 16 containing rare earth and aluminium, to filtrate containing aluminium
Middle addition sodium hydroxide solution carries out precipitation reaction, and reaction is carried out under agitation；The precipitation reaction is at a temperature of 10 DEG C
Continue 4h, the pH value of reaction end is 9.0；The precipitation of aluminium hydroxide is obtained, Al rates of deposition are 99.8% during this.
Embodiment 31
Filtrate containing aluminium that precipitating reagent obtains is added as feed liquid using pickle liquor of the embodiment 16 containing rare earth and aluminium, to filtrate containing aluminium
Middle addition sodium bicarbonate solution carries out precipitation reaction, and reaction is carried out under agitation；The precipitation reaction is at a temperature of 20 DEG C
Continue 2h, the pH value of reaction end is 7.0；The precipitation of aluminium hydroxide is obtained, Al rates of deposition are 99.5% during this.
Embodiment 32
Filtrate containing aluminium that precipitating reagent obtains is added as feed liquid using pickle liquor of the embodiment 16 containing rare earth and aluminium, to filtrate containing aluminium
Middle addition ammonia spirit carries out precipitation reaction, and reaction is carried out under agitation；The precipitation reaction continues at a temperature of 30 DEG C
3h, the pH value of reaction end is 5.0；The precipitation of aluminium hydroxide is obtained, Al rates of deposition are 99.3% during this.
The precipitation that embodiment 33 to 36 refers to aluminium hydroxide passes through the step of alkali transformation of ownership is for sodium metaaluminate：
Embodiment 33
The precipitation for the aluminium hydroxide that embodiment 28 is obtained is reacted with sodium hydrate aqueous solution, is filtrated to get after reaction partially
Sodium aluminate solution and aluminium white residue；In the alkali is gone to step, mole of aluminium atom in the precipitation of sodium hydroxide and aluminium hydroxide
Than for 1:1, reaction continues 0.5h at a temperature of 20 DEG C, and Al conversion ratios are 65.6% during this.
Embodiment 34
The precipitation for the aluminium hydroxide that embodiment 28 is obtained is reacted with sodium hydrate aqueous solution, is filtrated to get after reaction partially
Sodium aluminate solution and aluminium white residue；In the alkali is gone to step, mole of aluminium atom in the precipitation of sodium hydroxide and aluminium hydroxide
Than for 1.5:1, reaction continues 1h at a temperature of 50 DEG C, and Al conversion ratios are 78.1% during this.
Embodiment 35
The precipitation for the aluminium hydroxide that embodiment 28 is obtained is reacted with sodium hydrate aqueous solution, is filtrated to get after reaction partially
Sodium aluminate solution and aluminium white residue；In the alkali is gone to step, mole of aluminium atom in the precipitation of sodium hydroxide and aluminium hydroxide
Than for 2:1, reaction continues 4h at a temperature of 80 DEG C, and Al conversion ratios are 92.2% during this.
Embodiment 36
The precipitation for the aluminium hydroxide that embodiment 28 is obtained is reacted with sodium hydrate aqueous solution, is filtrated to get after reaction partially
Sodium aluminate solution and aluminium white residue；In the alkali is gone to step, mole of aluminium atom in the precipitation of sodium hydroxide and aluminium hydroxide
Than for 3:1, reaction continues 8h at a temperature of 120 DEG C, and Al conversion ratios are 89.5% during this.
The step of precipitation that embodiment 37 to 41 refers to aluminium hydroxide prepares aluminum sulfate by sulfuric acid dissolution：
Embodiment 37
The precipitation for the aluminium hydroxide that embodiment 29 is obtained obtains aluminum sulfate solution with sulfuric acid reaction.The aluminum sulfate of preparation
In solution, concentration is calculated as 70g/L with aluminum oxide, and pH value is 2.5.
Embodiment 38
The precipitation for the aluminium hydroxide that embodiment 28 is obtained obtains aluminum sulfate solution with sulfuric acid reaction.The aluminum sulfate of preparation
In solution, concentration is calculated as 85g/L with aluminum oxide, and pH value is 2.5.
Embodiment 39
The precipitation for the aluminium hydroxide that embodiment 28 is obtained obtains aluminum sulfate solution with sulfuric acid reaction.The aluminum sulfate of preparation
In solution, concentration is calculated as 95g/L with aluminum oxide, and pH value is 1.5.
Embodiment 40
The precipitation for the aluminium hydroxide that embodiment 27 is obtained obtains aluminum sulfate solution with sulfuric acid reaction.The aluminum sulfate of preparation
In solution, concentration is calculated as 110g/L with aluminum oxide, and pH value is 1.5.
Embodiment 41
The precipitation for the aluminium hydroxide that embodiment 28 is obtained obtains aluminum sulfate solution with sulfuric acid reaction.The aluminum sulfate of preparation
In solution, concentration is calculated as 85g/L with aluminum oxide, and pH value is 2.5.
Embodiment 42 to 46 refers to Silicon-rich slag and reacted with sodium hydrate aqueous solution or piece alkali, and water is filtrated to get after reaction
The step of glass and waste residue：
Embodiment 42
The Silicon-rich slag that embodiment 6 is obtained is reacted with sodium hydrate aqueous solution or piece alkali, and waterglass is filtrated to get after reaction
And waste residue.Wherein, the mol ratio of silicon atom and sodium hydroxide is 1.6 in Silicon-rich slag:1, reaction pressure 0.9MPa, react 240
Continue 2h at a temperature of DEG C.Conversion ratio of waterglass is 82% during this.
Embodiment 43
The Silicon-rich slag that embodiment 6 is obtained is reacted with sodium hydrate aqueous solution or piece alkali, and waterglass is filtrated to get after reaction
And waste residue.Wherein, the mol ratio of silicon atom and sodium hydroxide is 2 in Silicon-rich slag:1, reaction pressure 0.8MPa, react at 300 DEG C
At a temperature of continue 8h.Conversion ratio of waterglass is 88% during this.
Embodiment 44
The Silicon-rich slag that embodiment 6 is obtained is reacted with sodium hydrate aqueous solution or piece alkali, and waterglass is filtrated to get after reaction
And waste residue.Wherein, the mol ratio of silicon atom and sodium hydroxide is 2.4 in Silicon-rich slag:1, reaction pressure 1.2MPa, react 200
Continue 6h at a temperature of DEG C.Conversion ratio of waterglass is 75% during this.
Embodiment 45
The Silicon-rich slag that embodiment 6 is obtained is reacted with sodium hydrate aqueous solution or piece alkali, and waterglass is filtrated to get after reaction
And waste residue.Wherein, the mol ratio of silicon atom and sodium hydroxide is 3 in Silicon-rich slag:1, reaction pressure 0.5MPa, react at 180 DEG C
At a temperature of continue 10h.Conversion ratio of waterglass is 72% during this.
Embodiment 46
The Silicon-rich slag that embodiment 6 is obtained is reacted with sodium hydrate aqueous solution or piece alkali, and waterglass is filtrated to get after reaction
And waste residue.Wherein, the mol ratio of silicon atom and sodium hydroxide is 4.8 in Silicon-rich slag:1, reaction pressure 1MPa, react at 150 DEG C
At a temperature of continue 8h.Conversion ratio of waterglass is 65% during this.
Embodiment 47 to 50 is referred to when the aluminium scrap silicon main component such as following table containing rare earth, to the aluminium silicon containing rare earth
The step of aluminium in waste material is tentatively reclaimed：
| Composition | Al2O3 | REO | SiO2 | CaO |
| Content wt% | 49 | 7 | 15 | 1 |
Embodiment 47
Aluminium scrap silicon containing rare earth and sodium hydroxide are reacted, the mol ratio of aluminium atom in the sodium hydroxide and precipitation of addition
For 1:1, it is filtrated to get sodium aluminate solution after 0.5h, reaction are reacted at a temperature of 20 DEG C.Conversion ratio of aluminium is (with oxygen during this
Compound meter) it is 30%.
Embodiment 48
Aluminium scrap silicon containing rare earth and sodium hydroxide are reacted, the mol ratio of aluminium atom in the sodium hydroxide and precipitation of addition
For 1.5:1, it is filtrated to get sodium aluminate solution after 1h, reaction are reacted at a temperature of 50 DEG C.Conversion ratio of aluminium is (with oxygen during this
Compound meter) it is 65%.
Embodiment 49
Aluminium scrap silicon containing rare earth and sodium hydroxide are reacted, the mol ratio of aluminium atom in the sodium hydroxide and precipitation of addition
For 2:1, it is filtrated to get sodium aluminate solution after 4h, reaction are reacted at a temperature of 80 DEG C.Conversion ratio of aluminium is (to aoxidize during this
Thing meter) it is 80%.
Embodiment 50
Aluminium scrap silicon containing rare earth and sodium hydroxide are reacted, the mol ratio of aluminium atom in the sodium hydroxide and precipitation of addition
For 3:1, it is filtrated to get sodium aluminate solution after 8h, reaction are reacted at a temperature of 120 DEG C.Conversion ratio of aluminium is (with oxygen during this
Compound meter) it is 78%.
As can be seen from the above description, compared with prior art, on the one hand, The inventive method achieves rare earth
With being completely separated for aluminium, the two yield and purity greatly improved, while being recovered according to a price for silicon is completed, it is real to realize
The comprehensive reutilization of essential element in aluminium scrap silicon.On the other hand, method of the invention has alkaline consumption small, and water consume is small, gives up
The advantage such as water discharge capacity is small, while also having, fixed investment is few, and production cost is low, the characteristics of easily realizing industrialization production.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area
For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (11)
1. the comprehensive recovering process of a kind of aluminium scrap silicon middle rare earth, aluminium and silicon, comprises the following steps：S1, to aluminium scrap silicon acidleach
Obtain the pickle liquor containing rare earth and aluminium and Silicon-rich slag；S2, into the pickle liquor containing rare earth and aluminium, addition precipitating reagent obtains dilute
Native double salt precipitation and filtrate containing aluminium；S3, sodium metaaluminate or aluminum sulfate are prepared with the filtrate containing aluminium.
2. according to the method described in claim 1, wherein, methods described also includes：
S4, waterglass is prepared with the Silicon-rich slag；And/or
S5, by double salt of rare earth precipitation with being filtered after aqueous slkali reaction, obtains rare earth hydrate and waste liquid.
3. method according to claim 1 or 2, wherein, the process conditions of the step S1 are：The temperature for controlling acidleach is
10~80 DEG C, course of reaction pH value is 0.1~2.5, and the endpoint pH of the pickle liquor containing rare earth and aluminium is 0.5~2.0；
Preferably, the acid of the step S1 is selected from one kind of sulfuric acid solution, hydrochloric acid solution or salpeter solution.
4. method according to claim 1 or 2, wherein, the process conditions of the step S2 are：The precipitating reagent with it is described
The mol ratio of pickle liquor Rare Earth Ion containing rare earth and aluminium is 1:1~5:1；Precipitation reaction continues at a temperature of 10~60 DEG C
0.5~4h；
Preferably, the precipitating reagent in the step S2 is selected from ammonium sulfate, ammonium hydrogen sulfate, sodium sulphate, niter cake, potassium sulfate
Or one kind of potassium acid sulfate.
5. method according to claim 4, wherein, the step S3 is：The filtrate containing aluminium passes through alkali precipitation-alkali transformation of ownership
The standby sodium metaaluminate prepares the aluminum sulfate by alkali precipitation-sulfuric acid dissolution；
Preferably, the alkali precipitation step of the step S3 is：Organic basic material is added into the filtrate containing aluminium and/or inorganic
Alkaline matter carries out precipitation reaction, obtains the precipitation of aluminium hydroxide；
It is highly preferred that the precipitation reaction continues 0.5~4h at a temperature of 10~60 DEG C, the pH value of reaction end for 4.5~
9.0。
6. method according to claim 5, wherein, the alkali that the alkali precipitation-alkali of the step S3 turns go to step for：Will
The precipitation of the aluminium hydroxide is reacted with sodium hydroxide solution or piece alkali, and the sodium metaaluminate and aluminium silicon are filtrated to get after reaction
Slag；The sulfuric acid dissolution step of the step S3 is：The precipitation of the aluminium hydroxide and sulfuric acid reaction are obtained into the aluminum sulfate.
7. method according to claim 6, wherein, in the alkali is gone to step, sodium hydroxide and the aluminium hydroxide
Precipitation in aluminium atom mol ratio be 1:1~3:1；Reaction continues 0.5~8h at a temperature of 20~120 DEG C；In the sulfuric acid
In dissolving step, the obtained aluminum sulfate is aluminum sulfate solution, the concentration of the aluminum sulfate solution is calculated as 70 with aluminum oxide~
110g/L, preferably 85~95g/L, pH value are 1.5~2.5.
8. method according to claim 2, wherein, the step S4 is：The Silicon-rich slag and sodium hydroxide solution or piece
Alkali is reacted, and the waterglass and waste residue are filtrated to get after reaction；
Preferably, the mol ratio of silicon atom and sodium hydroxide is 1.6 in the Silicon-rich slag:1~4.8:1, reaction pressure 0.5~
1.2MPa, reaction continues 2~10 hours at a temperature of 150~300 DEG C.
9. method according to claim 2, wherein, the process conditions of the step S5 are：Hydroxyl in the aqueous slkali
The mol ratio that ion precipitates middle rare earth atom with the double salt of rare earth is 3:1~5:1, reaction continues 1 at a temperature of 50~100 DEG C
~5 hours.
10. method according to claim 1 or 2, wherein, when alumina-silica amount ratio is more than 1 in the aluminium scrap silicon:When 1,
Before the step S1, increase the step S6 tentatively reclaimed to the aluminium in the aluminium scrap silicon, the step tentatively reclaimed
Rapid S6 includes：The aluminium scrap silicon and sodium hydroxide are reacted, separation of solid and liquid obtains sodium aluminate solution and the aluminium silicon containing rare earth
Slag；
Preferably, the mol ratio of sodium hydroxide and aluminium atom in aluminium scrap silicon is 1:1~3:1, react at a temperature of 20~120 DEG C
Continue 0.5~8h.
11. method according to claim 2, wherein, the precipitating reagent in the step S2 is sodium sulphate or potassium sulfate,
The step S5 includes：
By double salt of rare earth precipitation with being filtered after sodium hydroxide or potassium hydroxide solution reaction, rare earth hydrate and sulfuric acid are obtained
Sodium solution or potassium sulfate solution；
The metabisulfite solution or potassium sulfate solution concentration and recovery are returned into the step S2 to use as the precipitating reagent.
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| CN112981123A (en) * | 2021-02-09 | 2021-06-18 | 昆明理工大学 | Method for recovering rare earth elements by using low-purity silicon and rare earth oxide-containing material |
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| CN111807400A (en) * | 2020-07-17 | 2020-10-23 | 斯瑞尔环境科技股份有限公司 | Method for preparing polyaluminium chloride and water glass by using FCC (fluid catalytic cracking) waste catalyst |
| CN112680605A (en) * | 2020-12-11 | 2021-04-20 | 江西理工大学 | Method for synchronously recovering rare earth in leaching mother liquor by utilizing cascade precipitation process |
| CN112981123A (en) * | 2021-02-09 | 2021-06-18 | 昆明理工大学 | Method for recovering rare earth elements by using low-purity silicon and rare earth oxide-containing material |
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