CN106032285A - Method for recovering alumina - Google Patents
Method for recovering alumina Download PDFInfo
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- CN106032285A CN106032285A CN201510112638.9A CN201510112638A CN106032285A CN 106032285 A CN106032285 A CN 106032285A CN 201510112638 A CN201510112638 A CN 201510112638A CN 106032285 A CN106032285 A CN 106032285A
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Abstract
The invention discloses a method for recovering alumina. The method comprises: dissolving out industrial waste containing aluminum and / or associated ore containing aluminum in a solution containing alcohol-alkali; and conducting washing, silicon impurity removal, crystallization treatment and roasting treatment to obtain alumina. Compared with the existing alumina recovery method, the alumina recovery method of the present invention has higher recovery rate and lower energy consumption.
Description
Technical field
The present invention relates to the recovery method of a kind of aluminium oxide.
Background technology
China's bauxite resource is the shortest, and China maintains the world about with the resource reserve accounting for the world 3%
The alumina producing amount of 30%, resource consumption is very serious, ensures that the time limit was less than 10 years；It addition, it is excellent
The most extremely shortage of the bauxite resource of matter, alumina/silica mass ratio (A/S) is low product in 4-6
Ore deposit, position accounts for the 60% of gross reserves.Therefore, China payes attention to especially from containing aluminum i ndustry waste residue with containing aluminum associated minerals
Reclaim the technical research of aluminium oxide.
At present China from containing aluminum i ndustry waste residue or containing aluminum half rawore reclaim the method for aluminium oxide and be broadly divided into
Alkaline process and acid system, wherein alkaline process has pyrogenic process and wet method, and acid system has ammonium sulfate method and hydrochloric acid method.
Alkaline process
Alkaline process is with reference to process for making alumina (being produced by bauxite), improves a little.Pyrogenic process
With the roasting method in wet method respectively corresponding alumina technology and Bayer process.The substantially technique of pyrogenic process is by containing aluminum
Waste residue or associated minerals high-temperature roasting, make Al activate, and other impurity elements solidify, then fired slags alkali
Al is leached by liquid, and recrystallization obtains Al (OH)3, by Al (OH)3Al is obtained after roasting2O3.Wet method base
Originally being that high-concentration alkali liquor leaches, then crystallization obtains crude sodium aluminate/potassium, then is dissolved in by crude sodium aluminate/potassium
In sig water, recrystallization after remove impurity, obtain Al (OH)3, by Al (OH)3Al is obtained after roasting2O3。
Containing substantial amounts of Si in general Aluminiferous waste slag or associated minerals, and Al and Si has one in aqueous slkali
Fixed dissolubility, therefore, the separation of impurity Si is alkali method process design focal point.In pyrogenic process, due to Si
It is calcined solidification, so the separation rate of Al and Si is that comparison is high in pyrogenic process, therefore, has a large amount of patent
The method is used to be used for alum recovery, such as CN201110117710.9.But, due to the sintering temperature of roasting method
Spending higher, energy consumption is 2-4 times of Bayer process, the most economical in aluminum oxide industry, the most gradually by
Eliminate.And Al content is generally significantly less than bauxite in Aluminiferous waste slag and associated minerals, therefore, pyrogenic process is used
Process Aluminiferous waste slag or associated minerals, it is also difficult to economical.
Bayer process is the prevailing technology of current alumina producing, but is to be limited by separation Si impurity equally,
It is only applicable to the higher mineral of A/S, because Si and Al can form more stable insoluble matter in alkali liquor,
Except Si can cause Al to lose, and substantially remove Si and can lose equimolar Al.In order to avoid this
The situation of kind, has document and patent to use twice crystallization to the Si content reducing in alkali liquor, removes Si to reduce
The Al loss of process, i.e. hydrometallurgic recovery aluminium oxide, such as CN201010565571.1 and
CN200810102216.3.But, in two sections of crystallizations, the concentration of alkali liquor differs greatly, and alkali liquor in wet method
Being to recycle, the most each circulation is directed to dilution and the evaporation of alkali liquor, and energy consumption is very big, substantially
Suitable with roasting method；And the alkali concn of high-alkali part is the highest, often leads to evaporation equipment and high-alkali part
The seriously corroded of leaching equipment.
Therefore, no matter pyrogenic process or wet method in alkaline process, due to energy consumption and the problem of equipment corrosion, it is difficult to big
The application of scope.
Acid system
Si is the major impurity of Aluminiferous waste slag or associated minerals, and Si is the most insoluble, it addition,
In general Aluminiferous waste slag or half rawore, Fe content is the most fewer, so, there are document and patent to use acid system
Reclaiming aluminium oxide, acid system is divided into ammonium sulfate method and hydrochloric acid method.
The general step of ammonium sulfate method is first to allocate into ammonium sulfate in Aluminiferous waste slag or associated minerals to carry out roasting,
Then fired slags leaches the solution obtaining sulfur acid aluminum ammonium, and this solution obtains essence by re-dissolved after crystallization
The aluminum ammonium sulfate solution of system, is then passed through ammonia in solution and obtains Al (OH)3And ammonium sulfate.Will
Al(OH)3Al is obtained after roasting2O3；Ammonium sulfate, after evaporation, continues cycling through use.Relevant is special
Profit is such as CN200910187282.x and CN200710118679.4 etc..
The drawback that the method exists has: when 1, reclaiming ammonium sulfate, water evaporates amount is big；2, in course of reaction
Ammonia loss amount is big, needs timing to mend ammonia；3, the response rate of aluminum is low.
Leaching Aluminiferous waste slag or associated minerals with hydrochloric acid solution, the solution crystallization of formation obtains AlCl3Solid,
Solid is fired obtains hydrochloric acid and thick aluminium oxide, hydrochloric acid reuse, the process step of thick aluminium oxide and Bayer process
Basic simlarity alkali crystallizes after leaching.Relevant patent such as CN201110103782.8 with
CN201010294267.8 etc..
The method relates to acid, alkali simultaneously, during inevitably acid-base neutralization cause acid, alkali loss
Amount is big；It addition, AlCl3During hydrochloric acid is reclaimed in roasting, roaster and subsidiary conduit can be caused seriously
Corrosion, the requirement to material is the highest.
Summary of the invention
It is an object of the invention to provide the recovery method of a kind of aluminium oxide, the method uses wet method dissolution to process
From containing aluminum i ndustry waste residue and/or containing aluminum associated minerals reclaim aluminium oxide, use the solution of containing alcohol alkali as dissolution
The solvent processed, the response rate that improve aluminium oxide the energy consumption reducing in removal process.
To achieve these goals, the present invention provides the recovery method of a kind of aluminium oxide, and the method includes:
A, dissolution process mistake will be carried out containing aluminum i ndustry waste residue and/or containing the solution of aluminum associated minerals containing alcohol alkali
Filter, obtains filtrate and the filtering residue containing aluminum；The alcoholic solution that solution is alkali metal containing alkoxide of described containing alcohol alkali or
The solution of the alcohol and water of alkali metal containing alkoxide；
B, the aqueous solution of the filtering residue alkali of gained in step a is washed and filters, obtain thick rich aluminum
Liquid and slag；
C, the thick rich aluminum liquid of gained in step b is carried out desiliconization remove impurity process, obtain the rich aluminum liquid of essence and silicon
Slag；
D, the rich aluminum liquid of essence of gained in step c is carried out crystallization treatment, obtain crystalline mother solution and hydroxide
Aluminum；
E, the aluminium hydroxide of gained in step d is carried out calcination process, obtain aluminium oxide.
Preferably, wherein, described in step a containing aluminum i ndustry waste residue and/or containing aluminum associated minerals aluminium oxide/
The mass ratio of silicon oxide is 0.6～1.5.Described containing aluminum i ndustry waste residue selected from flyash, red mud, coal gasification
At least one in lime-ash, aluminum ash, FCC poising agent and gangue, described containing aluminum associated minerals selected from kaolinite
At least one in soil, clay and dawsonite.
Preferably, wherein, the alcohol described in the solution of containing alcohol alkali described in step a is selected from the one of C1-C4
At least one in the polyhydric alcohol of unit's alcohol and C2-C4；Described alkali metal alcoholates is selected from C1-C4 monohydric alcohol
Alkali metal alcoholates and at least one hydroxyl hydrogen atom of C2-C4 polyhydric alcohol replaced institute by alkali metal atom
At least one in the alkoxide obtained.
Preferably, wherein, the alcohol described in the solution of containing alcohol alkali described in step a is methanol and/or ethanol,
At least one in Feldalat NM, Feldalat KM, Sodium ethylate and potassium ethoxide of described alcohol alkali.
Preferably, wherein, the containing alcohol alkali alcosol described in step a is by alkali metal oxide or alkali gold
Belong to hydroxide and react prepared with alcohol, or by alkali metal oxide or alkali metal hydroxide and alcohol and water
Mixed liquor reaction prepares.
Preferably, wherein, the condition that dissolution described in step a processes includes: the temperature that dissolution processes is
160-300 DEG C, the time that dissolution processes is 15-300 minute, the volume of the solution of described containing alcohol alkali and institute
State containing aluminum i ndustry waste residue and/or the ratio of gross mass containing aluminum associated minerals be 4-10 liter/kilogram, described containing alcohol alkali
Solution in alkali-metal total concentration be that 1-12 mol/L and the water ratio with the volume of alcohol is less than 3:7.
Preferably, wherein, the condition that dissolution described in step a processes includes: the temperature that dissolution processes is
210-260 DEG C, the time that dissolution processes is 90-150 minute, the volume of the solution of described containing alcohol alkali and institute
State containing aluminum i ndustry waste residue and/or the ratio of gross mass containing aluminum associated minerals be 5-8 liter/kilogram, described containing alcohol alkali
Solution in alkali-metal total concentration be that 2-6 mol/L and the water ratio with the volume of alcohol is less than 1:4.
Preferably, wherein, the method also includes: using the filtrate of gained in step a as described containing alcohol alkali
Solution at least some of reuse (return) to described dissolution process in.
Preferably, wherein, the method also includes: carry out described after adding solid silicea in described filtrate again
Reuse, or after directly adding solid silicea in the solution of described containing alcohol alkali, then carry out described dissolution process.
Preferably, wherein, the aqueous solution of alkali described in step b is sodium hydroxide and/or potassium hydroxide
Aqueous solution.
Preferably, wherein, described in step b, the condition of washing includes: wash temperature is 40-80 DEG C,
Wash time is 10-40 minute；In terms of the quality of oxide, in the aqueous solution of described alkali, the concentration of alkali is
90-130 grams per liter；The volume of the aqueous solution of described alkali is 1.5-3 liter/thousand with the mass ratio of described filtering residue
Gram.
Preferably, wherein, the method also includes: use solid silicea to described thick rich aluminum liquid in step c
Carry out described desiliconization remove impurity to process.
Preferably, wherein, described solid silicea is oxide and/or the hydroxide of calcic；Institute in step a
The addition stating solid silicea is described 1-5 mass % containing aluminum i ndustry waste residue and/or containing aluminum associated minerals quality.
Preferably, wherein, the condition of crystallization treatment described in step d is: the temperature of crystallization treatment is
30-50 DEG C, the time of crystallization treatment is 60-120 hour, the concentration of alkali in essence richness aluminum liquid during crystallization treatment
For 70-100 grams per liter, crystal seed coefficient is 1.5-2.
Preferably, wherein, using water-soluble as alkali described in step b of the crystalline mother solution of gained in step d
Being back to use at least partially in described washing of liquid.
The alumina recovery method of the present invention, owing to using dissolution to process containing aluminum i ndustry waste residue and/or containing aluminum
Associated minerals and Two Liquid Phases circulation technology, have higher desilication efficiency, improve the recovery of aluminium oxide
Rate；It addition, use Two Liquid Phases circulation to avoid the alkali concn fluctuation of conventional wet list liquid phase circulation, reduce
Evaporation energy consumption.
Other features and advantages of the present invention will be described in detail in detailed description of the invention part subsequently.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and constitutes the part of description, with
Detailed description below is used for explaining the present invention together, but is not intended that limitation of the present invention.?
In accompanying drawing:
Fig. 1 is the schematic flow sheet of a kind of detailed description of the invention of alumina recovery method of the present invention；
Fig. 2 is the XRD spectra of the used red mud of the embodiment of the present invention；
Fig. 3 is that the method using the present invention reclaims in alumina process, and red mud carries out institute after dissolution process
The XRD spectra (i.e. the XRD figure of embodiment 3 gained filtering residue) of the filtering residue obtained.
Detailed description of the invention
Below in conjunction with accompanying drawing, the detailed description of the invention of the present invention is described in detail.It should be appreciated that
Detailed description of the invention described herein is merely to illustrate and explains the present invention, is not limited to this
Bright.
According to the present invention, described containing aluminum i ndustry waste residue and containing aluminum associated minerals be all those skilled in the art institute ripe
Know, containing aluminum i ndustry waste residue and/or the quality of the alumina/silica containing aluminum associated minerals described in step a
Ratio can be 0.6～1.5, such as, described in step a containing aluminum i ndustry waste residue can be selected from flyash,
At least one in red mud, coal gasification lime-ash, aluminum ash, FCC poising agent and gangue, described containing aluminum companion
Rawore can be at least one in Kaolin, clay and dawsonite.
According to the present invention, the alcoholic solution that solution is alkali metal containing alkoxide of described containing alcohol alkali or alkali metal containing alcohol
The solution of the alcohol and water of salt, refers to the class that the hydroxyl hydrogen atom in alcohol is formed after being replaced by alkali metal atom
Compound, alcohol therein can be monohydric alcohol or polyhydric alcohol, the hydroxyl hydrogen atom being replaced in polyhydric alcohol
Number can be one, it is also possible to for multiple.Containing alcohol alkali alcosol described in step a can be by alkali
Metal-oxide or alkali metal hydroxide react with alcohol and prepare, or can be by alkali metal oxide or alkali gold
Belong to hydroxide and react prepared with the mixed liquor of alcohol and water.Preferably, containing alcohol alkali described in step a is molten
Alcohol described in liquid can be selected from least one in the polyhydric alcohol of the monohydric alcohol of C1-C4 and C2-C4；
Described alkali metal alcoholates can be selected from the alkali metal alcoholates of C1-C4 monohydric alcohol and C2-C4 polyhydric alcohol
At least one hydroxyl hydrogen atom is replaced at least one in the alkoxide of gained by alkali metal atom；The most excellent
Selection of land, the alcohol described in the solution of containing alcohol alkali described in step a can be methanol and/or ethanol, described alcohol
Alkali can be selected from least one in Feldalat NM, Feldalat KM, Sodium ethylate and potassium ethoxide.
The present inventor, according to the low feature of the dissolubility in the solution of containing alcohol of the salt containing aluminum, will contain aluminum
Industrial residue and/or carry out dissolution process in the solution of containing alcohol alkali containing aluminum associated minerals.Described dissolution processes
Refer to destroy containing aluminum i ndustry waste residue and/or the crystal structure containing aluminum associated minerals in the solution of containing alcohol alkali,
Thus be formed at the solution of containing alcohol alkali is difficult to dissolution and be prone in the aqueous solution of alkali dissolution containing aluminum group
Point, reach the alumina recovery effect similar with roasting method but energy consumption during alumina recovery is less than again
Bayer process.Wherein, the condition that dissolution described in step a processes may include that the temperature that dissolution processes is
160-300 DEG C, the time that dissolution processes is 15-300 minute, the volume of the solution of described containing alcohol alkali and institute
Stating the ratio (can be referred to as liquid-solid ratio) containing aluminum i ndustry waste residue and/or the gross mass containing aluminum associated minerals is 4-10
Rise/kilogram, in the solution of described containing alcohol alkali, alkali-metal total concentration is 1-12 mol/L and water and alcohol
The ratio of volume is less than 3:7；The optimum condition that dissolution described in step a processes may include that dissolution processes
Temperature be 210-260 DEG C, dissolution process time be 90-150 minute, the solution of described containing alcohol alkali
Volume and described containing aluminum i ndustry waste residue and/or the ratio of gross mass containing aluminum associated minerals be 5-8 liter/kilogram, institute
State alkali-metal total concentration in the solution of containing alcohol alkali be 2-6 mol/L and water little with the ratio of the volume of alcohol
In 2:8.
According to the present invention, after processing due to dissolution containing aluminum i ndustry waste residue and/or containing the silicon in aluminum associated minerals and
Aluminum is difficult to dissolve in alcoholic solution, and after therefore dissolution processes, the composition of the solution of containing alcohol alkali does not produce the biggest
Change, therefore, it can the filtrate of gained in step a as at least of solution of described containing alcohol alkali
In dividing reuse (recycling) to process to described dissolution.Preferably, can add in described filtrate admittedly
Carry out described reuse after silicea again, or directly can add solid silicea in the solution of described containing alcohol alkali
After, then carry out described dissolution process.Described solid silicea is well-known to those skilled in the art, mainly makees
With being for the resolution of precipitate a small amount of silicon containing component in alkali liquor, can be oxide and/or the hydrogen-oxygen of calcic
Compound；The addition of solid silicea described in step a can be described containing aluminum i ndustry waste residue and/or the association in aluminum
1-5 mass % of ore deposit weight.
According to the present invention, the aqueous solution of alkali described in step b is well-known to those skilled in the art, only
If the aqueous solution that can wash the alkali of Aluminum from filtering residue all can use, can be such as sodium hydroxide and
/ or the aqueous solution of potassium hydroxide.The condition of washing described in step b can be according to routine in prior art
Wash conditions determines, such as, the condition of described washing may include that wash temperature is 40-80 DEG C,
Wash time is 10-40 minute；In terms of the quality of oxide, in the aqueous solution of described alkali, the concentration of alkali is
90-130 grams per liter；The volume of the aqueous solution of described alkali (can also be called for short with the mass ratio of described filtering residue
For liquid-solid ratio) be 1.5-3 liter/kilogram.
It will be appreciated by persons skilled in the art that the method can also include: by gained in step b
In described slag and step c, the white residue of gained is for the preparation of construction material, and the present invention repeats no more.
According to the present invention, it is well-known to those skilled in the art that desiliconization remove impurity described in step c processes,
Can use solid silicea that described thick rich aluminum liquid is carried out described desiliconization remove impurity in step c to process, described solid
It is identical that silicea used with step a can consolidate silicea, makes the siliceous modulus in thick rich aluminum liquid be promoted to 200
Above.Siliceous modulus described herein is well-known to those skilled in the art, for aluminium oxide in solution and two
The mass ratio of silicon oxide.Furthermore it is also possible to the alkali concn reducing the aqueous solution of alkali carries out desiliconization process, can
With reference to desiliconization removal step of the prior art and treatment conditions such as Bayer process, to produce in existing sintering process
Also using during aluminium oxide, the present invention repeats no more.
According to the present invention, crystallization treatment described in step d is well-known to those skilled in the art, permissible
Add aluminium hydroxide crystal seed or be passed through carbon dioxide, it is also possible to directly cooling dilution crystallization, the present invention is preferred
Use and add aluminium hydroxide crystal seed cooling dilution crystallization.Owing to the temperature of washing of the present invention is relatively low, step
Described in rapid d, the condition of crystallization treatment is gentleer, such as, can be: the temperature of crystallization treatment is
30-50 DEG C, the time of crystallization treatment is 60-120 hour, the concentration of alkali in essence richness aluminum liquid during crystallization treatment
For 70-100 grams per liter, crystal seed coefficient is 1.5-2, and wherein said crystal seed coefficient is those skilled in the art institutes
Known to, for adding alumina content and the ratio of alumina content in solution in crystal seed.It addition, this
Bright can also using the crystalline mother solution of gained in step d as alkali described in step b aqueous solution at least one
Part is back to use in described washing, can be adjusted by crystalline mother solution, such as, add alkali before carrying out reuse
Or carry out remove impurity, make up to the standard of the aqueous solution of step b residue washing alkali.
According to the present invention, calcination process described in step e is well-known to those skilled in the art, typically
Sintering temperature can be 950-1100 DEG C, and roasting time can be 15-30 hour, and the present invention repeats no more.
By embodiment, the method for the present invention will be further detailed below, but the most therefore limit
The present invention processed.Instrument and equipment used if no special instructions, is conventional instrument in prior art and sets
Standby.
Following example use red mud, flyash, FCC poising agent and coal gasification lime-ash to test, and relate to
And the chemical element composition of the above-mentioned raw materials arrived uses X-ray fluorescence spectroscopy according to YS/T
575.23-2009 standard method (" bauxitic ore chemical analysis method ", the People's Republic of China (PRC) industry and
Informationization portion writes, and within 2009, December is issued on the 4th) measure, composition is respectively as shown in table 1-4.Red
The XRD figure spectrum of mud is as in figure 2 it is shown, XRD spectra uses Philips XPERT Series X-ray powder
Diffractometer, test condition is: Co K alpha ray (λ=0.17903nm), Fe wave filter, voltage 40kV,
Electric current 30mA, sweep limits is 5-70 °.
The response rate computational methods of aluminium oxide are: the quality of alumina recovery rate=alumina product/and (containing aluminum
Industrial residue and/or the quality containing aluminum associated minerals × containing aluminum i ndustry waste residue and/or containing aluminium oxide in aluminum associated minerals
Content) × 100%.
Embodiment 1-7 provides detailed description of the invention and the result of the alumina recovery method of the present invention.
Embodiment 1
The solution of containing alcohol alkali, wherein, second alcohol and water is allocated by a certain percentage with ethanol, potassium hydroxide and water
The proportional arrangement of 9:1 by volume, potassium hydroxide reaches by making the concentration of potassium in the solution of containing alcohol alkali
The amount of 6mol/L adds.
By in solution broken, that levigate flyash to 80 μm joins deployed containing alcohol alkali,
The volume of solution making containing alcohol alkali is 5 liters/kilogram (liquid-solid ratioes) with the mass ratio of flyash.Then exist
At 210 DEG C, dissolution processes 150min.Dissolution process is filtered after terminating, and obtains filtrate and filtering residue.
Filtrate, by filling into appropriate potassium hydroxide, second alcohol and water, makes each parameter consistent with the solution of containing alcohol alkali
After, it is back to flyash dissolution and processes.The aqueous solution of filtering residue alkali washs, and the aqueous solution of alkali is dense
The potassium hydroxide aqueous solution of degree 130g/L, the volume of the aqueous solution of alkali and the mass ratio of filtering residue be 1.5 liters/
Kilogram (liquid-solid ratio), washs 40min at 40 DEG C.Washing is filtered after terminating, obtain thick rich aluminum liquid and
Slag.
After thick rich aluminum liquid is by adjustment alkali concn to 100g/L, the solid silicea calcium oxide of addition carries out desiliconization and removes
Miscellaneous, make solution siliceous modulus reach 300, then obtain the rich aluminum liquid of essence and white residue.White residue and slag are together
Outer row, uses as construction material.The rich aluminum liquid of essence obtains aluminium hydroxide and crystalline mother solution by crystallization, knot
Brilliant temperature is 50 DEG C, and crystallization time is 70 hours, during crystallization in essence richness aluminum liquid the concentration of alkali be 100 grams/
Rise, crystal seed coefficient 1.5.Crystalline mother solution, by adjusting, after making each parameter consistent with the aqueous solution of alkali, returns
It is back to residue washing；Aluminium hydroxide passes through 950 DEG C, and the roasting of 30 minutes obtains aluminium oxide.
In this embodiment, the response rate of aluminium oxide reaches 62 mass %.
Embodiment 2
Allocate the solution of containing alcohol alkali with Feldalat NM and methanol, Feldalat NM is by making the dense of sodium in the solution of containing alcohol alkali
Degree reaches the amount of 2mol/L and adds.
By in solution broken, that levigate flyash to 80 μm joins deployed containing alcohol alkali,
The volume of solution making containing alcohol alkali is 8 liters/kilogram (liquid-solid ratioes) with the mass ratio of flyash.Then exist
Under the conditions of 260 DEG C, dissolution processes 90min.Dissolution process is filtered after terminating, and obtains filtrate and filtering residue.
Filtrate, by filling into proper amount of methanol sodium and methanol, after making each parameter consistent with the solution of containing alcohol alkali, is returned
It is back to flyash dissolution process.The solution washing of filtering residue alkali, the aqueous solution of alkali is concentration 90g/L
Sodium hydrate aqueous solution, the volume of the aqueous solution of alkali and the mass ratio of filtering residue are 3 liters/kilogram (liquid-solid ratioes),
10min is washed at 80 DEG C.Washing is filtered after terminating, and obtains thick rich aluminum liquid and slag.
After thick rich aluminum liquid is by adjustment alkali concn to 70g/L, adds solid silicea calcium oxide and carry out desiliconization remove impurity,
Make solution siliceous modulus reach 300, then obtain the rich aluminum liquid of essence and white residue.White residue and slag are the most exclusive
And use as construction material.The rich aluminum liquid of essence obtains aluminium hydroxide and crystalline mother solution, crystallization temperature by crystallization
Spending 30 DEG C, crystallization time 60 hours, during crystallization, the alkali concn in essence richness aluminum liquid is 70g/L, crystal seed system
Several 2.Crystalline mother solution, by adjusting, after making each parameter consistent with the aqueous solution of alkali, is back to residue washing；
Aluminium hydroxide passes through 1100 DEG C, and the roasting of 15 minutes obtains aluminium oxide.
In this embodiment, the response rate of aluminium oxide reaches 69 mass %.
Embodiment 3
The solution of containing alcohol alkali, wherein, first alcohol and water 7:3 by volume is allocated with methanol, sodium hydroxide and water
Proportional arrangement, sodium hydroxide is added by the amount making the concentration of sodium in the solution of containing alcohol alkali reach 12mol/L；
And in the solution of containing alcohol alkali, add solid silicea calcium oxide, Gu the addition of silicea is follow-up red mud addition
1 mass %.
By in solution broken, that levigate red mud to 80 μm joins deployed containing alcohol alkali, make
The volume of the solution of containing alcohol alkali and the mass ratio of red mud are 7 liters/kilogram (liquid-solid ratioes).Then at 240 DEG C
Under the conditions of dissolution process 15min.Dissolution process is filtered after terminating, and obtains filtrate and filtering residue.Filtering residue XRD
Shown in collection of illustrative plates Fig. 3.
Filtrate, by filling into proper amount of methanol, sodium hydroxide, water, makes each parameter consistent with the solution of containing alcohol alkali
And after adding solid silicea calcium oxide, be back to red mud dissolution and process.The solution washing of filtering residue alkali, alkali
The sodium hydrate aqueous solution that aqueous solution is concentration 120g/L, the volume of the aqueous solution of alkali and the matter of filtering residue
Amount ratio is 2.5 liters/kilogram (liquid-solid ratioes), washs 30min at 70 DEG C.Washing is filtered after terminating,
To thick rich aluminum liquid and slag.
After thick rich aluminum liquid is by adjustment alkali concn to 90g/L, adds solid silicea calcium oxide and carry out desiliconization remove impurity,
Make solution siliceous modulus reach 300, then obtain the rich aluminum liquid of essence and white residue.White residue and slag are the most exclusive
And use as construction material.The rich aluminum liquid of essence obtains aluminium hydroxide and crystalline mother solution, crystallization temperature by crystallization
Spending 40 DEG C, crystallization time 70 hours, during crystallization, the alkali concn in essence richness aluminum liquid is 90g/L, crystal seed system
Several 1.7, crystalline mother solution, by adjusting, after making each parameter consistent with the aqueous solution of alkali, is back to filtering residue and washes
Wash；Aluminium hydroxide passes through 1000 DEG C, and the roasting of 25 minutes obtains aluminium oxide.
In this embodiment, alumina recovery rate reaches 61 mass %.
Embodiment 4
With ethanol, the solution of sodium hydroxide allotment containing alcohol alkali, sodium hydroxide is by making sodium in the solution of containing alcohol alkali
Concentration reach 4mol/L amount add.
By in solution broken, that levigate red mud to 80 μm joins deployed containing alcohol alkali, make
The volume of the solution of containing alcohol alkali and the mass ratio of red mud are 7 liters/kilogram (liquid-solid ratioes).Then at 240 DEG C
Under the conditions of dissolution process 300min.Dissolution process is filtered after terminating, and obtains filtrate and filtering residue.
Filtrate is by filling into ethanol in proper amount, sodium hydroxide, after making each parameter consistent with the solution of containing alcohol alkali,
After the solid silicea calcium hydroxide of 5 mass % adding follow-up red mud addition, it is back to red mud dissolution and processes.
The solution washing of filtering residue alkali, the aqueous solution of alkali is the sodium hydrate aqueous solution of concentration 120g/L, alkali
The volume of aqueous solution and the mass ratio of filtering residue be 2.5 liters/kilogram (liquid-solid ratioes), wash at 70 DEG C
30min.Washing is filtered after terminating, and obtains thick rich aluminum liquid and slag.
After thick rich aluminum liquid is by adjustment alkali concn to 90g/L, adds solid silicea calcium oxide and carry out desiliconization remove impurity,
Make solution siliceous modulus reach 300, then obtain the rich aluminum liquid of essence and white residue.White residue and slag are the most exclusive
And use as construction material.The rich aluminum liquid of essence obtains aluminium hydroxide and crystalline mother solution, crystallization temperature by crystallization
Spending 40 DEG C, crystallization time 70 hours, during crystallization, the alkali concn in essence richness aluminum liquid is 90g/L, crystal seed system
Several 2.Crystalline mother solution, by adjusting, after making each parameter consistent with the aqueous solution of alkali, is back to residue washing；
Aluminium hydroxide passes through 1000 DEG C, and the roasting of 25 minutes obtains aluminium oxide.
In this embodiment, the response rate of aluminium oxide reaches 65 mass %.
Embodiment 5
With butanol, the solution of sodium hydroxide allotment containing alcohol alkali, sodium hydroxide is by making sodium in the solution of containing alcohol alkali
Concentration reach 4mol/L amount add；And in the solution of containing alcohol alkali, add solid silicea calcium hydroxide,
Gu 3 mass % that the addition of silicea is follow-up FCC poising agent addition.
By solution broken, that levigate FCC poising agent to 80 μm joins deployed containing alcohol alkali
In, making the volume of solution of containing alcohol alkali and the mass ratio of FCC poising agent is 7 liters/kilogram (liquid-solid ratioes).
Then under the conditions of 240 DEG C, dissolution processes 120min.Dissolution process is filtered after terminating, and obtains filtrate and filter
Slag.
Filtrate, by filling into appropriate butanol, sodium hydroxide, makes each parameter consistent with the solution of containing alcohol alkali and adds
After entering solid silicea calcium hydroxide, it is back to FCC poising agent dissolution and processes.The aqueous solution of filtering residue alkali is washed
Washing, the aqueous solution of alkali is the sodium hydrate aqueous solution of concentration 120g/L, the volume of the aqueous solution of alkali and filter
The mass ratio of slag is 2.5 liters/kilogram (liquid-solid ratioes), washs 30min at 70 DEG C.Wash mistake after terminating
Filter, obtains thick rich aluminum liquid and slag.
After thick rich aluminum liquid is by adjustment alkali concn to 90g/L, adds solid silicea sodium oxide and carry out desiliconization remove impurity,
The siliceous modulus making solution reaches 300, then obtains the rich aluminum liquid of essence and white residue.White residue and slag are together arranged
Outward and use as construction material.The rich aluminum liquid of essence obtains aluminium hydroxide and crystalline mother solution by crystallization, crystallization
Temperature 40 DEG C, crystallization time 70 hours, during crystallization, the alkali concn in essence richness aluminum liquid is 90g/L, crystal seed
Coefficient 1.7.Crystalline mother solution, by adjusting, after making each parameter consistent with the aqueous solution of alkali, is back to filtering residue
Washing；Aluminium hydroxide passes through 1000 DEG C, and the roasting of 25 minutes obtains aluminium oxide.
In this embodiment, the response rate of aluminium oxide reaches 50 mass %.
Embodiment 6
With ethanol, the solution of sodium oxide allotment containing alcohol alkali, sodium oxide is by making the dense of sodium in the solution of containing alcohol alkali
Degree reaches the amount of 1mol/L and adds.
By solution broken, that levigate coal gasification lime-ash to 80 μm joins deployed containing alcohol alkali
In, making the volume of solution of containing alcohol alkali and the mass ratio of coal gasification lime-ash is 4 liters/kilogram (liquid-solid ratioes).
Then under the conditions of 160 DEG C, dissolution processes 45min.Dissolution process is filtered after terminating, and obtains filtrate and filter
Slag.
Filtrate, by filling into ethanol in proper amount, sodium oxide, after making each parameter consistent with the solution of containing alcohol alkali, is returned
It is back to coal gasification lime-ash dissolution process.The solution washing of filtering residue alkali, the aqueous solution of alkali is concentration
The sodium hydrate aqueous solution of 120g/L, the volume of the aqueous solution of alkali and the mass ratio of filtering residue are 2.5 liters/kilogram
(liquid-solid ratio), washs 30min at 70 DEG C.Washing is filtered after terminating, and obtains thick rich aluminum liquid and slag.
After thick rich aluminum liquid is by adjustment alkali concn to 90g/L, adds solid silicea calcium oxide and carry out desiliconization remove impurity,
Make solution siliceous modulus reach 300, then obtain the rich aluminum liquid of essence and white residue.White residue and slag are the most exclusive
And use as construction material.The rich aluminum liquid of essence obtains aluminium hydroxide and crystalline mother solution, crystallization temperature by crystallization
Spending 40 DEG C, crystallization time 70 hours, during crystallization, the alkali concn in essence richness aluminum liquid is 90g/L, crystal seed system
Several 1.7.Crystalline mother solution, by adjusting, after making each parameter consistent with the aqueous solution of alkali, is back to filtering residue and washes
Wash；Aluminium hydroxide passes through 1000 DEG C, and the roasting of 25 minutes obtains aluminium oxide.
In this embodiment, the response rate of aluminium oxide reaches 63 mass %.
Embodiment 7
The solution of spent glycol, potassium hydroxide allotment containing alcohol alkali, potassium hydroxide is by the solution making containing alcohol alkali
The concentration of potassium reaches the amount of 4mol/L and adds.
Red mud broken, that levigate mass ratio to 80 μm is 1:1 and mixture of fly ash are added
In the solution of deployed containing alcohol alkali, make volume and red mud and the mixture of fly ash of the solution of containing alcohol alkali
Mass ratio be 10 liters/kilogram (liquid-solid ratioes).Then under the conditions of 300 DEG C, dissolution processes 120min.
Dissolution process is filtered after terminating, and obtains filtrate and filtering residue.
Filtrate is by filling into proper amount of glycol, potassium hydroxide, after making each parameter consistent with the solution of containing alcohol alkali,
It is back to red mud and mixture of fly ash dissolution processes.The solution washing of filtering residue alkali, the aqueous solution of alkali
For the potassium hydroxide aqueous solution of concentration 120g/L, the volume of the aqueous solution of alkali and the mass ratio of filtering residue are 2.5
Rise/kilogram (liquid-solid ratio), at 70 DEG C, wash 30min.Washing is filtered after terminating, and obtains thick rich aluminum liquid
And slag.
After thick rich aluminum liquid is by adjustment alkali concn to 90g/L, adds solid silicea and carry out desiliconization remove impurity, make molten
The siliceous modulus of liquid reaches 300, then obtains the rich aluminum liquid of essence and white residue.White residue and slag are the most exclusive also
Use as construction material.The rich aluminum liquid of essence obtains aluminium hydroxide and crystalline mother solution, crystallization temperature by crystallization
40 DEG C, crystallization time 70 hours, during crystallization, the alkali concn in essence richness aluminum liquid is 90g/L, crystal seed coefficient
1.7.Crystalline mother solution, by adjusting, after making each parameter consistent with the aqueous solution of alkali, is back to residue washing；
Aluminium hydroxide passes through 1000 DEG C, and the roasting of 25 minutes obtains aluminium oxide.
In this embodiment, the response rate of aluminium oxide reaches 58 mass %.
Comparative example 1 provides detailed description of the invention and the result thereof using Bayer process to reclaim aluminium oxide.
With sodium hydroxide, aluminium hydroxide allotment sodium aluminate solution, the alkali concn in solution is made to reach 230g/L
(based on sodium oxide), in solution, the mol ratio of sodium hydroxide and aluminium hydroxide is 3.
Broken, levigate red mud to 80 μm are joined in deployed sodium aluminate solution, makes aluminum
The volume of acid sodium solution and the mass ratio of red mud are 6 liters/kilogram, and addition accounts for 2 mass % red mud quality
Gu silicea calcium oxide, then under the conditions of 240 DEG C, dissolution processes 120min.Dissolution process is filtered after terminating,
Obtain filtrate and filtering residue.
Use pure water filtering residue, and rear liquid will be washed mix with filtrate, make the alkali concn of filtrate drop to
90g/L, and the solid silicea calcium oxide of addition carries out desiliconization remove impurity again, makes the siliceous modulus of filtrate reach 300.
Then filtrate obtains aluminium hydroxide and crystalline mother solution, crystallization temperature 40 DEG C, crystallization time 70 by crystallization
Hour, crystal seed coefficient 2.
Crystalline mother solution, by evaporation, makes alkali concn with after the sodium aluminate solution of exsolution red mud is consistent, returns
It is back to red mud dissolution；Aluminium hydroxide passes through 1000 DEG C, and the roasting of 25 minutes obtains aluminium oxide.
In this comparative example, the response rate of aluminium oxide is 6 mass %.
It can be seen that the method for the present invention and prior art phase from embodiments of the invention and comparative example
Ratio, the response rate of aluminium oxide is high, and destroys containing aluminum i ndustry waste residue and/or containing aluminum associated minerals without roasting
Structure and avoid the wide fluctuations of alkali concn in process in leaching and crystallization process, thus reduce energy
Consumption.
Table 1 is the content (quality %) of the element in the red mud that the embodiment of the present invention is used in terms of oxide.
| Al2O3 | Fe2O3 | SiO2 | Na2O | CaO | TiO2 |
| 21.49 | 22.13 | 18.46 | 10.46 | 6.89 | 3.14 |
Table 2 is the content (quality %) of the element in the flyash that the embodiment of the present invention is used in terms of oxide.
| Al2O3 | SiO2 | CaO | Fe2O3 | TiO2 |
| 30.79 | 37.80 | 9.41 | 2.91 | 1.12 |
Table 3 is the content (matter of the element in the FCC poising agent that the embodiment of the present invention is used in terms of oxide
Amount %).
| Al2O3 | SiO2 | La2O3 | CeO2 | Fe2O3 | NiO |
| 49.80 | 40.05 | 1.34 | 2.81 | 1.44 | 1.16 |
Table 4 is the content (matter of the element in the coal gasification lime-ash that the embodiment of the present invention is used in terms of oxide
Amount %).
| Al2O3 | SiO2 | Fe2O3 | CaO | MgO | TiO2 | K2O |
| 27.90 | 41.00 | 5.71 | 5.81 | 2.05 | 2.07 | 1.01 |
Claims (16)
1. a recovery method for aluminium oxide, the method includes:
A, dissolution process mistake will be carried out containing aluminum i ndustry waste residue and/or containing the solution of aluminum associated minerals containing alcohol alkali
Filter, obtains filtrate and the filtering residue containing aluminum；The alcoholic solution that solution is alkali metal containing alkoxide of described containing alcohol alkali or
The solution of the alcohol and water of alkali metal containing alkoxide；
B, the aqueous solution of the filtering residue alkali of gained in step a is washed and filters, obtain thick rich aluminum
Liquid and slag；
C, the thick rich aluminum liquid of gained in step b is carried out desiliconization remove impurity process, obtain the rich aluminum liquid of essence and silicon
Slag；
D, the rich aluminum liquid of essence of gained in step c is carried out crystallization treatment, obtain crystalline mother solution and hydroxide
Aluminum；
E, the aluminium hydroxide of gained in step d is carried out calcination process, obtain aluminium oxide.
Method the most according to claim 1, wherein, contains aluminum i ndustry waste residue and/or contains described in step a
The mass ratio of the alumina/silica of aluminum associated minerals is 0.6～1.5.
Method the most according to claim 1, wherein, contains aluminum i ndustry waste residue and/or contains described in step a
Aluminum associated minerals are in flyash, red mud, coal gasification lime-ash, aluminum ash, FCC poising agent and gangue
At least one, described is at least one in Kaolin, clay and dawsonite containing aluminum associated minerals.
Method the most according to claim 1, wherein, described in the solution of containing alcohol alkali described in step a
At least one in the polyhydric alcohol of the monohydric alcohol of C1-C4 and C2-C4 of alcohol；Described alkali metal alcohol
Salt is selected from alkali metal alcoholates and at least one hydroxyl hydrogen atom of C2-C4 polyhydric alcohol of C1-C4 monohydric alcohol
At least one in the alkoxide of gained is replaced by alkali metal atom.
Method the most according to claim 1, wherein, described in the solution of containing alcohol alkali described in step a
Alcohol be methanol and/or ethanol, described alcohol alkali is in Feldalat NM, Feldalat KM, Sodium ethylate and potassium ethoxide
At least one.
Method the most according to claim 1, wherein, the containing alcohol alkali alcosol described in step a by
Alkali metal oxide or alkali metal hydroxide react with alcohol and prepare, or by alkali metal oxide or alkali metal
Hydroxide reacts prepared with the mixed liquor of alcohol and water.
Method the most according to claim 1, wherein, the condition that dissolution described in step a processes includes:
The temperature that dissolution processes is 160-300 DEG C, and the time that dissolution processes is 15-300 minute, described containing alcohol alkali
Solution volume with described containing aluminum i ndustry waste residue and/or the ratio of gross mass containing aluminum associated minerals be 4-10 liter/
Kilogram, in the solution of described containing alcohol alkali, alkali-metal total concentration is the body of 1-12 mol/L and water and alcohol
Long-pending ratio is less than 3:7.
Method the most according to claim 7, wherein, the condition that dissolution described in step a processes includes:
The temperature that dissolution processes is 210-260 DEG C, and the time that dissolution processes is 90-150 minute, described containing alcohol alkali
Solution volume with described containing aluminum i ndustry waste residue and/or the ratio of gross mass containing aluminum associated minerals be 5-8 liter/
Kilogram, in the solution of described containing alcohol alkali, alkali-metal total concentration is the volume of 2-6 mol/L and water and alcohol
Ratio less than 1:4.
Method the most according to claim 1, wherein, the method also includes: by gained in step a
Filtrate as described containing alcohol alkali solution be back to use at least partially described dissolution process in.
Method the most according to claim 9, wherein, the method also includes: add in described filtrate
Gu carry out described reuse after silicea again, or after directly adding solid silicea in the solution of described containing alcohol alkali,
Carry out described dissolution process again.
11. methods according to claim 1, wherein, the aqueous solution of alkali described in step b is hydroxide
Sodium and/or the aqueous solution of potassium hydroxide.
12. methods according to claim 1, wherein, described in step b, the condition of washing includes: wash
Washing temperature and be 40-80 DEG C, wash time is 10-40 minute；In terms of the quality of oxide, described alkali
In aqueous solution, the concentration of alkali is 90-130 grams per liter；The volume of the aqueous solution of described alkali and the matter of described filtering residue
The ratio of amount be 1.5-3 liter/kilogram.
13. methods according to claim 1, wherein, the method also includes: use solid in step c
Silicea carries out described desiliconization remove impurity to described thick rich aluminum liquid and processes.
14. according to the method for claim 10 or 13, and wherein, described solid silicea is the oxide of calcic
And/or hydroxide；The addition of solid silicea described in step a is described containing aluminum i ndustry waste residue and/or contain
1-5 mass % of aluminum associated minerals quality.
15. methods according to claim 1, wherein, the condition of crystallization treatment described in step d is:
The temperature of crystallization treatment is 30-50 DEG C, and the time of crystallization treatment is 60-120 hour, essence during crystallization treatment
In rich aluminum liquid, the concentration of alkali is 70-100 grams per liter, and crystal seed coefficient is 1.5-2.
16. methods according to claim 1, wherein, using the crystalline mother solution of gained in step d as step
Described in rapid b, the aqueous solution of alkali is back to use in described washing at least partially.
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| CN112645372A (en) * | 2021-01-19 | 2021-04-13 | 广西化工研究院有限公司 | Method for recycling waste activated alumina regenerant for hydrogen peroxide |
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| CN114717417A (en) * | 2020-12-21 | 2022-07-08 | 青岛惠城环保科技股份有限公司 | Treatment method of heavy metal-containing silicon-aluminum-based waste residue, amorphous silicon-aluminum powder and application thereof |
| CN112645372A (en) * | 2021-01-19 | 2021-04-13 | 广西化工研究院有限公司 | Method for recycling waste activated alumina regenerant for hydrogen peroxide |
| CN112645372B (en) * | 2021-01-19 | 2023-05-05 | 广西化工研究院有限公司 | Method for recycling waste activated alumina regenerant for hydrogen peroxide |
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