CN105886779B - A kind of recycling processing method of chromium-contained aluminum mud - Google Patents
A kind of recycling processing method of chromium-contained aluminum mud Download PDFInfo
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- CN105886779B CN105886779B CN201610403435.XA CN201610403435A CN105886779B CN 105886779 B CN105886779 B CN 105886779B CN 201610403435 A CN201610403435 A CN 201610403435A CN 105886779 B CN105886779 B CN 105886779B
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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
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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
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
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Abstract
The invention discloses a kind of recycling processing method of chromium-contained aluminum mud, including：Step 1, water mixing is added in chromium-contained aluminum mud, is filtered through rising temperature for dissolving, is obtained containing chromium (VI) aqueous solution and containing aluminium (III) filter cake；Step 2, obtain containing chromium (III) aqueous solution through electroreduction containing chromium (VI) aqueous solution；Step 3, handled containing chromium (III) aqueous solution through bipolar membrane electrodialysis, obtain NaOH solution and chromic acid solution；Step 4, the NaOH solution in step 3 is concentrated using membrane distillation, obtains the NaOH solution of clear water and concentration, clear water is back to the water-soluble process in step 1；Step 5, using the filter cake containing aluminium in the NaOH solution dissolving step 1 after concentrating in step 4, temperature reaction, it is separated by filtration to obtain NaAlO2Solution.The present invention has not only handled aluminium mud solid waste, and recycling recycles the chromium and aluminium in solid waste.
Description
Technical field
The present invention relates to chemical industrial waste thing recycling process field, and in particular to a kind of recycling treatment side of chromium-contained aluminum mud
Method.
Background technology
Chromium-contained aluminum mud is caused accessory substance during chromium salt production, and industrial general production 1t sodium dichromates about produce 30
~50kg aluminium mud, contain substantial amounts of aluminium (III) and chromium (VI) in aluminium mud.At present, processing side of the sodium dichromate factory to aluminium mud
Formula：1st, fill；2nd, the relatively advanced manufacturer of technique, it is calcined using by aluminium mud together with chromite, extraction recovery is most of
Chromium, then aluminium slag as discarded object fill, though the method can reclaim most of chromium, also have weak point, 2 still suffered from aluminium slag
~3% or so chromium (VI).Traditional aluminium slag offal treatment mode, large amount of land resources are not only taken up, and it is hidden pollution to be present
Suffer from, the wasting of resources and environmental pollution can be caused.
In recent years, domestic and international researcher has done numerous studies in terms of the chromium-contained aluminum mud comprehensive regulation, clay using aluminium
Tanning extracts and cement, phosphoric acid chemistry neutralisation are except aluminium, high-temperature roasting are except chromium, strong flocculant are except chromium, reducing agent reduction are except chromium etc..But
Process conditions that this kind of method has are harsh, equipment investment is high, have the rate of recovery is low, product quality fluctuation is big, and all unsuitable industry should
With.
Publication No. CN103318934A patent document discloses a kind of method that chromium-contained aluminum mud prepares high-purity aluminate,
Recovery section Cr first6+, then with dissolved aluminum mud, iron removaling, prepare Al (OH)3With Cr (OH)3Mixture and recovery section Cr6+, so
Al (OH) is carried out afterwards3With Cr (OH)3The alkali fusion and Cr of mixture3+, high-purity aluminate is finally prepared.Though the invention technique is simple
It is single, it is easy to industrialization, but other chemical reagent need to be added.
Publication No. CN104805288A patent document discloses a kind of comprehensive utilization chromium-contained aluminum mud recovery chromium and aluminium
Process, aluminium mud are used to produce sodium dichromate product, taken off through being beaten the isolated chromium acid sodium solutions of technique such as washing, electrodialysis
Aluminium mud after chromium processing, dissolved through NaOH solution, repeatedly continuous carbon method obtains high-purity metallurgical-grade aluminum oxide product.
The content of the invention
The invention provides a kind of recycling processing method of chromium-contained aluminum mud, the chromium in chromium-contained aluminum mud and aluminium are reclaimed
Utilize.
A kind of recycling processing method of chromium-contained aluminum mud, including：
Step 1, water mixing is added in chromium-contained aluminum mud, is filtered through rising temperature for dissolving, is obtained containing chromium (VI) aqueous solution and containing aluminium (III)
Filter cake；
Step 2, obtain containing chromium (III) aqueous solution through electroreduction containing chromium (VI) aqueous solution；
Step 3, handled containing chromium (III) aqueous solution through bipolar membrane electrodialysis, obtain NaOH solution and chromic acid solution；
Step 4, the NaOH solution in step 3 is concentrated using membrane distillation, obtains the NaOH solution of clear water and concentration, clearly
Water-soluble process of the Water circulation in step 1；
Step 5, the filter cake containing aluminium in the NaOH solution dissolving step 1 after being concentrated in step 4, temperature reaction, filtering are utilized
Isolated NaAlO2Solution.
The present invention carries out recycling treatment for chromium-contained aluminum mud, not only reduces aluminium mud solid waste, and realizes time of chromium and aluminium
Receive and utilize.
Chromium-contained aluminum mud is that discarded object of power boiler discharge caused by the aluminium stage is removed in chromium salt production, not only land occupation, pollutes ring
Border, and serious waste resource.Such as chromite production sodium dichromate (sodium dichromate), typically often production 1t sodium dichromates can about produce
30~50kg aluminium mud.
Preferably, in step 1, the mass ratio of chromium-contained aluminum mud and water is 1：3~9.
In chromium-contained aluminum mud plus after suitable quantity of water dilution, heat up stirring and dissolving, and the dosage of water is excessive or very few, can all influence
The solute effect of chromium-contained aluminum mud.
In step 1, after chromium-contained aluminum mud and water mixing heating stirring reaction, using suitable quantity of water repeated washing at least more than 3 times,
After washing lotion and reaction product are merged, filtered, obtain containing chromium (VI) aqueous solution and filter cake containing aluminium.
In order to promote dissolving of the chromium-contained aluminum mud in water, it is preferable that be warming up to 60~80 DEG C of stirring and dissolvings.Mixing time according to
Factually depending on the dissolving situation on border, it is defined by the mixed solution for forming homogeneous.
Preferably, in step 1, moisture batch is added in chromium-contained aluminum mud.
When adding water in chromium-contained aluminum mud, it can disposably add, can also add in batches, make the chromium (VI) in aluminium mud molten
Solution is more abundant.
Preferably, the electrode of electroreduction is using graphite electrode, metal Ti electrode, titanium plating ruthenium or titanium plating iridium electricity in step 2
One kind in extremely；Amberplex is separated with electroreduction groove, current density is 40~300A/m2。
Bipolar Membrane is a kind of new ion-exchange composite membranes, (is urged by cation exchange layer (N-type film), interface hydrophilic layer
Change layer) and cation exchange layer (p-type film) be combined.Under DC electric field effect, Bipolar Membrane can be by water decomposition, in film both sides
Obtain H+、OH-.Using this feature, bipolar membrane electrodialysis system that Bipolar Membrane and anion and cation exchange membrane are combined into can be
In the case of not introducing other components, salt is converted into corresponding bronsted lowry acids and bases bronsted lowry.
In order to ensure the efficient progress of bipolar membrane electrodialysis, it is preferable that in step 3, the condition of bipolar membrane electrodialysis is：Matter
The conducting solution that amount fraction is 0.1~5% is pole liquid, 1~40 DEG C of reaction temperature, 200~700A/m of current density2。
Further preferably, in step 3, the condition of bipolar membrane electrodialysis is：Mass fraction is 0.5~4% conducting solution
For pole liquid, 15~35 DEG C of reaction temperature, 300~600A/m of current density2。
Most preferably, in step 3, the condition of bipolar membrane electrodialysis is：The conducting solution that mass fraction is 1.5~3% is pole
Liquid, 25~35 DEG C of reaction temperature, 400~500A/m of current density2。
Membrane distillation process is a kind of thermal drivers process, and separate hot material liquid (heat is surveyed) by hydrophobic porous film surveys with passing through
(cold side), because the vapour pressure that charging is surveyed is higher than the vapour pressure through side, under differential pressure gradients effect, steam molecule is surveyed by heat and passed through
Fenestra is migrated to cold side, condensed, obtains pure component.Membrane distillation can regard the combination of membrane process and still-process as, be a kind of
New high efficient separation technology.
Preferably, in step 4, membrane distillation uses hollow-fibre membrane or laminar film, and membrane material selects polytetrafluoroethylene (PTFE)
(PTFE), at least one of Kynoar (PVDF), polypropylene (PP), polyethylene (PE).
In order that NaOH solution being capable of rapid concentration, it is preferable that in step 4, membrane porosity is 60 used by membrane distillation
~95%, aperture is 0.1~1.0 μm, and thickness is 0.04~0.25mm.
Further preferably, in step 4, membrane distillation uses hollow-fibre membrane, and membrane porosity is 80~90%, aperture 0.2
~0.8 μm, thickness is 0.1~0.2mm.
NaOH solution is concentrated to be reacted with filter cake containing aluminium in step 4, the reaction equation in step 5 is as follows：
Al(OH)3+ NaOH=NaAlO2+2H2O。
When feeding intake, it then follows the stoichiometric proportion shown in above-mentioned reaction equation, NaOH dosage is with filter cake containing aluminium
Calculated on the basis of alumina content.
In order that NaOH concentration matches with the aluminium content in filter cake containing aluminium in NaOH solution, therefore, it is necessary to NaOH
Solution is concentrated into suitable concentration, selects NaOH solution being concentrated into saturation state in the present invention, described saturation state is not
Proper saturation, but allow certain error, close to saturation state.
In order that the reaction of step 5 is smoothed out, it is preferable that in step 5, it is warming up to 90~110 DEG C, stirring reaction 2~
6h。
The present invention is combined processing chromium-contained aluminum mud by electroreduction technology, bipolar membrane electrodialysis technology with film distillation technology,
In the case of not introducing other chemical reagent, the problem of chromium-contained aluminum mud disposal is not only solved, and recycling has recycled aluminium
Aluminium and chromium resource in mud.
Brief description of the drawings
Fig. 1 is the flow chart of the recycling processing method of chromium-contained aluminum mud of the present invention.
Embodiment
The flow of the recycling processing method of chromium-contained aluminum mud provided by the invention is as shown in figure 1, chromium-contained aluminum mud is dissolved in water
Afterwards, filter cake containing aluminium and chromium-containing solution are filtrated to get；Chromium-containing solution is three prices through electroreduction hexavalent chrome reduction, then through double
Pole EDBM obtains NaOH solution and chromic acid solution；NaOH solution is through membrane distillation, the NaOH solution after being concentrated, after concentration
NaOH solution and filter cake containing aluminium reaction, obtain NaAlO2Solution.
Embodiment 1
Caused waste residue during certain chromium salt factory production sodium dichromate, moisture content about 60% (mass fraction), in dry aluminium mud
Mainly contain Al2O3、Cr2O3、Na2CrO4、SiO2And Fe2O3Deng.
(1) it is water-soluble：Water is added in waste residue, and (mass ratio of waste residue and water is 1：3), in 70 DEG C of stirring reaction 1h, water repeatedly
Wash 3 times, chromium (VI) aqueous solution and filter cake containing aluminium must be contained by filtering.
(2) electroreduction：Through electroreduction it is three prices by hexavalent chrome reduction containing chromium (VI) aqueous solution；Electroreduction parameter：Anode
Electrode is Ru-Ir/Ti, and negative electrode is Ti plates, current density 150A/m2, amberplex is added in electrolytic cell, by anode and the moon
Pole separates.
(3) bipolar membrane electrodialysis：Handled at normal temperatures through bipolar membrane electrodialysis containing chromium (III) aqueous solution, obtain NaOH solution
And chromic acid solution；The reaction condition of bipolar membrane electrodialysis：1% metabisulfite solution is pole liquid, and reaction temperature is 30 DEG C, current density
For 500A/m2。
(4) membrane distillation：The NaOH solution that step (3) obtains, to nearly saturation state, obtains clear water and concentration through membrane distillation concentration
NaOH solution, clear water is back to the water-soluble process in step 1.
Membrane distillation uses PTFE hollow-fibre membranes, thickness 0.2mm, and aperture is 0.4 μm, and porosity is more than 80%.
(5) alkali soluble：The filter cake that NaOH solution dissolving step (1) after the concentration that step (4) obtains obtains, is stirred in 100 DEG C
Reaction 4h is mixed, is separated by filtration to obtain NaAlO2Solution, the chemical equation of this step are：Al(OH)3+ NaOH=NaAlO2+
2H2O。
Comparative example 1
Experiment condition is same as Example 1, the difference is that only, during step (1) is water-soluble, the quality of waste residue and water
Than for 1:9, disposable washing, the solute effect of aluminium mud is deteriorated compared with embodiment 1.
Comparative example 2
Experiment condition is same as Example 1, the difference is that only, it is close to reduce bipolar membrane electrodialysis electric current in step (3)
Spend to 400A/m2, the reduction of Bipolar Membrane disposal ability, extend containing chromium (III) aqueous solution processing time.
Comparative example 3
Experiment condition is same as Example 1, the difference is that only, reduces in step (2) electroreduction current density extremely
50A/m2, the reduction of electroreduction ability, extend containing chromium (VI) aqueous solution recovery time.
Embodiment 2
Caused waste residue during certain chromium salt factory production sodium dichromate, moisture content about 60% (mass fraction), dry aluminium mud master
Contain Al2O3、Cr2O3、Na2CrO4、SiO2And Fe2O3Deng.
(1) it is water-soluble：Water is added in waste residue, and (mass ratio of waste residue and water is 1：3), in 70 DEG C of stirring reaction 1h, water repeatedly
Wash 3 times, chromium (VI) aqueous solution and filter cake containing aluminium must be contained by filtering.
(2) electroreduction：Through electroreduction it is three prices by hexavalent chrome reduction containing chromium (VI) aqueous solution；Electroreduction parameter：Anode
Electrode is Ru-Ir/Ti, and negative electrode is Ti plates, current density 150A/m2, amberplex is added in electrolytic cell, by anode and the moon
Pole separates.
(3) bipolar membrane electrodialysis：Handled at normal temperatures through bipolar membrane electrodialysis containing chromium (III) aqueous solution, obtain NaOH solution
And chromic acid solution；The reaction condition of bipolar membrane electrodialysis：1% metabisulfite solution is pole liquid, and reaction temperature is 30 DEG C, current density
For 500A/m2。
(4) membrane distillation：The NaOH solution that step (3) obtains, to nearly saturation state, obtains clear water and concentration through membrane distillation concentration
NaOH solution, clear water is back to the water-soluble process in step 1.Membrane distillation uses PVDF/PTFF composite double layer hollow-fibre membranes,
To strengthen the hydrophobicity of film appearance, thickness 0.2mm, aperture is 0.4 μm, and porosity is more than 80%.
(5) alkali soluble：The filter cake that NaOH solution dissolving step (1) after the concentration that step (4) obtains obtains, is stirred in 100 DEG C
Reaction 4h is mixed, is separated by filtration to obtain NaAlO2Solution.
Embodiment 3
Caused waste residue during certain chromium salt factory production sodium dichromate, moisture content about 60% (mass fraction), dry aluminium mud master
Contain Al2O3、Cr2O3、Na2CrO4、SiO2And Fe2O3Deng.
(1) it is water-soluble：Water is added in waste residue, and (mass ratio of waste residue and water is 1：3), in 60 DEG C of stirring reaction 1h, water repeatedly
Wash 3 times, chromium (VI) aqueous solution and filter cake containing aluminium must be contained by filtering.
(2) electroreduction：Through electroreduction it is three prices by hexavalent chrome reduction containing chromium (VI) aqueous solution；Electroreduction parameter：Anode
Electrode is Ru-Ir/Ti, and negative electrode is Ti plates, current density 150A/m2, amberplex is added in electrolytic cell, by anode and the moon
Pole separates.
(3) bipolar membrane electrodialysis：Handled at normal temperatures through bipolar membrane electrodialysis containing chromium (III) aqueous solution, obtain NaOH solution
And chromic acid solution；The reaction condition of bipolar membrane electrodialysis：1% metabisulfite solution is pole liquid, and reaction temperature is 20 DEG C, current density
For 400A/m2。
(4) membrane distillation：The NaOH solution that step (3) obtains, to nearly saturation state, obtains clear water and concentration through membrane distillation concentration
NaOH solution, clear water is back to the water-soluble process in step 1.Membrane distillation uses PVDF/PTFF composite double layer hollow-fibre membranes,
To strengthen the hydrophobicity of film appearance, thickness 0.2mm, aperture is 0.6 μm, and porosity is more than 70%.
(5) alkali soluble：The filter cake that NaOH solution dissolving step (1) after the concentration that step (4) obtains obtains, is stirred in 100 DEG C
Reaction 4h is mixed, is separated by filtration to obtain NaAlO2Solution.
Embodiment 4
Caused waste residue during certain chromium salt factory production sodium dichromate, moisture content about 60% (mass fraction), dry aluminium mud master
Contain Al2O3、Cr2O3、Na2CrO4、SiO2And Fe2O3Deng.
(1) it is water-soluble：Water is added in waste residue, and (mass ratio of waste residue and water is 1：3), in 80 DEG C of stirring reaction 1h, water repeatedly
Wash 3 times, chromium (VI) aqueous solution and filter cake containing aluminium must be contained by filtering.
(2) electroreduction：Through electroreduction it is three prices by hexavalent chrome reduction containing chromium (VI) aqueous solution；Electroreduction parameter：Anode
Electrode is Ru-Ir/Ti, and negative electrode is Ti plates, current density 150A/m2, amberplex is added in electrolytic cell, by anode and the moon
Pole separates.
(3) bipolar membrane electrodialysis：Handled at normal temperatures through bipolar membrane electrodialysis containing chromium (III) aqueous solution, obtain NaOH solution
And chromic acid solution；The reaction condition of bipolar membrane electrodialysis：1% metabisulfite solution is pole liquid, and reaction temperature is 25 DEG C, current density
For 500A/m2。
(4) membrane distillation：The NaOH solution that step (3) obtains, to nearly saturation state, obtains clear water and concentration through membrane distillation concentration
NaOH solution, clear water is back to the water-soluble process in step 1.Membrane distillation uses polypropylene screen, to strengthen the hydrophobic of film appearance
Property, thickness 0.1mm, aperture is 0.4 μm, and porosity is more than 80%.
(5) alkali soluble：The filter cake that NaOH solution dissolving step (1) after the concentration that step (4) obtains obtains, in 90 DEG C of stirrings
4h is reacted, is separated by filtration to obtain NaAlO2Solution.
Claims (8)
- A kind of 1. recycling processing method of chromium-contained aluminum mud, it is characterised in that including：Step 1, water mixing is added in chromium-contained aluminum mud, is filtered through rising temperature for dissolving, is obtained containing chromium (VI) aqueous solution and containing aluminium (III) filter cake；Step 2, obtain containing chromium (III) aqueous solution through electroreduction containing chromium (VI) aqueous solution；Step 3, handled containing chromium (III) aqueous solution through bipolar membrane electrodialysis, obtain NaOH solution and chromic acid solution；The condition of bipolar membrane electrodialysis is：The conducting solution that mass fraction is 0.1~5% is pole liquid, 1~40 DEG C of reaction temperature, 200~700A/m of current density2；Step 4, the NaOH solution in step 3 is concentrated using membrane distillation, obtains the NaOH solution of clear water and concentration, clear water returns For the water-soluble process in step 1；Step 5, using the filter cake containing aluminium in the NaOH solution dissolving step 1 after being concentrated in step 4, temperature reaction, it is separated by filtration Obtain NaAlO2Solution.
- 2. the recycling processing method of chromium-contained aluminum mud as claimed in claim 1, it is characterised in that in step 1, chromium-contained aluminum mud with The mass ratio of water is 1：3~9.
- 3. the recycling processing method of chromium-contained aluminum mud as claimed in claim 1, it is characterised in that in step 1, it is warming up to 60~ 80 DEG C of stirring and dissolvings.
- 4. the recycling processing method of chromium-contained aluminum mud as claimed in claim 1, it is characterised in that in step 1, moisture batch adds Enter in chromium-contained aluminum mud.
- 5. the recycling processing method of chromium-contained aluminum mud as claimed in claim 1, it is characterised in that the electricity of electroreduction in step 2 Pole is using one kind in graphite electrode, metal Ti electrode, titanium plating ruthenium or titanium plating iridium electrode；Ion exchange is separated with electroreduction groove Film, current density are 40~300A/m2。
- 6. the recycling processing method of chromium-contained aluminum mud as claimed in claim 1, it is characterised in that in step 4, membrane distillation uses Hollow-fibre membrane or laminar film, membrane material is from least one of polytetrafluoroethylene (PTFE), Kynoar, polypropylene, polyethylene.
- 7. the recycling processing method of chromium-contained aluminum mud as claimed in claim 1, it is characterised in that in step 4, membrane distillation is adopted Membrane porosity is 60~95%, and aperture is 0.1~1.0 μm, and thickness is 0.04~0.25mm.
- 8. the recycling processing method of chromium-contained aluminum mud as claimed in claim 1, it is characterised in that in step 5, it is warming up to 90~ 110 DEG C, 2~6h of stirring reaction.
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| CN110255675B (en) * | 2019-07-03 | 2021-08-10 | 福建师范大学泉港石化研究院 | Bipolar membrane electrodialysis method for recovering chromium in wastewater by combining oxidation |
| CN113249582B (en) * | 2021-05-06 | 2022-03-29 | 中南大学 | A kind of treatment method of aluminum metallurgy solid waste |
| CN119320190B (en) * | 2024-12-18 | 2025-06-24 | 同济大学 | Method and device for preparing sewage treatment agent by using red mud as raw material |
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| JP4544970B2 (en) * | 2004-11-09 | 2010-09-15 | Ｊｆｅスチール株式会社 | Processing method for pickling waste liquid and processing equipment for pickling waste liquid |
| CN101863512B (en) * | 2010-04-15 | 2011-12-28 | 彭运林 | Acid method recycling process of chromium-containing aluminum mud |
| CN102417312B (en) * | 2011-08-25 | 2013-06-19 | 甘肃锦世化工有限责任公司 | Resource utilization method for chrome-containing aluminum sludge |
| CN104131166A (en) * | 2014-07-08 | 2014-11-05 | 泰州明锋资源再生科技有限公司 | Pollution-free treatment and recycling method of sludge generated during stainless steel acid washing process |
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