CN110844963A - Method for separating and recovering aluminum-containing high-iron-salt-acid wastewater - Google Patents
Method for separating and recovering aluminum-containing high-iron-salt-acid wastewater Download PDFInfo
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- CN110844963A CN110844963A CN201911151661.3A CN201911151661A CN110844963A CN 110844963 A CN110844963 A CN 110844963A CN 201911151661 A CN201911151661 A CN 201911151661A CN 110844963 A CN110844963 A CN 110844963A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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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
- C22B21/00—Obtaining aluminium
- C22B21/0038—Obtaining aluminium by other processes
- C22B21/0069—Obtaining aluminium by other processes from scrap, skimmings or any secondary source aluminium, e.g. recovery of alloy constituents
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/28—Amines
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
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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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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/203—Iron or iron compound
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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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Abstract
The invention discloses a method for separating and recovering aluminum-containing high-iron-salt-acid wastewater, wherein aluminum and iron in the wastewater are respectively Al of aluminum chloride3+And Fe of ferric chloride3+Extracting iron in the wastewater by using an extraction system to obtain low-iron raffinate and an iron-containing loaded organic phase; carrying out back extraction on the loaded organic phase by using a back extractant to obtain an iron chloride solution so as to recover iron chloride or iron oxide red; the extraction system of the invention has large saturated capacity of extracted iron, and the iron is selectedHigh selectivity, basically no extraction of aluminum, thorough separation of iron and aluminum, and easy back extraction of iron.
Description
Technical Field
The invention relates to a method for extracting and separating iron and aluminum, in particular to an iron extraction technology in hydrometallurgy, and particularly relates to a method for extracting and separating iron and aluminum from aluminum-containing ferric sulfate waste water.
Background
Aluminum/iron is widely present in various minerals in the nature, almost all metallurgical processes relate to separation and extraction of aluminum and iron, and particularly, in recent years, with the increase of the yield of alumina in China and the shortage of domestic resources, the development and utilization of low-grade bauxite resources and non-traditional alumina resources become hot spots of attention of people. The fly ash is one of the largest industrial waste residues in China at present, and is usually rich in Al2O3The method is an important non-traditional alumina resource and a potential bauxite substitute resource, so that the extraction of alumina from the fly ash becomes a great research hotspot. The process for extracting the aluminum oxide from the fly ash by the one-step acid dissolution method is researched and developed by Shenhua quasi-energy resource comprehensive development limited company, and at present, the process has industrial implementation conditions, but the aluminum-containing high-iron-salt-acid-containing wastewater produced by the process needs to be treated to realize recycling.
In the traditional hydrometallurgical industry, the precipitation method is mainly adopted to remove iron in solution, such as jarosite method, goethite method, hematite method and the like, and the problems of large aluminum loss, difficult sediment recovery, easy secondary pollution and the like exist. In order to further separate aluminum and iron from the solution, the research on removing iron by a solvent extraction method, particularly the iron removal research on aluminum sulfate with low iron content, is the most since the 60 th age of the 20 th century, but the research on separating aluminum and iron in a hydrochloric acid system, particularly the separation research on ferric chloride with high concentration, is rarely reported.
Chinese patent CN101659438A discloses a method for removing iron from aluminum sulfate solution, which adopts primary amine N1923-N-octanol-kerosene as organic phase, and the removal rate of iron in aluminum sulfate reaches 100%, but it mainly aims at sulfate system, and it does not mention chloride system.
Zhang Xiuli (journal of the college of engineering of Jilin, 20(4), 17-20) extracted from Fe-containing materials by using tertiary amine3+The iron removal effect is good when the aluminum chloride solution contains 0.02mol/L of iron, but the iron content in the solution is low and is only about L g/L.
The prumingyu and the like invent a method for extracting and separating iron and aluminum from a hydrochloric acid system, an extraction system is N503-TBP-N-octanol-sulfonated kerosene, the extraction system has high selectivity, aluminum is not extracted, and the concentration of the aimed ferric iron is about 50 g/L.
In the existing literature, solvent extraction for iron removal is mainly concentrated on a sulfate system, and is mostly concentrated on removal of low-concentration iron in a feed liquid, how to efficiently extract high-concentration iron in the feed liquid, and a third phase problem which is easily caused by high concentration is eliminated or avoided, particularly the problem which needs to be solved in aluminum extraction by a fly ash hydrochloric acid method.
Disclosure of Invention
Aiming at overcoming the defects and shortcomings that the existing iron and aluminum extraction separation system is low in selectivity and small in saturation capacity, a third phase is easy to generate in the extraction process of high-concentration iron, and back extraction is not easy, the invention aims to provide a low-cost method for separating and recovering aluminum-containing ferric picrate wastewater by extracting, separating and recovering iron and aluminum from wastewater containing aluminum chloride, ferric chloride and hydrochloric acid.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for separating and recovering aluminum-containing high-iron salt acid wastewater, wherein aluminum and iron in the wastewater are respectively Al of aluminum chloride3+And Fe of ferric chloride3+The separation and recovery method is to use the organic phase to carry out the separation and recovery on the wastewater relative to the iron in the wastewaterExtracting to obtain low-iron raffinate and an iron-containing loaded organic extract phase; carrying out back extraction on the loaded organic extraction phase by using a back extractant to obtain a ferric chloride solution so as to recover ferric chloride or iron oxide red; wherein
The organic phase comprises an extracting agent, a modifier and a diluent;
the extraction agent is trialkyl tertiary amine and/or phosphate ester, wherein the trialkyl tertiary amine has a general formula shown in a formula (1):
r in the formula (1)1、R2、R3Respectively selected from alkyl with 8-10 carbon atoms such as 9 carbon atoms, for example, straight chain or branched chain alkyl;
the phosphate ester has a general formula shown in formula (2):
r in the formula (2)4Selected from alkyl groups of 4 to 8, such as 5, 6 or 7 carbon atoms, for example straight or branched chain alkyl;
the modifier is C8~C10One or more of alcohols;
the diluent is sulfonated kerosene and/or kerosene;
the stripping agent is dilute hydrochloric acid.
In the invention, the volume ratio of the extracting agent to the modifying agent to the diluent is preferably (1-5): (1-5): (2-6), for example, the extracting agent is 2, 3 or 4 parts by volume, the modifying agent is 2, 3 or 4 parts by volume, and the diluting agent is 3, 4 or 5 parts by volume.
In the present invention, the extractant is trialkyl tertiary amine and/or phosphate, preferably trioctyl decyl tertiary amine (N235) and tributyl phosphate. In one embodiment, the volume ratio of the tertiary amine to the phosphate ester is preferably (1-5): (5-1), for example, 1: (2-5), 1:3 or 1: 4;
in the invention, the modifier is C8~10Alcohols, such as linear or branched mono-or diols; preferably a secondary octanol;
in the invention, the diluent is sulfonated kerosene and/or kerosene, preferably sulfonated kerosene.
It was found that, in the present invention, modifier C8~10The addition of the alcohol can effectively improve the phase separation effect of the extraction system, has the synergistic extraction effect and has good effect in the extraction of the wastewater system.
In the invention, in the hydrochloric acid wastewater containing ferric iron and aluminum, the content of ferric iron is preferably 60-140 g/L, the content of aluminum is not particularly limited, and good separation can be realized, but the hydrochloric acid concentration is known to be lower than a saturated concentration, such as less than or equal to 25g/L, such as 10, 13, 15 or 20g/L, and the hydrochloric acid concentration is preferably 1.5-4.5 mol/L, such as 2mol/L or 3 mol/L;
in one embodiment of the invention, the volume ratio of extraction (O/A) V is obtained when the wastewater is extracted by the extraction systemExtraction system:VAqueous phasePreferably 6: 1-1: 1, such as 5:1, 4:1, 3:1 or 2:1, at normal temperature, and the extraction time is preferably 2-10 min, such as 4, 6 or 8 min; more preferably, the ratio is O/A ═ (3-4): 1;
in one embodiment of the present invention, the volume ratio of ferric iron in the loaded organic phase stripped by stripping agent is VLoaded with organic compounds:VStripping agent6: 1-1: 1, performing at normal temperature, wherein the back extraction time is preferably 2-10 min, such as 4, 6 or 8min, and the pH of the back extractant is 1-2;
in the invention, the purity of ferric chloride in the solute of the obtained ferric chloride solution is more than or equal to 99.9 wt%.
The separation method comprises extraction and back extraction, wherein the extraction can be multistage extraction, and the back extraction can be multistage back extraction. Wherein "multi-stage" means at least 2 stages.
Preferably, the extraction is 4-7 grade extraction and the back extraction is 4-6 grade back extraction.
The extraction and back extraction processes are as follows: extracting the wastewater in multiple stages (such as 4-7 stages) in an extraction section by using an extracting agent, wherein the extraction residual liquid (namely raffinate) is an acidic solution mainly containing aluminum chloride, the extraction rate of iron ions is more than 99 percent, such as more than 99.4 percent, and the iron ions can be returned to the fly ash for aluminum leaching or further recovering aluminum chloride or aluminum hydroxide; carrying out multi-stage (such as 4-6 stages) back extraction on the extracted loaded organic phase by using a back extractant to obtain a back extraction solution which is an iron chloride solution; the organic phase after back extraction is a no-load organic phase and can continuously return to the extraction section for extraction.
The invention relates to an aluminum-containing high-iron hydrochloric acid wastewater/solution, in particular to a method for treating aluminum-containing high-iron hydrochloric acid wastewater generated by a process for extracting aluminum oxide from fly ash by a one-step acid dissolving method, which has the following beneficial effects:
the extraction system of the invention has large saturation capacity of extracting iron, high selectivity, basically no extraction of aluminum, complete separation of iron and aluminum, and easy back extraction of iron (more than 99.99%).
Detailed Description
The technical solution and effects of the present invention will be further described below by way of specific embodiments. The following embodiments are merely illustrative of the present invention, and the present invention is not limited to the following embodiments or examples. Simple modifications of the invention applying the inventive concept are within the scope of the invention as claimed.
Example 1
The extraction stock solution is a solution containing 66.24g/L of iron, 8.82g/L of aluminum and 3.0mol/L of hydrochloric acid, and the extraction system is trioctyl decyl tertiary amine: tributyl phosphate: secondary octanol: sulfonated kerosene 1: 2.5: 3: and 4.5, performing six-stage countercurrent extraction on the extract with the phase ratio of O/A of 3/1 for 4 min.
TABLE 1 data sheet for six-stage countercurrent cascade extraction
And sequentially taking the loaded organic phase for back extraction, wherein the back extraction ratio is 3.5/1, the back extraction agent is dilute hydrochloric acid with the pH value of 1, the time is 5min, the room temperature is 14 ℃, six-stage countercurrent back extraction experiments are carried out, and the data are sequentially recorded in the following table.
Table 2 table of the six stage counter current cascade stripping data.
Example 2
The extraction stock solution contains 118.09g/L iron, 10.37g/L aluminum and 3.5mol/L hydrochloric acid, and the extraction system is trioctyl decyl tertiary amine: tributyl phosphate: secondary octanol: sulfonated kerosene 1: 5: 6: and 8, performing five-stage countercurrent extraction on the extract at the O/A ratio of 3.5/1 for 4 min.
TABLE 3 five-stage countercurrent cascade extraction data sheet
The loaded organic phase is taken out in sequence, and a six-stage counter-current back extraction experiment is carried out in an O/A (oxygen/oxygen) 3/1 condition with a back extraction agent of dilute hydrochloric acid with the pH value of 1 for 5min at room temperature, and the data are recorded in the following table in sequence.
TABLE 4 data sheet for counter-current cascade counter-extraction of six stages
Example 3
When the extraction stock solution is a solution containing 94.32g/L of iron, 9.15g/L of aluminum and 3.3mol/L of hydrochloric acid, the extraction system is trioctyl decyl tertiary amine: tributyl phosphate: secondary octanol: sulfonated kerosene 1: 4: 5: and 6, performing six-stage countercurrent extraction on the extract at the O/A ratio of 3.3/1 for 4 min.
TABLE 5 data sheet for six-stage countercurrent cascade extraction
And sequentially taking the loaded organic phase to perform back extraction, wherein the back extraction ratio is 3.2/1, the back extraction agent is dilute hydrochloric acid with the pH value of 2, the time is 5min, the room temperature is 15 ℃, five-stage countercurrent back extraction experiments are performed, and the data are sequentially recorded in the following table.
Table 6 table of five-stage countercurrent cascade back extraction data.
In each table, 100 is greater than 99.99%; 0 is less than 0.01%.
Claims (10)
1. A method for separating and recovering aluminum-containing high-iron salt acid wastewater, wherein aluminum and iron in the wastewater are respectively Al of aluminum chloride3+And Fe of ferric chloride3+The method is characterized in that the wastewater is extracted with iron by an extraction system to obtain low-iron raffinate and an iron-containing loaded organic phase; carrying out back extraction on the loaded organic phase by using a back extractant to obtain an iron chloride solution so as to recover iron chloride or iron oxide red; wherein
The extraction system comprises an extracting agent, a modifier and a diluent;
the extraction agent is trialkyl tertiary amine and/or phosphate ester, wherein the trialkyl tertiary amine has a general formula shown in a formula (1):
r in the formula (1)1、R2、R3Respectively selected from alkyl with 8-10 carbon atoms;
the phosphate ester has a general formula shown in formula (2):
r in the formula (2)4Selected from alkyl with 4-8 carbon atoms;
the modifier is C8~C10One or more of alcohols;
the diluent is sulfonated kerosene and/or kerosene;
the stripping agent is dilute hydrochloric acid.
2. The method of claim 1, wherein: the volume ratio of the extracting agent to the modifying agent to the diluting agent is (1-5): (1-5): (2-6).
3. The method according to any of the preceding claims, wherein: the volume ratio of the tertiary amine to the phosphate in the extractant is (1: 5) - (5: 1).
4. The method according to any of the preceding claims, wherein: the iron content in the wastewater is 60-140 g/L, wherein the concentration of hydrochloric acid is 1.5-4.5 mol/L.
5. The method according to any of the preceding claims, wherein: when the extraction system is used for extraction, the extraction phase ratio is VExtraction system:VAqueous phase6: 1-2: 1; preferably, the extraction is carried out at normal temperature, and the extraction time is 2-10 min.
6. The method of claim 5, wherein: the extraction ratio is (3-4) and 1.
7. The method according to any of the preceding claims, wherein: when the stripping agent for the loaded organic phase is used for back extraction of iron, the back extraction phase ratio V isLoaded with organic compounds:VBack extraction6: 1-1: 1; preferably, the back extraction is carried out at normal temperature, the back extraction time is 2-10 min, and the pH value of a back extractant is 1-2.
8. The method according to any of the preceding claims, wherein: the alcohol is a secondary octanol.
9. The method according to any of the preceding claims, wherein: the tertiary amine is trioctyl decyl tertiary amine.
10. The method according to any of the preceding claims, wherein: the phosphate is tributyl phosphate.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110395766A (en) * | 2019-08-26 | 2019-11-01 | 广东省稀有金属研究所 | A kind of preparation method of solid sulphuric acid vanadyl |
CN112390320A (en) * | 2020-10-30 | 2021-02-23 | 神华准能资源综合开发有限公司 | Extraction agent composition and resource utilization method of iron-containing wastewater |
CN112481497A (en) * | 2020-10-30 | 2021-03-12 | 神华准能资源综合开发有限公司 | Method for removing heavy metal from aluminum-containing hydrochloric acid wastewater |
CN115231647A (en) * | 2022-07-27 | 2022-10-25 | 赣州步莱铽新资源有限公司 | Recovery method of back extraction waste acid |
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CN108165748A (en) * | 2017-12-29 | 2018-06-15 | 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 | A kind of zinc replacement slag leachate extraction is except the method for iron |
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CN112390320A (en) * | 2020-10-30 | 2021-02-23 | 神华准能资源综合开发有限公司 | Extraction agent composition and resource utilization method of iron-containing wastewater |
CN112481497A (en) * | 2020-10-30 | 2021-03-12 | 神华准能资源综合开发有限公司 | Method for removing heavy metal from aluminum-containing hydrochloric acid wastewater |
CN115231647A (en) * | 2022-07-27 | 2022-10-25 | 赣州步莱铽新资源有限公司 | Recovery method of back extraction waste acid |
CN115231647B (en) * | 2022-07-27 | 2023-08-15 | 赣州步莱铽新资源有限公司 | Method for recycling back-extraction waste acid |
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