CN106521194B - A kind of extractant and its application method for emulsion liquid membrane extracting rare earth - Google Patents
A kind of extractant and its application method for emulsion liquid membrane extracting rare earth Download PDFInfo
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- CN106521194B CN106521194B CN201610998017.XA CN201610998017A CN106521194B CN 106521194 B CN106521194 B CN 106521194B CN 201610998017 A CN201610998017 A CN 201610998017A CN 106521194 B CN106521194 B CN 106521194B
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- rare earth
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- VPYGKOKPRDYTCW-CKCLTMHVSA-N [BH+]/C=C\C=C1\C=CCCC1 Chemical compound [BH+]/C=C\C=C1\C=CCCC1 VPYGKOKPRDYTCW-CKCLTMHVSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
-
- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/065—Nitric acids or salts thereof
-
- 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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- 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
-
- 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
Abstract
The present invention discloses a kind of extractant for emulsion liquid membrane extracting rare earth, it is characterised in that：The general formula structure of the extractant is as follows：R1, R2=Cn in formula1, n1=8；Cn2, n2=1~18.Belong to chemical separating with extraction field, provide it is a kind of from highly acid, strong oxidizing property phosphorus ore leachate in Extraction of rare earth method.It is characterized in that by flowing carrier 4%~16% (volume fraction, similarly hereinafter), surfactant T154 be 4%~16%, membrane solvent sulfonated kerosene be used as oil phase, with interior phase parsing agent according to volume ratio 1:1, high-speed stirred is made emulsion, and stirring at low speed extracts leachate middle rare earth, and the volume ratio of emulsion and outer aqueous phase leachate is 1:10~1:100, which reaches as high as 82% or more to the extraction efficiency of phosphorus ore leachate middle rare earth.
Description
Technical field
The invention belongs to chemical separating with extraction field, provide it is a kind of from highly acid, strong oxidizing property phosphorus ore leachate in
The method of Extraction of rare earth.
Background technology
China's rare earth resources mainly use electrolyte solution leaching process ore at present mostly from low-grade Rare-earth Mine
Method, and be mostly to use oxalic acid or ammonium bicarbonate precipitation rare earth to leachate processing, separation and Extraction effect is poor.At present
China compares in the research fields such as the deep processing of rare earth, the exploitation of new material and external advanced country, still has sizable
Gap.In order to efficient Extraction of rare earth element, it is necessary to seek cost-efficiently isolation technics.Liquid Membrane Separation Technique it is efficient
Selectivity, high directivity, great permeability are the sharpest edges of its separation and Extraction.
For the raw material of common liquid membrane extraction rare earth mostly from phosphorus ore, pH value is generally 2.5~5, and in phosphorus ore acid hydrolysis liquid due to
There are a large amount of phosphate radicals, easily generate and precipitate with rare earth ion, so only rare earth can just be deposited in the form of an ion under highly acidity
It is being suitable for liquid film separation.The liquid film separation of rare earth is frequently with traditional rare-earth extractant as flowing carrier.
Zhang Lichang etc. uses aniline as flowing carrier, and T154 makees surfactant, and 6mol/L hydrochloric acid makees interior mutually parsing agent, sulphur
Change kerosene and make membrane solvent, oily internal ratio is 1:1 produces emulsion liquid film to low concentration of rare earth element in phosphorus ore leachate under hydrochloric acid system
It is extracted, to the earth solution of pH=-0.5, a concentration of 100mg/L, ratio of milk and water 1:10, recovery rate highest can reach
94.68%.But as outer aqueous phase solution system from concentrated hydrochloric acid becomes concentrated nitric acid, under identical conditions, recovery rate is only 60%
Left and right, meanwhile, liquid film swelling is very big.In summary, aniline cannot be extracted efficiently as flowing carrier in concentrated nitric acid medium
Rare earth element, it is therefore necessary to a kind of Novel Extractant is synthesized, it can be in the middle and high acidity of concentrated nitric acid system and phosphorus ore leachate rare earth
Under conditions of content is low, reduces the swelling of liquid film and realize that rare earth ion efficiently separates extraction.
Invention content
The technical problem to be solved by the present invention is to：It solves to realize to containing low concentration of rare earth high efficiency extraction in concentrated nitric acid system
Technology provides a kind of process for producing emulsion liquid film high efficiency extraction rare earth element with self-control extractant.
The technical scheme is that：A kind of extractant for emulsion liquid membrane extracting rare earth, the general formula knot of the extractant
Structure is as follows：
R1, R2=Cn in formula1, n1=8；Or Cn2, n2=1~18.
A kind of application method of extractant for emulsion liquid membrane extracting rare earth, comprises the steps of：
1) rock phosphate in powder of concentrated nitric acid, concentrated sulfuric acid dissolution containing rare earth is used, solution is entered in the form of rare earth ion, obtains phosphorus ore
Leachate；
2) extractant, surfactant, diluent are mixed with interior phase parsing agent hydrochloric acid, sulfuric acid, nitric acid, emulsus is made
Liquid；
3) phosphorus ore leachate is mixed with emulsion, Extraction of rare earth element.
In the step 2), surfactant T154, diluent is sulfonated kerosene.
In the step 2), the volume fraction of extractant and surfactant is 4%~16% in oil phase, diluent
Volume fraction is 80%, and oil phase and inner aqueous phase are pressed 1:1 volume ratio mixing, high-speed stirred 20min obtain white water-in-oil type
Emulsion.
In the step 3), by emulsion liquid film and pH value be -0.1~1.0 phosphorus ore leachate according to volume ratio 1:10
~1:100 mixing extractions, extraction time 20min.
Beneficial effects of the present invention：The present invention selects structure 1 to produce emulsion extracting rare-earth as flowing carrier, it is dilute
Native content is relatively low, and higher in earth solution acidity, has very high extraction efficiency.
When extraction, in the case that other extraction conditions are constant, ratio of milk and water is reduced to 1:When 100, still there is higher extracted effect
Rate greatly reduces the recycling amount of organic phase.
The structure 1 that the present invention selects compared with common flowing carrier P204, P507 and aniline etc., extracts as flowing carrier
Efficiency is taken to greatly improve.
The present invention can also extract in phosphorus ore sulphuric leachate using structure 1 as emulsion liquid film made of flowing carrier
Rare earth, extraction efficiency can reach 78.5%.
Emulsion liquid film extraction system used in the present invention has higher extraction yield simultaneously, and effect of extracting is good, quickly, selects
The advantages that selecting property is high.Integrated artistic is simple, and rare earth yield is high, and consumption of raw materials is few.Effective recycling to rare earth is realized, is phosphorus
The comprehensive utilization of mine provides a feasible, reasonable, effective approach.
Specific implementation mode
Embodiment (one)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8,) volume fraction be 12%, T154 volume fractions be 8%, sulfonated kerosene 80%, by oil phase with it is interior
Mutually parsing agent is according to 1:1 volume ratio mixing, high-speed stirred 20min.It is according to volume ratio with phosphorus ore leachate by emulsion liquid film
1:10, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Efficiency is taken to reach 82.68%.
Embodiment (two)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8,) volume fraction be 8%, T154 volume fractions be 12%, sulfonated kerosene 80%, by oil phase with it is interior
Mutually parsing agent is according to 1:1 volume ratio mixing, high-speed stirred 20min.It is according to volume ratio with phosphorus ore leachate by emulsion liquid film
1:10, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Efficiency is taken to reach 75.31%.
Embodiment (three)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8,) volume fraction be 4%, T154 volume fractions be 16%, sulfonated kerosene 80%, by oil phase with it is interior
Mutually parsing agent is according to 1:1 volume ratio mixing, high-speed stirred 20min.It is according to volume ratio with phosphorus ore leachate by emulsion liquid film
1:10, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Efficiency is taken to reach 78.25%.
Embodiment (four)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8,) volume fraction be 16%, T154 volume fractions be 4%, sulfonated kerosene 80%, by oil phase with it is interior
Mutually parsing agent is according to 1:1 volume ratio mixing, high-speed stirred 20min.It is according to volume ratio with phosphorus ore leachate by emulsion liquid film
1:10, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Efficiency is taken to reach 82.56%.
Embodiment (five)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8,) volume fraction be 10%, T154 volume fractions be 10%, sulfonated kerosene 80%, by oil phase with it is interior
Mutually parsing agent is according to 1:1 volume ratio mixing, high-speed stirred 20min.It is according to volume ratio with phosphorus ore leachate by emulsion liquid film
1:10, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Efficiency is taken to reach 80.07%.
Embodiment (six)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8,) volume fraction be 12%, T154 volume fractions be 8%, sulfonated kerosene 80%, by oil phase with it is interior
Mutually parsing agent is according to 1:1 volume ratio mixing, high-speed stirred 20min.It is according to volume ratio with phosphorus ore leachate by emulsion liquid film
1:30, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Efficiency is taken to reach 74.63%.
Embodiment (seven)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8,) volume fraction be 12%, T154 volume fractions be 8%, sulfonated kerosene 80%, by oil phase with it is interior
Mutually parsing agent is according to 1:1 volume ratio mixing, high-speed stirred 20min.It is according to volume ratio with phosphorus ore leachate by emulsion liquid film
1:50, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Efficiency is taken to reach 67.5%.
Embodiment (eight)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8,) volume fraction be 12%, T154 volume fractions be 8%, sulfonated kerosene 80%, by oil phase with it is interior
Mutually parsing agent is according to 1:1 volume ratio mixing, high-speed stirred 20min.It is according to volume ratio with phosphorus ore leachate by emulsion liquid film
1:100, extraction 20min is mixed slowly, is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Extraction efficiency is 64.67%.
Embodiment (nine)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8,) volume fraction be 12%, T154 volume fractions be 8%, sulfonated kerosene 80%, by oil phase with
Interior phase parses agent according to 1:1 volume ratio mixing, high-speed stirred 20min.By emulsion liquid film and phosphorus ore leachate according to volume ratio
It is 1:10, extraction 20min is mixed slowly, is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Extraction efficiency is 64%.
Embodiment (ten)
The sulphuric leachate of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.10g/L.Structure 1 in oil phase
(R1, R2=C8,) volume fraction be 12%, T154 volume fractions be 8%, sulfonated kerosene 80%, by oil phase with it is interior
Mutually parsing agent is according to 1:1 volume ratio mixing, high-speed stirred 20min.It is according to volume ratio with phosphorus ore leachate by emulsion liquid film
1:10, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
It is 78.5% to take efficiency.
Embodiment (11)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8, R3=C4) volume fraction be 12%, T154 volume fractions be 8%, sulfonated kerosene 80%, by oil phase and interior phase
Agent is parsed according to 1:1 volume ratio mixing, high-speed stirred 20min.According to volume ratio it is 1 by emulsion liquid film and phosphorus ore leachate:
10, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Efficiency is 79.8%.
Embodiment (12)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8, R3=C6) volume fraction be 12%, T154 volume fractions be 8%, sulfonated kerosene 80%, by oil phase and interior phase
Agent is parsed according to 1:1 volume ratio mixing, high-speed stirred 20min.According to volume ratio it is 1 by emulsion liquid film and phosphorus ore leachate:
10, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
Efficiency is 76.56%.
Embodiment (13)
The leaching solution of phosphorus ore is extracted, phosphorus ore leachate rare earth concentration is 0.303g/L.Structure 1 in oil phase
(R1, R2=C8, R3=C18) volume fraction be 12%, T154 volume fractions be 8%, sulfonated kerosene 80%, by oil phase with it is interior
Mutually parsing agent is according to 1:1 volume ratio mixing, high-speed stirred 20min.It is according to volume ratio with phosphorus ore leachate by emulsion liquid film
1:10, extraction 20min is mixed slowly, extraction is measured with GB/T 6730.24-2006 extraction and separation-chlorophosphonazo mA spectrophotometry
It is 77% to take efficiency.
The rare earth for extracting the low concentration of association from phosphorus ore leachate using the present invention, can substantially reduce production cost,
The waste for reducing resource, has great application prospect.
Claims (5)
1. a kind of extractant for emulsion liquid membrane extracting rare earth, it is characterised in that：The general formula structure of the extractant is as follows：
R1, R2=Cn in formula1, n1=8；Or Cn2, n2=1~18.
2. a kind of application method of the extractant as described in claim 1 for emulsion liquid membrane extracting rare earth, it is characterised in that：
It comprises the steps of：
1) rock phosphate in powder of concentrated nitric acid, concentrated sulfuric acid dissolution containing rare earth is used, solution is entered in the form of rare earth ion, obtains phosphorus ore leaching
Liquid；
2) extractant, surfactant, diluent are mixed with interior phase parsing agent hydrochloric acid, sulfuric acid, nitric acid, emulsion is made；
3) phosphorus ore leachate is mixed with emulsion, Extraction of rare earth element.
3. the application method of the extractant according to claim 2 for emulsion liquid membrane extracting rare earth, it is characterised in that：Institute
In the step 2) stated, surfactant T154, diluent is sulfonated kerosene.
4. the application method of the extractant according to claim 2 or 3 for emulsion liquid membrane extracting rare earth, feature exist
In：In the step 2), the volume fraction of extractant and surfactant is 4%~16% in oil phase, diluent volume
Score is 80%, and oil phase and inner aqueous phase are pressed 1:1 volume ratio mixing, high-speed stirred 20min obtain white water-in-oil type emulsus
Liquid.
5. the application method of the extractant according to claim 2 for emulsion liquid membrane extracting rare earth, it is characterised in that：Institute
In the step 3) stated, by emulsion liquid film and pH value be -0.1~1.0 phosphorus ore leachate according to volume ratio 1:10~1:100 mixing
Extraction, extraction time 20min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058995A (en) * | 1990-08-15 | 1992-02-26 | 中国科学院长春应用化学研究所 | Centrifugal extraction of rare-earth mother liquid with naphthenic acid |
| CN102304628A (en) * | 2011-07-29 | 2012-01-04 | 江西理工大学 | Method for extracting rare earth from phosphate rock by utilizing liquid membrane |
| CN105219960A (en) * | 2015-11-19 | 2016-01-06 | 贵州大学 | A kind of method of emulsion liquid membrane extracting rare earth |
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| CA3109603C (en) * | 2012-09-18 | 2022-09-27 | Chemtor, Lp | Use of a fiber conduit contactor for metal and/or metalloid extraction |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1058995A (en) * | 1990-08-15 | 1992-02-26 | 中国科学院长春应用化学研究所 | Centrifugal extraction of rare-earth mother liquid with naphthenic acid |
| CN102304628A (en) * | 2011-07-29 | 2012-01-04 | 江西理工大学 | Method for extracting rare earth from phosphate rock by utilizing liquid membrane |
| CN105219960A (en) * | 2015-11-19 | 2016-01-06 | 贵州大学 | A kind of method of emulsion liquid membrane extracting rare earth |
Non-Patent Citations (3)
| Title |
|---|
| 乳状液-中空纤维膜萃取钕及其传质性能研究;龚福忠等;《中国稀土学报》;20060630;第24卷(第3期);第298-303页 * |
| 乳状液膜法提取模拟湿法磷酸中的稀土镧;范文娟等;《膜科学与技术》;20120430;第32卷(第2期);第46-51、64页 * |
| 新型萃取剂Cyanex272为载体的乳状液膜富集稀土的研究;秦庆伟;《南方冶金学院学报》;20010731;第22卷(第4期);第304-308页 * |
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