CN103146921B - Method for removing aluminum in rare-earth solution - Google Patents

Method for removing aluminum in rare-earth solution Download PDF

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CN103146921B
CN103146921B CN201310115296.7A CN201310115296A CN103146921B CN 103146921 B CN103146921 B CN 103146921B CN 201310115296 A CN201310115296 A CN 201310115296A CN 103146921 B CN103146921 B CN 103146921B
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rare earth
feed liquid
organic phase
extraction
rare
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CN103146921A (en
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赵治华
邢全生
刘建军
桑晓云
郭晓辉
赵志强
张文斌
李旭
王喜刚
姜东波
王平
孙祥
李俊林
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China north rare earth (Group) hi tech Limited by Share Ltd
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INNER MONGOLIA BAOGANG RARE EARTH (GROUP) HIGH TECHNOLOGY Co Ltd
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Abstract

The invention relates to a method for removing aluminum in rare-earth solution. The method comprises the following steps of: carrying out saponification for an organic phase, separating aluminum from rare-earth liquid via a method of distilling and extracting, and a distilling and extracting flow rate is as following: a volume ratio of the organic phase: rare-earth solution : washing liquid: reverse liquid is (40-60): (100-200): (3-20): (1-3) L/min; the concentration of REO (rare-earth oxide) in rare-earth solution is (1.6-1.77) mol/L, the concentration of Al2O3 is (0.003-0.03) mol/L, the acidity of washing liquid is (0.1-3.0) mol/L, and the acidity of reverse liquid is (1.0-4.5) mol/L; a distilling and extracting class is that an extracting section: a washing section: a reverse-extracting section equals to 8:10:7; and a recovery rate of rare earth reaches above 99.98 percent. According to the method, a process for removing aluminum is shortened, the phenomenon of emulsification in the extraction is eliminated, the separation efficiency is good, linkage extraction is realized, the recovery rate of rare earth is high, and produced waste water is easier to treat.

Description

A kind of method removing aluminium in earth solution
Technical field
The present invention relates to a kind of method removing aluminium in earth solution.
Background technology
From the process of rare-earth mineral recovering rare earth solution, a great deal of aluminum ion enters in leach liquor with rare earth.Aluminum removing method conventional in current production mainly contains alkaline process, acid system, hydrolysis method, extraction process etc.Wherein traditional extraction process is the organic phase system formed with 25% naphthenic acid-20% isooctyl alcohol-kerosene (volume ratio), add ammoniacal liquor or sodium hydroxide saponification, then utilize single-stage steel basin or multi-stage solvent extraction groove and rare earth feed liquid to be uniformly mixed, strip liquor realizes rare earth with being separated of aluminium and recovering rare earth through oxalic acid precipitation again.The loss of this method rare earth extraction is comparatively large, and except aluminium effect is general, and the pH value of rare earth feed liquid must strictly control, otherwise easily cause system emulsification that extraction process cannot be carried out, in addition, use oxalic acid precipitation not only to increase production cost, too increase the difficulty of wastewater treatment.
The aluminum removing method of rare earth feed liquid disclosed in CN101979680A the organic phase of naphthenic acid-ol-kerosene composition is added in steel basin with rare earth feed liquid to mix, add ammoniacal liquor or NaOH stirring again, leave standstill after separate aqueous phase, organic phase again through persalt back extraction, oxalic acid precipitation strip liquor recovering rare earth.Though the method can control the emulsion of feed liquid, step is more, uses oxalic acid to precipitate strip liquor, too increases production cost and wastewater treatment difficulty.
Summary of the invention
For the above-mentioned defect existed in prior art, the present invention aims to provide a kind of easy and simple to handle, and production cost is lower, and the tractable earth solution of waste water is except aluminum technology scheme.
The present invention adopts naphthenic acid-RECl 3-HCl-kerosene system, realizes the separation of aluminium in rare earth feed liquid by the method for fractionation extraction.The present invention determines washing amount, the extraction quantity that earth solution carries out fractionation extraction, and extraction, washing and the progression of back extraction distribute, make the impurity aluminum in earth solution enter into load organic phases to greatest extent, realize being separated of aluminium and rare earth, finally obtain the earth solution that aluminium content is low.
The present invention is achieved through the following technical solutions:
A kind of method removing aluminium from rare earth feed liquid, use naphthenic acid: isooctyl alcohol: kerosene volume ratio is that the mixing solutions of 5 ~ 25%: 10 ~ 20%: 85 ~ 55% is as organic phase, it is characterized in that: first saponification is carried out to organic phase, organic phase saponification deg controls at 0.1 ~ 0.7mol/L, use the aluminium in the method rare-earth separating feed liquid of fractionation extraction again, fractionation extraction throughput ratio adopts organic phase: earth solution: washing lotion: anti-liquid volume ratio is 40 ~ 60: 100 ~ 200: 3 ~ 20: 1 ~ 3L/min; Described method middle-weight rare earths feed concentration REO is 1.6 ~ 1.77mol/L, wherein Al 2o 3be 0.003 ~ 0.03mol/L, washing lotion acidity is 0.1 ~ 3.0mol/L, and anti-liquid acidity is 1.0 ~ 4.5mol/L; Fractionation extraction progression is extraction section: washing section: stripping section equals 8: 10: 7; Extraction mixing-time is 5 ~ 10min, and mixing section and clarifying chamber's volume ratio are 1: 3 ~ 5; According to aforesaid method except after aluminium, rare earth yield reaches more than 99.98%.
Further, the rare earth feed liquid used in the method for the invention can be praseodymium chloride neodymium solution or chlorination sm-eu-gd solution.
Further, the anti-liquid used in the method for the invention is hydrochloric acid.
Further, the organic phase used in the method for the invention is naphthenic acid: isooctyl alcohol: kerosene volume ratio is 25%: 20%: 55%.
Further, the preferred 5min of extraction mixing-time in the method for the invention.
With the aluminium in the method for the invention rare-earth separating feed liquid, the Al in earth solution 3+be extracted in extraction process in organic phase, through back extraction with AlCl 3form is separated; Al more than rare earth in liquid 2o 3/ REO can effectively control below 0.005%.
The method of the invention exploitativeness is strong, remarkable in economical benefits, more existing single-stage extraction technique, and oxide compound per ton can save oxalic acid 25 kilograms, reduces discharging oxalate waste water 0.2m 3.To produce rare earth oxide 20000 tons every year, oxalic acid 100 tons can be saved, reduce discharging oxalate waste water 800m 3.
The present invention compared with prior art, achieves the fractionation extraction of rare earth and impurity aluminum, has got rid of the strip liquor oxalic acid precipitation recovering rare earth operation of single-stage extraction method, not only flow process shortens, good separating effect, rare earth yield is high, and produce waste water comparatively single-stage extraction more easily process; Owing to optimizing extractant condition, adopt first saponification organic phase, and then extract the fractionation extraction process of feed liquid, eliminate the emulsion in extraction, substantially increase the utilization ratio of equipment, and it is continuous more easily to realize production process, be convenient to same aftertreatment technology be connected, product cost is low.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1
In praseodymium neodymium rare earth feed liquid, REO is 1.68mol/L, Al 2o 3be 0.003 ~ 0.03mol/L.Adopt the method for fractionation extraction, first carry out saponification to organic phase, then extract above-mentioned feed liquid, fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
Organic phase saponification deg controls at 0.1 ~ 0.5mol/L;
Fractionation extraction throughput ratio is: organic phase: rare earth feed liquid: washing lotion: the volume ratio of anti-liquid is 40 ~ 60: 50 ~ 80: 3 ~ 20: 1 ~ 3L/min, and wherein washing lotion acidity is 0.1 ~ 3.0mol/L, and anti-liquid acidity is 1.0 ~ 4.5mol/L;
Fractionation extraction progression is assigned as: extraction section: washing section: stripping section progression ratio is 8: 10: 7;
Extraction mixing-time is 5min;
The volume ratio of mixing section and clarifying chamber is 1: 4.
Commerical test runs one month, and experimental result is that the praseodymium neodymium re chloride obtained after aluminium detects by analysis: rare earth concentration 1.48mol/L, Al 2o 3/ REO is 0.0035%, and namely rare earth yield is 99.99%.
Embodiment 2
In praseodymium neodymium rare earth feed liquid, REO is 1.68mol/L, Al 2o 3be 0.003 ~ 0.03mol/L.Adopt the method for fractionation extraction, first carry out saponification to organic phase, then extract above-mentioned feed liquid, fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
Organic phase saponification deg controls at 0.1 ~ 0.5mol/L;
Fractionation extraction throughput ratio is: organic phase: rare earth feed liquid: washing lotion: the volume ratio of anti-liquid is 40 ~ 60: 80 ~ 120: 3 ~ 20: 1 ~ 3L/min; Washing lotion acidity is 0.1 ~ 3.0mol/L, and anti-liquid acidity is 1.0 ~ 4.5mol/L;
Fractionation extraction progression is assigned as: extraction section: washing section: stripping section progression ratio is 8: 10: 7;
Extraction mixing-time is 5min;
The volume ratio of mixing section and clarifying chamber is 1: 4.
Commerical test runs one month, and experimental result is that the praseodymium neodymium re chloride obtained after aluminium detects by analysis: rare earth concentration 1.48mol/L, Al 2o 3/ REO is 0.0038%, and namely rare earth yield is 99.99%.
Embodiment 3
In praseodymium neodymium rare earth feed liquid, REO is 1.68mol/L, Al 2o 3be 0.003 ~ 0.03mol/L.Adopt the method for fractionation extraction, first carry out saponification to organic phase, then extract above-mentioned feed liquid, fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
Organic phase saponification deg controls at 0.1 ~ 0.5mol/L;
Fractionation extraction throughput ratio is: organic phase: rare earth feed liquid: washing lotion: the volume ratio of anti-liquid is 40 ~ 60: 120 ~ 200: 3 ~ 20: 1 ~ 3L/min; Washing lotion acidity is 0.1 ~ 3.0mol/L, and anti-liquid acidity is 1.0 ~ 4.5mol/L;
Fractionation extraction progression is assigned as: extraction section: washing section: stripping section is 8: 10: 7;
Extraction mixing-time is 5min;
The volume ratio of mixing section and clarifying chamber is 1: 4.
Commerical test runs one month, and experimental result is that the praseodymium neodymium re chloride obtained after aluminium detects by analysis: rare earth concentration 1.48mol/L, Al 2o 3/ REO is 0.0038%, and namely rare earth yield is 99.99%.
Embodiment 4
In sm-eu-gd re chloride, REO is 1.62mol/L, Al 2o 3for 0.0032mol/L.Adopt the method for fractionation extraction, first carry out saponification to organic phase, then extract above-mentioned feed liquid, fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
Organic phase saponification deg controls at 0.15 ~ 0.30mol/L;
Fractionation extraction throughput ratio is: organic phase: rare earth feed liquid: washing lotion: the volume ratio of anti-liquid is 50 ~ 80: 60 ~ 80: 10 ~ 18: 1 ~ 3L/min; Washing lotion acidity is 0.1 ~ 3.0mol/L, and anti-liquid acidity is 1.0 ~ 4.5mol/L;
Fractionation extraction progression is assigned as: extraction section: washing section: stripping section is 8: 10: 7;
Extraction mixing-time is 5min;
Experimental result is that the sm-eu-gd re chloride obtained after aluminium detects by analysis: rare earth concentration 1.53mol/L, Al 2o 3/ REO is 0.0176%, and namely rare earth yield is 99.98%.
Embodiment 5
In sm-eu-gd re chloride, REO is 1.62mol/L, Al 2o 3for 0.0032mol/L.Adopt the method for fractionation extraction, first carry out saponification to organic phase, then extract above-mentioned feed liquid, fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
Organic extractant phase naphthenic acid saponification deg controls at 0.15 ~ 0.30mol/L;
Fractionation extraction throughput ratio is: organic phase: rare earth feed liquid: washing lotion: the volume ratio of anti-liquid is 100 ~ 120: 60 ~ 80: 10 ~ 20: 1 ~ 3L/min; Washing lotion acidity is 0.1 ~ 3.0mol/L, and anti-liquid acidity is 1.0 ~ 4.5mol/L;
Fractionation extraction progression is assigned as: extraction section: washing section: stripping section is 8: 10: 7;
Extraction mixing-time is 5min;
Experimental result is that the sm-eu-gd re chloride obtained after aluminium detects by analysis: rare earth concentration 1.51mol/L, Al 2o 3/ REO is 0.016%, and namely rare earth yield is 99.98%.
Embodiment 6
In sm-eu-gd re chloride, REO is 1.62mol/L, Al 2o 3for 0.0032mol/L.Adopt the method for fractionation extraction, first carry out saponification to organic phase, then extract above-mentioned feed liquid, fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
Organic phase saponification deg controls at 0.15 ~ 0.30mol/L;
Fractionation extraction throughput ratio is: organic phase: rare earth feed liquid: washing lotion: the volume ratio of anti-liquid is 60 ~ 80: 100 ~ 120: 8 ~ 14: 1 ~ 3L/min; Washing lotion acidity is 0.1 ~ 3.0mol/L, and anti-liquid acidity is 1.0 ~ 4.5mol/L;
Fractionation extraction progression is assigned as: extraction section: washing section: stripping section is 8: 10: 7;
Extraction mixing-time is 5min;
Experimental result is that the sm-eu-gd re chloride obtained after aluminium detects by analysis: rare earth concentration 1.56mol/L, Al 2o 3/ REO is 0.042%, and namely rare earth yield is 99.98%.

Claims (7)

1. one kind is removed the method for aluminium from rare earth feed liquid, use naphthenic acid: isooctyl alcohol: kerosene volume ratio is that the mixing solutions of 25%:20%:55% is as organic phase, it is characterized in that: first saponification is carried out to organic phase, organic phase saponification deg controls at 0.1 ~ 0.7 mol/L, use the aluminium in the method rare-earth separating feed liquid of fractionation extraction again, fractionation extraction throughput ratio adopts organic phase: earth solution: washing lotion: anti-liquid volume ratio is 40 ~ 60:100 ~ 200:3 ~ 20:1 ~ 3L/min; Described method middle-weight rare earths feed concentration REO is 1.6 ~ 1.77mol/L, wherein Al 2o 3be 0.003 ~ 0.03 mol/L, washing lotion acidity is 0.1 ~ 3.0mol/L, and anti-liquid acidity is 1.0 ~ 4.5mol/L; Fractionation extraction progression is extraction section: washing section: stripping section equals 8:10:7; Extraction mixing-time is 5 ~ 10min, and mixing section and clarifying chamber's volume ratio are 1:3 ~ 5; According to aforesaid method except after aluminium, rare earth yield reaches more than 99.98%.
2. the method removing aluminium from rare earth feed liquid as claimed in claim 1, is characterized in that: described rare earth feed liquid can be praseodymium chloride neodymium solution.
3. the method removing aluminium from rare earth feed liquid as claimed in claim 2, is characterized in that: described organic phase saponification deg is 0.1 ~ 0.5mol/L.
4. the method removing aluminium from rare earth feed liquid as claimed in claim 1, is characterized in that: described rare earth feed liquid can be samarium trichloride europium gadolinium solution.
5. the method removing aluminium from rare earth feed liquid as claimed in claim 4, is characterized in that: described organic phase saponification deg is 0.15 ~ 0.30mol/L.
6. the method removing aluminium from rare earth feed liquid as described in claim 1,2 or 4, is characterized in that: described anti-liquid is hydrochloric acid.
7. the method removing aluminium from rare earth feed liquid according to any one of claim 1-5, is characterized in that: described extraction mixing-time is 5min.
CN201310115296.7A 2013-04-07 2013-04-07 Method for removing aluminum in rare-earth solution Active CN103146921B (en)

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CN103773955B (en) * 2013-11-04 2016-08-31 中铝广西有色金源稀土股份有限公司 A kind of remove the method for aluminium in rare earth feed liquid
CN103966441A (en) * 2014-05-08 2014-08-06 广东省工业技术研究院(广州有色金属研究院) Method for continuously extracting aluminum from rare earth liquid
CN104372186B (en) * 2014-10-28 2016-08-24 江西稀有金属钨业控股集团有限公司 The abstraction impurity removal method of mischmetal feed liquid and system
CN107522222A (en) * 2017-09-29 2017-12-29 吉安鑫泰科技股份有限公司 A kind of new technology for precipitating praseodymium chloride neodymium
CN110438351A (en) * 2019-08-29 2019-11-12 中稀(常州)稀土新材料有限公司 A kind of rare earth impurities separation method
CN110964913A (en) * 2019-12-25 2020-04-07 中稀(常州)稀土新材料有限公司 Method for preparing praseodymium-neodymium enrichment by adopting light soda ash precipitation
CN111944998A (en) * 2020-08-25 2020-11-17 赣州有色冶金研究所 Method for removing aluminum from rare earth feed liquid
CN115287474B (en) * 2022-08-10 2023-07-14 吉水金诚新材料加工有限公司 Method for removing aluminum ions from praseodymium chloride neodymium feed liquid

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