CN103146921A - Method for removing aluminum in rare-earth solution - Google Patents

Method for removing aluminum in rare-earth solution Download PDF

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CN103146921A
CN103146921A CN2013101152967A CN201310115296A CN103146921A CN 103146921 A CN103146921 A CN 103146921A CN 2013101152967 A CN2013101152967 A CN 2013101152967A CN 201310115296 A CN201310115296 A CN 201310115296A CN 103146921 A CN103146921 A CN 103146921A
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rare earth
feed liquid
organic phase
aluminium
extraction
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CN103146921B (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 of removing aluminium in earth solution
Technical field
The present invention relates to a kind of method of 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.Produce at present upper aluminum removing method commonly used and mainly contain alkaline process, acid system, hydrolysis method, extraction process etc.Wherein traditional extraction process is the organic phase system that forms 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 mix, strip liquor again through oxalic acid precipitation realize rare earth with separating of aluminium recovering rare earth.The loss of this method rare earth extraction is larger, removes the aluminium effect general, and the pH value of rare earth feed liquid must strictly be controlled, otherwise easily cause system emulsification that extraction process can't be carried out, in addition, use oxalic acid precipitation not only to increase production cost, also increased the difficulty of wastewater treatment.
In CN101979680A, disclosed rare earth feed liquid aluminum removing method is the organic phase that naphthenic acid-alcohol-kerosene forms to be added in steel basin with rare earth feed liquid mix, add again ammoniacal liquor or NaOH to stir, tell water after standing, organic phase is again through the persalt back extraction, oxalic acid precipitation strip liquor recovering rare earth.Though the method can be controlled the emulsion of feed liquid, step is more, uses oxalic acid that strip liquor is precipitated, and has also increased production cost and wastewater treatment difficulty.
Summary of the invention
For the defects that exists 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 the 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 has determined that earth solution carries out washing amount, the extraction quantity of fractionation extraction, and the progression of extraction, washing and back extraction distributes, make the impurity aluminum in earth solution enter into to greatest extent load organic phases, realize separating of aluminium and rare earth, finally obtain the low earth solution of aluminium content.
The present invention is achieved through the following technical solutions:
A kind of method of removing aluminium from rare earth feed liquid, use naphthenic acid: isooctyl alcohol: the kerosene volume ratio is 5～25%: 10～20%: 85～55% mixing solutions is as organic phase, it is characterized in that: first organic phase is carried out saponification, the organic phase saponification deg is controlled at 0.1～0.7mol/L, use the aluminium in the method rare-earth separating feed liquid of fractionation extraction, the 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 again; 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; Except after aluminium, rare earth yield reaches more than 99.98% according to aforesaid method.
Further, the rare earth feed liquid that uses in the method for the invention can be praseodymium chloride neodymium solution or chlorination sm-eu-gd solution.
Further, the anti-liquid that uses in the method for the invention is hydrochloric acid.
Further, the organic phase of using in the method for the invention is naphthenic acid: isooctyl alcohol: the 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 in the remaining liquid of rare earth 2O 3/ REO can effectively be controlled at below 0.005%.
The method of the invention exploitativeness is strong, remarkable in economical benefits, and more existing single-stage extraction technique, oxide compound per ton can be saved 25 kilograms of oxalic acid, reduces discharging oxalate waste water 0.2m 3To produce 20000 tons of rare earth oxides every year, can save 100 tons of oxalic acid, reduce discharging oxalate waste water 800m 3
The present invention has compared with prior art realized 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 the waste water that produces is more easily processed than single-stage extraction; Owing to having optimized extractant condition, adopt first saponification organic phase, and then the fractionation extraction process of extraction feed liquid, eliminated the emulsion in the extraction, greatly improved the utilization ratio of equipment, and realized that more easily production process is continuous, be convenient to be connected with aftertreatment technology, product cost is low.
Description of drawings
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 organic phase is carried out saponification, then extract above-mentioned feed liquid, the fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
The organic phase saponification deg is controlled at 0.1～0.5mol/L;
The 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, 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 operation one month, experimental result is for detecting by analysis except the praseodymium neodymium re chloride that obtains after aluminium: 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 organic phase is carried out saponification, then extract above-mentioned feed liquid, the fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
The organic phase saponification deg is controlled at 0.1～0.5mol/L;
The 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 operation one month, experimental result is for detecting by analysis except the praseodymium neodymium re chloride that obtains after aluminium: 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 organic phase is carried out saponification, then extract above-mentioned feed liquid, the fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
The organic phase saponification deg is controlled at 0.1～0.5mol/L;
The 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 operation one month, experimental result is for detecting by analysis except the praseodymium neodymium re chloride that obtains after aluminium: rare earth concentration 1.48mol/L, Al 2O 3/ REO is 0.0038%, and namely rare earth yield is 99.99%.
Embodiment 4
In the sm-eu-gd re chloride, REO is 1.62mol/L, Al 2O 3Be 0.0032mol/L.Adopt the method for fractionation extraction, first organic phase is carried out saponification, then extract above-mentioned feed liquid, the fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
The organic phase saponification deg is controlled at 0.15～0.30mol/L;
The 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 for detecting by analysis except the sm-eu-gd re chloride that obtains after aluminium: rare earth concentration 1.53mol/L, Al 2O 3/ REO is 0.0176%, and namely rare earth yield is 99.98%.
Embodiment 5
In the sm-eu-gd re chloride, REO is 1.62mol/L, Al 2O 3Be 0.0032mol/L.Adopt the method for fractionation extraction, first organic phase is carried out saponification, then extract above-mentioned feed liquid, the 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 degree is controlled at 0.15～0.30mol/L;
The 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 for detecting by analysis except the sm-eu-gd re chloride that obtains after aluminium: rare earth concentration 1.51mol/L, Al 2O 3/ REO is 0.016%, and namely rare earth yield is 99.98%.
Embodiment 6
In the sm-eu-gd re chloride, REO is 1.62mol/L, Al 2O 3Be 0.0032mol/L.Adopt the method for fractionation extraction, first organic phase is carried out saponification, then extract above-mentioned feed liquid, the fractionation extraction process condition is:
Organic phase is formulated as: naphthenic acid: isooctyl alcohol: the volume ratio of kerosene is 25%: 20%: 55%;
The organic phase saponification deg is controlled at 0.15～0.30mol/L;
The 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 for detecting by analysis except the sm-eu-gd re chloride that obtains after aluminium: rare earth concentration 1.56mol/L, Al 2O 3/ REO is 0.042%, and namely rare earth yield is 99.98%.

Claims (8)

  1. One kind from rare earth feed liquid except the method for aluminium, use naphthenic acid: isooctyl alcohol: the kerosene volume ratio is 5～25%: 10～20%: 85～55% mixing solutions is as organic phase, it is characterized in that: first organic phase is carried out saponification, the organic phase saponification deg is controlled at 0.1～0.7mol/L, use the aluminium in the method rare-earth separating feed liquid of fractionation extraction, the 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 again; 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; Except after aluminium, rare earth yield reaches more than 99.98% according to aforesaid method.
  2. As claimed in claim 1 from rare earth feed liquid except the method for aluminium, it is characterized in that: described rare earth feed liquid can be the wrong neodymium solution of chlorination.
  3. As claimed in claim 2 from rare earth feed liquid except the method for aluminium, it is characterized in that: described organic phase saponification deg is 0.1～0.5mol/L.
  4. As claimed in claim 1 from rare earth feed liquid except the method for aluminium, it is characterized in that: described rare earth feed liquid can be samarium trichloride europium gadolinium solution.
  5. As claimed in claim 4 from rare earth feed liquid except the method for aluminium, it is characterized in that: described organic phase saponification deg is 0.15～0.30mol/L.
  6. 6. as claim 1, the 2 or 4 described methods of removing aluminium from rare earth feed liquid, it is characterized in that: described anti-liquid is hydrochloric acid.
  7. 7. as claim 1, the 2 or 4 described methods of removing aluminium from rare earth feed liquid, it is characterized in that: described organic phase is naphthenic acid: isooctyl alcohol: the kerosene volume ratio is 25%: 20%: 55%.
  8. As claimed in claim 7 from rare earth feed liquid except the method for aluminium, it is characterized in that: described extraction mixing-time is 5min.
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Cited By (8)

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CN103773955A (en) * 2013-11-04 2014-05-07 中铝广西有色金源稀土股份有限公司 Method for removing aluminium in tombarthite 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
CN104372186A (en) * 2014-10-28 2015-02-25 江西稀有金属钨业控股集团有限公司 Extraction and impurity removal method and system for mixed rare earth liquor
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
CN115287474A (en) * 2022-08-10 2022-11-04 吉水金诚新材料加工有限公司 Method for removing aluminum ions from praseodymium-neodymium chloride feed liquid

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103773955A (en) * 2013-11-04 2014-05-07 中铝广西有色金源稀土股份有限公司 Method for removing aluminium in tombarthite feed liquid
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
CN104372186A (en) * 2014-10-28 2015-02-25 江西稀有金属钨业控股集团有限公司 Extraction and impurity removal method and system for mixed rare earth liquor
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
CN115287474A (en) * 2022-08-10 2022-11-04 吉水金诚新材料加工有限公司 Method for removing aluminum ions from praseodymium-neodymium chloride 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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