CN108893625B - Process for preparing high-purity lanthanum by extraction method - Google Patents
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Abstract
The invention relates to a process for preparing high-purity lanthanum by an extraction method, which comprises the steps of taking a 3N industrial-grade lanthanum chloride aqueous solution as a feed liquid and P204-TBP as a composite extractant, and concretely comprises five steps of fractional extraction and separation of NaMgCaBaPbZnLa/LaCePrNdAlSmFe, fractional extraction and separation of NaMgCaBaPbZn/La, fractional extraction and separation of La/CePrNdAlSmFe, and a back extraction section 1 and a back extraction section 2. By implementing the process, the separation of lanthanum from cerium, praseodymium, neodymium, samarium, iron, aluminum, zinc, lead, barium, calcium, magnesium, sodium and other metal elements can be smoothly realized, and the relative purity of the high-purity lanthanum chloride solution is 99.9991-99.9998%. The method has the characteristics of short process flow, less reagent consumption, low production cost, high purity of lanthanum chloride products, high yield of lanthanum and the like.
Description
Technical Field
The invention relates to a process for preparing high-purity lanthanum by an extraction method, which specifically comprises the steps of taking a 3N industrial-grade lanthanum chloride aqueous solution as a feed liquid, taking P204-TBP as a composite extractant, and separating a target element lanthanum from metal impurity elements such as cerium, praseodymium, neodymium, samarium, iron, aluminum, zinc, lead, barium, calcium, magnesium, sodium and the like by a fractional extraction process to prepare the lanthanum chloride with the relative purity of 99.9991-99.9998%. The invention belongs to the technical field of preparing high-purity lanthanum chloride by a fractional extraction method.
Background
With the development of science and technology, the demand of high-purity lanthanum products is increasing. Lanthanum chloride with the purity of more than or equal to 99.999 percent is not only an important high-purity lanthanum product, but also one of basic raw materials for preparing other high-purity lanthanum products. For example, high-purity lanthanum carbonate can be obtained by taking a high-purity lanthanum chloride solution as a lanthanum source and precipitating with ammonium bicarbonate, and high-purity lanthanum oxide can be obtained by burning; the high-purity lanthanum metal can be prepared by electrolyzing anhydrous high-purity lanthanum chloride or thermally reducing high-purity lanthanum oxide. High-purity lanthanum oxide and high-purity metal lanthanum have extremely important application in various fields.
In 1989, chinese patent application No. 89103773.X proposed: the lanthanum-rich lanthanum in medium yttrium is used as a rare earth raw material, naphthenic acid is used for extraction and grouping, and then three P507 outlets are used for separating lanthanum-yttrium mixed rare earth, so that a lanthanum product with the purity of 4N grade (99.99 percent) can be obtained. The main technical content of application No. 89103773.X is the separation between lanthanum and yttrium and other rare earth elements, and the separation between lanthanum and yttrium, respectively.
In 2007, chinese patent with application number 200710019946.2 proposed: lanthanum enrichment is used as a lanthanum raw material, an ultrasonic fractionation extraction method is adopted, TBP extraction separation and impurity removal are carried out in a nitric acid system through a solid adsorbent, and a lanthanum product with the purity of 4N grade (99.99%) can be prepared. The main separation technology content of application No. 200710019946.2 is separation of lanthanum and praseodymium neodymium, adsorption and impurity removal (specific adsorption and removal of impurities, which is not detailed in the original text) by an adsorbent (activated carbon or ion exchange resin).
In 2013, a Chinese patent with the application number of 201310686894.X proposes: A2N-grade lanthanum compound is used as a lanthanum raw material, a saponification cascade extraction method is adopted, calcium and lanthanum are separated through P507 extraction in a hydrochloric acid system, and a lanthanum product with the purity of 99.9995% can be prepared. The main separation technology content of application No. 201310686894.X is the separation of lanthanum from calcium.
In 2017, chinese patent with application number 201710797893.0 proposed: lanthanum chloride is used as a lanthanum raw material, an ultrasonic extraction method is adopted, lanthanum is extracted from a P507 organic phase modified by 1,2, 5-thiadiazole-3, 4-mercaptan in a hydrochloric acid system, and then lanthanum is back extracted by oxalic acid, so that a lanthanum product with the purity of 99.999 percent can be prepared. The main separation technique of application No. 201710797893.0 is the separation of lanthanum from the difficult-to-extract impurities (specific ones, which are not detailed).
In fact, the preparation of 5N grade lanthanum products, the key separation techniques, involves the separation of lanthanum from rare earth impurities (cerium, praseodymium and neodymium as the main rare earth impurities), and lanthanum from non-rare earth impurities (iron, aluminum, zinc, lead, barium, calcium, magnesium, sodium as the main non-rare earth impurities). In the existing technical scheme for preparing 5N-grade lanthanum products, the separation of lanthanum and rare earth impurities and the separation of lanthanum and non-rare earth metal element impurities are realized by a plurality of different separation processes. Therefore, the existing 5N grade lanthanum product preparation has the defects of multiple processes, complex process, high cost and the like.
Aiming at the defects of the prior art for preparing 5N-level lanthanum products, the invention establishes a simple and efficient method for separating impurities such as cerium, praseodymium, neodymium, samarium, iron, aluminum, zinc, lead, barium, calcium, magnesium, sodium and the like in industrial 3N-level lanthanum chloride solution, and prepares the 5N-level lanthanum chloride solution in one separation process.
Disclosure of Invention
The invention provides a process for preparing high-purity lanthanum by an extraction method, which aims at the defects of the existing process for preparing 5N-grade high-purity lanthanum chloride and provides a method for preparing 5N-grade lanthanum chloride from 3N industrial-grade lanthanum chloride feed liquid.
The 3N industrial grade lanthanum chloride aqueous solution is used as feed liquid, di (2-ethylhexyl) phosphoric acid (P204 for short) is used as an extracting agent, and the extracting agent consists of fractional extraction separation of NaMgCaBaPbZnLa/LaCePrNdAlSmFe, fractional extraction separation of NaMgCaBaPbZn/La and fractional extraction separation of La/CePrNdAlSmFe; the NaMgCaBaPbZn/La separation and the La/CePrNdAlSmFe separation are connected in series, an organic phase with lanthanum loaded on an outlet organic phase of the NaMgCaBaPbZn/La separation is fractionated and extracted to serve as an extraction organic phase of the La/CePrNdAlSmFe separation, and an outlet water phase 5N-grade lanthanum chloride of the La/CePrNdAlSmFe separation is fractionated and extracted to serve as a washing agent of the La/CePrNdAlSmFe separation; thereby realizing the separation of lanthanum from metal elements such as cerium, praseodymium, neodymium, samarium, iron, aluminum, zinc, lead, barium, calcium, magnesium, sodium and the like, and preparing 5N-level lanthanum chloride.
The invention relates to a process for preparing high-purity lanthanum by an extraction method, which takes a 3N industrial-grade lanthanum chloride aqueous solution as a feed liquid and P204-TBP as a composite extractant, and consists of 3 fractional extraction steps and 2 back extraction steps: the 3 fractional extraction steps are fractional extraction separation of NaMgCaBaPbZnLa/LaCePrNdAlSmFe, fractional extraction separation of NaMgCaBaPbZn/La and fractional extraction separation of La/CePrNdAlSmFe respectively; the 2 back extraction steps are respectively a back extraction section 1 and a back extraction section 2;
the outlet organic phase of the NaMgCaBaPbZn/La separated by fractional extraction directly enters the 1 st stage of the La/CePrNdAlSmFe separated by fractional extraction, and the 1 st stage outlet aqueous phase of the La/CePrNdAlSmFe separated by fractional extraction is used as a washing agent for separating the NaMgCaBaPbZn/La by fractional extraction;
the process comprises the following specific steps:
step 1: fractional extraction and separation of NaMgCaBaPbZnLa/LaCePrNdAlSmFe
A P204-TBP organic phase is taken as an extraction organic phase, a 3N industrial grade lanthanum chloride aqueous solution is taken as a lanthanum chloride feed liquid, and 1.5mol/LHCl is taken as a washing acid. The P204-TBP organic phase enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 1 st stage, the lanthanum chloride feed liquid enters the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the feeding stage, and 1.5mol/LHCl washing acid enters the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the last 1 st stage. The extraction section of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system realizes the separation of NaMgCaBaPbZn/La, and the washing section realizes the separation of La/CePrNdAlSmFe. Obtaining a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn from a grade 1 outlet water phase of a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and using the lanthanum chloride aqueous solution as a feed liquid for fractional extraction separation of NaMgCaBaPbZn/La; and obtaining a loaded LaCePrNdAlSmFe organic phase from the final stage 1 outlet organic phase of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and using the loaded LaCePrNdAlSmFe organic phase as feed liquid for fractional extraction and separation of La/CePrNdAlSmFe.
Step 2: fractional extraction separation of NaMgCaBaPbZn/La
Taking a P204-TBP organic phase as an extraction organic phase, obtaining a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn as a feed liquid by using a No. 1 outlet water phase of a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and obtaining 5N grade lanthanum chloride LaCl by performing fractional extraction and separation on the La/CePrNdAlSmFe No. 1 outlet water phase3The aqueous solution of (a) is a detergent. The P204-TBP organic phase enters a NaMgCaBaPbZn/La fractionation extraction system from the 1 st stage, a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn enters the NaMgCaBaPbZn/La fractionation extraction system from the feeding stage, and a 5N-level lanthanum chloride detergent enters the NaMgCaBaPbZn/La fractionation extraction system from the last 1 st stage. And obtaining a mixed solution containing sodium chloride, magnesium chloride, calcium chloride, barium chloride, lead chloride, zinc chloride, lanthanum chloride and hydrochloric acid from the water phase at the 1 st stage outlet of the NaMgCaBaPbZn/La fractional extraction system, and recycling lanthanum. Obtaining a P204-TBP organic phase loaded with lanthanum from the final stage 1 outlet organic phase of the NaMgCaBaPbZn/La fractional extraction system, and using the P204-TBP organic phase as lanthanum saponification P204-TBP extraction organic phase for fractional extraction and separation of La/CePrNdAlSmFe.
And step 3: fractional extraction and separation of La/CePrNdAlSmFe
A lanthanum-loaded P204-TBP organic phase obtained from the last 1-stage outlet organic phase of a NaMgCaBaPbZn/La fractional extraction system is taken as a lanthanum saponification P204-TBP extraction organic phase, a LaCePrNdAlSmFe-loaded organic phase obtained from the last 1-stage outlet organic phase of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system is taken as feed liquid, and 1.5mol/L of HCl is taken as washing acid. The lanthanum saponification P204-TBP extraction organic phase enters a La/CePrNdAlSmFe fractional extraction system from the 1 st stage, the loaded LaCePrNdAlSmFe organic phase enters the La/CePrNdAlSmFe fractional extraction system from the feeding stage, and 1.5mol/L HCl washing acid enters the La/CePrNdAlSmFe fractional extraction system from the last 1 st stage. And obtaining 5N-grade lanthanum chloride aqueous solution from the 1 st-grade outlet water phase of the La/CePrNdAlSmFe fractional extraction system, and taking the aqueous solution as a target separation product, namely high-purity lanthanum. And obtaining a loaded CePrNdAlSmFe organic phase from the organic phase at the last stage 1 of the La/CePrNdAlSmFe fractional extraction system, and transferring the loaded CePrNdAlSmFe organic phase to a stripping section 1 for treatment.
And 4, step 4: stripping section 1
And 3mol/L HCl is used as stripping acid, and 9-stage countercurrent stripping is carried out on the loaded CePrNdAlSmFe organic phase. The water phase at the back extraction outlet is a mixture solution containing cerium chloride, praseodymium chloride, neodymium chloride, aluminum chloride, samarium chloride, iron calcium chloride and hydrochloric acid, and is used for recovering rare earth in the mixture solution. The organic phase outlet is a P204-TBP organic phase with residual iron and aluminum, and the organic phase is transferred to a stripping section 2 for treatment.
And 5: stripping section 2
And (3) carrying out 6-stage countercurrent stripping on the P204-TBP organic phase of the residual iron and aluminum by taking 1mol/L ammonium bifluoride as a stripping agent. The water phase at the back extraction outlet is waste liquid containing iron and aluminum, and is discharged after being neutralized by lime. The organic phase outlet is a P204-TBP organic phase which is recycled.
The P204-TBP organic phase is sulfonated kerosene solution of extracting agent P204 and TBP, wherein the volume percentage of P204 is 30%, the volume percentage of TBP is 15%, and the volume percentage of sulfonated kerosene solution is 55%.
The 3N industrial grade lanthanum chloride aqueous solution is an aqueous solution containing lanthanum chloride, and comprises the following components: Na0.0050g/L-0.020 g/L, Mg 0.0050 g/L-0.020 g/L, Ca0.010 g/L-0.050 g/L, Ba0.0050g/L-0.020 g/L, Pb 0.0020 g/L-0.010 g/L, Zn 0.0050 g/L-0.020 g/L, La135.0g/L-145.0 g/L, Ce 0.020 g/L-0.080 g/L, Pr0.010 g/L-0.030 g/L, Nd0.0050g/L-0.0050 g/L, Al 0.0050 g/L-0.010 g/L, Sm 0.0050 g/L-0.010 g/L and Fe0g/L-0.005010 g/L.
The 5N-level lanthanum chloride aqueous solution comprises the following components: na 0.000015 g/L-0.000048 g/L, Mg0.000016g/L-0.000067 g/L, Ca0.000035 g/L-0.00015 g/L, Ba 0.000019 g/L-0.000063 g/L, Pb 0.0000078 g/L-0.000032 g/L, Zn 0.000020 g/L-0.000070 g/L, La67.50g/L-72.50 g/L, Ce0.000080 g/L-0.00056 g/L, Pr 0.000040 g/L-0.000068 g/L, Nd0.000020g/L-0.000022 g/L, Al0.000020 g/L-0.000021 g/L, Sm 0.000019 g/L-0.000020 g/L, and Fe0.000019 g/L-0.000020 g/L.
The invention has the beneficial effects that: 1) the purity of the separated lanthanum chloride product is high. The process can separate and remove rare earth impurities in the raw materials, the relative purity of the target product lanthanum chloride solution is 99.9991-99.9998%, and non-rare earth impurities in the raw materials, including sodium, magnesium, calcium, barium, lead, zinc, aluminum, iron and non-metal impurities (such as phosphate radical, sulfate radical and the like), can be separated and removed. 2) The yield of lanthanum is high, and the yield of lanthanum in the process is as high as 97-99%. Obtaining a mixed solution containing sodium chloride, magnesium chloride, calcium chloride, barium chloride, lead chloride, zinc chloride, lanthanum chloride and hydrochloric acid from a water phase at the 1 st stage outlet of a NaMgCaBaPbZn/La fractional extraction system, and recovering lanthanum from the mixed solution by adopting a quicklime neutralization method. The water phase at the back extraction outlet of the back extraction section 1 is a mixture solution containing cerium chloride, praseodymium chloride, neodymium chloride, aluminum chloride, samarium chloride, iron calcium chloride and hydrochloric acid, and rare earth elements in the water phase can be recovered by an oxalic acid precipitation method. For recovering rare earth therefrom. 3) The reagent consumption is low. The organic phase extracted by the composite extractant P204-TBP for separating NaMgCaBaPbZnLa/LaCePrNdAlSmFe by fractional extraction does not need saponification, so that the consumption of an alkaline saponifier for separating NaMgCaBaPbZnLa/LaCePrNdAlSmFe by fractional extraction is saved; the organic phase extracted by the composite extractant P204-TBP for separating NaMgCaBaPbZn/La by fractional extraction does not need saponification, so that the consumption of an alkaline saponifier for separating NaMgCaBaPbZn/La by fractional extraction is saved; the outlet organic phase of the NaMgCaBaPbZn/La separated by fractional extraction directly enters the 1 st stage of the La/CePrNdAlSmFe separated by fractional extraction, so that the consumption of an alkaline saponifier for separating the La/CePrNdAlSmFe by fractional extraction is saved; the water phase at the 1 st stage outlet of the La/CePrNdAlSmFe fractional extraction separation is used as a washing agent for the NaMgCaBaPbZn/La fractional extraction separation, so that the consumption of acid washing for the NaMgCaBaPbZn/La fractional extraction separation is saved. The composite extractant P204-TBP can be used for extracting organic phase circularly. 4) Short process flow, simple equipment, simple and convenient operation, good operation environment and contribution to large-scale industrial production. 5) The production cost is low. The fractional extraction system does not require the consumption of alkaline saponification reagents such as sodium hydroxide, ammonia, and the like.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The process for preparing high purity lanthanum by extraction according to the present invention is further described below with reference to the following specific examples.
Example 1
P204-TBP organic phase: extracting agent P204 and TBP, wherein the volume percentage of P204 is 30%, the volume percentage of TBP is 15%, and the volume percentage of sulfonated kerosene solution is 55%.
Lanthanum chloride feed liquid: the 3N industrial grade lanthanum chloride aqueous solution comprises 0.020g/L of Na, 0.020g/L of Mg, 0.050g/L of Ca0.050g/L, 0.020g/L of Ba, 0.010g/L of Pb, 0.020g/L of Zn, 145.0g/L of La, 0.080g/L of Ce, 0.030g/L of Pr0.010g/L of Nd, 0.010g/L of Al, 0.010g/L of Sm and 0.010g/L of Fe.
Step 1: fractional extraction and separation of NaMgCaBaPbZnLa/LaCePrNdAlSmFe
The P204-TBP organic phase enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 1 st stage, the lanthanum chloride feed liquid enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 12 th stage, and 1.5mol/L HCl washing acid enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 42 th stage. The extraction section of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system realizes the separation of NaMgCaBaPbZn/La, and the washing section realizes the separation of La/CePrNdAlSmFe. Obtaining a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn from a grade 1 outlet water phase of a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and using the lanthanum chloride aqueous solution as a feed liquid for fractional extraction separation of NaMgCaBaPbZn/La; and obtaining a loaded LaCePrNdAlSmFe organic phase from a 42 th-stage outlet organic phase of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and using the loaded LaCePrNdAlSmFe organic phase as feed liquid for fractional extraction and separation of La/CePrNdAlSmFe.
Step 2: fractional extraction separation of NaMgCaBaPbZn/La
Using a P204-TBP organic phase as an extraction organic phase, and fractionating NaMgCaBaPbZnLa/LaCePrNdAlSmFeObtaining lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn as feed liquid from the 1 st level outlet water phase of the extraction system, and obtaining 5N level lanthanum chloride LaCl from the 1 st level outlet water phase of La/CePrNdAlSmFe through fractional extraction and separation3The aqueous solution of (a) is a detergent. The P204-TBP organic phase enters a NaMgCaBaPbZn/La fractional extraction system from the 1 st stage, a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn enters the NaMgCaBaPbZn/La fractional extraction system from the 10 th stage, and a 5N-grade lanthanum chloride detergent enters the NaMgCaBaPbZn/La fractional extraction system from the 64 th stage. And obtaining a mixed solution containing sodium chloride, magnesium chloride, calcium chloride, barium chloride, lead chloride, zinc chloride, lanthanum chloride and hydrochloric acid from the water phase at the 1 st stage outlet of the NaMgCaBaPbZn/La fractional extraction system, and recycling lanthanum. Obtaining a P204-TBP organic phase loaded with lanthanum from a 64 th-stage outlet organic phase of a NaMgCaBaPbZn/La fractional extraction system, and using the P204-TBP organic phase as a lanthanum saponification P204-TBP extraction organic phase for fractional extraction and separation of La/CePrNdAlSmFe.
And step 3: fractional extraction and separation of La/CePrNdAlSmFe
A lanthanum-loaded P204-TBP organic phase obtained from the last 1-stage outlet organic phase of a NaMgCaBaPbZn/La fractional extraction system is taken as a lanthanum saponification P204-TBP extraction organic phase, a LaCePrNdAlSmFe-loaded organic phase obtained from the last 1-stage outlet organic phase of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system is taken as feed liquid, and 1.5mol/L of HCl is taken as washing acid. The lanthanum saponification P204-TBP extraction organic phase enters a La/CePrNdAlSmFe fractional extraction system from the level 1, the loaded LaCePrNdAlSmFe organic phase enters a La/CePrNdAlSmFe fractional extraction system from the level 50, and 1.5mol/L HCl washing acid enters the La/CePrNdAlSmFe fractional extraction system from the level 76. And obtaining 5N-grade lanthanum chloride aqueous solution from the 1 st-grade outlet water phase of the La/CePrNdAlSmFe fractional extraction system to obtain the target separation product high-purity lanthanum. And obtaining a loaded CePrNdAlSmFe organic phase from the 76 th grade outlet organic phase of the La/CePrNdAlSmFe fractional extraction system, and transferring the loaded CePrNdAlSmFe organic phase to a stripping section 1 for treatment.
And 4, step 4: stripping section 1
And 3mol/L HCl is used as stripping acid, and 9-stage countercurrent stripping is carried out on the loaded CePrNdAlSmFe organic phase. The water phase at the back extraction outlet is a mixture solution containing cerium chloride, praseodymium chloride, neodymium chloride, aluminum chloride, samarium chloride, iron calcium chloride and hydrochloric acid, and is used for recovering rare earth in the mixture solution. The organic phase outlet is a P204-TBP organic phase with residual iron and aluminum, and the organic phase is transferred to a stripping section 2 for treatment.
And 5: stripping section 2
And (3) carrying out 6-stage countercurrent stripping on the P204-TBP organic phase of the residual iron and aluminum by taking 1mol/L ammonium bifluoride as a stripping agent. The water phase at the back extraction outlet is waste liquid containing iron and aluminum, and is discharged after the lime neutralization treatment. The organic phase outlet is a P204-TBP organic phase which is recycled.
Target isolated product: 5N grade lanthanum chloride aqueous solution, which comprises the following components: na 0.000048g/L, Mg0.000067g/L, Ca 0.00015g/L, Ba 0.000063g/L, Pb 0.000032g/L, Zn 0.000070g/L, La 72.50g/L, Ce0.00056g/L, Pr 0.000068g/L, Nd 0.000022g/L, Al 0.000021g/L, Sm 0.000020g/L and Fe0.000021g/L. The relative purity of the aqueous solution of lanthanum chloride grade 5N was 99.9991%. The yield of lanthanum was 97%.
Example 2
P204-TBP organic phase: extracting agent P204 and TBP, wherein the volume percentage of P204 is 30%, the volume percentage of TBP is 15%, and the volume percentage of sulfonated kerosene solution is 55%.
Lanthanum chloride feed liquid: the 3N industrial grade lanthanum chloride aqueous solution comprises 0.012g/L of Na, 0.010g/L of Mg, 0.030g/L of Ca0.030g/L, 0.010g/L of Ba, 0.0050g/L of Pb, 0.010g/L of Zn, 140.0g/L of La, 0.050g/L of Ce, Pr0.020g/L, 0.0080g/L of Nd, 0.0080g/L of Al, 0.0070g/L of Sm and 0.0070g/L of Fe.
Step 1: fractional extraction and separation of NaMgCaBaPbZnLa/LaCePrNdAlSmFe
The P204-TBP organic phase enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 1 st stage, the lanthanum chloride feed liquid enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 12 th stage, and 1.5mol/L HCl washing acid enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 40 th stage. The extraction section of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system realizes the separation of NaMgCaBaPbZn/La, and the washing section realizes the separation of La/CePrNdAlSmFe. Obtaining a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn from a grade 1 outlet water phase of a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and using the lanthanum chloride aqueous solution as a feed liquid for fractional extraction separation of NaMgCaBaPbZn/La; and obtaining a loaded LaCePrNdAlSmFe organic phase from a 40 th-stage outlet organic phase of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and using the loaded LaCePrNdAlSmFe organic phase as feed liquid for fractional extraction and separation of La/CePrNdAlSmFe.
Step 2: fractional extraction separation of NaMgCaBaPbZn/La
Taking a P204-TBP organic phase as an extraction organic phase, obtaining a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn as a feed liquid by using a No. 1 outlet water phase of a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and obtaining 5N grade lanthanum chloride LaCl by performing fractional extraction and separation on the La/CePrNdAlSmFe No. 1 outlet water phase3The aqueous solution of (a) is a detergent. The P204-TBP organic phase enters a NaMgCaBaPbZn/La fractional extraction system from the 1 st stage, a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn enters the NaMgCaBaPbZn/La fractional extraction system from the 10 th stage, and a 5N-grade lanthanum chloride detergent enters the NaMgCaBaPbZn/La fractional extraction system from the 62 nd stage. And obtaining a mixed solution containing sodium chloride, magnesium chloride, calcium chloride, barium chloride, lead chloride, zinc chloride, lanthanum chloride and hydrochloric acid from the water phase at the 1 st stage outlet of the NaMgCaBaPbZn/La fractional extraction system, and recycling lanthanum. Obtaining a P204-TBP organic phase loaded with lanthanum from the outlet organic phase of the 62 th stage of the NaMgCaBaPbZn/La fractional extraction system, and using the P204-TBP organic phase as lanthanum saponification P204-TBP extraction organic phase for fractional extraction and separation of La/CePrNdAlSmFe.
And step 3: fractional extraction and separation of La/CePrNdAlSmFe
A lanthanum-loaded P204-TBP organic phase obtained from the last 1-stage outlet organic phase of a NaMgCaBaPbZn/La fractional extraction system is taken as a lanthanum saponification P204-TBP extraction organic phase, a LaCePrNdAlSmFe-loaded organic phase obtained from the last 1-stage outlet organic phase of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system is taken as feed liquid, and 1.5mol/L of HCl is taken as washing acid. The lanthanum saponification P204-TBP extraction organic phase enters a La/CePrNdAlSmFe fractional extraction system from the level 1, the loaded LaCePrNdAlSmFe organic phase enters the La/CePrNdAlSmFe fractional extraction system from the level 48, and 1.5mol/L HCl washing acid enters the La/CePrNdAlSmFe fractional extraction system from the level 74. And obtaining 5N-grade lanthanum chloride aqueous solution from the 1 st-grade outlet water phase of the La/CePrNdAlSmFe fractional extraction system to obtain the target separation product high-purity lanthanum. And obtaining a loaded CePrNdAlSmFe organic phase from a 74 th grade outlet organic phase of the La/CePrNdAlSmFe fractional extraction system, and transferring the loaded CePrNdAlSmFe organic phase to a stripping section 1 for treatment.
And 4, step 4: stripping section 1
And 3mol/L HCl is used as stripping acid, and 9-stage countercurrent stripping is carried out on the loaded CePrNdAlSmFe organic phase. The water phase at the back extraction outlet is a mixture solution containing cerium chloride, praseodymium chloride, neodymium chloride, aluminum chloride, samarium chloride, iron calcium chloride and hydrochloric acid, and is used for recovering rare earth in the mixture solution. The organic phase outlet is a P204-TBP organic phase with residual iron and aluminum, and the organic phase is transferred to a stripping section 2 for treatment.
And 5: stripping section 2
And (3) carrying out 6-stage countercurrent stripping on the P204-TBP organic phase of the residual iron and aluminum by taking 1mol/L ammonium bifluoride as a stripping agent. The water phase at the back extraction outlet is waste liquid containing iron and aluminum, and is discharged after the lime neutralization treatment. The organic phase outlet is a P204-TBP organic phase which is recycled.
Target isolated product: 5N grade lanthanum chloride aqueous solution, which comprises the following components: na 0.000032g/L, Mg 0.000029g/L, Ca 0.000094g/L, Ba 0.000033g/L, Pb 0.000017g/L, Zn 0.000036g/L, La 70.00g/L, Ce0.00013g/L, Pr 0.000047g/L, Nd 0.000018g/L, Al0.000020g/L, Sm 0.000020g/L and Fe0.000020g/L. The relative purity of the aqueous solution of 5N grade lanthanum chloride is 99.9996%. The yield of lanthanum was 98%.
Example 3
P204-TBP organic phase: extracting agent P204 and TBP, wherein the volume percentage of P204 is 30%, the volume percentage of TBP is 15%, and the volume percentage of sulfonated kerosene solution is 55%.
Lanthanum chloride feed liquid: A3N industrial grade lanthanum chloride aqueous solution comprises 0.0050g/L of Na, 0.0050g/L of Mg, 0.010g/L of Ca0.0050 g/L of Ba, 0.0020g/L of Pb, 0.0050g/L of Zn, 135.0g/L of La, 0.020g/L of Ce, Pr0.010g/L of Nd, 0.0050g/L of Al, 0.0050g/L of Sm and 0.0050g/L of Fe.
Step 1: fractional extraction and separation of NaMgCaBaPbZnLa/LaCePrNdAlSmFe
The P204-TBP organic phase enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 1 st level, the lanthanum chloride feed liquid enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 12 th level, and 1.5mol/L HCl washing acid enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 36 th level. The extraction section of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system realizes the separation of NaMgCaBaPbZn/La, and the washing section realizes the separation of La/CePrNdAlSmFe. Obtaining a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn from a grade 1 outlet water phase of a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and using the lanthanum chloride aqueous solution as a feed liquid for fractional extraction separation of NaMgCaBaPbZn/La; and obtaining a loaded LaCePrNdAlSmFe organic phase from a 36 th-stage outlet organic phase of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and using the loaded LaCePrNdAlSmFe organic phase as feed liquid for fractional extraction and separation of La/CePrNdAlSmFe.
Step 2: fractional extraction separation of NaMgCaBaPbZn/La
Taking a P204-TBP organic phase as an extraction organic phase, obtaining a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn as a feed liquid by using a No. 1 outlet water phase of a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and obtaining 5N grade lanthanum chloride LaCl by performing fractional extraction and separation on the La/CePrNdAlSmFe No. 1 outlet water phase3The aqueous solution of (a) is a detergent. The P204-TBP organic phase enters a NaMgCaBaPbZn/La fractional extraction system from the 1 st stage, a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn enters the NaMgCaBaPbZn/La fractional extraction system from the 12 th stage, and a 5N-level lanthanum chloride detergent enters the NaMgCaBaPbZn/La fractional extraction system from the 58 th stage. And obtaining a mixed solution containing sodium chloride, magnesium chloride, calcium chloride, barium chloride, lead chloride, zinc chloride, lanthanum chloride and hydrochloric acid from the water phase at the 1 st stage outlet of the NaMgCaBaPbZn/La fractional extraction system, and recycling lanthanum. Obtaining a P204-TBP organic phase loaded with lanthanum from a 58 th-stage outlet organic phase of a NaMgCaBaPbZn/La fractional extraction system, and using the P204-TBP organic phase as a lanthanum saponification P204-TBP extraction organic phase for fractional extraction and separation of La/CePrNdAlSmFe.
And step 3: fractional extraction and separation of La/CePrNdAlSmFe
A lanthanum-loaded P204-TBP organic phase obtained from the last 1-stage outlet organic phase of a NaMgCaBaPbZn/La fractional extraction system is taken as a lanthanum saponification P204-TBP extraction organic phase, a LaCePrNdAlSmFe-loaded organic phase obtained from the last 1-stage outlet organic phase of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system is taken as feed liquid, and 1.5mol/L of HCl is taken as washing acid. The lanthanum saponification P204-TBP extraction organic phase enters a La/CePrNdAlSmFe fractional extraction system from the level 1, the loaded LaCePrNdAlSmFe organic phase enters the La/CePrNdAlSmFe fractional extraction system from the level 44, and 1.5mol/L HCl washing acid enters the La/CePrNdAlSmFe fractional extraction system from the level 72. And obtaining 5N-grade lanthanum chloride aqueous solution from the 1 st-grade outlet water phase of the La/CePrNdAlSmFe fractional extraction system to obtain the target separation product high-purity lanthanum. And obtaining a loaded CePrNdAlSmFe organic phase from a 72 th-stage outlet organic phase of the La/CePrNdAlSmFe fractional extraction system, and transferring the loaded CePrNdAlSmFe organic phase to a stripping section 1 for treatment.
And 4, step 4: stripping section 1
And 3mol/L HCl is used as stripping acid, and 9-stage countercurrent stripping is carried out on the loaded CePrNdAlSmFe organic phase. The water phase at the back extraction outlet is a mixture solution containing cerium chloride, praseodymium chloride, neodymium chloride, aluminum chloride, samarium chloride, iron calcium chloride and hydrochloric acid, and is used for recovering rare earth in the mixture solution. The organic phase outlet is a P204-TBP organic phase with residual iron and aluminum, and the organic phase is transferred to a stripping section 2 for treatment.
And 5: stripping section 2
And (3) carrying out 6-stage countercurrent stripping on the P204-TBP organic phase of the residual iron and aluminum by taking 1mol/L ammonium bifluoride as a stripping agent. The water phase at the back extraction outlet is waste liquid containing iron and aluminum, and is discharged after the lime neutralization treatment. The organic phase outlet is a P204-TBP organic phase which is recycled.
Target isolated product: 5N grade lanthanum chloride aqueous solution, which comprises the following components: na 0.000015g/L, Mg0.000016g/L, Ca0.000035g/L, Ba 0.000019g/L, Pb 0.0000078g/L, Zn 0.000020g/L, La67.50g/L, Ce0.000080g/L, Pr 0.000040g/L, Nd0.000020g/L, Al0.000020g/L, Sm 0.000019g/L, and Fe0.000019g/L. The relative purity of the aqueous solution of 5N grade lanthanum chloride is 99.9998%. The yield of lanthanum was 99%.
Claims (4)
1. A process for preparing high-purity lanthanum by an extraction method is characterized by comprising the following steps: the process takes 3N industrial grade lanthanum chloride aqueous solution as feed liquid, P204-TBP as a composite extractant, and consists of 3 fractional extraction steps and 2 back extraction steps: the 3 fractional extraction steps are fractional extraction separation of NaMgCaBaPbZnLa/LaCePrNdAlSmFe, fractional extraction separation of NaMgCaBaPbZn/La and fractional extraction separation of La/CePrNdAlSmFe respectively; the 2 back extraction steps are respectively a back extraction section 1 and a back extraction section 2;
the outlet organic phase of the NaMgCaBaPbZn/La separated by fractional extraction directly enters the 1 st stage of the La/CePrNdAlSmFe separated by fractional extraction, and the 1 st stage outlet aqueous phase of the La/CePrNdAlSmFe separated by fractional extraction is used as a washing agent for separating the NaMgCaBaPbZn/La by fractional extraction;
the process comprises the following specific steps:
step 1: fractional extraction and separation of NaMgCaBaPbZnLa/LaCePrNdAlSmFe
Taking a P204-TBP organic phase as an extraction organic phase, taking a 3N industrial grade lanthanum chloride aqueous solution as a lanthanum chloride feed liquid, and taking 1.5mol/L HCl as a washing acid; the P204-TBP organic phase enters a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the 1 st stage, the lanthanum chloride feed liquid enters the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the feeding stage, and 1.5mol/L HCl washing acid enters the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system from the last 1 st stage; the extraction section of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system realizes the separation of NaMgCaBaPbZn/La, and the washing section realizes the separation of La/CePrNdAlSmFe; obtaining a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn from a grade 1 outlet water phase of a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and using the lanthanum chloride aqueous solution as a feed liquid for fractional extraction separation of NaMgCaBaPbZn/La; obtaining a loaded LaCePrNdAlSmFe organic phase from the final grade 1 outlet organic phase of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and using the loaded LaCePrNdAlSmFe organic phase as feed liquid for fractional extraction and separation of La/CePrNdAlSmFe;
step 2: fractional extraction separation of NaMgCaBaPbZn/La
Taking a P204-TBP organic phase as an extraction organic phase, obtaining a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn as a feed liquid by using a No. 1 outlet water phase of a NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and obtaining 5N grade lanthanum chloride LaCl by performing fractional extraction and separation on the La/CePrNdAlSmFe No. 1 outlet water phase3The aqueous solution of (a) is a detergent; the P204-TBP organic phase enters a NaMgCaBaPbZn/La fractionation extraction system from the 1 st stage, a lanthanum chloride aqueous solution containing Na, Mg, Ca, Ba, Pb and Zn enters the NaMgCaBaPbZn/La fractionation extraction system from the feeding stage, and a 5N-level lanthanum chloride detergent enters the NaMgCaBaPbZn/La fractionation extraction system from the last 1 st stage; fractionation of the extraction System from NaMgCaBaPbZn/LaObtaining a mixed solution containing sodium chloride, magnesium chloride, calcium chloride, barium chloride, lead chloride, zinc chloride, lanthanum chloride and hydrochloric acid from the water phase at the outlet of the level 1 for recovering lanthanum; obtaining a lanthanum-loaded P204-TBP organic phase from the last grade 1 outlet organic phase of the NaMgCaBaPbZn/La fractional extraction system, and using the lanthanum-loaded P204-TBP organic phase as a lanthanum saponification P204-TBP extraction organic phase for fractional extraction and separation of La/CePrNdAlSmFe;
and step 3: fractional extraction and separation of La/CePrNdAlSmFe
Taking a lanthanum-loaded P204-TBP organic phase obtained from the last 1-stage outlet organic phase of a NaMgCaBaPbZn/La fractional extraction system as a lanthanum saponification P204-TBP extraction organic phase, obtaining a LaCePrNdAlSmFe-loaded organic phase as feed liquid from the last 1-stage outlet organic phase of the NaMgCaBaPbZnLa/LaCePrNdAlSmFe fractional extraction system, and taking 1.5mol/L HCl as washing acid; the lanthanum saponification P204-TBP extraction organic phase enters a La/CePrNdAlSmFe fractionation and extraction system from the 1 st stage, the loaded LaCePrNdAlSmFe organic phase enters the La/CePrNdAlSmFe fractionation and extraction system from the feeding stage, and 1.5mol/L HCl washing acid enters the La/CePrNdAlSmFe fractionation and extraction system from the last 1 st stage; obtaining 5N-grade lanthanum chloride aqueous solution from the 1 st-grade outlet water phase of the La/CePrNdAlSmFe fractional extraction system, and taking the aqueous solution as a target separation product, namely high-purity lanthanum; obtaining a loaded CePrNdAlSmFe organic phase from the last 1-grade outlet organic phase of the La/CePrNdAlSmFe fractional extraction system, and transferring the loaded CePrNdAlSmFe organic phase to a stripping section 1 for treatment;
and 4, step 4: stripping section 1
3mol/L HCl is used as stripping acid, and 9-grade countercurrent stripping is carried out to load a CePrNdAlSmFe organic phase; the back extraction outlet water phase is a mixture solution containing cerium chloride, praseodymium chloride, neodymium chloride, aluminum chloride, samarium chloride, ferric chloride and hydrochloric acid and is used for recovering rare earth in the mixture solution; the outlet of the organic phase is a P204-TBP organic phase with residual iron and aluminum, and the organic phase is transferred to a back extraction section 2 for treatment;
and 5: stripping section 2
1mol/L ammonium bifluoride is taken as a stripping agent to carry out 6-stage countercurrent stripping on the P204-TBP organic phase of the residual iron and aluminum; the water phase at the back extraction outlet is waste liquid containing iron and aluminum, and is discharged after being neutralized by lime; the organic phase outlet is a P204-TBP organic phase which is recycled.
2. The process for preparing high-purity lanthanum by the extraction method as claimed in claim 1, wherein the extraction method comprises the following steps: the P204-TBP organic phase is sulfonated kerosene solution of extracting agent P204 and TBP, wherein the volume percentage of P204 is 30%, the volume percentage of TBP is 15%, and the volume percentage of sulfonated kerosene solution is 55%.
3. The process for preparing high-purity lanthanum by the extraction method as claimed in claim 1, wherein the extraction method comprises the following steps: the 3N industrial grade lanthanum chloride aqueous solution is an aqueous solution containing lanthanum chloride, and comprises the following components: 0.0050 g/L-0.020 g/L Na, 0.0050 g/L-0.020 g/L Mg, 0.010g/L Ca-0.050 g/L Ba, 0.0050 g/L-0.020 g/L Pb, 0.0020 g/L-0.010 g/L Pb, 0.0050 g/L-0.020 g/L Zn, 135.0 g/L-145.0 g/L La, 0.020 g/L-0.080 g/L Ce, 0.010g/L-0.030 g/L Pr0.0050 g/L Nd, 0.0050 g/L-0.0050 g/L Al, 0.0050 g/L-0.010 g/L Sm, and 0.0050 g/L-0.010 g/L Fe.
4. The process for preparing high-purity lanthanum by the extraction method as claimed in claim 1, wherein the extraction method comprises the following steps: the 5N-level lanthanum chloride aqueous solution comprises the following components: na 0.000015 g/L-0.000048 g/L, Mg0.000016g/L-0.000067 g/L, Ca0.000035g/L-0.00015 g/L, Ba 0.000019 g/L-0.000063 g/L, Pb 0.0000078 g/L-0.000032 g/L, Zn 0.000020 g/L-0.000070 g/L, La67.50 g/L-72.50 g/L, Ce0.000080 g/L-0.00056 g/L, Pr 0.000040 g/L-0.000068 g/L, Nd0.000020 g/L-0.000022 g/L, Al0.000020g/L-0.000021 g/L, Sm 0.000019 g/L-0.000020 g/L, Fe0.000019 g/L-0.000020 g/L.
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