CN110306047A - A kind of technique separating light rare earth in southern ion adsorption type rare earth ore - Google Patents

A kind of technique separating light rare earth in southern ion adsorption type rare earth ore Download PDF

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CN110306047A
CN110306047A CN201910688297.8A CN201910688297A CN110306047A CN 110306047 A CN110306047 A CN 110306047A CN 201910688297 A CN201910688297 A CN 201910688297A CN 110306047 A CN110306047 A CN 110306047A
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钟学明
刘俊辰
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Nanchang Hangkong University
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Abstract

A kind of technique for separating light rare earth in southern ion adsorption type rare earth ore of the present invention is grouped separating obtained complexes aqueous solution as feed liquid using southern ion adsorption type rare earth ore, and P507 is extractant;It is made of three fractional extraction systems, respectively La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system, bis- feed inlet fractional extraction separation system of bis- feed inlet fractional extraction separation system of La/Ce and Pr/Nd.By the combination of three fractional extraction systems, four kinds of 5N grades of lanthanum chlorides, 3N grades of cerium chlorides, 3N grades of praseodymium chlorides and 4N grades of neodymium chlorides separation products are directly obtained.The present invention has target separation product purity high, the high income of rare earth element, the advantages such as acid and alkali consumption is low, and process flow is short, and separation costs are low.

Description

A kind of technique separating light rare earth in southern ion adsorption type rare earth ore
Technical field
The present invention relates to a kind of techniques for separating light rare earth in southern ion adsorption type rare earth ore, specifically with the suction of southern ion It is feed liquid that attached type Rare Earth Mine, which is grouped separating obtained complexes aqueous solution, and P507 is extractant, realizes light rare earth elements Lanthanum, cerium, the separation between four elements of praseodymium and neodymium, obtain 5N grades of lanthanum chlorides, 3N grades of cerium chlorides, 3N grades of praseodymium chlorides and 4N grades of chlorinations Four kinds of products of neodymium.Particular technique field of the invention is the Isolating chlorinated light rare earth of fractional-distillation extraction.
Background technique
Although southern ion adsorption type rare earth ore is the most important rare earth of heavy rare earth single-element net product in separation and Extraction Raw material, but southern ion adsorption type rare earth ore also contains a certain amount of light rare earth elements.It is light dilute by taking middle yttrium richness europium mine as an example The content of earth elements is about 55%.Therefore, creative research and development are related efficiently separates light rare earth in southern ion adsorption type rare earth ore Technique be very important.
The conventional method for separating light rare earth LaCePrNd in southern ion adsorption type rare earth ore is LaCe/PrNd extraction and separation Technique or hydrogen peroxide oxidation precipitate cerium separating technology.Since the separation costs of traditional handicraft are high, the power in Rare Earth Separation field Prestige scientist proposes La//Ce/PrNd tri- and exports fractional extraction separating technology, so that isolated acid and alkali consumption about declines 30%, As the current preferred technique for separating light rare earth in southern ion adsorption type rare earth ore.But the outlet La//Ce/PrNd tri- fractionation The purity that extraction separates four kinds of separation products of light rare earth technique in southern ion adsorption type rare earth ore is respectively as follows: the purity of lanthanum It is 3N~4N grades, the purity of cerium is 3N grades, and the purity of praseodymium is 2N grades, and the purity of neodymium is 3N grades.It follows that products obtained therefrom is pure It spends not high enough, needs to further increase.It is separated in southern ion adsorption type rare earth ore gently in addition, La//Ce/PrNd tri- exports method The acid and alkali consumption of rare-earth process is still higher, there is the space further decreased.It follows that the southern ion type of existing separation There are product purity is not high enough and the higher deficiency of acid and alkali consumption for light rare earth technique in Rare Earth Mine.
The present invention is established for deficiency present in light rare earth technique in the southern ion adsorption type rare earth ore of existing separation It is a kind of to efficiently separate southern ion adsorption type rare earth ore and be grouped separating obtained light rare earth mixture, directly obtain 5N grades of chlorinations The method of lanthanum, 3N grade cerium chloride, 3N grades of praseodymium chlorides and 4N grades of neodymium chlorides.
Summary of the invention
A kind of technique for separating light rare earth in southern ion adsorption type rare earth ore of the present invention is directed to existing separation LaCePrNd Light rare earth mixture method establishes a kind of low acid and alkali consumption separation there are product purity is not high enough and the higher deficiency of acid and alkali consumption Southern ion adsorption type rare earth ore is grouped separating obtained light rare earth mixture, directly obtain 5N grades of lanthanum chlorides, 3N grades of cerium chlorides, The technique of 3N grades of praseodymium chlorides and 4N grades of neodymium chlorides.
A kind of technique for separating light rare earth in southern ion adsorption type rare earth ore of the present invention, with southern ion adsorption type re It is feed liquid, di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester hexyl phosphonic acids that mine, which is grouped separating obtained complexes aqueous solution, (abbreviation P507) is extractant, is made of three fractional extraction systems, and respectively La/LaCe/PrNd/Nd tetra- exports fractional extraction Bis- feed inlet fractional extraction separation system of separation system, bis- feed inlet fractional extraction separation system of La/Ce and Pr/Nd.Pass through institute The combination for the three fractional extraction systems stated directly obtains 5N grades of lanthanum chlorides, 3N grades of cerium chlorides, 3N grades of praseodymium chlorides and 4N grades of chlorinations Four kinds of separation products of neodymium.
La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system and opens up that there are four outlets, respectively first outlet, the Two outlets, third outlet and the 4th outlet.First outlet is opened in La/LaCe/PrNd/Nd tetra- and exports fractional extraction separation system 1st grade of water phase;Second outlet is opened in the water among the outlet La/LaCe/PrNd/Nd tetra- fractional extraction separation system extraction section Phase;Third outlet is opened in the water phase among the outlet La/LaCe/PrNd/Nd tetra- fractional extraction separation system washing section;4th goes out Mouth is opened in La/LaCe/PrNd/Nd tetra- and exports last 1 grade of the organic phase of fractional extraction separation system.First outlet goes out with second Mouth is preceding extraction section, is rear extraction section between second outlet and charging grade, and feeding between grade and third outlet is preceding washing section, the It is rear washing section between three outlets and the 4th outlet.Preceding extraction section and rear extraction section are collectively referred to as extraction section, and preceding washing section is washed with after It washs section and is collectively referred to as washing section.The preceding extraction section that La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system realizes La/Ce points From the rear extraction section that La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system realizes LaCe/Pr separation, La/LaCe/ The preceding washing section that PrNd/Nd tetra- exports fractional extraction separation system realizes Ce/PrNd separation, and La/LaCe/PrNd/Nd tetra- is exported The rear washing section of fractional extraction separation system realizes Pr/Nd separation.
Bis- feed inlet fractional extraction separation system of La/Ce is equipped with 2 feed inlets, respectively first charging aperture and the second charging Mouthful.The 1st grade of bis- feed inlet fractional extraction separation system of La/Ce is extraction section, first charging aperture and the between first charging aperture Wash section between two feed inlets for extraction, second charging aperture and it is 1 grade last between be washing section.
Bis- feed inlet fractional extraction separation system of Pr/Nd is equipped with 2 feed inlets, respectively first charging aperture and the second charging Mouthful.The 1st grade of bis- feed inlet fractional extraction separation system of Pr/Nd is extraction section, first charging aperture and the between first charging aperture Wash section between two feed inlets for extraction, second charging aperture and it is 1 grade last between be washing section.
Three fractional extraction systems are specific as follows:
1) La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system
It is extraction organic phase with 2N lanthanum saponification P507 organic phase, southern ion adsorption type rare earth ore is grouped separating obtained light Aqueous solution of rare earth chloride is feed liquid, and 3.0mol/L HCl is washing acid.2N lanthanum is saponified P507 organic phase and enters La/ from the 1st grade LaCe/PrNd/Nd tetra- exports fractional extraction separation system, and complexes aqueous solution enters La/LaCe/ from charging grade PrNd/Nd tetra- exports fractional extraction separation system, and washing acid 3.0mol/L HCl enters La/LaCe/PrNd/Nd from last 1 grade Four outlet fractional extraction separation systems.The first outlet for exporting fractional extraction separation system from La/LaCe/PrNd/Nd tetra- obtains 2N lanthanum chloride solution, the first feed liquid as bis- feed inlet fractional extraction separation system of La/Ce;From La/LaCe/PrNd/ The second outlet that Nd tetra- exports fractional extraction separation system obtains lanthanum-cerium chloride aqueous solution, is used as bis- feed inlet of La/Ce fractionation extraction Take second of feed liquid of separation system;It is obtained from the third outlet that La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system Praseodymium chloride neodymium aqueous solution, the first feed liquid as bis- feed inlet fractional extraction separation system of Pr/Nd;From La/LaCe/PrNd/ Nd tetra- exports the outlet of fractional extraction separation system the 4th and obtains load PrNd organic phase, is used as bis- feed inlet fractional extraction of Pr/Nd Second of feed liquid of separation system.
2) bis- feed inlet fractional extraction separation system of La/Ce
It is extraction organic phase with 5N lanthanum saponification P507 organic phase, exports fractional extraction point from La/LaCe/PrNd/Nd tetra- The lanthanum-cerium chloride aqueous solution for being in vitro first outlet acquisition is the first feed liquid, from the outlet La/LaCe/PrNd/Nd tetra- fractionation It is second of feed liquid that the second outlet of extraction and separation system, which obtains lanthanum-cerium chloride aqueous solution, and 3.0mol/L HCl is washing acid.5N Lanthanum is saponified P507 organic phase and enters bis- feed inlet fractional extraction separation system of La/Ce from the 1st grade, the first feed liquid comes from La/ LaCe/PrNd/Nd tetra- export fractional extraction separation system first outlet obtain lanthanum-cerium chloride aqueous solution from first charging aperture into Enter bis- feed inlet fractional extraction separation system of La/Ce, second of feed liquid exports fractional extraction point from La/LaCe/PrNd/Nd tetra- The second outlet for being in vitro obtains lanthanum-cerium chloride aqueous solution and enters bis- feed inlet fractional extraction chorista of La/Ce from second charging aperture System, washing acid 3.0mol/L HCl enter bis- feed inlet fractional extraction separation system of La/Ce from last 1 grade.It is fed from La/Ce bis- 1st grade of outlet water phase of mouth fractional extraction separation system obtains product 5N grades of lanthanum chloride solution of separation;From bis- feed inlet of La/Ce Last 1 grade of outlet organic phase of fractional extraction separation system obtains cerium-carrying organic phase, through being stripped with 6 grades of 3.2mol/L HCl Obtain product 3N grades of cerium chloride aqueous solution of separation.
3) bis- feed inlet fractional extraction separation system of Pr/Nd
It is extraction organic phase with 3N praseodymium saponification P507 organic phase, exports fractional extraction point from La/LaCe/PrNd/Nd tetra- The praseodymium chloride neodymium aqueous solution for the third outlet for being in vitro is the first feed liquid;Fractionation extraction is exported from La/LaCe/PrNd/Nd tetra- Taking the outlet of separation system the 4th to obtain load PrNd organic phase is second of feed liquid, and 3.0mol/L HCl is washing acid.3N praseodymium soap Change P507 organic phase and enter bis- feed inlet fractional extraction separation system of Pr/Nd from the 1st grade, the first feed liquid comes from La/LaCe/ The praseodymium chloride neodymium aqueous solution that PrNd/Nd tetra- exports the third outlet of fractional extraction separation system enters Pr/Nd from first charging aperture Two feed inlet fractional extraction separation systems, second of feed liquid export fractional extraction separation system from La/LaCe/PrNd/Nd tetra- 4th outlet obtains load PrNd organic phase and enters bis- feed inlet fractional extraction separation system of Pr/Nd from second charging aperture, washs Sour 3.0mol/L HCl enters bis- feed inlet fractional extraction separation system of Pr/Nd from last 1 grade.It is fractionated from bis- feed inlet of Pr/Nd 1st grade of outlet water phase of extraction and separation system obtains product 3N grades of praseodymium chloride aqueous solution of separation;It is fractionated and extracts from bis- feed inlet of Pr/Nd Last 1 grade of outlet organic phase of separation system is taken to obtain the organic phase of load neodymium, through obtaining with 6 grades of back extraction of 3.5mol/L HCl Separate product 4N grades of neodymium chloride aqueous solution.
The P507 organic phase is the sulfonated kerosene solution of extractant P507, and wherein the percentage by volume of P507 is 30%, the percentage by volume of sulfonated kerosene is 70%.In use, being obtained after corresponding saponification must being implemented using general method for saponification Obtain corresponding rare-earth sodium saponification organic phase.
The southern ion adsorption type rare earth ore is grouped the composition of separating obtained complexes aqueous solution are as follows: La 60.0g/L~70.0g/L, Ce 5.0g/L~7.0g/L, Pr 13.0g/L~17.0g/L, Nd 50.0g/L~60.0g/L, Sm 0.00050g/L~0.0020g/L.
The composition of the 5N grade lanthanum chloride solution are as follows: La 136.0g/L~142.0g/L, Ce 0.00020g/L~ 0.00080g/L, Pr 0.00010g/L~0.00030g/L, Nd 0.000030g/L~0.00010g/L, Sm 0.000010g/ L~0.000030g/L.
The composition of the 3N grade cerium chloride aqueous solution are as follows: La 0.010g/L~0.030g/L, Ce 136.0g/L~ 140.0g/L, Pr 0.040g/L~0.080g/L, Nd 0.0050g/L~0.020g/L, Sm 0.00010g/L~ 0.00030g/L。
The composition of the 3N grade praseodymium chloride aqueous solution are as follows: La 0.00020g/L~0.0010g/L, Ce 0.0010g/L ~0.0030g/L, Pr 135.0g/L~141.0g/L, Nd 0.020g/L~0.10g/L, Sm 0.00010g/L~ 0.00050g/L。
The composition of the 4N grade neodymium chloride aqueous solution are as follows: La 0.00010g/L~0.00050g/L, Ce 0.00020g/ L~0.00080g/L, Pr 0.0010g/L~0.0070g/L, Nd 139.0g/L~145.0g/L, Sm 0.0012g/L~ 0.0054g/L。
Beneficial effects of the present invention: the 1) purity is high of target separation product single rare earth chloride.The present invention obtains simultaneously The 5N grade lanthanum chloride solution that relative purity is 99.9990%~99.9997%, relative purity are 99.90%~99.96% 3N grades of cerium chloride aqueous solutions, the 3N grade praseodymium chloride aqueous solution that relative purity is 99.90%~99.98%, relative purity are 99.990%~99.998% 4N grade neodymium chloride aqueous solution.2) high income of rare earth element.The yield of lanthanum is 97%~99%, The yield of cerium is 94%~96%, and the yield of praseodymium is 96%~98%, and the yield of neodymium is 97%~99%.3) acid and alkali consumption is low. La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system and takes full advantage of the work of separation, reduces its acid and alkali consumption;La/Ce Two feed inlet fractional extraction separation systems and bis- feed inlet fractional extraction separation system separative efficiency of Pr/Nd are high, reduce its acid Alkali consumption;It does not need further to purify, directly obtains 5N grades of lanthanum chlorides and 4N grades of neodymium chlorides, saved and isolated and purified accordingly Acid and alkali consumption.5N grades of lanthanum chlorides, 3N grades of cerium chlorides, 3N grades of praseodymium chlorides are prepared using identical complexes raw material with existing It compares with 4N grades of neodymium chloride methods, acid and alkali consumption about saves 30%.4) process flow is short.Directly obtain 5N grades of lanthanum chlorides, 3N Grade cerium chloride, 3N grades of praseodymium chlorides and 4N grades of neodymium chlorides, do not need further separation purifying technique.5) separation costs are low.Substantially Degree reduces acid and alkali consumption, and process flow is short, to reduce separation costs.
Detailed description of the invention
A kind of Fig. 1: separation process schematic diagram for separating the technique of light rare earth in southern ion adsorption type rare earth ore of the present invention.
Specific embodiment
The technique for separating light rare earth in southern ion adsorption type rare earth ore a kind of to the present invention combined with specific embodiments below It is further described.
Embodiment 1
P507 organic phase is the sulfonated kerosene solution of extractant P507, and wherein the percentage by volume of P507 is 30%, sulfonation The percentage by volume of kerosene is 70%.In use, being obtained after corresponding saponification must be implemented using general method for saponification corresponding Rare-earth sodium saponification organic phase.
Southern ion adsorption type rare earth ore is grouped the composition of separating obtained complexes aqueous solution are as follows: La 60.0g/L, Ce 7.0g/L, Pr 13.0g/L, Nd 60.0g/L, Sm 0.00050g/L.
1) La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system
It is extraction organic phase with 2N lanthanum saponification P507 organic phase, southern ion adsorption type rare earth ore is grouped separating obtained light Aqueous solution of rare earth chloride is feed liquid, and 3.0mol/L HCl is washing acid.2N lanthanum is saponified P507 organic phase and enters La/ from the 1st grade LaCe/PrNd/Nd tetra- exports fractional extraction separation system, and complexes aqueous solution enters La/LaCe/ from the 24th grade PrNd/Nd tetra- exports fractional extraction separation system, and washing acid 3.0mol/L HCl enters La/LaCe/PrNd/Nd tetra- from the 88th grade Export fractional extraction separation system.The 1st grade of first outlet for exporting fractional extraction separation system from La/LaCe/PrNd/Nd tetra- obtains Obtain 2N lanthanum chloride solution, the first feed liquid as bis- feed inlet fractional extraction separation system of La/Ce;From La/LaCe/ PrNd/Nd tetra- export fractional extraction separation system the 8th grade of acquisitions lanthanum-cerium chloride aqueous solution of second outlet, as La/Ce bis- into Second of feed liquid of material mouth fractional extraction separation system;The of fractional extraction separation system is exported from La/LaCe/PrNd/Nd tetra- Three the 50th grade of acquisition praseodymium chloride neodymium aqueous solutions in outlet, the first feed liquid as bis- feed inlet fractional extraction separation system of Pr/Nd; The 88th grade of the outlet of fractional extraction separation system the 4th is exported from La/LaCe/PrNd/Nd tetra- and obtains load PrNd organic phase, is used as Second of feed liquid of bis- feed inlet fractional extraction separation system of Pr/Nd.
2) bis- feed inlet fractional extraction separation system of La/Ce
It is extraction organic phase with 5N lanthanum saponification P507 organic phase, exports fractional extraction point from La/LaCe/PrNd/Nd tetra- The lanthanum-cerium chloride aqueous solution for being in vitro first outlet acquisition is the first feed liquid, from the outlet La/LaCe/PrNd/Nd tetra- fractionation It is second of feed liquid that the second outlet of extraction and separation system, which obtains lanthanum-cerium chloride aqueous solution, and 3.0mol/L HCl is washing acid.5N Lanthanum is saponified P507 organic phase and enters bis- feed inlet fractional extraction separation system of La/Ce from the 1st grade, the first feed liquid comes from La/ LaCe/PrNd/Nd tetra- exports lanthanum-cerium chloride aqueous solution that fractional extraction separation system first outlet obtains from first charging aperture the 55 grades enter bis- feed inlet fractional extraction separation system of La/Ce, and second of feed liquid is from the outlet La/LaCe/PrNd/Nd tetra- fractionation The second outlet of extraction and separation system obtains lanthanum-cerium chloride aqueous solution and enters bis- feed inlet of La/Ce point from the 62nd grade of second charging aperture Extraction and separation system is evaporated, washing acid 3.0mol/L HCl enters bis- feed inlet fractional extraction separation system of La/Ce from the 76th grade.From 1st grade of outlet water phase of bis- feed inlet fractional extraction separation system of La/Ce obtains product 5N grades of lanthanum chloride solution of separation;From 76th grade of outlet organic phase of bis- feed inlet fractional extraction separation system of La/Ce obtains cerium-carrying organic phase, through with 3.2mol/L 6 grades of back extraction of HCl obtain product 3N grades of cerium chloride aqueous solution of separation.
3) bis- feed inlet fractional extraction separation system of Pr/Nd
It is extraction organic phase with 3N praseodymium saponification P507 organic phase, exports fractional extraction point from La/LaCe/PrNd/Nd tetra- The praseodymium chloride neodymium aqueous solution for the third outlet for being in vitro is the first feed liquid;Fractionation extraction is exported from La/LaCe/PrNd/Nd tetra- Taking the outlet of separation system the 4th to obtain load PrNd organic phase is second of feed liquid, and 3.0mol/L HCl is washing acid.3N praseodymium soap Change P507 organic phase and enter bis- feed inlet fractional extraction separation system of Pr/Nd from the 1st grade, the first feed liquid comes from La/LaCe/ The praseodymium chloride neodymium aqueous solution that PrNd/Nd tetra- exports the third outlet of fractional extraction separation system enters from the 25th grade of first charging aperture Bis- feed inlet fractional extraction separation system of Pr/Nd, second of feed liquid export fractional extraction separation from La/LaCe/PrNd/Nd tetra- The outlet of system the 4th obtains load PrNd organic phase and enters bis- feed inlet fractional extraction of Pr/Nd separation from the 54th grade of second charging aperture System, washing acid 3.0mol/L HCl enter bis- feed inlet fractional extraction separation system of Pr/Nd from the 102nd grade.From Pr/Nd bis- into 1st grade of outlet water phase of material mouth fractional extraction separation system obtains product 3N grades of praseodymium chloride aqueous solution of separation;It is fed from Pr/Nd bis- 102nd grade of outlet organic phase of mouth fractional extraction separation system obtains the organic phase of load neodymium, through with 6 grades of 3.5mol/L HCl Back extraction obtains product 4N grades of neodymium chloride aqueous solution of separation.
The composition of the 5N grade lanthanum chloride solution are as follows: La 136.0g/L, Ce 0.00080g/L, Pr 0.00030g/ L, Nd 0.00010g/L, Sm 0.000030g/L.The relative purity of 5N grades of lanthanum chloride solutions is 99.9990%.The yield of lanthanum It is 99%.
The composition of the 3N grade cerium chloride aqueous solution are as follows: La 0.010g/L, Ce 140.0g/L, Pr 0.040g/L, Nd 0.0050g/L, Sm 0.00010g/L.The relative purity of 3N grades of cerium chloride aqueous solutions is 99.96%.The yield of cerium is 94%.
The composition of the 3N grade praseodymium chloride aqueous solution are as follows: La 0.0010g/L, Ce 0.0030g/L, Pr 135.0g/L, Nd 0.10g/L, Sm 0.00050g/L.The relative purity of 3N grades of praseodymium chloride aqueous solutions is 99.90%.The yield of praseodymium is 98%.
The composition of the 4N grade neodymium chloride aqueous solution are as follows: La 0.00010g/L, Ce 0.00020g/L, Pr 0.0010g/L, Nd 145.0g/L, Sm 0.0012g/L.The relative purity of 4N grades of neodymium chloride aqueous solutions is 99.998%.Neodymium Yield is 97%.
Embodiment 2
P507 organic phase is the sulfonated kerosene solution of extractant P507, and wherein the percentage by volume of P507 is 30%, sulfonation The percentage by volume of kerosene is 70%.In use, being obtained after corresponding saponification must be implemented using general method for saponification corresponding Rare-earth sodium saponification organic phase.
Southern ion adsorption type rare earth ore is grouped the composition of separating obtained complexes aqueous solution are as follows: La 65.0g/L, Ce 6.0g/L, Pr 15.0g/L, Nd 55.0g/L, Sm 0.0010g/L.
1) La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system
It is extraction organic phase with 2N lanthanum saponification P507 organic phase, southern ion adsorption type rare earth ore is grouped separating obtained light Aqueous solution of rare earth chloride is feed liquid, and 3.0mol/L HCl is washing acid.2N lanthanum is saponified P507 organic phase and enters La/ from the 1st grade LaCe/PrNd/Nd tetra- exports fractional extraction separation system, and complexes aqueous solution enters La/LaCe/ from the 23rd grade PrNd/Nd tetra- exports fractional extraction separation system, and washing acid 3.0mol/L HCl enters La/LaCe/PrNd/Nd tetra- from the 87th grade Export fractional extraction separation system.The 1st grade of first outlet for exporting fractional extraction separation system from La/LaCe/PrNd/Nd tetra- obtains Obtain 2N lanthanum chloride solution, the first feed liquid as bis- feed inlet fractional extraction separation system of La/Ce;From La/LaCe/ PrNd/Nd tetra- export fractional extraction separation system the 8th grade of acquisitions lanthanum-cerium chloride aqueous solution of second outlet, as La/Ce bis- into Second of feed liquid of material mouth fractional extraction separation system;The of fractional extraction separation system is exported from La/LaCe/PrNd/Nd tetra- Three the 49th grade of acquisition praseodymium chloride neodymium aqueous solutions in outlet, the first feed liquid as bis- feed inlet fractional extraction separation system of Pr/Nd; The 87th grade of the outlet of fractional extraction separation system the 4th is exported from La/LaCe/PrNd/Nd tetra- and obtains load PrNd organic phase, is used as Second of feed liquid of bis- feed inlet fractional extraction separation system of Pr/Nd.
2) bis- feed inlet fractional extraction separation system of La/Ce
It is extraction organic phase with 5N lanthanum saponification P507 organic phase, exports fractional extraction point from La/LaCe/PrNd/Nd tetra- The lanthanum-cerium chloride aqueous solution for being in vitro first outlet acquisition is the first feed liquid, from the outlet La/LaCe/PrNd/Nd tetra- fractionation It is second of feed liquid that the second outlet of extraction and separation system, which obtains lanthanum-cerium chloride aqueous solution, and 3.0mol/L HCl is washing acid.5N Lanthanum is saponified P507 organic phase and enters bis- feed inlet fractional extraction separation system of La/Ce from the 1st grade, the first feed liquid comes from La/ LaCe/PrNd/Nd tetra- exports lanthanum-cerium chloride aqueous solution that fractional extraction separation system first outlet obtains from first charging aperture the 80 grades enter bis- feed inlet fractional extraction separation system of La/Ce, and second of feed liquid is from the outlet La/LaCe/PrNd/Nd tetra- fractionation The second outlet of extraction and separation system obtains lanthanum-cerium chloride aqueous solution and enters bis- feed inlet of La/Ce point from the 87th grade of second charging aperture Extraction and separation system is evaporated, washing acid 3.0mol/L HCl enters bis- feed inlet fractional extraction separation system of La/Ce from the 101st grade. Product 5N grades of lanthanum chloride solution of separation is obtained from the 1st grade of outlet water phase of bis- feed inlet fractional extraction separation system of La/Ce;From 101st grade of outlet organic phase of bis- feed inlet fractional extraction separation system of La/Ce obtains cerium-carrying organic phase, through with 3.2mol/L 6 grades of back extraction of HCl obtain product 3N grades of cerium chloride aqueous solution of separation.
3) bis- feed inlet fractional extraction separation system of Pr/Nd
It is extraction organic phase with 3N praseodymium saponification P507 organic phase, exports fractional extraction point from La/LaCe/PrNd/Nd tetra- The praseodymium chloride neodymium aqueous solution for the third outlet for being in vitro is the first feed liquid;Fractionation extraction is exported from La/LaCe/PrNd/Nd tetra- Taking the outlet of separation system the 4th to obtain load PrNd organic phase is second of feed liquid, and 3.0mol/L HCl is washing acid.3N praseodymium soap Change P507 organic phase and enter bis- feed inlet fractional extraction separation system of Pr/Nd from the 1st grade, the first feed liquid comes from La/LaCe/ The praseodymium chloride neodymium aqueous solution that PrNd/Nd tetra- exports the third outlet of fractional extraction separation system enters from the 25th grade of first charging aperture Bis- feed inlet fractional extraction separation system of Pr/Nd, second of feed liquid export fractional extraction separation from La/LaCe/PrNd/Nd tetra- The outlet of system the 4th obtains load PrNd organic phase and enters bis- feed inlet fractional extraction of Pr/Nd separation from the 55th grade of second charging aperture System, washing acid 3.0mol/L HCl enter bis- feed inlet fractional extraction separation system of Pr/Nd from the 103rd grade.From Pr/Nd bis- into 1st grade of outlet water phase of material mouth fractional extraction separation system obtains product 3N grades of praseodymium chloride aqueous solution of separation;It is fed from Pr/Nd bis- 103rd grade of outlet organic phase of mouth fractional extraction separation system obtains the organic phase of load neodymium, through with 6 grades of 3.5mol/L HCl Back extraction obtains product 4N grades of neodymium chloride aqueous solution of separation.
The composition of the 5N grade lanthanum chloride solution are as follows: La 139.0g/L, Ce 0.00050g/L, Pr 0.00020g/ L, Nd 0.000060g/L, Sm 0.000020g/L.The relative purity of 5N grades of lanthanum chloride solutions is 99.9994%.The receipts of lanthanum Rate is 98%.
The composition of the 3N grade cerium chloride aqueous solution are as follows: La 0.020g/L, Ce 138.0g/L, Pr 0.060g/L, Nd 0.010g/L, Sm 0.00020g/L.The relative purity of 3N grades of cerium chloride aqueous solutions is 99.93%.The yield of cerium is 95%.
The composition of the 3N grade praseodymium chloride aqueous solution are as follows: La 0.00050g/L, Ce 0.0020g/L~, Pr 138.0g/L, Nd 0.050g/L, Sm 0.00030g/L.The relative purity of 3N grades of praseodymium chloride aqueous solutions is 99.95%.The receipts of praseodymium Rate is 97%.
The composition of the 4N grade neodymium chloride aqueous solution are as follows: La 0.00030g/L, Ce 0.00050g/L, Pr 0.0040g/L, Nd 142.0g/L, Sm 0.0025g/L.The relative purity of 4N grades of neodymium chloride aqueous solutions is 99.995%.Neodymium Yield is 98%.
Embodiment 3
P507 organic phase is the sulfonated kerosene solution of extractant P507, and wherein the percentage by volume of P507 is 30%, sulfonation The percentage by volume of kerosene is 70%.In use, being obtained after corresponding saponification must be implemented using general method for saponification corresponding Rare-earth sodium saponification organic phase.
Southern ion adsorption type rare earth ore is grouped the composition of separating obtained complexes aqueous solution are as follows: La 70.0g/L, Ce 5.0g/L, Pr 17.0g/L, Nd 50.0g/L, Sm 0.00020g/L.
1) La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system
It is extraction organic phase with 2N lanthanum saponification P507 organic phase, southern ion adsorption type rare earth ore is grouped separating obtained light Aqueous solution of rare earth chloride is feed liquid, and 3.0mol/L HCl is washing acid.2N lanthanum is saponified P507 organic phase and enters La/ from the 1st grade LaCe/PrNd/Nd tetra- exports fractional extraction separation system, and complexes aqueous solution enters La/LaCe/ from the 23rd grade PrNd/Nd tetra- exports fractional extraction separation system, and washing acid 3.0mol/L HCl enters La/LaCe/PrNd/Nd tetra- from the 87th grade Export fractional extraction separation system.The 1st grade of first outlet for exporting fractional extraction separation system from La/LaCe/PrNd/Nd tetra- obtains Obtain 2N lanthanum chloride solution, the first feed liquid as bis- feed inlet fractional extraction separation system of La/Ce;From La/LaCe/ PrNd/Nd tetra- export fractional extraction separation system the 8th grade of acquisitions lanthanum-cerium chloride aqueous solution of second outlet, as La/Ce bis- into Second of feed liquid of material mouth fractional extraction separation system;The of fractional extraction separation system is exported from La/LaCe/PrNd/Nd tetra- Three the 49th grade of acquisition praseodymium chloride neodymium aqueous solutions in outlet, the first feed liquid as bis- feed inlet fractional extraction separation system of Pr/Nd; The 87th grade of the outlet of fractional extraction separation system the 4th is exported from La/LaCe/PrNd/Nd tetra- and obtains load PrNd organic phase, is used as Second of feed liquid of bis- feed inlet fractional extraction separation system of Pr/Nd.
2) bis- feed inlet fractional extraction separation system of La/Ce
It is extraction organic phase with 5N lanthanum saponification P507 organic phase, exports fractional extraction point from La/LaCe/PrNd/Nd tetra- The lanthanum-cerium chloride aqueous solution for being in vitro first outlet acquisition is the first feed liquid, from the outlet La/LaCe/PrNd/Nd tetra- fractionation It is second of feed liquid that the second outlet of extraction and separation system, which obtains lanthanum-cerium chloride aqueous solution, and 3.0mol/L HCl is washing acid.5N Lanthanum is saponified P507 organic phase and enters bis- feed inlet fractional extraction separation system of La/Ce from the 1st grade, the first feed liquid comes from La/ LaCe/PrNd/Nd tetra- exports lanthanum-cerium chloride aqueous solution that fractional extraction separation system first outlet obtains from first charging aperture the 75 grades enter bis- feed inlet fractional extraction separation system of La/Ce, and second of feed liquid is from the outlet La/LaCe/PrNd/Nd tetra- fractionation The second outlet of extraction and separation system obtains lanthanum-cerium chloride aqueous solution and enters bis- feed inlet of La/Ce point from the 82nd grade of second charging aperture Extraction and separation system is evaporated, washing acid 3.0mol/L HCl enters bis- feed inlet fractional extraction separation system of La/Ce from the 96th grade.From 1st grade of outlet water phase of bis- feed inlet fractional extraction separation system of La/Ce obtains product 5N grades of lanthanum chloride solution of separation;From 96th grade of outlet organic phase of bis- feed inlet fractional extraction separation system of La/Ce obtains cerium-carrying organic phase, through with 3.2mol/L 6 grades of back extraction of HCl obtain product 3N grades of cerium chloride aqueous solution of separation.
3) bis- feed inlet fractional extraction separation system of Pr/Nd
It is extraction organic phase with 3N praseodymium saponification P507 organic phase, exports fractional extraction point from La/LaCe/PrNd/Nd tetra- The praseodymium chloride neodymium aqueous solution for the third outlet for being in vitro is the first feed liquid;Fractionation extraction is exported from La/LaCe/PrNd/Nd tetra- Taking the outlet of separation system the 4th to obtain load PrNd organic phase is second of feed liquid, and 3.0mol/L HCl is washing acid.3N praseodymium soap Change P507 organic phase and enter bis- feed inlet fractional extraction separation system of Pr/Nd from the 1st grade, the first feed liquid comes from La/LaCe/ The praseodymium chloride neodymium aqueous solution that PrNd/Nd tetra- exports the third outlet of fractional extraction separation system enters from the 25th grade of first charging aperture Bis- feed inlet fractional extraction separation system of Pr/Nd, second of feed liquid export fractional extraction separation from La/LaCe/PrNd/Nd tetra- The outlet of system the 4th obtains load PrNd organic phase and enters bis- feed inlet fractional extraction of Pr/Nd separation from the 55th grade of second charging aperture System, washing acid 3.0mol/L HCl enter bis- feed inlet fractional extraction separation system of Pr/Nd from the 103rd grade.From Pr/Nd bis- into 1st grade of outlet water phase of material mouth fractional extraction separation system obtains product 3N grades of praseodymium chloride aqueous solution of separation;It is fed from Pr/Nd bis- 103rd grade of outlet organic phase of mouth fractional extraction separation system obtains the organic phase of load neodymium, through with 6 grades of 3.5mol/L HCl Back extraction obtains product 4N grades of neodymium chloride aqueous solution of separation.
The composition of the 5N grade lanthanum chloride solution are as follows: 142.0g/L, Ce 0.00020g/L, Pr 0.00010g/L, Nd 0.000030g/L, Sm 0.000010g/L.The relative purity of 5N grades of lanthanum chloride solutions is 99.9997%.The yield of lanthanum It is 97%.
The composition of the 3N grade cerium chloride aqueous solution are as follows: La 0.030g/L, Ce 136.0g/L, Pr 0.080g/L, Nd 0.020g/L, Sm 0.00030g/L.The relative purity of 3N grades of cerium chloride aqueous solutions is 99.90%.The yield of cerium is 96%.
The composition of the 3N grade praseodymium chloride aqueous solution are as follows: La 0.00020g/L, Ce 0.0010g/L, Pr 141.0g/ L, Nd 0.020g/L, Sm 0.00010g/L.The relative purity of 3N grades of praseodymium chloride aqueous solutions is 99.98%.The yield of praseodymium is 96%.
The composition of the 4N grade neodymium chloride aqueous solution are as follows: La 0.00050g/L, Ce 0.00080g/L, Pr 0.0070g/L, Nd 139.0g/L, Sm 0.0054g/L.The relative purity of 4N grades of neodymium chloride aqueous solutions is 99.990%.Neodymium Yield is 99%.

Claims (7)

1. a kind of technique for separating light rare earth in southern ion adsorption type rare earth ore, it is characterised in that: the technique is with south It is feed liquid that ion adsorption type rare earth ore, which is grouped separating obtained complexes aqueous solution, and P507 is extractant, by three points Extraction system composition is evaporated, respectively La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system, the fractionation of bis- feed inlet of La/Ce Bis- feed inlet fractional extraction separation system of extraction and separation system and Pr/Nd;By the combination of three fractional extraction systems, Directly obtain four kinds of 5N grades of lanthanum chlorides, 3N grades of cerium chlorides, 3N grades of praseodymium chlorides and 4N grades of neodymium chlorides separation products;
La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system and opens up there are four outlet, and respectively first outlet, second go out Mouth, third outlet and the 4th outlet;First outlet is opened in La/LaCe/PrNd/Nd tetra- and exports fractional extraction separation system the 1st The water phase of grade;Second outlet is opened in the water phase among the outlet La/LaCe/PrNd/Nd tetra- fractional extraction separation system extraction section; Third outlet is opened in the water phase among the outlet La/LaCe/PrNd/Nd tetra- fractional extraction separation system washing section;4th outlet It is opened in La/LaCe/PrNd/Nd tetra- and exports last 1 grade of the organic phase of fractional extraction separation system;First outlet and second outlet It is rear extraction section between second outlet and charging grade for preceding extraction section, feeding between grade and third outlet is preceding washing section, third It is rear washing section between outlet and the 4th outlet;Preceding extraction section and rear extraction section are collectively referred to as extraction section, preceding washing section and rear washing Section is collectively referred to as washing section;The preceding extraction section that La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system realizes La/Ce separation, The rear extraction section that La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system realizes LaCe/Pr separation, La/LaCe/PrNd/ The preceding washing section that Nd tetra- exports fractional extraction separation system realizes Ce/PrNd separation, the outlet La/LaCe/PrNd/Nd tetra- fractionation extraction The rear washing section of separation system is taken to realize Pr/Nd separation;
Bis- feed inlet fractional extraction separation system of La/Ce is equipped with 2 feed inlets, respectively first charging aperture and second charging aperture; The 1st grade of bis- feed inlet fractional extraction separation system of La/Ce between first charging aperture be extraction section, first charging aperture with second into Wash section between material mouth for extraction, second charging aperture and it is 1 grade last between be washing section;
Bis- feed inlet fractional extraction separation system of Pr/Nd is equipped with 2 feed inlets, respectively first charging aperture and second charging aperture; The 1st grade of bis- feed inlet fractional extraction separation system of Pr/Nd between first charging aperture be extraction section, first charging aperture with second into Wash section between material mouth for extraction, second charging aperture and it is 1 grade last between be washing section;
Three fractional extraction systems are specific as follows:
1) La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system
It is extraction organic phase with 2N lanthanum saponification P507 organic phase, southern ion adsorption type rare earth ore is grouped separating obtained light rare earth Aqueous chloride solution is feed liquid, and 3.0mol/L HCl is washing acid;2N lanthanum is saponified P507 organic phase and enters La/LaCe/ from the 1st grade PrNd/Nd tetra- exports fractional extraction separation system, and complexes aqueous solution enters La/LaCe/PrNd/Nd tetra- from charging grade Fractional extraction separation system is exported, washing acid 3.0mol/L HCl enters the outlet La/LaCe/PrNd/Nd tetra- fractionation from last 1 grade Extraction and separation system;The first outlet for exporting fractional extraction separation system from La/LaCe/PrNd/Nd tetra- obtains 2N lanthanum chloride water Solution, the first feed liquid as bis- feed inlet fractional extraction separation system of La/Ce;From the outlet point La/LaCe/PrNd/Nd tetra- The second outlet for evaporating extraction and separation system obtains lanthanum-cerium chloride aqueous solution, is used as bis- feed inlet fractional extraction separation system of La/Ce Second of feed liquid;Praseodymium chloride neodymium water is obtained from the third outlet that La/LaCe/PrNd/Nd tetra- exports fractional extraction separation system Solution, the first feed liquid as bis- feed inlet fractional extraction separation system of Pr/Nd;From the outlet point La/LaCe/PrNd/Nd tetra- It evaporates the outlet of extraction and separation system the 4th and obtains load PrNd organic phase, as bis- feed inlet fractional extraction separation system of Pr/Nd Second of feed liquid;
2) bis- feed inlet fractional extraction separation system of La/Ce
It is extraction organic phase with 5N lanthanum saponification P507 organic phase, exports fractional extraction chorista from La/LaCe/PrNd/Nd tetra- The lanthanum-cerium chloride aqueous solution for being first outlet acquisition is the first feed liquid, exports fractional extraction from La/LaCe/PrNd/Nd tetra- It is second of feed liquid that the second outlet of separation system, which obtains lanthanum-cerium chloride aqueous solution, and 3.0mol/L HCl is washing acid;5N lanthanum soap Change P507 organic phase and enter bis- feed inlet fractional extraction separation system of La/Ce from the 1st grade, the first feed liquid comes from La/LaCe/ PrNd/Nd tetra- exports the lanthanum-cerium chloride aqueous solution that fractional extraction separation system first outlet obtains and enters La/ from first charging aperture Bis- feed inlet fractional extraction separation system of Ce, second of feed liquid export fractional extraction chorista from La/LaCe/PrNd/Nd tetra- The second outlet of system obtains lanthanum-cerium chloride aqueous solution and enters bis- feed inlet fractional extraction separation system of La/Ce from second charging aperture, Washing acid 3.0mol/L HCl enters bis- feed inlet fractional extraction separation system of La/Ce from last 1 grade;From bis- feed inlet of La/Ce 1st grade of outlet water phase of fractional extraction separation system obtains product 5N grades of lanthanum chloride solution of separation;From bis- feed inlet of La/Ce point The last 1 grade of outlet organic phase for evaporating extraction and separation system obtains cerium-carrying organic phase, through being obtained with 6 grades of back extraction of 3.2mol/L HCl 3N grades of cerium chloride aqueous solutions of product must be separated;
3) bis- feed inlet fractional extraction separation system of Pr/Nd
It is extraction organic phase with 3N praseodymium saponification P507 organic phase, exports fractional extraction chorista from La/LaCe/PrNd/Nd tetra- The praseodymium chloride neodymium aqueous solution of the third outlet of system is the first feed liquid;Fractional extraction point is exported from La/LaCe/PrNd/Nd tetra- It is in vitro that the 4th outlet obtains load PrNd organic phase as second of feed liquid, 3.0mol/L HCl is washing acid;The saponification of 3N praseodymium P507 organic phase enters bis- feed inlet fractional extraction separation system of Pr/Nd from the 1st grade, the first feed liquid comes from La/LaCe/ The praseodymium chloride neodymium aqueous solution that PrNd/Nd tetra- exports the third outlet of fractional extraction separation system enters Pr/Nd from first charging aperture Two feed inlet fractional extraction separation systems, second of feed liquid export fractional extraction separation system from La/LaCe/PrNd/Nd tetra- 4th outlet obtains load PrNd organic phase and enters bis- feed inlet fractional extraction separation system of Pr/Nd from second charging aperture, washs Sour 3.0mol/L HCl enters bis- feed inlet fractional extraction separation system of Pr/Nd from last 1 grade;It is fractionated from bis- feed inlet of Pr/Nd 1st grade of outlet water phase of extraction and separation system obtains product 3N grades of praseodymium chloride aqueous solution of separation;It is fractionated and extracts from bis- feed inlet of Pr/Nd Last 1 grade of outlet organic phase of separation system is taken to obtain the organic phase of load neodymium, through obtaining with 6 grades of back extraction of 3.5mol/L HCl Separate product 4N grades of neodymium chloride aqueous solution.
2. a kind of technique for separating light rare earth in southern ion adsorption type rare earth ore according to claim 1, feature exist In: the P507 organic phase is the sulfonated kerosene solution of extractant P507, and wherein the percentage by volume of P507 is 30%, sulfonation The percentage by volume of kerosene is 70%;In use, being obtained after corresponding saponification must be implemented using general method for saponification corresponding Rare-earth sodium saponification organic phase.
3. a kind of technique for separating light rare earth in southern ion adsorption type rare earth ore according to claim 1, feature exist In: the southern ion adsorption type rare earth ore is grouped the composition of separating obtained complexes aqueous solution are as follows: La 60.0g/L~70.0g/L, Ce 5.0g/L~7.0g/L, Pr 13.0g/L~17.0g/L, Nd 50.0g/L~60.0g/L, Sm 0.00050g/L~0.0020g/L.
4. a kind of technique for separating light rare earth in southern ion adsorption type rare earth ore according to claim 1, feature exist In: the composition of the 5N grade lanthanum chloride solution are as follows: La 136.0g/L~142.0g/L, Ce 0.00020g/L~ 0.00080g/L, Pr 0.00010g/L~0.00030g/L, Nd 0.000030g/L~0.00010g/L, Sm 0.000010g/ L~0.000030g/L.
5. a kind of technique for separating light rare earth in southern ion adsorption type rare earth ore according to claim 1, feature exist In: the composition of the 3N grade cerium chloride aqueous solution are as follows: La 0.010g/L~0.030g/L, Ce 136.0g/L~140.0g/ L, Pr 0.040g/L~0.080g/L, Nd 0.0050g/L~0.020g/L, Sm 0.00010g/L~0.00030g/L.
6. a kind of technique for separating light rare earth in southern ion adsorption type rare earth ore according to claim 1, feature exist In: the composition of the 3N grade praseodymium chloride aqueous solution are as follows: La 0.00020g/L~0.0010g/L, Ce 0.0010g/L~ 0.0030g/L, Pr 135.0g/L~141.0g/L, Nd 0.020g/L~0.10g/L, Sm 0.00010g/L~0.00050g/ L。
7. a kind of technique for separating light rare earth in southern ion adsorption type rare earth ore according to claim 1, feature exist In: the composition of the 4N grade neodymium chloride aqueous solution are as follows: La 0.00010g/L~0.00050g/L, Ce 0.00020g/L~ 0.00080g/L, Pr 0.0010g/L~0.0070g/L, Nd 139.0g/L~145.0g/L, Sm 0.0012g/L~ 0.0054g/L。
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