CN100513600C - Technique for extracting and separating rare earth elements from non-saponification system - Google Patents

Technique for extracting and separating rare earth elements from non-saponification system Download PDF

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CN100513600C
CN100513600C CNB2006100726682A CN200610072668A CN100513600C CN 100513600 C CN100513600 C CN 100513600C CN B2006100726682 A CNB2006100726682 A CN B2006100726682A CN 200610072668 A CN200610072668 A CN 200610072668A CN 100513600 C CN100513600 C CN 100513600C
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rare earth
saponification
extraction
neodymium
praseodymium
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CN101050488A (en
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龙志奇
黄小卫
彭新林
李建宁
朱兆武
赵娜
崔大立
张顺利
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Grirem Advanced Materials Co Ltd
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Grirem Advanced Materials Co Ltd
Beijing General Research Institute for Non Ferrous Metals
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Abstract

This invention provides a process for extracting and separating rare earth elements by using non-saponification extractant. The process comprises: utilizing rare earth sulfate solution containing two or more rare earth elements obtained by treating rare earth ore as the raw material, performing Nd/Sm multi-stage fractionation and extraction by using non-saponification extractant P507 to obtain Sm/Eu/Gd enriched product and La/Ce/Pr/Nd extraction raffinate, and further extracting and separating rare earth compounds with non-saponification extractant. The process has such advantages as no emulsification under low-acidity extraction, easy back extraction of medium-molecular-weight rare earth elements, low acid consumption, and high productivity.

Description

A kind of technology of extracting and separating rare earth elements from non-saponification system
Technical field
The present invention relates to a kind of technology of extracting and separating rear earth element.Specifically the rare earth sulfate solution that contains at least two kinds of rare earth elements that obtains with the processing rare-earth mineral is a raw material, adopt non-saponification P507 to carry out neodymium/samarium extraction grouping, obtain sm-eu-gd enriched substance and LaCePrNd raffinate, adopt the mixed extractant of one or both preparations among non-saponified P204 or non-saponified P204 and non-saponification P507, C272, C301, C302, HEOPPA, P350, the TBP again, the technology of extracting and separating rear earth element in the mixing solutions of LaCePrNd sulfuric acid rare earth and rare earth chloride or rare earth nitrate.
Background technology
Lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium, 17 elements of scandium are referred to as rare earth element, its character is closely similar, except that the promethium nature does not exist, other element co-exists in the rare-earth mineral, because atomic radius is close, chemical property is extremely close, separates relatively difficulty, and the main solvent extration that adopts separates on the industrial production at present.
At present, the rare earth element extraction separating method is a lot, and method commonly used on the general industry has: 1, saponification P507 hydrochloric acid system extracting and separating rear earth element ([1] rare earth chemistry collection of thesis, institute, nineteen eighty-two, Science Press should be changed in Changchun); 2, saponification naphthenate acid system separate the purification yttrium oxide ([2] Xu Guangxian chief editor, rare earth, the 2nd edition (first volume), metallurgical industry press, 2002, P590); 3, TBP nitric acid system extracting and separating rear earth element ([2] Xu Guangxian chief editor, rare earth, the 2nd edition (first volume), metallurgical industry press, 2002, P495); 4, non-saponification P204 extracting and separating rear earth element ([3] Chinese patent CN 80105043.6) from sulfuric acid system.1st, 2 kinds of method good separating effects are used very extensively, but must adopt saponification such as ammoniacal liquor or bicarbonate of ammonia, produce a large amount of ammonia nitrogen waste waters, and environment is caused bigger pollution.The 3rd kind of method is the technology that French Rhodia, U.S. molybdenum company adopt, and it is to be derived from the rare earth nitrate solution that obtains when handling solitary stone ore to come rare-earth separating, this technology extraction system concentration of nitric acid height, and therefore, the production cost height is in halted state at present substantially.The 4th kind of technology is Beijing Non-Ferrous Metal Research General Academy's invention, extracting and separating rear earth element the rare earth sulfate solution that is applied to when sulfuric acid roasting method is handled the packet header rare-earth mineral, obtain, the non-saponification P204 of this process using extracting and separating, do not produce ammonia nitrogen waste water, alkali consumption is few, but since the sulfuric acid system rare earth concentration low (＜45g/L), the investment of equipment extraction agent is big, P204 extracting power under acidic conditions is very strong, easily produce emulsification when feed acidity is low, need add a certain amount of acid during extraction, and middle heavy rare earths back extraction is very difficult, strip liquor spent acid height, acid consumption is big.
Summary of the invention
The technology that the purpose of this invention is to provide a kind of extracting and separating rare earth elements from non-saponification system, this technology extract under low acidity and emulsification do not occur, and middle heavy rare earths back extraction is easy, reduces acid consumption and cost, improves production capacity, the minimizing investment.
The present invention is by the following technical solutions for achieving the above object:
The present invention utilizes the more weak characteristic of P507 acidity, adopts non-saponification P507 to carry out neodymium/samarium extraction grouping in rare earth sulfate solution, emulsification do not occur to realize extraction under the low acidity.
The present invention adopts non-saponification P507 as extraction agent, to reduce strip liquor spent acid, consumes and cost thereby reduce acid.
The present invention is in order to improve the rare earth concentration of organic phase and aqueous phase in the extraction process, replace the sulfuric acid of 1N to make washing lotion with high density chlorination rare earth or rare earth nitrate strip liquor, make extraction extracting and separating rear earth element in the mixed solution system of the sulfuric acid rare earth of high density and rare earth chloride or rare earth nitrate, to reduce sour consumption, improve production capacity, reduce investment.
The rare earth sulfate solution that contains at least two kinds of rare earth elements that obtains with the processing rare-earth mineral is a raw material, adopt non-saponification P507 (organic phase) to carry out the multistage fractionation extraction grouping of neodymium/samarium, obtain sm-eu-gd enriched substance and LaCePrNd raffinate, adopt the further extracting and separating rear earth compound of non-saponifiable extraction agent again
Described raw material is that sulfuric acid process is handled the rare earth sulfate solution that the light rare earths ore deposit obtains, and its acidity is pH 1-5, and content of rare earth REO is 10-100g/L, and this solution also may contain a small amount of Cl -And/or NO 3 -And/or multiple non-rare earth ion; One or more organic solvent dilutings to 0.1-1.7mol/L in used organic phase kerosene, solvent oil, alkane, the alcohols.
Described rare earth sulfate solution adopts the non-saponification P507 of 0.5-1.5mol/L to carry out the multistage fractionation extraction grouping of neodymium/samarium, washing lotion adopts 2-7N hydrochloric acid or nitric acid or rare earth concentration 100-300gREO/L to contain the strip liquor of sm-eu-gd rare earth chloride or rare earth nitrate, the supported rare earth organic phase obtains the sm-eu-gd enriched substance with the back extraction of 3-7N hydrochloric acid, further extracting and separating samarium, europium, gadolinium; What obtain contains the mixing solutions that the LaCePrNd raffinate is LaCePrNd sulfuric acid rare earth and rare earth chloride or rare earth nitrate (water), be neutralized to PH2-5, use the non-saponification P204 of 0.5-1.7mol/L (D2EHPA again, two (2-ethylhexyl phosphates)) or non-saponified P204 and non-saponification P507 (HEH/EHP, di-2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester), C272 (two (2,4, the 4-tri-methyl-amyl) phosphonic acids), C301 (two (2,4, the 4-tri-methyl-amyl) phosphonothionic acid), C302 (two (2,4, the 4-tri-methyl-amyl) single phosphonothionic acid), C 923 (HEOPPA straight chained alkyl phosphine oxide), P350 (methyl acid phosphate dimethyl heptyl ester), the mixed extractant (organic phase) of one or both preparations among the TBP (tributyl phosphate) carries out abstraction and type-reverting or further extracting and separating rear earth compound.
(1) described LaCePrNd raffinate is neutralized to PH2-5, use again the non-saponification P204 of 0.5-1.7mol/L with whole rare earth extractions in organic phase, use 3-7N hydrochloric acid or nitric acid back extraction to prepare LaCePrNd rare earth chloride or rare earth nitrate then.
(2) described contain the LaCePrNd raffinate and be neutralized to pH2-5 after, adopt non-saponification P204 of 0.5-1.7mol/L or non-saponification mixed extractant to carry out praseodymium/neodymium extracting and separating, it is rare earth chloride or the rare earth nitrate strip liquor that 100-300g/L REO contains neodymium that washing lotion adopts 2-7N hydrochloric acid or nitric acid or rare earth concentration; The supported rare earth organic phase obtains Neodymium trichloride or neodymium nitrate with 2-7N hydrochloric acid or nitric acid back extraction; Obtain contain the La-Ce-Pr raffinate and be neutralized to PH2-5 again after, with the non-saponification P204 extraction of 0.5-1.7mol/L La-Ce-Pr, 2-7N hydrochloric acid or nitric acid back extraction prepare La-Ce-Pr rare earth chloride or rare earth nitrate.
(3) described contain the LaCePrNd raffinate and be neutralized to pH2-5 after, adopt non-saponification P204 of 0.5-1.7mol/L or non-saponification mixed extractant to carry out cerium/praseodymium extraction grouping, it is rare earth chloride or the rare earth nitrate strip liquor that 100-300g/L REO contains the praseodymium neodymium that washing lotion adopts 2-7N hydrochloric acid or nitric acid or rare earth concentration; The supported rare earth organic phase obtains praseodymium chloride neodymium or praseodymium nitrate neodymium with 2-7N hydrochloric acid or nitric acid back extraction; The lanthanum cerium raffinate that contains that obtains is produced the Phosbloc cerium with ammonium bicarbonate precipitation, or after being neutralized to PH2-5, with the non-saponification P204 extraction of 0.5-1.7mol/L lanthanum cerium, 2-7N hydrochloric acid or nitric acid back extraction prepare lanthanum cerium rare earth chloride or rare earth nitrate, and praseodymium neodymium and lanthanum cerium compound be further extracting and separating single rare earth compound all.
(4) the described LaCePrNd raffinate that contains is neutralized to pH2-5, adopt non-saponification P204 of 0.5-1.7mol/L or non-saponification mixed extractant to carry out lanthanum/cerium/praseodymium three outlet extracting and separating, employing contains 2-7N hydrochloric acid or nitric acid or praseodymium neodymium rare earth chloride or rare earth nitrate strip liquor wash load rare earth organic phase, open a water in extraction section and export out a part of cerium-rich solution, its cerium oxide content〉65%, produce rich cerium product through precipitation; Load praseodymium neodymium organic phase obtains praseodymium chloride neodymium or praseodymium nitrate neodymium with 2-7N hydrochloric acid or nitric acid back extraction; The lanthanum raffinate that contains that obtains is produced Phosbloc or lanthanum trioxide with ammonium bicarbonate precipitation, or after being neutralized to PH2-5, with the non-saponification P204 extraction of 0.5-1.7mol/L, hydrochloric acid or nitric acid back extraction prepare the compound of the lanthanum of 99.9-99.99%.
Advantage of the present invention:
When 1) non-saponified P204 carries out neodymium/samarium extraction grouping in earth solution, because extraction quantity, compare (organic/water, volume ratio) less, P204 extracting rare-earth in low acidic solution is very capable, must in feed liquid, add sulfuric acid acidity is adjusted to 0.2N from PH4, need add 0.26 ton of vitriol oil by rare earth oxide calculating per ton, P204 just can not produce supersaturation emulsification, the present invention adopts in the non-saponification P507 earth solution and carries out extracting and separating, the extraction feed liquid need not added acid, and the easy back extraction of the organic extractant of heavy rare earths in the load, strip liquor spent acid is reduced more than 50%, reduce acid consumption about 30%;
2) replace the sulfuric acid of 1N to make washing lotion with high density chlorination rare earth or rare earth nitrate strip liquor, make extraction extracting and separating rear earth element in the mixed rare earth solution of the sulfuric acid rare earth of high density and rare earth chloride or rare earth nitrate, the rare earth concentration of outlet organic phase and washing section aqueous phase improves 3-4 times, can improve stripping efficiency, reduce sour consumption 10%, improve throughput, reduce investment;
4) adopt the non-saponification organic phase extracting rare-earth separating, technology is simply continuous, easy to control, and main chemical materials consumes low, and extraction process do not produce ammonia nitrogen waste water, can save three wastes processing cost greatly.
Embodiment
Below with embodiment technology of the present invention is described further.Protection domain of the present invention is not subjected to the restriction of these embodiment, and protection domain of the present invention is determined by claims.
Embodiment 1
Hamartite and monazite mixed type rare-earth mineral (REO 50%) through sulfuric acid baking, water logging, in and removal of impurities, obtain purified rare earth sulfate solution, its acidity is pH 4, main component is REO 40g/L, Fe＜0.05g/L, P＜0.005g/L, ThO 2＜0.001g/L, directly adopt non-saponification 1.0mol/L P507 to carry out Nd/Sm extraction grouping, adopt 8 grades of extractions, 15 grades of washings, 8 grades of back extractions, compare: organic/feed liquid/backwash acid=0.20/1/0.012, washing lotion adopts the re chloride that contains sm-eu-gd 245g/l, acidity 0.2N, the washing section rare earth concentration is 252g/l, and the supported rare earth organic phase contains rare earth 15g/l, with the back extraction of 5N hydrochloric acid, obtain containing REO 245g/l, acidity is the re chloride of the sm-eu-gd enriched substance of 0.2N, produces sm-eu-gd enriched substance product, wherein Nd through oxalic acid precipitation-calcination 2O 3Content is less than 0.01%.
LaCePrNd raffinate (the Sm that obtains 2O 3Content is less than 0.005%), be neutralized to PH4 with magnesium oxide, adopt the non-saponification P204 of 1.5mol/l to extract entirely, 5.5N the hydrochloric acid back extraction obtains containing the re chloride of LaCePrNd 267g/l, produces LaCePrNd rare earth chloride product through condensing crystal, REO wherein〉45%, Sm 2O 3Content is less than 0.005%.From the rare earth sulfate solution to the product, the rare earth total recovery is 98.2%.
Embodiment 2
Hamartite (REO 60%) is through sulfuric acid baking, water logging, in and removal of impurities, obtain purified rare earth sulfate solution, its acidity is pH 4.5, rare earth concentration is REO 36g/L, carry out Nd/Sm extraction grouping with non-saponification 0.5mol/L P507, adopt 10 grades of extractions, 18 grades of washings, 9 grades of back extractions, washing lotion are adopted and are contained sm-eu-gd 255g/l, the re chloride of acidity 0.3N, the supported rare earth organic phase contains rare earth 12g/l, with the back extraction of 5.2N hydrochloric acid, obtain containing REO 255g/l, acidity is the sm-eu-gd re chloride of 0.3N, and sm-eu-gd enriched substance or further extracting and separating extraction samarium are produced in calcination through the precipitation oxalic acid precipitation, europium, gadolinium single rare earth product.
The LaCePrNd raffinate that contains that obtains is neutralized to pH4.5 with magnesium oxide, adopt 85% (volume percent then, below all with) the non-saponification P204 of 1.3mol/L carries out praseodymium/neodymium fractionation extraction with the mixed extractant of the non-saponification P507 of 15%1.3mol/L and separates, washing lotion adopts and contains neodymium rare earth nitrate strip liquor (REO 240g/L), the 5.5N nitric acid back extraction of supported rare earth organic phase; Through 32 grades of extractions, 38 grades of washings, 6 grades of back extractions obtain neodymium nitrate (REO 240g/L, Nd 2O 3Purity is greater than 99.9%); Raffinate is neutralized to PH4.5, with the non-saponification P204 of 1.5mol/L extraction La-Ce-Pr, the back extraction of 6N hydrochloric acid, condensing crystal prepare La-Ce-Pr rare earth chloride product (REO〉45%, Nd 2O 3Content is less than 0.05%).From the rare earth sulfate solution to the product, the rare earth total recovery is 96.8%.
Embodiment 3
The fore portion operation is with embodiment 2
The LaCePrNd raffinate that contains that obtains is neutralized to pH4 with magnesium oxide, adopts the mixed extractant (with No. 200 solvent oils dilutions) of the non-saponification C272 of the non-saponification P204 of 90% 1.5mol/L and 10% 1.5mol/L to carry out cerium/praseodymium fractionation extraction grouping then.Washing lotion adopts and contains praseodymium neodymium rare earth chloride strip liquor (REO 258g/L), the 6.0N hydrochloric acid back extraction of supported rare earth organic phase; Through 23 grades of extractions, 32 grades of washings, 6 grades of back extractions obtain praseodymium chloride neodymium (CeO 2Content is less than 0.05%); Raffinate is neutralized to PH4.5 with magnesium oxide, with the non-saponification P204 of 1.5mol/L extraction lanthanum cerium, the back extraction of 5.3N hydrochloric acid, the lanthanum-cerium chloride solution that obtains through condensing crystal prepare lanthanum cerium rare earth chloride (REO〉45%, Pr 6O 11, Nd 2O 3Content is all less than 0.05%).From the rare earth sulfate solution to the product, the rare earth total recovery is 97.3%.
Embodiment 4
The fore portion operation is with embodiment 2.
The LaCePrNd raffinate is neutralized to pH4 with magnesium oxide, adopts the non-saponification P204 of 1.2mol/L (with No. 200 solvent oil dilutions) organic phase to carry out lanthanum/cerium/praseodymium three outlet extracting and separating then.Employing contains praseodymium neodymium rare earth chloride strip liquor (REO 240g/L) washing organic phase, opens a water outlet (the 3rd outlet) 22 grades of extraction sections and goes out a part of lanthanum cerium solution (cerium〉65%), produces rich cerium product through precipitation; The supported rare earth organic phase obtains praseodymium neodymium re chloride with the back extraction of 5.5N hydrochloric acid, produces praseodymium neodymium oxides product (CeO through the oxalic acid precipitation calcination 2Content is less than 0.05%, Sm 2O 3Content is less than 0.01%); It is 99.9% Phosbloc that raffinate obtains purity with ammonium bicarbonate precipitation, and calcination obtains lanthanum trioxide.From the rare earth sulfate solution to the product, the rare earth total recovery is 97.1%.

Claims (9)

1, a kind of technology of non-saponifiable extraction agent extracting and separating rear earth element is characterized in that: the rare earth sulfate solution that contains at least two kinds of rare earth elements that obtains with the processing rare-earth mineral is a raw material, adopt non-saponification P507 to carry out the multistage fractionation extraction grouping of neodymium/samarium, obtain sm-eu-gd enriched substance and LaCePrNd raffinate, adopt the further extracting and separating rear earth compound of non-saponifiable extraction agent again.
2, technology as claimed in claim 1, it is characterized in that, described raw material is that sulfuric acid process is handled the rare earth sulfate solution that the light rare earths ore deposit obtains, its acidity is pH1-5, rare earth REO content is 10-100g/L, one or more organic solvent dilutings to the 0.1-1.7mol/L in used organic phase kerosene, solvent oil, alkane, the alcohols.
3, technology as claimed in claim 1, it is characterized in that, described rare earth sulfate solution adopts the non-saponification P507 of 0.5-1.5mol/L to carry out the multistage fractionation extraction grouping of neodymium/samarium, washing lotion adopts 2-7N hydrochloric acid or nitric acid or contains the strip liquor of sm-eu-gd rare earth chloride or rare earth nitrate, and its rare earth concentration REO is 100-300g/L; The supported rare earth organic phase obtains the sm-eu-gd enriched substance with the back extraction of 3-7N hydrochloric acid, the LaCePrNd raffinate that contains that obtains is neutralized to pH2-5, uses the mixed extractant of one or both preparations among non-saponification P204 of 0.5-1.7mol/L or non-saponified P204 and non-saponification P507, C272, C301, C302, HEOPPA, P350, the TBP to carry out extracting and separating again.
4, technology as claimed in claim 3, it is characterized in that, described LaCePrNd raffinate is the mixing solutions of LaCePrNd sulfuric acid rare earth and rare earth chloride or rare earth nitrate, employing 1.0-1.7mol/L P204 in organic phase, uses 3-7N hydrochloric acid or nitric acid back extraction to prepare LaCePrNd rare earth chloride or rare earth nitrate whole rare earth extractions then.
5, the described technology of claim 3, it is characterized in that, described contain the LaCePrNd raffinate and be neutralized to pH2-5 after, adopt non-saponification P204 of 0.5-1.7mol/L or non-saponification mixed extractant to carry out praseodymium/neodymium extracting and separating, it is the strip liquor that contains neodymium rare earth chloride or rare earth nitrate of 100-300g/L REO that washing lotion adopts 2-7N hydrochloric acid or nitric acid or rare earth concentration, and the supported rare earth organic phase obtains Neodymium trichloride or neodymium nitrate with 2-7N hydrochloric acid or nitric acid back extraction; Obtain contain the La-Ce-Pr raffinate and be neutralized to PH2-5 again after, with the non-saponification P204 extraction of 0.5-1.7mol/L La-Ce-Pr, 2-7N hydrochloric acid or nitric acid back extraction prepare La-Ce-Pr rare earth chloride or rare earth nitrate.
6, technology as claimed in claim 3, it is characterized in that, described contain the LaCePrNd raffinate and be neutralized to pH2-5 after, adopt non-saponification P204 of 0.5-1.7mol/L or non-saponification mixed extractant to carry out cerium/praseodymium extraction grouping, washing lotion adopt 2-7N hydrochloric acid or nitric acid or rare earth concentration be 100-300g/L REO contain praseodymium neodymium rare earth chloride or rare earth nitrate strip liquor; The supported rare earth organic phase obtains praseodymium chloride neodymium or praseodymium nitrate neodymium with 2-7N hydrochloric acid or nitric acid back extraction; The lanthanum cerium raffinate that contains that obtains is produced the Phosbloc cerium with ammonium bicarbonate precipitation, or after being neutralized to PH2-5, with the non-saponification P204 extraction of 0.5-1.7mol/L lanthanum cerium, 2-7N hydrochloric acid or nitric acid back extraction prepare lanthanum cerium rare earth chloride or rare earth nitrate.
7, technology as claimed in claim 6 is characterized in that, described praseodymium neodymium and the further extracting and separating single rare earth of lanthanum cerium compound compound.
8, technology as claimed in claim 3, it is characterized in that, the described LaCePrNd raffinate that contains is neutralized to pH2-5, adopt non-saponification P204 of 0.5-1.7mol/L or non-saponification mixed extractant to carry out lanthanum/cerium/praseodymium three outlet extracting and separating, employing contains 2-7N hydrochloric acid or nitric acid or praseodymium neodymium rare earth chloride or rare earth nitrate strip liquor wash load rare earth organic phase, open a water in extraction section and export out a part of cerium-rich solution, its cerium oxide content 65%, produce rich cerium product through precipitation; Load praseodymium neodymium organic phase obtains praseodymium chloride neodymium or praseodymium nitrate neodymium with 2-7N hydrochloric acid or nitric acid back extraction; The lanthanum raffinate that contains that obtains is produced Phosbloc or lanthanum trioxide with ammonium bicarbonate precipitation, or after being neutralized to PH2-5, with the non-saponification P204 extraction of 0.5-1.7mol/L, hydrochloric acid or nitric acid back extraction prepare the compound of the lanthanum of 99.9-99.99%.
9, technology as claimed in claim 1 or 2 is characterized in that, the further extracting and separating of described sm-eu-gd enriched substance.
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