CN102828026A - Method for extracting and separating rare earth element by utilizing acidic extractant - Google Patents
Method for extracting and separating rare earth element by utilizing acidic extractant Download PDFInfo
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- CN102828026A CN102828026A CN2012103673254A CN201210367325A CN102828026A CN 102828026 A CN102828026 A CN 102828026A CN 2012103673254 A CN2012103673254 A CN 2012103673254A CN 201210367325 A CN201210367325 A CN 201210367325A CN 102828026 A CN102828026 A CN 102828026A
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Abstract
The invention relates to a method for extracting and separating rare earth element by utilizing an acidic extractant. The method comprises the key points that citric acid or citrate is added into a rare earth chloride solution to form a rare earth chloride-hydrochloric acid-citric acid mixed solution as a water phase and a P204 or P507 acidic phosphorous type extractant used for extraction and separation, kerosene is diluted to be taken as an organic phase for extraction and separation, and extraction, washing and reextraction are carried out in an extraction tank, thus rare earth element is separated; and raffinate containing the citric acid is returned and recycled. The method disclosed by the invention has the characteristics that complexing action of the citric acid and the rare earth element is utilized, the effect for separating the rare earth element by the acidic phosphorous type extractant is enhanced, and especially the rare earth elements in high-concentration rare earth solution with REO (rare earth oxide) being equal to 200-300g/L can be separated; and the acidic phosphorous type extractant still has higher rare earth element extracting capacity and effect without being subjected to saponification treatment conditions. The method disclosed by the invention has less investment and low production cost and reduces pollution to the environment.
Description
Technical field
The present invention relates to a kind of method of acidic extractant extracting and separating rear earth element, be specifically related to from contain multiple REE chloride soln, adopt acidic extractant complexing extraction to isolate the method for single or a few group rare-earth elements.
Background technology
REE is lanthanum and lanthanon and the scandium in the periodic table of elements, the general name of yttrium.These elements have special physics and chemical property, and in metallurgy, petrochemical complex, glass-ceramic field and various functional materials, the normal a kind of or a few kinds of elements wherein of selecting use as additive and necessary moity.
Symbiosis is together in natural mineral for REE.REE in hamartite, solitary stone ore and fluorine carbon cerium and the urdite mixed type rare-earth mineral is main with bright-coloured, cerium, praseodymium, neodymium and a spot of other REEs, so be called the light rare earths mineral.With yttrium is that the mineral of main rare earth composition are called the heavy rare earths mineral.Hamartite often adopts oxidizing roasting to decompose, and solitary stone ore and fluorine carbon cerium and urdite mixed type rare-earth mineral mainly adopt sulfuric acid baking or sodium hydroxide to decompose.Mineral after the decomposition add mineral acid (hydrochloric acid, sulfuric acid, nitric acid) solution, through leaching and removing the non-rare earth impurity technological process and can prepare the identical mixing solutions of REE (hereafter is a light rare earths ore deposit partition) that contains with former mineral.
In order to obtain single rare earth element or a few kinds of products that rare earth is elementary composition, organic solvent extract extraction process commonly used separates its REE in the industry.The technology of typical organic solvent extract extracting and separating rear earth element can be divided into following several types by the molecular structure of extraction agent:
1, neutral extraction agent: TBP (tbp) or P350 (the hot fat of methyl acid phosphate di-secondary) separation of rare earth elements method.At first neutral extraction agent is diluted to the organic phase that contains the finite concentration extraction agent with kerosene in this technology, then organic phase separates REE with rare earth nitrate solution through repeatedly mixing with the clarification operation again.Because this technology is main industrial chemicals with nitric acid, become to produce the cost height, and operating environment is relatively poor, seldom adopt at present.
2, carboxylic acid extraction agent: naphthenic acid separation of rare earth elements method.At first naphthenic acid is diluted to the organic phase that contains the finite concentration extraction agent with kerosene and alcohol mixture in this technology, then organic phase separates REE with hydrochloric acid or rare earth sulfate solution through repeatedly mixing with the clarification operation again.Because naphthenic acid and acidic organophosphorus extractant for extraction REE order difference, this technology has remarkable advantages aspect the high-purity yttrium extracting, still for the full separation of REE far away from other several kinds of extraction agents.
3, acidic organophosphorus extractant: two (2 one ethylhexyl phosphoric acid) (P204 hereinafter referred to as) or 2 one ethylhexyl phosphoric acid list ethylhexyl fat (being called P507) extraction agent separation of rare earth elements.At first P204 or P507 are diluted to the organic phase that contains the finite concentration extraction agent with kerosene in this technology, then organic phase separates REE with hydrochloric acid or rare earth sulfate solution through repeatedly mixing with the clarification operation again.
Naphthenic acid, P204 and P507 belong to the acid type extraction agent; Hydrogen ion generation replacement(metathesis)reaction in the hydroxyl of the shuttle base of the metallic cation of extraction process aqueous phase and naphthenic acid or P204 and P507; Metals ion and extraction agent help collection; Hydrogen ion gets into organic phase, and with constantly carrying out of extraction process, the acidity of aqueous phase increases.Because acid type extraction agent extracting metals ionic ability increases and significantly reduces with the acidity in the aqueous solution, causes extraction agent to lose extracting power the most at last.Solution to this problem is before the extracting metals ion, at first extraction agent is carried out saponification, promptly with containing Na
+, NH4
+Or Ca
2+The ionic basic soln is handled extraction agent, with Na
+, NH4
+Or Ca
2+The tradable H of part in the ionic replacement extraction agent
+Dry ion.Extraction agent after the saponification has the good extracting power and the effect of separation of rare earth elements, makes P204 and P507 extraction agent can satisfy the requirement of the full separation industries of rare earth, and particularly the P507 extraction agent has been widely used in the separation of produced of REE.
Na
+Or NH4
+Method for saponification need be used a large amount of alkali, and saponification again at every turn in organic phase recycles, and production cost is increased, and has reduced economic benefit.Patent 200410050948.4 discloses a kind of Ca
2+Or Mg
2+The method of basic soln saponification acid type extraction agent.This kind method replaces sodium hydroxide and ammoniacal liquor and bicarbonate of ammonia with the oxide compound or the carbonate of inexpensive calcium or magnesium, and production cost is reduced.But find in producing that the calcium of industrial level or the oxide compound or the carbonate of magnesium contain a spot of aluminium impurity, when using as saponifying agent with it, aluminium is enrichment in extraction tank, often causes the purity of rare-earth products not reach customer requirements.If oxide compound or carbonate with highly purified calcium or magnesium then do not have remarkable advantages on the price.
Comparatively speaking, with ammoniacal liquor or hydrogen-carbonate by the NH4 that is raw material
+The method for saponification production cost is moderate, and the purity of rare-earth products does not receive the influence of saponifying agent, is that the separation of rare earth elements main method is gone up in industry at present.The shortcoming of this kind method is to contain a large amount of ammonia nitriding compounds in the extraction wastewater, and directly discharging is with the polluted water resource.To this problem, once reclaimed ammonium chloride in the production, but seldom adopted because cost recovery is too high with evaporation concentration method.
This shows that in today of industrial production and nature harmonious coexistence, the solvent extraction method separation of rare earth elements technology of exploitation cleaning is imperative.In order to reach this purpose, preferred measure is under non-saponifying prerequisite, improves P204 and P507 extraction agent extracting metals ion ability.Patent 200510098261.4 discloses the method for non-saponified P204 and P507 extraction agent separation of rare earth elements in earth solution.This method in P204, add a certain proportion of P507, overcome P204 is easy to emulsification and the difficult back extraction of middle heavy rare earth element during the extracting rare-earth ion under low acidity feed liquid condition problem.No ammonia nitrogen waste water produces in this extraction process, and has reduced sour consumption.But patent 200510098261.4 application examples have only confirmed that (effect of extracting of REO ≦ 48g/L) does not relate to the earth solution (REO=200 of high density to this method at lower following of concentration of metal ions
~3008/L) rare earth extraction division technique.
Summary of the invention
The present invention seeks to weak point, a kind of method of acidic extractant extracting and separating rear earth element is provided to prior art.Promptly adopt the rare earth chloride one hydrochloric acid one Hydrocerol A mixing solutions that in re chloride, adds Hydrocerol A or Citrate trianion formation; Utilize the complexing action of Hydrocerol A; Strengthened the effect of acidic organophosphorus extractant separation of rare earth elements, especially solving the earth solution that goes for high density is REO=200
~The rare earth extraction separating effect of 300g/L.This kind is the method for the acidic phosphorus type extracting and separating rear earth element of complexing agent with the Hydrocerol A; Still have and identical ability and the separation of rare earth elements effect of saponifiable extraction agent extraction rare earth element under the saponification treatment condition at acidic organophosphorus extractant; Reach simultaneously and reduce production costs, and reduced environmental pollution.
The technical scheme that realizes the object of the invention is: being called P204 or 2 one ethylhexyl phosphoric acid list ethylhexyl fat with two (2 one ethylhexyl phosphoric acids), to be called P507 be acidic organophosphorus extractant; With the organic phase of kerosene dilution as extracting and separating; Main points are in re chloride, to add Hydrocerol A or Citrate trianion forms the water of rare earth chloride one hydrochloric acid one Hydrocerol A mixing solutions as extracting and separating, contain Hydrocerol A or Hydrocerol A salt concn ≦ 0.25mol/L in the solution; The organic phase of above-mentioned extracting and separating and water through extraction, washing and reextraction, separate REE in extraction tank; The raffinate that contains Hydrocerol A returns and recycles.
As the kerosene that thinner is used, select 260 for use
#Sulfonated kerosene or aviation kerosene are 1.0 with the acidic organophosphorus extractant dilution for concentration
~1.5 mol/L is with this organic phase as extracting and separating.
At least contain two kinds of REEs in the above-mentioned re chloride.This solution is with the rare earth oxide summation meter, and concentration is REO=10
~300 grams per liters.Selecting and choosing strength of solution earlier is REO=200
~3 00 grams per liters.
The Citrate trianion that in re chloride, adds recited above is selected Trisodium Citrate or Hydrocerol A lanthanum for use
The present invention selects for use with two (2 one ethylhexyl phosphoric acids) when being acidic organophosphorus extractant, and the pH value of rare earth chloride-hydrochloric acid one Hydrocerol A mixing solutions of preparation is 0.5
~2, when being acidic organophosphorus extractant with 2 one ethylhexyl phosphoric acid list ethylhexyl fat, the pH value of the rare earth chloride one hydrochloric acid one Hydrocerol A mixing solutions of preparation is 1
~1.5.
The present invention is to returning use through the raffinate that contains Hydrocerol A of isolating REE; Be meant that with rare earth carbonate or rare-earth hydroxide deposition circulation is used to prepare rare earth chloride one hydrochloric acid, one Hydrocerol A mixing solutions or preparation Hydrocerol A rare-earth products to the rare earth Citrate trianion that obtains as additive.
The present invention and oneself have compared with techniques; Outstanding feature is: select for use Hydrocerol A as helping the collection agent, add in the re chloride, utilize the complexing action of Hydrocerol A; Strengthened the effect of acidic organophosphorus extractant separation of rare earth elements; This kind is the acidic organophosphorus extractant separation of rare earth elements of complexing agent with the Hydrocerol A, need not pass through under the condition that saponification handles at acidic organophosphorus extractant, still can reach the effect of the ability separation of rare earth elements identical with saponifiable extraction agent extracting rare-earth element.
In addition, the raffinate that contain Hydrocerol A of the present invention behind the extracting and separating rear earth element can obtain sufficient recycle.
By the characteristics that the invention described above had, and produced tangible positively effect:
1, do not need saponifying agent in the production, reduced production cost, omitted the saponification treating processes, saved the saponification facility investment and reduced pollution, more help production process control and management simultaneously environment;
2, with the Hydrocerol A be complexing agent,, can realize making the earth solution REO=2003 of high density as the method that helps collection agent separation of rare earth elements of acidic organophosphorus extractant
~REE among 00 g/L is able to separate.
3, owing to contain the recycle of the raffinate of Hydrocerol A, production cost can not improved because of the use of Hydrocerol A.
Embodiment
Related re chloride all is by hamartite in the instance of the present invention, and solitary stone ore or hamartite and urdite mixed type rare-earth mineral are raw material, adopts known method formulated, to this, below no longer repeat among the embodiment.
Example 1
Is the organic phase that contains P204=1.5 ± 0.2mo1/L with P204 (commercially available) extraction agent with 26 few sulfonated kerosene (commercially available) dilutions.By the re chloride that the preparation of solitary stone ore obtains, the total concn REO=280 ± 20g/L partition of rare earth element wherein that contains REE in the percentage ratio of each REE quality of oxide compound and the ratio of total rare earth oxide compound REO quality is: La
2O
3/ REO=25%; CeO
2=51%; Pr
6O
11=6.5%; Nd
2O
3=15.5%; Middle heavy rare earths (in oxide compound)=2%.In this solution, add Hydrocerol A; Be mixed with and contain Hydrocerol A 0.23 ± 0.02mo1/L, the rare earth aqueous solution of pH=0.5-1, with the organic phase for preparing and rare earth aqueous solution by volume 1:l charge into extraction tank; Carrying out LaCePrNd with the fractionation extn mode separates with middle heavy rare earths; The fractionation extn progression that adopts is: extract 14 grades, wash 8 grades, strip 8 grades; Stream than (get into the volumetric flow rate of the various liquid of extraction tank, unit representes with L/min) is: organic phase: earth solution: washing lotion=2.1:1:0.3; Collection has the basin acid elution of the organic phase of REE with 3N, and the hydrochloric acid of 6N is stripped, and returns extraction cycle through the organic phase of stripping and uses.The solution of heavy rare-earth oxide 230g/L during this time extracting and separating obtains containing, this solution is used for producing the heavy rare-earth oxide product.
Separate with middle heavy rare earths through above-mentioned LaCePrNd and to obtain raffinate and contain La
2O
3+ CeO
2+ Pr
6O
11+ Nd20
3=230g/L, acidity=0.2N, this solution is neutralized to pH=1 with the carbonate of light rare earths, carries out NdPr with fractionation extn side's same form and separates with CeLa.The fractionation extn progression that adopts is: extract 47 grades, wash 43 grades, strip 8 grades; Stream is than being: organic phase: earth solution: washing lotion=7.5:1:0.5; Collection has the salt acid elution of the organic phase of REE with 3N, and the hydrochloric acid of 6N is stripped.Contain praseodymium neodymium rare earth compound 210g/L in the anti-stripping agent after the extracting and separating, this solution is used to produce mishmetal praseodymium neodymium oxides product.
Separate the raffinate acidity that contains the lanthanum Ce elements that obtains with CeLa through NdPr and be about 0.1
~0.2N.This solution can be neutralized to pH=1 with the cerium carbonated rare earth, 25 grades of extractions, washs 35 grades, carries out C in 8 grades the fractionation extn groove of stripping.Separate with La; Stream is than being organic phase: earth solution: washing lotion=8.5:1:0.2; Collection has the salt acid elution of the organic phase of Ce element with 3N, and the hydrochloric acid of 6N is stripped, and obtains containing Ce0
2=230}g/L, the solution of acidity=0.2N, this solution is used to produce cerium oxide product.
The raffinate acidity that contains lanthanum element is about 0.1N, can be neutralized to pH=4 with Phosbloc or lanthanum hydroxide earlier, makes Hydrocerol A and lanthanum in the solution form the solid rare earth Citrate trianion, and from solution, precipitates and separate out.The solid rare earth Citrate trianion that obtains thus replaces Hydrocerol A to add in the mixed rare earth solution as additive, is recycled and reused for preparation muriate one Hydrocerol A mixing solutions or is used to prepare the Hydrocerol A rare-earth products.
The method that the above-mentioned various earth solutions that obtain through extracting and separating can be further used for producing rare earth oxide is: adopt oxalic acid or ammonium bicarbonate precipitation respectively, be converted into corresponding rare-earth salts, again through the baked for producing rare earth oxide.Resulting rare earth oxide product gas purity is respectively: middle heavy rare-earth oxide=230g/L, Pr
6O
11+ Nd20
3/ REO>=99.9%; CeO
2/ RE0>=99%; La
2O
3/ RE0>=99%.The utilization ratio of whole process Hydrocerol A is greater than 85%, and the yield of REE is greater than 95%.
Embodiment 2
The separation method that present embodiment adopted is identical with embodiment 1, and difference is: (1) with P204 (commercially available) extraction agent with commercially available 260
#Sulfonated kerosene (commercially available) dilution is for containing the organic phase of P204=1.0 ± 0.2mo1/L.(2) mixed rare earth solution that obtains by fluorine carbon cerium and urdite mixed type rare-earth mineral; Employing is obtained by the dissolving with hydrochloric acid mixed rare earth carbonate; This solution contains REE, and (re chloride of REO=220 ± 20g/L), the partition of rare earth element in the solution in the percentage ratio of each REE quality of oxide compound and the ratio of total rare earth oxide compound REO quality is: La
2O
3/ REO=53%; Ce0
2=15%; Pr
60
11=10%; Nd
20
3=20%; Middle heavy rare earths (in oxide compound)=2%.(3) add Hydrocerol A, be mixed with and contain Hydrocerol A 0.23 ± 0.02mo1/L, pH=1.0
~2.0 rare earth aqueous solution.(4) LaCePrNd and middle heavy rare earth element are separated in 15 grades of extractions, wash 15 grades, carry out in 8 grades the fractionation extn groove of stripping; Stream is than being: organic phase: earth solution: washing lotion=2.3:1:0.2; NdPr: be separated in 52 grades of extractions with CeLa, wash 18 grades, 8 grades the fractionation apple of stripping is got in the groove and is carried out, and flows than being: organic phase: earth solution: washing lotion two 6.8:1:1.09; Ce separates with La and is separated in 27 grades of extractions, wash 24 grades, carries out in 8 grades the fractionation extn groove of stripping: flow than being organic phase: earth solution: washing lotion=4.5:1:0.7.
Resulting rare earth oxide product gas purity is respectively Pr
6O
11+ Nd20
3/ REO>=99.9%; CeO
2/ RE0>=99%; La
2O
3/ RE0>=99%; Sm-eu-gd enriched substance (Eu
20
3/ REO>=8%).The utilization ratio of whole process Hydrocerol A is greater than 85%, and the yield of REE is greater than 95%.
Claims (4)
1. the method for an acidic extractant extracting and separating rear earth element; With two (2 one ethylhexyl phosphoric acids) or 2 one ethylhexyl phosphoric acid list ethylhexyl fat is acidic organophosphorus extractant; With the organic phase of kerosene dilution as extracting and separating; Interpolation Hydrocerol A or Citrate trianion are mixed with the water of rare earth chloride one hydrochloric acid one Hydrocerol A mixing solutions as extracting and separating in re chloride, and this mixing solutions contains Hydrocerol A or Hydrocerol A salt concn ≦ 0.25mo1/L; It is characterized in that selecting for use with two (2 one ethylhexyl phosphoric acids) when being extraction agent, the pH value of rare monochloride one hydrochloric acid one Hydrocerol A mixing solutions of preparation is 0.5
~2, when being extraction agent with 2 one second hexyl mono phosphoric acid ester ethylhexyl fat, the pH value of the rare earth chloride one hydrochloric acid one Hydrocerol A mixing solutions of preparation is 1
~1.5; The organic phase of extracting and separating and water; Process extraction, washing and reextraction in extraction tank; REE is separated; It is with rare earth carbonate or rare-earth hydroxide deposition that the raffinate that contains Hydrocerol A returns when using, and circulation is used to prepare rare earth chloride one hydrochloric acid, one Hydrocerol A mixing solutions or preparation Hydrocerol A rare-earth products to the rare earth Citrate trianion that obtains as additive.
2. according to the method for the described a kind of acidic extractant extracting and separating rear earth element of claim 1, it is characterized in that described kerosene selects 260 for use
#Sulfonated kerosene or aviation kerosene, with the have machine phase of acidic organophosphorus extractant dilution for extracting and separating, concentration is 1.0
~1.5 mol/L, the rare earth oxide in the re chloride contain two kinds of REEs at least, this solution is with the rare earth oxide summation meter, and concentration is REO=10
~300 grams per liters.
3. according to the method for claim 1 or 2 described a kind of acidic extractant extracting and separating rear earth elements, it is characterized in that the rare earth oxide summation meter in the re chloride, selecting and selecting strength of solution earlier for use is REO=200
~300 grams per liters.
4. according to the method for the described a kind of acidic extractant extracting and separating rear earth element of claim 1, the Citrate trianion that it is characterized in that in re chloride being added is selected Trisodium Citrate or Hydrocerol A lanthanum for use.
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|---|---|---|---|---|
| CN103725880A (en) * | 2014-01-09 | 2014-04-16 | 中国科学院上海有机化学研究所 | Extraction system, extraction method and reextraction method |
| CN104651613A (en) * | 2013-11-19 | 2015-05-27 | 中国石油天然气股份有限公司 | Method for separating and recycling rare earth from waste rare earth-type Y molecular sieve catalyst |
| CN109735729A (en) * | 2019-03-22 | 2019-05-10 | 中南大学 | A kind of method that organic acid calcium salt assists acidic extractant extracting and separating rear earth element |
| CN112609073A (en) * | 2020-12-21 | 2021-04-06 | 江苏南方永磁科技有限公司 | Rare earth extraction composite material, preparation method and application |
| CN113697858A (en) * | 2021-07-23 | 2021-11-26 | 福建金鑫钨业股份有限公司 | Preparation method of tungstic acid |
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| CN104651613A (en) * | 2013-11-19 | 2015-05-27 | 中国石油天然气股份有限公司 | Method for separating and recycling rare earth from waste rare earth-type Y molecular sieve catalyst |
| CN104651613B (en) * | 2013-11-19 | 2017-06-06 | 中国石油天然气股份有限公司 | A kind of method that rare earth is separated and recovered from useless rare-earth type Y molecular sieve catalyst |
| CN103725880A (en) * | 2014-01-09 | 2014-04-16 | 中国科学院上海有机化学研究所 | Extraction system, extraction method and reextraction method |
| CN103725880B (en) * | 2014-01-09 | 2016-04-13 | 中国科学院上海有机化学研究所 | A kind of extraction system, extracting process and reextraction method |
| CN109735729A (en) * | 2019-03-22 | 2019-05-10 | 中南大学 | A kind of method that organic acid calcium salt assists acidic extractant extracting and separating rear earth element |
| CN112609073A (en) * | 2020-12-21 | 2021-04-06 | 江苏南方永磁科技有限公司 | Rare earth extraction composite material, preparation method and application |
| CN112609073B (en) * | 2020-12-21 | 2022-04-12 | 江苏南方永磁科技有限公司 | Rare earth extraction composite material, preparation method and application |
| CN113697858A (en) * | 2021-07-23 | 2021-11-26 | 福建金鑫钨业股份有限公司 | Preparation method of tungstic acid |
| CN113697858B (en) * | 2021-07-23 | 2024-04-19 | 福建鑫鹭钨业有限公司 | Preparation method of tungstic acid |
| RU2814787C1 (en) * | 2023-06-16 | 2024-03-04 | Акционерное общество "Леоли Кэпитал Групп" | Method of producing scandium concentrate |
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Application publication date: 20121219 |