CN109517985B - Method for extracting and separating light rare earth elements by using bifunctional ionic liquid - Google Patents
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Abstract
The invention belongs to the technical field of rare earth separation and ionic liquid extraction, and particularly relates to a method for extracting and separating light rare earth elements by using a bifunctional ionic liquid. The method comprises the steps of taking an aqueous solution containing light rare earth elements as a raw material solution, combining 2-ethylhexyl phosphonic acid mono-2-ethylhexyl with N-octyl pyridinium chloride, adding sodium hydroxide for regulation, retaining the combination of anions of the 2-ethylhexyl phosphonic acid mono-2-ethylhexyl with cations of the N-octyl pyridinium chloride, synthesizing bifunctional ionic liquid, performing mixed extraction on the bifunctional ionic liquid and the acidic raw material solution, performing centrifugation to obtain an organic phase loaded with rare earth and raffinate, performing back extraction on the rare earth by using a back extraction agent, and performing centrifugation to obtain a pure rare earth solution and a recyclable ionic liquid. The invention has high extraction efficiency, short balance time and simple operation, and does not generate emulsification phenomenon.
Description
Technical Field
The invention belongs to the technical field of rare earth separation and ionic liquid extraction, and particularly relates to a method for extracting and separating light rare earth elements by using a bifunctional ionic liquid.
Background
Rare earth is an important strategic non-renewable resource, can be divided into light rare earth and heavy rare earth according to chemical properties and separation process requirements, is widely applied to the fields of new materials and new technologies, and the reserves of rare earth in China are the first place in the world, wherein the contents of light rare earth elements in southern ion-adsorption rare earth ores and northern bastnaesite are very high, the application range of the light rare earth elements is wide, and the rare earth elements play a role in improving the weight of the application of the light rare earth elements, so that the effective separation and purification of the light rare earth elements has important significance for expanding the application fields of the light rare earth elements.
The physical and chemical properties of rare earth elements are similar, the separation and purification are difficult, the solvent extraction method is a method commonly used for industrial rare earth separation, and the extracting agent 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester (P) is used 507) And di (2-ethylhexyl) phosphonate (P) 204) Although the acidic phosphine extractant has a good extraction effect on light rare earth elements, the acidic phosphine extractant also has the problems of high back extraction acidity, incomplete back extraction, ammonia nitrogen wastewater, high-salinity wastewater and the like in the process of separating rare earth. Therefore, the search for efficient and environmentally friendly extraction and separation processes is imminent.
The ionic liquid has low vapor pressure and good thermal stability, can be applied to the field of extraction and separation, has already been reported by research on the application of rare earth separation by using the ionic liquid as an extracting agent, and Chinese patent (publication No. CN102876893A) discloses A method for extracting rare earth elements in a sulfuric acid system by using a quaternary ammonium salt ionic liquid extractant; chinese patent CN103320629A discloses a method for efficiently extracting rare earth cerium in a sulfuric acid system by using a bifunctional ionic liquid, and chinese patent (publication No. CN102618736A) discloses a method for extracting rare earth elements in a nitrate system by using a bifunctional ionic liquid. However, the use of N-octyl pyridinium chloride ([ OPy) ][Cl]) With 2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester (P) 507) Combined with the research report of extracting rare earth elements by the bifunctional ionic liquid.
Disclosure of Invention
Aiming at the problems that the back extraction is difficult and secondary pollution is easily caused by using an acidic phosphine extractant in the current rare earth extraction process, the invention aims to provide a method for extracting and separating light rare earth elements by utilizing bifunctional ionic liquid, and the traditional extractant P is prepared by utilizing the characteristics of non-volatility, good chemical property stability and the like of the ionic liquid 507The method is combined with the ionic liquid, and the bifunctional ionic liquid is used for extracting the rare earth, so that the extraction efficiency is high, and the problem of ammonia nitrogen wastewater pollution is solved.
The technical scheme of the invention is as follows:
A method for extracting and separating light rare earth elements by using bifunctional ionic liquid comprises the following steps:
(1) preparing an aqueous solution containing light rare earth elements as a raw material solution, wherein the concentration of the light rare earth in the raw material solution is 0.01-0.04 mol/L, and the pH of the solution is 1-5.5;
(2) Preparing bifunctional ionic liquid as extractant, N-octyl pyridine chloride salt ([ OPy ] ][Cl]) With 2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester (P) 507) In a molar ratio of 1:1 to 1:3, P 507the concentration of the N-octyl pyridine chloride salt is 0.03-0.1 mol/L, and the concentration of the N-octyl pyridine chloride salt is 0.03-0.1 mol/L;
(3) Mixing and extracting the raw material liquid and the bifunctional ionic liquid in an oscillator, wherein the mixing ratio is 1:1, the rotating speed in the extraction process is 50-150 r/min, the extraction time is 15-30 min, the extraction temperature is 5-35 ℃, and the mixed solution after extraction is subjected to centrifugal separation to obtain a rare earth-loaded organic phase and raffinate;
(4) And (3) back-extracting the organic phase loaded with the rare earth by using a back-extracting agent, wherein the centrifugal speed of back-extraction centrifugal separation is 2000-3500 r/min, the centrifugal time is 2-8 min, and pure rare earth solution and ionic liquid are obtained through centrifugation.
The method for extracting and separating the light rare earth elements by using the bifunctional ionic liquid is characterized in that the light rare earth elements are lanthanum, cerium, praseodymium or neodymium.
The method for extracting and separating the light rare earth elements by using the bifunctional ionic liquid is characterized in that the aqueous solution containing the light rare earth elements is a rare earth chloride solution or a rare earth nitrate solution, and the most preferable is a rare earth chloride solution.
The method for extracting and separating the light rare earth elements by using the bifunctional ionic liquid, wherein in the bifunctional ionic liquid, the cation is N-octyl pyridine [ Opy ] ]+The anion is [ P ] 507]-The structural formula of the anions and cations of the bifunctional ionic liquid is shown as formula 1:
The method for extracting and separating the light rare earth elements by using the bifunctional ionic liquid comprises the step (3), wherein the centrifugal rotating speed is 2000-3500 r/min, and the centrifugal time is 2-8 min.
The method for extracting and separating the light rare earth elements by using the bifunctional ionic liquid comprises that in the bifunctional ionic liquid, N-octyl pyridinium chloride ([ OPy) ][Cl]) With 2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester (P) 507) N-pentanol is selected as the diluent.
The method for extracting and separating the light rare earth elements by using the bifunctional ionic liquid, P 507The saponification rate of (2) was 100%.
according to the method for extracting and separating the light rare earth elements by using the bifunctional ionic liquid, the back-extraction agent adopts 0.05-0.3 mol/L ammonium chloride aqueous solution.
The design idea of the invention is as follows:
The ionic liquid has low vapor pressure and good thermal stability, is widely used as a green solvent in hydrometallurgy, and is often used for dissolving substances by the ionic liquid in the past research The purpose of separation and purification can be achieved. The invention explores the role of the ionic liquid as an extracting agent in the separation process of light rare earth from a new scientific perspective, realizes the inverse attack of the ionic liquid from the 'mating angle' identity of a 'green solvent' to the 'main angle' identity of the extracting agent, adopts the organic coordination of the pyridine ionic liquid and the traditional acidic phosphine extracting agent to form the dual-functional ionic liquid, and completes the P-type separation of the light rare earth by 507The function of the traditional acidic extractant is changed into the ionic liquid, so that the high extraction performance is maintained, and the environment-friendly separation of the rare earth elements is realized.
The invention has the advantages and beneficial effects that:
The method comprises the steps of taking an aqueous solution containing light rare earth elements as a raw material solution, combining 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester with N-octyl pyridinium chloride, adding sodium hydroxide for regulation, keeping the combination of anions of the 2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester and cations of the N-octyl pyridinium chloride, synthesizing bifunctional ionic liquid, performing mixed extraction on the bifunctional ionic liquid and the acidic raw material solution, centrifuging to obtain an organic phase loaded with rare earth and raffinate, performing back extraction on the rare earth by using a back extraction agent, and centrifuging to obtain a pure rare earth solution and a recyclable ionic liquid. The invention not only keeps the advantages of the ionic liquid, but also has the advantage of high extraction performance of the traditional extractant. The invention has the advantages of high extraction efficiency, good separation effect, short balance time, simple operation, no emulsification phenomenon, recyclable ionic liquid, and wide application prospect as a green extractant of the bifunctional ionic liquid.
Detailed Description
In the specific implementation process, after the extraction and back extraction separation process is finished, the rare earth concentration in the raffinate and the back extraction liquid can be determined by an EDTA titration method (ethylene diamine tetraacetic acid titration method) according to the GB/T14635-2008 rare earth metal and chemical analysis method of the rare earth metal compound, and the rare earth concentration in the ionic liquid is obtained by a differential subtraction method.
The rare earth extraction rate E is calculated according to formula 2:
Formula 2
The rare earth back-extraction rate S is calculated according to formula 3:
And (3) formula.
In the formula: c t、Cerespectively the rare earth concentration, mol/L, in the aqueous phase before and after extraction ]ain order to balance the concentration of rare earth in the aqueous phase, mol/L ]ois the initial concentration of the organic phase, mol/L.
For a further understanding of the present invention, embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples do not show the specific conditions, and the procedures are carried out according to the conventional conditions or the conditions recommended by the manufacturer, and the equipment and reagents used are not shown by the manufacturer, and are all conventional products which can be purchased commercially.
Example 1
In this embodiment, the method for extracting and separating light rare earth elements by using the bifunctional ionic liquid is performed according to the following steps:
(1) lanthanum-containing rare earth chloride solution is used as raw material liquid, the concentration of lanthanum in the raw material liquid is 0.04 mol/L, and the pH value is 5.5.
(2) Preparing bifunctional ionic liquid as an extracting agent, selecting N-amyl alcohol as a diluting agent, N-octyl pyridine chloride salt and P 507In a molar ratio of 1:1, P 507has a concentration of 0.1 mol/L, a concentration of N-octylpyridinium chloride of 0.1 mol/L, P 507The saponification rate of (2) was 100%.
(3) Mixing and extracting the raw material liquid and the bifunctional ionic liquid in an oscillator, wherein the mixing ratio is O/A (1: 1), the rotating speed in the extraction process is 50r/min, the extraction time is 30min, the extraction temperature is 25 ℃, the mixed solution is subjected to centrifugal separation after extraction is finished to obtain a rare earth-loaded organic phase and raffinate, the centrifugal rotating speed is 2000r/min, the centrifugal time is 5min, and the concentration of lanthanum in the raffinate is measured to obtain the extraction rate of 27.19%.
(4) and (2) carrying out back extraction on the organic phase loaded with the rare earth by adopting a back extraction agent, wherein the back extraction agent is 0.3 mol/L ammonium chloride aqueous solution, the ratio of O/A is 1:1, the rotating speed in the back extraction process is 50r/min, the back extraction time is 30min, the rare earth is recovered from the mixed solution after the back extraction is finished through centrifugal separation, the centrifugal rotating speed of the centrifugal separation is 2000r/min, the centrifugal time is 5 mm, the separated ionic liquid is recycled, and the back extraction rate is 17.12% by calculation.
Example 2
In this embodiment, the method for extracting and separating light rare earth elements by using the bifunctional ionic liquid is performed according to the following steps:
(1) A cerium-containing rare earth chloride solution is used as a raw material solution, the concentration of cerium in the raw material solution is 0.02 mol/L, and the pH value is 1.
(2) Preparing bifunctional ionic liquid as an extracting agent, selecting N-amyl alcohol as a diluting agent, N-octyl pyridine chloride salt and P 507In a molar ratio of 1:3, P 507has a concentration of 0.08 mol/L, a concentration of N-octyl pyridinium chloride of 0.08 mol/L, P 507The saponification rate of (2) was 100%.
(3) Mixing and extracting the raw material liquid and the bifunctional ionic liquid in an oscillator, wherein the mixing ratio is O/A (1: 1), the rotating speed in the extraction process is 75r/min, the extraction time is 25min, the extraction temperature is 35 ℃, the mixed solution is subjected to centrifugal separation after extraction is finished to obtain a rare earth-loaded organic phase and raffinate, the centrifugal rotating speed is 3000r/min, the centrifugal time is 8min, and the concentration of lanthanum in the raffinate is measured to obtain the extraction rate of 15%.
(4) and (2) carrying out back extraction on the organic phase loaded with the rare earth by adopting a back extraction agent, wherein the back extraction agent is 0.1 mol/L ammonium chloride aqueous solution, the ratio of O/A is 1:1, the rotating speed in the back extraction process is 75r/min, the back extraction time is 25min, the rare earth is recovered from the mixed solution after the back extraction is finished through centrifugal separation, the centrifugal rotating speed of the centrifugal separation is 3000r/min, the centrifugal time is 8 mm, the separated ionic liquid is recycled, and the back extraction rate is 57.15% through calculation.
Example 3
In this embodiment, the method for extracting and separating light rare earth elements by using the bifunctional ionic liquid is performed according to the following steps:
(1) the praseodymium-containing rare earth chloride solution is used as a raw material solution, the concentration of the praseodymium in the raw material solution is 0.01 mol/L, and the pH value is 2.5.
(2) Preparing bifunctional ionic liquid as an extracting agent, selecting N-amyl alcohol as a diluting agent, N-octyl pyridine chloride salt and P 507In a molar ratio of 1:1, P 507has a concentration of 0.05 mol/L, a concentration of N-octyl pyridinium chloride of 0.05 mol/L, P 507The saponification rate of (2) was 100%.
(3) Mixing and extracting the raw material liquid and the bifunctional ionic liquid in an oscillator, wherein the mixing ratio is O/A (1: 1), the rotating speed in the extraction process is 100r/min, the extraction time is 20min, the extraction temperature is 15 ℃, the mixed solution is subjected to centrifugal separation after extraction is finished to obtain a rare earth-loaded organic phase and raffinate, the centrifugal rotating speed is 2500r/min, the centrifugal time is 3min, and the concentration of lanthanum in the raffinate is measured to obtain the extraction rate of 89.87%.
(4) and (2) carrying out back extraction on the organic phase loaded with the rare earth by adopting a back extraction agent, wherein the back extraction agent is 0.08 mol/L ammonium chloride aqueous solution, the ratio of O/A is 1:4, the rotating speed in the back extraction process is 100r/min, the back extraction time is 20min, the rare earth is recovered from the mixed solution after the back extraction is finished through centrifugal separation, the centrifugal rotating speed of the centrifugal separation is 2500r/min, the centrifugal time is 3 mm, the separated ionic liquid is recycled, and the back extraction rate is 11% by calculation.
Example 4
In this embodiment, the method for extracting and separating light rare earth elements by using the bifunctional ionic liquid is performed according to the following steps:
(1) the neodymium-containing rare earth nitrate solution is used as a raw material solution, the concentration of neodymium in the raw material solution is 0.01 mol/L, and the pH value is 3.
(2) Preparing bifunctional ionic liquid as an extracting agent, selecting N-amyl alcohol as a diluting agent, N-octyl pyridine chloride salt and P 507In a molar ratio of 1:1, P 507the concentration of (A) is 0.03 mol/L, the concentration of N-octyl pyridine chloride salt is 0.03 mol/L, P 507The saponification rate of (2) was 100%.
(3) Mixing and extracting the raw material liquid and the bifunctional ionic liquid in an oscillator, wherein the mixing ratio is O/A (1: 1), the rotating speed in the extraction process is 150r/min, the extraction time is 15min, the extraction temperature is 5 ℃, the mixed solution is subjected to centrifugal separation after extraction is finished to obtain a rare earth-loaded organic phase and raffinate, the centrifugal rotating speed is 3500r/min, the centrifugal time is 2min, and the concentration of lanthanum in the raffinate is measured to obtain the extraction rate of 60.02 percent.
(4) and (2) back-extracting the organic phase loaded with the rare earth by using a back-extracting agent, wherein the back-extracting agent is 0.05 mol/L ammonium chloride aqueous solution, the ratio of O/A is 1:2, the rotating speed in the back-extracting process is 150r/min, the back-extracting time is 15min, the rare earth is recovered from the mixed solution after the back-extracting is finished through centrifugal separation, the centrifugal rotating speed of the centrifugal separation is 3500r/min, the centrifugal time is 2 mm, the separated ionic liquid is recycled, and the back-extracting rate is 15% by calculation.
The results of the examples show that the method for extracting rare earth by using the bifunctional ionic liquid has the following advantages: the extraction efficiency is high, the balance time is short, the two phases are clearly layered after extraction, no emulsification phenomenon is generated, and no secondary pollution is generated in the extraction process.
Claims (7)
1. A method for extracting and separating light rare earth elements by using bifunctional ionic liquid is characterized by comprising the following steps:
(1) preparing an aqueous solution containing light rare earth elements as a raw material solution, wherein the concentration of the light rare earth in the raw material solution is 0.01-0.04 mol/L, and the pH of the solution is 1-5.5;
(2) Preparing bifunctional ionic liquid as extractant, N-octyl pyridine chloride salt ([ OPy ] ][Cl]) With 2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester (P) 507) In a molar ratio of 1:1 to 1:3, P 507the concentration of the N-octyl pyridine chloride salt is 0.03-0.1 mol/L, and the concentration of the N-octyl pyridine chloride salt is 0.03-0.1 mol/L;
(3) Mixing and extracting the raw material liquid and the bifunctional ionic liquid in an oscillator, wherein the mixing ratio is 1:1, the rotating speed in the extraction process is 50-150 r/min, the extraction time is 15-30 min, the extraction temperature is 5-35 ℃, and the mixed solution after extraction is subjected to centrifugal separation to obtain a rare earth-loaded organic phase and raffinate;
(4) Back-extracting the organic phase loaded with the rare earth by using a back-extracting agent, wherein the centrifugal speed of back-extraction centrifugal separation is 2000-3500 r/min, the centrifugal time is 2-8 min, and pure rare earth solution and ionic liquid are obtained through centrifugation;
In the bifunctional ionic liquid, the cation is N-octyl pyridine [ Opy ] ]+The anion is [ P ] 507]-The structural formula of the anions and cations of the bifunctional ionic liquid is shown as formula 1:
2. The method for extractive separation of light rare earth elements using a bifunctional ionic liquid as claimed in claim 1, wherein the light rare earth element is lanthanum, cerium, praseodymium or neodymium.
3. The method for the extractive separation of light rare earth elements using bifunctional ionic liquids as claimed in claim 1, wherein the aqueous solution containing light rare earth elements is a rare earth chloride solution or a rare earth nitrate solution, most preferably a rare earth chloride solution.
4. The method for extracting and separating light rare earth elements by using the bifunctional ionic liquid as claimed in claim 1, wherein in the step (3), the centrifugal rotation speed is 2000-3500 r/min, and the centrifugal time is 2-8 min.
5. The process for the extractive separation of light rare earth elements using a bifunctional ionic liquid as claimed in claim 1, wherein in the bifunctional ionic liquid, N-octylpyridinium chloride ([ OPy) ][Cl]) With 2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester (P) 507) N-pentanol is selected as the diluent.
6. The process for the extractive separation of light rare earths using bifunctional ionic liquids according to claim 1, characterized in that P 507The saponification rate of (2) was 100%.
7. the method for extracting and separating light rare earth elements by using the bifunctional ionic liquid as claimed in claim 1, wherein the back-extracting agent adopts an ammonium chloride aqueous solution with the concentration of 0.05-0.3 mol/L.
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| CN112695214B (en) * | 2020-12-21 | 2022-04-12 | 江苏南方永磁科技有限公司 | Lanthanum extraction material and preparation method thereof |
| CN112588274B (en) * | 2020-12-21 | 2023-03-28 | 江苏南方永磁科技有限公司 | Extraction material for separating cerium and preparation method thereof |
| CN113106271B (en) * | 2021-04-06 | 2022-01-14 | 中国科学院过程工程研究所 | Method for purifying rare earth element gadolinium with high purity by using carboxylic acid functionalized ionic liquid |
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