CN1394972A - Process for separating high-purity yttrium by using oxyl substituted acetic acid as extracting agent - Google Patents
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Abstract
The present invention relates to a process for preparing high-purity yttrium from yttrium-containing mixed rare earth by using oxyl substituted acetic acid or oxyl substituted acetic acid+monobase phosphoric (phosphonic) acid or its monothioderivative as extracting agent, in which Y is 30-70%, pH is 2-4; 0.5-3 mol/L hydrochloric acid or nitric acid can be used as washing acid; it uses ammonia water, sodium hydroxide, ammonium hydrogen carbonate of sodium arbonate as saponification agent, and the flow ratio of organic phase, slurry liquid and washing acid is 5-15:1-1-6; number of steps of extraction stage is 20-40 steps; number of steps of washing stage is 5-20 steps; fractionation extraction mixing time is 5-10 min; clear time is 10-25 min.; experimental temp. is 10-35 deg.C, purity of yttrium can be up to 99.0%-99.996% and its yield is greater than 95%.
Description
Technical Field
The invention belongs to a separation process of rare earth metal in hydrometallurgy, in particular to a process for separating high-purity yttrium from yttrium-containing rare earth by using oxyl substituted acetic acid as an extracting agent.
Background
Yttrium has important application in high-tech fields such as metallurgy, ceramics, laser, electronics and the like, and particularly, the demand of high-purity yttrium oxide in fluorescent luminescent materials including color television fluorescent powder, fluorescent lamp powder, laser materials and the like is increasing day by day. Because of their close chemical properties, yttrium and lanthanides often coexist with minerals. Currently, the hydrometallurgical composition of yttriumNaphthenic acid systems are widely used in separation processes. Chinese patent CN85102220B discloses a technique of 'solvent extraction separation of high purity yttrium' in Thanatv capacity, etc., which uses 0.8-0.9M naphthenic acid and ammonium naphthenate as extractant to separate Y from Y2O3The high-purity Y with the yield of more than 98 percent and the purity of more than 99.99 percent is obtained from the enrichment material with 63 percent of content and mainly containing heavy rare earth by a one-step method2O3. However, production practice shows that naphthenic acid is a byproduct in petroleum, has complex composition and high water solubility, the components of an extractant are changed after long-term use, and the phenomenon of emulsification is easily caused because the pKa value is high and rare earth needs to be extracted at a high pH value. Also, since lanthanum and yttrium have a separation coefficient of only 1 to 1.4, separation between them is difficult.
An extractant for separating rare-earth metals, named "extractant for separating rare-earth metals" in Chinese patent application No. 93112500.6, is disclosed by Ligustrum victorii et al2By substitution of acetic acid with hydrocarbyloxy groups of COOHA carboxylic acid type extractant for separating rare earth metals. The extractant has better chemical stability and simpler composition, and the pKa values of the extractant are smaller than that of naphthenic acid, so that rare earth elements can be extracted at lower pH, the extractant is favorable for overcoming the emulsification generated when the naphthenic acid extracts the rare earth, and the extractant is a carboxylic acid type extractant which is hopeful to replace the naphthenic acid to be separated into yttrium. The invention shows the rare earth extraction performance of sec-octyl phenoxy substituted acetic acid (represented by HA), and compared with the extraction performance of naphthenic acid. The results show that HA extracts Y less than all lanthanides (denoted Ln). The Ln-Y separation coefficient reaches 3.0-4.9, which is obviously superior to naphthenic acid, and the lowest Lu-Y reaches 1.4. Therefore, Y can be effectively separated from all Ln. It should be noted that in HA systems, the separation coefficient of Y from heavy Ln such as Er, Tm, Yb, Lu is small, ranging from 1.4 to 1.7. Therefore, the separation of high purity yttrium from yttrium-containing heavy rare earth mixtures using the HA system is difficult, and the patent does not study the process for separating yttrium using the HA system.
Chinese patent application No. 99118261.8 discloses a process for preparing high-purity yttrium oxide by using yttrium-containing misch metal or yttrium-enriched material as feed liquid and HAB-ROH-alkane or arene to form an organic phase. HAB is composed of HA + HB, HA is sec-octylPhenoxy-substituted acetic acids, HB being a phosphonium (phospho) acid salt such as P204, P507, Cyanex272, 302, etc., HCl or HNO3Washing solution and back extraction solution. The high-purity yttrium oxide product with the purity of 99.99 percent and the yield of more than 95 percent can be obtained by multi-stage fractional extraction. The patent does not study the process of preparing high-purity yttrium by using other alkoxy substituted acetic acid as an extracting agent.
Disclosure of Invention
The invention aims to provide a process for separating high-purity yttrium by using oxyl substituted acetic acid as an extracting agent, wherein the process uses the oxyl substituted acetic acid or the oxyl substituted acetic acid plus one-base phosphorus (phosphonic) acid or a monosulfo derivative thereof as the extracting agent to prepare the high-purity yttrium from yttrium-containing mixed rare earth.
The invention provides a process for preparing high-purity yttrium from yttrium-containing rare earth by using alkoxy substituted acetic acid based on the following principle, and the reaction mechanism of HA extraction Ln (III) and Y (III) is as follows:
in which M represents Ln and Y, H2A2Represents a dimer of alkoxy-substituted acetic acids; (o) represents an organic phase and (a) an aqueous phase. HB is monobasic phosphoric (phosphonic) acid or its monothio derivatives, such as bis (2-ethylhexyl) phosphate (P204), 2-ethylhexyl phosphonate mono 2-ethylhexyl (P507), bis (2, 4, 4-trimethylpentyl) phosphonic acid (Cyanex272), bis (2-ethylhexyl) monothio phosphate, bis (2, 4, 4-trimethylpentyl) monothio phosphonic acid (Cyanex302), and the like. When RE (III) is extracted from a mineral acid medium, the extraction capacity of the compound is increased according to the increase of the atomic number of Ln, and Y is positioned between Ho and Er. The invention adopts HA + HB to form a HAB double-solvent extraction system to separate high-purity yttrium, in the system, the extraction capacity of Ln (III) is higher than that of Y (III), and the average separation coefficient of Y and Ln is more than 2. The HAB system keeps the advantage that the separation coefficient of Y and light lanthanum in the HA system is higher than that of naphthenic acid, and overcomes the defect that the separation coefficient of Y and heavy lanthanum (Er-Lu) in the HA system is small.
The method adopts the saponified HAB to improve the capacity and the separation coefficient of the HAB for extracting RE (III). Due to liquid-liquid extractionIn the formulae RE (III) and H in HAB+The exchange is carried out, so that the acidity in the raffinate water phase is continuously improved, and the further extraction separation of RE (III) is influenced. In order to maintain the extractive separation of Y from Ln at a certain separation factor, HAB must be pre-saponified to maintain the desired pH for the equilibrium aqueous phase during the separation process.
The extraction agent HA oxyl substituted acetic acid, such as sec-heptyl phenoxyl substituted acetic acid or sec-nonyl phenoxyl substituted acetic acid and the like, HAs the molecular formula:
in the formula, R is hexyl, heptyl, nonyl or decyl, and taking secondary nonylphenoxy substituted acetic acid as an example, when rare earth is extracted from a mineral acid medium, the average separation coefficient of yttrium from light lanthanides (La, Ce, Pr and Nd) is 5.87, the average separation coefficient of yttrium from medium lanthanides (Sm, Eu, Gd, Tb and Dy) is 5.54, the average separation coefficient of heavy lanthanides (Ho, Er, Tm, Yb and Lu) is 2.02, and the separation coefficient of scandium reaches 407.38, so that the purposes of separating yttrium from other rare earth and preparing high-purity yttrium can be achieved through multi-stage extraction.
The invention adopts mixed alcohol ROH as an additive of the HAB system, the ROH can improve the physical phenomenon of the HAB system and eliminate emulsification, and alkane or arene is used as a diluent to form an HAB-ROH-alkane or arene extractant system. Using chlorinated or nitrated rare earth as feed liquid and hydrochloric acid or nitric acid as washing acid. The purity of the obtained yttrium (III) can reach 99.0-99.996%. The yield is more than 95 percent.
The invention adopts a fractional extraction mode, the HA concentration in the extracting agent is 0.2-1.0mol/L, the amount of HB is dependent on the content of Er-Lu in the feed liquid and accounts for 0-30% (mol percentage content) of HAB; ROH is adopted as an additive of HA, R is straight-chain or branched alkane with carbon number of C6-C10, and the content of the alkane is 5% -30%; ammonia water, sodium hydroxide, ammonium bicarbonate or sodium carbonate and the like are used as saponifying agents, and the saponification rate of HAB is 60-90%; using yttrium-containing mixed rare earth chloride or nitrated rare earth as feed liquid, wherein Y accounts for 30-70% (weight percentage), and the pH value is 2-4; the washing liquid is 0.5-3mol/LHCl or HNO3(ii) a The flow ratio of the organic phase, the feed liquid and the washing acid is 5-15: 1-6; the number of stages of the extraction section is 20-40 stages; number of washing stagesGrade 5-20; the fractional extraction mixing time is 5-10 minutes; the clarification time is 10-25 minutes; the experimental temperature was 10-35 ℃. Under the process conditions, a high-purity yttrium product can be obtained, the purity of yttrium can reach 99.0-99.996% (wt%), and the yield is more than 95%. The obtained product is analyzed and identified by plasma atomic emission spectrometry and mass spectrometry.
The invention has the advantages of high efficiency, clean new process for preparing high-purity yttrium, and suitability for separating various grades of yttrium-containing mixed rare earth or concentrates. The yttrium has high yield and good quality, and simultaneously, the used extracting agent has good chemical stability and easy preparation, and the pKa values of the yttrium and the extracting agent are smaller than that of naphthenic acid, so that rare earth elements can be extracted at lower pH, and the method is favorable for overcoming the emulsification generated when the naphthenic acid is used for extracting rare earth.
Detailed Description
In order to illustrate the present invention more clearly, the following examples are given without any limitation to the scope of the invention.
Example 1
0.75M secondary heptyl phenoxy substituted acetic acid-15% methyl heptanol-kerosene as an extracting agent, 90% ammoniation and 1.0M rare earth chloride feed liquid, wherein Y51%, Tb-Lu 28.6%, La-Gd 20.4% and washing acid 1.8M HCl have the flow ratio of organic phase to feed liquid to washing acid of 12.0: 1: 5.5. After 40-stage fractional extraction, 23 stages of extraction and 17 stages of washing, test results: the purity of Y in the organic phase was 99.2% with a yield of 99%.
Example 2
0.75M sec-nonyl phenoxy substituted acetic acid-15% methyl heptanol-kerosene as extractant, 90% ammoniation and 1.0M rare earth nitrate feed liquid, wherein Y51%, Tb-Lu 28.6%, La-Gd 20.4%, and washing acid 1.8M HNO3The flow ratio of the organic phase to the feed liquid to the washing acid is 12.3: 1: 5.7. After 42-stage fractional extraction, 28-stage extraction and 14-stage washing, the purity of Y in the organic phase is 99.9% and the yield is 97%. The contents of various rare earth elements are as follows:
la Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu103.9140.428.9103.950.017330.81.9161.655.8159.715.4111.69.6
Example 3
0.6M of extractant, 0.10 to 20 percent of secondary decyl phenoxy substituted acetic acid, 0.10 to 0.10M P204 percent of mixed alcohol (C7 to C9) and kerosene, ammoniation 90 percent and rare earth chloride feed liquid 1.0M, wherein Y51 percent, Tb-Lu28.6 percent, La-Gd 20.4 percent and washing acid 1.8M HCl have the flow ratio of organic phase, feed liquid and washing acid being 8.1: 1: 3. 32-stage fractional extraction is carried out, wherein 22 stages of extraction and 10 stages of washing are carried out, and the test result is as follows: in the organic phase
The purity of Y was 99.98% and the yield was 97.1%.
Example 4
0.58M of secondary nonyl phenoxy substituted acetic acid as extractant-0.06M P507-20%, 90% of methyl heptanol-kerosene ammoniation, 1.0M of rare earth nitrate feed liquid, wherein Y is 61.5%, Tb-Lu is 20.8%, La-Gd17.7%, and washing acid is 1.2M HNO3The flow ratio of the organic phase to the feed liquid to the washing acid is 7.5: 1: 2.6. The extraction is carried out by 40-stage fractional extraction, wherein 30 stages of extraction and 10 stages of washing are carried out. And (3) test results: the purity of Y in the organic phase is 99.993%, the yield is 97.5%, wherein the contents of various rare earth elements are as follows:
la Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu5.47.31.55.42.60.91.60.110.45.910.33.810.85.5
Example 5
0.85M secondary heptyl phenoxy substituted acetic acid as an extractant, 0.12M Cyanex 272-25% mixed alcohol (C8-C10) -kerosene, 85% ammoniation and 1.0M rare earth chloride feed liquid, wherein Y51%, Tb-Lu 28.6%, La-Gd 20.4% and washing acid 1.5M HCl are adopted, and the flow ratio of an organic phase to the feed liquid to the washing acid is 6.5: 1: 2.4. 32 stages of extraction and 13 stages of washing are carried out by 45-stage fractional extraction, and the test result is as follows: the purity of Y in the organic phase was 99.995% with a yield of 96.1%, wherein the contents of the various rare earth elements are as follows:
la Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu5.16.91.45.12.50.91.50.18.02.87.90.85.50.5
Example 6
0.85M sec-nonyl phenoxy substituted acetic acid as extractant, 0.12M P507-25% methyl heptanol-kerosene, 85% ammoniation and 1.0M rare earth chloride feed liquid, wherein Y is 61.5%, Tb-Lu is 20.8%, La-Gd17.7% and washing acid is 1.2M HCl, and the flow ratio is 5.6: 1: 2.6. The extraction is carried out by 50-stage fractional extraction, wherein 38 stages of extraction and 12 stages of washing are carried out. And (3) test results: the purity of Y in the organic phase was 99.996%, yield 95%.
Claims (8)
1. A process for separating high-purity yttrium by using oxyl substituted acetic acid as extractant features that the oxyl is sec-octylphenoxy whose molecular formula is:the compound is characterized in that R in the formula is hexyl, heptyl, nonyl or decyl, and the concentration of the compound is 0.2-1.0 mol/L; chloridizing or nitrifying rare earth feed liquid, wherein the pH value is 2-4, and Y accounts for 30-70% (weight percentage); 0.5-3mol/L hydrochloric acid or nitric acid is used as washing acid; the flow ratio of the organic phase, the feed liquid and the washing acid is 5-15: 1-6; the number of stages of the extraction section is 20-40 stages; the number of washing stages is 5-20; the fractional extraction mixing timeis 5-10 minutes; the clarification time is 10-25 minutes; the extraction temperature is 10-35 ℃.
2. The separation process of claim 1, wherein the extractant is a hydrocarbyloxy-substituted acetic acid + monohydroxy phosphonic (phosphine) acid, wherein the monohydroxy phosphonic (phosphine) acid comprises from 0 to 30 mole percent of the extractant.
3. The separation process of claim 1, wherein the monobasic phospho (phosphine) acid is a monosulfur derivative thereof.
4. The separation process according to claim 1 or 2, wherein the additive is mixed alcohol, the content of which is 5-30%, and R in the mixed alcohol ROH is C6-C10 straight chain or branched chain alkyl.
5. The separation process according to claim 1 or 2, wherein ammonia, sodium hydroxide, ammonium bicarbonate or sodium carbonate is used as a saponifying agent, and the saponification rate is 60-90%.
6. The separation process of claim 1 or 2, wherein the hydrocarbyloxy-substituted acetic acid is a secondary hexylphenoxy-substituted acetic acid, a secondary heptylphenoxy-substituted acetic acid, a secondary nonylphenoxy-substituted acetic acid, or a secondary decylphenoxy-substituted acetic acid.
7. The separation process of claim 2, wherein the monobasic phosphonium (phosphine) acid is bis (2-ethylhexyl) phosphoric acid (P204), 2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester (P507), or bis (2, 4, 4-trimethylpentyl) phosphonic acid (Cyanex 272).
8. The separation process of claim 3, wherein the monosulfur derivative of monobasic phosphoric (phosphonic) acid is bis (2-ethylhexyl) monosulfur phosphoric acid or bis (2, 4, 4-trimethylpentyl) monosulfur phosphonic acid (Cyanex 302).
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| Application Number | Priority Date | Filing Date | Title |
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| CN02123912A CN1394972A (en) | 2002-07-09 | 2002-07-09 | Process for separating high-purity yttrium by using oxyl substituted acetic acid as extracting agent |
| JP2003272363A JP4046660B2 (en) | 2002-07-09 | 2003-07-09 | Separation of high-purity yttrium by extraction solvent containing phenoxy-substituted acetic acid |
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| CN02123912A CN1394972A (en) | 2002-07-09 | 2002-07-09 | Process for separating high-purity yttrium by using oxyl substituted acetic acid as extracting agent |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100352954C (en) * | 2005-04-05 | 2007-12-05 | 中国科学院长春应用化学研究所 | Technology for separating rare earth element by extraction system added with modifier |
| CN100435899C (en) * | 2006-01-24 | 2008-11-26 | 北京有色金属研究总院 | Saponification of organic extractant |
| CN100451140C (en) * | 2004-07-01 | 2009-01-14 | 包头市京瑞新材料有限公司 | Self protection process for preparing fluorescent grade europium oxide extractor by reducing extracting method |
| CN106916948A (en) * | 2017-03-07 | 2017-07-04 | 四川省冕宁县方兴稀土有限公司 | A kind of saponification agent and its application process of rare earth organic extractant |
| CN108456792A (en) * | 2017-02-17 | 2018-08-28 | 厦门稀土材料研究所 | A kind of rare earth extraction separation extractant and preparation method thereof and extraction separating method |
| CN110002487A (en) * | 2019-04-17 | 2019-07-12 | 中国科学院长春应用化学研究所 | A kind of method of high yttrium type Rare Earth Mine grouping separation yttrium oxide |
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| EP2730668A4 (en) | 2011-07-06 | 2015-06-24 | Jx Nippon Mining & Metals Corp | High-purity yttrium, process for producing high-purity yttrium, high-purity yttrium sputtering target, metal gate film deposited with high-purity yttrium sputtering target, and semiconductor element and device equipped with said metal gate film |
| CN102676853B (en) * | 2012-05-28 | 2013-11-20 | 五矿（北京）稀土研究院有限公司 | Rare earth separation method with material linkage cyclic utilization function |
| CN115818693B (en) * | 2022-11-21 | 2024-02-13 | 江苏南方永磁科技有限公司 | Gadolinium oxide production process |
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2002
- 2002-07-09 CN CN02123912A patent/CN1394972A/en active Pending
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- 2003-07-09 JP JP2003272363A patent/JP4046660B2/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100451140C (en) * | 2004-07-01 | 2009-01-14 | 包头市京瑞新材料有限公司 | Self protection process for preparing fluorescent grade europium oxide extractor by reducing extracting method |
| CN100352954C (en) * | 2005-04-05 | 2007-12-05 | 中国科学院长春应用化学研究所 | Technology for separating rare earth element by extraction system added with modifier |
| CN100435899C (en) * | 2006-01-24 | 2008-11-26 | 北京有色金属研究总院 | Saponification of organic extractant |
| CN108456792A (en) * | 2017-02-17 | 2018-08-28 | 厦门稀土材料研究所 | A kind of rare earth extraction separation extractant and preparation method thereof and extraction separating method |
| CN106916948A (en) * | 2017-03-07 | 2017-07-04 | 四川省冕宁县方兴稀土有限公司 | A kind of saponification agent and its application process of rare earth organic extractant |
| CN106916948B (en) * | 2017-03-07 | 2019-07-09 | 四川省冕宁县方兴稀土有限公司 | A kind of saponification agent and its application method of rare earth organic extractant |
| CN110002487A (en) * | 2019-04-17 | 2019-07-12 | 中国科学院长春应用化学研究所 | A kind of method of high yttrium type Rare Earth Mine grouping separation yttrium oxide |
| CN112457188A (en) * | 2020-11-24 | 2021-03-09 | 北京博萃循环科技有限公司 | Carboxylic acid compound and preparation method and application thereof |
| WO2022110821A1 (en) * | 2020-11-24 | 2022-06-02 | 苏州博萃循环科技有限公司 | Carboxylic acid compound, preparation method therefor and use thereof |
| CN112457188B (en) * | 2020-11-24 | 2022-07-08 | 苏州博萃循环科技有限公司 | Carboxylic acid compound and preparation method and application thereof |
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| JP2004036003A (en) | 2004-02-05 |
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