CN103602812A - Rare-earth organic extractant and back-extraction process thereof - Google Patents
Rare-earth organic extractant and back-extraction process thereof Download PDFInfo
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Abstract
The invention discloses a rare-earth organic extractant and a back-extraction process thereof. The organic extractant contains the ingredients in percentage by volume: 20-35% of cyclohexane, 15-45% of liquid ammonia saponification extractant, 15-35% of N235 and 20-40% of sulfonated kerosene, wherein the liquid ammonia saponification extractant is either P507 or P204. The back-extraction process comprises the steps of preparing loading organic phases containing different rare earth concentrations through extraction, back-extracting and precipitating, thereby obtaining rare-earth oxalate with large grain diameter. A non-saponification extraction system is provided by the invention, and near-zero emission of ammonia nitrogen is realized; the back-extraction process disclosed by the invention has the advantages of high phase separation speed, obvious two-phase boundary and high back-extraction ratio; and a crystal is not deposited on a bottom plate of a back-extraction tank and does not scar on the periphery.
Description
Technical field
The invention belongs to field of metallurgy and chemical engineering, relate to a kind of rare earth organic extractant and stripping process thereof.
Background technology
South, Jiangxi ion type rareearth ore mostly is middle heavy rare earths ore deposit, often adopt extraction agent extracting and separating rear earth elements in hydrochloric acid system such as P507, P204 of ammoniacal liquor or liquefied ammonia saponification, but this technique exists the problems such as soda acid consumption is large, cost is high, wastewater discharge is large.Updating and upgrading along with extraction and separation technology, concept without saponifiable extraction has been proposed, compare with former technique the acid-base consumption that can save nearly 30%, significantly reduce industrial cost, without saponifiable extraction technology, removed saponifying process, can solve from source ammonia and nitrogen pollution problem in saponifiable extraction process, realize without emission intensity.But still need further to improve without the lifting of the back extraction ratio under saponifiable extraction technique, deposition rate and the preparation of large particle diameter rare earth compound, therefore, find suitable reverse-extraction agent, and the optimum process condition of definite back extraction and post precipitation thereof has important application prospect.
Now the back extraction report of rare earth loaded organic phase is had: patent " without the method for saponifiable extraction separate sulfur acid rare earth " [Yang Wenhao, Zhang Shanghu, Liao Chunsheng etc., application for a patent for invention numbers 201110408625.8, authorize publication number CN102417983A], " a kind of technique of extracting rare earth element by non-saponifiable phosphorous mixing extractant " [Huang little Wei, Li Jianning, Peng Xinlin etc., application for a patent for invention numbers 200510137231.8, authorize publication number CN1804063A.], " a kind of without saponification rare-earth extraction separating process " [Yang Youming, Nie Huaping, Deng Shenghua etc., application for a patent for invention numbers 201210290516.5, authorize publication number CN102766766A.] etc. all adopt hydrochloric acid to go the rare earth loaded organic phase of back extraction as extraction agent.HDEHP and HEH/EHP system have been compared in the researchs such as Huang little Wei, under uniform acidity condition, and HCl, HNO
3, H
2sO
4to same load organic phases (Y
3+) back extraction performance, the back extraction best results of HCl [imperial will is strange etc., rare earth, 2008,29 (3): 5-9. for Huang little Wei, Zhang Yongqi] wherein.Zhang Yongqi etc. with regard to HCl to HDEHP and Cyanex272 hybrid extraction system load Y
3+the back extraction performance of organic phase is studied, and when HCl concentration is 3mol/L, single-stage back extraction ratio can reach 96% [Zhang Yongqi, Huang little Wei, Wang Chunmei etc., rare metal, 2009,33 (1): 124-128.].
Can find out, the back extraction effect that the hydrochloric acid of usining carries out back extraction as reverse-extraction agent to rare earth loaded organic phase is better, is first-selected reverse-extraction agent.And rare-earth products major part is oxide compound, the solubility product of rare earth oxalate is little, is easy to be sintered into oxide compound, therefore adopt oxalic acid as precipitation agent.But at present from rare earth loaded organic phase back extraction and post precipitation operation without saponification, the grain diameter of its back extraction ratio and rare earth oxalate thereof need to promote.
Summary of the invention
The object of this invention is to provide a kind of rare earth organic extractant and stripping process thereof.
For achieving the above object, the present invention is by the following technical solutions:
A rare earth organic extractant, the volume fraction containing hexanaphthene in organic extractant is 20% ~ 35%, and the volume fraction that the volume fraction of liquefied ammonia Saponified Extractants is 15% ~ 45%, N235 is 15% ~ 35%, and the volume fraction of sulfonated kerosene is 20% ~ 40%; Wherein, liquefied ammonia Saponified Extractants is a kind of in P507, P204.
A rare earth organic extractant stripping process, comprises the following steps:
(1) take described rare earth organic extractant is organic phase, by certain volume, than extracting rare-earth, obtains rare earth loaded organic phase;
(2) load organic phases is adopted and to add hydrochloric acid and carry out back extraction;
(3) control corresponding conditions, liquid after rare earth is added to oxalic acid precipitation, obtain the rare earth oxalate of macrobead particle diameter.
In described step (1), the rare earth concentration of the load organic phases after extraction is 0.05-0.20mol/L.
In described step (2), the concentration of hydrochloric acid is 2.0mol/L ~ 4.0mol/L, and the volume flow ratio O/A of load organic phases and hydrochloric acid is 1:2 ~ 1:1, makes final single-stage stripping rate be greater than 98%.
In described step (2), back extraction process duration of oscillation is 1min ~ 40min, and the single-stage stripping rate of back extraction process is greater than 98%.
In described step (3), temperature is controlled at 15 ℃ ~ 75 ℃, and adding oxalic acid amount is 100% ~ 150% of theoretical oxalic acid amount, and stirring velocity is 100r/min ~ 1200r/min, after precipitation 10h ~ 40h, filters, and dries, and obtains grain graininess at the rare earth oxalate of 20 ~ 70 μ m.
Beneficial effect of the present invention is, a kind of non-saponifiable extraction system is provided, and has realized ammonia nitrogen near zero release, reduces environmental pollution, reduces acid consumption, has reduced industrial cost, has made the rare earth oxalate (20 μ m ~ 70 μ m) of large particle diameter.Compare with extraction systems such as traditional P507-hydrochloric acid, P507-nitric acid, P204-sulfuric acid, stripping process of the present invention divides phase velocity fast, and two-phase boundary is obvious, and back extraction ratio is high.Crystal does not deposit, in surrounding, does not scab on the base plate of reextraction groove.
Embodiment
Embodiment 1: get the load organic phases (concentration of La is 0.0593mol/L, and wherein organic phase volume ratio is 30% hexanaphthene+15%P507+35% N235+20% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1) of 3.0mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 1min that vibrates on vibrator, standing observation, its 0-1min phase-splitting, minute phase velocity is slightly slow, interface is clear, and water is limpid, and calculating back extraction ratio is 98.02%.
Embodiment 2: get the load organic phases (concentration of La is 0.0976 mol/L, and wherein organic phase volume ratio is 20% hexanaphthene+45%P204+15% N235+20% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1.2) of 2.5mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 25min that vibrates on vibrator, standing observation, its 0-1min phase-splitting that is exceedingly fast, minute phase effect is fine, water is clear, and calculating back extraction ratio is 98.48%.
Embodiment 3: get the load organic phases (concentration of La is 0.1566 mol/L, and wherein organic phase volume ratio is 20% hexanaphthene+35%P507+30% N235+20% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1) of 3.5mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 40min that vibrates on vibrator, standing observation, its 0-1min High-speed clarification, interface is clear, water is limpid, and calculating back extraction ratio is 99.04%.
Embodiment 4: get the load organic phases (concentration of Ce is 0.0553mol/L, and wherein organic phase volume ratio is 35% hexanaphthene+15%P507+20% N235+30% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1) of 2.0mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 10min that vibrates on vibrator, standing observation, its 0-1min clarifies at once, and interface is clear, and calculating back extraction ratio is 98.16%.
Embodiment 5: get the load organic phases (concentration of Ce is 0.1490mol/L, and wherein organic phase volume ratio is 22.5% hexanaphthene+30%P507+25% N235+22.5% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1) of 3.5mol/L, be made into after mixing solutions in separating funnel, move on stand standing observation after being placed in the 25min that vibrates on vibrator; Its 1-2min phase-splitting is complete, and interface is clear, and water is limpid, and calculating back extraction ratio is 99.56%.
Embodiment 6: get the load organic phases (concentration of Ce is 0.0951 mol/L, and wherein organic phase volume ratio is 30% hexanaphthene+22.5%P204+27.5% N235+20% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1.5) of 2.5mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 40min that vibrates on vibrator, standing observation, its 0-1min phase-splitting that is exceedingly fast, minute phase effect is fine, water is clear, and calculating back extraction ratio is 98.74%.
Embodiment 7: get the load organic phases (concentration of Pr is 0.0524 mol/L, and wherein organic phase volume ratio is 20% hexanaphthene+15%P507+25% N235+40% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1.2) of 2.5mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 3min that vibrates on vibrator, standing observation, its 0-1min phase-splitting that is exceedingly fast, interface is clear, water is clear, and calculating back extraction ratio is 98.26%.
Embodiment 8: get the load organic phases (concentration of Pr is 0.1432 mol/L, and wherein organic phase volume ratio is 22.5% hexanaphthene+35%P507+20% N235+22.5% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1) of 4.0mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 15min that vibrates on vibrator, standing observation, its 1-2min phase-splitting, two-phase boundary is clear, water is clear, and calculating back extraction ratio is 99.36%.
Embodiment 9: get the load organic phases (concentration of Pr is 0.0886 mol/L, and wherein organic phase volume ratio is 25% hexanaphthene+25%P507+25% N235+25% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1.5) of 3.0mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 20min that vibrates on vibrator, standing observation, its 0-1min phase-splitting that is exceedingly fast, minute phase effect is fine, water is clear, and calculating back extraction ratio is 98.48%.
Embodiment 10: get the load organic phases (concentration of Nd is 0.0641 mol/L, and wherein organic phase volume ratio is 22.5% hexanaphthene+40%P204+15% N235+22.5% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1.5) of 2.0mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 30min that vibrates on vibrator, standing observation, it is phase-splitting at once, and interface is clear, two alternately have a little bubble, and calculating back extraction ratio is 98.03%.
Embodiment 11: get the load organic phases (concentration of Nd is 0.1348 mol/L, and wherein organic phase volume ratio is 27.5% hexanaphthene+30%P507+20% N235+22.5% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1) of 3.0mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 5min that vibrates on vibrator, standing observation, it is phase-splitting at once, and interface is clear, and calculating back extraction ratio is 98.76%.
Embodiment 12: get load organic phases (concentration of Nd is 0.1680 mol/L) after extraction wherein organic phase volume ratio be 22.5% hexanaphthene+30%P507+25% N235+22.5% sulfonated kerosene); Adopt the hydrochloric acid back extraction (comparing 1:2) of 3.5mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 15min that vibrates on vibrator, standing observation, it is phase-splitting at once, and interface is clear, and calculating back extraction ratio is 99.19%.
Embodiment 13: get the load organic phases (concentration of Y is 0.0575 mol/L, and wherein organic phase volume ratio is 25% hexanaphthene+15%P507+30% N235+30% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1.2) of 2mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 10min that vibrates on vibrator, standing observation, its 0-1min phase-splitting that is exceedingly fast, minute phase effect is fine, water is clear, and calculating back extraction ratio is 98.65%.
Embodiment 14: get the load organic phases (concentration of Y is 0.1185 mol/L, and wherein organic phase volume ratio is 25% hexanaphthene+25%P507+30% N235+20% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1.5) of 2.5mol/L, be made into after mixing solutions in separating funnel, move on stand after being placed in the 25min that vibrates on vibrator, standing observation, its 0-1min phase-splitting that is exceedingly fast, minute phase effect is fine, water is clear, and calculating back extraction ratio is 99.15%.
Embodiment 15: get the load organic phases (concentration of Y is 0.1728mol/L, and wherein organic phase volume ratio is 22.5% hexanaphthene+30%P507+25% N235+22.5% sulfonated kerosene) after extraction; Adopt the hydrochloric acid back extraction (comparing 1:1) of 3.0mol/L, be made into after mixing solutions in separating funnel, move on stand standing observation after being placed in the 40min that vibrates on vibrator; It is phase-splitting at once, and interface is clear, and calculating back extraction ratio is 99.40%.
Embodiment 16: the rare earth feed liquid (LaCl after negate extraction
3concentration 0.0581mol/L); In temperature, be 35 ℃, stirring velocity is under 250r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.1373g, and after the 30h precipitation time, the particle diameter that filtration washing oven dry obtains lanthanum oxalate is 36.2um.
Embodiment 17: the rare earth feed liquid (LaCl after negate extraction
3concentration 0.0961mol/L); In temperature, be 15 ℃, stirring velocity is under 500r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.1817g, and after the 18h precipitation time, the particle diameter that filtration washing oven dry obtains lanthanum oxalate is 25.5um.
Embodiment 18: the rare earth feed liquid (LaCl after negate extraction
3concentration 0.1551mol/L); In temperature, be 60 ℃, stirring velocity is under 950r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.4106g, and after the 36h precipitation time, the particle diameter that filtration washing oven dry obtains lanthanum oxalate is 32.1um.
Embodiment 19: the rare earth feed liquid (CeCl after negate extraction
3concentration 0.0543mol/L); In temperature, be 65 ℃, stirring velocity is under 1200r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.1438g, and after the 24h precipitation time, the particle diameter that filtration washing oven dry obtains Sedemesis is 37.3um.
Embodiment 20: the rare earth feed liquid (CeCl after negate extraction
3concentration 0.1483mol/L); In temperature, be 35 ℃, stirring velocity is under 550r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.3365g, and after the 30h precipitation time, the particle diameter that filtration washing oven dry obtains Sedemesis is 51.3um.
Embodiment 21: the rare earth feed liquid (CeCl after negate extraction
3concentration 0.0939mol/L); In temperature, be 25 ℃, stirring velocity is under 100r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.2042g, and after the 40h precipitation time, the particle diameter that filtration washing oven dry obtains Sedemesis is 45.8um.
Embodiment 22: the rare earth feed liquid (PrCl after negate extraction
3concentration 0.0515mol/L); In temperature, be 55 ℃, stirring velocity is under 300r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.1266g, and after the 20h precipitation time, the particle diameter that filtration washing oven dry obtains praseodymium oxalate is 30.8um.
Embodiment 23: the rare earth feed liquid (PrCl after negate extraction
3concentration 0.1423mol/L); In temperature, be 35 ℃, stirring velocity is under 500r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.3229g, and after the 30h precipitation time, the particle diameter that filtration washing oven dry obtains praseodymium oxalate is 58.4um.
Embodiment 24: the rare earth feed liquid (PrCl after negate extraction
3concentration 0.0873mol/L); In temperature, be 25 ℃, stirring velocity is under 650r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.2476g, and after the 10h precipitation time, the particle diameter that filtration washing oven dry obtains praseodymium oxalate is 35.4um.
Embodiment 25: the rare earth feed liquid (NdCl after negate extraction
3concentration 0.0628mol/L); In temperature, be 25 ℃, stirring velocity is under 150r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.1663g, and after the 24h precipitation time, the particle diameter that filtration washing oven dry obtains neodymium oxalate is 28.2um.
Embodiment 26: the rare earth feed liquid (NdCl after negate extraction
3concentration 0.1331mol/L); In temperature, be 75 ℃, stirring velocity is under 400r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.2895g, and after the 18h precipitation time, the particle diameter that filtration washing oven dry obtains neodymium oxalate is 38.6um.
Embodiment 27: the rare earth feed liquid (NdCl after negate extraction
3concentration 0.1668mol/L); In temperature, be 35 ℃, stirring velocity is under 550r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.3943g, and after the 30h precipitation time, the particle diameter that filtration washing oven dry obtains neodymium oxalate is 55.8um.
Embodiment 28: the rare earth feed liquid (YCl after negate extraction
3concentration 0.0567mol/L); In temperature, be 45 ℃, stirring velocity is under 450r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.1340g, and after the 25h precipitation time, the particle diameter that filtration washing oven dry obtains yttrium oxalate is 41.3um.
Embodiment 29: the rare earth feed liquid (YCl after negate extraction
3concentration 0.1175mol/L); In temperature, be 55 ℃, stirring velocity is under 500r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.2666g, and after the 30h precipitation time, the particle diameter that filtration washing oven dry obtains yttrium oxalate is 68.1um.
Embodiment 30: the rare earth feed liquid (YCl after negate extraction
3concentration 0.1718mol/L); In temperature, be 65 ℃, stirring velocity is under 700r/min condition, adds the oxalic acid precipitation rare earth feed liquid of 0.3249g, and after the 18h precipitation time, the particle diameter that filtration washing oven dry obtains yttrium oxalate is 30.6um.
Claims (8)
1. a rare earth organic extractant, it is characterized in that: the volume fraction containing hexanaphthene in organic extractant is 20% ~ 35%, the volume fraction of liquefied ammonia Saponified Extractants is that the volume fraction of 15% ~ 45%, N235 is 15% ~ 35%, and the volume fraction of sulfonated kerosene is 20% ~ 40%; Wherein, liquefied ammonia Saponified Extractants is a kind of in P507, P204.
2. a rare earth organic extractant stripping process described in claim 1, is characterized in that comprising the following steps:
(1) right to use requires rare earth organic extractant extraction described in 1 to prepare the load organic phases containing different rare earth concentrations;
(2) load organic phases is adopted and to add hydrochloric acid and carry out back extraction;
(3) liquid after rare earth is added to oxalic acid precipitation, obtain the rare earth oxalate of macrobead particle diameter.
3. a kind of rare earth organic extractant stripping process according to claim 2, is characterized in that: in described step (1), the rare earth concentration of the load organic phases after extraction is 0.05-0.20mol/L.
4. a kind of rare earth organic extractant stripping process according to claim 2, is characterized in that: in described step (2), the concentration of hydrochloric acid is 2.0mol/L ~ 4.0mol/L, and the volume flow ratio O/A of load organic phases and hydrochloric acid is 1:2 ~ 1:1.
5. a kind of rare earth organic extractant stripping process according to claim 2, is characterized in that: in described step (2), back extraction process duration of oscillation is 1min ~ 40min, and the single-stage stripping rate of back extraction process is greater than 98%.
6. a kind of rare earth organic extractant stripping process according to claim 2, is characterized in that: in described step (3), adopt 100% ~ 150% precipitating rare earth of oxalic acid theoretical amount.
7. a kind of rare earth organic extractant stripping process according to claim 2, it is characterized in that: in described step (3), the temperature of oxalic acid precipitation is 15 ℃ ~ 75 ℃, the stirring velocity of precipitation process is 100r/min ~ 1200r/min, and the precipitation time that liquid after rare earth is added after oxalic acid precipitation is 10h ~ 40h.
8. a kind of rare earth organic extractant stripping process according to claim 2, is characterized in that: in described step (3), the particle diameter of rare earth oxalate is 20-70 μ m.
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| CN109912093A (en) * | 2019-02-19 | 2019-06-21 | 北京中科康仑环境科技研究院有限公司 | A kind of zero-discharge production process based on praseodymium, neodymium anti-stripping agent |
| CN109912093B (en) * | 2019-02-19 | 2021-11-30 | 北京中科康仑环境科技研究院有限公司 | Zero-emission production process based on praseodymium and neodymium back-extraction liquid |
| CN109797287A (en) * | 2019-02-20 | 2019-05-24 | 中铝稀土（江苏）有限公司 | The rare-earth smelting separation method of high-salt wastewater resource utilization |
| CN110961086A (en) * | 2019-12-15 | 2020-04-07 | 江西理工大学 | Extractant functionalized magnetic nano-adsorption material, preparation method and application |
| CN110961086B (en) * | 2019-12-15 | 2021-12-03 | 江西理工大学 | Extractant functionalized magnetic nano-adsorption material, preparation method and application |
| WO2022014234A1 (en) * | 2020-07-13 | 2022-01-20 | 住友金属鉱山株式会社 | Method for recovering scandium |
| JP7528581B2 (en) | 2020-07-13 | 2024-08-06 | 住友金属鉱山株式会社 | How to recover scandium |
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