CN102417983A - Saponification-free method for extracting and separating rare earth sulfate - Google Patents
Saponification-free method for extracting and separating rare earth sulfate Download PDFInfo
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- CN102417983A CN102417983A CN2011104086258A CN201110408625A CN102417983A CN 102417983 A CN102417983 A CN 102417983A CN 2011104086258 A CN2011104086258 A CN 2011104086258A CN 201110408625 A CN201110408625 A CN 201110408625A CN 102417983 A CN102417983 A CN 102417983A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The invention discloses a saponification-free method for extracting and separating a rare earth sulfate. The method comprises the following steps of: (1) extracting and separating the water extract of the rare earth sulfate by using non-saponified P507 in a system of hydrochloric acid, P507 and kerosene to obtain a samarium-free rare earth sulfate carrying an organic phase; (2) refluxing the carried organic phase in the (1) by using a part of samarium europium gadolinium concentrate to obtain a carried organic phase of low-lanthanum lanthanum-cerium-praseodymium-neodymium rare earth chloride and samarium europium gadolinium; and (3) back extracting the carried organic phase in the (2) by using 5.4mol/L hydrochloric acid to obtain a pure samarium europium gadolinium concentrate and a blank organic phase. By the method, the characteristic of high pH value of the water extract is fully utilized by substituting P204 for the P507, a certain amount of low-europium rare earth chloride is produced, 10 to 20 percent of low-lanthanum lanthanum-cerium-praseodymium-neodymium rare earth chloride is educed, 10 to 20 percent of separation pressure of a fished rare earth transformation extraction and separation line is lightened, and the consumption of magnesium oxide required by neutralizing the acidity of the separation line is reduced by 10 to 20 percent.
Description
Technical field
The invention belongs to rare earth extraction purification technique field, specially refer to the baotite method for subsequent processing of the northern rare-earth mineral sinter process that is representative, promptly do not have the method for saponifiable extraction separate sulfur acid rare earth.
Background technology
It with the baotite rare earth sulfate solution of the total composition that after sulfuric acid high-temperature roasting, water logging, obtains of the northern ore deposit of representative.To pass through P in the former production
204Carry out the neodymium samarium and divide into groups, obtain heavy rare earths and few europium sulfuric acid rare earth, the shortcoming that this method exists is: 1. P
204With P
507It is anti-that extraction agent is compared Yi Cuinan, and the back extraction progression that needs is long, sour regurgitation concentration is high, increased the difficulty of back extraction, and the production environment Air quality is poor simultaneously.2. because P
204Extracting power strong, under the situation that does not add acid adjustment liquid, normal operation is produced in the easy emulsification influence of casing for itself and infusion (Ph value 2.5 ~ 4.5 sulfuric acid rare earth).Need regulate the acidity of introducing acid adjustment liquid with Natural manganese dioxide when 3. producing, increase material consumption.Do not draw the LaCePrNd rare earth chloride of low lanthanum in the technology (patent No. 200610072668.2) of a kind of extracting and separating rare earth elements from non-saponification system of professor Long Zhiqi of Beijing Non-Ferrous Metal Research General Academy invention, increased follow-up transition of processing burden and magnesian consumption.
Summary of the invention
The present invention provides a kind of method of not having saponifiable extraction separate sulfur acid rare earth; Through improvement to existing technology; Drawn the LaCePrNd rare earth chloride of the low lanthanum of 10%-20%; Not only alleviated the separating pressure that drags for rare earth extracting and separating line transition 10%-20%, and reduced and dragged in rare earth extracting and separating line transition and the 10%-20% of acidity requisite oxygen magnesium consumption.
For this reason, adopt following technical scheme: a kind of method of not having saponifiable extraction separate sulfur acid rare earth, this method may further comprise the steps:
(1) at hydrochloric acid, P
507In the extraction system of (2-ethylhexyl phosphonic acids single 2-ethyl is ester), kerosene, use without saponified P
507Extracting and separating sulfuric acid rare earth infusion obtains the sulfuric acid rare earth of load organic phases and no samarium;
(2), obtain the LaCePrNd rare earth chloride of low lanthanum and the load organic phases of sm-eu-gd with the load organic phases described in a part of sm-eu-gd enriched substance back scrubbing (1);
(3), obtain pure sm-eu-gd enriched substance with blank organic with the load organic phases of the sm-eu-gd of gained in the hydrochloric acid back extraction (2) of 5.4mol/L.
(1) the sulfuric acid rare earth infusion content described in is 25 ~ 35g/L, and acidity pH is 2.0 ~ 4.5.
In the LaCePrNd of the low lanthanum (2) samarium can not be arranged.
(3) content of pure sm-eu-gd enriched substance is 100 ~ 280g/L described in, and acidity requires H
+Concentration is 0.2 ~ 2.5mol/L.
The present invention uses P
507Replace P
204The high characteristics of Ph value of infusion have been made full use of; A certain amount of few europium rare earth chloride that can also attach output; Drawn the LaCePrNd rare earth chloride of the low lanthanum of 10%-20%; Not only alleviated the separating pressure that drags for rare earth extracting and separating line transition 10%-20%, and reduced and dragged in rare earth extracting and separating line transition and the 10%-20% of the consumption of acidity requisite oxygen magnesium.
Embodiment
A kind of method of not having saponifiable extraction separate sulfur acid rare earth
,Adopt three outlet technologies, after sulfuric acid high-temperature roasting, water logging, obtain sulfuric acid rare earth (C with northern ore deposit
RE=25 ~ 35g/L, Ph=2.0 ~ 4.5) solution is feed liquid, in hydrochloric acid and kerosene system, with P
507(2-ethylhexyl phosphonic acids single 2-ethyl is ester) is extraction agent, with the hydrochloric acid of 5.4mol/L as reverse-extraction agent; Primary outlet is a raffinate, and its composition is a rare earth sulfate solution; Second outlet water is for hanging down the LaCePrNd solution of lanthanum, and the 3rd outlet water is the sm-eu-gd enriched substance; Concrete case is following:
Embodiment 1: be 27g/L with concentration, the rare earth sulfate solution of Ph=2.0 ~ 4.5 is a feed liquid, and flow is 500L/min; P
507(2-ethylhexyl phosphonic acids single 2-ethyl is ester) is extraction agent, and flow is 60L/min, carries out counter-current extraction, and extraction reaches after the balance with C
H+The hydrochloric acid of=5.4mol/L carries out back extraction, and its flow is 10L/min.Primary outlet is a raffinate, and its composition is rare earth sulfate solution (content: 24g/L, Ph=1.5 ~ 2.0); With part sm-eu-gd solution is washing lotion; The principle of utilization IX is come the wash load organic phase; Must through and dragging for rare earth line transition at the LaCePrNd rare earth chloride of second low lanthanum of outlet output (content: 250g/L, Ph=1.5 ~ 2.0, Samarium trioxide < 1%), reduce the magnesian consumption that with acidity consume in required its transition.The 3rd outlet water is sm-eu-gd enriched substance (content: 250gL, acidity 0.5mol/L, Neodymium trioxide < 0.1%).
Embodiment 2: be 35g/L with concentration, the rare earth sulfate solution of Ph=2.0 ~ 4.5 is a feed liquid, and flow is 400L/min; P
507(2-ethylhexyl phosphonic acids single 2-ethyl is ester) is extraction agent, and flow is 50L/min, carries out counter-current extraction, and extraction reaches after the balance with C
H+The hydrochloric acid of=5.4mol/L carries out back extraction, and its flow is 10L/min.Primary outlet is a raffinate, and its composition is rare earth sulfate solution (content: 27g/L, Ph=1.5 ~ 2.0); With part sm-eu-gd solution is washing lotion; The principle of utilization IX is come the wash load organic phase; Must through and dragging for rare earth line transition at the LaCePrNd rare earth chloride of second low lanthanum of outlet output (content: 245g/L, Ph=1.5 ~ 2.0, Samarium trioxide < 1%), reduce the magnesian consumption that with acidity consume in required its transition.The 3rd outlet water is sm-eu-gd enriched substance (content: 245gL, acidity 0.6mol/L, Neodymium trioxide < 0.1%).
Claims (4)
1. method of not having saponifiable extraction separate sulfur acid rare earth, this method may further comprise the steps:
At hydrochloric acid, P
507In the extraction system of (2-ethylhexyl phosphonic acids single 2-ethyl is ester), kerosene, use without saponified P
507Extracting and separating sulfuric acid rare earth infusion obtains the sulfuric acid rare earth of load organic phases and no samarium;
With the load organic phases described in a part of sm-eu-gd enriched substance back scrubbing (1), obtain the LaCePrNd rare earth chloride of low lanthanum and the load organic phases of sm-eu-gd;
With the load organic phases of the sm-eu-gd of gained in the hydrochloric acid back extraction (2) of 5.4mol/L, obtain pure sm-eu-gd enriched substance with blank organic.
2. method according to claim 1 is characterized in that: the sulfuric acid rare earth infusion content described in (1) is 25 ~ 35g/L, and acidity pH is 2.0 ~ 4.5.
3. method according to claim 1 is characterized in that: in the LaCePrNd of the low lanthanum described in (2) samarium can not be arranged.
4. method according to claim 1 is characterized in that: the content of pure sm-eu-gd enriched substance is 100 ~ 280g/L described in (3), and acidity requires H
+Concentration is 0.2 ~ 2.5mol/L.
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| CN2011104086258A CN102417983A (en) | 2011-12-09 | 2011-12-09 | Saponification-free method for extracting and separating rare earth sulfate |
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| CN2011104086258A CN102417983A (en) | 2011-12-09 | 2011-12-09 | Saponification-free method for extracting and separating rare earth sulfate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526058A (en) * | 2013-10-21 | 2014-01-22 | 南昌航空大学 | Technique for preparing high-purity praseodymium from industrial praseodymium raw material |
| CN104232949A (en) * | 2014-10-14 | 2014-12-24 | 包头稀土研究院 | Recycling method for rare earth leaching and leaching water of sulfuric acid roasted rare earth ore concentrate |
| CN111074072A (en) * | 2019-12-19 | 2020-04-28 | 包头华美稀土高科有限公司 | Method for removing non-rare earth impurities in organic load of transition clarifying tank |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1880489A (en) * | 2006-02-27 | 2006-12-20 | 有研稀土新材料股份有限公司 | Non-saponifiable extraction full-separating process for high concentration rare earth solution |
| CN101050488A (en) * | 2006-04-07 | 2007-10-10 | 北京有色金属研究总院 | Technique for extracting and separating rare earth elements from non-saponification system |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1880489A (en) * | 2006-02-27 | 2006-12-20 | 有研稀土新材料股份有限公司 | Non-saponifiable extraction full-separating process for high concentration rare earth solution |
| CN101050488A (en) * | 2006-04-07 | 2007-10-10 | 北京有色金属研究总院 | Technique for extracting and separating rare earth elements from non-saponification system |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526058A (en) * | 2013-10-21 | 2014-01-22 | 南昌航空大学 | Technique for preparing high-purity praseodymium from industrial praseodymium raw material |
| CN103526058B (en) * | 2013-10-21 | 2014-10-08 | 南昌航空大学 | Technique for preparing high-purity praseodymium from industrial praseodymium raw material |
| CN104232949A (en) * | 2014-10-14 | 2014-12-24 | 包头稀土研究院 | Recycling method for rare earth leaching and leaching water of sulfuric acid roasted rare earth ore concentrate |
| CN104232949B (en) * | 2014-10-14 | 2016-03-02 | 包头稀土研究院 | The rare earth of sulphating roasting rare earth concentrate leaches and leaches the circulation utilization method of water |
| CN111074072A (en) * | 2019-12-19 | 2020-04-28 | 包头华美稀土高科有限公司 | Method for removing non-rare earth impurities in organic load of transition clarifying tank |
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Application publication date: 20120418 |