CN1131200A - Solvent extraction and separation new system of thulium, ytterbium and lutetium - Google Patents
Solvent extraction and separation new system of thulium, ytterbium and lutetium Download PDFInfo
- Publication number
- CN1131200A CN1131200A CN95117986A CN95117986A CN1131200A CN 1131200 A CN1131200 A CN 1131200A CN 95117986 A CN95117986 A CN 95117986A CN 95117986 A CN95117986 A CN 95117986A CN 1131200 A CN1131200 A CN 1131200A
- Authority
- CN
- China
- Prior art keywords
- ytterbium
- thulium
- organic phase
- lutetium
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to a new type method for solvent-extracting and separating heavy rare earth elements of thulium, ytterbium and lutecium. It can obtain the above-mentioned elements with high purity. Said invention breaks through the shackles of conventional extraction chromatography or ion-exchange chromatography for producing high-purity thulium, ytterbium and lutecium, and overcomes the main disadvantages of chromatography for production of high-purity heavy rare earths so as to simplify technological condition and reduce its production cost.
Description
The present invention relates to the method for a kind of novel dissolvent extracting and separating thulium, ytterbium, lutetium, and can obtain straight product.
China's Rare Earth Production mainly adopts solvent extration, and what the extraction agent that generally adopts was main at present is naphthenic acid, P204 (2-ethylhexyl phosphoric acid dibasic acid esters) and P507 (2-ethylhexyl phosphoric acid single 2-ethyl hexyl fat).Because P204 and P507 acidity are stronger, make their balance acidity height when extracting rare-earth, this phenomenon is even more serious in its extraction to heavy rare earths.Along with the increase of institute's extracting rare-earth ordination number, their reextraction more and more is stranded piebald horse.Though the rare earth extraction balance acidity of P507 is low slightly than P204, it is difficult to finish with extraction process the separation fully of all rare earth elements.The naphthenic acid low price, extraction equilibrium acidity is low, but it is only applicable to extract yttrium oxide from mishmetal.All there is not the extraction agent that ideal separates heavy rare earths thulium, ytterbium, lutetium at present both at home and abroad.
The present invention selects the class new extractant shown in the following formula (I) for use according to the relation of solvent extraction principle and extractant molecules structure and extraction ability, can produce highly purified thulium, ytterbium, lutetium:
O
R
1R
2N(CH
2)
1-8P-OR
3 (I)
OR
4
N=1-8 in the formula; R
1, R
2, R
3, R
4Represent C
1-10Alkyl, aromatic base or hydrogen, they can be identical or inequality.This kind of extractants is called for short JS.
Method of the present invention comprises:
(1) with JS is extraction agent, C
4-10Alcohol or their mixture be additive, kerosene is thinner, be collectively referred to as organic phase, wherein the volume ratio of each component is followed successively by: extraction agent: alcohol: kerosene equals (20-25): (5-10): (70-75), the concentration of extraction agent is 0.5-0.6mol/L, this organic phase is used after ammoniacal liquor or sodium hydroxide saponification, and saponification deg is 20-50%; Heavy rare earth mixture with any mol ratio is a raw material; In hydrochloric acid medium, carry out fractionation extraction, produce and the corresponding single heavy rare earths product of raw material.The separation that is used for ytterbium-lutetium can obtain high-purity lutecium oxide and ytterbium oxide or thulium, ytterbium mixture; Obtain high-purity trioxide and ytterbium oxide, lutetium mixture with thulium-ytterbium separating technology.
(2) adopt described extraction system, the significant parameter of ytterbium-lutetium segregation section technology is: saponification organic phase and rare earth and flow the 2-4 level after, advance groove with the rare earth soap form, feed concentration 0.5-1.0mol/L, the about pH=1-3 of acidity washes acid concentration 2.0-4.5mol/L, and extraction section progression is 50-60, washing section progression is 35-40, and stream is than being: organic phase: feed liquid: wash acid=8-10: 1: 1.5-2.0.Under the described conditions, the ytterbium of concentration 0.5-0.8mol/L, the about pH=1 of acidity or thulium, ytterbium mishmetal can be obtained, the feed liquid of thulium-ytterbium segregation section can be made from the water raffinate; Can obtain the straight product of lutetium from the organic phase outlet.
(3) extraction section and the washing section progression of thulium-ytterbium segregation section technology are respectively 20-40 and 25-35, each mutually stream than being: organic phase: feed liquid: wash acid=5-7: 1: 1.5-2.0 can obtain the thulium straight product of concentration 0.3-0.5mol/L, the about pH=1 of acidity under these conditions from the water raffinate; Can obtain pure ytterbium product or ytterbium, lutetium mixture from organic phase outlet.
The advantage of the inventive method is: broken and produced the habitual extraction chromatography of high-purity thulium, ytterbium, lutetium or the circle of ion-exchange chromatography method, overcome with chromatography and produced the main drawback that exists in high-purity heavy rare earths technology, simplified technical process.Under the condition of same turnout, but the present invention reduces equipment and reagent investment than the chromatography several times, reduce production cost, and production process is continuous, easy and simple to handle, is easy to other Rare Earth Production lines supportingly, has remarkable economic efficiency; Because extraction agent price of the present invention is suitable with the P507 extraction agent, equipment used has been widely used in domestic and international Rare Earth Production, thereby wide adaptability, and is simple.
In order to be illustrated more clearly in the present invention, enumerate following examples, but it there is not any restriction to scope of the present invention.
Example 1:
1.. as shown in drawings, adopting fractionation extraction process to carry out ytterbium-lutetium separates, the volume percent of extracted organic phase is: JS404: secondary octanol: kerosene=20: 10: 70, the concentration 0.6mol/L of JS404 wherein, the saponification deg of extracted organic phase is 50%, saponification organic phase and rare earth and flow 4 grades after enter the extraction section first step: rare earth feed liquid concentration is 0.5mol/L, the about pH=1 of acidity, wherein contain lutetium 7-10%, all the other element T m
2O
3Contain 7-10%, Yb
2O
3Contain 80-86%; The washing lotion concentration of hydrochloric acid is 2.0mol/L, and extraction section progression is 50, and washing section progression is 35, and stream is than being: organic phase: feed liquid: wash acid=15: 1: 2.2.Obtain thulium, the ytterbium mixture of concentration 0.5mol/L, the about pH=1 of acidity under the described conditions from the water raffinate; Can obtain pure lutetium product (99-99.9%) from the organic phase outlet.
2.. with 1. water raffinate outlet thulium, ytterbium mixture is raw material, adopts with 1. identical organic phase and washes acid, and extraction section progression is 30, and washing section progression is 25, flows than being: organic phase: feed liquid: wash acid=10: 1: 1.8.Under the described conditions, can obtain the pure thulium product (99-99.9%) of concentration 0.5mol/L, the about pH=1 of acidity from the water raffinate; Can obtain pure ytterbium product (99-99.9%) from the organic phase outlet.
Example 2:
1.. as shown in drawings, adopting fractionation extraction process to carry out ytterbium-lutetium separates, the volume percent of extracted organic phase is: JS401: secondary octanol: kerosene=20: 10: 70, the concentration 0.6mol/L of JS401 wherein, the saponification deg of extracted organic phase is 50%, saponification organic phase and rare earth and flow 4 grades after enter the extraction section first step; Rare earth feed liquid concentration is 0.5mol/L, and the about pH=1 of acidity wherein contains lutetium 7-10%, all the other element T m
2O
3Contain 7-10%, Yb
2O
3Contain 80-86%; The washing lotion concentration of hydrochloric acid is 2.0mol/L, and extraction section progression is 50, and washing section progression is 35, and stream is than being: organic phase: feed liquid: wash acid=15: 1: 2.2.Obtain thulium, the ytterbium mishmetal feed liquid of concentration 0.5mol/L, the about pH=1 of acidity under the described conditions from the water raffinate; Can obtain the straight product (99-99.9%) of lutetium from the organic phase outlet.
2.. with 1. water raffinate outlet thulium, ytterbium mixture is raw material, adopts with 1. identical organic phase and washes acid, and extraction section progression is 40, and washing section progression is 30, flows than being: organic phase: feed liquid: wash acid=10: 1: 1.8.Under the described conditions, can obtain the pure thulium product (99-99.9%) of concentration 0.5mol/L, the about pH=1 of acidity from the water raffinate; Can obtain pure ytterbium product (99-99.9%) from the organic phase outlet.
Brief Description Of Drawings:
The technical process schematic block diagram.
1. saponification organic phase 2. feed liquids
3. washing lotion 4. saponification organic phases
5. 6. washing lotion of raffinate (rare earth soap feed liquid and feed liquid)
Claims (1)
1. the method for an extracting and separating thulium, ytterbium, lutetium is characterized in that described method comprises:
(1). with JS is extraction agent, C
4-10Alcohol or their mixture be additive, kerosene is thinner, be collectively referred to as extracted organic phase, wherein the volume ratio of each component is followed successively by: extraction agent: alcohol: kerosene equals (20-25): (5-10): (70-75), the concentration of extraction agent is 0.5-0.6mol/L, this organic phase is used after ammoniacal liquor or sodium hydroxide saponification, and saponification deg is 20-50%; Heavy rare earth mixture with any mol ratio is a raw material; In hydrochloric acid medium, carry out fractionation extraction, produce and the corresponding single heavy rare earths product of raw material.The separation that is used for ytterbium-lutetium can obtain high-purity lutecium oxide and ytterbium oxide or thulium, ytterbium mixture; Obtain high-purity trioxide and ytterbium oxide or ytterbium, lutetium mixture with thulium-ytterbium separating technology.
(2) adopt described extraction system, the significant parameter of ytterbium-lutetium segregation section technology is: saponification organic phase and rare earth and flow the 2-4 level after, advance groove with the rare earth soap form, feed concentration 0.5-1.0mol/L, the about pH=1-3 of acidity washes acid concentration 2.0-4.5mol/L, and extraction section progression is 50-60, washing section progression is 35-40, and stream is than being: organic phase: feed liquid: wash acid=8-10: 1: 1.5-2.0.Under the described conditions, the ytterbium of concentration 0.5-0.8mol/L, the about pH=1 of acidity or thulium, ytterbium mishmetal can be obtained, the feed liquid of thulium-ytterbium segregation section can be made from the water raffinate; Can obtain the straight product of lutetium from the organic phase outlet.
(3) extraction section and the washing section progression of thulium-ytterbium segregation section technology are respectively 20-40 and 25-35, each flows mutually than being: organic phase.: feed liquid: wash acid=5-7: 1: 1.5-2.0, under these conditions, can obtain the thulium straight product of concentration 0.3-0.5mol/L, the about pH=1 of acidity from the water raffinate; Can obtain pure ytterbium product or ytterbium lutetium mixture from the organic phase outlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95117986A CN1054644C (en) | 1995-11-08 | 1995-11-08 | Solvent extraction and separation new system of thulium, ytterbium and lutetium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN95117986A CN1054644C (en) | 1995-11-08 | 1995-11-08 | Solvent extraction and separation new system of thulium, ytterbium and lutetium |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1131200A true CN1131200A (en) | 1996-09-18 |
| CN1054644C CN1054644C (en) | 2000-07-19 |
Family
ID=5081503
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95117986A Expired - Lifetime CN1054644C (en) | 1995-11-08 | 1995-11-08 | Solvent extraction and separation new system of thulium, ytterbium and lutetium |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1054644C (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1101476C (en) * | 1998-01-13 | 2003-02-12 | 北京大学 | Process for producing high-purity lutetium oxide by extracting separation method |
| CN100435899C (en) * | 2006-01-24 | 2008-11-26 | 北京有色金属研究总院 | Saponification of organic extractant |
| CN1872377B (en) * | 2006-01-04 | 2010-08-18 | 有研稀土新材料股份有限公司 | Method for saponifying extraction agent |
| CN101748275B (en) * | 2009-12-22 | 2011-02-02 | 江阴加华新材料资源有限公司 | Preparation method of low-thorium lutetium oxide |
| CN103718250A (en) * | 2011-07-15 | 2014-04-09 | Itm同位素技术慕尼黑股份公司 | Method for producing high-purity 177Lu compound added without carrier and 177Lu compound added without carrier |
| CN108717008A (en) * | 2018-03-13 | 2018-10-30 | 力合科技（湖南）股份有限公司 | Water quality detecting device and detection method |
| RU2686502C1 (en) * | 2018-12-17 | 2019-04-29 | федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский горный университет" | Method of extracting lutetium (iii) from solutions of salts |
| CN110386617A (en) * | 2019-07-22 | 2019-10-29 | 南昌航空大学 | A kind of method of solvent extraction and separation thulium ytterbium lutetium enriched substance |
| CN115679130A (en) * | 2021-07-21 | 2023-02-03 | 中国科学院长春应用化学研究所 | A kind of grouping method of ionic rare earth ore erbium and thulium |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049695C (en) * | 1994-07-28 | 2000-02-23 | 北京大学 | Method for purifying noble metal with double function extracting agent containing nitrogen and phosphorus |
-
1995
- 1995-11-08 CN CN95117986A patent/CN1054644C/en not_active Expired - Lifetime
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1101476C (en) * | 1998-01-13 | 2003-02-12 | 北京大学 | Process for producing high-purity lutetium oxide by extracting separation method |
| CN1872377B (en) * | 2006-01-04 | 2010-08-18 | 有研稀土新材料股份有限公司 | Method for saponifying extraction agent |
| CN100435899C (en) * | 2006-01-24 | 2008-11-26 | 北京有色金属研究总院 | Saponification of organic extractant |
| CN101748275B (en) * | 2009-12-22 | 2011-02-02 | 江阴加华新材料资源有限公司 | Preparation method of low-thorium lutetium oxide |
| US9816156B2 (en) | 2011-07-15 | 2017-11-14 | ITM Isotopen Technologien München AG | Method of manufacturing non-carrier-added high-purity 177Lu compounds as well as non-carrier-added 177Lu compounds |
| CN103718250B (en) * | 2011-07-15 | 2016-06-01 | Itm同位素技术慕尼黑股份公司 | The high purity that production carrier free is added177The method of Lu compound and carrier free are added177Lu compound |
| CN103718250A (en) * | 2011-07-15 | 2014-04-09 | Itm同位素技术慕尼黑股份公司 | Method for producing high-purity 177Lu compound added without carrier and 177Lu compound added without carrier |
| CN108717008A (en) * | 2018-03-13 | 2018-10-30 | 力合科技（湖南）股份有限公司 | Water quality detecting device and detection method |
| CN108717008B (en) * | 2018-03-13 | 2021-04-06 | 力合科技（湖南）股份有限公司 | Water quality detection device and detection method |
| RU2686502C1 (en) * | 2018-12-17 | 2019-04-29 | федеральное государственное бюджетное образовательное учреждение высшего образования "Санкт-Петербургский горный университет" | Method of extracting lutetium (iii) from solutions of salts |
| CN110386617A (en) * | 2019-07-22 | 2019-10-29 | 南昌航空大学 | A kind of method of solvent extraction and separation thulium ytterbium lutetium enriched substance |
| CN110386617B (en) * | 2019-07-22 | 2022-01-18 | 南昌航空大学 | Method for separating thulium, ytterbium and lutetium enrichment through solvent extraction |
| CN115679130A (en) * | 2021-07-21 | 2023-02-03 | 中国科学院长春应用化学研究所 | A kind of grouping method of ionic rare earth ore erbium and thulium |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1054644C (en) | 2000-07-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1131200A (en) | Solvent extraction and separation new system of thulium, ytterbium and lutetium | |
| CN101306989B (en) | Process for separating acetic acid from water by salt-containing extracting, rectifying and separating | |
| AU2012375748A2 (en) | Method for extracting and separating rare-earth element | |
| CN105779762B (en) | The technique that a kind of extract and separate prepares 5N erbiums | |
| CN104561546A (en) | Two-feeding-opening fully-loaded rare earth fractional extraction separation process method | |
| CN100584969C (en) | Technique for extraction separation of quadravalence cerium, thorium and cerium less tervalence rare earth from sulphuric acid rare earth solution | |
| CN104087748A (en) | Method for extracting and separating high-purity dysprosium oxide and terbium oxide from terbium-dysprosium rare earth enrichment matters | |
| CN105936977A (en) | P204 extraction separation method for preparing 5N neodymium | |
| CN112458319A (en) | Method for separating heavy rare earth elements based on ionic liquid extraction system | |
| CN105861824B (en) | A kind of solvent extraction prepares the separating technology of 5N terbiums | |
| CN106498193A (en) | A kind of packet separates the extracting process of three kinds of rare earths materials | |
| CN105861859B (en) | A kind of method that technical grade holmium raw material prepares 5N holmiums | |
| CN1101476C (en) | Process for producing high-purity lutetium oxide by extracting separation method | |
| CN1044409A (en) | Solvent extraction | |
| CN1086424C (en) | Process for producing rare-earth with various kinds of pureness specifications by separation method | |
| CN1257291C (en) | A process for enriching and preparing high-purity scandium by substituting alkoxyl for acetic acid as extractant | |
| CN1109103A (en) | Impregnation process for separation of cerium oxide and mixed low-cerium rare earth elements | |
| CN1049695C (en) | Method for purifying noble metal with double function extracting agent containing nitrogen and phosphorus | |
| CN113234923B (en) | Method for preparing high-purity hafnium oxide by extracting and separating zirconium and hafnium with solvent | |
| CN1127791A (en) | Method for enriching and making high purity scandium from rare-earth mixture contg. Sc | |
| CN1042570A (en) | High-purity terbium oxide preparation by use of fractional extraction method | |
| CN1651335A (en) | Method for producing strontium inorganic salt by utilizing high barium and high calcium celestite | |
| CN1015801B (en) | Preparation method of high purity yttrium oxide and lanthanum oxide | |
| CN1058994A (en) | One-step method for extracting and separating pure yttrium, crude erbium and heavy rare earth | |
| CN1061246A (en) | The method of extracting and separating zirconium from Scium trioxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CX01 | Expiry of patent term |
Granted publication date: 20000719 |
|
| EXPY | Termination of patent right or utility model |