SU1370076A1 - Method of extracting rare-earth elements from sulfate solutions - Google Patents
Method of extracting rare-earth elements from sulfate solutions Download PDFInfo
- Publication number
- SU1370076A1 SU1370076A1 SU864029656A SU4029656A SU1370076A1 SU 1370076 A1 SU1370076 A1 SU 1370076A1 SU 864029656 A SU864029656 A SU 864029656A SU 4029656 A SU4029656 A SU 4029656A SU 1370076 A1 SU1370076 A1 SU 1370076A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- extraction
- earth elements
- solution
- chloride
- extracting rare
- Prior art date
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 7
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 title claims abstract description 4
- 238000000605 extraction Methods 0.000 claims abstract description 11
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract 3
- 125000000217 alkyl group Chemical group 0.000 claims abstract 2
- 239000008346 aqueous phase Substances 0.000 claims abstract 2
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 229910021653 sulphate ion Inorganic materials 0.000 claims description 3
- 125000005210 alkyl ammonium group Chemical group 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 3
- -1 sulphate ions Chemical class 0.000 claims 2
- 239000003960 organic solvent Substances 0.000 claims 1
- 238000011084 recovery Methods 0.000 claims 1
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 abstract 1
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- 229910052720 vanadium Inorganic materials 0.000 description 8
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 229910052726 zirconium Inorganic materials 0.000 description 7
- 239000000203 mixture Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 3
- 239000012074 organic phase Substances 0.000 description 3
- YVBCULSIZWMTFY-UHFFFAOYSA-N Heptan-4-ol Chemical compound CCCC(O)CCC YVBCULSIZWMTFY-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- AZCDFTXEUCARGI-UHFFFAOYSA-M heptadecyl(trimethyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCC[N+](C)(C)C AZCDFTXEUCARGI-UHFFFAOYSA-M 0.000 description 1
- IXQWNVPHFNLUGD-UHFFFAOYSA-N iron titanium Chemical compound [Ti].[Fe] IXQWNVPHFNLUGD-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid group Chemical class S(O)(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- CEYYIKYYFSTQRU-UHFFFAOYSA-M trimethyl(tetradecyl)azanium;chloride Chemical compound [Cl-].CCCCCCCCCCCCCC[N+](C)(C)C CEYYIKYYFSTQRU-UHFFFAOYSA-M 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
Изобретение относитс к способам экстракции редкоземельных элементов и обеспечивает повышение полноты извлечени . Экстракцию ведут из раствора с содержанием сульфат- ионов 0,05-0,5 М раствором триметила- лкиламмони , где алкил при корректируемом значении рН равновесной водной фазы 9,5-11,5. В качестве растворител используют хлороформ, метилизобутилкетон или толуол с добавкой гейтанола в соотношении 1:4-6. 1 з.п. ф-лы, 1 табл.This invention relates to methods for extracting rare earth elements and provides for improved extraction completeness. Extraction is carried out from a solution with a sulfate-ion content of 0.05-0.5 M solution of trimethylalkylammonium, where alkyl is when the pH of the equilibrium aqueous phase is adjusted to pH 9.5-11.5. Chloroform, methyl isobutyl ketone or toluene with the addition of geithanol in a ratio of 1: 4-6 is used as a solvent. 1 hp f-ly, 1 tab.
Description
1П1P
Изобретение относитс к способу экстракции редкоземельных элементов из сульфатных растворов и может быть использовано при извлечении ценных компонентов из растворов, используемых в производстве, а также в аналитических цел х.The invention relates to a method for extracting rare earth elements from sulphate solutions and can be used in extracting valuable components from solutions used in production, as well as for analytical purposes.
Цель изобретени - повышение полноты извлечени .The purpose of the invention is to increase the completeness of extraction.
Пример 1. В делительную воронку вместимостью 100 см помещают 10 см 0,05 М раствора сульфата кали , содержащего 1 мг редкоземельных элементов, по 5 г железа, титана, ванади и циркони , и 10 см 0,05 М раствора хлорида триметилтетрадеци- ламмони в смеси толуола и пропано- ла 5:1. Устанавливают гидроксидом кали равновесное рН 9,5 и экстрагируют в течение 4 мин. После расслоени органическую фазу отдел ют. Реэкстракцию провод т растворами хлористоводородной, хлорной, азотной или серной кислот при равновесном рН 67. Атомно-абсорбционным.методом и химическим анализом установлено , что 97% редкоземельных элементов находитс в реэкстракте. Железо , титан, ванадий в экстракте не найдены,Example 1. In a separating funnel with a capacity of 100 cm, 10 cm of a 0.05 M solution of potassium sulfate containing 1 mg of rare earth elements, 5 g of iron, titanium, vanadium and zirconium, and 10 cm of a 0.05 M solution of trimethyltetradecylammonium chloride are placed a mixture of toluene and propanol 5: 1. The potassium hydroxide is adjusted to an equilibrium pH of 9.5 and extracted for 4 minutes. After separation, the organic phase is separated. The reextraction is carried out with solutions of hydrochloric, perchloric, nitric or sulfuric acids at an equilibrium pH of 67. The atomic absorption method and chemical analysis revealed that 97% of rare earth elements are in reextract. Iron, titanium, vanadium were not found in the extract,
Пример2. К10см 0,15М сульфата натри , содержащего 5 мг редкоземельных элементов по 5 мг елеза, титана, ванади и циркони , и 10 см 0.1 раствора хлорида три- метилгептадециламмони в смеси хлороформа и гептанола 5:1. Устанавливают гидроксидом натри равновесное рН 10,5 и экстрагируют 4 мин, В органическую фазу переходит 97% редкоземельных элементов. Железо, титан , ванадий и цирконий в экстракте не найдены.Example2. K10cm 0.15M sodium sulfate, containing 5 mg of rare earth elements, 5 mg each of iron, titanium, vanadium and zirconium, and 10 cm of a 0.1 solution of trimethylheptadecylammonium chloride in a mixture of chloroform and heptanol 5: 1. The sodium hydroxide is set at an equilibrium pH of 10.5 and extracted for 4 minutes. 97% of rare-earth elements pass into the organic phase. Iron, titanium, vanadium and zirconium were not found in the extract.
Примерз, К 10 см о,50 М сульфата аммони , содержащего 3 мг редкоземельных элементов по 5 мг железа, титана, ванади и циркони , и 10 см 0,1 М раствора триметил- октадеципаммони в смеси метилизобу тилкетона и гептанола 4:1, Экстрагируют при равновесном рН 11,5 4 мимPrimerz, K 10 cm o, 50 M ammonium sulfate, containing 3 mg of rare earth elements, 5 mg of iron, titanium, vanadium and zirconium, and 10 cm of a 0.1 M solution of trimethyl-octadecymonium in a mixture of methyl isobu tilketone and heptanol 4: 1, are extracted at an equilibrium pH of 11.5 4 mime
0076200762
В орг лническук фазу переходит 95% редкоземельных элементов. Железо титан , ванадий и цирконий в экстракте 95% of rare-earth elements pass into the organic phase. Iron titanium, vanadium and zirconium in the extract
, не обнаружены., not detected.
Добавка спирта сокращает врем расслоени фаз от 40 мин (в случае неразбавленно1 о разбавител ) до 20 мин при соотношении спирт:органичес10 кий разбавитель 1:8 и до 4 мин при соотношении спирт:органический разбавитель 1 : (4-6),The addition of alcohol reduces the phase separation time from 40 minutes (in the case of undiluted 1 about diluent) to 20 minutes with an alcohol: organic diluent ratio of 1: 8 and up to 4 minutes with an alcohol: organic diluent ratio of 1: (4-6),
Введение большего количества спирта ухудшает экстракцию при соот1Г ношении гептанол:хлороформ 1:3, в примере 2 извлечение редкоземельных элементов составл ет 85%, при соотношении 1:2 -40%.The introduction of a larger amount of alcohol impairs the extraction when heptanol: chloroform is 1: 3, and in example 2, the extraction of rare earth elements is 85%, with a ratio of 1: 2 to 40%.
В таблице приведены значени сте20 пени извлечени редкоземельных элементов железа, ванади , титана, циркони в зависимости от рН раствора дл предлагаемого способа и известного . Состав раствора до экстракции:The table shows the degree of extraction of rare-earth elements iron, vanadium, titanium, zirconium, depending on the pH of the solution for the proposed method and the known one. The composition of the solution before extraction:
25 редкоземельные элементы 0,5 г/л, железо, титан, ванадий, цирконий - по 1 г/л. Экстрагент - 0,1 М раствор соли алкиламмони в хлороформе +10 об.% гептанола.25 rare earth elements 0.5 g / l, iron, titanium, vanadium, zirconium - 1 g / l. Extractant - 0.1 M solution of alkylammonium salt in chloroform +10 vol.% Heptanol.
30thirty
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU864029656A SU1370076A1 (en) | 1986-01-20 | 1986-01-20 | Method of extracting rare-earth elements from sulfate solutions |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU864029656A SU1370076A1 (en) | 1986-01-20 | 1986-01-20 | Method of extracting rare-earth elements from sulfate solutions |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU1370076A1 true SU1370076A1 (en) | 1988-01-30 |
Family
ID=21223605
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU864029656A SU1370076A1 (en) | 1986-01-20 | 1986-01-20 | Method of extracting rare-earth elements from sulfate solutions |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU1370076A1 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140154155A1 (en) * | 2012-12-04 | 2014-06-05 | Lixivia, Inc. | Refining methods and agents for rare earth production |
| WO2014137238A1 (en) * | 2013-03-05 | 2014-09-12 | Opened Joint Stock Company "United Chemical Company Uralchem" | A method for re-extraction of rare-earth metals from organic solutions and preparing concentrate of rare-earth metals |
| US9631258B2 (en) | 2013-03-05 | 2017-04-25 | Opened Joint Stock Company “United Chemical Company Uralchem” | Methods for extracting rare-earth metals and preparing gypsum plaster from phosphogypsum hemihydrate |
| US9657371B2 (en) | 2013-03-05 | 2017-05-23 | Opened Joint-Stock Company “United Chemical Company Uralchem” | Methods for extracting rare-earth metals and preparing gypsum plaster from phosphogypsum hemihydrate |
| US10011891B2 (en) | 2013-03-18 | 2018-07-03 | Open Joint-Stock Company “United Chemical Company Uralchem” | Methods for concentrating rare-earth metals in phosphogypsum and removing thereof from wet process phosphoric acid |
-
1986
- 1986-01-20 SU SU864029656A patent/SU1370076A1/en active
Non-Patent Citations (1)
| Title |
|---|
| Авторское свидетельство ЧССР № 216101, кл. В 01 D 11/04, 1984. Патент US № 3259472, 23-312, 1966. Veno К., Saito А. Extraction of Rave .Elements in sulfate Solutions Analit. Chim. Acta, 1971, v.56, № 3, p.427. * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140154155A1 (en) * | 2012-12-04 | 2014-06-05 | Lixivia, Inc. | Refining methods and agents for rare earth production |
| US9499881B2 (en) * | 2012-12-04 | 2016-11-22 | Lixivia, Inc. | Refining methods and agents for rare earth production |
| WO2014137238A1 (en) * | 2013-03-05 | 2014-09-12 | Opened Joint Stock Company "United Chemical Company Uralchem" | A method for re-extraction of rare-earth metals from organic solutions and preparing concentrate of rare-earth metals |
| RU2538863C2 (en) * | 2013-03-05 | 2015-01-10 | Открытое акционерное общество "Объединенная химическая компания "УРАЛХИМ" | Re-extraction method of rare-earth metals from organic solutions and obtainment of concentrate from rare-earth metals |
| US9631258B2 (en) | 2013-03-05 | 2017-04-25 | Opened Joint Stock Company “United Chemical Company Uralchem” | Methods for extracting rare-earth metals and preparing gypsum plaster from phosphogypsum hemihydrate |
| US9657371B2 (en) | 2013-03-05 | 2017-05-23 | Opened Joint-Stock Company “United Chemical Company Uralchem” | Methods for extracting rare-earth metals and preparing gypsum plaster from phosphogypsum hemihydrate |
| US9896743B2 (en) | 2013-03-05 | 2018-02-20 | Opened Joint Stock Company “United Chemical Company Uralchem” | Method for re-extraction of rare-earth metals from organic solutions and preparing concentrate of rare-earth metals |
| US10011891B2 (en) | 2013-03-18 | 2018-07-03 | Open Joint-Stock Company “United Chemical Company Uralchem” | Methods for concentrating rare-earth metals in phosphogypsum and removing thereof from wet process phosphoric acid |
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