SU1370076A1 - Method of extracting rare-earth elements from sulfate solutions - Google Patents

Method of extracting rare-earth elements from sulfate solutions Download PDF

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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
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USSR - Soviet Union
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extraction
earth elements
solution
chloride
extracting rare
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SU864029656A
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Russian (ru)
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Иван Алексеевич Шевчук
Андрей Яковлевич Махно
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Донецкий государственный университет
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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

1P

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)

Формула изобре.тени Formula invented 1 , Способ извлечени  редкоземельных элементов из сульфатных растводс , ров экстракцией растворами солей алкиламмони  в органических растворител х , отличающийс  тем, что, с целью повьш)ени  полноты извлечени , в исходном растворе под40 держивают концентрацию сульфат-ионов 0,05-0,3 М и экстракцию ведут раствором хлорида триметилалкиламмони , где алкил -С,, -С,д при корректируемом значении рН равновесной водной фазы1, A method for extracting rare earth elements from sulphate solutions, extraction with solutions of alkylammonium salts in organic solvents, characterized in that, in order to increase the completeness of extraction, the concentration of sulphate ions in the initial solution is 0.05-0.3 M and extraction is carried out with a solution of trimethylalkylammonium chloride, where alkyl is -C ,, -C, d with a corrected pH value of the equilibrium aqueous phase 45 9,5-11,5,45 9.5-11.5, 2. Способ ПОП.1, отличающийс  тем, что экстракцию ведут с использованием в качестве растворителей хлороформа, метилизобутилке50 тона или толуола с добавкой гептанола в соотношении спирт:растворитель 1:(4-6).2. Method POP.1, characterized in that the extraction is carried out using chloroform, methyl isobutyl 50 tones or toluene with the addition of heptanol in the ratio of alcohol: solvent 1: (4-6) as solvents. ЗкгтZkgt Мотнлтриоктил мнпииП хлорид (ичвеггныЛ )Motnltrioktil MPnI chloride (ichlorbyl) ЗкгтрагентPartner Триметилгексадецилшммоннй хлорид (предлагаемьЛ спосоО)Trimethylhexadecylsmonium Chloride (suggested as LOS) Степень извлечени , ZRecovery rate, z РЗЭ FP(III) V(V) Ti(IV) Zr(IV) РЗЭ FeCIII) V(V) Ti(IV) 2r(IV)REE FP (III) V (V) Ti (IV) Zr (IV) REE FeCIII) V (V) Ti (IV) 2r (IV) 66 1one tltl 1one itit 99 99 I «.199 99 I ".1 «1"one 1one 95 95 95 6295 95 95 62 4040 1one 1one 1one -cl-cl 56 8156 81 1one II -1 1-eleven
SU864029656A 1986-01-20 1986-01-20 Method of extracting rare-earth elements from sulfate solutions SU1370076A1 (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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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