RU2060944C1 - Method for isolation of europium from mixture of rare-earth elements - Google Patents
Method for isolation of europium from mixture of rare-earth elements Download PDFInfo
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- RU2060944C1 RU2060944C1 RU9292001109A RU92001109A RU2060944C1 RU 2060944 C1 RU2060944 C1 RU 2060944C1 RU 9292001109 A RU9292001109 A RU 9292001109A RU 92001109 A RU92001109 A RU 92001109A RU 2060944 C1 RU2060944 C1 RU 2060944C1
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- RU
- Russia
- Prior art keywords
- europium
- earth elements
- mixture
- rare
- isolation
- Prior art date
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- 229910052693 Europium Inorganic materials 0.000 title claims abstract description 22
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 15
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 11
- 239000000203 mixture Substances 0.000 title claims description 5
- 238000002955 isolation Methods 0.000 title description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 5
- 229910052731 fluorine Inorganic materials 0.000 claims description 3
- 239000011737 fluorine Substances 0.000 claims description 3
- -1 fluorine ions Chemical class 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000003929 acidic solution Substances 0.000 claims 1
- 239000012141 concentrate Substances 0.000 claims 1
- MGVUQZZTJGLWJV-UHFFFAOYSA-N europium(2+) Chemical compound [Eu+2] MGVUQZZTJGLWJV-UHFFFAOYSA-N 0.000 claims 1
- LNBHUCHAFZUEGJ-UHFFFAOYSA-N europium(3+) Chemical compound [Eu+3] LNBHUCHAFZUEGJ-UHFFFAOYSA-N 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 abstract description 9
- 239000002244 precipitate Substances 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract description 2
- 238000000605 extraction Methods 0.000 abstract description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 abstract 2
- 239000004411 aluminium Substances 0.000 abstract 1
- 235000013024 sodium fluoride Nutrition 0.000 abstract 1
- 239000011775 sodium fluoride Substances 0.000 abstract 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 229910000497 Amalgam Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 150000001243 acetic acids Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 235000011167 hydrochloric acid Nutrition 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 235000016804 zinc Nutrition 0.000 description 1
Landscapes
- Removal Of Specific Substances (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
Изобретение относится к химической технологии редкоземельных элементов и может быть использовано в производстве продуктов европия. The invention relates to the chemical technology of rare earth elements and can be used in the manufacture of europium products.
Известны способы выделения европия, основанные на восстановлении его до двухвалентного состояния в растворах солей смеси РЗЭ и последующем отделении в виде труднорастворимого осадка [1,2]
Недостатками используемых химических методов выделения европия из смеси РЗЭ являются необходимость применения дорогостоящих и токсичных реагентов (ртуть, свинец, цинк, соляная и уксусная кислоты), сложность оборудования, проблема утилизации жидких сбросов, содержащих хлор, цинк и др.Known methods for the separation of europium, based on the restoration of it to a divalent state in solutions of salts of a mixture of REE and subsequent separation in the form of a sparingly soluble precipitate [1,2]
The disadvantages of the chemical methods used to isolate europium from the REE mixture are the need for expensive and toxic reagents (mercury, lead, zinc, hydrochloric and acetic acids), the complexity of the equipment, the problem of disposal of liquid effluents containing chlorine, zinc, etc.
Из металлов-восстановителей относительно дешев и нетоксичен алюминий. Of the reducing metals, aluminum is relatively cheap and non-toxic.
Метод с использованием алюминия для перевода европия в двухвалентное состояние [2] прост в осуществлении. The method using aluminum to transfer europium to the divalent state [2] is simple to implement.
Однако алюминий (в виде амальгамы) восстанавливает европий только в соляно-уксуснокислых растворах. Это ухудшает санитарные условия проведения процесса. However, aluminum (in the form of an amalgam) reduces europium only in hydrochloric acetic acid solutions. This affects the sanitary conditions of the process.
Предлагаемый способ позволяет избежать перечисленных недостатков известных химических методов выделения европия из смеси РЗЭ. The proposed method avoids the above disadvantages of the known chemical methods for the isolation of europium from a mixture of REE.
Сущность предлагаемого способа состоит в том, что европий восстанавливают металлическим алюминием (пыль, порошок, гранулы) в сернокислом растворе РЗЭ в присутствии фтор-ионов, вносимых в виде водорастворимых соединений, например NaF, NH4HF2, HF и др. На ход и показатели процесса влияют температура и рН среды, продолжительность агитации пульпы и соотношение вводимых алюминия и фтора.The essence of the proposed method consists in the fact that europium is reduced with aluminum metal (dust, powder, granules) in a sulfuric acid solution of REE in the presence of fluoride ions introduced in the form of water-soluble compounds, for example, NaF, NH 4 HF 2 , HF, etc. process indicators affect the temperature and pH of the medium, the duration of pulp agitation and the ratio of aluminum and fluorine introduced.
Предлагаемый метод дает возможность извлекать из суммы РЗЭ до 98,5% европия и получать продукт, содержащий до 99,9% европия. В зависимости от требований к качеству конечного продукта европия параметры процесса могут изменяться в следующих пределах: рН среды 0,1-5,0 Температура пульпы, оС 5-50
Количество вводимого
алюминия, от стехио- метрически необходимого 100-300
Количество вводимого
фтора от массы вводимого алюминия 0,045-0,45 Время агитации пульпы,ч 0,5-3,5
П р и м е р 1. В сернокислый раствор с концентрацией Н2SO4 24,5 г/дм3, РЗ2О3 100 г (в том числе 9,8 г европия) вносили 15 г алюминия (порошок, марка ПА-4) и 10 г NaF, затем перемешивали в течение 90 мин при комнатной температуре. Выход европия в отфильтрованный и отмытый осадок 98,1% содержание европия в сумме РЗ2O3 осадка 94,2%
П р и м е р 2. В аналогичный первому сернокислый раствор вносили 20 г алюминия и 10 г NaF, затем перемешивали в течение 1,5 ч при температуре 40оС. Выход европия в отфильтрованный и отмытый осадок составил 98,3% содержание европия в сумме РЗ2О3 осадка 98,5%
Полученные фильтраты использованы при изготовлении исходных растворов.The proposed method makes it possible to extract from the amount of REE up to 98.5% europium and obtain a product containing up to 99.9% europium. Depending on the quality requirements of the europium end product, process parameters can vary in the following ranges: pH of the medium 0.1-5.0 Pulp temperature, о С 5-50
The amount of input
aluminum, from stoichiometrically necessary 100-300
The amount of input
fluorine by weight of aluminum introduced 0.045-0.45 Pulp agitation time, h 0.5-3.5
PRI me R 1. In a sulfuric acid solution with a concentration of H 2 SO 4 24.5 g / DM 3 , RE 2 About 3 100 g (including 9.8 g of europium) was made 15 g of aluminum (powder, grade PA -4) and 10 g of NaF, then stirred for 90 min at room temperature. The output of europium in the filtered and washed precipitate 98.1% of the content of europium in the amount of RE 2 O 3 precipitate 94.2%
EXAMPLE EXAMPLE 2 In similar to the first sulfate solution was added 20 g of aluminum and 10 g of NaF, followed by stirring for 1.5 hours at 40 C. The yield of europium in the filtered and washed precipitate was 98.3% of the content of europium in the amount of RE 2 O 3 precipitate 98.5%
The obtained filtrates were used in the manufacture of stock solutions.
Таким образом, предлагаемый способ выделения европия из РЗЭ по сравнению с известными химическими методами позволяет повысить извлечение и качество европия, использовать более дешевые и менее токсичные реагенты, решить проблему утилизации жидких сбросов. Thus, the proposed method for the separation of europium from REE in comparison with known chemical methods can improve the extraction and quality of europium, use cheaper and less toxic reagents, and solve the problem of disposal of liquid effluents.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU9292001109A RU2060944C1 (en) | 1992-10-19 | 1992-10-19 | Method for isolation of europium from mixture of rare-earth elements |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| RU9292001109A RU2060944C1 (en) | 1992-10-19 | 1992-10-19 | Method for isolation of europium from mixture of rare-earth elements |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| RU92001109A RU92001109A (en) | 1995-03-27 |
| RU2060944C1 true RU2060944C1 (en) | 1996-05-27 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| RU9292001109A RU2060944C1 (en) | 1992-10-19 | 1992-10-19 | Method for isolation of europium from mixture of rare-earth elements |
Country Status (1)
| Country | Link |
|---|---|
| RU (1) | RU2060944C1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2349547C2 (en) * | 2007-04-16 | 2009-03-20 | Институт нефтехимии и катализа РАН | Method of producing europium dichloride |
| RU2471710C1 (en) * | 2011-05-31 | 2013-01-10 | Учреждение Российской Академии Наук Институт Нефтехимии И Катализа Ран | Method of obtaining compounds of divalent lanthanides |
-
1992
- 1992-10-19 RU RU9292001109A patent/RU2060944C1/en active
Non-Patent Citations (1)
| Title |
|---|
| 1. Химия и технология редких и рассеянных элементов. / Под ред. К.А.Большакова. М.: Высшая школа, 1976, ч.II, с.114-117. 2. Серебренников В.В. Редкоземельные элементы. Томск: изд-во Томского государственного университета, 1961, т.2, с.407. * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2349547C2 (en) * | 2007-04-16 | 2009-03-20 | Институт нефтехимии и катализа РАН | Method of producing europium dichloride |
| RU2471710C1 (en) * | 2011-05-31 | 2013-01-10 | Учреждение Российской Академии Наук Институт Нефтехимии И Катализа Ран | Method of obtaining compounds of divalent lanthanides |
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