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SU1551653A1 - Method of obtaining powder-like lithium and yttrium double fluoride - Google Patents

Method of obtaining powder-like lithium and yttrium double fluoride Download PDF

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Publication number
SU1551653A1
SU1551653A1 SU874375314A SU4375314A SU1551653A1 SU 1551653 A1 SU1551653 A1 SU 1551653A1 SU 874375314 A SU874375314 A SU 874375314A SU 4375314 A SU4375314 A SU 4375314A SU 1551653 A1 SU1551653 A1 SU 1551653A1
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SU
USSR - Soviet Union
Prior art keywords
yttrium
lithium
product
fluorides
nitrates
Prior art date
Application number
SU874375314A
Other languages
Russian (ru)
Inventor
Евгения Ивановна Мельниченко
Тамара Александровна Калачева
Original Assignee
Институт Химии Дальневосточного Отделения Ан Ссср
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Priority to SU874375314A priority Critical patent/SU1551653A1/en
Application granted granted Critical
Publication of SU1551653A1 publication Critical patent/SU1551653A1/en

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/30Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
    • C01F17/36Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 halogen being the only anion, e.g. NaYF4

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

Изобретение относитс  к способам получени  соединени  LIYF4 и позвол ет сократить длительность процесса. К смеси карбонатов, хлоридов или нитратов иттри  и лити  в мольном соотношении Y:LI=1:(1,5-1,7) добавл ют концентрированную фтористоводородную кислоту с избытком 9,4-32,8% от теоретически необходимого количества дл  перевода исходных соединений во фториды, продукт спекают при 400-500°С, отмывают последовательно концентрированной азотной кислотой и водой и сушат. Перед сушкой продукт обрабатывают этиловым спиртом. Длительность способа по сравнению с прототипом сокращаетс  в 24 раза. 1 з.п.ф-лы.The invention relates to methods for producing the compound LIYF 4 and reduces the processing time. To a mixture of yttrium and lithium carbonates, chlorides or nitrates in a molar ratio of Y: LI = 1: (1.5-1.7) is added concentrated hydrofluoric acid with an excess of 9.4-32.8% of the theoretically required amount for transferring the original compounds in fluorides, the product is sintered at 400-500 ° C, washed sequentially with concentrated nitric acid and water and dried. Before drying, the product is treated with ethyl alcohol. The duration of the method compared with the prototype is reduced by 24 times. 1 hp ff.

Description

Изобретение относитс  к способам получени  фторидов редкоземельных и щелочных металлов, которые могут быть использованы в лазерной технике.The invention relates to methods for producing rare earth and alkali metal fluorides, which can be used in laser technology.

Целью изобретени   вл етс  сокращение длительности процесса.The aim of the invention is to reduce the duration of the process.

Пример 1. Берут 5,0 г Y2(C03V ЗН20 ХЧ 1 и 1,35 г Li2C03 ОСЧ. Соотношение иттри  и лити  составл ет 1:1,5. Перемешивают, добавл ют 7,0 мл HF, что на 0,6 мм или на Э,% превышает необходимое количество дл  привода карбонатов во фториды . Тигель со смесью накрывают крышкой , в течение 1 ч поднимают температуру до 500°С. Спекают смесь в течение 5 ч. Спек легко рассыпаетс  в порошок: примесь LiF отмывают 50 мл концентрированной азотной кислоты водой до рН 6-7 и 10 мл этилового спирта . Сушат продукт при 120°С в течечие 2 ч. Получают U,Об г LiYF4. Выход 99,6/;.Example 1. Take 5.0 g of Y2 (C03V ЗН20 ХЧ 1 and 1.35 g of Li2C03 OCC. The ratio of yttrium and lithium is 1: 1.5. Mix 7.0 ml of HF, which is 0.6 mm or by% exceeds the required amount to drive carbonates to fluorides. The crucible with the mixture is covered with a lid, the temperature is raised to 500 ° C for 1 hour, the mixture is sintered for 5 hours. nitric acid with water to a pH of 6-7 and 10 ml of ethyl alcohol.The product is dried at 120 ° C for 2 h. U, About g LiYF4 is obtained.

Пример 2. Ведут процесс в услови х примера 1, но с добавкой 8,6 мл HF, что на 2,1 мл или 32,8% превышает необходимый расход кислоты дл  образовани  фторидов. Спекание ведут при 50ЙГ. Выход продукта 99,8.Example 2. The process is carried out under the conditions of example 1, but with the addition of 8.6 ml of HF, which is 2.1 ml or 32.8% higher than the required acid consumption for the formation of fluorides. Sintering is carried out at 50JG. The product yield is 99.8.

Длительность СПРКЭНИЯ 6 ч, сушки 2 ч.Duration SPR. 6 h, drying 2 h.

П р и м е р 3. В услови х примера 1, но с использованием хлоридов ҐС1з-6,95НгО и LiCl-1,25HaO получают продукт с выходом 99,65. Длительность спекани  5 ч, сушки 2 ч.EXAMPLE 3 Under the conditions of Example 1, but using the chlorides ҐC1-6.95HgO and LiCl-1.25HaO, the product is obtained with a yield of 99.65. The duration of sintering 5 hours, drying 2 hours

Пример. В услови х примера 1, но с использованием нитратов Y(NOj}3- 6H2U и получают продукт с выходом 99,В/ . Длительность спекани  6 ч, сушки 2 ч.Example. Under the conditions of Example 1, but using Y nitrates (NOj} 3-6H2U, the product is obtained with the yield 99, V /. Sintering time is 6 hours, drying is 2 hours.

елate

СПSP

3535

СЛSL

0000

Пример 5. В услови х примера 1 ведут процесс при соотношении Y:Li 1:1,7 и температуре спекани  400°С. Длительность спекани  6 ч, сушки 2 ч.Example 5. Under the conditions of Example 1, the process is conducted at a Y: Li ratio of 1: 1.7 and a sintering temperature of 400 ° C. The duration of sintering 6 hours, drying 2 hours

По сравнению с известным способом, достигаетс  сокращение времени синтеза в 2 раза, процесс осуществл етс  при более низкой температуре и/не требует наличи  вакуума или инертной атмосферы.Compared with the known method, the synthesis time is reduced by 2 times, the process is carried out at a lower temperature and / does not require the presence of a vacuum or inert atmosphere.

Claims (2)

Формула изобретени  1. Способ получени  порошкообразного двойного фторида лити  и иттри  LiYF термообработкой иттрий- и ли- тийсодержащих соединений, отличающийс  тем, что, с целью сокращени  длительности процесса, в качестве исходных соединений берутClaim 1. A method for producing powdered lithium fluoride double and yttrium LiYF by heat treatment of yttrium- and lithium-containing compounds, characterized in that, in order to reduce the process time, as starting compounds карбонаты, хлориды или нитраты иттри  и лити  в мол рном соотношении Y:Li « 1:(1,5-1,7), лобавл ют к смеси концентрированную фтористоводородную кислоту с избытком 9| 32|Р % от теоретически необходимого количества дл  привода исходных соединений во фториды , продукт спекают при 00-500 С, отмывают последовательно концентрированной азотной кислотой и водой иyttrium and lithium carbonates, chlorides or nitrates in a molar ratio of Y: Li "1: (1.5-1.7), add to the mixture concentrated hydrofluoric acid with an excess of 9 | 32 | P% of the theoretically required amount to drive the starting compounds into fluorides, the product is sintered at 00-500 ° C, washed sequentially with concentrated nitric acid and water and 5 сушат.5 dried. 2. Способ по п.1,отличаю- щ и и с   тем, что перед сушкой продукт обрабатывают этиловым спиртом.2. The method according to claim 1, characterized by the fact that before drying the product is treated with ethyl alcohol.
SU874375314A 1987-12-30 1987-12-30 Method of obtaining powder-like lithium and yttrium double fluoride SU1551653A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SU874375314A SU1551653A1 (en) 1987-12-30 1987-12-30 Method of obtaining powder-like lithium and yttrium double fluoride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
SU874375314A SU1551653A1 (en) 1987-12-30 1987-12-30 Method of obtaining powder-like lithium and yttrium double fluoride

Publications (1)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1759765A1 (en) * 2005-09-01 2007-03-07 Ludwig-Maximilians-Universität München Solutions of anhydrous lanthanide salts and its preparation
RU2494416C2 (en) * 2008-03-24 2013-09-27 Токуяма Корпорейшн Scintillator for detecting neutrons and neutron detector

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Thoma R.E., Weaver С.Г., Friedman Н.А. Phase equilibria in the system LiF-YE,.- Phys. Chen. 1961, v. 65, N 7, P. 1096-1039. ( СПОСОБ ПОЛУЧЕНИЯ ПОРОШКООБРАЗНОГО ДВОЙНОГО ФТОРИДА ЛИТИЯ И ИТТРИЯ *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1759765A1 (en) * 2005-09-01 2007-03-07 Ludwig-Maximilians-Universität München Solutions of anhydrous lanthanide salts and its preparation
WO2007026014A1 (en) * 2005-09-01 2007-03-08 Ludwig-Maximilians-Universitaet Muenchen Solutions of anhydrous lanthanide salts and its preparation
CN101277763B (en) * 2005-09-01 2012-08-22 慕尼黑路德维格-马克西米利安斯大学 Solutions of anhydrous lanthanide salts and its preparation
RU2494416C2 (en) * 2008-03-24 2013-09-27 Токуяма Корпорейшн Scintillator for detecting neutrons and neutron detector

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