SU827398A1 - Method of producing anhydrous light lanthanides tribromides - Google Patents
Method of producing anhydrous light lanthanides tribromides Download PDFInfo
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- SU827398A1 SU827398A1 SU792730803A SU2730803A SU827398A1 SU 827398 A1 SU827398 A1 SU 827398A1 SU 792730803 A SU792730803 A SU 792730803A SU 2730803 A SU2730803 A SU 2730803A SU 827398 A1 SU827398 A1 SU 827398A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- tribromides
- producing anhydrous
- anhydrous light
- lanthanides
- light lanthanides
- Prior art date
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/253—Halides
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Insulating Materials (AREA)
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Description
обезвоживани гидратированных трибромидов редкоземельных элементов (РЗЭ) затрачивают 2-2,5 ч. Температуру в печи 630-650°С выдерживают около 1 ч, затем печь опускают и охлаждают ампулу до комнатной температуры (при посто нном токе азота). Далее ампулу извлекают, закрывают пробками на шлифах и перенос т в сухой бокс, наполненный азотом. Максимальна температура синтеза не должна превышать разницу от точки плавлени получаемого трибромида лантанида в 30-40°С и тем более не должна превышать его температуру плавлени .dehydration of hydrated rare earth elements (REE) spend 2-2.5 hours. The furnace temperature is 630-650 ° C for about 1 hour, then the furnace is lowered and the ampoule is cooled to room temperature (with constant nitrogen flow). Next, the ampoule is removed, sealed with plugs on thin sections, and transferred to a dry box filled with nitrogen. The maximum synthesis temperature should not exceed the difference from the melting point of the lanthanide tribromide obtained in 30-40 ° C and, moreover, should not exceed its melting point.
Способ позвол ет за один цикл (6- 6,5 ч) пробромировать до 35 г окиси РЗЭ и получить безводные трибромиды легких лантанидов с выходом 90-93%, что обеспечивает преимущество предложенного способа перед известным.The method allows for one cycle (6-6.5 h) to sample up to 35 g of REE oxide and to obtain anhydrous light lanthanide tribromides with a yield of 90-93%, which provides the advantage of the proposed method over the known one.
Пример. 30,50 г окиси празеодима РгбОц марки Про-1 в виде порошка загружают в коническую колбу, куда затем нриливают 95 мл концентрированной НВг (d 1,486) марки ЧДА (ГОСТ 2062-67). Содержимое колбы слегка нагревают до начала бурного выделени брома. После растворени оКИси гор чий раствор фильтруют (если есть нерастворимый осадок) и упаривают до половины. Затем упаренный раствор церенос т в двухгорлую ампулу (заполненную перекристаллизованным и сухим NH4Br, вз тым в количестве 24,40 г. Далее собирают установку синтеза и провод т все вышеуказанные операции. Максимальна температура синтеза 650°С. Весь цикл вместе с охлаждением занимает 5,5-6,0 ч. Выход 64,20 г (94,1%). Образец полученного трибромида празеодима моментально и полностью раствор етс в воде, что указывает на отсутствие в нем оксибромида.Example. 30.50 g of praseodymium oxide Prod-1 PbsoC in powder form is loaded into a conical flask, to which 95 ml of concentrated NVB (d 1.486) of analytical grade (GOST 2062-67) is then poured. The contents of the flask are heated slightly until the onset of rapid release of bromine. After the oxide dissolves, the hot solution is filtered (if there is an insoluble precipitate) and evaporated to half. Then one stripped off solution is transferred to a two-neck ampoule (filled with recrystallized and dry NH4Br, taken in an amount of 24.40 g. Next, a synthesis unit is assembled and all of the above operations are performed. The maximum synthesis temperature is 650 ° C. 5-6.0 hours. Yield: 64.20 g (94.1%). A sample of praseodymium tribromide obtained instantly and completely dissolved in water, which indicates the absence of oxybromide in it.
Найдено, %: Рг 37,00; Вг 63,00.Found,%: Pr 37.00; Br 63.00.
РгВг (3,0026).PrgVg (3.0026).
Вычислено, %: Рг 37,02; Вг 62,98.Calculated,%: Pr 37.02; Br 62.98.
Результаты спектрального анализа, %: Si , Fe 10-3-10- Mg 10- Мп 10 и менее; РЬ 10 и менее; Сг 10 ; AI 10-; Си 10, Со - не обнаружен (и. о.) при чувствительности Ni, Са и Ti не обнаружены .The results of spectral analysis,%: Si, Fe 10-3-10- Mg 10-Mp 10 or less; Pb 10 and less; Cr 10; AI 10-; Cu 10, Co - not detected (I. O.) at the sensitivity of Ni, Ca and Ti were not detected.
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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SU792730803A SU827398A1 (en) | 1979-02-26 | 1979-02-26 | Method of producing anhydrous light lanthanides tribromides |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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SU792730803A SU827398A1 (en) | 1979-02-26 | 1979-02-26 | Method of producing anhydrous light lanthanides tribromides |
Publications (1)
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SU827398A1 true SU827398A1 (en) | 1981-05-07 |
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SU792730803A SU827398A1 (en) | 1979-02-26 | 1979-02-26 | Method of producing anhydrous light lanthanides tribromides |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102502757A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Preparation of high-purity anhydrous lanthanum chloride or cerium chloride by programmed heating method |
CN102502755A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Preparation of high-purity anhydrous lanthanum bromide or cerium bromide with temperature programmed method |
CN102502756A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Preparation of high-purity anhydrous praseodymium chloride or neodymium chloride by programmed heating method |
-
1979
- 1979-02-26 SU SU792730803A patent/SU827398A1/en active
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102502757A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Preparation of high-purity anhydrous lanthanum chloride or cerium chloride by programmed heating method |
CN102502755A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Preparation of high-purity anhydrous lanthanum bromide or cerium bromide with temperature programmed method |
CN102502756A (en) * | 2011-10-28 | 2012-06-20 | 包头市京瑞新材料有限公司 | Preparation of high-purity anhydrous praseodymium chloride or neodymium chloride by programmed heating method |
CN102502755B (en) * | 2011-10-28 | 2013-07-03 | 包头市京瑞新材料有限公司 | Preparation of high-purity anhydrous lanthanum bromide or cerium bromide with temperature programmed method |
CN102502756B (en) * | 2011-10-28 | 2013-07-24 | 包头市京瑞新材料有限公司 | Preparation of high-purity anhydrous praseodymium chloride or neodymium chloride by programmed heating method |
CN102502757B (en) * | 2011-10-28 | 2013-08-14 | 包头市京瑞新材料有限公司 | Method for preparing high-purity anhydrous lanthanum chloride or cerium chloride by programmed heating method |
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