RU2295495C1 - COMPOUND KSc2F7 PREPARATION METHOD - Google Patents
COMPOUND KSc2F7 PREPARATION METHOD Download PDFInfo
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- RU2295495C1 RU2295495C1 RU2005133506/15A RU2005133506A RU2295495C1 RU 2295495 C1 RU2295495 C1 RU 2295495C1 RU 2005133506/15 A RU2005133506/15 A RU 2005133506/15A RU 2005133506 A RU2005133506 A RU 2005133506A RU 2295495 C1 RU2295495 C1 RU 2295495C1
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- scandium
- ksc
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- molar ratio
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- 150000001875 compounds Chemical class 0.000 title claims description 14
- 238000002360 preparation method Methods 0.000 title abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 5
- 239000011591 potassium Substances 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 230000003993 interaction Effects 0.000 claims abstract description 4
- 150000003325 scandium Chemical class 0.000 claims abstract description 4
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 4
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 4
- 150000002910 rare earth metals Chemical class 0.000 abstract description 4
- 235000019441 ethanol Nutrition 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 238000003181 co-melting Methods 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000000921 elemental analysis Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- OEKDNFRQVZLFBZ-UHFFFAOYSA-K scandium fluoride Chemical compound F[Sc](F)F OEKDNFRQVZLFBZ-UHFFFAOYSA-K 0.000 description 3
- -1 fluoride ions Chemical class 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- FVIZARNDLVOMSU-UHFFFAOYSA-N ginsenoside K Natural products C1CC(C2(CCC3C(C)(C)C(O)CCC3(C)C2CC2O)C)(C)C2C1C(C)(CCC=C(C)C)OC1OC(CO)C(O)C(O)C1O FVIZARNDLVOMSU-UHFFFAOYSA-N 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
Description
Изобретение относится к неорганической химии редкоземельных металлов, в частности к неорганической химии скандия.The invention relates to inorganic chemistry of rare earth metals, in particular to inorganic chemistry of scandium.
Известен способ получения соединения KSc2F7 твердофазным синтезом из оксида или фторида скандия и фторида или гидродифторида калия (Sobolev B.P. / The Rare Earth Trifluorides. Part 1. The high Temperature Chemistry of the Rare Earth Trifluorides. Institute of Cristallography. Moscow. Russia. Institute d'Estudis Catalans. Barselona. Spain. 2000. 520 p.). Недостатком данного метода является использование высокой температуры для синтеза указанного соединения. Данные о синтезе этого соединения в растворе в известной литературе отсутствуют. Этот способ принят за прототип.A known method of producing compounds KSc 2 F 7 by solid phase synthesis from scandium oxide or fluoride and potassium fluoride or hydrodifluoride (Sobolev BP / The Rare Earth Trifluorides. Part 1. The high Temperature Chemistry of the Rare Earth Trifluorides. Institute of Cristallography. Moscow. Russia. Institute d'Estudis Catalans. Barselona. Spain. 2000.520 p.). The disadvantage of this method is the use of high temperature for the synthesis of this compound. There are no data on the synthesis of this compound in solution in the known literature. This method is adopted as a prototype.
С целью упрощения разработан способ получения соединения KSc2F7, включающий взаимодействие между раствором соли скандия и твердым гидродифторидом калия при комнатной температуре. При этом для концентрации скандия в растворе 0,6 моль/л мольное отношение F:Sc (n) должно составлять от 5 до 9. Установлено, что в случае n=4 получается смесь фторида скандия и KSc2F7, при n≤3 фторид скандия. При значении n=10-12 продуктом является соединение K5Sc3F14. Предлагаемый способ позволяет исключить операцию сплавления, т.е. упростить синтез соединения.In order to simplify, a method has been developed for the preparation of KSc 2 F 7 , which includes the interaction between a solution of scandium salt and solid potassium hydrodifluoride at room temperature. Moreover, for a concentration of scandium in a solution of 0.6 mol / L, the molar ratio F: Sc (n) should be from 5 to 9. It was found that in the case n = 4 a mixture of scandium fluoride and KSc 2 F 7 is obtained, with n≤3 scandium fluoride. When n = 10-12, the product is a compound K 5 Sc 3 F 14 . The proposed method eliminates the fusion operation, i.e. simplify the synthesis of the compound.
Пример 1. К раствору ScCl3 с концентрацией 0,6 моль/л объемом 100 мл добавили при перемешивании 11,7 г твердого KHF2 для получения мольного отношения F:Sc=5. Смесь выдержали при перемешивании 30 мин. Получили гель, занимающий весь объем сосуда, разделение фаз в котором самопроизвольно достигается в течение нескольких месяцев. Осадок промыли дистиллированной водой, этиловым спиртом, просушили и прокалили при температуре 300°С до постоянного веса. Потери при прокаливании составили 1%.Example 1. To a solution of ScCl 3 with a concentration of 0.6 mol / L, a volume of 100 ml was added with stirring 11.7 g of solid KHF 2 to obtain a molar ratio F: Sc = 5. The mixture was kept under stirring for 30 minutes. Got a gel that occupies the entire volume of the vessel, the phase separation in which spontaneously is achieved within a few months. The precipitate was washed with distilled water, ethyl alcohol, dried and calcined at a temperature of 300 ° C to constant weight. Loss on ignition was 1%.
По данным рентгенофазового анализа (РФА) полученное вещество представляет собой соединение KSc2F7, имеющее орторомбическую кристаллическую решетку с параметрами решетки, которые приведены в работе [1]. Результаты элементного анализа (рентгеноспектральный метод, позволяющий определять элементы от бора до урана при их присутствии в образце с максимальной ошибкой 0,3%) даны в таблице. Разность в содержании элементов по сравнению с расчетными значениями для этого соединения в опыте 1 связана, по-видимому, с захватом ионов калия и фтора, а также гидрофторид-иона, входящих в состав осадителя, из маточного раствора из-за низкой эффективности отмывки полученного студенистого осадка.According to x-ray phase analysis (XRD), the resulting substance is a compound KSc 2 F 7 having an orthorhombic crystal lattice with lattice parameters that are given in [1]. The results of elemental analysis (X-ray spectral method, which allows to determine elements from boron to uranium when they are present in the sample with a maximum error of 0.3%) are given in the table. The difference in the content of elements compared with the calculated values for this compound in experiment 1 is apparently associated with the capture of potassium and fluoride ions, as well as hydrofluoride ions, which are part of the precipitator, from the mother liquor due to the low washing efficiency of the gelatinous draft.
Пример 2. Эксперимент проводили, как в примере 1, но использовали мольное отношение F:Sc=4. Продуктом, по данным РФА и элементного анализа (таблица), является смесь соединений KSc2F7 и фторида скандия.Example 2. The experiment was carried out as in example 1, but used the molar ratio F: Sc = 4. The product, according to the XRD and elemental analysis (table), is a mixture of compounds KSc 2 F 7 and scandium fluoride.
Пример 3. Эксперимент проводили, как в примере 1, но мольное отношение F:Sc равнялось 10. Получен кристаллический осадок, который, по данным РФА, представляет собой соединение состава K5Sc3F14.Example 3. The experiment was carried out as in example 1, but the molar ratio F: Sc was 10. A crystalline precipitate was obtained, which, according to the XRD data, was a compound of the composition K 5 Sc 3 F 14 .
Пример 4. Эксперимент проводили, как в примере 1, но использовали мольное отношение F:Sc=9. Продуктом, по данным РФА, является соединение KSc2F7.Example 4. The experiment was carried out as in example 1, but used the molar ratio F: Sc = 9. The product, according to the XRD, is a compound KSc 2 F 7 .
Пример 5. Эксперимент проводили, как в примере 1, но мольное отношение F:Sc равнялось 12. Получен кристаллический осадок, который, по данным РФА и элементного анализа, представляет собой соединение состава K5Sc3F14.Example 5. The experiment was carried out as in example 1, but the molar ratio F: Sc was 12. A crystalline precipitate was obtained, which, according to XRD and elemental analysis, was a compound of the composition K 5 Sc 3 F 14 .
Результаты опытов и характеристики твердых фаз представлены в таблице.The experimental results and characteristics of the solid phases are presented in the table.
При другом значении концентрации соли скандия интервал мольных отношений F:Sc может быть другим. Например, при концентрации ScCl3 0,3 моль/л и n=12 получено соединение KSc2F7. Более подробно этот вопрос не изучен.For a different concentration of scandium salt, the range of the molar ratio F: Sc may be different. For example, at a concentration of ScCl 3 of 0.3 mol / L and n = 12, the compound KSc 2 F 7 was obtained. This issue has not been studied in more detail.
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| Application Number | Priority Date | Filing Date | Title |
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| RU2005133506/15A RU2295495C1 (en) | 2005-11-01 | 2005-11-01 | COMPOUND KSc2F7 PREPARATION METHOD |
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| RU2005133506/15A RU2295495C1 (en) | 2005-11-01 | 2005-11-01 | COMPOUND KSc2F7 PREPARATION METHOD |
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| RU2295495C1 true RU2295495C1 (en) | 2007-03-20 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305222A (en) * | 2013-06-18 | 2013-09-18 | 南京大学 | KSc2F7: yb, preparation method and application of Er up-conversion fluorescent nanorods |
| CN105238405A (en) * | 2015-10-30 | 2016-01-13 | 中国科学院福建物质结构研究所 | Method for improving luminous intensity of rare earth ion co-doped up-conversion nano material |
| CN110204209A (en) * | 2019-05-08 | 2019-09-06 | 杭州电子科技大学 | A kind of upper conversion glass ceramic composite material of the rear-earth-doped scandium base fluorinated nano crystalline substance of selectivity |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2037548C1 (en) * | 1992-05-20 | 1995-06-19 | Юлия Васильевна Соколова | Method to produce scandium fluoride product from solutions or pulps of complex salt composition |
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2005
- 2005-11-01 RU RU2005133506/15A patent/RU2295495C1/en not_active IP Right Cessation
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2037548C1 (en) * | 1992-05-20 | 1995-06-19 | Юлия Васильевна Соколова | Method to produce scandium fluoride product from solutions or pulps of complex salt composition |
Non-Patent Citations (2)
| Title |
|---|
| GUEDE, KLAUS et al, The crystal of potassium heptafluorodiscandate, (реферат), Zeitschrift fuer Naturforschung, Teil B: Anorganische Chemie, Ordanische Cheme, 40B(6), 726-729, 1985. CHAMPARNAUD-MESSARD, JEAN CLAUDE et al, The univalent metal (M) fluoride-scandium fluoride systems (M = lithium, sodium, potassium, rubidium, cesium, thallium, ammonium), (реферат). Journal of the Less-Common Metals, 167(2), 319-327, 1991. * |
| SOBOLEV В.Р., The Rare Earth Trifluorides, The high Temperature Chemistry of the Rare Earth Trifluorides, Institute d'estudis Catalans, Barselona, part 1, 2000, p.182-237. * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305222A (en) * | 2013-06-18 | 2013-09-18 | 南京大学 | KSc2F7: yb, preparation method and application of Er up-conversion fluorescent nanorods |
| CN103305222B (en) * | 2013-06-18 | 2014-11-26 | 南京大学 | KSc2F7: yb, preparation method and application of Er up-conversion fluorescent nanorods |
| CN105238405A (en) * | 2015-10-30 | 2016-01-13 | 中国科学院福建物质结构研究所 | Method for improving luminous intensity of rare earth ion co-doped up-conversion nano material |
| CN110204209A (en) * | 2019-05-08 | 2019-09-06 | 杭州电子科技大学 | A kind of upper conversion glass ceramic composite material of the rear-earth-doped scandium base fluorinated nano crystalline substance of selectivity |
| CN110204209B (en) * | 2019-05-08 | 2022-01-04 | 杭州电子科技大学 | Up-conversion glass ceramic composite material of selective rare earth doped scandium-based fluorinated nanocrystalline |
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