RU2040471C1 - Method of preparing 99%-th scandium oxide from the fluoride concentrate - Google Patents
Method of preparing 99%-th scandium oxide from the fluoride concentrate Download PDFInfo
- Publication number
- RU2040471C1 RU2040471C1 SU925049810A SU5049810A RU2040471C1 RU 2040471 C1 RU2040471 C1 RU 2040471C1 SU 925049810 A SU925049810 A SU 925049810A SU 5049810 A SU5049810 A SU 5049810A RU 2040471 C1 RU2040471 C1 RU 2040471C1
- Authority
- RU
- Russia
- Prior art keywords
- fluoride
- scandium
- solution
- scandium oxide
- concentrate
- Prior art date
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- HYXGAEYDKFCVMU-UHFFFAOYSA-N scandium oxide Chemical compound O=[Sc]O[Sc]=O HYXGAEYDKFCVMU-UHFFFAOYSA-N 0.000 title claims abstract description 7
- 239000012141 concentrate Substances 0.000 title claims abstract description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 title claims description 4
- 238000000034 method Methods 0.000 title abstract description 7
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract 2
- 229910052706 scandium Inorganic materials 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 238000002386 leaching Methods 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 3
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims 1
- OEKDNFRQVZLFBZ-UHFFFAOYSA-K scandium fluoride Chemical compound F[Sc](F)F OEKDNFRQVZLFBZ-UHFFFAOYSA-K 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 239000002244 precipitate Substances 0.000 abstract description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 2
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 abstract 2
- 235000013024 sodium fluoride Nutrition 0.000 abstract 1
- 239000011775 sodium fluoride Substances 0.000 abstract 1
- 229910017855 NH 4 F Inorganic materials 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 229910052726 zirconium Inorganic materials 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910052776 Thorium Inorganic materials 0.000 description 3
- 229910052770 Uranium Inorganic materials 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000005272 metallurgy Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 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
- 239000000203 mixture Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Landscapes
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
Изобретение относится к металлургии редких металлов, в частности к металлургии скандия. The invention relates to the metallurgy of rare metals, in particular to the metallurgy of scandium.
Наиболее близким к изобретению является способ получения оксида скандия с содержанием основного вещества более 99 мас. из фторидного концентрата (ФК), содержащего Sc, Th, Ti, Zr, Fe, Si и U, включающий выщелачивание ФК 15% -ным раствором NaOH при 75-90оС, растворение осадка гидроксидов при нагревании в растворе НCl с последующим двойным гидролитическим отделением примесей Ti, Zr, Si, Fe и Th, оксалатную очистку Sc от Fe и U, прокаливание оксалата Sc до Sc2O3, растворение Sc2O3 в растворе НСl, экстракционную очистку, осаждение Sc(OH)3 и его прокаливание до Sc2O3.Closest to the invention is a method for producing scandium oxide with a basic substance content of more than 99 wt. of fluoride concentrate (FC) containing Sc, Th, Ti, Zr, Fe, Si and U, comprising leaching FC 15% solution of NaOH at 75-90 ° C, dissolving the hydroxide precipitate by heating in HCl solution followed by hydrolytic double separation of Ti, Zr, Si, Fe, and Th impurities, oxalate purification of Sc from Fe and U, calcination of oxalate Sc to Sc 2 O 3 , dissolution of Sc 2 O 3 in HCl solution, extraction purification, precipitation of Sc (OH) 3 and its calcination up to Sc 2 O 3 .
Недостатком этого способа является его многостадийность. The disadvantage of this method is its multi-stage.
Задача изобретения создание более простого способа получения 99%-ного Sc2O3 из ФК за счет использования более эффективных операций очистки исходного концентрата.The objective of the invention is the creation of a simpler way to obtain 99% Sc 2 O 3 from FC through the use of more efficient operations for the purification of the initial concentrate.
Способ заключается в избирательном выщелачивании Sc из ФК раствором NH4F, осаждении Sc из раствора NH4F кристаллическим NaF в виде двойного фторскандиата или раствором НNO3 в виде фторида скандия, гидролизе двойного фторскандиата Na-NH4 (при использовании NaFкр) с получением фторида скандия и конверсие ScF3 в Sc2O3 при температуре ≥700оС в токе воздуха. Предлагаемый способ позволяет провести эффективное отделение Sc от примесей Са, Мg, Al, Ti, Y, РЗЭ, Zr, Na, U и Тh на стадии выщелачивания ФК раствором NH4F и дополнительно от Тi, Zr, U, Fe и Мg, образующих растворимые фторидные комплексы, при осаждении Sc из раствора NH4F в виде фтористых солей. Предлагаемый способ в отличие от прототипа позволяет провести получение 99%-ного Sc2O3 из ФК без вскрытия ФК, что иллюстрируется следующими примерами.The method consists in selectively leaching Sc from FC to a solution of NH 4 F, precipitating Sc from a solution of NH 4 F with crystalline NaF in the form of double fluoroscandiate or a solution of НNO 3 in the form of scandium fluoride, hydrolysis of double fluoroscandiate Na-NH 4 (using NaF cr ) to obtain scandium fluoride ScF 3 and conversion into Sc 2 O 3 at a temperature of ≥700 ° C in flowing air. The proposed method allows efficient separation of Sc from Ca, Mg, Al, Ti, Y, REE, Zr, Na, U, and Th impurities at the stage of leaching of the FC with a solution of NH 4 F and additionally from Ti, Zr, U, Fe, and Mg, which form soluble fluoride complexes upon precipitation of Sc from a solution of NH 4 F in the form of fluoride salts. The proposed method, in contrast to the prototype, allows to obtain 99% Sc 2 O 3 from FC without opening the FC, which is illustrated by the following examples.
П р и м е р 1. 10 г фторидного концентрата состава, мас. Sc 26,1; Na 4,3; Mg 2,5; Fe 0,9; Al 1,0; Ca 3,4 обрабатывали 10%-ным раствором NH4F (V 1 л) в течение 1 ч. Нерастворимый осадок отделяли фильтрованием. Из раствора NH4F осаждали двойной фторскандиат добавлением NaFкр в количестве 150% от стехиометрии на образование ScF3, осадок фильтровали, промывали горячим 1% -ным раствором HNO3, сушили и прокаливали при 700оС в токе воздуха в течение 3 ч. Результаты РФА указывают на образование в остатке от прокаливания Sc2O3. Чистота полученного оксида скандия составила, мас. основное вещество 99,5. Сr 5˙10-4; Si 0,05; Mg 0,04; Mn 0,001; Al 0,001; Ni 0,005; Fe 0,008; Cu 3˙10-5; Ti < 2˙10-3; Zr < 0,01; Y < 0,001; Yb < 5˙10-4; Ca 0,02.PRI me R 1. 10 g of fluoride concentrate composition, wt. Sc 26.1; Na 4.3; Mg 2.5; Fe 0.9; Al 1.0; Ca 3,4 was treated with 10% NH 4 F solution (V 1 L) for 1 h. Insoluble precipitate was separated by filtration. From the NH 4 F solution was precipitated by addition of NaF dual ftorskandiat Cr in an amount of 150% of the stoichiometry of the formation of ScF 3, and the precipitate was filtered, washed with hot 1% solution of HNO 3, dried, and calcined at 700 ° C in flowing air for 3 hours. XRD results indicate the formation of Sc 2 O 3 in the residue from calcination. The purity of the obtained scandium oxide was, wt. the main substance is 99.5. Cr 5-10 -4 ; Si 0.05; Mg 0.04; Mn 0.001; Al 0.001; Ni 0.005; Fe 0.008; Cu 3˙10 -5; Ti <2˙10 -3 ; Zr <0.01; Y <0.001; Yb <5˙10 -4 ; Ca 0.02.
П р и м е р 2. Процесс проводили как в примере 1, но осаждали Sc из раствора NH4F добавлением азотной кислоты до избыточной кислотности ≈30 г/л. Результаты РФА подтвердили наличие фазы Sc2O3 после прокаливания фторида скандия при 700оС в токе воздуха в течение 3 ч. Чистота полученного оксида скандия составила, мас. основное вещество 99,4; Cr 1˙10-4; Si 0,06; Mg 0,08; Mn 0,001; Al 0,05; Ni 0,001; Fe 0,01; Cu 0,0004; Ca 0,15; Ti < 0,002; Zr 0,01; Y < 0,001; Yb < 0,0005.PRI me R 2. The process was carried out as in example 1, but Sc was precipitated from a solution of NH 4 F by adding nitric acid to an excess acidity of ≈30 g / l. XRD results confirmed the presence of phase Sc 2 O 3 after calcination scandium fluoride at 700 o C in flowing air for 3 hours. The purity of scandium oxide was wt. basic substance 99.4; Cr 1˙10 -4; Si 0.06; Mg 0.08; Mn 0.001; Al 0.05; Ni 0.001; Fe 0.01; Cu 0,0004; Ca 0.15; Ti <0.002; Zr 0.01; Y <0.001; Yb <0,0005.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU925049810A RU2040471C1 (en) | 1992-06-25 | 1992-06-25 | Method of preparing 99%-th scandium oxide from the fluoride concentrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU925049810A RU2040471C1 (en) | 1992-06-25 | 1992-06-25 | Method of preparing 99%-th scandium oxide from the fluoride concentrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| RU2040471C1 true RU2040471C1 (en) | 1995-07-25 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU925049810A RU2040471C1 (en) | 1992-06-25 | 1992-06-25 | Method of preparing 99%-th scandium oxide from the fluoride concentrate |
Country Status (1)
| Country | Link |
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| RU (1) | RU2040471C1 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2236375C2 (en) * | 2002-04-29 | 2004-09-20 | ООО "Ромекс" | Method for preparing sodium hexafluoroscandiate |
| CN106430278A (en) * | 2016-09-28 | 2017-02-22 | 益阳鸿源稀土有限责任公司 | Method for preparing high-purity anhydrous scandium acetate and high-purity scandium oxide |
-
1992
- 1992-06-25 RU SU925049810A patent/RU2040471C1/en active
Non-Patent Citations (1)
| Title |
|---|
| Коршунов Б.Г. и др. Скандий. М.: Металлургия, 1987., с.146. * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2236375C2 (en) * | 2002-04-29 | 2004-09-20 | ООО "Ромекс" | Method for preparing sodium hexafluoroscandiate |
| CN106430278A (en) * | 2016-09-28 | 2017-02-22 | 益阳鸿源稀土有限责任公司 | Method for preparing high-purity anhydrous scandium acetate and high-purity scandium oxide |
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