WO2009146986A1 - Verfahren zur herstellung von reinem ammoniumperrhenat - Google Patents
Verfahren zur herstellung von reinem ammoniumperrhenat Download PDFInfo
- Publication number
- WO2009146986A1 WO2009146986A1 PCT/EP2009/055174 EP2009055174W WO2009146986A1 WO 2009146986 A1 WO2009146986 A1 WO 2009146986A1 EP 2009055174 W EP2009055174 W EP 2009055174W WO 2009146986 A1 WO2009146986 A1 WO 2009146986A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- ammonium perrhenate
- acid
- suspension
- potassium
- ammonia
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G47/00—Compounds of rhenium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G47/00—Compounds of rhenium
- C01G47/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B61/00—Obtaining metals not elsewhere provided for in this subclass
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Definitions
- the concentration of nitric acid in the suspension may be 0.5 to 10 mol / l, preferably 0.5 to 8 mol / l, more preferably 0.5 to 7 mol / l, particularly preferably 1 to 5 mol / l. Good results are achieved with a concentration of nitric acid of 2 to 4 mol / l.
- the supply of nitric acid can be batchwise or continuously. The continuous supply of nitric acid has the advantage that the amount required in each case is automatically adapted to the current flowing through the electrolysis and the entire process can be optimally controlled.
- the temperature of the suspension in the reservoir should not fall below 50 ° C in order to achieve a sufficiently high rate of decomposition of the ammonium ions.
- the temperature in the reservoir is> 60 ° C, preferably> 70 0 C, more preferably> 80 ° C and particularly preferably> 95 ° C.
- a very important role in the process according to the invention is played by the current density at which the cathodic reduction of nitric acid (HNO 3 ) to nitrous acid (HNO 2 ) takes place or is operated with the electrolysis cell.
- the reduction of nitric acid can be carried out at current densities of 100 to 4000 A / m 2 .
- the quality of the perrhenic acid thus obtained is already sufficient and this can be used directly or after a subsequent complete reaction with ammonia as pre-purified ammonium perrhenate.
- the quality is not yet sufficient, since the potassium content of such perrhenic acid is still too high.
- Ammonium perrhenate as a solid (5) prepared a suspension.
- Ammonium perrhenate as a solid (5) prepared a suspension.
- the dip tube (6) with a pump (7) low-solids suspension through the heat exchanger (8) in the
- Electrolytic cell (10) promoted. Through the free overflow (11), the catholyte flows back into the reactor (1). In the reactor (1) via the heat exchanger (3) has a temperature of > 50 ° C maintained. Before the low-solids suspension is pumped into the cell with the pump (7), the heat exchanger (8) may cool it down to ⁇ 80 ° C.
- the pressure filter (21) serves to separate any precipitated potassium perrhenate already here (23).
- the perrhenic acid which may contain up to 300 ppm, or 400-500 ppm of potassium (based on rhenium), collected.
- pump (24) this perrhenic acid is sent for further processing.
- the further processing of the potassium-containing perrhenic acid to purest ammonium perrhenate can be carried out in different ways.
- the purification is preferably carried out by means of a precipitation of the ammonium perrhenate, FIG. 2.
- the potassium-containing perrhenic acid is pumped by pump (24) into the precipitation reactor (25). While stirring (26), the solution is cooled with heat exchanger (27).
- the extracted Mother liquor can be fed via pump (39) to the earlier process stages of rhenium production or fed back to the reactor (1) via pump (4).
- the purest ammonium perrhenate is removed from the suction filter via (40) and further processed, for example, by reduction to give the purest re-metal powder.
- an ion exchanger is used. After this process, the potassium-containing perrhenic acid after cooling in the reactor (26) is conveyed by the pump (29) through the ion exchange column (42) in the reactor (32). The ion exchange column is previously filled via (41) with cation exchanger in the protonated form so that the potassium ions contained in the perrhenic acid are exchanged for H + ions. The perrhenic acid then contains less than 5 ppm of potassium, based on rhenium. The main reactor (32) then precipitates the purest Ammoniumperrhenates, as described above. If the ion exchanger no longer absorbs enough potassium, it is fed to (43) regeneration with mineral acids.
- the anolyte of the electrolytic cell (10) consisted of 40% HReO4 and was conveyed from a circulation tank (12) with pump (13) into the anode compartment of the two-divided electrolysis cell (10) and flowed through the free overflow (14) in the circulation container (12) back.
- a temperature of 30 0 C was maintained by means of the heat exchanger (15).
- the losses were compensated by water decomposition and transfer into the cathode compartment.
- 705 g / h of nitric acid (50%) were pumped into the reactor (1) with pump (17) and a current of 300 A was set in the electrolysis cell (10) by applying a voltage of about 4 V.
- Examples 3-5 were carried out analogously to Example 2, wherein the proportion of pre-precipitated Ammoniumperrhenates was gradually increased.
- Table 1 the parameters and the results of Examples 2 to 5 are summarized.
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2011512053A JP2011522127A (ja) | 2008-06-05 | 2009-04-29 | 純粋な過レニウム酸アンモニウムの製造方法 |
CA2726438A CA2726438A1 (en) | 2008-06-05 | 2009-04-29 | Process for producing pure ammonium perrhenate |
RU2010154378/05A RU2514941C2 (ru) | 2008-06-05 | 2009-04-29 | Способ получения чистого перрената аммония |
EP09757369A EP2291327A1 (de) | 2008-06-05 | 2009-04-29 | Verfahren zur herstellung von reinem ammoniumperrhenat |
US12/996,016 US8795509B2 (en) | 2008-06-05 | 2009-04-29 | Process for producing pure ammonium perrhenate |
US14/309,902 US20140301939A1 (en) | 2008-06-05 | 2014-06-20 | Process for producing pure ammonium perrhenate |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102008026910A DE102008026910A1 (de) | 2008-06-05 | 2008-06-05 | Verfahren zur Herstellung von reinem Ammoniumperrphenat |
DE102008026910.7 | 2008-06-05 |
Related Child Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US12/996,016 A-371-Of-International US8795509B2 (en) | 2008-06-05 | 2009-04-29 | Process for producing pure ammonium perrhenate |
US14/309,902 Continuation US20140301939A1 (en) | 2008-06-05 | 2014-06-20 | Process for producing pure ammonium perrhenate |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2009146986A1 true WO2009146986A1 (de) | 2009-12-10 |
Family
ID=40852006
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2009/055174 WO2009146986A1 (de) | 2008-06-05 | 2009-04-29 | Verfahren zur herstellung von reinem ammoniumperrhenat |
Country Status (7)
Country | Link |
---|---|
US (2) | US8795509B2 (de) |
EP (1) | EP2291327A1 (de) |
JP (1) | JP2011522127A (de) |
CA (1) | CA2726438A1 (de) |
DE (1) | DE102008026910A1 (de) |
RU (1) | RU2514941C2 (de) |
WO (1) | WO2009146986A1 (de) |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104176784B (zh) * | 2014-08-16 | 2016-03-16 | 厦门世达膜科技有限公司 | 一种制备高铼酸铵的方法 |
DE102016010977A1 (de) * | 2016-09-13 | 2018-03-15 | H.C. Starck Surface Technology and Ceramic Powders GmbH | Verfahren zur Herstellung von Ammoniumperrhenat |
DE102017115125A1 (de) | 2017-07-06 | 2019-01-10 | Claas Selbstfahrende Erntemaschinen Gmbh | Kabinendach einer Kabine für ein landwirtschaftliches Arbeitsfahrzeug |
CN115072789B (zh) * | 2022-08-08 | 2024-06-07 | 中国地质科学院郑州矿产综合利用研究所 | 一种高纯铼酸铵的制备方法 |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1185167B (de) * | 1960-05-02 | 1965-01-14 | Chase Brass & Copper Co | Verfahren zur Reinigung von Perrheniumsaeure |
AT292629B (de) * | 1969-10-20 | 1971-09-10 | Inst Neorganicheskoi Khim An L | Verfahren zur Herstellung von Ammoniumperrhenat |
DD200566A1 (de) * | 1981-08-24 | 1983-05-18 | Siegfried Gerisch | Verfahren zur gewinnung von perrhenatverbindungen aus waessrigen loesungen |
EP0512633A2 (de) * | 1991-05-07 | 1992-11-11 | Metallwerk Plansee Gesellschaft M.B.H. | Verfahren zur Nachbehandlung der Brennbahn von Röntgendrehanoden |
DE19811765A1 (de) * | 1997-05-12 | 1998-11-19 | Heraeus Gmbh W C | Verfahren zur Herstellung von Rhenium enthaltenden Legierungen und danach hergestellte Legierungen |
Family Cites Families (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE200566C (de) | 1907-08-10 | |||
JPS5844155B2 (ja) * | 1978-10-06 | 1983-10-01 | 旭化成株式会社 | 亜硝酸塩の製造法 |
JPS62123021A (ja) * | 1985-11-25 | 1987-06-04 | Nippon Mining Co Ltd | 過レニウム酸アンモニウムの製造方法 |
JPS62146227A (ja) * | 1985-12-20 | 1987-06-30 | Nippon Mining Co Ltd | 金属レニウムの製造方法 |
US6039920A (en) * | 1997-05-12 | 2000-03-21 | W. C. Heraeus Gmbh & Co. Kg | Process for making rhenium-containing alloys |
DE102005003445B4 (de) * | 2005-01-21 | 2009-06-04 | H.C. Starck Hermsdorf Gmbh | Metallsubstrat-Werkstoff für die Anodenteller von Drehanodenröntgenröhren, Verfahren zur Herstellung eines solchen Werkstoffes sowie Verfahren zur Herstellung eines Anodentellers unter Verwendung eines solchen Werkstoffes |
JP5109115B2 (ja) * | 2005-04-07 | 2012-12-26 | 国立大学法人 長崎大学 | ニッケル基超合金及びその製造方法 |
RU2355640C2 (ru) * | 2007-07-04 | 2009-05-20 | Открытое акционерное общество "Красноярский завод цветных металлов имени В.Н. Гулидова" (ОАО "Красцветмет") | Способ получения перрената аммония |
-
2008
- 2008-06-05 DE DE102008026910A patent/DE102008026910A1/de not_active Ceased
-
2009
- 2009-04-29 US US12/996,016 patent/US8795509B2/en not_active Expired - Fee Related
- 2009-04-29 CA CA2726438A patent/CA2726438A1/en not_active Abandoned
- 2009-04-29 RU RU2010154378/05A patent/RU2514941C2/ru not_active IP Right Cessation
- 2009-04-29 EP EP09757369A patent/EP2291327A1/de not_active Withdrawn
- 2009-04-29 JP JP2011512053A patent/JP2011522127A/ja not_active Ceased
- 2009-04-29 WO PCT/EP2009/055174 patent/WO2009146986A1/de active Application Filing
-
2014
- 2014-06-20 US US14/309,902 patent/US20140301939A1/en not_active Abandoned
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1185167B (de) * | 1960-05-02 | 1965-01-14 | Chase Brass & Copper Co | Verfahren zur Reinigung von Perrheniumsaeure |
AT292629B (de) * | 1969-10-20 | 1971-09-10 | Inst Neorganicheskoi Khim An L | Verfahren zur Herstellung von Ammoniumperrhenat |
DD200566A1 (de) * | 1981-08-24 | 1983-05-18 | Siegfried Gerisch | Verfahren zur gewinnung von perrhenatverbindungen aus waessrigen loesungen |
EP0512633A2 (de) * | 1991-05-07 | 1992-11-11 | Metallwerk Plansee Gesellschaft M.B.H. | Verfahren zur Nachbehandlung der Brennbahn von Röntgendrehanoden |
DE19811765A1 (de) * | 1997-05-12 | 1998-11-19 | Heraeus Gmbh W C | Verfahren zur Herstellung von Rhenium enthaltenden Legierungen und danach hergestellte Legierungen |
Non-Patent Citations (3)
Title |
---|
DATABASE COMPENDEX [online] ENGINEERING INFORMATION, INC., NEW YORK, NY, US; PALANT A A ET AL: "Electrochemical production of concentrated solutions of rhenium acid under the effect of alternative current with commercial frequency", XP002538960, Database accession no. E2005439432862 * |
ELUTIN A V ET AL: "Usage of electrodialysis method for preparing high-purity rhenium chemical compounds", TMS ANNUAL MEETING, XX, XX, 1 January 1997 (1997-01-01), pages 209 - 215, XP008108640 * |
TSVETNYE METALLY 2005 RUDA I METALLY RU, no. 5-6, 2005, pages 128 - 130 * |
Also Published As
Publication number | Publication date |
---|---|
US20140301939A1 (en) | 2014-10-09 |
US20110123709A1 (en) | 2011-05-26 |
RU2514941C2 (ru) | 2014-05-10 |
CA2726438A1 (en) | 2009-12-10 |
US8795509B2 (en) | 2014-08-05 |
RU2010154378A (ru) | 2012-07-20 |
JP2011522127A (ja) | 2011-07-28 |
EP2291327A1 (de) | 2011-03-09 |
DE102008026910A1 (de) | 2009-12-10 |
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