DE2312297A1 - METHOD FOR PRODUCING ELEMENTAL FLUORINE - Google Patents
METHOD FOR PRODUCING ELEMENTAL FLUORINEInfo
- Publication number
- DE2312297A1 DE2312297A1 DE2312297A DE2312297A DE2312297A1 DE 2312297 A1 DE2312297 A1 DE 2312297A1 DE 2312297 A DE2312297 A DE 2312297A DE 2312297 A DE2312297 A DE 2312297A DE 2312297 A1 DE2312297 A1 DE 2312297A1
- Authority
- DE
- Germany
- Prior art keywords
- electrolyte
- barium
- fluoride
- elemental fluorine
- corrosion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 title claims description 6
- 229910052731 fluorine Inorganic materials 0.000 title claims description 6
- 239000011737 fluorine Substances 0.000 title claims description 6
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000003792 electrolyte Substances 0.000 claims description 16
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 10
- 229910001422 barium ion Inorganic materials 0.000 claims description 9
- 229910001427 strontium ion Inorganic materials 0.000 claims description 8
- 238000005868 electrolysis reaction Methods 0.000 claims description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 5
- 229910000040 hydrogen fluoride Inorganic materials 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000005260 corrosion Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 229910052788 barium Inorganic materials 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- 229910000792 Monel Inorganic materials 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 239000011698 potassium fluoride Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 description 1
- 229910001632 barium fluoride Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000003438 strontium compounds Chemical class 0.000 description 1
- FVRNDBHWWSPNOM-UHFFFAOYSA-L strontium fluoride Chemical compound [F-].[F-].[Sr+2] FVRNDBHWWSPNOM-UHFFFAOYSA-L 0.000 description 1
- 229910001637 strontium fluoride Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/24—Halogens or compounds thereof
- C25B1/245—Fluorine; Compounds thereof
Description
Verfahren zur Herstellung von elementarem FluorProcess for the production of elemental fluorine
Fluor, dessen industrielle Bedeutung in der jüngsten Vergangenheit
erheblich zugenommen hat, wird technisch durch Elektrolyse einer Lösung eines Fluorids in wasserfreiem Fluorwasserstoff
dargestellt. Der Zusatz von Fluoriden ist notwendig, um die Leitfähigkeit zu erhöhen, den Dampfdruck des Fluorwasserstoffs
herabzusetzen und das Auftreten von sogenannten Anodeneffekten weitgehend zu verhindern. Als Fluoride werden bevorzugt
Kaliumfluorid, daneben u.a. die des Lithiums, Natriums
und Ammoniums eingesetzt. An die Rohstoffe für den Elektrolyten werden hohe Reinheitsanforderungen gestellt, beispielsweise
bezüglich des Gehaltes an Wasser, Schwefel-, Silicium-
und Schwermetallverbindungen. Als obere Grenze für den Wassergehalt wird in der Regel 0,1 % für noch zulässig erachtet.
Fluorine, the industrial importance of which has increased considerably in the recent past, is technically produced by the electrolysis of a solution of a fluoride in anhydrous hydrogen fluoride. The addition of fluorides is necessary to increase the conductivity, to lower the vapor pressure of the hydrogen fluoride and to largely prevent the occurrence of so-called anode effects. Potassium fluoride is preferred as the fluoride, along with those of lithium and sodium, among others
and ammonium used. The raw materials for the electrolyte are subject to high purity requirements, for example with regard to the content of water, sulfur, silicon
and heavy metal compounds. The upper limit for the water content is generally considered to be 0.1% still permissible.
Die Elektrolysezelle ist in verschiedenen Ausführungsformen bekannt.
Der Zellentrog besteht meistens aus Stahl oder Monel und
dient als Kathode. Am Zellendeckel sind die Anoden elektrisch isoliert befestigt und außerdem in den Elektrolyten hineinragende
Elemente zur Trennung des Kathoden_gasraumes vom Anodengasraum. Die Trennelemente (Schürzen) bestehen üblicherweise
aus Monel oder einer Magnesiumlegierung.The electrolytic cell is known in various embodiments. The cell trough is usually made of steel or Monel and serves as a cathode. The anodes are attached to the cell cover in an electrically insulated manner and also elements protruding into the electrolyte to separate the cathode gas space from the anode gas space. The separating elements (aprons) usually exist
made of Monel or a magnesium alloy.
Ein ernsthaftes Problem beim Betrieb der Zellen sind Korrosionserscheinungen, die besonders an den Schürzen auftreten und zur Verunreinigung des Elektrolyten durch gelöstes Schürzenmaterial führen. Wenn die Korrosion bis zur Perforation derA serious problem with the operation of the cells is corrosion, which occur particularly on the aprons and lead to contamination of the electrolyte by dissolved apron material to lead. If the corrosion is up to the perforation of the
-2--2-
409839/0856409839/0856
Schürzen fortschreitet, tritt der Wasserstoff im Kathodenraum mit dem Fluor im Anodenraum explosionsartig in Reaktion. Eine häufige Kontrolle der Schürzen ist. daher erfoderlich.· Dazu muß die Zelle außer Betrieb gesetzt und demontiert werden.As aprons progresses, the hydrogen in the cathode compartment reacts explosively with the fluorine in the anode compartment. One frequent control of the aprons. therefore required. · To do this, the cell must be taken out of service and dismantled.
Bei den Explosionen werden in der Regel die Anoden teilweise zerstört, so üaB tier Elektrolyt mit Kohlenstoff verunreinigt und dadurch unbrauchbar wird. Bei heftigen Explosionen kommt es vor, daß der Druckanstieg ein Abheben des Zellendeckels zur Folge hat, dadurch tritt heißer Elektrolyt aus den Zellen und stellt eine ernsthafte Gefahr für das Bedienungspersonal dar. Außerdem kaum es zu erheblichen Schädigungen der umliegenden Anlageteile kommen.In the explosion, the anodes are usually partially destroyed, so that the electrolyte is contaminated with carbon and thus becomes unusable. In the case of violent explosions, the rise in pressure causes the cell cover to lift off, causing hot electrolyte to escape from the cells and posing a serious risk to the operating personnel. In addition, there is hardly any significant damage to the surrounding system parts.
Die durchschnittliche Lebensdauer der Elektrolys.ezellen beträgt zwischen 1 und 12 Monaten Betriebszeit {s. A.J. Rudge in Α.Ϊ. Kuhn Industr. Electrochemical Processes» Kap,1 Eisevier Publishing Co, Amsterdam, Hew York, London (1971).The average lifespan of the electrolysis cells is between 1 and 12 months of operation {s. A.J. Rudge in Α.Ϊ. Kuhn Industr. Electrochemical Processes »Chap, 1 Eisevier Publishing Co, Amsterdam, Hew York, London (1971).
Es wurde nun überraschenderweise gefunden, daß durch Zusatz von Barium- und/oder Strontiumionen zum Elektrolyten die Korrosion weitgehend eingeschränkt werden kann, so daß die Lebensdauer der Zelle xon ein Vielfaches erhöht wird.It has now surprisingly been found that the addition of barium and / or strontium ions to the electrolyte reduces corrosion can be largely restricted, so that the life of the cell xon is increased many times over.
Das erfindungsgemäße Verfahren zur Herstellung von elementarem Fluor durch Elektrolyse eines Gemisches von Fluorwasserstoff tait einem Fluorid ist dadurch gekennzeichnet» daß der Elektrolyt" Barium- und/oder Strontiumionen enthält.The process according to the invention for the production of elemental fluorine by electrolysis of a mixture of hydrogen fluoride with a fluoride is characterized in that the electrolyte contains barium and / or strontium ions.
Es hat sich gezeigt, daß bereits Mengen von 0,05 bis 0,9 %, vorzugsweise 0,10 bis 0,35 Jo, an Barium- und/oder Strontiumionen die Korrosionsrate um einen Faktor von 10 bis 100 verringern.It has been shown that even amounts of 0.05 to 0.9 %, preferably 0.10 to 0.35 Jo, of barium and / or strontium ions reduce the corrosion rate by a factor of 10 to 100.
-3-409839/0858 -3-409839 / 0858
Die Barium- oder Strontiumionen können in Form von Bariumoder Strontiumverbindungen, vorzugsweise als Pluorid,zugesetzt werden.The barium or strontium ions can be added in the form of barium or strontium compounds, preferably as fluoride will.
In einer neuen Elektrolysezelle vom Typ der Allied Chem. Corp., wie sie beispielsweise in Kirk-Othmer: Encyclopedia of Chemical Technology 2nd Ed., Vol.9, S. 513, beschrieben ist, wurde ein Elektrolyt der Zusammensetzung KF · 2,0 HF und mit einem Bariumgehalt von 0,15 % Bariumionen, die in Form von Bariumfluorid dem Elektrolyten zugesetzt wurden, unter kontinuierlicher 'Zuführung von Fluorwasserstoff mit einem durchschnittlichen Gehalt an HF von 99,90 % und einem durchschnittlichen Wassergehalt von 0,02 % unter den, in der oben zitierten Literaturstelle auf S. 514 beschriebenen Betriebsbedingungen über einen Zeitraum entsprechend 26 Betriebsmonaten elektrolysiert. Nach dieser Zeit ergab eine Untersuchung der Elektrolytzusammensetzung einen Gehalt an Magnesium von 0,008 %. Auch das Aussehen der Schürzen und der Deckelunterseite ließ darauf schließen, daß praktisch keine Korrosion eingetreten war.In a new electrolysis cell of the Allied Chem. Corp. type, as described, for example, in Kirk-Othmer: Encyclopedia of Chemical Technology 2nd Ed., Vol.9, p. 513, an electrolyte of the composition KF * 2.0 HF and with a barium content of 0.15 % barium ions, which were added to the electrolyte in the form of barium fluoride, with continuous' supply of hydrogen fluoride with an average content of HF of 99.90 % and an average water content of 0.02 % below the , in the above-cited reference on page 514 operating conditions described over a period corresponding to 26 months of operation. After this time, an examination of the electrolyte composition showed a magnesium content of 0.008 %. The appearance of the aprons and the underside of the lid also indicated that practically no corrosion had occurred.
Werden anstelle von 0,15 % Bariumionen 0,12 % Strontiumionen in Form von Strontiumfluorid dem Elektrolyten zugesetzt, so konnte ebenfalls nach der angegebenen Betriebszeit praktisch keine Korrosion festgestellt werden.If 0.12% strontium ions in the form of strontium fluoride were added to the electrolyte instead of 0.15 % barium ions, then practically no corrosion could also be found after the specified operating time.
Der Versuch wurde unter den gleichen Bedingungen, ebenfalls in einer neuen Elektrolysezelle wiederholt, nur mit der Ausnahme, daß der Elektrolyt keine Barium- oder Strontiumionen enthielt. Nach 2 Monaten Betriebszeit betrug der Magnesiumgehalt des Elektrolyten bereits 0,81 % und die Schürzen zeigten sehr starke Korrosionserscheinungen.The experiment was repeated under the same conditions, also in a new electrolysis cell, with the exception that the electrolyte did not contain any barium or strontium ions. After 2 months of operation, the magnesium content of the electrolyte was already 0.81 % and the aprons showed very strong signs of corrosion.
409839/0856409839/0856
Allein schon an Hand des Vergleichs der aus den Schürzen und der Deckelinnenseite stammenden Magnesiumverunreinigungen in den beiden Versuchen läßt sich die beachtliche Verringerung der Korrosion durch die Anwesenheit von Barium- bzw« Strontlmmionen im Elektrolyten meßbar feststellen.Already based on the comparison of the magnesium contamination from the aprons and the inside of the lid in the Both attempts can show the considerable reduction in Corrosion due to the presence of barium or current ions detectable in the electrolyte.
403833/O8SB403833 / O8SB
Claims (2)
Priority Applications (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19732312297 DE2312297C3 (en) | 1973-03-13 | Process for the production of elemental fluorine | |
| GB938974A GB1407579A (en) | 1973-03-13 | 1974-03-01 | Method of electrolytically producing elemental fluorine |
| JP2672974A JPS5644152B2 (en) | 1973-03-13 | 1974-03-07 | |
| US450487A US3860504A (en) | 1973-03-13 | 1974-03-12 | Process for the production of elemental fluorine by electrolysis |
| FR7408406A FR2221400B1 (en) | 1973-03-13 | 1974-03-12 | |
| IT20687/74A IT1007448B (en) | 1973-03-13 | 1974-04-08 | PROCEDURE FOR PREPARING ELEMENTARY FLUORIDE |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19732312297 DE2312297C3 (en) | 1973-03-13 | Process for the production of elemental fluorine |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| DE2312297A1 true DE2312297A1 (en) | 1974-09-26 |
| DE2312297B2 DE2312297B2 (en) | 1977-03-03 |
| DE2312297C3 DE2312297C3 (en) | 1977-10-20 |
Family
ID=
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5411641A (en) * | 1993-11-22 | 1995-05-02 | E. I. Du Pont De Nemours And Company | Electrochemical conversion of anhydrous hydrogen halide to halogen gas using a cation-transporting membrane |
| US5798036A (en) * | 1993-11-22 | 1998-08-25 | E. I. Du Pont De Nemours And Company | Electrochemical conversion of anhydrous hydrogen halide to halogens gas using a membrane-electrode assembly or gas diffusion electrodes |
| US5855748A (en) * | 1993-11-22 | 1999-01-05 | E. I. Du Pont De Nemours And Company | Electrochemical cell having a mass flow field made of glassy carbon |
| US5855759A (en) * | 1993-11-22 | 1999-01-05 | E. I. Du Pont De Nemours And Company | Electrochemical cell and process for splitting a sulfate solution and producing a hyroxide solution sulfuric acid and a halogen gas |
| US5961795A (en) * | 1993-11-22 | 1999-10-05 | E. I. Du Pont De Nemours And Company | Electrochemical cell having a resilient flow field |
| US5976346A (en) * | 1993-11-22 | 1999-11-02 | E. I. Du Pont De Nemours And Company | Membrane hydration in electrochemical conversion of anhydrous hydrogen halide to halogen gas |
| US6042702A (en) * | 1993-11-22 | 2000-03-28 | E.I. Du Pont De Nemours And Company | Electrochemical cell having a current distributor comprising a conductive polymer composite material |
| US6180163B1 (en) | 1993-11-22 | 2001-01-30 | E. I. Du Pont De Nemours And Company | Method of making a membrane-electrode assembly |
| USRE37433E1 (en) | 1993-11-22 | 2001-11-06 | E. I. Du Pont De Nemours And Company | Electrochemical conversion of anhydrous hydrogen halide to halogen gas using a membrane-electrode assembly or gas diffusion electrodes |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5411641A (en) * | 1993-11-22 | 1995-05-02 | E. I. Du Pont De Nemours And Company | Electrochemical conversion of anhydrous hydrogen halide to halogen gas using a cation-transporting membrane |
| US5580437A (en) * | 1993-11-22 | 1996-12-03 | E. I. Du Pont De Nemours And Company | Anode useful for electrochemical conversion of anhydrous hydrogen halide to halogen gas |
| US5798036A (en) * | 1993-11-22 | 1998-08-25 | E. I. Du Pont De Nemours And Company | Electrochemical conversion of anhydrous hydrogen halide to halogens gas using a membrane-electrode assembly or gas diffusion electrodes |
| US5855748A (en) * | 1993-11-22 | 1999-01-05 | E. I. Du Pont De Nemours And Company | Electrochemical cell having a mass flow field made of glassy carbon |
| US5855759A (en) * | 1993-11-22 | 1999-01-05 | E. I. Du Pont De Nemours And Company | Electrochemical cell and process for splitting a sulfate solution and producing a hyroxide solution sulfuric acid and a halogen gas |
| US5961795A (en) * | 1993-11-22 | 1999-10-05 | E. I. Du Pont De Nemours And Company | Electrochemical cell having a resilient flow field |
| US5976346A (en) * | 1993-11-22 | 1999-11-02 | E. I. Du Pont De Nemours And Company | Membrane hydration in electrochemical conversion of anhydrous hydrogen halide to halogen gas |
| US6042702A (en) * | 1993-11-22 | 2000-03-28 | E.I. Du Pont De Nemours And Company | Electrochemical cell having a current distributor comprising a conductive polymer composite material |
| USRE36985E (en) * | 1993-11-22 | 2000-12-12 | E. I. Du Pont De Nemours And Company | Anode useful for electrochemical conversion of anhydrous hydrogen halide to halogen gas |
| US6180163B1 (en) | 1993-11-22 | 2001-01-30 | E. I. Du Pont De Nemours And Company | Method of making a membrane-electrode assembly |
| USRE37042E1 (en) * | 1993-11-22 | 2001-02-06 | E. I. Du Pont De Nemours And Company | Electrochemical conversion of anhydrous hydrogen halide to halogen gas using a cation-transporting membrane |
| US6203675B1 (en) | 1993-11-22 | 2001-03-20 | E. I. Du Pont De Nemours And Company | Electrochemical conversion of anhydrous hydrogen halide to halogen gas using an electrochemical cell |
| USRE37433E1 (en) | 1993-11-22 | 2001-11-06 | E. I. Du Pont De Nemours And Company | Electrochemical conversion of anhydrous hydrogen halide to halogen gas using a membrane-electrode assembly or gas diffusion electrodes |
Also Published As
| Publication number | Publication date |
|---|---|
| GB1407579A (en) | 1975-09-24 |
| JPS5025494A (en) | 1975-03-18 |
| DE2312297B2 (en) | 1977-03-03 |
| FR2221400B1 (en) | 1976-12-17 |
| IT1007448B (en) | 1976-10-30 |
| US3860504A (en) | 1975-01-14 |
| JPS5644152B2 (en) | 1981-10-17 |
| FR2221400A1 (en) | 1974-10-11 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C3 | Grant after two publication steps (3rd publication) | ||
| E77 | Valid patent as to the heymanns-index 1977 |