DE1467030A1 - Process for removing small amounts of hydrogen fluoride from hydrogen chloride - Google Patents
Process for removing small amounts of hydrogen fluoride from hydrogen chlorideInfo
- Publication number
- DE1467030A1 DE1467030A1 DE19641467030 DE1467030A DE1467030A1 DE 1467030 A1 DE1467030 A1 DE 1467030A1 DE 19641467030 DE19641467030 DE 19641467030 DE 1467030 A DE1467030 A DE 1467030A DE 1467030 A1 DE1467030 A1 DE 1467030A1
- Authority
- DE
- Germany
- Prior art keywords
- hydrogen
- small amounts
- hydrogen fluoride
- hydrogen chloride
- removing small
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Extraction Or Liquid Replacement (AREA)
Description
DYNAMIT NOBEL AKTIENGESELLSCHAFT Troisdorf / Bez. KölnDYNAMIT NOBEL AKTIENGESELLSCHAFT Troisdorf / Bez. Cologne
Verfahren zur Entfernung kleiner Mengen Fluorwasserstoff aus Chlorwasserstoff"Process for removing small amounts of hydrogen fluoride from hydrogen chloride "
Die meisten Fluorierungsverfahren organischer Verbindungen beruhen auf einem Halogenaustausch zwischen Fluorwasserstoff und Chlor enthaltenden Verbindungen. Dabei entsteht wasserfreier Chlorwasserstoff, der von den letzten Spuren Fluorwasserstoff nur sehr schwer zu befreien ist. Dadurch wird dieses an sich relativ wertvolle Nebenprodukt für fast alle Zwecke unbrauchbar. Daher sind neben der schwierigen destillativen Trennung auch chemische Verfahren vorgeschlagen worden, um den Fluorwasserstoff zu entfernen. Zum Beispiel sind hier die Abtrennung mittels Kieselgel bei erhöhtem Druck und die Abtrennung durch hochkonzentrierte wässrige Salzsäure, gegebenenfalls mit Zusätzen von Metallsalzen, insbesondere, von Calcium- oder Aluminiumsalzen, zu nennen.Most of the fluorination processes of organic compounds are based on a halogen exchange between hydrogen fluoride and chlorine containing compounds. This creates anhydrous hydrogen chloride, that of the last traces of hydrogen fluoride only very much hard to break free. This makes this by-product, which is relatively valuable in itself, unusable for almost all purposes. Hence are In addition to the difficult separation by distillation, chemical processes have also been proposed to remove the hydrogen fluoride. For example, the separation by means of silica gel is here at increased Pressure and the separation by highly concentrated aqueous hydrochloric acid, optionally with the addition of metal salts, in particular, of calcium or aluminum salts.
In dem einen Fall ist die Kompression so aggressiver Gase ein Störungsfaktor, im anderen die hohe Korrosionsgefahr durch die stark salzsauren wässrigen Lösungen. Auch ist die Bildung flüchtiger Fluorverbindungen, wie z.B. SiF. oder BF,, die bei einem weiteren bekannten Verfahren entstehen, für manche Verwendungszwecke ein ausschließendes Hindernis.In one case the compression is so aggressive gases one Disturbance factor, in the other the high risk of corrosion due to the strong hydrochloric aqueous solutions. There is also the formation of volatile fluorine compounds such as SiF. or BF ,, which at another known processes arise, for some purposes an exclusive obstacle.
Es wurde nun gefunden, daß man bei Normaldruck und Normaltemperatur in einem Verfahren ohne Wasseranwendung den FluorwasserstoffIt has now been found that at normal pressure and normal temperature in a process without the use of water, the hydrogen fluoride
809901/0655 > 809901/0655 >
ohne großen Aufwand restlos, dazu ohne Auftreten störender, flüchtiger Fluorverbindungen, aus Chlorwasserstoff entfernen kann, indea man ihn durch eine Schicht von oberflächenreichem AIpO, oder AIO(OH) strömen läßt. 13s war zv/ar bekannt, daß diese Verbindungen mit HF reagieren, doch konnte nicht erwartet werden, daß diese Reaktion bei Verdünnungen von wesentlich unter einem Prozent so leicht und vor allem vollständig verlaufen würde.can remove completely from hydrogen chloride without great effort and without the occurrence of disruptive, volatile fluorine compounds, indea it can be replaced by a layer of high-surface AlpO, or AIO (OH) flows. 13s it was known that these connections react with HF but could not be expected to react at dilutions substantially below one Percent would be so easy and, above all, complete.
Das entstehende AlF,, oder anfänglich auch AlOF, ist nicht flüchtig. Auch wurde sogar bei AIO(OH) als Ausgangsmaterial kein Auftreten von Wasserdampf gefunden, vielmehr wird die relativ geringe Menge Wasser von AlF, oder dem oberflächenreichen Aluminiumoxid gebunden. Die Ausnutzung des Absorptionsmittels geht zwar nicht bis zu 100 fo, aber doch relativ weit, im Mittel bis zu etwa 60 $, so daß der Materialverbrauch nicht hoch ist. Zweckmäßig benutzt man die absorbierende oxidische Aluminiumverbindung in einer körnigen oder granulierten Form, um den Strömungswiderstand gering zu halten, doch ist die Reaktion auch mit feinem, pulverförmigem Korn durchzuführen.The resulting AlF ,, or initially also AlOF, is not volatile. Even with AIO (OH) as the starting material, no occurrence of water vapor was found, rather the relatively small amount of water is bound by AlF or the surface-rich aluminum oxide. The absorption medium is not used up to 100 %, but it is still relatively far, on average up to about $ 60, so that the material consumption is not high. The absorbent oxidic aluminum compound is expediently used in a granular or granulated form in order to keep the flow resistance low, but the reaction can also be carried out with fine, powdery grains.
Das nach der Sättigung mit HF entstandene verbrauchte Absorptionsmaterial kann als wertvolle Fluor-Duelle, etwa zur Fabrikation von Kryolith weiter verwertet werden} es ist also kein wertloses und zu beseitigendes Abfallprodukt.The used up absorption material produced after saturation with HF can be used as valuable fluorine duels, for example for the manufacture of Cryolite can be recycled} so it is not a worthless waste product that needs to be disposed of.
LO Beispiel: LO example:
ο Ein Rohr von 80 mm lichter Weite wurde mit kugelförmiger Aktiv-ο A tube with a clearance of 80 mm was fitted with a spherical active
*~ tonerde, ihirchmesser 5-5 mm, in einer Schichthöhe von 200 mm ο* ~ clay, diameter 5-5 mm, in a layer height of 200 mm ο
*? gefüllt. Das Gewicht der Schicht betrug 9 kg. Durch diese Ab-O0 sorptionsschicht wurde mehrere Tage lang ein Strom von 6 m /h HCl hindurchgeleitet, der zwischen 0,25 und 0,5 HF enthielt. Unter diesen Umständen war die Verweilzeit 6 see. Erst nachdem 2,4 kg HF*? filled. The weight of the layer was 9 kg. Was prepared by this Ab-O 0 sorption for several days, a current of 6 m / h HCl passed, containing between 0.25 and 0.5 HF. Under these circumstances the residence time was 6 seconds. Only after 2.4 kg HF
— 3 —- 3 -
aufgenommen waren, ließ sich HF am Ausgang nachweisen. Der Gehalt der Oxidkugeln, die ihre Form nicht wesentlich verändert hatten, betrug am unteren Ende der Schicht etwa 22 rfo F, am oberen finde etwa 12 <fo F. were recorded, HF could be detected at the exit. The content of the oxide spheres, which had not changed their shape significantly, was about 22 rfo F at the lower end of the layer, and about 12 <fo F at the upper end .
0 9 9 0 1 / η R5 50 9 9 0 1 / η R5 5
Claims (1)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DED0045573 | 1964-10-06 |
Publications (1)
Publication Number | Publication Date |
---|---|
DE1467030A1 true DE1467030A1 (en) | 1969-01-02 |
Family
ID=7049103
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE19641467030 Pending DE1467030A1 (en) | 1964-10-06 | 1964-10-06 | Process for removing small amounts of hydrogen fluoride from hydrogen chloride |
Country Status (4)
Country | Link |
---|---|
BE (1) | BE670429A (en) |
DE (1) | DE1467030A1 (en) |
ES (1) | ES318102A1 (en) |
NL (1) | NL6512951A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS51130696A (en) * | 1975-04-25 | 1976-11-13 | Lummus Co | Separating process for hydrogen fluoride from hydrogen chloride gas |
DE19500785C1 (en) * | 1995-01-13 | 1996-07-04 | Metallgesellschaft Ag | Process for the separation of HF from hydrochloric acid |
-
1964
- 1964-10-06 DE DE19641467030 patent/DE1467030A1/en active Pending
-
1965
- 1965-10-01 BE BE670429A patent/BE670429A/xx unknown
- 1965-10-04 ES ES0318102A patent/ES318102A1/en not_active Expired
- 1965-10-06 NL NL6512951A patent/NL6512951A/xx unknown
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS51130696A (en) * | 1975-04-25 | 1976-11-13 | Lummus Co | Separating process for hydrogen fluoride from hydrogen chloride gas |
DE19500785C1 (en) * | 1995-01-13 | 1996-07-04 | Metallgesellschaft Ag | Process for the separation of HF from hydrochloric acid |
EP0721916A1 (en) | 1995-01-13 | 1996-07-17 | Metallgesellschaft Ag | Process for the separation of HF from hydrochloric acid |
Also Published As
Publication number | Publication date |
---|---|
NL6512951A (en) | 1966-04-07 |
BE670429A (en) | 1966-04-01 |
ES318102A1 (en) | 1965-12-16 |
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