DE509405C - Process for the production of nitryl chloride - Google Patents
Process for the production of nitryl chlorideInfo
- Publication number
- DE509405C DE509405C DEI39163D DEI0039163D DE509405C DE 509405 C DE509405 C DE 509405C DE I39163 D DEI39163 D DE I39163D DE I0039163 D DEI0039163 D DE I0039163D DE 509405 C DE509405 C DE 509405C
- Authority
- DE
- Germany
- Prior art keywords
- production
- chloride
- acid
- nitryl chloride
- nitryl
- 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.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/083—Compounds containing nitrogen and non-metals and optionally metals containing one or more halogen atoms
- C01B21/084—Compounds containing nitrogen and non-metals and optionally metals containing one or more halogen atoms containing also one or more oxygen atoms, e.g. nitrosyl halides
- C01B21/0842—Halides of nitrogen oxides
- C01B21/0846—Nitrosyl chloride
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Herstellung von Nitrylchlorid Es wurde gefunden, daß sich N itrylchlorid leicht und in sehrguterAusbeute durchEinwirkung von Chlorsulfonsäure auf konzentrierte Salpetersäure darstellen läßt. Ist die Salpetersäure frei von Wasser und nitrosen Gasen, so bilden sich Chlor und Stickoxyde nicht oder mir in Spuren. Es hat sich als zweckmäßig erwiesen, die handelsübliche konzentrierte Salpetersäure (etwa 9S?,)ig) durch Zusatz von Oleum wasserfrei zu machen (ein . Gehalt an freiem SO; ist jedoch zu vermeiden) und die Chlorsulfonsäure unter Rühren und Kühlung in die Salpetersäure einfließen zu lassen. Nach der Gleichung: CISO;,H + HNO, - H_SO, -f- NO=Cl entwickelt sich in dem Maße, wie Chlorsulfonsäure zuläuft, ein gleichmäßiger Gasstrom von Nitrylehlorid, welches durch Waschen mit konzentrierter Schwefelsäure von mitgerissenen Säurenebeln und einem etwaigen Gehalt an Stickoxyden. befreit werden kann.Process for the preparation of nitryl chloride It has been found that N itryl chloride can easily and in very good yield through the action of chlorosulfonic acid can represent concentrated nitric acid. Is the nitric acid free from Water and nitrous gases, chlorine and nitrogen oxides are not formed or are formed in them Traces. It has proven to be useful to use the commercially available concentrated nitric acid (about 9S?,) ig) to make anhydrous by adding oleum (a. content of free SO; should, however, be avoided) and the chlorosulfonic acid with stirring and cooling in let the nitric acid flow in. According to the equation: CISO;, H + HNO, - H_SO, -f- NO = Cl develops more evenly as chlorosulphonic acid flows in Gas stream of nitrile chloride obtained by washing with concentrated sulfuric acid of entrained acid mist and a possible content of nitrogen oxides. freed can be.
Im Vergleich zu dem bekannten Verfahren zur Herstellung von Nitrylchlorid durch Ozonisieren des N itrosylchlorids stellt das Verfahren gemäß der vorliegenden Erfindung eine erhebliche Vereinfachung und Verbilligung dar. Man verwendet leicht zugängliche und wohlfeile Ausgangsmaterialien und kann das Produkt in einfacher Apparatur herstellen.Compared to the known process for the production of nitryl chloride ozonizing the nitrosyl chloride provides the process according to the present invention Invention represents a considerable simplification and cheaper. One uses easily accessible and inexpensive raw materials and can produce the product in a simpler way Manufacture apparatus.
Beispiel In 63,o- 9,I,q.5,ige Salpetersäure läßt man unter Rühren langsam i 16,5 g Chlorsulfonsäure einfließen (zweckmäßig unter die Oberfläche der Salpetersäure) und hält durch Kühlung das Reaktionsgemisch auf etwa 5 bis i o°. Das sich stetig entwickelnde N itr ylchlorid wird mit 96"'oiger Schwefelsäure gewaschen und durch Tiefkühlung kondensiert. Man erhält 73 bis 7.4. g flüssiges Nitry lchlorid, was einer Ausbeute von rund 9o °1" der Theorie entspricht. EXAMPLE 1 6.5 g of chlorosulfonic acid are slowly poured into 63.0-9, I, q.5, nitric acid with stirring (expediently below the surface of the nitric acid) and the reaction mixture is kept at about 5 to 10 ° by cooling. The steadily developing nitryl chloride is washed with 96% sulfuric acid and condensed by freezing. 73 to 7.4 g of liquid nitryl chloride are obtained, which corresponds to a yield of around 90 ° 1 "of theory.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEI39163D DE509405C (en) | 1929-08-30 | 1929-08-30 | Process for the production of nitryl chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEI39163D DE509405C (en) | 1929-08-30 | 1929-08-30 | Process for the production of nitryl chloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE509405C true DE509405C (en) | 1930-10-07 |
Family
ID=7189989
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DEI39163D Expired DE509405C (en) | 1929-08-30 | 1929-08-30 | Process for the production of nitryl chloride |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE509405C (en) |
-
1929
- 1929-08-30 DE DEI39163D patent/DE509405C/en not_active Expired
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