It will be apparent that changes in design may be made so that the hydrogen chloride used in steps (b) and (d) are supplied separately from different supply sources, and the resulting nitrosyl chlorides are taken out separately and then collected together. To illustrate the invention further, several modes of practicing the method of the invention will be described by means ofthe following examples. The reaction can be satisfactorily carried out by blowing hydrogen chloride gas into the foregoing solution. Prolonged exposure to fire or heat can cause containers to rupture violently and rocket . Other objects and advantages of the present invention will become apparent from the description which follows: The method of the invention comprises a method of preparing nitrosyl chloride which comprises, in com-bination, the following steps: (a) reacting a mixed gas comprising nitric oxide and nitrogen peroxide with a volume of sulphuric acid thereby preparing an increased volume of solution of nitrosyl sulphuric acid in sulphuric acid; (b) reacting the solution obtained in (a) with hydrogen chloride, thereby generating nitrosyl chloride which is separated; (c) removing a volume of liquid from the spent liquor from step (b') substantially equal in volume to the volume of sulphuric acid initially used in step (a) and reacting this liquid in a subsequent step (a) with further nitric oxide and nitrogen peroxide to regenerate a solu- Patented Aug. 29, 1967 tion of nitrosyl sulphuric acid in sulphuric acid which is recycled for a subsequent operation of step (b) above; and.

A mixed nitrogen monoxide-nitrogen peroxide gas was blown into this at a temperature of 48 C. and a sulfuric acid solution of nitrosylsulfuric acid was formed which was then introduced into tank 2. nitrosyl halides, Process for the continuous preparation of nitrosyl chloride, Continuous preparation of nitrosyl fluoride, Process for the recovery of free chlorine from chlorides, Process of reacting chlorides with nitric acid. The full text of this article hosted at is unavailable due to technical difficulties. and you may need to create a new Wiley Online Library account. The concentration of nitrosylsulfuric acid in the so obtained spent liquor resulting from the secondary generation was 0.7% by weight.

In the figures, 1 is the nitrosulfuric acid preparation tank in which the mixed gas comprising nitrogen monoxide and nitrogen peroxide is reacted in step (a) with sulfuric acid to obtain the sulfuric acid solution of nitrosylsulfuric acid; 2 is the primary generating tank in which said solution is reacted with the primary hydrogen chloride gas in step (b) to generate nitrosyl chloride; 3 is the secondary generating tank for generating nitrosyl chloride by means of the secondary hydrogen chloride gas in step (d); 4 is the tank for the spent liquor resulting from the step (d); 5 is the supply tank for the sulfuric acid to be used for replenishing the sulfuric acid portion of the cycling spent liquor; 6 is the supply tank for hydrogen chloride gas; and 7 is the storage tank for the nitrosyl chloride which is generated in step (b). However, this method of obtaining nitrosyl chloride from nitrosylsulfuric acid and hydrogen chloride gas had been practiced hitherto only on a laboratory scale. (Cl. The reaction is preferably carried out at less than 50‹ C. In a cyclic process the NOCl may be oxidized to NO 2 and Cl 2 or thermally decomposed to NOOCl 2 , and the NO 2 recycled or the NO oxidized and recycled, whilst the Cl 2 may be used to chlorinate ethylene to 1 : 2- dichloro ethane which may then be cracked to give vinyl chloride and HCl, the HCl being recycled to the NOCl synthesis. Preparation of nitrosyl chloride Download PDF Info Publication number US3338887A. The latter amounted to 2,033 kg. Das NOCl(g) wurde IR‐spektroskopisch und durch Analyse charakterisiert. In order to reduce the concentration of nitrosylsulphuric acid in the spent liquor in this step (d), the reaction with hydrogen chloride is preferably at a temperature of to 200 C. The spent liquor which remains after step (d) has been carried out contains less than 3% by weight of nitrosylsulphuric acid and, as stated previously, this liquor may be utilized as an acid catalyst in the Beckmann rearrangement of cycloalkanone oxime hydrochlorides. Thus, of spent liquor resulting from the primary generation whose concentration of nitrosylsulfuric acid had fallen to 23.8% by weight was cycled to tank 1 and the remaining 10% was drawn off to the secondary generation system. 1 is a flow diagram illustrating the process for the preparation of nitrosyl chloride; and. Very toxic by inhalation. What we claim is 1. It is a yellow gas that is most commonly encountered as a decomposition product of aqua regia, a mixture of hydrochloric acid and nitric acid. Process for the preparation of cyclohexanone oxime, Process for the separation of gaseous mixtures of cyanogen chloride and hydrogen chloride, Process for preparing nitrogen trifluoride, Process for production of potassium sulfate and hydrochloric acid, Conversion of methanol to formaldehyde combination catalysts, Method of simultaneously producing chlorine dioxide and a sulfate salt, Integrated process for producing urea and melamine. The nitrosyl chloride gas has been characterized by i.r. New methods for the Preparation of Nitrosyl Chloride. Next, an example of a combination of operational steps suitable for carrying the method of the present invention into effect will be described with reference to the accompanying drawings, in which: FIG. The quantity of gas generated was 785 Nm. US3338887A US24691462A US3338887A US 3338887 A US3338887 A US 3338887A US 24691462 A US24691462 A US 24691462A US 3338887 A US3338887 A US 3338887A Authority US United States Prior art keywords acid hydrogen chloride nitrosyl Ten kg. The reaction mixture may also contain a metal (e.g. Stopped-Flow Ultra-Rapid-Scanning Fourier Transform Infrared Spectroscopy on the Millisecond Time Scale. Dr. D. K. Padma. at a temperature of 150 C. to reduce the concentration of nitrosylsulfuric acid to less than 3% by weight.

Noncombustible, but accelerates burning of combustible material. R. G. Kalbandkeri. of sulfuric anhydride from tank 5 was added to tank 1 containing 94.5 kg. In order to carry out a similar method on a commercial scale,'we have previously proposed a method of obtaining nitrosyl chloride continuously by reacting the oxides of nitrogen with sulphuric acid to obtain a sulphuric acid solution of nitrosylsulphuric acid, blowing hydrogen chloride gas into this solution and generating nitrosyl chloride, then again blowing oxides of nitrogen into the spent liquor from the nitrosyl chloride generation step in order to reproduce a nitrosylsulphuric acid solution and in order to set up a cyclic system for preparing the nitrosyl chloride by adding to the system only the oxides of nitrogen and hydrogen chloride. As the quantity used of the hydrogen chloride gas in the main process was 650 kg., when this spent liquor taken out to the outside of the system was reacted at 200 C. under the condition that 19 moles of hydrogen chloride gas was used to each mole of nitrosylsulfuric acid, the concentration of the nitrosylsulfuric acid was reduced to as low as 0.8% by weight. It is generally known to obtain nitrosyl chloride by obtaining a sulfuric acid solution of nitrosylsulfuric acid by causing a mixed gas comprising nitrogen monoxide and nitrogen peroxide, such as a nitrose gas, to be absorbed into sulfuric acid in accordance with the following Equation 1, and thereafter reacting as in Equation 2 by blowing in hydrogen chloride gas into this solution.

Considerable restrictions are also imposed as to the uses to which the nitric acid formed can be employed. Nitrosyl chloride appears as a yellow to yellowish red gas. In this continuous method water is produced constantly as indicated in Equation 1 and the water formed has to be converted into sulphuric acid by means of fuming sulphuric acid or sulphur trioxide and a part of the spent liquor has to be taken out of the cyclic system in order to maintain its material balance, or, alternatively, the water has to be taken out of the cyclic system by distillation of the spent liquor under reduced pressure.

When the nitrosylsulphuric acid content of a spent liquor exceeds 3% by weight, it cannot be used in the Beckmann rearrangement without causing adulteration of the lactam. FIG. HNO3 oder durch Reaktion von PCl3 mit NaNO3 in Anwesenheit von Wasser dargestellt werden. It is preferred to use hydrogen chloride gas in excess amounts according to the method of the present invention, normally the use of hydrogen chloride gas in an amount on the order of 5 mols to each mol of nitrosylsulfuric acid being preferred. 1280223 Nitrosyl chloride; nitrates; chlorine IMPERIAL CHEMICAL INDUSTRIES Ltd 23 March 1970 [21 April 1969] 20268/69 Heading C1A NOCl is prepared by reacting NO 2 and HCl in the presence of 65-75% w/w HNO 3 . at a temperature of 170 C. whereby the concentration of the nitrosylsulfuric acid was reduced to 0.7% by weight. Other than that it is desirable that the water content of the sulphuric acid solution of nitrosylsulphuric acid formed in step (a) does not depart from a concentration of 2 to 13% by weight of the solution; there is no restriction as to the concentration of the sulphuric acid starting material. of Science, Bangalore‐560012 (India) Search for more papers by this author. On the other hand, when the reaction with a greatly excess amount of hydrogen chloride gas is not carried out, the yield falls to about 85% Example 3 Following the process as shown in FIG. of this spent liquor in tank 9 of FIG. When the NOCl is thermally decomposed, chlorination may take place either before or after separation of NO and Cl 2 .

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