No. To illustrate the invention further, several modes of practicing the method of the invention will be described by means ofthe following examples. nitrosyl halides, Process for the preparation of nitrosyl chloride, Process for the recovery of free chlorine from chlorides, Process of purifying chlorine and reaction therefor, Production of omega-amino dodecane acid lactam, Method of producing nitroso compounds or oximes, Method for the preparation of nitrosyl chloride, Continuous production method of chlorine dioxide, Production of epoxy compounds from olefinic compounds. While the spent liquor which has been taken out to the outside of the system by the above method can be used for other purposes as sulfuric acid by being converted thereto by the conventional nitric oxide process for sulfuric acid manufacture, the recovery of the oxides of nitrogen which are formed in this instance is a disadvantage from the commercial standpoint. and it contained therein 42.8% of nitrosylsulfuric acid. Dept. Thus, of the spent liquor resulting from the primary generation whose concentration as nitrosylsulfuric acid had declined to 31.4% was cycled to tank 1, and the remaining 20% was drawn off to the secondary generation system. The reaction can be satisfactorily carried out by blowing hydrogen chloride gas into the foregoing solution. Learn about our remote access options, Dept. 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. 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. 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. Enter your email address below and we will send you your username, If the address matches an existing account you will receive an email with instructions to retrieve your username, I have read and accept the Wiley Online Library Terms and Conditions of Use. was reacted with the primary hydrogen chloride gas in a greatly excessive amount of 153 kg. And from this was obtained e-caprolactam of good quality. With this, which amounted to 10.5 kg. In this instance,- the foregoing solution contained'45% by weight of nitrosylsulfuric acid, and the quantity formed was 963 kg. 1 is a flow diagram illustrating the process for the preparation of nitrosyl chloride; and. 1, the sulfuric acid solution of'nitrosylsulfuric acid formed at tank 1 by' blowing a nitrose gas into sulfuric acid of 20% by weight concentration at a temperature of 40 C. was introduced to the primary generation tank 2. of an 11.2% fuming sulfuric acid fed from tank 5 was blown in nitrose gas at a temperature of 50 C., after which the sulfuric acid solution of nitrosylsulfuric acid which was formed was introduced to the primary generation tank 2. Although the hydrogen chloride gas may contain some water in this instance, as an increase in the water content as well as an increase in the temperature accelerates the decomposition of the nitrosylsulfuric acid and/or nitrosyl chloride, it is advisable to blow in as anhydrous a gas as possible. The NO 2 and HCl may be used in any convenient liquid or gaseous form, and the NO 2 may be formed in situ from NO and O 2 or alternatively nitrogen trioxide (NO+NO 2 ) may be used, with or without O 2 . Nitrosyl chloride is the chemical compound with the formula NOCl. In this instance, the quantity of the above solution introduced was 10,410 kg. By this means it is possible to achieve substantially complete utilization of the nitrosyl group in the nitrosylsulphuric acid produced in step (a).