CS200396B1 - Process for the production of cyclic nitrezeaalnevnitrosolysis by hexamethylenetetramlan - Google Patents

Abstract

The invention relates to a method for the production of cyclic nitrosoamines from hexamethylenetetramine. The subject of the invention is nitroselysis under the action of nitrites in an acidic environment, which is created by dosing an acidic gas or an acidic mixture of gases or substances forming an acidic environment "in situ", while the conditions are chosen so that any excess of the acidic component is subsequently purged with gas and/or suction under reduced pressure.

Description

The invention aa relates to a process for the production of cyclic nitrosoamines, wherein the conditions of eu called to substantially influence the yield and quality of the product and to affect the economy.

BOTOXY PROCEDURES ARE IMPOSED FOR THE PRODUCTION OF CYCLOCOLIC NITRESOAMINES OF NITROGELISION OF HEXAMOTHYLENEETHERAMIAN CONTAINED KE, 5-ENDEMETHYLE-3,7 ** UIAITRAZO-1,3,5,7-TETRAYL EYKLOOKTEAU for the use of native acids, e.g. Mayer P., Ber. 21 2883 (1883) discloses that dinitrosopentamethylenetetramine is formed by the treatment of sodium nitrite with urotropin in the presence of a small amount of nitric acid at low temperature (~ 8 ° C), the reaction mass having a pH in the range of 3-6. 70 jjBaehman V. £., Bono N. 0. Am. Chem. Soo., 73, 2777 (1951) J shows the effect of pH on nitroso-lononine yield when adding Hydrocarboxylic acid and sodium nitrite solution to urotrepline solution at 2 to 5 ° C and considers maximum yield at pH 3. It also considers a nitrosation with sodium nitrite in oeto acid , leading to long-term fusion. The maximum yield (76 ¢) of the diaitroso compound is obtained at pBb of 3 to 4 and concludes that the order of component mixing for this prooos does not affect. In obtaining the aritroso compound using Bashmsn hydrocyanic acid, potassium phthalate was added as a buffer to maintain the pH of the environment in the range of 3-4. Anboratoin P «, My. poudroe, 33, 227 (1951) and also Boujjol G., Mém. peudros, 34, 712 (1952) used sulfuric acid to obtain the palitroso compound. The authors consider that a mixture of dl- and tri-nitroso-lononin is formed in a largely acidic environment. The use of sulfuric acid is disclosed in Indian Patent 67,677, as well as Japanese Patent 21,533, employing sulfuric acid in the second step in combination with ammonium hydroxide.

The drawbacks of these processes are mainly due to the fact that they are problematic, the preparation of fertile acids, the consumption of water and neutralization, the high salt content in edpadaýdh water and the like. All the weaves and the flaws of the prior art rioii tanto invention.

The aforementioned drawbacks are eliminated by a process for the production of cycloocyclic nitrazoomines by aitroselysis of hexamethyleneteretramine by acidic nitrates at pB 1 to 6 and a temperature of -5 to 35 ° C according to the invention, which is based on the fact that the acid medium is and / or the substances form an acidic environment "in situ", continuously, semi-continuously and / or kentinuitae into the reaction mass, preferably into the lower part thereof, which possible excess is collected in the Salts, preferably by blowing gas and / or sucking off the reduced pressure and these derivatives are lysed.

As acid gas and / or acid exchange gases and / or alloys, the acidic environment in situ may be used as a chlorine, hydrogen halide, sulfur dioxide or mixed sulfur or nitrogen oxides. Excellent results have been obtained by using natural gas with less acid or inort gas, e.g. air, nitrogen and the like. Good results and the use of substances that form a acidic environment in the sieve ^{8 and, for} example, are useful. thionyl chloride, sulfur trichloride, oic acid, and padzahn®. Good results have been lost in reeycleage of acidic dysplasia.

Okre® nitr & terosial amime colosyme, homethylenetetramine can be converted by this method. nitrosoia of secondary aliphatic or arcmatic asalns.

The nitroelectric process is illustrated by the following examples.

Example X

To a 50 L reactor equipped with mixing and ehladamim, ea introduced 12.5 L of water β containing 2.07 kg of hexamethylenetetamine and 2.79 kg of sodium nitrite. After cooling the system to 0, hydrogen chloride was introduced into the bottom of the reactor over a period of 30 minutes at a rate of 1.3 kg. The temperature during the process was kept between 0 and 5 ° C and the pg of the reaction system was between 3 and 4. After 10 minutes of reaction, the solution was purged with air and neutralized with 0.20 l 27 of ammonium hydroxide. 2,60 kg.

EXAMPLE 2 A reactor of Example 1 was converted to heaeamethylenetetramine nitrosate using 1.9 kg of oic acid anhydride as the acid component e and the product obtained after neutralization and drying was 2.57 kg.

Claims (3)

Extracts have been used to produce acid-forming substances in a liquid, thionyl chloride, sulfur sulfide, and anhydride, and the like. The bisphosphonates were resolved by cycloocyclic chlorides. The tertiary amine, hemamethylenetetramine, tertiary amine, Okre® nitrosolyses can be run in the same way as the N-nitrosoacetic acid, e.g. EXAMPLE X In a reactor of 50 [mu] l equipped with agitation and oliladea, 12.5 iv of 2 kg of hoxamethylenetotramine and 2.79 kg of sodium nitrite were introduced, after being pumped into the reactor and fed to the bottom of the reactor during 30 had a hydrogen chloride content of 1.3 kg. The temperature during the process and kept between 0 and 5 ° C and the pg of the reaction system in rosaa 3 to 4. 1 27 ammonium hydroxide. Filter and oil wash, wash with water, and wash was 2.10 kg · Example 2 tore Reactor in Example 1a and provided nitrosulphene ethylene traminin, while using acidic anhydride at 1.9 kg · Acid the product of neutrallysis and drying was 2.57 kg of the object of the invention, a process for the production of cyclic nitrosoaldehyde nitrousysis of hexamethylenetetramine by affixing nitrites to a pH of 1 to 6 at a temperature of - 5 to 35 ° C, characterized in that the acid formed by metering the acid gas and / or acid gases of the gases and / or the substances forming the acidic composition "in situ", breaking, pelletizing and / or contaminating the reaction mass, preferably into the bottom thereof, which may be any excess. and, in Salč, stripped off, preferably by blowing gas and / or aspirated under reduced pressure, and the obtained nitro derivatives are isolated from 2. The process according to claim 1, characterized in that sulfuric oxide, sulfur dioxide, sulfur dioxide, hydrogen chloride and / or sieve-forming acid are preferably used as acidic gas and preferably by decomposition of ooji anhydride, thionyl chloride and the like. sulfuryl chloride; 3. The method according to claim 1, wherein the acidic gases are diluted and / or disintegrated from the liquid mass, preferably by air, with nitrogen or carbon dioxide.