Ketazine methyl ethyl

Peroxide-Ketazine Process. Elf Atochem in France operates a process patented by Produits Chimiques Ugine Kuhhnaim (PCUK). Hydrogen peroxide (qv), rather than chlorine or hypochlorite, is used to oxidize ammonia. The reaction is carried out in the presence of methyl ethyl ketone (MEK) at atmospheric pressure and 50°C. The ratio of H202 MEK NH2 used is 1 2 4. Hydrogen peroxide is activated by acetamide and disodium hydrogen phosphate (117). Eigure 6 is a simplified flow sheet of this process. The overall reaction results in the formation of methyl ethyl ketazine [5921-54-0] (39) and water ... 

The methyl ethyl ketazine forms an immiscible upper organic layer easily removed by decantation. The lower, aqueous phase, containing acetamide and sodium phosphate, is concentrated to remove water formed in the reaction and is then recycled to the reactor after a purge of water-soluble impurities. Organic by-products are separated from the ketazine layer by distillation. The purified ketazine is then hydrolyzed under pressure (0.2—1.5 MPa (2—15 atm)) to give aqueous hydrazine and methyl ethyl ketone overhead, which is recycled (122). The aqueous hydrazine is concentrated in a final distillation column. 

Methyl ethyl ether, 10 567 Methyl ethyl ketazine (MEK), 13 582, 583 Methyl ethyl ketone (MEK), 13 700 14 581 adipic acid solubility, l 555t azeotrope with methanol, 8 801 in MEK—MIPK—water system, 22 304-305, 306, 307 peroxide, 14 292... 

The reaction pathway involves the formation of an intermediate that is able to oxidize ammonia to a hydrazine derivative. The methyl ethyl ketazine is insoluble in the reaction mixture and is separated by decantation and is then purified by distillation. The purified ketazine is hydrolyzed under pressure (0.8 to 10 MPa) to give concentrated aqueous hydrazine and MEK that is recycled132. 

However, Atochem uses hydrogen peroxide as the oxidant with methyl ethyl ketone to form the ketazine intermediate.313 The ketazine forms as a separate phase in the reaction, and is then purified before hydrolysis to hydrazine and ketone re-cycle. No salt or other aqueous effluent is produced, making the process relatively environmentally benign. It is operated at a 10 kilo-tonne per year scale and now represents nearly 25% of the world hydrazine production (Figure 3.84). 

Kaur, R., Machiraju, R., and Nigam, K.D.R (2007) Agitation effects in a gas-liquid-liquid reactor system methyl ethyl ketazine production. Int. /. Chem. Reactor Eng., S, 1-19. 

Subha, R. Praveena, S. Ramesh, B. V. S. Virendra, U. Prasad, D. H. L. Vapor-hquid equilibrium in methyl ethyl ketone + ketazine and liquid-hquid equilibrium in water + ketazine mixtures. J. Chem. Eng. Data 2001, 46, 1497-1498. 

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