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Isolation of tert-butyl hydroperoxide

Journal Article · · J. Appl. Chem. USSR (Engl. Transl.); (United States)
OSTI ID:6290492
A hazard-free method of purifying tert-butyl hydroperoxide (TBH) consists in using an alkali extraction. To isolate it in this way, the mixture was treated at 0-10/sup 0/C with a 20% sodium hydroxide solution. After separation of the TBP, the solution of the sodium salt of TBH was washed with ether and acidified with sulfuric acid. The TBH was separated in the form of an organic layer, which was washed with NaHCO/sub 3/ and H/sub 2/O, and was dried with Na/sub 2/SO/sub 4/. In the present work the authors present parameter information on the yield and concentration of TBH from experience in using the alkali extraction method. TBH of a purity up to 96% has been obtained from a crude product containing 30-70% hydroperoxide. A very pure hydroperoxide is obtained when a 20% NaOH solution is used to precipitate the Na-TBS salt, at an NaOH:TBH ratio of 1.3:1 and a temperature of 0-5/sup 0/C. The crystallization time for the salt should be not less than 2 h; the time for drying the precipitate, 20 h. A 50-80% H/sub 2/SO/sub 4/ solution can be used to dissolve the salt (using it until a pH of 6 is developed).
Research Organization:
Polytechnic Institute, Szczecin (Poland)
OSTI ID:
6290492
Journal Information:
J. Appl. Chem. USSR (Engl. Transl.); (United States), Journal Name: J. Appl. Chem. USSR (Engl. Transl.); (United States) Vol. 61:5; ISSN JAPUA
Country of Publication:
United States
Language:
English