发明名称 |
Process for preparing solid amine oxides |
摘要 |
A highly pure, white, solid amine oxide is prepared in high yield with minimal decomposition of the solvent by (A) reacting a tert-amine with a 15-20% stoichiometric excess of concentrated hydrogen peroxide at 50 DEG -55 DEG C. in the presence of controlled amounts of carbon dioxide and ethyl acetate until the reaction mixture contains 35-45 % by weight of ethyl acetate and less than 0.8% by weight of unreacted amine, (B) catalytically decomposing residual hydrogen peroxide, (C) separating the reaction mixture from the decomposition catalyst, (D) cooling the reaction mixture to 0 DEG C. to form a slurry, (E) centrifuging the slurry to separate the amine oxide, and (F) vacuum drying the amine oxide at ambient temperature-the reaction mixture being diluted to an amine oxide content of 25-30% by weight with additional ethyl acetate or a mixture thereof with a co-solvent, such as a low-boiling n-alkane, after the completion of Step A and prior to the beginning of Step D.
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申请公布号 |
US5693861(A) |
申请公布日期 |
1997.12.02 |
申请号 |
US19930078500 |
申请日期 |
1993.06.21 |
申请人 |
ALBEMARLE CORPORATION |
发明人 |
SMITH, REBECCA F.;CHEN, Y.-D. MARK;WILSON, JR., R. WOODROW;SHAH, MAYUR P.;SMITH, KIM R.;MCGEE, SHARON B. |
分类号 |
C07C291/04;(IPC1-7):C07C291/00 |
主分类号 |
C07C291/04 |
代理机构 |
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代理人 |
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主权项 |
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地址 |
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