Abstract:
NITROALCOHOLS ARE PRODUCED BY REACTING A NITROPARAFFIN WITH A STOICHIOMETRIC EXCESS OF FORMALDEHYDE, SAID EXCESS BEING FROM ABOUT 5 TO 60% EQUIVALENTS, DEIONIZING THE REACTION PRODUCT THEREOF TO REMOVE THE METAL ION OF SAID CATALYST FRACTIONATING SAID DEIONIZED REACTION PRODUCT WITH METHANOL IN THE PRESENCE OF A MINERAL ACID, TOLUENE SULFONIC ACID OR CATION EXCHANGE RESIN IN AN AMOUNT SUFFICIENT TO CATALYZE THE REACTION OF THE EXCESS OF THE FORMALDEHYDE AND METHANOL, THE METHANOL BEING USED IN AN AMOUNT SUFFICIENT TO REACT WITH THE ALDEHYDE REMAINING IN SAID FRACTIONATED PRODUCT, AND REMOVING THE REACTION PRODUCT OF SAID FORMALDEHYDE AND METHANOL FROM THE RESULTING MIXTURE.
Abstract:
1,218,706. Separation of nitroalkanes and alkanes. COMMERCIAL SOLVENTS CORP. 9 July, 1969 [26 Aug., 1968], No. 34622/69. Heading C2C. [Also in Division C5] A mixture of one or more nitroalkanes having 2 to 4 carbon atoms and one or more alkanes (including cycloalkanes) having 5 to 9 carbon atoms is separated by (a) adding methanol to the mixture in an amount sufficient to initiate co-distillation with the alkane or alkanes when said mixture is heated, (b) heating and codistilling the alkane-methanol thereby effecting separation of the alkane or alkanes and producing a residue of nitroalkane or nitroalkanes and methanol, and (c) separating the methanol from the nitroalkane or nitroalkanes. The alkanemethanol distillate may be condensed into two layers, and the lower methanol layer returned to the distillation unit until alkane no longer comes over in the distillate. The upper alkane is suitable for re-use without further treatment or it can be freed from methanol by distillation or washing with water.
Abstract:
Nitromethane is recovered from mixtures with higher nitroalkanes by adding to said mixtures sufficient water and C6- 8 alkane or cycloalkane to form an azeotropic mixture with said nitromethane, and heating the mixture to distil off said azeotrope. The said azeotrope condenses into three layers, the lowest of which contains the nitromethane with minor amounts of water and alkane. The water and alkane may be removed by further distillation up to 101.5 DEG C.