| 摘要 |
Preparation of an organo alkoxydialkylsilane by introduction of an alcohol onto a mixture of silane and an organic solvent phase with elimination of the halogeno acid formed, recovery of the organo alkoxydialkylsilane and recycling of the solvent. The preparation of the organo alkoxydialkylsilane of formula R 1>O --- (R 2>)(R 3>)Si --- (CH 2) 3---A (III) comprises contacting an alcohol R 1>OH (I) with a silane of formula Hal --- (R 2>)(R 3>)Si - (CH 2) 3--- A (II) to establish the equilibrium reaction: Hal - (R 2>)(R 3>)Si --- A + R 1>OH -----> R 1>O --- (R 2>)(R 3>)Si --- (CH 2) 3--- A + H-Hal; Hal : Cl, Br or I; R 1>1 - 15C alkyl or 2 - 8C alkoxyalkyl; R 2>, R 3>1 - 6C alkyl or phenyl; A : a detachable group which is either Hal, para-R 0>-C 6H 4-SO 2-O-, R 0>-SO 2-O- or R 0>-COO-; R 0>1 - 4C alkyl. The reaction is operated at or differing from atmospheric pressure in a stirred reactor with a distillation column and condenser. A flow of the alcohol is introduced in a mixture of the silane (II) and an organic solvent phase ; the solvent phase may be mixed, in part, with the alcohol ; the halogenated acid, H-Hal formed is eliminated by entrainment with the solvent phase. The reaction product (III) is recovered by any appropriate method. The process is characterized by: (1) the silane(II) and solvent mixture is heated to its boiling point and alcohol is introduced when the condenser is charged and in a stationary reflux state; (2) the solvent phase is chosen so as to eliminate the formed halogen acid by vapor entrainment and to present a liquid-vapor equilibrium with the alcohol to allow an alcohol concentration of 5 - 30 %; (3) the mode of introduction of the alcohol follows a procedure which avoids an accumulation of the acid H-Hal in the reactor does not exceed 90 % of the acid formed; (4) the total quantity of alcohol introduced is such that the molar ratio alcohol(I) / silane (II) is between 1 and less than 3; (5) the quantity of solvent in the reactor is a function of the nature of the phase and is determined so that the concentration of alcohol in the alcohol/solvent phase should be 5 - 30 %. An independent claim is also included for the preparation of organosilicon polysulfides from the organo alkoxysilanes obtained. |
