Preparation method for isoalkylalkenyloxysilane

Abstract

The invention discloses a preparation method for isoalkylalkenyloxysilane. The preparation method comprises the following steps: adding alkyl ketone, an acid binding agent and a catalyst in a mass ratio of 1000: 1090: (1-5) into a reaction vessel, and carrying out heating under stirring until the temperature of the reaction vessel is 40 DEG C; maintaining the temperature of the reaction vessel tobe 20 to 60 DEG C, adding chlorosilane into the reaction vessel drop by drop within 20 to 40 min, carrying out heat-preserved reflux after completion of addition of chlorosilane until the content of isoalkylalkenyloxysilane in the reaction vessel is greater than 30%, and hermetically filtering out a tertiary amine hydrochloride solid so as to obtain a first filtrate; subjecting the first filtrateto distillation at normal pressure so as to first mother liquor; adding solid paraffin and a chloride ion neutralizer into the first mother liquor, maintaining the temperature of the reaction vessel to be 40 to 60 DEG C, carrying out a reaction for 1 to 3 h, and then carrying out filtering under the condition that vessel temperature is 35 to 40 DEG C so as to obtain a second filtrate; and subjecting the second filtrate to vacuum rectification at a temperature of 124 to 126 DEG C and a pressure of 0.0130 to 0.0140 MPa so as to obtain isoalkylalkenyloxysilane. The isoalkylalkenyloxysilane prepared in the invention has a purity of 94% or above and yield of more than 63%.

Description

technical field [0001] The invention relates to a preparation method of isoalkenyloxysilane, in particular to a method for preparing isoalkenyloxysilane by the isomerization method of alkyl ketone. Background technique [0002] Isoalkenyloxysilane is a kind of silane crosslinking agent with special application. Because the molecular structure contains isoalkenyloxy group and functional group of alkyl, alkenyl or phenyl, it is widely used in the treatment of polyethylene, polypropylene, Unsaturated polyester and other polymers are modified to give them excellent pressure cracking resistance, memory, wear resistance and impact resistance; to improve the affinity between glass fibers, inorganic fillers and vinyl-reactive resins, It is often used for the aging resistance of silane cross-linked polyethylene cables and pipes; it can be copolymerized with acrylic paints to make special exterior wall coatings, which have good weather resistance and dust resistance; it is used for cr...

AI Technical Summary

Problems solved by technology

At present, there are few reports on the synthesis of isoalkenyloxysilanes. Usually, cuprous chloride is used as a catalyst, triethylamine is used as an acid-binding agent, and toxic aromatic compounds are used as solvents. The reaction time is as long as 20 to 50 hours. Reaction of alkyltrichlorosilane and alkyl ketone to produce alkylisoalkenyloxysilane silane yield less than 50%

Among them, there are literature reports that the yield of vinyl triisopropenyloxysilane is 45.7%, and related literature reports that the yield of phenyl triisopropenoxysilane is 43%. The isoalkenyloxysilane prepared by the above method In addition to the low yield, there are also the following disadvantages: the use of toxic benzene compounds as solvents, low operational safety, long reaction time, high cost, and high temperature and high pressure are required, which is not conducive to industrial production and application