Condensation method of m-,p-mixed di-(tert-butyl isopropyl peroxide)benzene

Abstract

The invention discloses a condensation method of m-,p-mixed di-(tert-butyl isopropyl peroxide)benzene. In the method, di-(2-hydroxy-2-propyl)benzene and tert-butyl hydrogen peroxide are taken as starting raw materials; perchloric acid of which the concentration is 50-52 percent by weight is taken as a catalyst; 6# solvent oil is taken as a solvent; the molar ratio of di-(2-hydroxy-2-propyl)benzene to tert-butyl hydrogen peroxide is 1:(2.30-2.90); the weight ratio of di-(2-hydroxy-2-propyl)benzene to perchloric acid is 100:(0.35-0.75); and the weight ratio of di-(2-hydroxy-2-propyl)benzene to 6# solvent oil is 100:(250-410). The method comprises the following steps of: controlling the reaction temperature at 39-56 DEG C and controlling the reaction pressure at 0-0.056MPa for performing a reduced pressure nitrogen bubbling dehydration reflux condensation reaction; after reacting to a final point, adding an alkali for terminating the reaction; washing a reaction liquid with an alkali water and water to obtain a condensation liquid; and concentrating the condensation liquid to obtain di-(tert-butyl isopropyl peroxide)benzene. The method has the characteristics of easiness in controlling reaction, short condensation reaction time, small quantity of side products and high yield.

Description

technical field [0001] The invention relates to a chemical synthesis method of organic matter, in particular to a condensation method of meta- and para-position mixed bis-(tert-butylperoxyisopropyl)benzene. Background technique [0002] At present, di-(2-hydroxy-2-propyl)benzene (DC for short) is the organic peroxide bis-(tert-butyl peroxyisopropyl)benzene (Di-(2-tert-butyl peroxy isopropyl)benzene , hereinafter referred to as DBP) and an important starting material for the intermediate monomer peroxide tert-butyl hydroperoxide (abbreviated as TBHP). The condensation synthesis technology uses concentrated sulfuric acid as a catalyst. Its disadvantage is that the reaction temperature is low, which generally needs to be controlled at 0-15°C. Overheating will easily cause decomposition and reduce the yield of DBP. At the same time, due to the strong acidity of concentrated sulfuric acid, the condensation reaction is difficult to control , During the reaction, the material is g...

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Problems solved by technology

[0002] At present, bis-(2-hydroxy-2-propyl)benzene (abbreviated as DC) is an organic peroxide bis-(tert-butylperoxyisopropyl) ) Benzene (Di-(2-tert-butyl peroxy isopropyl)benzene, hereinafter referred to as DBP) and an important starting material for the intermediate monomer peroxide tert-butyl hydroperoxide (abbreviated as TBHP), meta- and para-mixed bis -The commonly used condensation synthesis technology of (tert-butylperoxyisopropyl)benzene is to use concentrated sulfuric acid as a catalyst. Its disadvantage is that the reaction temperature is low, and generally needs to be controlled at 0-15°C. Overheating can easily cause decomposition and reduce DBP Yield; at the same time, due to the strong acidity of concentrated sulfuric acid, the condensation reaction is difficult to control, and the material is gradually carbonized in the reaction, and the color turns black, reducing product quality and yield

[0003] At the same time, the TBHP used in the above reaction contains about 30% water, but in production, the water in TBHP was not removed before the reaction, and the condensation Nitrogen bubbling was not used to remove reaction water during the reaction, which prolongs the reaction time and reduces the yield

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