Continuous flow synthesis process of tert-amyl hydroperoxide

Abstract

The invention relates to the technical field of chemistry and chemical engineering, in particular to a continuous flow synthesis process of tert-amyl hydroperoxide. The continuous flow synthesis process of tert-amyl hydroperoxide comprises the following steps: in an integrated continuous flow reactor, reacting sulfuric acid with hydrogen peroxide to generate peroxymonosulfuric acid; and carrying out esterification reaction on peroxymonosulfuric acid and tert-amyl alcohol, and quenching to obtain tert-amyl hydroperoxide. By adopting the synthesis process, the reaction process is optimized, thegeneration of byproducts is reduced, the product quality is stable, the product yield is improved, the product yield is 99% or above, and the purity is 91% or above; the total reaction time is less than or equal to 180s. Compared with the traditional production process, the reaction temperature is greatly increased, the total reaction time is greatly shortened, the product index is stable and thereproducibility is good.

Description

technical field [0001] The invention relates to the technical field of chemistry and chemical engineering, in particular to a continuous flow synthesis process of tert-amyl hydroperoxide. Background technique [0002] Organic peroxides are derivatives after one or two hydrogen atoms in the hydrogen peroxide molecule are replaced by organic groups, and its general formula is R-O-O-R. At present, the industrial organic synthesis oxidants mainly include tert-amyl hydroperoxide (TAHP) and the like. Tert-amyl hydroperoxide (TAHP), also known as t-amyl hydroperoxide, is a commonly used initiator for free radical reactions. It is characterized by good thermal stability, safe use, and easy control; below 50 °C, its The activity has no obvious change within three months, and there is no need for high-cost frozen storage, and can be used in the fields of emulsion polymerization, water phase polymerization, solidification and graft polymerization. TAHP is also widely used in styrene ...

AI Technical Summary

Problems solved by technology

[0003] From the prior art, it can be seen that the existing synthesis techniques of tert-amyl hydroperoxide (TAHP) all have amplification effects in different degrees, leading to industrial scale-up It will consume a lot of manpower and material resources and there are many uncertainties; there are also problems with the reliability of the process after amplification, and the product quality is unstable and difficult to control; at the same time, the production process lacks flexibility and has potential safety risks; The total reaction time is too long, and the yield is not high, which reduces the production efficiency, which increases the difficulty of industrialization

The inability to achieve mass production limits its application

[0004] Chinese patent CN101298429A discloses a production method of di-tert-butyl peroxide, which mixes a certain concentration of sulfuric acid, hydrogen peroxide and phosphotungstic acid, Add tert-butanol to the mixed solution to react to obtain a mixture of tert-butyl hydroperoxide and di-tert-butyl hydroperoxide. This method adds phosphotungstic acid and stabilizers, which increases the cost and difficulty of post-treatment, and the product It is a mixture of tert-butyl hydroperoxide and di-tert-butyl peroxide, which needs to be separated by pressurized distillation, which increases the processing cost. In addition, the method uses 35% concentrated sulfuric acid, which increases the waste water after reaction.

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