A continuous-flow synthesis process of tert-butyl peroxyneodecanoate without amplification effect

Abstract

The present invention provides an amplification-effect-free continuous flow synthesis process of tert-butyl peroxyneodecanoate. According to the synthesis process, tert-butyl hydroperoxide, an alkaliliquid and neodecanoyl chloride are used as raw materials and are continuously and sequentially subjected to an alkalization reaction, an esterification reaction and a quenching step to obtain the tert-butyl peroxyneodecanoate; and the synthesis process is performed in an integrated continuous flow reactor, the reaction raw materials such as the tert-butyl hydroperoxide, the alkali liquid and theneodecanoyl chloride are continuously added into the material inlet of the integrated continuous flow reactor, and the tert-butyl peroxyneodecanoate is continuously obtained from the material outlet of the integrated continuous flow reactor, wherein the amplification effect does not exist, and the total reaction time is less than or equal to 180 s. Compared with the traditional production process,the synthesis process of the present invention has advantages of substantially improved temperature, substantially shortened total reaction time, no amplification effect, stable product index and good reproducibility.

Description

Technical field [0001] The invention relates to the field of chemistry, in particular to a continuous flow synthesis process of tert-butyl peroxide neodecanoate. Background technique [0002] Peroxyesters are important organic peroxides, such as tert-butyl peroxyneodecanoate, cumyl peroxyneodecanoate, and 1,1,3,3-tetramethylbutyl peroxyneodecanoate ester. Peroxyester is a low-temperature initiator of free radical polymerization, widely used in polyethylene (LDPE), polyvinyl chloride (PVC), polystyrene (PS), styrene copolymer (such as ABS), polymethacrylic acid Production areas such as ester (PMMA) and polyvinyl acetate (PVAc). At the same time, it is also a high temperature curing agent for unsaturated polyester. [0003] Since Baeyer and Villiger reported that the first peroxyester was produced in 1901, many peroxyester products have come out, ranging from laboratory scale to industrial scale preparation. At present, generally speaking, most of the preparation of peroxyesters ...

AI Technical Summary

Problems solved by technology

[0016] Although a small number of continuous flow processes have been developed, there are problems: there is inevitably an amplification effect, which brings many uncertainties to further industrial applications; some continuous flow processes are not fully reacted in a short period of time, and need to increase The reaction time is used to increase the conversion rate, resulting in a decrease in production efficiency

Compared with the batch process, although the advantages of the microreactor in mass and heat transfer have been used to improve the reaction temperature of the esterification reaction and shorten the reaction time to a certain extent, there are still many shortcomings: one is that the esterification reaction temperature is still low. Low (15-35°C), resulting in insufficient reaction; second, in order to further fully react and cool down, a delay line must be used to achieve the purpose of the reaction

That is to say, the scheme fails to completely avoid the problem of amplification effect in the batch process, and increases the difficulty of process amplification, causing problems in process reliability, product quality stability and production safety; third, due to insufficient reaction, delay pipelines are used , resulting in a longer total reaction time, usually at least 5 minutes or even as long as 20 minutes, resulting in low production efficiency

In addition, the tubular reactor needed for the delay line needs to occupy a certain amount of space, resulting in a waste of space

[0020] As can be seen from the prior art, the synthesis technique of existing tert-butyl peroxyneodecanoate all has amplification effects in various degrees, and because the reaction temperature is low, the total reaction time is too long, and the productive rate is not high, increasing the difficulty of industrialization

Unable to achieve large-scale production, which limits its application

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