Preparation method of 3,6,9-triethyl-3,6,9-trimethyl-1,4,7-triperoxynonane

Abstract

The invention belongs to the field of organic synthesis and discloses a preparation method of 3,6,9-triethyl-3,6,9-trimethyl-1,4,7-triperoxynonane. The preparation method mainly comprises peroxidatic reaction, condensation polymerization reaction and a blending refining process and particularly comprises the following steps of: stirring concentrated sulfuric acid used as a catalyst as well as hydrogen peroxide and methyl ethyl ketone used as raw materials at the temperature condition of 10-50 DEG C for reacting for 0.5-6.0h, then cooling to 20 DEG C, standing for layering, and retaining an organic layer, wherein the molar ratio of the methyl ethyl ketone to the hydrogen peroxide to the concentrated sulfuric acid is 3:(1-6):(0.3-3); neutralizing the reaction solution with aqueous alkali with the concentration of 10-50% in the organic layer, carrying out washing refining, removing byproducts, after the reaction, standing, cooling, separating the solution, drying, and filtering to obtain a pure target product; and adding a diluent to obtain a finished product. The preparation method disclosed by the invention is simple in reaction process, higher in yield, safe and environment-friendly.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of 3,6,9-triethyl-3,6,9-trimethyl-1,4,7-triperoxynonane. Background technique [0002] Organic peroxides are an important and special chemical substance with strong oxidizing properties. The peroxygen bond (-O-O-) in organic peroxide molecules is easily decomposed into active free radicals and oxygen when heated. It has the ability to release free radicals, so it is widely used in polypropylene, polyethylene, polyvinyl chloride, polystyrene, polyester, synthetic resin, synthetic rubber and other industries and other industries. Free radical polymerization is an efficient method for the large-scale production of various olefinic polymers. The advantages of free radical polymerization are that there are many kinds of monomers that can be polymerized, the reaction conditions are mild and easy to control, and it is easy to realize industrial producti...

AI Technical Summary

Problems solved by technology

[0006] ①The presence of a large number of inert diluents and solvents reduces the concentration of raw materials. In order to achieve the desired synthesis effect, the input amount and concentration of raw materials must be increased, especially the use of high-concentration concentrated sulfuric acid and hydrogen peroxide, which is harmful to raw material storage and safe production. pose a major safety hazard

[0007] ②The reaction rate is reduced, the effective contact between raw materials is reduced, and the stirring effect is reduced. In order to achieve a high conversion rate, a longer reaction time is required, which greatly prolongs the reaction process

Due to the lengthening of the reaction time, the probability of various safety accidents is increased, the labor and energy consumption of personnel are increased, and the requirements for equipment are higher, which is not conducive to energy conservation and environmental protection.

[0008] ③The addition of a large amount of inert diluents and solvents increases the difficulty of removing by-products and impurities generated during synthesis, resulting in increased processing capacity and reduced processing effects, resulting in insufficient product purity and high impurity content

[0009] ④The inert diluent and solvent are added before the reaction. Due to the uncertainty of the reaction process, in order to ensure the active oxygen content of the organic peroxide in the finished product, a second deployment is required, resulting in material loss and energy consumption

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