Bis(t-butylperoxyisopropyl)benzene production method

Abstract

The present invention provides a bis(t-butylperoxyisopropyl)benzene (abbreviated as BIPB) production method, wherein a condensation dehydration reaction is performed under a negative pressure condition by adopting di-(2-hydroxyisopropyl)benzene and a t-butyl hydrogen peroxide aqueous solution as raw materials, adopting a perchloric acid aqueous solution as a catalyst, and by adopting toluene as a solvent, such that the loss of t-butyl hydrogen peroxide is reduced, the side effect is less, the conversion rate of the raw materials is improved, the BIPB product having high yield and high purity is obtained, and the production cost is reduced.

Description

technical field [0001] The invention relates to a production method of an organic peroxide, in particular to a production method of bis(tert-butylperoxycumyl)benzene. Background technique [0002] 1,3(1,4)-bis(tert-butylperoxyisopropyl)benzene (BIPB for short) is an upgraded product of dicumyl peroxide (DCP), commonly known as "odorless DCP", which is second only to The dialkyl organic peroxide crosslinking agent of DCP was industrialized abroad in the early 1960s. new type peroxide products. The BIPB molecule contains two peroxy bonds, which belong to the diperoxide compound, and the molecular formula is C 20 h 34 o 4 , molecular weight 338, its theoretical active oxygen content is 9.45%. Pure m-BIPB is a white crystal with a melting point of 50-52°C; pure p-BIPB is a white crystal with a melting point of 77-79°C; the melting point of m-BIPB and p-BIPB mixed is 45-55°C. For decades, there have been two types of BIPB products available on the market: a mixture of m-BIP...

AI Technical Summary

Problems solved by technology

[0014] (1) Sulfuric acid is greatly excessive, and every ton of BIPB product synthesized will produce 3 to 4 tons of deep black and red waste sulfuric acid with a concentration of 50% to 60%, which contains tert-butyl hydroperoxide, BIPB and various acid decomposition by-products , can neither be recycled, but also difficult to deal with discharge, which is very unfavorable to environmental protection;

[0015] (2) Owing to using a large amount of acid catalysts, the reaction speed is too fast (about 1 hour), because tert-butyl hydroperoxide, DC and BIPB and reaction intermediate monoperoxide are all very unstable to acid, the side reaction The speed will also increase, which can be controlled in the laboratory. In industrial production, once there is a power failure or failure of the refrigeration system or agitator, it is likely to cause a safety accident due to temperature out of control or violent reaction at the oil-water interface;

[0016] (3) Severe corrosion of production equipment by a large amount of sulfuric acid

At the end of the reaction, quickly add hot water at 85°C to 90°C. Since a large amount of sulfuric acid in the reaction system is mixed with hot water, an exothermic reaction is likely to occur, causing the temperature of the di-tert-butyl peroxide solution of BIPB to rise. , thus causing the acid-catalyzed decomposition of BIPB, which has potential safety hazards and has a great impact on the reaction yield and product purity;

[0017] (4) di-tert-butyl peroxide itself as solvent is a kind of organic peroxide, unstable to strong acid and high temperature, easily produces static electricity again, there is potential safety hazard in using it as the reaction solvent of synthetic BIPB

[0020] (1) Phosphotungstic heteropoly acid has strong hygroscopicity, and it is inconvenient to store and use;

[0021] (2) The price of phosphotungstic heteropoly acid is expensive, the dosage is large, and the cost of raw materials is high. Due to the adsorption of a large amount of water and peroxide in the used heteropoly acid catalyst, the residual peroxide It is easy to decompose and explode, and it is difficult to recycle and regenerate, so it is difficult to recycle;

[0022] (3) The reaction time is 15 to 25 hours reaction, because the reaction time is too long, the reaction efficiency is very low;

[0023] (4) use the same amount of heteropolyacid catalyst as DC weight, react at 45 DEG C for 16 hours, the yield of BIPB obtained has only 50.8% (embodiment 2); the reaction yield is low, illustrating its reaction conversion rate and selectivity are not high

[0027] (1) the consumption of tert-butyl hydroperoxide is more, and production cost is higher;

[0028] (2) The reaction time is long, the side reaction is many, and the reaction yield and product purity are not high;

[0029] (3) Since the mol ratio of two (2-hydroxy-2-propyl) benzene and tert-butyl hydroperoxide in Examples 1 to 3 is about 1:1, according to the following reaction scheme, the main product of the reaction is 1-(tert-butylperoxyisopropyl)-3(4)-(2-hydroxyisopropyl)benzene and a small amount of BIPB, the yield of BIPB cannot reach more than 95%

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