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Process for continuous preparation of diisopropylbenzene dihydroperoxide

A technology of dicumyl dihydroperoxide and a preparation process is applied in the preparation of peroxy compounds, preparation of organic compounds, organic chemistry, etc., and can solve problems such as low production efficiency, long precipitation time, increased energy consumption, and the like, Achieve the effect of saving energy consumption, improving quality and purity, and shortening reaction time

Inactive Publication Date: 2009-09-30
HUNAN YIXIANG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

On the one hand, this process method has certain dangers due to the use of metal catalysts, because peroxides are very sensitive to many metal salts, easily decomposed and have the possibility of explosion; on the other hand, this process method is a batch operation process, Because DHP must be centrifuged and filtered, the mother liquor can return to the system for circulation and oxidation, which makes the production efficiency low
U.S. Patents US4088699 and US4053520 have studied the continuous preparation process of para-DHP, but the time for DHP to rely on cooling precipitation from the oxidizing solution is long, the temperature is low, and the purity is not high, and a large amount of by-product impurities are precipitated together with DHP. Repeated recrystallization with solvent in order to obtain higher purity DHP, the cost is very high
In addition, in order to return the separated DHP raffinate to carry out the circulation oxidation reaction smoothly, the above-mentioned US patent also adopts the method of stripping and distillation to remove the impurities which may inhibit the oxidation reaction, which further increases the energy consumption and the operation is cumbersome

Method used

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  • Process for continuous preparation of diisopropylbenzene dihydroperoxide

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Experimental program
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Effect test

Embodiment 1

[0016] A kind of continuous preparation process of dicumyl dihydroperoxide of the present invention, comprises the following steps:

[0017] First drop into 430gDIPB in oxidation reactor as reaction raw material (the mass ratio of its middle dicumyl and p-dicumyl is 35: 65), then add 0.25g dibenzoyl peroxide, then be heated to 95 ℃ and Keep warm, feed compressed air at a flow rate of 90L / h for bubbling oxidation, keep the pressure of the reaction system at 0.45MPa during the reaction, and the reaction time is 14h; The liquid is analyzed by high-performance liquid chromatography (HPLC), and its main components (here, the component content is expressed by area percentage, the same below) include 3.9% DIPB, 60.7% DHP and 31.6% MHP;

[0018] The oxidation solution after the above oxidation reaction is sent into an extraction reactor equipped with 220g sodium hydroxide solution (mass concentration 15%), after stirring and extracting for 30min, the DHP in the oxidation solution is d...

Embodiment 2

[0020] A kind of continuous preparation process of dicumyl dihydroperoxide of the present invention, comprises the following steps:

[0021] First drop into 430gDIPB in oxidation reactor as reaction raw material (the weight ratio of middle dicumyl and p-dicumyl is 35:65), then add 1.2g dihydroperoxide dicumyl, then heat to 115 ℃ and heat preservation, and the flow rate of 70L / h is passed into the compressed air for bubbling oxidation. During the reaction, the pressure of the reaction system is kept at 0.45MPa, and the reaction time is 16h; Take the oxidized solution for HPLC analysis, its main components include 2.4% DIPB, 63.5% DHP and 28.7% MHP;

[0022] The oxidized solution after the above reaction is sent into an extraction reactor equipped with 260 g of sodium hydroxide solution (mass concentration is 20%), and after stirring and extracting for 30 minutes, the DHP in the oxidized solution is dissolved in the sodium hydroxide solution, and the unconverted DIPB and MHP ar...

Embodiment 3

[0024] A kind of continuous preparation process of dicumyl dihydroperoxide of the present invention, comprises the following steps:

[0025] First put 430g DIPB into the oxidation reactor as the reaction raw material (the weight ratio of m-dicumene and p-dicumene is 35:65), then add 1.3g of azobisisobutyronitrile, and then heat to 85°C And keep warm, pass into compressed air with the flow rate of 85L / h and carry out bubbling oxidation, keep the pressure of reaction system during the reaction process as 0.56MPa, and the reaction time is 18h; The oxidation solution was analyzed by HPLC, and its main components included 1.6% DIPB, 66.5% DHP and 28.1% MHP;

[0026] The oxidation solution after the above-mentioned oxidation reaction is sent into the extraction reactor that 300g sodium hydroxide solution (mass concentration is 18%) is housed, after stirring and extracting for 30 minutes, the DHP in the oxidation solution is dissolved in the sodium hydroxide solution, and does not T...

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Abstract

The present invention discloses a process for continuous preparation of diisopropylbenzene dihydroperoxide. Its preparation process includes: Input the oxidizing material that is obtained from peroxidation and contains diisopropylbenzene dihydroperoxide into an alkaline solution for extraction to dissolve diisopropylbenzene dihydroperoxide, separate the oil phase and water phase of the mixed solution after extraction, circulate the oil phase back to reaction system, acidify the water phase with inorganic acid, and collect the upper-layer isolate to obtain diisopropylbenzene dihydroperoxide. The preparation process of the present invention has the following main advantages: moderate reaction conditions, high safety and reliability, simple operation, good selectivity, high raw material utilization ratio and effective reduction of cost and energy consumption.

Description

technical field [0001] The invention relates to the preparation of a peroxide containing an organic aromatic ring, in particular to a preparation process of dicumyl dihydroperoxide. Background technique [0002] 1,3- or 1,4-dicumyl hydroperoxide (abbreviated as DHP) is the raw material for preparing resorcinol or hydroquinone, and also the initiator of polyolefin polymerization, and it is easy to use in industry. The mixture of the obtained m-dicumene and p-dicumene (in the present invention, the dicumyl mixture composed of m-dicumene and p-dicumene is referred to as DIPB) to prepare efficient and environment-friendly crosslinking agent α , an important intermediate of α'-bis(tert-butylperoxy)diisopropylbenzene (abbreviated as BIPB). [0003] The process of preparing DHP from DIPB by air oxidation includes: DIPB is first oxidized to generate intermediate / p-isopropyl hydroperoxide cumene (abbreviated as MHP), and MHP is further oxidized to generate DHP. The molecular struct...

Claims

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Application Information

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IPC IPC(8): C07C409/12C07C407/00
Inventor 李玉新单文伟彭敏
Owner HUNAN YIXIANG TECH
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