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Method for preparing m-diisopropylbenzene hydrogen peroxide and p-diisopropylbenzene hydrogen peroxide

A kind of technology of m-dicumyl dihydroperoxide and dicumyl dihydroperoxide, which is applied in the field of preparing m-dicumyl dihydroperoxide and p-dicumyl dihydroperoxide, It can solve the problems of difficult separation of p-dicumyl dihydroperoxide, low yield of reaction products, equipment corrosion, etc.

Active Publication Date: 2021-04-20
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is in order to overcome prior art existence with meta-position two-(2-hydroxyisopropyl) benzene (m-DC) and para-position two-(2-hydroxyisopropyl) benzene (p-DC) The meta-dicumyl dihydroperoxide (m-DHP) and p-dicumyl dihydroperoxide (p-DHP) prepared by the mixture are not easy to separate, and a large amount of acidic solvent is used in the reaction to cause corrosion to the equipment, and the reaction The problem of low product yield provides a kind of method for preparing m-dicumyl dihydroperoxide and p-dicumene dihydroperoxide, and realizes that the m-di-(2-hydroxyisopropyl) benzene and para-position di-(2-hydroxyisopropyl) benzene as raw material to prepare meta-position dicumyl dihydroperoxide and para-position dicumyl dihydroperoxide respectively, and obtain higher yield and purity the goal of

Method used

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  • Method for preparing m-diisopropylbenzene hydrogen peroxide and p-diisopropylbenzene hydrogen peroxide

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Embodiment approach

[0033] According to a preferred embodiment of the present invention, the method further includes cooling the reaction mixture before solid-liquid separation, preferably, cooling the reaction mixture to 0-20°C before solid-liquid separation; more preferably , cooling the reaction mixture to 5-10° C. before solid-liquid separation.

[0034] According to the present invention, the method of solid-liquid separation is not particularly limited, and it may be a method of solid-liquid separation commonly used in the art, such as suction filtration or centrifugation.

[0035] According to the present invention, in order to improve the purity and the yield of the obtained p-dicumyl dihydroperoxide, the method may also include washing the solid phase containing p-dicumene dihydroperoxide to obtain Para-Dicumyl Dihydroperoxide Solid.

[0036] According to the present invention, the method of washing the solid phase containing p-dicumene dihydroperoxide includes washing the solid phase c...

Embodiment 1

[0044] 1) 100 milliliters of toluene, 10 grams of raw materials containing 98% by weight of m-DC and p-DC (the weight ratio of the two is 2.5:1), 17.5 grams of 50% by weight hydrogen peroxide and 0.25 gram of sulfuric acid (concentration is 98% by weight %) were mixed, started to stir, and reacted at 50°C under the condition of 0.02MPa. During the reaction, the water generated by the reaction was removed in time, and the evaporated toluene was returned to the reaction system for reuse, and the reaction was carried out for 3 hours. Gas chromatography Measure the content of m-HHP in the reaction solution to be 0.09% by weight, stop stirring, cool the reaction solution to 7°C for suction filtration, wash the obtained filter cake with a small amount of 7°C toluene and distilled water, dry the filter cake after washing, and obtain p -DHP product with a yield of 96% and a purity of 99.0%.

[0045] 2) The obtained filtrate removes the water phase to obtain an oil phase, and the oil p...

Embodiment 2

[0047] 1) 150 milliliters of toluene, 10 grams of raw materials containing 98% by weight of m-DC and p-DC (the weight ratio of the two is 2:1), 35 grams of 30% by weight hydrogen peroxide and 1.15 grams of phosphoric acid (concentration is 85% by weight %) for mixing, start stirring, and react at 40°C and 0.015MPa, remove the water generated by the reaction in time during the reaction, and return the evaporated toluene to the reaction system for reuse, react for 5 hours, and perform gas chromatography Measure the content of m-HHP in the reaction solution to be 0.09% by weight, cool the reaction solution to 10°C for suction filtration, wash the obtained filter cake with a small amount of 10°C toluene and distilled water, dry the filter cake after washing, and obtain the p-DHP product , the yield was 93.1%, and the purity was 98.6%.

[0048] 2) The obtained filtrate removes the water phase to obtain an oil phase, and the oil phase is washed with a small amount of distilled water...

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Abstract

The invention relates to the field of organic synthesis, and discloses a method for preparing m-diisopropylbenzene hydrogen peroxide and p-diisopropylbenzene hydrogen peroxide, which comprises the following steps: contacting a material containing m-di (2-hydroxy isopropyl) benzene and p-di (2-hydroxy isopropyl) benzene with hydrogen peroxide to react; obtaining a reaction mixture containing m-diisopropylbenzene hydroperoxide and p-diisopropylbenzene hydroperoxide; and carrying out solid-liquid separation on the reaction mixture to obtain a liquid phase containing m-diisopropylbenzene hydroperoxide and a solid phase containing p-diisopropylbenzene hydroperoxide. The m-diisopropylbenzene hydrogen peroxide prepared by the method provided by the invention has the purity of 95% or more and the yield of 82% or more, the p-diisopropylbenzene hydrogen peroxide has the purity of 97% or more and the yield of 86% or more, and the method has the advantages of less waste acid generation amount, cleanness, environmental protection, mild reaction conditions and easy control of reaction, and is suitable for industrialization.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for preparing m-dicumene diperoxide and p-dicumene diperoxide. Background technique [0002] m-DHP and p-DHP are important fine organic intermediates widely used in resorcinol and p-DHP Synthetic production of quinone. Meta-position and para-position DHP can be used as polymerization initiator, also can be used as the initiator of dicumyl air (oxygen) oxidation reaction, can also be used to synthesize the epoxide of propylene oxide or butylene oxide. Utilizing the activity of hydroperoxyl, it can also be used as a raw material for synthesizing other organic peroxides. [0003] The traditional meta- and para-dicumene dihydroperoxide production process is prepared through the oxidation synthesis process of pure meta-dicumene raw material or pure para-dicumene raw material. [0004] Pure meta- and para-dicumene raw materials are obtained by separating the mixture of meta...

Claims

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Application Information

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IPC IPC(8): C07C407/00C07C409/12
Inventor 谭永生崔敏华潘新民许耀新
Owner CHINA PETROLEUM & CHEM CORP
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