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Method of preparing aromatic isopropyl hydrogen peroxide compounds by microchannel oxidation process

A propyl hydroperoxide and compound technology, which is applied in the preparation of peroxy compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of high reaction safety factor, high production cost, short reaction time, etc. Good quality and heat transfer effect, short reaction time, and the effect of improving yield

Inactive Publication Date: 2019-04-05
ZHEJIANG UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Chinese patent (CN102382024) reports the microchannel ozone oxidation method. In a continuous tubular reactor, ozone is used as an oxidant to oxidize cumene to cumene hydroperoxide, 0.5MPa, 60°C, and 6 minutes of reaction. The yield is 38.2%. The process has a short reaction time and a high reaction safety factor, but the yield is low, ozone is more expensive, and the production cost is high

Method used

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  • Method of preparing aromatic isopropyl hydrogen peroxide compounds by microchannel oxidation process
  • Method of preparing aromatic isopropyl hydrogen peroxide compounds by microchannel oxidation process

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Add 32.4 g (200 mmol) of m-dicumene (200 mmol), 3.3 g (20 mmol) of N-hydroxyphthalimide, 1 g (6 mmol) of azobisisobutyronitrile and 200 mL of acetonitrile into the preheater, Mix and dissolve, and preheat to 60°C to obtain a reaction raw material solution for use.

[0024] The temperature of the JD-SSIC silicon carbide plate microchannel reactor was raised to 75°C, and oxygen was introduced, the pressure was 2.6Mpa, and the flow rate of oxygen was 0.2mL / min. Feed into the reaction raw material liquid, the flow rate is 30mL / min, after the reacted feed liquid is subjected to gas-liquid separation, the separated reaction mixture is passed into the microchannel reactor for cyclic reaction, the one-way reaction time is 2min, and the cumulative reaction time is 180min. Finally, the cumene m-dihydroperoxide solution was obtained, which was analyzed by a liquid chromatograph, and the yield was 49%, and the selectivity was 92.1%.

Embodiment 2

[0026] 4.2 g (20 mmol) of N-hydroxy-4-nitrophthalimide was used instead of 3.3 g (20 mmol) of N-hydroxyphthalimide, and other reaction conditions and operating procedures were the same as in Example 1. A cumene m-dihydroperoxide solution was obtained with a yield of 43.2% and a selectivity of 90.2%.

Embodiment 3

[0028] 4.0 g (20 mmol) of N-hydroxy-4-chlorophthalimide was substituted for 3.3 g (20 mmol) of N-hydroxyphthalimide, and the other reaction conditions and operating procedures were the same as in Example 1. A cumene m-dihydroperoxide solution was obtained with a yield of 43.8% and a selectivity of 90.6%.

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Abstract

The invention discloses a method of preparing aromatic isopropyl hydrogen peroxide compounds by a microchannel oxidation process. The method includes: with a N-hydroxyphthalimide hydroxylamine compound as a catalyst and an azodiisobutyronitrile azo compound as an initiator, using a JD-SSIC silicon carbide plate micro-channel reactor to continuously introduce oxygen at certain flow rate maintained,with reaction pressure reaching a range of 0.5-4.5 MPa; mixing an aromatic isopropyl compound, the catalyst and the initiator, adding suitable solvent, preheating, allowing a flow into a microchannelthrough a metering pump, allowing oxidative reaction at 60-95 DEG C for 30-180 min, and carrying out gas-liquid separation after reaction to obtain finished aromatic isopropyl hydrogen peroxide compound solution, with the product yield reaching 49%. An organic-phase homogenous catalytic oxidation system and the microchannel reactor are utilized; mass transfer and heat transfer are effective; oxidative reaction time is short; explosion proneness of reaction is effectively avoided; therefore, the yield is high, selectivity is good, and safety is high.

Description

technical field [0001] The invention relates to the preparation of aromatic isopropyl hydroperoxide by oxidation, in particular to a method for preparing aromatic isopropyl hydroperoxide by microchannel oxidation. Background technique [0002] Aromatic isopropyl hydroperoxide is an important chemical intermediate, which is widely used in the fields of medicine, pesticide and rubber, and they can also prepare phenolic compounds through hydrolysis. [0003] At present, the domestic method for synthesizing aromatic isopropyl hydroperoxide mainly adopts the oxidation method of aromatic isopropyl compounds. Oxidation methods mainly include base catalysis, metal catalysis, organic matter catalysis and microchannel ozone oxidation. [0004] The US patent (US4237319) reported the base catalysis method. In an autoclave, using sodium hydroxide aqueous solution as the catalyst, air as the oxidant, 0.65MPa, 106°C, reaction for 31 hours, m-diisopropylbenzene was oxidized to m-diperoxide...

Claims

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Application Information

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IPC IPC(8): C07C407/00C07C409/12C07C409/10
CPCC07C407/00C07C409/12C07C409/10
Inventor 李小青陈亚玲郑昆许响生
Owner ZHEJIANG UNIV OF TECH
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