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2,4-di-(1-phenylisopropyl) phenol preparation method

A technology of cumylphenol and phenol, applied in the field of preparation 2, which can solve the problems of complex post-processing and low selectivity

Active Publication Date: 2009-07-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is the low selectivity of 2,4-dicumylphenol and complicated post-reaction treatment in the prior art, and a new method for preparing 2,4-dicumylphenol is provided

Method used

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  • 2,4-di-(1-phenylisopropyl) phenol preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Put 659.0 g (7 moles) of molten phenol and 19.3 g of Amberlyst 31H into a 2-liter four-neck flask equipped with a mechanical stirrer, a thermometer, a condenser tube and an addition funnel, and add 275.7 g of α-methylstyrene dropwise at 70 to 75 ° C grams (2.33 moles), gas chromatography analysis α-methylstyrene conversion rate of 100%, can be used as the end of the reaction, about 6 hours. After cooling, the catalyst was removed by filtration, and the excess phenol was evaporated from the filtrate under reduced pressure at 20KPa. The residue was cooled, and 500 ml of cyclohexane was added for recrystallization to obtain 404 g of white needle-like crystals, melting point: 75.8° C., and its mass fraction was 98.5% according to chromatographic analysis.

[0018] Add 12.7 grams of molten phenol and 200 grams of xylene to another similarly prepared 1-liter four-neck flask, mix them, heat and reflux to remove water, it takes about 3 to 4 hours, add 1.21 grams of aluminum pow...

Embodiment 2

[0020] Put 564.6 grams (6 moles) of molten phenol and 16.5 grams of Amberlyst 15H into a 2-liter four-necked flask equipped with a mechanical stirrer, a thermometer, a condenser tube and an addition funnel, and add α-methylstyrene 236.4 grams dropwise at 70-75°C gram (2 moles), the conversion rate of α-methylstyrene by gas chromatography analysis reaches 100%, which can be used as the end point of the reaction, and it takes about 6 hours. After cooling, the catalyst was removed by filtration, and the excess phenol was evaporated from the filtrate under reduced pressure at 20KPa to obtain 15.6 g of residue A4 for subsequent use. The ratio of 4-cumylphenol in the chromatographic analysis product was 92.5%.

[0021] Add 24.4 grams of molten phenol and 200 grams of xylene to another similarly prepared 1-liter four-neck flask, mix them, heat and reflux to remove water, it takes about 3 to 4 hours, add 2.30 grams of aluminum powder under nitrogen protection, and continue to reflux un...

Embodiment 3

[0024] Add 470.5 grams (5 moles) of HD-811.8 grams of molten phenol into a 1-liter four-necked flask equipped with a mechanical stirrer, a thermometer, a condenser tube and an addition funnel, and add 236.4 grams of α-methylstyrene (2 mol), the conversion rate of α-methylstyrene by gas chromatography analysis reaches 100%, which can be used as the end point of the reaction, and it takes about 5 hours. After cooling, the catalyst was removed by filtration, and the excess phenol was evaporated from the filtrate under reduced pressure at 20KPa to obtain 26.3 g of residue B4 for subsequent use. The ratio of 4-cumylphenol in the chromatographic analysis product was 93.6%.

[0025] Add 8.3 grams of molten phenol and 200 grams of xylene to another similarly prepared 1-liter four-neck flask, mix them, heat and reflux to remove water, it takes about 3 to 4 hours, add 0.8 grams of aluminum powder under nitrogen protection, and continue to reflux until the aluminum powder is completely d...

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Abstract

The invention relates to a method for preparing 2,4-dicumylphenol, which mainly solves the technical problems of low selectivity of 2,4-dicumylphenol, complicated post-reaction treatment and the like existing in the prior art. The present invention is by adopting with phenol and α-methyl styrene as raw material, with strongly acidic macroporous cation exchange resin as catalyst, catalyst consumption is 1~15% of phenol weight, and raw material molar ratio is 4: 2~1, at 65 React at ~145°C for 2 to 8 hours to obtain 4-cumylphenol; then use aluminum phenoxide as a catalyst, the molar ratio of 4-cumylphenol to α-methylstyrene is 1:1~1.4, and the amount of aluminum powder is 0.1-0.8% of the weight of 4-cumylphenol is reacted at a temperature of 120-140°C for 3-8 hours to obtain the technical scheme of 2,4-dicumylphenol, which solves this problem well and can be applied to 2 , In the industrial production of 4-dicumylphenol.

Description

technical field [0001] The invention relates to a method for preparing 2,4-dicumylphenol. Background technique [0002] Phenol and its aromatic hydrocarbon alkylation products have attracted the attention of researchers due to their wide range of uses. α-Methylstyrene is a by-product of the synthesis of phenol and acetone by the cumene method. It is used as the starting material to carry out the alkylation reaction of phenol, and the alkylation products of various structures can be obtained, such as 2-cumyl Phenol (2-cumylphenol), 4-cumylphenol (4-cumylphenol), 2,4-dicumylphenol (2,4-dicumylphenol), 2,6-dicumylphenol (2,6-dicumylphenol), 2,4,6-tricumylphenol (2,4,6-tricumylphenol) and the like. Among them, 4-cumylphenol, 2,4-dicumylphenol and 2,4,6-tricumylphenol are most widely used. In addition, while the alkylation reaction occurs, dimers (2,4-diphenyl-4-methylpentene), trimers and intramolecular cyclization products of α-methylstyrene are also formed. 1,1,3-Trimethyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/14C07C39/15
Inventor 沈之芹王芳李斌
Owner CHINA PETROLEUM & CHEM CORP