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Preparation method of 4-tertoctyl-2,6-dicumylphenol

A technology of tertoctylphenol and cumylphenol, applied in the field of preparation of 4-tertoctyl-2,6-dicumylphenol, which can solve the problems of disproportionation and poor reaction selectivity

Inactive Publication Date: 2017-01-18
HARBIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to solve the problems of poor reaction selectivity and disproportionation at high temperature in the existing 4-tetraoctyl-2,6-dicumylphenol production process, and provides a 4-tetraoctyl-2,6-dicumylphenol The preparation method of base phenol

Method used

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  • Preparation method of 4-tertoctyl-2,6-dicumylphenol
  • Preparation method of 4-tertoctyl-2,6-dicumylphenol

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specific Embodiment approach 1

[0024] Specific embodiment 1: The preparation method of 4-tertoctyl-2,6-dicumylphenol in this embodiment is carried out according to the following steps:

[0025] 1. Preparation of composite catalyst: Add 4-tetraoctylphenol, metal aluminum and rare earth chloride into the reactor, and under the protection of nitrogen, heat the reaction system to 110-140°C for reaction, until no more bubbles are released. Keep warm for 0.4-0.6h, then add ionic liquid, mix evenly to get the mixture of 4-tertoctylphenol and composite catalyst;

[0026] 2. Alkylation reaction: Add α-methylstyrene dropwise to the mixture of 4-tertoctylphenol and composite catalyst, control the rate of addition to keep the system temperature at 100-180°C, wait for α-methylstyrene to drop After the addition was completed, the reaction was continued for 0.8 to 1.2 hours to obtain a reaction mixture;

[0027] 3. Product refining: add dilute sulfuric acid with a mass concentration of 10% to 30% to the reaction mixture ...

specific Embodiment approach 2

[0029] Specific embodiment two: the difference between this embodiment and specific embodiment one is: the composite catalyst in the mixture of 4-tertoctylphenol and composite catalyst obtained in step one is 4-tertoctylphenol aluminum, ionic liquid and chlorinated Rare earth composite catalyst. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0030] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is: in step one, the ionic liquid is tetrafluoroborate or p-toluenesulfonate of alkylimidazole, and its general formula is:

[0031]

[0032] R=C 2 h 5 , n-C 4 h 9

[0033]

[0034] Others are the same as in the first or second embodiment.

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Abstract

The invention relates to the method for preparing 4-tert-octyl-2,6-dicumyl phenol. The method is used for solving the problems in the existing 4-tert-octyl-2,6-dicumyl phenol production processes that the reaction selectivity is poor and disproportionation occurs at high temperatures. The method comprises the steps: (1) adding 4-tert-octyl phenol, metallic aluminum and rare earth chloride into a reactor, heating to carry out reaction until no bubble is discharged, carrying out heat preservation, adding ionic liquid into the reaction product, and uniformly mixing the ionic liquid and the reaction product, thereby obtaining a mixture; (2) dropwise adding alpha-methyl styrene into the mixture, and continuing to carry out reaction after alpha-methyl styrene is dropwise added completely, so as to obtain a reaction mixture; and (3) adding dilute sulfuric acid into the reaction mixture, adding an organic solvent into the dilute sulfuric acid added reaction mixture, precipitating to separate a water layer, then, directly cooling to precipitate crystals, filtrating the precipitated crystals to obtain a crude product, and recrystallizing the crude product with an ethanol-water mixed solvent, thereby obtaining 4-tert-octyl-2,6-dicumyl phenol. According to the method, the selectivity of 4-tert-octyl-2,6-dicumyl phenol is greatly improved. 4-tert-octyl phenol is effectively prevented from being disproportionated into phenol. The method is used for preparing 4-tert-octyl-2,6-dicumyl phenol.

Description

technical field [0001] The invention relates to a preparation method of 4-tertoctyl-2,6-dicumylphenol. Background technique [0002] 4-tertoctyl-2,6-dicumylphenol is a new type of fine chemical raw material. The results of technical research and development show that it can be used in the production of fine chemicals such as plastic additives and surfactants, especially in the production of plastics for auto parts Modified additives for products, so it has a good market prospect. [0003] So far, there is no literature report on the preparation method of 4-tetyl-2,6-dicumylphenol at home and abroad. According to the traditional synthetic method of cumyl phenol products, Lewis acid or aluminum phenate can be selected as catalyst or aluminum phenate as catalyst. However, the experimental results show that using 4-tertoctylphenol as a raw material, if Lewis acid is used as a catalyst, when the molar ratio of 4-tertoctylphenol to α-methylstyrene reaches 1:2~3, the product 4- ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/15C07C37/14B01J31/26
CPCY02P20/52
Inventor 由君姜玉富李忠林刘波祁亚楠
Owner HARBIN UNIV OF SCI & TECH
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