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Preparation method of p-hydroxyacetophenone

A technology for the preparation process of p-hydroxyacetophenone, which is applied in the field of preparation of p-hydroxyacetophenone, can solve the problems of multiple by-products, low catalytic activity, and influence on the yield and purity of hydroxyacetophenone

Pending Publication Date: 2022-03-11
JIANGXI YONGTONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional synthesis process, the catalyst used can shorten the reaction time, but there are often defects such as low catalytic activity and poor product selectivity, and more by-products will be produced during the reaction process, which affects the recovery of p-hydroxyacetophenone. rate and purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] A kind of preparation method of p-hydroxyacetophenone proposed by the present invention is prepared from phenol and acetyl chloride as raw materials and a modified catalyst as a catalyst; the weight ratio of the phenol and the modified catalyst is 100:1.5; the The preparation method of modified catalyst comprises the following steps:

[0021] S1. Mix graphene oxide with water, disperse evenly, add n-butylamine, stir evenly, add aluminum isopropoxide and sodium silicate, wherein the molar ratio of aluminum isopropoxide and sodium silicate is 1:55 The mol ratio of the n-butylamine and aluminum isopropoxide is 11:1; the weight of the graphene oxide is 19% of the total weight of aluminum isopropoxide and sodium silicate, after stirring at 30°C for 30min, the temperature is raised to Stir at 85°C for 3 hours, wash with ethanol and deionized water, transfer to a polytetrafluoroethylene-lined autoclave, heat up to 110°C for crystallization for 18 hours, then heat up to 150°C f...

Embodiment 2

[0027] A kind of preparation method of p-hydroxyacetophenone proposed by the present invention is prepared by taking phenol and acetyl chloride as raw materials and using a modified catalyst as a catalyst; the weight ratio of the phenol and the modified catalyst is 100:0.3; the The preparation method of modified catalyst comprises the following steps:

[0028] S1. Mix graphene oxide with water, disperse evenly, add n-butylamine, stir evenly, add aluminum isopropoxide and sodium silicate, and the molar ratio of aluminum isopropoxide and sodium silicate is 1:60; The molar ratio of n-butylamine to aluminum isopropoxide is 15:1; the weight of graphene oxide is 25% of the total weight of aluminum isopropoxide and sodium silicate, and the temperature is raised to 70°C after stirring at 25°C for 60min Stir for 5 hours, wash with ethanol and deionized water, transfer to a polytetrafluoroethylene-lined autoclave, heat up to 100°C for crystallization for 20 hours, then heat up to 180°C ...

Embodiment 3

[0034] A kind of preparation method of p-hydroxyacetophenone proposed by the present invention comprises the following steps: putting phenol and modified catalyst into an acylation kettle, the weight ratio of said phenol and modified catalyst is 100:0.5, heating up to 55°C, Acetyl chloride is added dropwise under negative pressure. During the dropwise addition, the temperature in the acylation tank is kept at 110°C. After the dropwise addition, it is kept for 7 hours, cooled, hydrolyzed, washed with water, separated from the water layer, distilled, frozen and crystallized, and then centrifuged to obtain p-Hydroxyacetophenone;

[0035] The preparation method of described modified catalyst comprises the following steps:

[0036]S1. Mix graphene oxide with water, disperse evenly, add n-butylamine, stir evenly, add aluminum isopropoxide and sodium silicate, and the molar ratio of aluminum isopropoxide and sodium silicate is 1:65; The molar ratio of n-butylamine to aluminum isopro...

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Abstract

The invention discloses a preparation method of p-hydroxyacetophenone. The p-hydroxyacetophenone is prepared by taking a modified catalyst as a catalyst, the preparation method of the modified catalyst comprises the following steps: uniformly mixing graphene oxide and water, adding n-butylamine, uniformly stirring, adding aluminum isopropoxide and sodium silicate, stirring at 70-85 DEG C for 3-5 hours, washing, heating to 100-130 DEG C, crystallizing for 10-20 hours, heating to 150-185 DEG C, crystallizing for 10-30 hours, washing, drying and roasting to obtain a material A; exchanging the material A with an ammonium chloride aqueous solution, and calcining to obtain a material B; mixing citric acid, oxalic acid and water to obtain an acid solution, mixing the material B with the acid solution, heating to 70-80 DEG C, stirring for 9-20 hours, washing to be neutral, and drying to obtain a material C; and mixing lithium nitrate, ferric nitrate, cerium nitrate and water, mixing with the material C, stirring, standing, filtering, washing, drying, roasting, mixing with phosphotungstic acid, and ball-milling.

Description

technical field [0001] The invention relates to the technical field of synthesis, in particular to a preparation method of p-hydroxyacetophenone. Background technique [0002] p-Hydroxyacetophenone, also known as 4'-hydroxyacetophenone, contains functional groups such as hydroxyl and ketone groups connected to the benzene ring. Therefore, it is often used as an intermediate in organic synthesis to participate in reactions with other molecules to synthesize many important compound. In industry, p-hydroxyacetophenone is mainly obtained from phenol through acylation and Fries rearrangement. In the traditional synthesis process, the catalyst used can shorten the reaction time, but there are often defects such as low catalytic activity and poor product selectivity, and more by-products will be produced during the reaction process, which affects the recovery of p-hydroxyacetophenone. rate and purity. Contents of the invention [0003] Based on the technical problems existing ...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C49/825B01J29/06B01J35/10
CPCC07C45/45B01J29/06B01J35/61C07C49/825
Inventor 郑建章刘忠春曾秋明黄啟仕
Owner JIANGXI YONGTONG TECH
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