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Preparation method of 2,4,6-trimethylbenzoyl chloride and application of 2,4,6-trimethylbenzoyl chloride in preparing phosphorescence-containing initiators

A technology of trimethylbenzoyl chloride and mesitylene, which is applied in the field of preparation of 2,4,6-trimethylbenzoyl chloride, can solve the problems of less than 50% conversion rate, poor yield, and many wastes , to achieve the effects of less waste, good reaction selectivity, and low environmental pressure

Pending Publication Date: 2018-05-18
湖南久日新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of 2,4,6-trimethylbenzoic acid is generally prepared by reacting mesitylene and carbon dioxide under the catalysis of aluminum trichloride. This method is characterized by relatively poor yield, and the conversion rate of mesitylene less than 50%
But the current yield is still relatively low, and there are many three wastes, so a lot of improvement and optimization are still needed

Method used

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  • Preparation method of 2,4,6-trimethylbenzoyl chloride and application of 2,4,6-trimethylbenzoyl chloride in preparing phosphorescence-containing initiators

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Embodiment 1: the preparation of imidazole ionic liquid

[0041]Take 65.6 g of 1-methylimidazole (0.8 mol) and bromo(chloro)-n-butane (0.88 mol) in a 1000 mL four-neck flask and heat to reflux for 24 hours, then wash with 40 mL of ethyl acetate for 3 times while hot to remove untreated Reaction of 1-methylimidazole and excess bromo(chloro)-n-butane, and then vacuum removal of low-boiling impurities and a small amount of ethyl acetate to obtain 1-methyl-3-butylimidazolium bromide (chloride) ionic liquid (referred to as [MBIm]Br(Cl)). Mix 1-methyl-3-butylimidazolium bromide (chloride) ionic liquid and anhydrous aluminum trichloride solid according to the ratio of substances (2-1): 1, and slowly add aluminum trichloride to 1- In the methyl-3-butylimidazolium bromide (chloride) ionic liquid, stir at room temperature until the system becomes a uniform color liquid, and the preparation is abbreviated as [MBIm]Br·2AlCl 3 、[MBIm]Br·1.5AlCl 3 、[MBIm]Cl 2AlCl 3 、[MBIm]Br·AlC...

Embodiment 2

[0042] Embodiment 2: Preparation of quaternary ammonium ionic liquid

[0043] Under the protection of nitrogen, put 110.1g of triethylamine hydrochloride (0.8mol) in 200mL of n-heptane, and slowly add 1.0-2.0 times the amount of anhydrous aluminum trichloride in batches while stirring, The temperature was raised to 120°C, and the mixture was continuously stirred for 2-3 hours. After cooling, the brown ionic liquid in the lower layer was separated and dried for later use. Ionic liquids of quaternary ammonium salts can be prepared by referring to similar or disclosed methods in the prior art, such as tributylhexylammonium chloroaluminate bromide, trimethylammonium chloroaluminate hydrochloride, tetraethylammonium chloride bromide Aluminate, tetraethylammonium chloroaluminate, etc.

Embodiment 3

[0044] Embodiment 3: the preparation of 2,4,6-trimethylbenzoyl chloride

[0045] Add 120.2g of mesitylene (1.0mol) into a 500mL autoclave, add 291.5g of [MBIm]Br·2AlCl 3 (0.6mol), close the kettle, control the temperature at 5-10°C, start to pass carbon dioxide, and set the pressure in the kettle to 5-6Mpa. With the pressure in the kettle no longer dropping as the end point of the reaction, add 200mL of dichloromethane and 200mL of ethyl acetate, stir evenly, let stand to separate layers, and the upper layer is mesitylene, 2,4,6-trimethylbenzoic acid, ethyl acetate Ester mixture, the lower floor is the ionic liquid catalyst phase dichloromethane mixture, separate the lower floor and recycle it mechanically, wash the upper floor with water, then distill and reclaim ethyl acetate and a small amount of mesitylene, add 45.8g phosphorus trichloride dropwise in the residue, The temperature control is less than 60°C. After dropping, keep it warm at 55-60°C for 2 hours, stop stirring...

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Abstract

The invention relates to a preparation method of 2,4,6-trimethylbenzoyl chloride, in particular to a method for preparing 2,4,6-trimethylbenzoyl chloride with mesitylene as a raw material through a catalytic reaction in ionic liquid. The preparation method of 2,4,6-trimethylbenzoyl chloride is simple in process, low in environment pressure, economical and feasible. The method has the advantages that the purity is good, the yield is high, the purity of 90% or above can be reached without purification, and the method can be directly used for preparing photoinitiators TPO, 819 and TPO-L.

Description

technical field [0001] The present invention relates to a preparation method of 2,4,6-trimethylbenzoyl chloride, in particular to the preparation of 2,4,6-trimethylbenzoyl chloride by using mesitylene as a raw material in ionic liquid catalytic reaction method. Background technique [0002] 2,4,6-Trimethylbenzoyl chloride has a wide range of uses. It is used as a photoinitiator in photopolymerizable materials, unsaturated resin models and recording materials; it is used as a stabilizer in plastics and paints to improve its light resistance , heat resistance; in medicine, it is used to prepare antibiotics and antihistamines. It can be used to prepare coatings, dyes, moldings, adhesives, composite fiber materials, etc. It is also an important raw material for photoinitiators TPO, TPO-L, and 819. [0003] [0004] There are two main types of preparation methods: [0005] One is 2,4,6-trimethylbenzoic acid as raw material, Liang Taishuo et al. (Liang Taishuo, Hu Yongl...

Claims

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Application Information

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IPC IPC(8): C07C51/60C07C51/15C07C63/04C07F9/53C07F9/32
CPCC07C51/15C07C51/60C07F9/3252C07F9/5337C07C63/04
Inventor 毛桂红张建锋罗想寇福平胡祖飞刘川伟张齐
Owner 湖南久日新材料有限公司