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Preparation method of 2,4,6-trimethylbenzoic acid

A technology of trimethylbenzoic acid and mesitylene, which is applied to the preparation of carboxylate, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of low product yield, many reaction steps, serious three waste discharges, etc., To achieve the effect of easy availability of raw materials, few reaction steps and simple raw materials

Inactive Publication Date: 2012-06-13
TAIAN BOYANG CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention uses many raw materials and reaction steps, the product yield is low, and the discharge of three wastes in the production process is relatively serious

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Put 1200kg of mesitylene and 20kg of catalyst into the reactor, start stirring, the temperature inside the reactor is 15°C, then continuously add 220kg of carbon dioxide gas into the reactor for 5 hours, maintain the reaction temperature at 15-25°C, and the pressure inside the reactor is 0.18 -0.4MPa. After the addition of carbon dioxide is complete, the reaction temperature is raised to 24±1°C, and the reaction is maintained for 1 hour. After the reaction was completed, 30 kg of hydrochloric acid and water were added, the temperature was raised to 65° C., and the phases were separated after stirring for 1 hour. The catalyst is recovered by distillation in the water phase, and the 2,4,6-trimethylbenzoic acid product is obtained by crystallization in the oil phase.

Embodiment 2

[0015] Put 1200kg of mesitylene and 20kg of catalyst into the reactor, start stirring, the temperature inside the reactor is at 10°C, then add 220kg of carbon dioxide gas into the reactor continuously for 6 hours, maintain the reaction temperature at 20±2°C, and the pressure inside the reactor is 0.18 -0.4MPa. After the addition of carbon dioxide was complete, the reaction temperature was raised to 23±2°C, and the reaction was maintained for 1 hour. After the reaction was completed, 30 kg of hydrochloric acid and water were added, the temperature was raised to 70° C., and the phases were separated after stirring for 1.5 hours. The catalyst is recovered by distillation in the water phase, and the 2,4,6-trimethylbenzoic acid product is obtained by crystallization in the oil phase.

Embodiment 3

[0017] Put 1200kg of mesitylene and 20kg of catalyst into the reactor, start stirring, the temperature in the reactor is at 10°C, and then add 220kg of carbon dioxide gas into the reactor continuously for 7 hours, maintain the reaction temperature at 24±1°C, and the pressure in the reactor at 0.18 -0.3 MPa. After the addition of carbon dioxide was completed, the reaction temperature was raised to 24±1° C., and the reaction was maintained for 1 hour. After the reaction was completed, 30 kg of hydrochloric acid and water were added, the temperature was raised to 70° C., and the phases were separated after stirring for 2 hours. The catalyst is recovered by distillation in the water phase, and the 2,4,6-trimethylbenzoic acid product is obtained by crystallization in the oil phase.

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PUM

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Abstract

The invention discloses a preparation method of 2,4,6-trimethylbenzoic acid, which comprises the following steps: proportionally putting sym-trimethyl benzene and a catalyst into a reaction kettle, introducing carbon dioxide gas, maintaining the system to react for 6-12 hours, adding a certain amount of hydrochloric acid and water to react, recycling the catalyst from the water phase, and cooling the oil phase to crystallize, thereby obtaining the 2,4,6-trimethylbenzoic acid product. The invention has the advantages of fewer steps and simple preparation technique, and is an economical and green chemical reaction of atoms.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemicals, and in particular relates to a preparation method of 2,4,6-trimethylbenzoic acid. Background technique [0002] 2,4,6-Trimethylbenzoic acid is an important intermediate in the preparation of pesticides, medicines and photoinitiators. The traditional synthesis routes of 2,4,6-trimethylbenzoic acid are: mesitylene and oxalyl chloride are hydrolyzed under the action of anhydrous aluminum trichloride; mesitylene is added to carbon dioxide after bromination Grignard reaction Hydrolysis in the system; mesitylene and chloroacetyl chloride acylation reaction, and then after the haloform reaction and then hydrolysis derived. These methods all have the disadvantages of many reaction steps, complex process, low utilization rate of raw material atoms, serious discharge of three wastes, and the like. Chinese patent publication CN 100569726C states that 2,4,6-trimethylchloroacetophenone...

Claims

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Application Information

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IPC IPC(8): C07C63/04C07C51/15
CPCY02P20/584
Inventor 吴永生刘在琦
Owner TAIAN BOYANG CHEM TECH
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