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Environment-friendly synthetic method of 3,4-dimethylbenzaldehyde

A technology of dimethylbenzaldehyde and synthetic methods, which is applied in chemical instruments and methods, organic chemistry, physical/chemical process catalysts, etc., can solve the problems of harsh control of reaction conditions and complex catalyst recycling equipment, and achieve low cost, Reduced risk, low yield effect

Active Publication Date: 2019-02-22
ZHEJIANG BENLI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

HF-BF 3 It is a liquid superacid with strong formylation ability, and it is also prone to disproportionation reaction. The reaction conditions are strictly controlled, and the catalyst recycling equipment is relatively complicated.

Method used

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  • Environment-friendly synthetic method of 3,4-dimethylbenzaldehyde
  • Environment-friendly synthetic method of 3,4-dimethylbenzaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Add 500g of o-xylene into a 1L high-pressure reactor, replace it with nitrogen, start stirring, add 6.7g of anhydrous aluminum trichloride, cool to -10°C, slowly introduce 117g of boron trichloride, and control the temperature -15 ~-10°C, feed CO until the pressure is 1.0Mpa, when the pressure drops, continue to feed CO to maintain the pressure in the kettle until the pressure no longer drops, indicating the end of the reaction. The material is transferred to the flash evaporator, the temperature of the flash evaporator is controlled to be less than 50°C, and boron trichloride is recovered by double-stage condensation, which can be used in the reaction. The material after flashing is transferred in the flask that 300g ice water is housed again, stirs 30 minutes, leaves standstill layering, water layer extracts once with 50g o-xylene, merges organic layer, carries out vacuum fractionation, reclaims o-xylene can be Apply it to the reaction to obtain 3,4-dimethylbenzaldehy...

Embodiment 2

[0026] As described in Example 1, the difference is that 26.7g of anhydrous aluminum trichloride was added, the preparation steps and conditions were the same as in Example 1, and the resulting yield was 91.2%.

Embodiment 3

[0028] As described in Example 1, the difference is that 66.7g of anhydrous aluminum trichloride was added, the preparation steps and conditions were the same as in Example 1, and the resulting yield was 90.9%.

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Abstract

The invention relates to an environment-friendly synthetic method of 3,4-dimethylbenzaldehyde. The method comprises the following steps shown in the description: o-xylene is added to a high-pressure reactor, nitrogen is introduced for replacement, stirring is started, anhydrous aluminium trichloride is added, the mixture is cooled, boron trichloride is introduced slowly, temperature is controlled,CO is introduced to certain pressure, after pressure drops, CO is introduced continuously to keep pressure in the reactor until the pressure no longer drops which indicates reaction ending, an obtained material is transferred to a flash evaporator, temperature of the flash evaporator is controlled, and boron trichloride is recovered by two-stage condensing and can be applied to a reaction; a material obtained after flash evaporation is transferred into a flask containing ice water, stirred and left to stand for layering, an aqueous layer is extracted with o-xylene, organic layers are combinedand subjected to reduced-pressure fractional distillation, o-xylene is recovered and can be applied to the reaction, and high-purity 3,4-dimethylbenzaldehyde is obtained. The method is simple to operate, yield of synthesized 3,4-dimethylbenzaldehyde is high, cost is low, a little anhydrous aluminium trichloride is used, boron trichloride is recyclable, few three wastes are produced, and little environmental pollution is produced.

Description

technical field [0001] The invention relates to an environment-friendly synthesis method of 3,4-dimethylbenzaldehyde, which belongs to the technical field of preparing aromatic aldehydes through formylation reaction with ortho-xylene as a raw material with carbon monoxide. Background technique [0002] 3,4-Dimethylbenzaldehyde is widely used in the synthesis of fine chemicals such as medicine, pesticides, spices, beverages, food, etc., especially for the synthesis of polypropylene nucleating and transparent agent DMDBS [bis(3,4-dimethyl Dibenzylidene) sorbitol] is a new generation of non-toxic plastic additives and a new generation of food packaging materials. The methods of synthesizing 3,4-dimethylbenzaldehyde reported at home and abroad have: [0003] Chinese patent CN1439744A discloses the indirect electrolytic oxidation of 1,2,4-trimethylbenzene to synthesize 3,4-dimethylbenzaldehyde, in which there will be 2,4-dimethylbenzaldehyde and 2,5-dimethylbenzaldehyde Toluald...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/50C07C47/542B01J27/10
CPCC07C45/50B01J27/10C07C47/542
Inventor 徐洪顺吴政杰顾海宁余永志
Owner ZHEJIANG BENLI TECH CO LTD
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