Method for preparing p-methylacetophenone

A technology of p-methyl acetophenone and methyl acetophenone, which is applied in the field of preparation of p-methyl acetophenone, can solve the problems that the catalyst cannot be recycled, the economic benefit is poor, and the equipment is corroded after treatment, etc., and it is easy to scale The effect of modernization and continuous production, simple structure and stable operation

Inactive Publication Date: 2017-02-08
枣阳市先飞高科农药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The traditional reaction process for synthesizing p-methylacetophenone is mainly based on a simple batch reactor, which has the disadvantages of small reaction capacity, insufficient reaction, large reaction investment consumption, and poor economic benefits.
At present, the domestic method of synthesizin

Method used

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  • Method for preparing p-methylacetophenone
  • Method for preparing p-methylacetophenone
  • Method for preparing p-methylacetophenone

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Experimental program
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Effect test

Embodiment 1

[0020] Such as figure 1 Shown, a kind of preparation method of p-methylacetophenone of the present embodiment comprises following processing steps:

[0021] (1) raw material preparation: the production raw material of this methyl acetophenone comprises following components (parts by weight): 3 parts of toluene, 50 parts of acylating reagents, 100 parts of organic solvents, 5 parts of catalysts, 10 parts of aluminum trichloride, Wherein the acylating reagent comprises acetyl chloride, acetic anhydride and ethyl acetate, wherein the organic solvent is composed of benzene, acetic acid, sulfolane, chlorobenzene and nitrobenzene;

[0022] (2) Filling the catalyst: the catalyst is evenly filled into the fixed bed reactor, and the fixed bed is preheated. The preheating temperature is 120°C, and the preheating time is 10 minutes;

[0023] (3) Primary acylation reaction: send the toluene and acylating reagent in step (1) into the fixed bed reactor in proportion, and pressurize and hea...

Embodiment 2

[0027] Embodiment 2: all the other are identical with embodiment 1, difference is that in described step (1), production raw material comprises following component (weight part): toluene 4 parts, acylating reagent 60 parts, organic solvent 110 parts, catalyst 8 12 parts, 12 parts of aluminum trichloride, the preheating duration in the step (2) is 15min, and the preheating temperature is 1300° C., the pressurized heating pressure in the step (3) is 10 MPa, and the heating temperature is 180° C. The reaction duration is 25min, the reaction duration in the step (4) is 15min, the pressurized pressure in the step (5) is 20MPa, the reaction duration is 40min, and the heating temperature is 280°C, and the rectification in the step (6) The temperature was 170°C.

Embodiment 3

[0028] Embodiment 3: all the other are identical with embodiment 1, difference is that in described step (1), production raw material comprises following component (weight part): 5 parts of toluene, 60 parts of acylating reagents, 120 parts of organic solvents, catalyzer 10 parts part, 15 parts of aluminum trichloride, the preheating duration in the step (2) is 15min, and the preheating temperature is 150°C, the pressurized heating pressure in the step (3) is 15MPa, and the heating temperature is 200°C, The reaction duration is 30min, the reaction duration in the step (4) is 20min, the pressurized pressure in the step (5) is 25MPa, the reaction duration is 50min, and the heating temperature is 300°C, and the rectification in the step (6) The temperature was 180°C.

[0029] After the above process steps, the p-methylacetophenone sample is taken out to obtain the following data:

[0030]

[0031]

[0032] From the above data, it can be seen that the purity of p-methylacet...

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Abstract

The invention discloses a method for preparing p-methylacetophenone, which relates to the field of pesticide production. The method comprises six processes of raw materials preparation, filling of a catalyst, primary acylation reaction, addition of a resonance reaction, secondary acylation and purification processing. The method takes toluene and an acylating agent as the main raw materials, the raw materials are subjected to an acylation reaction to obtain p-methylacetophenone, one more time of the an acylation reaction flow is added based on traditional technological foundation, the method comprises the primary acylation reaction and secondary acylation reaction, and the p-methylacetophenone with higher purity can be obtained through the step-by-step acylation reaction. In the preparation method, a reactor has the advantages of simple structure, stable operation, convenient control, and easy realization of large scale and continuous production, and is worth of popularization.

Description

technical field [0001] The invention relates to the field of pesticide production, in particular to a preparation method of p-methylacetophenone. Background technique [0002] The traditional reaction process for synthesizing p-methylacetophenone is mainly based on a simple batch reactor, which has the disadvantages of small reaction capacity, insufficient reaction, large reaction investment consumption, and poor economic benefits. At present, the domestic method of synthesizing p-methylacetophenone is mainly obtained by the acylation reaction of toluene and acetic anhydride under the catalysis of Lewis acid or protonic acid, etc., and the catalyst itself cannot be recycled, which seriously corrodes the equipment and after-sales service. Deal with serious pollution and other defects. p-Methylacetophenone is an important fine chemical intermediate in the field of food and chemical industry. It has an aroma similar to hawthorn flowers, and has aromas like honey and strawberri...

Claims

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Application Information

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IPC IPC(8): C07C49/76C07C45/46C07C45/82
CPCC07C45/46C07C45/82C07C49/76
Inventor 李建新
Owner 枣阳市先飞高科农药有限公司
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