Production method of methyl cyclopentenolone via amination and step-by-step reaction

A technology of methylcyclopentenol ketone amine and production method, which is applied in chemical instruments and methods, organic chemistry, preparation of organic compounds, etc., can solve problems such as many side reactions, pollute the surrounding environment, and large product odor, and achieve The effect of shortening the reaction time of amination, solid environmental protection foundation, and increasing production yield

Inactive Publication Date: 2013-05-22
ANHUI JINGHE IND
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Problems solved by technology

The amination reaction time is as long as 56 hours and the output is low. Formaldehyde, dimethylamine, hydrochloric acid, the side reactions of the three materials react together, especially the side reaction products have a particularly strong smell and pollute the surrounding environment. Due to the many side reactions, resulting in The yield is low, the average yield is about 41%

Method used

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  • Production method of methyl cyclopentenolone via amination and step-by-step reaction

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Embodiment 1

[0016] First, add 700L of dimethylamine and 400L of hydrochloric acid to the amination salt-forming kettle, the pH value is about 6.5, and carry out the dehydration reaction. The temperature is controlled at 90°C, and the reaction is 12 hours. After the salt is formed, 570L of formaldehyde is added to dissolve the reaction. The reaction intermediate was obtained in 6 hours.

[0017] The reaction intermediate is pumped into the amination kettle, add 270L methanol and 400L dimethylfuran to carry out amine methylation reaction, the reaction temperature is 40°C, and the time is 8 hours. After the reaction is completed, it is heated to 60°C to dealcoholize, and then add lye 400L, the pH value is about 10, carry out alkalization reaction, the reaction temperature is 40 ℃, 4 hours, obtain about 700L of amination intermediate. The aminated intermediate undergoes ring-opening and ring-closing rearrangement by adding acid and base, and then hydrolyzes to obtain methylcyclopentenolone. ...

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Abstract

The invention relates to a production method of methyl cyclopentenolone via amination and step-by-step reaction. The production method disclosed by the invention comprises the following steps: a, adding dimethylamine and hydrochloric acid into a salt-forming kettle, adjusting a pH value at 6.5, carrying out a dehydration reaction, adding formaldehyde after reacting and forming salt to carry out dissolution reaction and obtain a reaction intermediate; and b, pumping the reaction intermediate into an amination kettle, adding methyl alcohol and dimethyl furan to carry out a mannich reaction, then adding an alkali liquor to adjust the pH value at 10, subsequently carrying out an alkalization reaction to obtain an amination intermediate. The production method of methyl cyclopentenolone via amination and step-by-step reaction disclosed by the invention has the advantages that the double-kettle amination reaction can be continuously and simultaneously carried out, so that the time of the amination reaction can be shortened and the yield is improved; due to the adoption of the step-by-step reaction, the generation of dimethylamine side reaction products can be prevented and the reactants in the later stage are prevented from being brought to the reaction in the earlier stage; the yield is increased from 41% originally to 51% at present; and the ton unit cost of the MCP (Methyl Cyclopentenolone) is reduced from 105,000 originally to 68,000 at present.

Description

Technical field: [0001] The invention relates to a method for producing methylcyclopentenolone (MCP). Background technique: [0002] In the existing production process of methylcyclopentenolone (MCP), the amination step is to install an amination kettle in the amination section, and all raw materials are added to the amination kettle step by step to react step by step. First add formaldehyde, dimethylamine, and hydrochloric acid to adjust the pH value, then carry out dehydration reaction, add methanol as a solvent after the reaction, add dimethylfuran to carry out amine methylation reaction, and finally add alkali to carry out alkalization reaction. The amination reaction time is as long as 56 hours and the output is low. Formaldehyde, dimethylamine, hydrochloric acid, the side reactions of the three materials react together, especially the side reaction products have a particularly strong smell and pollute the surrounding environment. Due to the many side reactions, resulti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C225/20C07C221/00
Inventor 程光锦王爱民
Owner ANHUI JINGHE IND
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