Pinacolone preparation method

A technology of pinacolone and reaction time, which is applied in the direction of hydrogen halide addition preparation, condensation preparation of carbonyl compounds, and hydrocarbon production from oxygen-containing organic compounds, etc., which can solve the problem of increased production cost of pinacolone, low conversion rate, and long reaction time and other problems, to achieve the effect of low equipment requirements, simple process and low cost

Inactive Publication Date: 2015-11-11
ZHANGJIAGANG CITY ZHENFANG CHEM
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Problems solved by technology

[0003] However, the existing technology for the preparation of 5-methyl-6,6-dimethyl-1,3-dioxocyclohexane mainly has the problems of low conversion rate

Method used

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  • Pinacolone preparation method

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Embodiment

[0019] The preparation method of pinatone comprises steps:

[0020] (1) Isoamyl alcohol is dehydrated to obtain isopentene, and then reacted with hydrochloric acid to obtain isopentyl chloride, the reaction temperature is 5-25°C, and the reaction time is 2-8 hours;

[0021] (2), under the action of Zn / Co / Sb composite catalyst, react the methanol solution of chloroisopentane and sodium methylate, the mol ratio of each component in the Zn / Co / Sb composite catalyst is (0.7~1.2 ):(0.5~1.5):(0.7~1.2). The reaction temperature is 0-60° C., the reaction time is 15-35 minutes, and the pinatone is obtained.

[0022] (3), pinacolone is dissolved in the carbon tetrachloride solution, then drips concentrated nitric acid at 30~40 ℃, the mass ratio of concentrated nitric acid is 65%. Cool to 20-25°C, filter out the white solid salt, then dissolve the white solid salt in carbon tetrachloride solution, adjust the pH value to 6-7, remove the solvent, and obtain the purified pinacolone solid. ...

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Abstract

The present invention discloses a pinacolone preparation method, which comprises that: (1) isoamyl alcohol is dewatered to prepare isoamylene, and the isoamylene and hydrochloric acid are subjected to an addition reaction to obtain chloroisopentane, wherein the reaction temperature is 5-25 DEG C, and the reaction time is 2-8 h; and (2) the chloroisopentane reacts with a methanol solution of sodium methoxide to obtain the pinacolone, wherein the reaction temperature is 0-60 DEG C, and the reaction time is 15-35 min. According to the present invention, the method has characteristics of simple process, low equipment requirement and low cost, and the purity of the product obtained through the method is more than or equal to 99.8%.

Description

technical field [0001] The application belongs to the technical field of chemical industry, in particular to a preparation method of pinacolone. Background technique [0002] Pinacolone, mainly used in the production of triazole pesticides, is also used in the production of herbicides and pharmaceutical products, and is one of the important chemical raw materials. In the preparation process of pinacolone, the intermediate chloropentane is usually placed under acidic conditions, and formaldehyde is added and reacted at 90-95°C for 2 hours to generate 5-methyl-6,6-di Methyl-1,3-dioxocyclohexane is decomposed and rearranged into pinacolone, so 5-methyl-6,6-dimethyl-1,3-dioxocyclohexane is prepared Pinacolone is a very important intermediate, and its content and production cost are directly related to the quality, yield and production cost of pinacolone. [0003] However, the existing technology for the preparation of 5-methyl-6,6-dimethyl-1,3-dioxocyclohexane mainly has the p...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C49/04
CPCC07C45/45C07C1/24C07C17/08C07C49/04C07C19/01C07C11/09
Inventor 曹爱春赵松雪郁培华
Owner ZHANGJIAGANG CITY ZHENFANG CHEM
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