Industrial production method of 1,3-cyclohexanedione

Abstract

The invention discloses a method for industrially producing 1, 3-cyclohexanedione. The method for industrially producing the 1, 3-cyclohexanedione comprises the following steps: putting quantitative m-phenol diamine, sodium hydroxide and water into a stainless steel batch box according to the mass ratio of 1 to 0.2-0.8 to 2-3.5, introducing materials into a stainless steel reaction kettle after dissolving and when the temperature is stabilized at about 40 DEG C, and adding a modified skeletal nickel catalyst which accounts for 3 to 4 percent of the mass of the m-phenol diamine into the stainless steel reaction kettle; introducing hydrogen after vacuum pumping to keep the pressure between 3.5 and 6.5 MPa, and discharging materials after keeping the temperature between 40 and 50 DEG C for 6 to 12 hours; putting the reaction materials into a crystallizing kettle after cooling, deposition and filtration, and adding industrial hydrochloric acid with the volume of 20 to 50 percent during stirring; and discharging material liquid when the temperature is reduced to between 5 DEG C below zero and 5 DEG C; and centrifuging, and drying the material liquid to obtain the finished product of the 1,3-cyclohexanedione. The product obtained in the embodiment of the invention is pure white, the purity is 99.9 percent, the raw material conversion rate is more than 99.9 percent, and the product yield is about 95 percent.

Description

technical field [0001] The invention relates to a production method of a medicinal compound, in particular to an industrial production method of 1,3-cyclohexanedione. Background technique [0002] At present, 1,3-cyclohexanedione has been found to have a wide range of uses. 1,3-cyclohexanedione can be used to prepare drugs such as antiarrhythmic drugs, antithrombotic drugs, antitumor drugs, analgesics, virucidal agents, and 5-HT antagonists. 1,3-cyclohexanedione can also be used to prepare pesticides such as low-toxicity and high-efficiency herbicides. [0003] Catalytic hydrogenation of resorcinol as raw material to synthesize 1,3-cyclohexanedione is a common process in the world. Domestically, the current domestic patents represented by the invention patent (Application No.: 200510048956.X, published on October 12, 2005) of "A Preparation Method for 1,3-Cyclohexanedione" declared by Zhejiang University of Technology in 2005 highest level. Its main technical scheme is a...

AI Technical Summary

Problems solved by technology

[0005] (1) The purity is below 99.5%, which cannot meet the purity requirements of downstream products, especially high-end pharmaceutical products;

[0006] (2) The product obtained by the existing process is off-white or light yellow, with inconspicuous crystallization and relatively sticky products, which will quickly turn dark yellow during storage and transportation, making downstream products unusable;

[0007] (3) The amount of inorganic alkali used in the existing process is relatively large, which will affect the processes such as post-treatment acidification, increase material consumption, increase by-products, and increase the cost of wastewater treatment links;

[0008] (4) The reaction temperature of the catalytic hydrogenation process of the existing process is too high, and corresponding boilers and other public thermal energy facilities are required, so the energy consumption is high and causes a certain degree of pollution

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