Preparation method of solid base catalyst and reaction method for catalytically synthesizing ionone series fragrance intermediates

Abstract

The invention discloses a preparation method of a solid alkali catalyst and a reaction method for the catalytic synthesis of an ionone fragrance intermediate by the solid alkali catalyst. The preparation method of the solid alkali catalyst comprises the following steps: putting a carrier in a flask, adding KF (Potassium Fluoride) aqueous solution, stirring for 4-9h at the temperature of 40-80DEG C in an ultrasonic oscillator, then, stirring at the temperature of 89-99DEG C until a mixture is viscous, drying the mixture, roasting for 4-7h at the temperature of 400-600DEG C, and cooling to obtain the solid alkali catalyst which loads KF on the carrier, wherein the carrier is one of aluminium oxide or magnesium oxide or calcium oxide. Since an ultrasonic-assisted excessive dipping method is adopted to prepare the solid alkali catalyst, the loading capability and the dipping rate of active components are effectively improved. In addition, when the solid alkali catalyst prepared with the preparation method is used for carrying out the catalytic synthesis of the ionone fragrance intermediate, a subsequent alkali neutralization operation carried out when liquid alkali catalyst is used is avoided, cost is lowered, sewage is reduced, catalytic reaction has a high yield, the catalyst and a product can be easily separated, and the catalyst can be repeatedly used.

Description

technical field [0001] The invention relates to a preparation method of a solid base catalyst for catalyzing and synthesizing an intermediate of ionone-series fragrance, and a reaction method for catalyzing the synthesis of an intermediate of ionone-series fragrance by using the catalyst. Background technique [0002] At present, pseudoionone and methyl pseudoionone are important intermediates for the synthesis of ionone, which are widely used in the industries of spices, medicine, and food additives. Ionone is a kind of precious spice with woody aroma. It is one of the largest and most important spices in the perfume industry. At the same time, the synthesized β-ionone is an important intermediate for the synthesis of vitamin A and β-carotene. [0003] The catalysts commonly used in the traditional synthesis process are liquid alkali catalysts, such as NaOH aqueous solution and Ba(OH)2 saturated aqueous solution, as well as alcohol solution systems such as EtONa / EtOH, NaOH / ...

AI Technical Summary

Problems solved by technology

The main disadvantages of using these liquid caustic soda catalysts are the difficulty of catalyst reuse, large equipment corrosion, serious environmental pollution and other problems.

In order to overcome the above shortcomings, domestic and foreign scholars have been exploring the improvement of the synthesis process of pseudoionone and its homologues. The current general idea is to replace the liquid alkali catalyst with a solid alkali catalyst, and use more such as hydrotalcite and MgO and Loaded alkali catalysts such as KNO3, KOH, K2CO3, and KF are immobilized on the Al2O3 carrier, which not only can realize a high-activity, high-selectivity catalytic reaction process, the catalyst is easy to recycle, and solves a series of environmental pollution problems. However, existing methods The prepared solid base catalyst was simply impregnated and did not use ultrasonic waves to assist in the production, so there were problems such as uneven distribution of active components on the load, and the content was low and uncontrollable, resulting in poor reproducibility of catalyst preparation.

[0004] In addition, when the existing liquid alkali catalyst is used to catalyze the synthesis of pseudoionone and its homologues, the operation of subsequent neutralization alkali is cumbersome, the cost is high, and the environment is polluted