Method for compounding lily-of-the-valley pyran through reaction under static bed loaded solid superacid catalysis

Abstract

The invention provides a preparation method of lily-of-the-valley pyran by using a static bed loaded with a solid superacid catalyst. The method comprises the steps of selection of a static bed, weighing of raw materials, feeding of the raw materials and reaction in the static bed; in the step of weighing of the raw materials, the mass ratio of isovaleraldehyde to allylic alcohols is 1 to 0.93-1; in the step of reaction in the static bed, for the static bed loaded solid superacid catalyst, the length ranges from 80 cm to 280 cm, the gas flow rate ranges from 0.2 m / s to 3 m / s, and the pressure ranges from 0.015 MPa to 0.3 MPa. According to the preparation method, static bed loaded solid superacid serves as the catalyst to prepare the lily-of-the-valley pyran for the first time, the product yield is high, according to the allylic alcohols, the yield ranges from 95.1% to 96.3%, and according to the isovaleraldehyde, the yield ranges from 80.2% to 86.2%; the content of a gas phase of a product is over 99%; the method has the advantages of being good in selectivity, high in reaction efficiency, long in service life, less in amount of three wastes and the like, and the raw material product is prone to separation.

Description

technical field [0001] The invention relates to a method for synthesizing spice compounds, in particular to a method for synthesizing lily of the valley pyran under the catalysis of a solid superacid supported on a fixed bed, and belongs to the field of fine chemicals. Background technique [0002] Lily of the valley pyran can be used in almost all types of perfumes. It can produce elegant and diffuse floral fragrance without changing the original fragrance characteristics of the essence. [0003] At present, there are four domestic and foreign companies producing this product, and there is no domestic manufacturer. The foreign companies are American International Fragrance Company (IFF), German BASF Company (BASF), Swiss Givaudan Company and lwnospec Company; the total market capacity of this product For 2000 tons. [0004] At present, there are mainly two synthetic methods of lily of the valley pyran in the industry: one is to react with prenol and prenal to obtain the in...

AI Technical Summary

Problems solved by technology

[0008] (1) The yield of lily of the valley pyran is not high and the content is low;

[0009] (2) The traditional oil-water two-phase batch reaction catalyzed by liquid acid has low selectivity and conversion;

[0010] (3) The products produced by the existing technology are of poor quality;

[0011] (4) The existing intermittent reaction takes 8-12 hours, the reaction time is long and the reaction speed is slow;

[0012] (5) The cost is high, a large amount of solvent is used, and the solvent needs to be recovered;

[0013] (6) The catalyst used has poor catalytic effect, inconvenient use, short service life and long reaction cycle;

[0014] (7) The waste acid has a large amount of water and is not environmentally friendly

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