Method for preparing isoamyl cinnamate

Abstract

The invention provides SO4<2-> / straw carbon-based solid sulfonic acid and a method for preparing isoamyl cinnamate by using the SO4<2-> / straw carbon-based solid sulfonic acid as a catalyst. The SO4<2-> / straw carbon-based solid sulfonic acid is prepared by the following steps of: adding straw powder into a sulfuric acid solution, quickly stirring until the straw powder is dissolved, performing constant-temperature carbonization at the temperature of between 70 and 90 DEG C to prepare straw carbon, adding into fuming sulphuric acid, performing constant-temperature sulfonation reaction at the temperature of between 70 and 90 DEG C, separating, drying, roasting and cooling. The isoamyl cinnamate is prepared by taking cinnamic acid and isoamyl alcohol as raw materials, home-made SO4<2-> / straw carbon-based solid sulfonic acid as the catalyst, and methylbenzene as a water-carrying agent. The raw materials have abundant sources, the method is low in cost, the using amount of the catalysts is small, a recovery method is simple, the catalyst can be used repeatedly, the reaction conditions are mild, the method is easy to operate, the quality of a product is stable and reliable, the yield of the product can reach over 90 percent, and the method is environment-friendly and is very suitable for industrial production.

Description

Technical field [0001] The invention relates to a method for preparing synthetic perfume, in particular to a method for preparing isoamyl cinnamate. Background technique [0002] Isoamyl cinnamate is also called β-phenyl isoamyl acrylate. As an important synthetic fragrance, it is often used in the preparation of edible flavors and daily chemical fragrances. It is a kind of fragrance that has a broad prospect and needs to be developed. [0003] At present, the preparation of isoamyl cinnamic acid is mainly obtained by esterification reaction with cinnamic acid and isoamyl alcohol as raw materials. There are the following methods according to the choice of catalyst: [0004] 1. It is obtained by esterification with sulfuric acid as a catalyst. In the process of esterification reaction, due to the poor selectivity of sulfuric acid and the functions of esterification, dehydration and oxidation, it leads to many side reactions, serious corrosion to equipment and long reaction time. , T...

AI Technical Summary

Problems solved by technology

[0004] 1. It is obtained by esterification with sulfuric acid as a catalyst. During the esterification reaction, due to the poor selectivity of sulfuric acid, it has the functions of esterification, dehydration and oxidation at the same time, resulting in many side reactions, serious corrosion of equipment, and long reaction time , Large amount of catalyst, deep color of the product, generation of "three wastes" and other shortcomings;

[0005] 2. It is obtained by catalytic synthesis of inorganic substances such as crystalline ferric chloride, crystalline sodium (potassium) bisulfate, crystalline tin tetrachloride, ammonium ferric sulfate dodecahydrate, titanium sulfate, etc., because such catalysts are easy to absorb moisture, It has certain solubility, weak acidity, large alcohol consumption, and low yield, resulting in difficulties in post-processing and high production costs;

[0006] 3. Obtained by using p-toluenesulfonic acid, strongly acidic cation exchange resin, solid superacid, heteropolyacid and other solid acids instead of sulfuric acid as catalyst. Although this method avoids a series of disadvantages caused by using sulfuric acid as catalyst, but Using p-toluenesulfonic acid as a catalyst, because it can be dissolved in the reaction system and consumes a lot of catalyst, while other new solid acids are expensive, resulting in high production costs;

[0007] 4. While using inorganic substances and solid acids as catalysts, the introduction of silica gel (resin) immobilization or microwave radiation can reduce the consumption of catalysts and improve the yield. However, due to silica gel (resin), microwave Reactor equipment is expensive, and the cost is greatly increased, and microwave technology is still in the exploration stage, making industrial production difficult