Method for synthesizing tricyclodecenyl propionate perfume by adopting loaded solid acid catalyst

Abstract

The invention discloses a synthesis method of a tricyclodecenyl propionate perfume. Petroleum coking byproducts dicyclopentadiene and propionic acid are used as the raw materials, under the catalysis of loaded solid acid, the raw materials directly have acetylation through electrophilic addition to prepare crude tricyclodecenyl propionate at one step, and meanwhile, a small amount of a propionic anhydride guard catalyst is added to prevent the crude tricyclodecenyl propionate from having hydrolysis reaction with a small amount of moisture in the material; then, propionic acid is recycled for applied mechanically, and the finished tricyclodecenyl propionate product is obtained through neutralizing, washing and rectification. According to the synthesis method, the petroleum coking byproducts used as the raw materials are easily available, the reaction condition is moderate, the reaction conversion rate is high, the technology is easier to implement, the discharge capacity of three wastes generated in the production process is low, the product yield is greatly increased, and the synthesis method belongs to technology of cleaner production. In addition, the content of tricyclo[5, 2, 1, 0<2.6>]-3-decene-9-yl acetate with delicate fragrance and fragrance and sweetness of anise is more than 92%, and the product green wood is pure, fine and mild in fragrance. The invention further provides a synthesis device special for the synthesis method of a tricyclodecenyl propionate perfume.

Description

technical field [0001] The invention relates to the technical field of fine chemical synthesis, in particular to a method for preparing organically synthesized spices. Background technique [0002] Tricyclodecenyl propionate is widely used in various flavor formulas in daily chemical flavors. It is commonly found in surface cleaners, shampoos, deodorants, detergents, soaps and other flavors. It has a sweet fruity aroma Floral fragrance, accompanied by the aroma of jasmine and anise, is an important synthetic fragrance in the cycloalkene family. The aroma is softer than tricyclodecenyl acetate. It is suitable for use with other cycloalkene family fragrances. The dosage can be adjusted Reaching within 10%, IFRA has not made restrictions on the use. [0003] Tricyclodecenyl Propionate has a woody and herbaceous aroma with floral and fruity aromas and woody notes. Appearance is colorless to light yellow transparent liquid, tricyclodecenyl propionate is a mixture of four isomer...

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Problems solved by technology

[0009] The binary compound acid of perchloric acid-phosphoric acid is used as a catalyst for the acetylation reaction. Compared with perchloric acid as a catalyst, the reaction conditions are optimized, the production cost is reduced, and the yield of the synthesis reaction is relatively improved. However, high-strength acid is harmful to equipment. The corrosion problem of TCDA is relatively serious, and the isomer ratio of the prepared TCDA cannot meet the requirements of aroma quality, and the product has a floral-fruity sweet tricyclic [5,2,1,0 2.6 The content of ]-3-decen-9-ol propionate is low, resulting in a sour aroma and affecting product quality

[0010] Boron trifluoride or boron trifluoride addition complexes are used as catalysts, and the molar ratio of propionic acid to dicyclopentadiene is at least 2.5:1, and the stripping process is used to recover propionic acid instead of using alkali for excess acid However, even distillation cannot provide commercially acceptable aroma and product quality, so the distilled material must be further purified by passing the target product through a chromatographic column containing activated carbon or marble to remove traces. Amount of BF 3 Catalyst and propionic acid to meet product quality requirements

However, ion exchange resins have well-known disadvantages such as high cost and loss of activity when recycled.

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