Method for preparing dehydrolinalyl acetate from dehydrolinalool

A technology of dehydrolinalool and linalyl ester, which is applied in the field of preparation of dehydrolinalyl acetate, can solve the problems of low catalyst activity, complicated separation process, lack of application value, etc., and achieve high reactivity and convenient separation , highly active effect

Inactive Publication Date: 2008-07-02
SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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  • Abstract
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Problems solved by technology

However, the activity of the catalyst used in the esterification process is very low, the reaction time is as long as more than ten hours, and the process of separating the catalyst from the product is also relatively complicated, which lacks application value

Method used

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  • Method for preparing dehydrolinalyl acetate from dehydrolinalool
  • Method for preparing dehydrolinalyl acetate from dehydrolinalool
  • Method for preparing dehydrolinalyl acetate from dehydrolinalool

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Embodiment 1～11

[0018] A 500ml three-necked flask with a stirring device is placed in a water bath, 152g of dehydrolinalool is added, nitrogen is purged for 20min, the temperature is raised to the reaction temperature with stirring, and acetic anhydride is dropped in according to the required molar ratio, and the The required amount of catalyst starts the reaction and maintains the required reaction time to complete the reaction. After the product obtained by the esterification reaction is cooled, the catalyst is separated by precipitation. The liquid phase is washed with water, and the oil and water phases are separated by static layering until the oil phase material is neutral, and the oil phase material is taken to obtain the dehydrolinalyl acetate product.

[0019] The catalyst is a macroporous sulfonic acid cation exchange resin with an exchange capacity of 4.8-5.0 mmol / g, a cross-linking degree of 16-18%, and a pore diameter of 15-20 nm.

[0020] The specific reaction conditions of eac...

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Abstract

The invention relates to a method for preparing dehydrolinalyl acetate from dehydrolinalool. The method comprises esterification between dehydrolinalool and acetic anhydride is carried out in the presence of catalyst so as to obtain dehydrolinalyl acetate. Molar ratio of raw material provided of dehydrolinalool to acetic anhydride is 1: (1-5); reaction temperature is 40-80 DEG C; reaction pressure is normal pressure; reaction time is 60-240min; the catalyst is macroporous sulfonic acidic cation exchange resin; exchange capacity of the catalyst is 4.8-5.0mmol/g; degree of cross linking of the catalyst is 16-18 percent; aperture of the catalyst is 15-20nm and dosage is 2-20wt percent of total amount of the raw material provided. The invention has the advantages that reaction activity of the esterification catalyst adopted is high; conversion of raw material and selectivity of product, etc. are ideal; the catalyst basically does not have corrosiveness or have environmental impact; removal of the catalyst from the product is convenient.

Description

technical field [0001] The invention relates to a preparation method of acid-containing linalyl ester, in particular to a preparation method of dehydrolinalyl acetate undergoing esterification reaction in the presence of an acidic catalyst to generate dehydrolinalyl acetate. Background technique [0002] Dehydrolinalyl acetate is an important fine chemical intermediate for the preparation of fragrances, and can be used to produce fine chemical products such as citral and ionone. Linalyl acetate can also be obtained through hydrogenation reaction of dehydrolinalyl acetate. Linalyl acetate is one of the main components of lavender oil. It has an elegant fragrance, similar to bergamot oil and lavender oil. An important raw material for spices or essences. In the prior art, linalyl acetate is mostly prepared by esterification of linalool and acetic anhydride, because linalool can be obtained from isoprene, the separated product of the C5 fraction of the by-product of petroleum ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/145
Inventor 安源郭世卓朱岳中吴卓
Owner SINOPEC SHANGHAI PETROCHEMICAL CO LTD
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