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Method for synthesizing natural perfume nonanal

A technology of natural spices and synthetic methods, which is applied in the direction of oxidative preparation of carbonyl compounds, organic chemistry, etc., which can solve the problems of unsatisfactory demand, unsafe production, and low content, etc., to improve the production process level, high conversion rate, and easy industrial operation Effect

Active Publication Date: 2009-12-09
黄山科宏生物香料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Nonanal naturally exists in essential oils such as rose oil, citrus oil, lime oil, and claret oil. Since its content in the above essential oils is very small, only 0.8-1.2‰, it cannot meet people's demand for this product
However, there are high pollution and unsafe factors in the current production of nonanal, so it is urgent to develop a new production process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] In a 1-liter flask, add 36 grams of trichloroisocyanuric acid, 580 milliliters of chloroform, 33 grams of calcium oxide and 75 grams of natural nonanol, and add dropwise 0.4 grams of catalyst dissolved in 20 milliliters of chloroform solution under stirring. The catalyst described above is triethanolamine, control the reaction temperature at about 40 degrees, stir for 2 hours, the product conversion is 70%, continue to stir for 2 hours, add 0.3 grams of catalyst triethanolamine, 15 grams of trichloroisocyanuric acid, and stir for another 2 hours Finally, the solid was removed, the liquid was washed until neutral, the solvent was recovered, the pressure was reduced to 0.097Mpa, and the boiling point was 102°C to obtain 12 g of the product with a purity of 94%.

Embodiment 2

[0013] Under nitrogen protection, in a 1-liter flask, add 36 grams of trichloroisocyanuric acid, 580 milliliters of chloroform, 33 grams of calcium oxide and 75 grams of natural nonanol, add dropwise 0.4 grams of catalyst dissolved in 20 milliliters of chloroform Methane solution, the catalyst is triethanolamine, control the reaction temperature at about 40 degrees, stir for 2 hours, the product conversion is 67%, continue to stir for 2 hours, add 0.3 grams of catalyst triethanolamine, 15 grams of trichloroisocyanuric acid, After stirring for another 2 hours, the solid was removed, the liquid was washed until neutral, the solvent was recovered, the pressure was reduced to 0.097Mpa, and the boiling point was 102°C to obtain 32 g of the product with a purity of 96%.

Embodiment 3

[0015] Under the protection of nitrogen, in a 1-liter flask, add 36 grams of powdered trichloroisocyanuric acid, 580 milliliters of chloroform, 33 grams of calcium oxide and 75 grams of natural nonanol, add dropwise 0.4 grams of catalyst in 20 milliliters of Chloroform solution, the catalyst is triethanolamine, control the reaction temperature below 40 degrees, stir for 2 hours, the product conversion is 72%, continue to stir for 2 hours, add 0.3 grams of catalyst triethanolamine, trichloroisocyanuric acid 15 After stirring for another 2 hours, the solid was removed, the liquid was washed until neutral, the solvent was recovered, the pressure was reduced to 0.097Mpa, and the boiling point was 102°C to obtain 42 g of the product with a purity of 98%.

[0016] To sum up the experimental results, the new process of using natural nonanol to prepare natural nonanal has achieved the purpose of high conversion rate, no pollution and easy industrial operation. Or the high pollution an...

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Abstract

The invention belongs to a new process for synthesizing natural identical perfume nonanal. The method comprises the following steps: mixing and stirring 36 grams of trichloroiminocyanuric acid, 580 milliliters of trichloromethane, 33 grams of calcium oxide and 75 grams of nonanol; dripping 20 milliliters of trichloromethane solution containing 0.4 gram of trolamine while stirring the solution, keeping on stirring the solution at a temperature of 40 DEG C to react for 4 hours; adding 0.3 gram of trolamine and 15 grams of trichloroiminocyanuric acid into the solution, and keeping on stirring at 40 DEG C to react for 2 hours; removing solid from the reaction solution, washing the solution to neutrality by liquid, recovering organic solvent, distilling the obtained organic solvent by decompressing to 0.097MPa, and obtaining the fraction at boiling point of 102 DEG C, which is the final product. The method of the invention prepares the nonanal by the new process with high conversion rate, no pollution and easy industrial operation.

Description

technical field [0001] The invention belongs to a new process for synthesizing natural equivalent spices, in particular to a synthetic method of natural spice nonanal. Background technique [0002] Natural fragrance nonanal, also known as natural nonanal, nonanal, geranium aldehyde, α-hydrononane, has rose aroma, is a kind of fragrance used in daily chemical fragrance formula, and is very widely used in the fragrance industry. Widely used, mainly used in rose, orange blossom, acacia and other floral and fantasy flavors, the dosage is generally 0.5-5%. Nonanal naturally exists in essential oils such as rose oil, citrus oil, lime oil, and claret oil. Because its content in the above essential oils is very small, only 0.8-1.2‰, it cannot meet people's demand for this product. However, the current production process of nonanal has high pollution and unsafe production factors, so it is urgent to develop a new production process. Contents of the invention [0003] The purpose ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/02C07C45/29
Inventor 程存照
Owner 黄山科宏生物香料股份有限公司
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