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Synthesis method of biomass-based gamma-octadecalactone

A synthesis method and biomass technology, applied in organic chemistry and other directions, can solve problems such as affecting quality and complicated procedures, and achieve the effects of improving quality, uniform microporous structure, and reducing synthesis procedures.

Active Publication Date: 2021-10-08
ANHUI HYEA AROMAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The γ-stearactone prepared in the existing synthesis process has obvious plastic smell or sour taste, which affects its quality. In addition, it is necessary to add a separate post-processing step to deodorize the product, and the process is complicated

Method used

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  • Synthesis method of biomass-based gamma-octadecalactone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of additives:

[0024] Step S11, mixing diatomaceous earth and deionized water, stirring and mixing at 50°C for 30 minutes, passing through a 100-mesh sieve, drying at 40°C to constant weight, and then roasting at 700°C for 2 hours, Then cool to room temperature to obtain solid A; wherein, the mass ratio of diatomaceous earth and deionized water is 1:20;

[0025] Step S12, mix solid A and alkali solution, and react at a temperature of 50°C for 1 hour. After the reaction, wash the reacted solution with distilled water until the washing liquid is neutral. , dried to constant weight to obtain the additive. The alkali solution is an aqueous sodium hydroxide solution, and the mass fraction of the alkali solution is 15%; the dosage ratio of the solid A to the alkali solution is 1 g: 3 mL.

Embodiment 2

[0027] Preparation of additives:

[0028] Step S11, mixing diatomaceous earth and deionized water, then stirring and mixing at 75°C for 50 minutes, passing through a 100-mesh sieve, drying at 40°C to constant weight, and then roasting at 800°C for 2 hours, Then cool to room temperature to obtain solid A; wherein, the mass ratio of diatomaceous earth and deionized water is 1:20;

[0029] Step S12, mix the solid A and the alkali solution, and react at a temperature of 60°C for 1 hour. After the reaction, wash the reacted solution with distilled water until the washing liquid is neutral. , dried to constant weight to obtain the additive. The alkali solution is ammonia water, and the mass fraction of the alkali solution is 15%; the dosage ratio of the solid A and the alkali solution is 1g:3mL.

Embodiment 3

[0031] The synthetic method based on biomass-based gamma-octadecalactone comprises the following steps:

[0032] The first step is to mix the solvent and oleic acid, add the catalyst and additives at a temperature of 0°C, and heat to reflux at a temperature of 70°C for 8 hours;

[0033] In the second step, after the reaction is completed, filter, and extract the filtrate with deionized water and ether, concentrate and dry the obtained organic phase under reduced pressure to obtain γ-stearactone.

[0034] Wherein, the catalyst is concentrated sulfuric acid with a mass fraction of 98%; the solvent is n-hexane. The temperature during drying was 30°C. The additive is prepared in Example 1.

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Abstract

The invention relates to a synthesis method of biomass-based gamma-octadecalactone, and belongs to the technical field of perfume synthesis. The synthesis method specifically comprises the following steps: 1, mixing a solvent and oleic acid, adding a catalyst and an additive at the temperature of 0-5 DEG C, and conducting heating and refluxing at the temperature of 70-85 DEG C for 8-10 hours; and 2, after the reaction is finished, conducting filtering, extracting the filtrate with deionized water and diethyl ether, concentrating the obtained organic phase under reduced pressure, and conducting drying to obtain gamma-octadecalactone. In the synthesis process, an additive is also prepared, the additive takes the diatomite as a raw material, after roasting, the microporous structure of the diatomite is more uniform, peculiar smell generated in the reaction process can be better absorbed, the product quality is improved, on the one hand, the alkali solution can react with metal oxides in the diatomite, the content of metal oxide is reduced, the content of silicon dioxide is increased, and the yield of the product is improved.

Description

technical field [0001] The invention belongs to the technical field of perfume synthesis, and in particular relates to a synthesis method based on biomass-based gamma-stearactone. Background technique [0002] Saturated γ-lactone compounds naturally exist in various fruits and are a very important class of food flavors, which are now widely used in various beverages, baked goods and desserts. Among them, γ-octadecanolide is a kind of fragrance substance commonly used in the field of daily chemical industry. Used in food, daily cosmetics and tobacco flavors and other fields. [0003] The γ-stearactone prepared in the existing synthesis process has obvious plastic smell or sour taste, which affects its quality. In addition, it is necessary to add a separate post-processing step to deodorize the product, and the process is complicated. Contents of the invention [0004] The object of the present invention is to provide a synthetic method based on biomass-based γ-stearactone...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33
CPCC07D307/33Y02P20/584
Inventor 王天义范一义汪洋张政吴旭何云飞汪炎
Owner ANHUI HYEA AROMAS
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