Production device and method of delta-caprolactone synthetic perfume

A technology for synthesizing fragrances and production methods, applied in chemical instruments and methods, sustainable manufacturing/processing, chemical industry, etc., can solve problems such as high cost, low yield of δ-caprolactone synthesis, complex process, etc., to achieve Effects of reducing waste, improving production efficiency, and increasing reaction yield

Pending Publication Date: 2021-01-26
安徽华业香料合肥有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a production device and method for synthesizing perfumes with δ-caprolactone. By using the production device, ethyl acetoacetate and methyl acrylate are used as starting materials,

Method used

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  • Production device and method of delta-caprolactone synthetic perfume

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Embodiment 1

[0031] A kind of production method of delta-caprolactone synthetic perfume, specifically comprises the following steps:

[0032] Step S1, open the circulating cooling water and agitator of the reaction kettle 3 of the fragrance production device, add 300 kg of ethyl acetoacetate from the ethyl acetoacetate header tank 1 to the reaction kettle 3, and then add 3 kg of sodium hydroxide to the reaction kettle 3 , stir evenly; open the steam valve of reactor 3, heat up reactor 3, control the temperature of the kettle at 35°C, then add 90kg of methyl acrylate dropwise from methyl acrylate head tank 2 through dripping pump 4 to reactor 3, drop Adding time is controlled at 5.5h. After the dropwise addition, keep the kettle temperature and stir for 1h, take a sample for gas chromatography detection, when the ethyl acetoacetate content is below 1%, the reaction is terminated, and the reaction solution is transferred to the still 5;

[0033] Step S2, open the steam valve of the still 5, ...

Embodiment 2

[0044] A kind of production method of delta-caprolactone synthetic perfume, specifically comprises the following steps:

[0045] Step S1, open the circulating cooling water and the agitator of the reaction kettle 3 of the fragrance production device, add 500 kg of ethyl acetoacetate from the ethyl acetoacetate header tank 1 to the reaction kettle 3, and then add 8 kg of sodium hydroxide to the reaction kettle 3 , stir evenly; open the steam valve of reactor 3, heat up reactor 3, control the temperature of the kettle at 45°C, then add 150kg of methyl acrylate dropwise from methyl acrylate head tank 2 through dripping pump 4 to reactor 3, drop Adding time is controlled at 8h. After the dropwise addition, keep the kettle temperature and stir for 1h, take a sample for gas chromatography detection, when the ethyl acetoacetate content is below 1%, the reaction is terminated, and the reaction solution is transferred to the still 5;

[0046] Step S2, open the steam valve of the still ...

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Abstract

The invention discloses a production device and method of delta-caprolactone synthetic perfume, which comprises the following steps: proportionally adding ethyl acetoacetate and sodium hydroxide intoa reaction kettle, uniformly stirring, heating, dropwisely adding methyl acrylate, and recovering excessive ethyl acetoacetate to obtain acetyl succinate; adding acetyl succinate and sulfuric acid into a decarboxylation kettle, heating and stirring for reaction, collecting a byproduct ethanol to obtain acetylbutyric acid, transferring the acetylbutyric acid into a water washing kettle for alkali washing and water washing, adding the acetylbutyric acid and methanol into a hydrogenation kettle, and introducing hydrogen for hydrogenation reaction; after the reaction is finished, carrying out solid-liquid separation through an automatic backwash precision filter, pressing a solid-phase catalyst back into the reaction kettle, continuing to apply the next batch of reaction, transferring a liquidphase into a rectifying kettle, and carrying out reduced pressure distillation to collect a delta-caprolactone product after methanol recovery at normal pressure is finished; according to the method,the problems of low delta caprolactone synthesis yield, high cost and complex process flow are solved.

Description

technical field [0001] The invention belongs to the technical field of perfume production, and in particular relates to a production device and method for synthesizing perfume with delta-caprolactone. Background technique [0002] δ-caprolactone is a colorless to light yellow oily liquid, which is an important organic compound and intermediate. It has broad application and development prospects in the fields of flavors and fragrances and drug synthesis. Natural products exist in coconut oil, hot milk fat, etc. GB2760 National Food Safety Standard stipulates that it is a food flavoring that is allowed to be used. It has a coconut oil and creamy aroma, with burnt and fruity aromas. It is used in food flavors such as almonds, cherries, butter, and cream, and is also used in tobacco flavors. [0003] There are many methods for the synthesis of δ-caprolactone, mainly including: one is the 1,5-hexanediol route, the raw materials of this method are not easy to obtain, and there is ...

Claims

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Application Information

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IPC IPC(8): C07D313/04B01J8/10B01J8/00B01D3/10
CPCC07D313/04B01J8/10B01J8/006B01D3/10Y02P20/50Y02P20/10
Inventor 王天义汪洋张政吴旭李方节
Owner 安徽华业香料合肥有限公司
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