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Method for producing epsilon-decalactone synthetic perfume

A technology for synthesizing spices and production methods, applied in the direction of organic chemistry, which can solve the problems of harsh reaction conditions, complicated operations, and low yields, and achieve the effects of readily available raw materials, high reaction yields, and overcoming incomplete reactions

Inactive Publication Date: 2019-05-14
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

However, the existing ε-decalactone production method has the disadvantages of high cost, harsh reaction conditions, complex operation and low yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] A kind of production method of epsilon-decalactone synthetic perfume:

[0075] S1: to 3m 3 Add 1950kg of clear water into the alkaline water mixing pot, turn on the agitator, and then put 50kg of sodium hydroxide through the hand hole, after stirring evenly, pump it into the high level tank of alkaline water with an anti-corrosion pump for later use;

[0076] S2: Add 145kg of n-butyraldehyde and 195kg of cyclohexanone to the 0.5m 3 In the stirring pot, stir the mixture A evenly, and beat the mixture A to 0.5m 3 Reserve the mixture in the overhead tank.

[0077] S3: 2.5% sodium hydroxide 2000kg in step S1 is added to 5m through the alkaline water head tank 3 In the reaction kettle, 195kg of cyclohexanone was added into the reaction kettle through the cyclohexanone head tank and mixed evenly, and then the steam valve was opened to raise the temperature of the reaction kettle to 75°C.

[0078] S4: Control the temperature of the reactor at 75°C, adopt multi-stage multi-...

Embodiment 2

[0090] A kind of production method of epsilon-decalactone synthetic perfume:

[0091] S1: to 5m 3 Add 3200kg of clear water to the alkaline water mixing pot, turn on the agitator, and then put in 85kg of sodium hydroxide through the hand hole. After stirring evenly, pump it into the high level tank of alkaline water with an anti-corrosion pump for later use.

[0092] S2: Add 250kg of n-butyraldehyde and 325kg of cyclohexanone to 1m 3 In the stirring pot, stir the mixture A evenly, and beat the mixture A to 1m 3 Reserve the mixture in the overhead tank.

[0093] S3: Add the sodium hydroxide solution configured in step S1 to 10m through the alkaline water head tank 3 In the reaction kettle, 330kg of cyclohexanone was added into the reaction kettle through the cyclohexanone head tank and mixed evenly, and then the steam valve was opened to raise the temperature of the reaction kettle to 80°C.

[0094] S4: Control the temperature of the reactor at 80°C, adopt the multi-stage m...

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PUM

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Abstract

The invention belongs to the technical field of perfume production and in particular relates to a method for producing an epsilon-decalactone synthetic perfume. The method comprises the following steps: (1) preparing alkaline water; (2) preparing a mixture A of cyclohexanone and n-butanal; (3) putting the alkaline water into a reaction kettle, and uniformly mixing a bottom material, namely the cyclohexanone, in the reaction kettle; (4) dropping the mixture A into the reaction kettle, dropping and stirring simultaneously, continuously stirring after dropping is completed, and performing thermalreaction till the content of n-butanal is less than 1%; and (5) purifying the product of the step (4), and carrying out hydrogenation, separation and purification, oxidation and separation and purification in sequence, thereby obtaining the epsilon-decalactone synthetic perfume. By adopting the n-butanal and the cyclohexanone as initial raw materials, an aldol condensation reaction is carried out, hydrogenation is further carried out, a peracetic acid oxidation ring enlargement reaction is performed to synthesize the epsilon-decalactone synthetic perfume, the excessive cyclohexanone is adopted as a reaction solvent which is recycled and applied mechanically, a reaction solvent separation and purification procedure is reduced, and in addition, the method is easy in raw material obtaining and high in reaction yield.

Description

technical field [0001] The invention belongs to the technical field of perfume production, and in particular relates to a production method of ε-decalactone synthetic perfume. Background technique [0002] ε-decalactone is a colorless to pale yellow liquid with a sweet creamy aroma, which can be used in food flavors and has been approved by the American Flavor and Extract Manufacturers Association (FEMA No.3613) and approved by the FDA. edible. ε-decalactone is widely used in milk, cream essence and baked goods. However, the existing production method of ε-decalactone has the disadvantages of high cost, harsh reaction conditions, complicated operation and low yield. Contents of the invention [0003] The purpose of the present invention is to overcome the deficiencies in the prior art and provide a production method of ε-decalactone synthetic perfume with high yield, low cost and simpler operation. [0004] In order to achieve the above object, the present invention ado...

Claims

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Application Information

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IPC IPC(8): C07D313/04
Inventor 王天义范一义徐基龙严四五
Owner 安徽华业香料合肥有限公司
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