Method for compounding gamma-decalactone synthetic perfume through reactive distillation

A technology for the synthesis of gamma-decalactone and fragrances, which is applied in the direction of sustainable manufacturing/processing, chemical industry, climate sustainability, etc. It can solve the problems of insufficient aroma quality, complicated separation and purification process, and low reaction yield. , to achieve the effect of saving equipment investment, shortening reaction time and simplifying the process

Inactive Publication Date: 2019-01-11
ANHUI HYEA AROMAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The purpose of the present invention is to overcome the common problems of complex separation and purification process, high energy consumption, low reaction yield and insufficient pure aroma quality in the existing synthetic method of gamma-decalactone, and to provide

Method used

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  • Method for compounding gamma-decalactone synthetic perfume through reactive distillation
  • Method for compounding gamma-decalactone synthetic perfume through reactive distillation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A method for synthesizing perfume by reactive distillation, characterized in that: comprising the following steps:

[0038] (a) Add 120g of heptanol, 90g of methyl acrylate, 1g of catalyst sodium borohydride and 15g of initiator di-tert-butyl peroxide into a 500mL three-necked flask according to the proportion of ingredients, and turn on the electromagnetic stirrer and the integrated cooling and heat exchange machine , keeping the temperature at 20±5°C to obtain the ingredient mixture;

[0039] (b) Weigh again 360g of heptanol, add it to the 1500mL heater of the reactive distillation tower, turn on the electromagnetic stirrer and the integrated cooling and heat exchange machine, raise the temperature of the heater to 115-175°C and keep it warm, then put The batching mixture in the step (a) is sent into the reaction zone of the reactive distillation tower through the dripping pump; the temperature of the heater is controlled at 145-175°C during the dripping, and the drop...

Embodiment 2

[0047] The present embodiment prepares the synthetic perfume of gamma-decalactone according to the method of Example 1, the difference is that in step (a), the addition of each material is: heptanol 160g, di-tert-butyl peroxide 24g, Sodium borohydride 1g, methyl acrylate 95g;

[0048] In step (b), the amount of heptanol is weighed again to be 257g; the rest remain unchanged to obtain the gamma-decalactone product.

[0049] In this example, a total of 37 g of by-product tert-butanol and methanol were separated from the top of the tower, 128 g of the crude product of gamma-decalactone was separated from the bottom of the tower, and 13 g of low-boiling impurities and residual heptanol were collected to obtain gamma-decalactone 112g.

Embodiment 3

[0051] The present embodiment prepares the synthetic fragrance of gamma-decalactone according to the method of Example 1, the difference is that in step (a), the addition amount of each material is: heptanol 177g, di-tert-butyl peroxide 32g, Sodium borohydride 1.6g, methyl acrylate 75g;

[0052] In step (b), the amount of heptanol is weighed again to be 405g; the rest remain unchanged to obtain the gamma-decalactone product.

[0053] In this example, a total of 39 g of by-products tert-butanol and methanol were separated from the top of the tower, 103 g of crude product of gamma-decalactone was separated from the bottom of the tower, and 10 g of low-boiling impurities and residual heptanol were collected to obtain gamma-decalactone 89g.

[0054] The GC conditions for product detection are: chromatographic column HP-5 (30m×0.32mm×0.25μm); detector FID, temperature 280°C; sample injection: injection volume is about 0.2μl, split ratio 1:100, inlet temperature 250 °C; carrier ga...

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Abstract

The invention belongs to the technical field of fine chemical engineering and specifically relates to a method for compounding a gamma-decalactone synthetic perfume through reactive distillation. Themethod comprises the following steps: (a) mixing heptanol, methyl acrylate, sodium borohydride and bi-tertiary butyl peroxide, thereby acquiring a mixture; (b) weighting heptanol, adding into a heaterof a reactive distillation column and using a dropwise adding pump for feeding the mixture acquired in the step (a) into a reaction zone of the reactive distillation column; (c) opening condensate water on the top of the reactive distillation column and separating a crude product of gamma-decalactone from column bottom; (d) transferring the crude product of gamma-decalactone into a rotary evaporator, controlling vacuum degree, temperature and rotational speed, and collecting gamma-decalactone. According to the invention, a reactive distillation technology is adopted, by-products are timely separated from a reaction system, separation is boosted by reaction, reaction is boosted by separation and the reaction yield is guaranteed.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for synthesizing gamma-decalactone and perfume through reactive distillation. Background technique [0002] Gamma-decalactone, CAS No. 706-14-9, chemical name γ-decalactone (5-hexyldihydro-2(3H)-furanone), naturally exists in peaches, almonds, strawberries and other fruits . Gammadecalactone normal pressure boiling point 281°C / 156°C (2.3kPa), soluble in ethanol (1ml in 1mL 90% ethanol), benzyl alcohol, benzyl benzoate, propylene glycol, lye, most non-volatile oils and mineral oil, practically insoluble in glycerin and water. It is a colorless transparent to yellowish viscous liquid with a strong coconut and peach fruity aroma, and a peach-like aroma when diluted. [0003] As one of the most commonly used fragrances, gamma-decalactone is the most important of the lactone series of synthetic fragrances, and it is also one of the products with the larg...

Claims

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Application Information

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IPC IPC(8): C07D307/33
CPCC07D307/33Y02P20/10
Inventor 王天义范一义徐基龙严四五
Owner ANHUI HYEA AROMAS
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