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Method for synthesizing gamma-undecalactone synthetic perfume by reactive distillation

A technology of reactive distillation and synthesis of fragrances, which is applied in sustainable manufacturing/processing, chemical industry, climate sustainability, etc., can solve the problems of complicated separation and purification process, low overall cost, and low reaction yield, and achieve the purpose of suppressing side effects. The amount of reaction and by-products produced, saving equipment investment, and improving the effect of reaction selectivity

Inactive Publication Date: 2018-12-14
ANHUI HYEA AROMAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The purpose of the present invention is to overcome the ubiquitous separation and purification process complex, high energy consumption, and low reaction yield deficiencies in the existing γ-undecalactone synthesis method, to provide a simple flow process, high reaction yield, and fast reaction speed , the overall cost is low, it is beneficial to form industrial scale production, and it is easy to realize the synthesis method of γ-undecalactone synthetic fragrance of product serialization

Method used

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  • Method for synthesizing gamma-undecalactone synthetic perfume by reactive distillation
  • Method for synthesizing gamma-undecalactone synthetic perfume by reactive distillation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A method for synthesizing γ-undecalactone by reactive distillation, comprising the following steps:

[0042] (a) Add 150g of octanol, 75g of acrylic acid and 15g of di-tert-butyl peroxide into a 500mL three-necked flask, turn on the electromagnetic stirrer and the integrated cooling and heat exchange machine, and keep the temperature at 20±5°C to obtain the ingredient mixture;

[0043] (b) Weigh 450g of octanol again, 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 120-180°C and keep it warm, then put the 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 150-180°C during the dripping, and the dropping time is controlled at 2-4h;

[0044] (c) Open the top condensed water of the reactive distillation tower,...

Embodiment 2

[0050] This example synthesizes γ-undecalactone synthetic perfume according to the method of Example 1, the difference is that in step (a), the addition amount of each material is: octanol 179g, di-tert-butyl peroxide 18.3g , 90g of acrylic acid;

[0051] In step (b), the amount of octanol taken again is 488g. The remaining method steps are consistent with the implementation method in Example 1.

[0052] In this example, a total of 29 g of by-product tert-butanol and water were separated from the top of the tower, 131 g of crude γ-undecalactone was separated from the bottom of the tower, and 11 g of low-boiling impurities and residual octanol were collected to obtain γ-undecalactone Lactone 118g.

Embodiment 3

[0054] This example synthesizes γ-undecalactone synthetic perfume according to the method of Example 1, the difference is that in step (a), the addition of each material is: octanol 195g, di-tert-butyl peroxide 24.4g , 60g of acrylic acid;

[0055] In step (b), the amount of octanol taken again is 542g. The remaining method steps are consistent with the implementation method in Example 1.

[0056] In this example, a total of 27 g of by-product tert-butanol and water were separated from the top of the tower, 110 g of crude γ-undecalactone was separated from the bottom of the tower, and 10 g of low-boiling impurities and residual octanol were collected to obtain γ-undecalactone Lactone 98g.

[0057] 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 gas: N 2 , flow rate 20L / min, column front pressu...

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Abstract

The invention belongs to the technical field of the fine chemical industry, and specifically relates to a method for synthesizing gamma-undecalactone synthetic perfume by reactive distillation. The method comprises the following steps: (a) mixing octanol, acrylic acid and di-tert-butyl peroxide to obtain a mixture of ingredients; (b) weighing octanol, adding octanol to a heater of a reactive distillation column, and feeding the mixture of ingredients in the step (a) into a reaction zone of the reaction distillation column; (c) opening condensate water at the top of the reaction distillation column, and separating a crude product of gamma-undecalactone from the bottom of the column; and (d) transferring the crude product of gamma-undecalactone into a rotary evaporator, controlling the vacuum degree, temperature and rotating speed and collecting gamma-undecalactone. The method provided by the present invention adopts a reactive distillation technology to separate by-products from the reaction system in time, the reaction is carried out in two directions through promoting the separation by the reaction and promoting the reaction by the separation, the reaction efficiency is improved,and the reaction yield is ensured.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a method for synthesizing gamma-undecalactone and perfume through reactive distillation. Background technique [0002] γ-Undecalactone, commonly known as gamma-undecalactone, peach aldehyde, tetradecaldehyde, CAS number 104-67-6, chemical name 5-heptyldihydro-2(3H)-furanone, natural Exist in peaches, apricots, sweet-scented osmanthus, soybean hydrolyzed protein, butter, egg fruit flowers, etc. γ-Undecalactone has a normal pressure boiling point of 297°C, soluble in ethanol (1ml in 5mL 60% ethanol), benzyl alcohol, benzyl benzoate, propylene glycol, lye, most non-volatile oils and mineral oils, almost insoluble In glycerin and water; it is a colorless transparent to light yellow viscous liquid with a strong fruity aroma, like peaches and almonds. [0003] As one of the most commonly used spices, γ-undecalactone is the most important and the most widely used pr...

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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