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Production method of synthesizing gamma-undecalactone synthetic perfume by reactive distillation

A technology of reactive distillation and synthesis of fragrances, which is applied in the direction of sustainable manufacturing/processing, chemical industry, climate sustainability, etc., can solve the problems of reaction yield decline, impact on aroma quality, bad smell of fuel consumption, etc., and improve reaction speed , shorten the reaction time, and save equipment investment

Pending 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

Using n-octanol and acrylic acid as the starting materials, di-tert-butyl peroxide as the initiator, adding the reaction solvent, first adopting the "one-pot cooking" method, free radical addition synthesis crude γ-undecalactone, distillation and recovery The reaction solvent is then purified by rectification to prepare γ-undecalactone. During this process, the by-products cannot be separated from the reaction system in time, resulting in a decrease in reaction yield, prolonged reaction time, and the product contains low boiling point Greasy smell of impurities, high boiling point impurities and bad smell of isomers, which affect the aroma quality of the final product of γ-undecalactone

Method used

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  • Production method of synthesizing gamma-undecalactone synthetic perfume by reactive distillation
  • Production method of synthesizing gamma-undecalactone synthetic perfume by reactive distillation

Examples

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Effect test

Embodiment 1

[0047] A production method for synthesizing gamma-undecalactone by reactive distillation, comprising the following steps:

[0048] (a) from octanol head tank, acrylic acid head tank and di-tert-butyl peroxide head tank respectively, utilize high-level pressure difference, discharge through pipeline, octanol 1500kg, acrylic acid 750kg and di-tert-butyl peroxide Add 150kg of material into the batching pot and mix evenly to obtain the batching mixture;

[0049] (b) Utilizing the high-level pressure difference from the octanol head tank, discharging 4500kg of octanol into the preheater through the pipeline, and the temperature of the preheater is raised to 100-180°C;

[0050] (c) Push the octanol in the preheater into the high boiling point feed section of the reaction zone of the reactive distillation tower through the material pump, and push the ingredient mixture in step (a) into the reactive distillation tower through the dripping pump The low-boiling point feed section of th...

Embodiment 2

[0060] The present embodiment produces γ-undecalactone synthetic perfume according to the method of Example 1, and the difference is that in step (a), the addition of each material is: octanol 1590kg, di-tert-butyl peroxide 162kg, Acrylic acid 800kg;

[0061] In step (b), the addition of octanol is 4337kg; All the other method steps are consistent with the implementation method in Example 1.

[0062] In the present embodiment, 238 kg of by-product tert-butanol and water are separated from the top of the rectifying section of the reactive distillation tower; 1393 kg of crude product γ-undecalactone is separated from the bottom of the reactive distillation tower;

[0063] Collect low-boiling point impurities, by-product 2-nonanone 35kg and residual octanol 106kg that do not participate in the reaction;

[0064] After collecting 15 kg of by-product octyl acrylate, γ-undecalactone was collected to obtain 1227 kg of γ-undecalactone product.

Embodiment 3

[0066] The present embodiment produces γ-undecalactone synthetic perfume according to the method of Example 1, and the difference is that in step (a), the addition of each material is: octanol 1887kg, di-tert-butyl peroxide 235kg, Acrylic acid 580kg;

[0067] In step (b), the addition of octanol is 5240g; All the other method steps are consistent with the implementation method in Example 1.

[0068] In the present embodiment, 306 kg of by-product tert-butanol and water are separated from the top of the rectifying section of the reactive distillation tower; 1049 kg of γ-undecalactone crude product is separated from the bottom of the reactive distillation tower;

[0069] Collect low-boiling point impurities, by-product 2-nonanone 24kg and residual octanol 117kg that do not participate in the reaction;

[0070] After collecting 11 kg of by-product octyl acrylate, γ-undecalactone was collected to obtain 890 kg of γ-undecalactone product.

[0071] The GC conditions for product de...

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Abstract

The invention belongs to the technical field of fine chemical production, and specifically relates to a production method of synthesizing gamma-undecalactone synthetic perfume by reactive distillation. The method includes the following steps: (a) mixing raw materials to obtain a mixture of ingredients; (b) discharging materials from an octanol elevated tank into a preheater for preheating; (c) pumping octanol into a high-boiling-point feed section of a reaction zone of a reactive distillation column, and pumping the mixture of ingredients into a low-boiling-point feed section of the reaction zone of the reactive distillation column; (d) separating out a crude product of gamma-undecalactone from the bottom of the reactive distillation column; (e) transferring the octanol separated in the step (d) to the preheater through a material pump to continue to participate in the reaction; and (f) further separating and purifying the crude product of gamma-undecalactone separated in the step (d).According to the production method provided by the present invention, a reactive distillation technology is adopted to timely separate by-product water, tert-butanol and low-boiling-point impuritiesproduced by a side reaction from the reaction system, so as to shorten the reaction time, improve the reaction speed and enhance the reaction efficiency.

Description

technical field [0001] The invention belongs to the technical field of fine chemical production, and in particular relates to a production 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 th...

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