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

A technology for the synthesis of gamma-decalactone and fragrances, which is applied in sustainable manufacturing/processing, chemical industry, climate sustainability, etc. It can solve problems such as poor fuel consumption, decreased reaction yield, and prolonged reaction time, so as to save energy Effects of energy consumption, reduction of reaction time, and improvement of reaction speed

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

Using n-heptanol and acrylic acid as the starting materials, di-tert-butyl peroxide as the initiator, adding the reaction solvent, first using the "one-pot cooking" method, the free radical addition synthesis of crude gamma-decalactone, distillation recovery reaction Solvent, and then prepare gamma-decalactone by rectification and purification. In 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 impurities. Greasy odor, high boiling point impurities and fuel consumption bad smell of isomers, thereby affecting the final product aroma quality of gamma-decalactone

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0045] A kind of production method of reactive distillation synthesis gamma-decalactone synthesis fragrance, comprises the following steps:

[0046] a) From the heptanol head tank, methyl acrylate head tank and di-tert-butyl peroxide head tank respectively, using the high pressure difference, through the pipeline discharge, 1200kg of heptanol, 860kg of methyl acrylate and di-tert-butyl 140kg of base peroxide is added to the batching pot according to the batching ratio, and 15kg of sodium borohydride is added into the batching pot according to the batching ratio from the feeding port of the batching pot, and mixed evenly.

[0047] b) Use the high pressure difference from the heptanol head tank to discharge 3200kg heptanol into the preheater through the pipeline, and the preheater is heated to 150-180°C.

[0048] c) Put the heptanol in the preheater into the high-boiling point feed section of the reaction zone of the reactive distillation column through the material pump, and in...

Embodiment 2

[0057] The present embodiment produces gamma-decalactone synthetic perfume according to the method of Example 1. The difference is that in step (a), the addition of each material is: heptanol 1485kg, di-tert-butyl peroxide 85kg, boron Sodium hydride 8.5kg, methyl acrylate 1000kg;

[0058] In step (b), feed heptanol 4049kg;

[0059] All the other remain unchanged, and the gamma-decalactone product is prepared;

[0060] In the present embodiment, 288 kg of by-product tert-butanol and methanol are separated from the top of the rectifying section of the reactive distillation tower; 1339 kg of crude product of gamma decanolide is separated from the bottom of the reactive distillation tower;

[0061] Add water 670kg for washing;

[0062] Collect low-boiling impurities, by-product 2-octanone 27kg and residual heptanol 106kg that do not participate in the reaction;

[0063] After collecting the by-product heptyl acrylate 13kg, collect the gamma-position decanolactone, obtain the ga...

Embodiment 3

[0065] The present embodiment produces gamma-decalactone synthetic perfume according to the method of Example 1. The difference is that in step (a), the addition of each material is: heptanol 1822kg, di-tert-butyl peroxide 255kg, boron Sodium hydride 64kg, methyl acrylate 750kg;

[0066] In step (b), feed heptanol 5062kg;

[0067] All the other remain unchanged, and the gamma-decalactone product is prepared;

[0068] In the present embodiment, 392 kg of by-product tert-butanol and methyl alcohol are separated from the top of the rectifying section of the reactive distillation tower; 937 kg of the crude product of gamma-decalactone are separated from the bottom of the reactive distillation tower;

[0069] Add water 1405kg for washing;

[0070] Collect low-boiling point impurities, by-product 2-octanone 19kg and residual unreacted heptanol 88kg;

[0071] After collecting the by-product heptyl acrylate 10kg, collect the gamma decanolactone to obtain 816 kg of the gamma decanol...

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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-decalactone synthetic perfume by reactive distillation.The method includes the following steps: (a) mixing materials through pipelines to obtain a mixture of ingredients; (b) discharging materials from a heptanol elevated tank into a preheater for preheating; (c) pumping heptanol 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-decalactone; (e) transferring the separated heptanol 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-decalactone. According to the production method provided by the present invention, the reactionis carried out in two directions through promoting the separation by the reaction and promoting the reaction by the separation, the reaction time is shortened, the reaction speed is improved, the reaction efficiency is improved, the energy is saved by using reaction heat, and equipment investment is saved.

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-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 p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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