Method for manufacturing carvacrol by carvone composite foot oil

A technology of carvone and carvacrol, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as waste, impurities, increased energy consumption, etc.

Active Publication Date: 2013-04-24
HUAIAN WAN BANG SPICE IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the production process of carvone, a large amount of synthetic foot oil will be produced after aeration and neutralization of the wastewater in each process, in which the content of carvone is about 30%. It is also difficult to purify and utilize it, which greatly increases energy consumption and affects the quality of the final product, so it is generally treated as waste, which not only causes waste, but also brings serious environmental protection problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In the state of stirring, put 187.5kg of water and 125kg of sodium bisulfite into the reaction kettle, mix it into a sodium bisulfite solution with a concentration of 40%, stir, heat up to 70°C, and drop 500kg of carvone containing 30% Synthetic foot oil, control the temperature at 70°C to 80°C during the dropping process, keep the temperature at 70°C to 80°C after the dripping is completed, take samples for analysis every 1 hour, and end when the content of carvone in the organic phase is lower than 0.5% reaction. Add 300kg of water to dilute, dissolve, let stand, remove the organic phase, and extract the water phase with toluene twice to obtain about 730kg of sodium α-hydroxysulfonate solution.

[0026] Add 160 kg of 30% sodium hydroxide solution into the above-mentioned α-hydroxysulfonate sodium solution, stir, heat up and reflux for 2 hours, cool down, neutralize to neutral with 40% sulfuric acid solution, let stand, and divide to remove water phase, about 145kg of...

Embodiment 2

[0030] Under the state of stirring, put 156kg of water and 104kg of sodium bisulfite into the reaction kettle, mix it into a sodium bisulfite solution with a mass concentration of 40%, stir, heat up to 70°C, and add 500kg of carvone containing 30% dropwise. Synthetic foot oil, control the temperature at 70°C to 80°C during the dropping process, keep the temperature at 70°C to 80°C after the dripping is completed, take samples for analysis every 1 hour, and end when the content of carvone in the organic phase is lower than 0.5% reaction. Add 300kg of water to dilute, dissolve, let stand, separate the organic phase, and extract the water phase with toluene twice to obtain about 725kg of α-hydroxysulfonate sodium solution.

[0031] Add 135 kg of 30% sodium hydroxide solution to the above-mentioned α-hydroxysulfonate sodium solution, stir, heat up and reflux for 2 hours, cool down, neutralize to neutral with 40% sulfuric acid solution, stand still, and divide to remove water phas...

Embodiment 3

[0035] In the stirring state, put 171.6kg of water and 114.4kg of sodium bisulfite into the reaction kettle, mix it into a sodium bisulfite solution with a concentration of 40%, stir, raise the temperature to 70°C, and add dropwise 500kg of 30% carvone Synthetic foot oil, the temperature is controlled at 70°C to 80°C during the dropping process, and the temperature is kept at 70°C to 80°C after the dripping, and the sample is analyzed every 1 hour. When the content of carvone in the organic phase is lower than 0.5% End the reaction. Add 300kg of water to dilute, dissolve, let stand, separate the organic phase, and extract the water phase with toluene twice to obtain about 727kg of α-hydroxysulfonate sodium solution.

[0036] Add 147kg of 30% sodium hydroxide solution to the above-mentioned α-hydroxysulfonate solution, stir, heat up and reflux for 2 hours, cool down, neutralize to neutral with 40% sulfuric acid solution, let stand, and divide to remove water phase, about 143kg...

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Abstract

The invention discloses a method for manufacturing carvacrol by carvone composite foot oil. The method comprises the steps of enabling sodium hydrogen sulfite and carvone of the composite foot oil to be subjected to an additive reaction, generating water-soluble alpha-hydroxy sodium sulfonate, separating insoluble organic impurities, then heating the alpha-hydroxy sodium sulfonate together with alkali, hydrolyzing the alpha-hydroxy sodium sulfonate and the alkali to be the carvone, isomerizing and rectifying the carvone, and obtaining the carvacrol. The alkali is sodium hydroxide. The method for manufacturing the carvacrol by the carvone composite foot oil has the advantages of being temperate in reaction condition, convenient to operate and prone to industrialization. Waste water generated in various steps of the reaction is neutral. A sulfuric acid solution can be repeatedly used. A recovery rate of the carvone of the composite foot oil is more than 80 percent. The manufactured carvacrol is more than 9.5 percent in content and product quality indexes are higher than the perfume grade standard.

Description

technical field [0001] The invention relates to a method for preparing another fragrance compound from a fragrance compound waste, in particular to a method for preparing carvacrol by a chemical method of synthesizing foot oil with carvone. Background technique [0002] Carvacrol (English name: Carvacrol) is a colorless to pale yellow viscous liquid with the molecular formula C 10 h 12 O, molecular weight 150.22, melting point 1oC, boiling point 236oC, insoluble in water, soluble in organic solvents such as ethanol. [0003] Carvacrol has herbal, spicy, cool, smoky, camphor, tobacco aroma and smoky, spicy, herbal, woody, phenolic taste. It has strong bactericidal properties and is widely used in food flavors, food additives, antioxidants, preservatives, etc. It is often used in toothpaste, mouthwash and medicinal cosmetics. It is a spice with broad market prospects. [0004] In the production process of carvone, a large amount of synthetic foot oil will be produced af...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/06C07C37/07
Inventor 陈文抗
Owner HUAIAN WAN BANG SPICE IND CO LTD
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