KR20190070128A - How to remove odor from the retinispora extract - Google Patents

Abstract

The present invention relates to a method for removing off-flavor from a retinispora essential oil extract to remove various off-flavor contained in essential oil, which is an extract extracted from retinispora, in a short time through heat treatment and ultrasonic treatment. The method comprises the steps of: a) extracting the retinispora essential oil from the retinispora; b) heating the retinispora essential oil of the step a) at the temperature of 60 to 100°C for 1 to 10 hours; and c) sonicating the heated retinispora essential oil of the step b) at the intensity of 10 to 300 W at 10 to 50 kHz.

Description

A method for removing odor from an extract of an essential oil of Timberwort

The present invention relates to a method for removing odor from a crude oil extracted from unshiu wood, and more particularly, to a method for removing various odor contained in an oil extracted from an unshiu tree by a heat treatment and an ultrasonic treatment in a short time, And a method for removing odor.

Retinispora is an evergreen tree of the Japanese origin, and it is also called asai, hinoki, cypress. The height is about 30 - 40m and the width is about 1-2m, the bark is reddish brown, and the small scaly leaves are densely grown on branches. Small flowers bloom on branches in spring, and green cones ripen in red in October. The cones are about 1 cm in diameter and consist of 7 to 9 shield-shaped scales. Leaves and wood contain about 1% essential oil and are mainly used for medicinal purposes.

Especially, it is known that the waxy tree has an excellent effect for eliminating harmful substances in the air such as formaldehyde and also for preventing the atopy and allergy as well as the antibacterial effect and the immune function increasing effect. This is due to the essential oil component contained in the leaves and timber of the unicorn tree, and the substance having the highest volatility and the greatest antimicrobial activity among the essential oil components contained in the unicorn tree is called 'phytoncide'.

Phytoncide is a natural antimicrobial substance in which trees excrete in the air to protect themselves from pests and microorganisms. It is a synonym for Greek, which means "phyton" and "cide", and collectively refers to the bactericidal substance that plants excrete. The major component of phytoncide is mainly composed of volatile terpenes, and contains many ingredients other than fragrance.

It is also known that phytoncide makes a sense of comfort, which is effective in stabilizing autonomic nerves by the effects of forest bathing, improving liver function or inducing sleep. Phytoncide also has a deodorizing / deodorizing function. When you enter the forest, you can feel the fresh air even though there are carcasses, rotten trees and plants that cause bad smell. The forest itself is made of phytoncide, And odor removal function. Such deodorizing and deodorizing action is also effective for taking a human life. In addition, phytoncide functions as an antimicrobial / insecticide. It can also be used for the preservation and sterilization of foods, fungicides in rooms and baths, insects such as mites, and also for pathogens harmful to human body due to its antibacterial action.

Therefore, in order to utilize the above-mentioned various effects, an attempt has been made to extract an extract containing phytoncide components from cottonwood and commercialize them.

However, in the process of extracting or processing the essential oil of the unicorn tree, due to the problems related to the essential oil, the essential oil has been exposed to the needs of the modern people, but the limit has been exposed in meeting the well-being demand of the consumers.

Therefore, the essential oil component extracted from the above-mentioned cottonwood contains various odor such as grass odor, burnt odor, and salty odor, so that the pretreatment work must be preceded. In order to remove such odor, it is common to ferment for about 1 month to 3 months or to carry out a process for removing a deodorant separately.

However, since the above-described deodorization method requires a complicated process and a long time, it is almost impossible to use the white oil after the extraction. Therefore, the commercial use is very limited, and the yield of the oil extracted from the white cotton is extremely low .

Korean Patent No. 10-1681258 (Nov. 24, 2016) Korean Patent No. 10-1625985 (May 25, 2015) Korean Patent Publication No. 10-2016-0023385 (Mar.

The present inventors have made intensive studies on a method of removing the odor of essential oil extracted from cottonwood in a short period of time and found that the physical and chemical destruction of the odorous component due to the thermal destruction and the generation of radicals having high reactivity And completed the present invention.

Accordingly, it is an object of the present invention to provide a method for removing odor of an extract of Prunus mulberry tree essential oil, which can remove odor of essential oil in a short time without any process such as fermentation for removing the odor of essential oil extracted from Prunus mume .

According to an aspect of the present invention, there is provided a process for producing a cotton fabric, comprising the steps of: a) extracting a white essential oil from a white cotton; b) heating the white essential oil of step a) at a temperature of 60 to 100 캜 for 1 to 10 hours; And c) sonicating the heated mono-faced essential oil of step b) at 10-50 kHz to an intensity of 10-300 W.

The extracting of the elixir of essential oil in step a) is carried out by any one extraction method selected from a hot water extraction method, a reduced pressure concentrated extraction method, a microwave extraction method, a supercritical extraction method and a continuous steam extraction method.

At this time, the method of extracting the untreated white essential oil using the microwave extraction method comprises the steps of (a) selecting one or two or more parts from the branches, leaves and fruits of the untransformed tree, drying the same, ; (b) irradiating the pulverized product of step (a) with microwaves; (c) mixing the pulverized material irradiated with the microwave in the step (b) and the purified water at a weight ratio of 1: 4.5-5.5 into a distillation tank, supplying steam of high temperature into the distillation tank to extract the extract step; (d) condensing the extract extracted by the high-temperature steam supplied into the distillation tank of step (c); (e) supplying the condensed extract of step (d) to another distillation tank so as to separate the remaining amount of the precipitate and the precipitate; And (f) discharging the separated precipitating solution of step (e) to the outside.

Also, the microwave irradiation dose in the step (b) is 1 to 15 kGy.

The method for removing odor of the extract of unshiu tree essential oil extract of the present invention is characterized in that physical and chemical destruction of the odor component can be achieved in a short time by heating and ultrasonic treatment of the essential oil extracted from the unshiu tree to improve the yield of the essential oil extract, In addition, there is an effect of simplifying a processing step for obtaining an essential oil extract.

FIG. 1 is a flowchart illustrating a method for removing odor and odor from an extract of Prunus mume extract according to a preferred embodiment of the present invention.

The method for removing odor of a crude oil extracted from essential oil of the present invention comprises:

a) extracting the white essential oil from the white plain;

b) heating the white essential oil of step a) at a temperature of 60 to 100 캜 for 1 to 10 hours; And

c) sonicating the heated mono-faced essential oil of step b) at 10-50 kHz to an intensity of 10-300 W.

The step a) is a step for extracting the white essential oil from the white plain tree. First, the white plain tree containing the white essential oil carries the white tree branch between the dormant November and the following February. Leaves are picked from the branches of the bare onion, and scissors, which are usually easy to cut, can be used. The leaves of the perilla trees are connected with small pellets so that they appear to be pelletized with beads.

Next, the collected white leaves are dried to remove impurities such as dust and the like. At this time, it is preferable to dry the unicorn tree leaf in a shady place, in order to prevent destruction of the useful ingredient by ultraviolet rays.

The dried planthopelas leaves can be subjected to a process for extracting the essential oil. According to a preferred embodiment of the present invention, the essential oil contained in the perilla leaf can be extracted through any one extraction method selected from the hydrothermal extraction method, the reduced pressure concentrated extraction method, the microwave extraction method, the supercritical extraction method and the continuous steam extraction method.

Meanwhile, as a preferred embodiment of the present invention, when the essential oil is extracted from the unicorn tree leaves by applying the microwave extraction method, the essential oil extract can be obtained through the following process.

First, any one or two or more of the branches, leaves, and fruits of the unicorn tree, preferably the leaves of the unicorn tree, are washed to remove various impurities, and then dried in a shady place for a certain period of time. When the drying is completed, the leaves of the perilla wood are milled to have a particle size of less than 1 mm so as to facilitate the irradiation of the microwaves to form pulverized material. For reference, the pulverized material may enlarge the surface area of the pulverized material to be irradiated with microwaves, and microwave irradiation may be performed over a wider area as the surface area is wider.

The size of the pulverized product is preferably less than 1 mm since the microwave is not uniformly irradiated when the size of the pulverized product is more than 1 mm. Therefore, it is preferable that the particle size of the pulverized product is less than 1 mm.

Next, the pulverized product is irradiated with microwaves at an irradiation dose of 1 kGy to 15 kGy. The pulverized material exposed to the microwaves changes its molecular structure. Specifically, it includes terpene and cellulose in the white wood containing the unicorn tree leaves, and these materials chemically tightly And is formed as a combined structure.

If the pulverized material is exposed to microwaves in this state, the pulverized material is physically damaged by microwaves, thereby affecting the molecular structure of the pulverized material and the cell walls. The molecular structure change of the pulverized product may include at least one of surface area, porosity, and basification.

Thus, through the above-described process, the chemical bonding structure of the unicellular or perilla leaves can be weakened and the cell wall can be influenced.

Exposure of the microwave may be performed by irradiating 1 kGy to 15 kGy. When the irradiation dose of the microwave is more than 15 kGy, an extract capable of decomposing terpene and cellulose contained in the perilla or perilla leaves and extracting the terpene and cellulose from the cellulase When the molecular weight is less than 1 kGy, molecular structure change and cell wall influence are insignificant.

As described above, the pulverized material exposed to the microwave is mixed with the purified water in a weight ratio of 1: 4.5-5.5, put into the distillation tank, and the steam is supplied into the distillation tank to extract the extract.

The reason for putting the pulverized product and the purified water together in the distillation tank is to increase the chemical reaction area of the pulverized product in powder form. In other words, when the purified water is mixed with the pulverized material having a modified molecular structure exposed to the microwave, the pulverized material absorbs the purified water and swells. This can expand the so-called reaction zone, which can cause a specific chemical reaction in the pulverized material with weak chemical bonding structure.

On the other hand, the water vapor can be maintained at a high temperature by using a heating means, and the heating means can be any one of a burner, an electric furnace, a heater and a boiler. In order to determine the yield of the extract, the irradiation dose of the microwave irradiated to the pulverized product may be adjusted.

Next, the extract extracted by the high-temperature steam supplied into the distillation tank is condensed. Specifically, the extracts moved by the pressure from the distillation tank can be heat-exchanged through a cooler or the like to be condensed.

The condensed extract can be fed to another distillation tank. The condensed extract is supplied to another distillation tank so that the essential component contained in the extract, that is, the sediment liquid and the remainder excluding the sediment is separated.

As described above, high-temperature steam can be supplied in the process of separating the sediment liquid from the remainder. The high-temperature steam is supplied to the distillation tank so that the sediment can be separated at the bottom. By discharging it to the outside, a whitening essential oil can be obtained.

In step b), the white essential oil of step a) is heated at a temperature of 60 to 100 캜 for 1 to 10 hours. At this time, when the above-mentioned mono-block essential oil is heated above 100 ° C, the oil component contained in the mono-block essential oil is destroyed and fails to exhibit its functionality. When heated to below 60 ° C, the deodorant reduction mechanism of the mono-block essential oil does not operate properly.

In addition, when the above-mentioned mono-faced essential oil is heated for more than 10 hours, the oil component contained in the mono-facial essential oil may be destroyed by excessive heating, and when it is heated for less than 1 hour, the ultraviolet radiation efficiency as a subsequent step sharply drops. Therefore, in the step b), the heating temperature of the white essential oil is preferably 60 to 100 ° C and the heating time is preferably 1 to 10 hours.

In the step c), the whitening essential oil is subjected to ultrasonic treatment at a frequency of 10 to 300 W at a frequency of 10 kHz to 50 kHz in order to remove the odor of the whitening essential oil heated in the step b).

The ultrasonic treatment technique for reducing the odor of the essential oil extracted from the white cotton tree according to the present invention will be described. The sound waves are classified into a vibration sound outside the audible frequency of 20 Hz - 20 kHz, an ultrasonic wave below that, and an ultrasonic wave below that. In other words, ultrasound is a sound wave of 20 kHz or more, and the pressure changes rapidly to high pressure and low pressure by mechanical vibration. Repeated high pressure and low pressure generated at this time are called cavitation. Ultrasonic waves using this principle of cavitation are generally used for cleaning, measuring, and medical equipment.

On the other hand, when ultrasonic waves are applied to the monoaxial essential oil, air bubbles are generated at the moment of dropping from a high pressure to a low pressure, and when the air pressure drops to low pressure, air bubbles become large. The odor component is covered. By removing the air bubbles which are generated instantaneously due to the ultrasonic treatment as described above, it is possible to efficiently remove the odorous components of the white essential oil.

More specifically, when ultrasonic waves are treated in a mono-fine oil, micro-bubbles are generated in the essential oil, and a so-called cavitation of high temperature and high pressure is caused by the continuous process of growth and collapse of the micro- Are induced by pyrolysis reaction and radical reaction.

The pyrolysis reaction refers to a pyrolysis reaction of a substance generating odor due to energy generated by breakage of a cavitation bubble during ultrasonic treatment. The reaction by the radicals is performed by ultrasonic treatment at the periphery of the joint bubble and in the oil refinery A radical is generated, and the radical is decomposed by the radical component.

By the ultrasonic treatment of the whitening essential oil containing the component causing the odor by the mechanism as described above, the pyrolysis reaction and the reaction by the radical are promoted, whereby the odor component contained in the whitening essential oil can be removed.

Meanwhile, the ultrasonic treatment of the present invention is preferably performed at 10 kHz to 50 kHz at an intensity of 10 W to 300 W. This is because the cell wall of the monoaxial essential oil is destroyed within the above range, the dissolution of the physiologically active substance is enhanced, and the deodorization efficiency can be maximized.

Hereinafter, the present invention will be described in more detail with reference to Examples and Experimental Examples.

[Example 1]

The essential oil extracted from the untreated white wood was extracted with ordinary hot water extraction method and heated at a temperature of 60 to 100 DEG C for 1 to 7 hours to prepare a heated white essential oil.

[Example 2]

The extracted leaves were extracted from the leaves by using ordinary hot water extraction method. Ultrasonic waves were applied to the extracted extracts at a frequency of 30W to 100W in a safe space to prepare an ultrasonic finishing oil.

[Example 3]

The essential oil was extracted from the leaved trees using ordinary hot water extraction method and then heat-treated at a temperature of 60 ° C to 100 ° C for 1 hour to 7 hours. The heated extracts were treated with ultrasonic waves at a frequency of 30 kHz to 100 W in a safe space, and heat treatment and ultrasonic treatment were provided.

[Experimental Example 1]

The sensory evaluation was carried out with different heating time and heating temperature in order to confirm the odor reducing ability of the white essential oil according to Example 1. Twenty students from Songwon National University were enrolled in this study. Ten students were instructed to use 10 point scale (10 points, average score: 5 points, very weak score: 1 point) Respectively. The evaluation results are shown in Table 1 below.

Heating time Heating temperature (℃) 60 80 100 0 10 10 10 One 9 9 8 3 9 7 7 5 9 7 7 7 8 7 8

[Experimental Example 2]

In order to confirm the odor reduction ability of the whitening essential oil according to Example 2, the sensory evaluation was carried out while varying the ultrasonic treatment time and the temperature during the ultrasonic treatment. Twenty students from Songwon National University were enrolled in this study. Ten students were instructed to use 10 point scale (10 points, average score: 5 points, very weak score: 1 point) Respectively. The evaluation results are shown in Table 2 below.

Ultrasonic processing time Temperature during ultrasonic treatment (℃) 40 60 80 0 9 9 9 One 8 7 7 2 7 6.5 6 3 7 6 6 4 6.5 6 6

[Experimental Example 3]

In order to confirm the off-odor reducing ability of the whitening essential oil according to Example 3, the sensory evaluation was carried out while varying the temperature during the ultrasonic treatment of the whitening essential oil preheated to the ultrasonic treatment time and the temperature of 80 ° C. Twenty students from Songwon National University were enrolled in this study. Ten students were instructed to use 10 point scale (10 points, average score: 5 points, very weak score: 1 point) Respectively. The evaluation results are shown in Table 3 below.

Ultrasonic processing time Preheating (80 ℃) 3 hours + Ultrasonic treatment temperature (℃) 40 60 80 0 6 6 6 One 6.5 5 4 2 5 5 3 3 5 4 3 4 5 4 3

Referring to Tables 1 to 3, it can be confirmed that, in Experiments 1 to 3, as the heating time or the ultrasonic treatment time is increased, the off-odor is reduced. In addition, it can be confirmed that the filtration efficiency is excellent at a heating temperature or an ultrasonic treatment temperature of about 60 to 80 캜.

In particular, it can be confirmed that the heated and ultrasonically treated monoaxial essential oil of Experimental Example 3 is the most excellent in the deodorizing ability, and it can be concluded that the method of removing the odor of the monoaxial essential oil extract according to the present invention is significant.

As described above, according to the present invention, physical and chemical destruction of the odorous components can be performed in a short time by heating and ultrasonic treatment of the essential oil extracted from the waxy tree, thereby improving the yield of the essential oil extract and obtaining the essential oil extract It is a useful invention that can be simplified.

Claims (4)

a) extracting the white essential oil from the white plain;
b) heating the white essential oil of step a) at a temperature of 60 to 100 캜 for 1 to 10 hours; And
and c) ultrasonically treating the heated monoaxial essential oil of step b) at a frequency of 10 to 300 W at a frequency of 10 to 50 kHz. The method according to claim 1,
In the step (a)
Wherein the extract is extracted by any one extraction method selected from hydrothermal extraction method, reduced pressure concentrated extraction method, microwave extraction method, supercritical extraction method and continuous steam extraction method. 3. The method of claim 2,
The method for extracting the elixir of woody plant using the microwave extraction method comprises:
(a) selecting any one or two or more parts of the egg white, leaf, and fruit of the specific grape seed, drying it, and pulverizing it to a particle size of less than 1 mm to form a pulverized product;
(b) irradiating the pulverized product of step (a) with microwaves;
(c) mixing the pulverized material irradiated with the microwave in the step (b) and the purified water at a weight ratio of 1: 4.5-5.5 into a distillation tank, supplying steam of high temperature into the distillation tank to extract the extract step;
(d) condensing the extract extracted by the high-temperature steam supplied into the distillation tank of step (c);
(e) supplying the condensed extract of step (d) to another distillation tank so as to separate the remaining amount of the precipitate and the precipitate; And
(f) discharging the separated precipitating solution of step (e) to the outside. The method of claim 3,
Wherein the microwave irradiation dose in step (b) is 1 to 15 kGy.

Images