KR101982735B1 - Manufacturing Method of Hydrosol - Google Patents

Abstract

The present invention can improve atmospheric pressure operation, distillation rate and production yield by using high boiling point polyol mixed liquid type high-speed steam distillation when producing aromatic hydrozols from medicinal crops such as cloves, mulberry leaves, papaya leaves, And a method for producing aromatic hydrozols using medicinal crops.

Description

{Manufacturing Method of Hydrosol}

The present invention relates to a process for preparing aromatic hydrogens from medicinal crops such as herbal extracts, horseradish, horsetail, clove, mulberry leaf, wisteria and the like, and more particularly to a process for producing aromatic hydrozols from high- And a method for producing aromatic hydrozols using medicinal crops, which can improve production efficiency such as simplification of process, shortening of operation time, operation cost and production cost by improving production yield.

As is well known, hydrosol is a term derived from Latin hydro , which means water, and sol , which is also referred to as directional distilled water or hydrozoal water. These hydrosols are obtained in the process of producing essential oils or in the process of distilling plants to obtain pure hydrogens. Steam distillation of plants results in the production of oil, the essential oil, and the hydrosol, a water component, which contains low levels of essential oils. Hydrosol is a water with aromatherapy value that can be used without difficulty in using high concentration of aroma oil or irritating to sensitive skin or infant. In addition, the hydrosol has antiseptic and germicidal effect, it regulates the pH of the skin, gives moisturizing effect to the skin, acts to prevent skin diseases and allergic reactions, and is used as a main ingredient of natural cosmetics.
Such a hydrosol is produced by distilling water vapor and refining the essential oil. Generally, it is divided into a water distillation method, a water-steam distillation method, and a steam distillation method. The water distillation method is a method of separating water and oil after cooling the water vapor and essential oil by heating the crude oil in water and heating it. Since the raw material is immersed in boiling water, it does not come into direct contact with water vapor. Orange flowers and roses that are massive are suitable. The water-steam distillation method is a method in which a crude oil is poured into a water vapor in a layer on a grid installed in a distillation section, and the water is heated from below to distill water vapor passing through the sample and a volatile essential oil component separated into water vapor. The steam distillation method is the most common method of oil extraction, in which a raw material is placed in a distillation kiln and steam is blown from the bottom to collect the rectification, which is a distillation method requiring low boiling point. In addition, since the steam distillation method extracts the essential oil with water vapor (water), it has little toxicity and is safe for application to the skin. In addition, it can extract the essential oil and obtain a hydrosol having aromatherapy effect.
Meanwhile, in the water distillation method or the steam distillation method, in order to improve the production rate and yield in the production process, a method of generating superheated water vapor by increasing the heat capacity of water under pressure at the time of generating steam is applied. However, It is necessary to construct the hydrosol. Therefore, the production cost of the hydrosol is increased.
Another method for improving the production rate and yield of the hydrosol is to increase the evaporation rate by lowering the water vapor pressure of the water under reduced pressure. However, since the process operation is performed at a low temperature, the extraction yield of the raw material can be reduced And the volatile organic compounds contained in the condensed water are very low because the volatile organic compounds and the like are discharged through the reduced pressure pump line in the condensation unit process.
In order to solve the problems of these processes, it is necessary to improve the evaporation rate of water in a temperature range in which the extraction yield of the raw material is not inhibited or can be improved under atmospheric pressure operating conditions.

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No. 10-2015-0023825 (Title of the invention: distillation apparatus for extracting essential oils and hydrogens from plant components in capsules Published date: March 05, 2015) Open No. 10-2005-0081564 (Title of the invention: Acne cosmetic composition containing natural fragrance and hydrosol. Published date: Aug. 19, 2005) Open Publication No. 10-2016-0034707 (Title of the Invention: Body oil composition having an aromatherapy effect containing natural essential oil and natural hydrazole Disclosure date: Mar. 30, 2016)

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It is an object of the present invention to provide a method for producing high quality aromatic hydrogens in a medicinal substance by using high boiling point polyol mixed liquid type high-speed steam distillation.
Another object of the present invention is to provide a method for producing aromatic hydrogens by using medicinal crops capable of improving atmospheric pressure operation, distillation rate and production yield when producing hydrogels.
It is another object of the present invention to provide a method for producing aromatic hydrogels using medicinal crops which can increase production efficiency such as simplification of production process, shortening of operation time, operation cost, and production cost reduction.

The present invention is directed to a method for producing a directional hydrazole from a medicinal crop using a polyol mixture liquid water vapor distillation. Preferably, the polyol mixture liquid has a boiling point polyol having a boiling point higher than that of water, Characterized in that any one polyol selected from the group consisting of mono or polyhydric alcohols, {ethylene glycol, propylene glycol, butylene glycol, tetramethylene glycol, glycerin} is used.
Further, it is preferable that the polyol mixture is blended in an amount of about 10 to 80% by weight when the polyol mixture is prepared, and the polyol mixture-type steam distillation is maintained at a temperature in the range of 120 to 150 ° C .

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Disclosure of the Invention The present invention has been made in view of the phenomenon of lowering the extraction yield of raw materials generated in a process of producing a hydrosol by a water distillation method, a steam distillation method, a vacuum distillation method, a pressure distillation method, It is possible to prevent the concentration of the volatile organic compound in the sol from being reduced. In addition, the present invention has the effect of solving the problems such as severe product (hydro-sol) quality deterioration and additional facility requirement of the rectification process due to the above advantages.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a view sequentially showing a method for producing a directional hydrosol using a medicinal plant according to a preferred embodiment of the present invention. FIG.

Hereinafter, embodiments of the present invention will be described with reference to the accompanying drawings. In the following detailed description, one exemplary embodiment of the present invention will be described in order to accomplish the above-mentioned technical problems. And other embodiments which may be presented by the present invention are replaced by descriptions in the constitution of the present invention.
The term " medicinal crop " used in the present invention refers to a plant that is used as a medicine or a raw material for a medicine and generally refers to a medicinal plant, and preferably a medicinal plant such as a herb, It refers to plants such as Angelica gigas, Myrrh, Dermis, Seokjangpo, Bokshin, Omija, Sanjoin, Fermentation, Brain, and Origin.
In the present invention, it is possible to improve the atmospheric pressure operation, the distillation rate and the production yield by using the high-boiling point polyol mixed liquid type high-speed steam distillation when producing aromatic hydrozols from medicinal crops such as cloves, horseradish, The present invention is directed to a method for producing aromatic hydrogens using medicinal crops.
The present invention also relates to a method for preparing aromatic hydrozols by using a medicinal crop which can significantly increase the evaporation rate of water compared with the conventional water distillation method or steam distillation method by raising the phase equilibrium temperature of the polyol functional solution using a high boiling point polyol present.
Since the present invention can inhibit the micro-liquid droplet entrainment of water, impurities in the condensed water (hydrosol) generated in the condensation step of the evaporation water when the hydrosol is produced by the conventional water distillation method or steam distillation method, And a method of manufacturing a directional hydrosol using medicinal crops capable of solving the problems of product quality deterioration such as additional concentration of condensation water and concentration of condensation water and increase of process facility cost.
Particularly, in the present invention, a high boiling polyol is used in producing a directional hydrosol from a medicinal crop, wherein the polyol is a polyhydric alcohol, that is, an aliphatic compound having two or more hydroxyl groups (-OH) Diethylene glycol, diethylene glycol, dipropylene glycol, polyethylene glycol, etc., in which ethylene glycol or propylene glycol is etherified, and the like. In addition, glycerol is representative with three hydroxyl groups, and pentaerythritol, which has four hydroxyl groups.
In the present invention, the polyol having a high boiling point as shown in Table 1 below is used.

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The A common name Boiling point (℃) C ₂ H ₆ O ₂ Ethylene glycol 197.85 C ₃ H ₈ O ₂ Propylene glycol 188.2 C ₄ H ₁₀ O ₂ Butylene glycol 207.4 C ₄ H ₁₀ O ₂ Tetramethylene glycol 229.1 C ₃ H ₅ (OH) ₃ glycerin 290
As described above, in the present invention, when extracting a hydrosol from a medicinal crop, the high boiling point polyol shown in Table 1 is blended with water and then used as water vapor distillation (i.e., high boiling point polyol mixed water vapor distillation) Features can be implemented.
That is, the properties of the polyol solution having a relatively high boiling point form an azeotrope depending on the mixing ratio of the polyol and water, and the phase equilibrium temperature at the azeotropic composition is greatly increased compared with the normal phase equilibrium temperature of the water. As a result, Therefore, it is possible to generate superheated water vapor at 120 ° C or more even at normal pressure. In addition, since the heat capacity of the superheated steam can be increased by increasing the polyol composition having a high boiling point, the extraction yield of the raw material can be increased, and the amount and rate of steam generation can also be increased. On the other hand, since all the operations are carried out at normal pressure, high-pressure equipment is not required, and entrainment of fine water particles can be suppressed, so that impurities can be prevented from being mixed in the condensed water (i.e., the hydrosol) It is commercially economical because additional operation of the rectification facility required for separation and concentration is not necessary.

Hereinafter, the present invention will be described in detail with reference to the preferred embodiments of the present invention, but the present invention is not limited thereto.

{Example 1}
FIG. 1 is a view showing a process for preparing a directional hydrosol from a medicinal crop using high-boiling point polyol mixed liquid type high-speed steam distillation according to a preferred embodiment of the present invention. Hereinafter, the process for preparing the hydrozole according to the present invention will be described in detail.

1. Raw material preparation step
1: 1: 1: 1: 1: 1: 1: 1: 1: 1: 1: 1: 1, 1, and 100 g of the powder was prepared.
At this time, when the medicinal crop has a specific blending range, the mixing ratio of the medicinal crop may be determined depending on the content and composition ratio of the target material according to the medicinal crop. In the case of a conventional blending range, blending ratios can be determined by 1: 1, 1: 1: 1, 1: 1: 1: 1, etc. depending on the number of mixed medicinal plants.

2. Polyol functional solution preparation step
The step of preparing the polyol solution is a step of preparing a polyol solution by adding a polyol solution to purified water, wherein 200 g of the glycerin shown in Table 1 and 800 g of water are mixed as the polyol solution to prepare 1,000 g of a polyol solution .
As described above, the polyol solution may be a single or complex polyhydric alcohol having two or more hydroxyl groups, and it is particularly preferable to use a high boiling polyol having a boiling point higher than that of water.
When the polyol solution is less than 10% by weight, the phase equilibrium rising period of the solution is low depending on the ratio of the azeotropic mixed composition, so that the distillation rate If the amount is more than 80% by weight, the phase shift of the solution due to the azeotropic mixture composition ratio is high, so that the production of carbide and the production of acidic volatile organic compounds during the extraction of the raw material are increased, There is a problem that quality can be deteriorated.

3. Distillation and equilibrium rate maintenance of the polyol solution
The distillation and equilibrium rate maintenance step of the polyol function solution is a step of generating superheated water vapor from the polyol function solution and maintaining the evaporation equilibrium speed. Specifically, the raw material prepared in the above step 1 is filled in a usual extraction vessel, The polyol functional solution is filled in an evaporation vessel and heated to maintain the equilibrium rate.
At this time, in the present invention, the phase equilibrium temperature was measured in the heating process, and the evaporation temperature was 140 ° C. In order to maintain the evaporation equilibrium velocity of water vapor, the evaporation rate was converted into the discharge flow rate of water using a wet gas meter, Purified water was added to the evaporation tank. The makeup water flow rate is 10 ml / min,
Meanwhile, in the present invention, the heating temperature of the superheated steam is maintained at 140 ° C., and the heating temperature range of the superheated steam can be set within the range of 120 to 150 ° C. If the heating temperature of the steam is less than 120 ° C, the extraction yield and extraction rate of the raw material are low, which is not in accordance with the object of the present invention. If the heating temperature is more than 150 ° C, And the amount of the acidic volatile organic compound to be produced increases, thereby deteriorating the quality of the hydrosol.
In addition, in the equilibrium rate maintenance step, the replenishment water flow rate of the evaporation tank should be equal to the discharge flow rate, because when the flow rate of the replenishing water is less than the discharge flow rate, the generation rate and flow rate of the superheated steam are increased but the temperature of superheated steam is increased If the discharge flow rate is exceeded, the generation rate and flow rate of the superheated steam may be decreased and the temperature of the superheated steam may be lowered, which may cause problems in the final production yield and quality standardization.

4. Steam extraction stage of medicinal crops
The step of extracting steam of medicinal crops is a step of extracting medicinal crops by superheated water vapor, and the superheated steam at 140 ° C evaporated in the evaporation tank is transferred to the absorption tower through the extraction tank.
At this time, the extraction step maintains the same condition as the critical meaning of step 3 described above, and the discharge flow rate is also set to be the same.

5. Removal of microscopic droplets
In order to prevent impurities from being mixed in the condensed water (that is, the hydrosol) due to the entrainment of the fine water particles generated during steam distillation, the absorption tower having the dehydrating agent filled in the upper part of the evaporation tower is installed Thereby removing fine water particles in the water vapor.
As the dehydrating agent which can be filled in the absorption tower, sodium sulfate anhydrous, calcium chloride, sodium bicarbonate, ammonium chloride or the like may be used, and in addition, a solid fill material which can be used for general dehydration or absorption purposes may be used.

6. Hydrosol condensation step
The hydrosol condensation step is a step of condensing the evaporated water flowing into the condenser through the absorption tower and storing it in the recovery tank, and the recovered flow rate is 9.8 ml / min per unit time.
At this time, it is preferable to set the range of the condensation temperature within the range of 4 to 70 ° C. If the condensation temperature is lower than 4 ° C, hydrated crystals are formed to form a hydrate to suspend the hydrosol, When the temperature exceeds 70 ° C, the condensation rate of the superheated water vapor is slowed, so that the overheat steam may flow into the heat exchanger to cause overload, thereby reducing the productivity of the hydroazole and decreasing the concentration of the volatile organic compounds can do.

7. Step for measuring the yield of the hydrosol
The hydrogel yield measurement step is a step of recovering the hydrosol prepared in the above-mentioned step.
At this time, the concentration of the recovered hydrosol is determined by multiplying the flow rate of the evaporated water to the amount of raw material times the recovery time. In the present invention, 588 ml of the hydrosol can be produced by operating for 1 hour.

{Comparative Example 2}
In the following comparative example, a method of producing a directional hydrosol using steam distillation from a medicinal crop is proposed.
1. Raw material preparation step
1: 1: 1: 1: 1: 1 ratio of cloves, cloves, mung bean leaves, herbaceous leaves, do.

2. Steam distillation step
In the steam distillation step, the raw material prepared in the step 1 was filled in an extraction vessel, and 1,000 g of purified water was filled in an evaporation vessel and heated to measure the phase equilibrium temperature. The evaporation temperature at this time was 100 ° C, The evaporation rate was converted into the discharge flow rate of water using a wet gas meter, and the evaporation flow rate at this time was 4 ml / min.

3. Steam extraction step of medicinal crops
In the water vapor extraction step of medicinal crops, steam at 100 ℃, which is evaporated in the evaporation tank, is transported to the absorption tower through the extraction tank.

4. Removal of microscopic droplets
In order to prevent impurities from entering into the condensed water due to entrainment of fine water particles generated during steam distillation, the absorption tower filled with dehydrating agent is installed in the upper part of the evaporation tower to remove minute water particles Respectively.

5. Evaporation Water Condensation Step
In the evaporation water condensation stage, the evaporated water flowing into the condenser through the tower tower is condensed and transferred to the recovery tank, and the recovered flow rate per unit time is 2.4 ml / min.

6. Measurement of the yield of the hydrosol
The concentration of the hydrosol was determined by multiplying the flow rate of the evaporated water to the feed amount by the recovery period. In this comparative example, 144 ml of a hydrosol It was able to produce.

As shown in the above Examples and Comparative Examples, when a hydrazole was prepared from a medicinal crop by using a polyol mixed liquid type high-speed steam distillation, about 588 ml of a hydrosol could be produced, and a conventional steam distillation To produce about 144 ml of the hydrosol.

As described above, it can be confirmed that the productivity of the hydrosol is improved by about four times as compared with the conventional one when the high boiling point polyol mixed liquid type high-speed steam distillation is used.

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Claims (6)

A method for producing a hydrosol from a medicinal crop,
Mixing a high boiling point polyol having a boiling point higher than that of water with water to prepare a polyol water solution;
Filling the medicinal crop into an extraction tank, filling the evaporation tank with 10 to 80% by weight of the polyol hydrate solution, and maintaining the equilibrium rate while heating it; Setting a heating temperature range of the superheated steam to 120 to 150 DEG C and making the replenishment water flow rate and the drain water flow rate of the evaporation tank equal to maintain the equilibrium speed;
Extracting water vapor of the medicinal crop while the superheated water vapor evaporated in the evaporation tank is transferred to the absorption tower through the extraction tank;
The absorption tower filled with dehydrating agent is installed to prevent impurities from being mixed in the condensed water due to entrainment of fine water particles generated during steam distillation of the medicinal crop;
Condensing the evaporated water flowing into the condenser through the absorption tower and storing the condensed water in a recovery tank; And setting the range of the condensation temperature to 4 to 70 占 폚.
The method according to claim 1,
Wherein the polyol hydrate solution is prepared by mixing water with any one of polyols selected from ethylene glycol, propylene glycol, butylene glycol, tetramethylene glycol, and glycerin, and water to prepare a directional hydrosol . delete delete delete delete

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