CN112745986A - Method and device for extracting essential oil by steam distillation - Google Patents
Method and device for extracting essential oil by steam distillation Download PDFInfo
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- CN112745986A CN112745986A CN202011478882.4A CN202011478882A CN112745986A CN 112745986 A CN112745986 A CN 112745986A CN 202011478882 A CN202011478882 A CN 202011478882A CN 112745986 A CN112745986 A CN 112745986A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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Abstract
The invention belongs to the technical field of essential oil preparation, and relates to a method and a device for extracting essential oil by steam distillation. The device comprises a distillation kettle, a deoiling tower, an oil-water separator, a heat exchanger and a heater, wherein a gas outlet at the top of the distillation kettle is connected with the lower part of the deoiling tower, the bottom of the deoiling tower is connected with the heat exchanger, the heat exchanger is connected with the oil-water separator, a water layer water gap of the oil-water separator is connected with the heat exchanger, the heat exchanger is connected with the heater, and the heater is connected with the top of the deoiling tower. The oily steam enters from the lower part of the deoiling tower and fully contacts with the water layer solution for adsorption and absorption in the rising process, so that the essential oil removing effect is improved. Reduce energy consumption and water consumption.
Description
Technical Field
The invention belongs to the technical field of essential oil preparation, and particularly relates to a method and a device for extracting essential oil by steam distillation.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
The essential oil is volatile aromatic substance extracted from flower, leaf, stem, root or fruit of plant by steam distillation, extrusion, cold soaking or solvent extraction.
Steam distillation techniques are commonly used for extraction of essential oils, and are also common separation techniques for mixtures in the chemical industry. Steam distillation is commonly used in the following specific cases: extracting essential oil from plant leaves and stems, and extracting volatile oil and natural medicines from traditional Chinese medicines. ② recovering benzene compounds in coal tar and petroleum industry. ③ combining steam distillation and solvent extraction (or solid phase adsorption) to measure the trace substances. Fatty acid, edible oil and polyester (high boiling point substance) are deodorized and the acidity is reduced. Separating out a small amount of volatile impurity components from a large amount of organic matters. Sixthly, recovering materials with high boiling point. The distillated material is unstable in its boiling point range or reacts with other components.
The water vapor distillation device is mainly composed of a distillation kettle, a condenser, an oil-water separator, a pipeline and a valve which are connected among the distillation kettle, the condenser and the oil-water separator. The separation principle is as follows: when water and a compound that is not (or is poorly) soluble in water are present together, the vapor pressure of the entire system should be the sum of the vapor pressures of the components, according to the law of partial pressure in daltons.
The steam distillation has the advantages of simple equipment, easy operation, large treatment capacity and the like. However, the traditional steam distillation method has large solid-liquid ratio, long distillation time and large energy consumption, and the oil-soluble essential oil and the water-soluble essential oil are easy to separate out due to mutual insolubility, so that the extraction efficiency is low. The traditional steam distillation method is used for seriously emulsifying condensate distilled from some essential oil, the oil-water separation is difficult, the condensate needs to be kept stand for 2-3 days for oil-water separation, a high-speed centrifuge is used for centrifugal separation after refrigeration or a water layer after oil-water separation is re-steamed sometimes, and due to long-time heating extraction, some heat-sensitive components in the essential oil can be decomposed, so that the quality of the essential oil is adversely affected.
The steam distillation improvement technology has many applications in industry, and related documents and patents are reported. The prior art, as proposed by the new patent "circulating water vapor distillation apparatus" (application No.: 201220420855.6), has the following disadvantages: continuously adding water into a distillation kettle in the system to supplement water consumption, so that the continuous operation of distillation is influenced, and the operation time is prolonged; a large amount of steam condensate water is generated in the distillation process, and organic wastewater is formed due to organic matters; the water temperature of the steam condensate water can still approach 100 ℃, and the steam condensate water contains more heat and cannot be recycled, so that the energy consumption is increased.
Disclosure of Invention
In view of the above problems in the prior art, it is an object of the present invention to provide a method and apparatus for extracting essential oil by steam distillation.
In order to solve the technical problems, the technical scheme of the invention is as follows:
according to the first aspect, the device for extracting the essential oil through steam distillation comprises a distillation kettle, a deoiling tower, an oil-water separator, a heat exchanger and a heater, wherein a gas outlet in the top of the distillation kettle is connected with the lower part of the deoiling tower, the bottom of the deoiling tower is connected with the heat exchanger, the heat exchanger is connected with the oil-water separator, a water layer outlet of the oil-water separator is connected with the heat exchanger, the heat exchanger is connected with the heater, and the heater is connected with the top of the deoiling tower.
The water layer of the oil-water separator contains a small amount of essential oil, the temperature of the water layer is increased after the water layer is heated by the heat exchanger and the heater, the water layer enters the deoiling tower to adsorb the essential oil in the oily vapor, and the separation of the essential oil in the oily vapor is facilitated.
The oily steam enters from the lower part of the deoiling tower and fully contacts with the water layer solution for adsorption and absorption in the rising process, so that the essential oil removing effect is improved.
In some embodiments of the invention, the top of the deoiler is connected to the still. The steam obtained from the top of the deoiling tower returns to the distillation still, the temperature of the steam is higher, and the steam can be repeatedly used for extracting the plant essential oil after returning to the distillation still.
In some embodiments of the invention, the oil-water separator is connected to the heat exchanger by a circulation pump.
In some embodiments of the invention, the distillation still is connected to the deoiling tower through a steam exhaust fan.
In a second aspect, a method for extracting essential oil by steam distillation comprises the following specific steps:
putting the plants into a distillation kettle, introducing steam into the distillation kettle to obtain oil-containing steam, and discharging the oil-containing steam from the distillation kettle into a deoiling tower;
absorbing the oily water vapor in a deoiling tower to obtain an oily solution and water vapor, discharging the water vapor from the top of the deoiling tower, discharging the oily solution from the bottom of the deoiling tower, and allowing the oily solution to enter an oil-water separator for separation to obtain essential oil and a water layer solution;
and heating the water layer solution, and then feeding the water layer solution into a deoiling tower for adsorption deoiling of oil-containing water vapor.
And introducing the water layer solution obtained in the oil-water separator into a deoiling tower to separate essential oil from the oil-containing water vapor. Separating essential oil and water vapor from water vapor, dissolving essential oil in water layer solution, and discharging water vapor from the top of the deoiling tower. This achieves the reuse of the aqueous layer solution.
The temperature of the water layer solution is lower when the water layer solution is discharged from the oil-water separator, the temperature of the water layer solution is raised through heat exchange and heating, and the effect of adsorbing essential oil is improved after the temperature reaches higher temperature.
The method for removing essential oil by using oil-containing water vapor in the prior art comprises the following steps: condensing the oil-containing water vapor, and then separating to obtain the essential oil. However, the standing separation takes a long time and the separation is not complete, and further centrifugation or re-distillation are required. And the water layer obtained by standing and separating needs to be heated again to form water vapor if the water layer is used for extracting essential oil, so that the energy consumption is increased. Therefore, the method does not need the operation step of condensing the oil-containing water vapor, and realizes the effect of saving energy.
In some embodiments of the invention, packing is provided in the deoiling tower, and the packing is stainless steel theta-mesh ring packing.
Furthermore, the height of the packing section is 1-1.5 m, the distance from the top of the packing section to the top of the deoiling tower is 0.1-0.3 m, and the distance from the bottom of the packing section to the bottom of the deoiling tower is 0.6-1.0 m.
The oil removing tower is internally provided with a filler, oil-containing steam enters the oil removing tower, and essential oil is separated through the adsorption effect. The oil-containing vapor contains oil-soluble essential oil and water-soluble essential oil, the oil-soluble essential oil is immiscible with water and is easy to separate, and the water-soluble essential oil is dissolved in the water-layer solution in the contact process of the water-layer solution and then discharged from the bottom of the deoiling tower.
The essential oil is removed by utilizing the principle of gas absorption in the deoiling tower.
In some embodiments of the invention, the temperature within the still pot is from 60 to 100 ℃.
After the essential oil of the oil-containing steam obtained from the distillation still is removed from the deoiling tower, the temperature of the obtained essential oil solution is still high, after the essential oil solution passes through the oil-water separator, the obtained water layer solution exchanges heat with the essential oil solution in a heat exchanger, the temperature of the water layer solution is increased, and then the water layer solution is heated by a heater, and the temperature is further increased to 95-105 ℃ so as to keep the circulation amount of the steam.
In some embodiments of the invention, the heater is connected to the deoiler or to both the deoiler and the still.
In some embodiments of the invention, the distillation still is under vacuum or atmospheric conditions.
In some embodiments of the invention, the aqueous layer contains 0.5% to 8% (mass percentage) of sodium chloride or sodium sulfate in the oil-water separator. The water layer in the oil-water separator contains sodium chloride or sodium sulfate, so that the oil-water separation effect is good, the essential oil in the water vapor is removed circularly, the discharge of organic wastewater is reduced, and the environment protection is facilitated.
In some embodiments of the invention, the temperature of the aqueous layer solution after being heated in the heater is 95 to 105 ℃. The water layer solution with the temperature in the range has better absorption effect on essential oil in the oily water vapor. At the same time, heating to the above temperature range is required in order to maintain the amount of vapor recycled back to the still pot. Or heating the water layer solution for gasification, introducing a part of steam into the distillation kettle, and keeping the amount of the steam in the distillation kettle.
One or more technical schemes of the invention have the following beneficial effects:
the water vapor obtained in the deoiling tower is discharged from the top of the deoiling tower and returns to the distillation kettle for recycling, so that the distilled water consumption is saved, and the energy is saved.
The essential oil is fully removed by utilizing the water layer solution and the gas adsorption principle in the deoiling tower.
The speed of the water vapor can be controlled by the exhaust fan, and when the controlled circulation speed is higher, the efficiency is greatly improved. And the increase of the circulation speed basically only increases the power consumption of the exhaust fan without condensation and vaporization steps, so that only a small amount of electric energy is consumed to greatly improve the efficiency.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic view of an apparatus for extracting essential oil by steam distillation;
wherein, 101-a distillation kettle; 102-a steam valve; 103-a steam exhaust fan; 104-a deoiling tower; 105-a heat exchanger; 106-oil water separator; 107-overflow tube; 108-a circulation pump; 109-a heater; 110-back pressure valve; 111-safety valve.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The invention will be further illustrated by the following examples
A device for extracting essential oil by steam distillation is shown in figure 1 and comprises a distillation still 101, a deoiling tower 104, an oil-water separator 106, a heat exchanger 105 and a heater 109, wherein a gas outlet of the distillation still 101 is connected with the lower part of the deoiling tower 104 through a steam exhaust fan 103, the bottom of the deoiling tower 104 is connected with the heat exchanger 105, the heat exchanger 105 is connected with the oil-water separator 106, a water layer outlet of the oil-water separator 106 is connected with the heat exchanger 105 through a circulating pump 108, the heat exchanger 105 is connected with the heater 109, and the heater 109 is connected with the top of the deoiling tower 104. The top of the deoiling column 104 is connected to the still 101 via a back pressure valve 110. The bottom of the distillation still 101 is provided with a steam valve 102, the upper part of the deoiling tower 104 is provided with a safety valve 111, and the upper part of the oil-water separator 106 is provided with an overflow pipe 107.
The height of the deoiling tower 104 is 2.2 meters, the inner diameter is 0.12 meter, stainless steel theta-net ring packing with the diameter and the height of 4mm is filled, the height of a packing section is 1.5 meters, the top of the packing section is 0.1 meter away from the top of the deoiling tower 104, and the bottom of the packing section is 0.6 meter away from the bottom of the deoiling tower 104; the feed inlet at the lower part of the deoiling tower 104 is 0.1 meter below the lower end of the packing section of the deoiling tower 104.
A method for extracting essential oil by steam distillation adopts a process flow shown in figure 1, 10kg of rose with water content of 83.0% (mass percent) is filled in a distillation kettle 101 with the volume of 100 liters as a raw material, the steam enters the distillation kettle 101 from the bottom of the distillation kettle 101 through a steam valve 102 for steam distillation, and the steam containing the essential oil is discharged from the top of the distillation kettle 101;
the water vapor containing the essential oil enters the deoiling tower 104 from the lower part of the deoiling tower 104 through a steam exhaust fan 103 (a variable-frequency high-temperature resistant blower) to remove the essential oil, is discharged from the top of the deoiling tower 104 in the form of water vapor, and then enters the distillation kettle 101 from the bottom of the distillation kettle 101 through a back pressure valve 110 to continuously extract the oil;
discharging the solution containing essential oil from the deoiling tower 104 from the bottom of the deoiling tower 104, cooling in a heat exchanger 105, introducing into an oil-water separator 106, leading out an essential oil layer through an overflow pipe 107 to obtain essential oil, drying with anhydrous sodium sulfate of 50% (mass percent) of the essential oil mass, and storing;
the circulating pump 108 adopts an YT600-1J industrial peristaltic pump produced by Lange constant flow pump company Limited, a water layer in the oil-water separator 106 enters the heater 109 after passing through the circulating pump 108 and the heat exchanger 105 at the speed of 5 liters/minute and is partially gasified, then enters the deoiling tower 104 from the upper part of the deoiling tower 104 to carry out gas-liquid mass transfer so as to remove essential oil in water vapor, a solution containing the essential oil is discharged from the bottom of the deoiling tower 104, and a gas phase part is discharged from the top of the deoiling tower 104 along with water vapor ascending in the deoiling tower 104 and then enters the distillation kettle 101 through the back pressure valve 110;
The steam discharge rate from the top of the still pot 101 was controlled to 3.6 cubic meters per hour by adjusting the steam discharge fan 103.
The temperature in the still pot 101 was adjusted to 95 ℃ by adjusting the back pressure valve 110.
The temperature of the aqueous layer solution after being heated in the heater is 100 ℃, and the liquid levels of the bottom of the deoiling tower 104 and the oil-water separator 106 are stabilized by controlling the gasification ratio of the aqueous layer in the oil-water separator 106 into the heater 109.
The water layer in the oil-water separator contained 4 mass% of sodium chloride.
The top of the deoiling tower 104 is provided with a safety valve 111.
The device is operated for 10 hours to obtain 4.50g of essential oil, 1.5kg of steam is consumed, and the electric energy is 10.5 degrees.
The method for extracting the essential oil by steam distillation realizes the recycling of the steam, and has remarkable energy-saving effect; the circulation rate of the steam is controlled by adjusting the steam exhaust fan, so that the essential oil extraction efficiency is improved; the water layer in the oil-water separator contains sodium chloride, so that the oil-water separation effect is good, the essential oil in the water vapor is circularly removed, the discharge of organic wastewater is reduced, and the environment protection is facilitated.
This embodiment adopts single stills to carry out the steam distillation and draws essential oil, also can adopt the stills of a plurality of series connection to carry out the steam distillation and draw essential oil for raising efficiency.
In this embodiment, the water layer solution is heated by the heater and then completely enters the deoiling tower or partially enters the distillation still through gasification.
Example 2:
the same parts of this embodiment as embodiment 1 will not be described again, but the differences are:
the height of the packing section in the deoiling tower 104 is 1.4 meters, the top of the packing section is 0.2 meters away from the top of the deoiling tower 104, and the bottom of the packing section is 0.6 meters away from the bottom of the deoiling tower 104.
10kg of spearmint having a water content of 83.5% (mass%) was charged as a raw material in a distillation still 101 having a capacity of 100 liters.
The temperature of the aqueous solution after heating in the heater was 105 ℃. The temperature in the still pot 101 was set to 100 ℃ by adjusting the back pressure valve 110.
The water layer in the oil-water separator contained 0.5% (by mass) of sodium chloride.
The device is operated for 11 hours, so that 51.4g of essential oil is obtained, 1.6kg of steam is consumed, and the electric energy is 11.8 degrees.
Example 3:
the same parts of this embodiment as embodiment 2 will not be described again, but the differences are:
the height of the packing section in the deoiling tower 104 is 1.3 meters, the top of the packing section is 0.3 meter away from the top of the deoiling tower 104, and the bottom of the packing section is 0.6 meter away from the bottom of the deoiling tower 104.
The exhaust fan 103 adopts a German MZ 2C NT type diaphragm pump produced by German VACUUBRAND company; the rate of water vapor withdrawal from the top of the still pot 101 was controlled to be 1.8 cubic meters per hour by adjusting the steam discharge fan 103.
The temperature of the aqueous layer solution after being heated in the heater was 95 ℃. The temperature in the still pot 101 was adjusted to 60 ℃ by adjusting the back pressure valve 110.
The water layer in the oil-water separator contained 8 mass% of sodium chloride.
The device is operated for 12 hours to obtain 58.2g of essential oil, 1.4kg of steam is consumed, and the electric energy is 13.1 degrees.
In the embodiment, the essential oil is extracted by steam distillation under vacuum, and the yield of the essential oil is improved.
Example 4:
the same parts of this embodiment as embodiment 3 will not be described again, except that:
the height of the packing section in the deoiling tower 104 is 1.2 meters, the top of the packing section is 0.3 meter away from the top of the deoiling tower 104, and the bottom of the packing section is 0.7 meter away from the bottom of the deoiling tower 104.
10kg of lavender having a water content of 85.0% (mass%) was charged as a raw material in a 100-liter still 101.
The temperature of the aqueous solution after heating in the heater was 96 ℃. The temperature in the still pot 101 was set to 70 ℃ by adjusting the back pressure valve 110.
The water layer in the oil-water separator contained 0.5% (mass%) of sodium sulfate.
The device is operated for 12 hours to obtain 53.5g of essential oil, 1.5kg of steam is consumed, and the electric energy is 12.4 degrees.
Example 5:
the same parts of this embodiment as those of embodiment 4 will not be described again, except that:
the height of the packing section in the deoiling tower 104 is 1.0 meter, the top of the packing section is 0.2 meter away from the top of the deoiling tower 104, and the bottom of the packing section is 1.0 meter away from the bottom of the deoiling tower 104.
The temperature of the aqueous layer solution after being heated in the heater was 97 ℃. The temperature in the still pot 101 was set to 80 ℃ by adjusting the back pressure valve 110.
The water layer in the oil-water separator contained 8 mass% sodium sulfate.
The device is operated for 12 hours to obtain 51.8g of essential oil, 1.5kg of consumed steam and 12.0 degrees of electric energy.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The utility model provides a device for steam distillation extracts essential oil which characterized in that: the device comprises a distillation kettle, a deoiling tower, an oil-water separator, a heat exchanger and a heater, wherein a gas outlet at the top of the distillation kettle is connected with the lower part of the deoiling tower, the bottom of the deoiling tower is connected with the heat exchanger, the heat exchanger is connected with the oil-water separator, a water layer water gap of the oil-water separator is connected with the heat exchanger, the heat exchanger is connected with the heater, and the heater is connected with the top of the deoiling tower.
2. The apparatus for extracting essential oil by steam distillation as claimed in claim 1, wherein: the top of the deoiling tower is connected with the distillation kettle.
3. The apparatus for extracting essential oil by steam distillation as claimed in claim 1, wherein: the oil-water separator is connected with the heat exchanger through a circulating pump.
4. The apparatus for extracting essential oil by steam distillation as claimed in claim 1, wherein: the distillation still is connected with the deoiling tower through a steam exhaust fan.
5. A method for extracting essential oil by steam distillation using the apparatus for extracting essential oil by steam distillation as claimed in any one of claims 1 to 4, characterized in that: the method comprises the following specific steps:
putting the plants into a distillation kettle, introducing steam into the distillation kettle to obtain oil-containing steam, and discharging the oil-containing steam from the distillation kettle into a deoiling tower;
absorbing the oily water vapor in a deoiling tower to obtain an oily solution and water vapor, discharging the water vapor from the top of the deoiling tower, discharging the oily solution from the bottom of the deoiling tower, and allowing the oily solution to enter an oil-water separator for separation to obtain essential oil and a water layer solution;
and heating the water layer solution, and then feeding the water layer solution into a deoiling tower for adsorption deoiling of oil-containing water vapor.
6. A process for the steam distillation of essential oils according to claim 5, characterized in that: the deoiling tower is internally provided with a filler which is a stainless steel theta net ring filler, further, the height of the filler section is 1-1.5 meters, the top of the filler section is 0.1-0.3 meter away from the top of the deoiling tower, and the bottom of the filler section is 0.6-1.0 meter away from the bottom of the deoiling tower.
7. A process for the steam distillation of essential oils according to claim 5, characterized in that: the temperature in the distillation kettle is 60-100 ℃.
8. A process for the steam distillation extraction of essential oils as claimed in claim 1, characterized in that: the distillation kettle is under vacuum condition or normal pressure condition.
9. A process for the steam distillation extraction of essential oils as claimed in claim 1, characterized in that: in the oil-water separator, the water layer contains 0.5-8% of sodium chloride or sodium sulfate.
10. A process for the steam distillation extraction of essential oils as claimed in claim 1, characterized in that: the temperature of the water layer liquid after being heated in the heater is 95-105 ℃.
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| CN106433984A (en) * | 2016-10-10 | 2017-02-22 | 罗定市荣兴香料有限公司 | Apparatus for extracting essential oil |
| CN109207262A (en) * | 2018-10-17 | 2019-01-15 | 武汉轻工大学 | The extraction element and extracting method of volatile plant essence oil |
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| CN201506783U (en) * | 2009-09-28 | 2010-06-16 | 潍坊中业化学有限公司 | Refining castor oil dehydration device |
| CN103466749A (en) * | 2012-06-06 | 2013-12-25 | 陈晗 | Effective method for removing oil content in aqueous solution |
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