CN107011995B - Dry distillation extraction method for plant aromatic oil - Google Patents
Dry distillation extraction method for plant aromatic oil Download PDFInfo
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- CN107011995B CN107011995B CN201710390343.7A CN201710390343A CN107011995B CN 107011995 B CN107011995 B CN 107011995B CN 201710390343 A CN201710390343 A CN 201710390343A CN 107011995 B CN107011995 B CN 107011995B
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- distillation
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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
Abstract
The invention relates to a method for extracting plant aromatic oil by dry distillation, which comprises the steps of cutting raw materials into small pieces, dropping the small pieces into a closed hopper, and conveying the small pieces into a dry heat distillation device by a closed conveying device arranged at the bottom of the hopper. The dry heat distillation device consists of a static shell and a rotary heat exchange tube bundle, a heat source medium with a preset temperature is introduced into the heat exchange tube bundle to indirectly heat materials in the dry heat distillation device, so that aromatic oil and moisture in the materials form mixed gas, the mixed gas flows out through a top outlet and is condensed into liquid state through a condenser, and the materials are output out of the device through a closed conveying device from a discharge port; preventing the loss of the plant aromatic oil; the quick distillation of the materials is facilitated, and the thermal efficiency of distillation is improved; is beneficial to distilling out the high boiling point aromatic oil component and obtaining the substance component which is not obtained by the traditional process.
Description
Technical Field
The invention relates to a method for extracting plant aromatic oil by dry distillation, in particular to a method for distilling aromatic oil by high-temperature indirect heating and continuous dry heating.
Background
At present, the distillation and extraction of the plant aromatic oil adopt an atmospheric retort type steam distillation method or a pressurized kettle type steam distillation method, and the two methods have the defects that:
1. although the atmospheric retort type steam distillation method has simple equipment and easy operation, because the distillation is carried out at the water boiling point temperature, the high boiling point aromatic oil component contained in the plant is difficult to be distilled off along with the steam in large quantity, the distillation is not thorough, and the yield of the aromatic oil is low; 2. although the pressurized kettle type steam distillation method can overcome the defects of the normal pressure retort type steam distillation method and realize high temperature distillation, the distillation kettle equipment is a pressure container, so that the equipment investment cost is high, the requirement on the operation of workers is high, and the potential safety hazard is large;
3. in addition, the two steam distillation processes have the common disadvantage that:
(1) a large amount of water vapor and heat energy are consumed, the heat energy of the heat medium (water vapor) is difficult to recover, and the energy cost is high;
(2) because a large amount of water vapor enters the volatilized aromatic oil, the cooling water consumption is large during subsequent cooling;
(3) the water content of the waste residue after distillation is large, and the treatment cost of drying and the like during subsequent utilization is high.
Based on the defects, the traditional distillation method has large water consumption and high energy cost, and the distillation rate of the aromatic oil can only reach 40-50 percent of the actual oil content, so that the resources can not be fully utilized.
Disclosure of Invention
The invention aims to provide a method for extracting plant aromatic oil by dry distillation, which can overcome the defects that the traditional method has low extraction efficiency and high energy consumption, and the water content of distilled waste residues is large and is not beneficial to subsequent utilization.
In order to achieve the purpose, the technical scheme adopted by the invention is that the method for extracting the plant aromatic oil by dry distillation adopts an indirect heating mode without contacting with a heat source medium to heat the raw materials, the aromatic oil contained in the raw materials is fully volatilized to form mixed gas, the mixed gas is escaped from a gas outlet, and the aromatic oil is obtained after cooling and separation.
Further, the raw material is one or more of roots, stems, leaves, flowers and fruits of plants.
Further, the raw materials are pulverized before heating.
The method for extracting the plant aromatic oil by dry distillation comprises the following steps:
a. after being crushed into crushed materials, the raw materials fall into a hopper, and the materials are conveyed into a dry heat distillation device by a conveying device arranged at the bottom of the hopper;
b. the material is indirectly heated by a heat source medium in a heat exchange tube bundle in a dry heat distillation device consisting of a static shell and a rotary heat exchange tube bundle;
c. under the action of heat, the aromatic oil and the water in the material form mixed gas, the mixed gas is collected at the top of the dry heat distillation device and flows into a condenser through a gas guide pipe to be condensed into liquid; the material automatically and uniformly turns in the dry heat distillation device and moves for 15-35 minutes along the axial direction, and waste residues are automatically discharged from a discharge port;
furthermore, the raw materials are in a closed space in the crushing and conveying processes.
Further, the crushed aggregates pass through a 10 mm sieve mesh.
Furthermore, the heat exchange tube bundles in the dry heat distillation device are arranged into a plurality of bundles, so that a better heating effect is achieved.
Further, the initial temperature of the heat source medium is 150-230 ℃, high-temperature short-time distillation is realized, and aromatic oil with higher boiling point can be distilled out.
Further, the heat source medium is one or a combination of more of methyl silicone oil, vegetable oil and synthetic engine oil.
Preferably, the top of the dry heat distillation device is provided with a filtering and dedusting net.
Preferably, the movement track of the materials in the tube bundle type dry heat distillation device is spiral movement.
Preferably, the material moves in the pipe bundle type dry heat distillation device in the direction opposite to the heat source medium.
The method has the following advantages:
1. continuous feeding, continuous distillation and continuous discharging, and improves daily processing capacity. Meanwhile, the labor intensity and the labor cost are effectively reduced;
2. the feeding and discharging are sealed to prevent the loss of the plant aromatic oil;
3. the dry heat distillation increases the distillation temperature, is beneficial to realizing the rapid distillation of materials and improves the thermal efficiency of distillation; the method is favorable for distilling out high-boiling-point aromatic oil components to obtain substance components which are not obtained by the traditional process, and can improve the oil yield by 30-40% compared with the traditional method;
4. compared with the traditional method, the method does not use water vapor in the distillation process, greatly reduces the total amount of distilled water-oil mixture, thereby greatly reducing the consumption of cooling water (20-30%);
5. by adopting an indirect heating mode, the heating medium and the waste heat thereof can be recycled, and the power cost is saved by 50-60% compared with the traditional method;
6. the obtained dry and hot material (waste residue) can be directly used as fuel or used for preparing raw materials of biomass briquette fuel or other purposes. Compared with the traditional steam distillation mode, the method saves the manpower or power cost of the subsequent drying process.
Drawings
FIG. 1 is a schematic view of a dry heat distiller used in examples 1 to 6.
Detailed Description
Example 1: a dry distillation extraction method of cinnamomum longepaniculatum branch and leaf aromatic oil comprises the following steps:
a. the cinnamomum longepaniculatum branches and leaves are fed into a chopper (1), the cinnamomum longepaniculatum leaves are chopped, and the crushed materials pass through a 10 mm sieve mesh.
b. The chopped materials naturally fall into a closed conveying device (2), the closed conveying device (2) conveys the chopped materials into a dry heat distillation device (3) through a feed inlet (31) of the dry heat distillation device (3), the materials are scooped up through a scoop plate (34) arranged on a heat exchange tube bundle (33) between a static shell (32) of the dry heat distillation device (3) and a plurality of rotary heat exchange tube bundles (33), the materials are refluxed at a high position, the materials are enabled to spirally move in the dry heat distillation device and fully and uniformly contact with the heat exchange tube bundle (33) for heating, and the initial temperature of a heat source medium in the heat exchange tube bundle is 180 ℃;
c. the generated oil-water mixed steam flows out of the steam outlet (35) to a cooler for cooling treatment, and when the oil-water mixed steam flows out of the steam outlet, dust is filtered through a filter (36) arranged on the steam outlet (35); the camphor branch leaf residues are automatically and uniformly turned in the dry heat distillation device (3) and axially move for 25 minutes, and the waste residues are automatically discharged from a discharge hole (37) and flow out to enter a closed conveyor (4) to be output in a dry material mode.
Example 2:
a method for extracting cinnamomum longepaniculatum aromatic oil by dry distillation comprises the following steps:
a. the cinnamomum camphora roots are fed to a chopper (1) and chopped, the particles being screened through a 10 mm mesh.
b. The chopped materials naturally fall into a closed conveying device (2), the closed conveying device (2) conveys the chopped materials into a dry heat distillation device (3) through a feed inlet (31) of the dry heat distillation device (3), the materials are scooped up through a scoop plate (34) arranged on a heat exchange tube bundle (33) between a static shell (32) of the dry heat distillation device (3) and a plurality of rotary heat exchange tube bundles (33), and flow back at a high position, so that the materials are in spiral motion in the dry heat distillation device and fully and uniformly contacted with the heat exchange tube bundle (33) for heating, and the initial temperature of a heat source medium in the heat exchange tube bundle is 230 ℃;
c. the generated oil-water mixed steam flows out of the steam outlet (35) to a cooler for cooling treatment, and when the oil-water mixed steam flows out of the steam outlet, dust is filtered through a filter (36) arranged on the steam outlet (35); the cinnamomum longepaniculatum root residues automatically and uniformly turn over in the dry heat distillation device (3) and axially move for 30 minutes, and the waste residues are automatically discharged from a discharge hole (37) and flow out to enter a closed conveyor (4) to be output in a dry material mode.
Example 3:
a dry distillation extraction method of cinnamomum japonicum branch and leaf aromatic oil comprises the following steps:
a. the Cinnamomum cassia twig and leaves are fed into a chopper (1), the Cinnamomum cassia twig and leaves are chopped, and the crushed materials are sieved by 6 mm sieve meshes.
b. The chopped materials naturally fall into a closed conveying device (2), the closed conveying device (2) conveys the chopped materials into a dry heat distillation device (3) through a feed inlet (31) of the dry heat distillation device (3), the materials are scooped up through a scoop plate (34) arranged on a heat exchange tube bundle (33) between a static shell (32) of the dry heat distillation device (3) and a plurality of rotary heat exchange tube bundles (33), and flow back at a high position, so that the materials are in spiral motion in the dry heat distillation device and fully and uniformly contacted with the heat exchange tube bundle (33) for heating, and the initial temperature of a heat source medium in the heat exchange tube bundle is 230 ℃;
c. the generated oil-water mixed steam flows out of the steam outlet (35) to a cooler for cooling treatment, and when the oil-water mixed steam flows out of the steam outlet, dust is filtered through a filter (36) arranged on the steam outlet (35); the cinnamomum cassia twig and leaf residues automatically and uniformly turn over in the dry heat distillation device (3) and move for 30 minutes along the axial direction, and the waste residues are automatically discharged from the discharge hole (37) and flow out to enter the closed conveyor (4) to be output in the form of dry materials.
Example 4:
a method for extracting litsea cubeba fruit aromatic oil by dry distillation comprises the following steps:
a. the litsea cubeba fruits are conveyed into a closed conveying device (2), the closed conveying device (2) conveys materials into a dry heat distillation device (3) through a feed inlet (31) of the dry heat distillation device (3), the materials are scooped up through a scoop plate (34) arranged on a heat exchange tube bundle (33) between a static shell (32) of the dry heat distillation device (3) and a plurality of rotary heat exchange tube bundles (33), the materials are refluxed at a high position, the materials are enabled to spirally move in the dry heat distillation device and fully and uniformly contact with the heat exchange tube bundle (33) for heating, and the initial temperature of a heat source medium in the heat exchange tube bundle is 150 ℃;
c. the generated oil-water mixed steam flows out of the steam outlet (35) to a cooler for cooling treatment, and when the oil-water mixed steam flows out of the steam outlet, dust is filtered through a filter (36) arranged on the steam outlet (35); the litsea cubeba fruit residues are automatically and uniformly turned in the dry heat distillation device (3) and axially move for 20 minutes, and the waste residues are automatically discharged from a discharge hole (37) and flow out to enter a closed conveyor (4) to be output in a dry material mode.
Example 5:
a dry distillation extraction method of cinnamon bark aromatic oil comprises the following steps:
a. feeding cortex Cinnamomi into a chopper (1), chopping the cortex Cinnamomi, and sieving with 10 mm sieve.
b. The chopped materials naturally fall into a closed conveying device (2), the closed conveying device (2) conveys the chopped materials into a dry heat distillation device (3) through a feed inlet (31) of the dry heat distillation device (3), the materials are scooped up through a scoop plate (34) arranged on a heat exchange tube bundle (33) between a static shell (32) of the dry heat distillation device (3) and a plurality of rotary heat exchange tube bundles (33), and flow back at a high position, so that the materials are in spiral motion in the dry heat distillation device and fully and uniformly contacted with the heat exchange tube bundle (33) for heating, and the initial temperature of a heat source medium in the heat exchange tube bundle is 230 ℃;
c. the generated oil-water mixed steam flows out of the steam outlet (35) to a cooler for cooling treatment, and when the oil-water mixed steam flows out of the steam outlet, dust is filtered through a filter (36) arranged on the steam outlet (35); the Sichuan osmanthus tree bark residues automatically and uniformly turn over in the dry heat distillation device (3) and move for 35 minutes along the axial direction, and the waste residues are automatically discharged from the discharge hole (37) and flow out to enter the closed conveyor (4) to be output in a dry material mode.
Example 6:
a method for extracting lavender flower aromatic oil by dry distillation comprises the following steps:
a. the lavender spikes are fed to a chopper (1) and chopped, the particles being screened through a 10 mm mesh.
b. The chopped materials naturally fall into a closed conveying device (2), the closed conveying device (2) conveys the chopped materials into a dry heat distillation device (3) through a feed inlet (31) of the dry heat distillation device (3), the materials are scooped up through a scoop plate (34) arranged on a heat exchange tube bundle (33) between a static shell (32) of the dry heat distillation device (3) and a plurality of rotary heat exchange tube bundles (33), and flow back at a high position, so that the materials are in spiral motion in the dry heat distillation device and fully and uniformly contacted with the heat exchange tube bundle (33) for heating, and the initial temperature of a heat source medium in the heat exchange tube bundle is 200 ℃;
c. the generated oil-water mixed steam flows out of the steam outlet (35) to a cooler for cooling treatment, and when the oil-water mixed steam flows out of the steam outlet, dust is filtered through a filter (36) arranged on the steam outlet (35); the lavender spica residue automatically and uniformly turns over in the dry heat distillation device (3) and moves for 15 minutes along the axial direction, the waste residue is automatically discharged from the discharge port (37), flows out and enters the closed conveyor (4) to be output in the form of dry materials.
Claims (4)
1. A method for extracting plant aromatic oil by dry distillation is characterized in that the raw material is heated by an indirect heating mode without contacting with a heat source medium, aromatic oil contained in the raw material is fully volatilized to form mixed gas, the mixed gas escapes from a gas outlet, and the aromatic oil is obtained after cooling and separation; the indirect heating mode is tubular heat exchange heating;
the method comprises the following steps:
a. after being crushed into crushed materials, the raw materials are conveyed into a dry heat distillation device;
b. the material is in the dry heat distillation device composed of a static shell and a rotary heat exchange tube bundle, and is indirectly heated by a heat source medium in the heat exchange tube bundle, the material is between the static shell and the plurality of rotary heat exchange tube bundles of the dry heat distillation device, and is scooped up by a scooping plate arranged on the heat exchange tube bundle and flows back at a high position, so that the material spirally moves in the dry heat distillation device, and the moving direction of the material is opposite to the flowing direction of the heat source medium;
c. under the action of heat, the aromatic oil and the water in the material form mixed gas, the mixed gas is collected at the top of the dry heat distillation device and flows into a condenser through a gas guide pipe to be condensed into liquid; the material automatically and uniformly turns in the dry heat distillation device and moves for 15-35 minutes along the axial direction, and waste residues are automatically discharged from a discharge port;
the raw materials are in a closed space in the crushing and conveying processes;
the initial temperature of the heat source medium is 150-230 ℃, and high-temperature short-time distillation is realized.
2. The method of claim 1, wherein the plant material is one or more of plant root, stem, leaf, flower, and fruit.
3. The method for extracting plant aroma oil by dry distillation as claimed in claim 1, wherein the raw material is pulverized and then passed through a 10 mm mesh.
4. The method for extracting plant aromatic oil by dry distillation according to claim 1, wherein the heat exchange tube bundle in the dry heat distillation device is provided with a plurality of tubes.
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| CN108315097A (en) * | 2018-02-09 | 2018-07-24 | 程勇 | A kind of charging/discharging device and its application method refining essential oil |
| CN108852897A (en) * | 2018-07-12 | 2018-11-23 | 江西中科硒谷功能农业发展有限公司 | A kind of preparation method of being Selenium in Plants nourishing skin liquid |
| CN110031455A (en) * | 2019-04-12 | 2019-07-19 | 宜宾学院 | A kind of quick detection natural aromatic oil mixes the method and kit of puppet |
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| CN1306079A (en) * | 2000-01-18 | 2001-08-01 | 四川省汉源外贸食品厂 | Low-temp low-pressure dry distillation process for extracting aromatic oil from Chinese pepper |
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