AU2020102533A4 - A method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations - Google Patents
A method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations Download PDFInfo
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- AU2020102533A4 AU2020102533A4 AU2020102533A AU2020102533A AU2020102533A4 AU 2020102533 A4 AU2020102533 A4 AU 2020102533A4 AU 2020102533 A AU2020102533 A AU 2020102533A AU 2020102533 A AU2020102533 A AU 2020102533A AU 2020102533 A4 AU2020102533 A4 AU 2020102533A4
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- steam
- distillation
- essential oil
- cinnamomum camphora
- pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/38—Steam distillation
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/115—Natural spices, flavouring agents or condiments; Extracts thereof obtained by distilling, stripping, or recovering of volatiles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
-
- 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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Fats And Perfumes (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a method of extracting Cinnamomum camphora essential oil by steam
distillation with twice continuous pressure regulations. Its specific process is as follows. After
filling branches and leaves in the distillation still, close the feed inlet port, and introduce steam
from the bottom of still to carry out steam distillation. Regulate the air pressure of introduced
steam by air pressure regulating device. There are two continuous distillation stages in the
steam distillation process- in the first stage, the steam pressure is controlled to be 0.3 ~ 0.6MPa,
and the distillation time is 3 ~ 10 min; in the second stage, the steam pressure is controlled to
be 0.05 ~ 0.2 MPa, and the distillation time to be 70 ~ 120 min. Compared with the existing
steam distillation methods, the present method reduces consumption of steam and production
energy. In addition, with a shorter distillation time and higher yield of essential oil, the method
improves production efficiency of Cinnamomum camphora essential oil and reduces the
extraction cost.
Description
A method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations
[01] The invention relates to an extraction method of Cinnamomum camphora essential oil, in particular to a method for extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations.
[02] Cinnamomum camphora (L.) Presl. belongs to Cinnamon of the Lauraceae. Its roots, stems, branches and leaves can be used to extract natural Cinnamomum camphora essential oil and at present, branches and leaves are mainly used to extract Cinnamomum camphora essential oil. As an important perfume material, natural Cinnamomum camphora essential oil is rich in linalool and has a wide range of uses in food flavours and fragrances and daily chemicals. At present, the main extraction methods of Cinnamomum camphora essential oil are steam distillation extraction, organic solvent extraction, microwave-assisted extraction, ultrasonic-assisted extraction, supercritical carbon dioxide fluid extraction and so on. There are some problems in organic solvent extraction method, such as low oil yield, solvent residue, and low purity of essential oil. Microwave-assisted extraction and ultrasonic-assisted extraction can partly overcome the low oil yield of organic solvent extraction, but there are still some problems such as solvent residue, low purity of essential oil and complicated production equipment. While supercritical carbon dioxide fluid extraction has the advantages of high extraction efficiency and no solvent residue, but it still has the disadvantages of complicated production equipment, high production cost and low treatment efficiency. Comparatively speaking, steam distillation extraction method has the advantages of simple process, simple equipment, low cost, stable output, and high purity of extracted essential oil, which is widely adopted by domestic and foreign manufacturers.
[03] At present, manufacturers often adopt steam distillation method to extract Cinnamomum camphora essential oil. However, most of the factories still use traditional steam distillation method, which has poor equipment and causes large volatile loss of essential oil, and only a few factories use modern steam distillation equipment. For modern equipment, there is an industrial boiler used to generate steam and a distillation still mostly made of stainless steel. The still can hold about 700 kg of branches and leaves at one time, which has the advantages of large processing capacity and less loss of essential oil. However, many factories usually use fixed steam pressure for distillation in the actual production process, which is not scientific. If the steam pressure is too high in the distillation process, the steam demand will increase, which will further lead to increased demand for the condensing area of the condensing equipment, and the demand for condensate water will also increase. At the same time, this will cause some essential oil volatilization loss, directly leading to the decrease of oil yield and increase of unit cost. If the steam pressure used in the distillation process is not enough, it is necessary to extend the distillation time, which will lead to the reduction of production efficiency, and cause the residue of essential oil in branches and leaves. Therefore, it is particularly important to develop a more scientific optimization control process of steam pressure.
[04] Based on this, the invention provides a method for extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations which utilizes the advantages of twice pressure regulations to overcome the defects of traditional steam distillation extraction, thereby realizing the efficient and rapid extraction of Cinnamomum camphora essential oil.
[05] In order to solve the problem of steam pressure control process existing in extraction of Cinnamomum camphora essential oil by steam distillation, the invention provides a method for extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations.
[06] The technical scheme adopted in the invention is as follows.
[07] A method for extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations comprise two continuous distillation stages with different steam pressure. It comprises following steps.
[08] (1) After filling branches and leaves in the distillation still, introduce steam to carry out the first stage distillation. At this time, the steam pressure is controlled to be 0.3-0.6 MPa, and the distillation time is 3~10 min.
[09] (2) After completing the first stage distillation, lower the steam pressure, and start the second stage distillation, with steam pressure controlled to be 0.05-0.2 MPa, and the distillation time to be 70~120 min.
[010] In step (1), the branches and leaves filled in the distillation still are fine branches and leaves cut by the branch crusher. The steam used for distillation comes from the steam boiler.
[011] In the first distillation stage, the steam pressure is controlled to be 0.3-0.6 MPa. That is because in the early stage of distillation, the temperature of the still and the branches and leaves in the still is low, a large amount of high-temperature steam is needed to realize rapid temperature rise of the still and the branches and leaves.
[012] In above first distillation stage, the steam pressure is controlled to be 0.3-0.6 MPa, and time is 3~10 min. Under the heating of a large amount of high temperature steam, the temperature of the still and the branches and leaves in the still keeps increasing until reaches the stable distillation temperature. At this time, the mixed gas of water vapor and Cinnamomum camphora essential oil will flow from the distillation still to the condenser. As a large amount of water vapor and Cinnamomum camphora essential oil mixed gas continues to pass through the condenser, part of the essential oil cannot be condensed, so the first distillation time should not be too long. After reaching the distillation temperature, it can be transferred to the second distillation.
[013] In the first stage of distillation, it is preferred that the steam pressure of is 0.4 MPa and the distillation time is 6 min.
[014] After the first distillation, lower the steam pressure to start the second distillation. Methods to reduce the pressure of the steam include to reduce the steam output of the steam generating equipment or to adjust the air pressure control valve of the steam pipe.
[015] In the second distillation stage, the steam pressure is controlled to be 0.05-0.2 MPa. Moreover, in order to ensure that the mixed gas of steam and Cinnamomum camphora essential oil can be completely condensed by the condenser and reduce the loss of essential oil, the amount of steam flowing into the still should not be too large.
[016] Further, in the second distillation stage, the distillation time is controlled to be 70-120 min. In order to reduce the remnant amount of Cinnamomum camphora essential oil in the residue as much as possible and realize the efficient extraction of Cinnamomum camphora essential oil, the second distillation needs to keep a certain time.
[017] In the second distillation, it is preferred that the steam pressure is 0.1 MPa and the distillation time is 85 min.
[018] After a large number of experimental verification and analysis, under the above optimal conditions, the efficient extraction of Cinnamomum camphora essential oil can be achieved. Compared with traditional distillation process, the yield of Cinnamomum camphora essential oil is equivalent, but the treatment amount of branches and leaves by a single reactor in one day is only about 3,000 kg, while the treatment amount of this invention can reach 4,200 kg, which indicating that the production efficiency is greatly improved. In addition, compared with the fixed steam pressure distillation process, the invention can effectively shorten the distillation time, reduce the energy consumption, and improve the yield of Cinnamomum camphora essential oil.
[019] The present invention is described in detail through the embodiment below, but the present invention is not limited to the following embodiments.
[020] Embodiment 1
[021] Fill the distillation still with 700 kg of treated leaves, then close it, and access steaming.
[022] At this time, regulate the inlet steam pressure to 0.4 MPa, and keep distillation at this steam pressure for 6 min. With the temperature of distillation still and the branches and leaves in the still increasing to reach a stable distillation temperature, access a mixed gas of water vapor and Cinnamomum camphora essential oil to the condenser through the distillation still.
[023] Then, reduce the steam pressure to 0.1 MPa, and keep distillation for 90 min under the steam pressure. Stop accessing steam and end the distillation. After the oil and water in the oil-water separator are completely stratified, separate Cinnamomum camphora essential oil, and weigh it. The yield rate of Cinnamomum camphora essential oil is calculated according to formula (1):
[024] Yield rate of Cinnamomum camphora essential oil = weight of Cinnamomum camphora essential oil / weight of branches and leavesx100% Formula
(1).
[025] It can be calculated that the yield of Cinnamomum camphora essential oil obtained by above process is 0.789%.
[026] Embodiment 2
[027] Fill the distillation still with 700 kg of treated leaves, then close it, and access steaming.
[028] At this time, regulate the inlet steam pressure to 0.3 MPa, and keep distillation at this steam pressure for 8 min. With the temperature of distillation still and the branches and leaves in the still increasing to reach a stable distillation temperature, access a mixed gas of water vapor and Cinnamomum camphora essential oil to the condenser through the distillation still.
[029] Then, reduce the steam pressure to 0.075 MPa, and keep distillation for 120 min under the steam pressure. Stop accessing steam and end the distillation. After the oil and water in the oil-water separator are completely stratified, separate Cinnamomum camphora essential oil, and weigh it. The yield rate of Cinnamomum camphora essential oil is calculated according to formula (1). It can be calculated that the yield of essential oil obtained by above process is 0.775%.
[030] Although the invention has been described with reference to specific examples, it will be appreciated by those skilled in the art that the invention may be embodied in many other forms, in keeping with the broad principles and the spirit of the invention described herein.
[031] The present invention and the described embodiments specifically include the best method known to the applicant of performing the invention. The present invention and the described preferred embodiments specifically include at least one feature that is industrially applicable
Claims (6)
1. A method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations, characterized by realizing highly efficient extraction of Cinnamomum camphora essential oil through steam distillation with twice continuous pressure regulations.
2. The method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations according to claim 1, characterized by comprising two continuous distillation stages with different steam pressure requirements.
3. The method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations according to claim 2, characterized in that in the first stage, the steam pressure is controlled to be 0.3~0.6 MPa, and in the second stage, the steam pressure is controlled to be 0.05-0.2 MPa.
4. The method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations according to claim 2, characterized in that in the first stage, the distillation time is 3-10 min, and in the second stage, the distillation time is 70~120 min.
5. The method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations according to claim 3, characterized in that the method of adjusting the steam pressure is to change the amount of steam flowing into the still.
6. The method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations according to claim 5, characterized in that the methods to reduce the pressure of the steam include to reduce the steam output of the steam generating equipment or to adjust the air pressure control valve of the steam pipe.
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| Application Number | Priority Date | Filing Date | Title |
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| AU2020102533A AU2020102533A4 (en) | 2020-09-30 | 2020-09-30 | A method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations |
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| AU2020102533A AU2020102533A4 (en) | 2020-09-30 | 2020-09-30 | A method of extracting Cinnamomum camphora essential oil by steam distillation with twice continuous pressure regulations |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114481662A (en) * | 2021-12-22 | 2022-05-13 | 岳阳林纸股份有限公司 | Camphorwood oil extraction pulping method |
| CN115011411A (en) * | 2022-06-14 | 2022-09-06 | 宜宾石平香料有限公司 | Production process for continuously extracting cinnamomum camphora oil |
| CN116497619A (en) * | 2023-05-17 | 2023-07-28 | 岳阳林纸股份有限公司 | Natural color chemimechanical pulping process for camphorwood sodium hydroxide |
-
2020
- 2020-09-30 AU AU2020102533A patent/AU2020102533A4/en not_active Ceased
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114481662A (en) * | 2021-12-22 | 2022-05-13 | 岳阳林纸股份有限公司 | Camphorwood oil extraction pulping method |
| CN115011411A (en) * | 2022-06-14 | 2022-09-06 | 宜宾石平香料有限公司 | Production process for continuously extracting cinnamomum camphora oil |
| CN116497619A (en) * | 2023-05-17 | 2023-07-28 | 岳阳林纸股份有限公司 | Natural color chemimechanical pulping process for camphorwood sodium hydroxide |
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