CN114989896B - Clove bud oil for cigarettes and extraction method thereof - Google Patents
Clove bud oil for cigarettes and extraction method thereof Download PDFInfo
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- CN114989896B CN114989896B CN202210853616.8A CN202210853616A CN114989896B CN 114989896 B CN114989896 B CN 114989896B CN 202210853616 A CN202210853616 A CN 202210853616A CN 114989896 B CN114989896 B CN 114989896B
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- 239000001902 eugenia caryophyllata l. bud oil Substances 0.000 title claims abstract description 77
- 238000000605 extraction Methods 0.000 title claims abstract description 66
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 110
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 235000019476 oil-water mixture Nutrition 0.000 claims abstract description 33
- 239000001353 eugenia caryophyllata l. Substances 0.000 claims abstract description 20
- 241000628997 Flos Species 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 12
- 235000019198 oils Nutrition 0.000 claims description 32
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical group [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 11
- 244000223014 Syzygium aromaticum Species 0.000 claims description 11
- 235000016639 Syzygium aromaticum Nutrition 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 3
- 239000000341 volatile oil Substances 0.000 abstract description 16
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000003921 oil Substances 0.000 description 31
- 238000009833 condensation Methods 0.000 description 22
- 230000005494 condensation Effects 0.000 description 22
- 239000008367 deionised water Substances 0.000 description 17
- 229910021641 deionized water Inorganic materials 0.000 description 17
- 238000010992 reflux Methods 0.000 description 13
- 238000005485 electric heating Methods 0.000 description 12
- 239000010779 crude oil Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000295 fuel oil Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000001256 steam distillation Methods 0.000 description 3
- 241000208125 Nicotiana Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000002457 bidirectional effect Effects 0.000 description 1
- 239000010634 clove oil Substances 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- 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
- C11B9/025—Recovery by solvent extraction
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Agronomy & Crop Science (AREA)
- Botany (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides an extraction method of clove bud oil for cigarettes, which comprises the following steps: a) Extracting and collecting flos Caryophylli bud in an extraction device to obtain a collecting solution of oil-water mixture; b) Mixing the collected liquid with water for demulsification, and then separating to obtain clove bud oil; the extraction device includes: the container is used for containing the clove buds and the extracting solvent, and a heating device is arranged below the container; the container mouth is connected with a three-way bent angle, a main pipe and a branch pipe of the three-way bent angle are respectively connected with a first condensing pipe and a second condensing pipe, and a collecting container is arranged at the outlet position of the second condensing pipe. According to the invention, the oil-water mixture of the clove bud oil is obtained by adopting a specific extraction device, and then the oil-water mixture is demulsified by adopting a specific demulsification method, so that the extraction method is simple and easy to implement, the applicability is strong, and the extraction efficiency of the essential oil is obviously improved.
Description
Technical Field
The invention belongs to the technical field of tobacco flavor, and particularly relates to clove bud oil for tobacco and an extraction method thereof.
Background
At present, in the technical field of extraction of natural essential oil of plants, an oil-water separator device is generally adopted for extracting the natural essential oil. Natural essential oils are also classified into light oils and heavy oils, i.e.: lighter than water is light oil, heavier than water is heavy oil, and most of essential oil belongs to light oil. The clove bud oil belongs to heavy oil, and is positioned at the lower layer of an oil collecting pipe of an oil-water separator during extraction by a steam distillation method, and the upper layer is water.
In the process of extracting essential oil by using an oil-water separator in the steam distillation method at present, oil-water mixed steam formed by the clove bud oil and water is easy to form emulsion after being condensed to form a stable milky white oil-water mixture, oil-water cannot be separated and layered, a series of processes of reflux, heating, steam and condensation are repeated, and the oil collecting pipe of the oil-water separator is difficult to collect the clove bud oil, so that the extraction yield of the clove bud oil is extremely low. The oil content of the clove buds is generally 10-20%, and the oil content of the clove buds is about 1% by adopting a steam distillation method to extract the oil of the clove buds by utilizing a traditional oil-water separator, which is far lower than the oil content of the clove buds. Therefore, the extraction method of the clove bud oil is needed at present, the yield of the essential oil is improved, and the production requirement of the clove bud oil is met.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide the clove bud oil for cigarettes and the extraction method thereof.
The invention provides an extraction method of clove bud oil for cigarettes, which comprises the following steps:
a) Extracting and collecting flos Caryophylli bud in an extraction device to obtain a collecting solution of oil-water mixture;
b) Mixing the collected liquid with water for demulsification, and then separating to obtain clove bud oil;
the extraction device includes:
the container is used for containing the clove buds and the extracting solvent, and a heating device is arranged below the container;
the container mouth is connected with a three-way bent angle, a main pipe and a branch pipe of the three-way bent angle are respectively connected with a first condensing pipe and a second condensing pipe, and a collecting container is arranged at the outlet position of the second condensing pipe.
Preferably, the extraction solvent is selected from water, and the mass ratio of the clove buds to the extraction solvent is 1: (5-9).
Preferably, the extraction temperature is 100 ℃ and the extraction time is 4-8 hours.
Preferably, the container for containing clove bud oil and extraction solvent is selected from a round-bottom flask, and the volume of the round-bottom flask is selected from one of 2000mL, 3000mL and 5000 mL.
Preferably, in the step B), the mass ratio of the collected liquid to water is 1: (2-3).
Preferably, the collecting container contains water;
and the collected liquid is collected, meanwhile, demulsification is carried out, and water is additionally added into a collecting container during demulsification.
Preferably, the collected liquid and water are stirred during demulsification, the stirring speed is 10-100 rpm, and the stirring time is 1-10 min.
Preferably, in step B), after the separation, a step of removing moisture is further included, and the moisture-removing substance is anhydrous sodium sulfate.
The invention also provides the clove bud oil extracted by the extraction method, and the yield of the clove bud oil is more than or equal to 9.9%.
Compared with the prior art, the invention provides a method for extracting clove bud oil for cigarettes, which comprises the following steps: a) Extracting and collecting flos Caryophylli bud in an extraction device to obtain a collecting solution of oil-water mixture; b) Mixing the collected liquid with water for demulsification, and then separating to obtain clove bud oil; the extraction device includes: the container is used for containing the clove buds and the extracting solvent, and a heating device is arranged below the container; the container mouth is connected with a three-way bent angle, a main pipe and a branch pipe of the three-way bent angle are respectively connected with a first condensing pipe and a second condensing pipe, and a collecting container is arranged at the outlet position of the second condensing pipe. According to the invention, the oil-water mixture of the clove bud oil is obtained by adopting a specific extraction device, and then the oil-water mixture is demulsified by adopting a specific demulsification method, so that the extraction method is simple and easy to implement, the applicability is strong, and the extraction efficiency of the essential oil is obviously improved.
Drawings
Fig. 1 is a schematic structural diagram of an extraction device of clove bud oil for cigarettes, which is provided by the invention;
in the figure: 1-electric heating sleeve, 2-round bottom flask, 3-three-way bent angle, 4-condenser tube, 41-water inlet, 42-water outlet, 5-condenser tube, 51-water inlet, 52-water outlet, 6-oil-water mixture drop, 7-beaker, 8-magnetic stirrer and 9-magnetic stirrer;
FIG. 2 is a schematic structural view of a prior art and comparative examples 1 and 2 of a device for extracting clove bud oil.
In the figure: 1-electric heating sleeve, 2-round bottom flask, 3-oil-water separator, 31-oil collecting pipe, 32-valve, 4-condensing pipe, 41-water inlet and 42-water outlet.
Detailed Description
The invention provides an extraction method of clove bud oil for cigarettes, which comprises the following steps:
a) Extracting and collecting flos Caryophylli bud in an extraction device to obtain a collecting solution of oil-water mixture;
b) Mixing the collected liquid with water for demulsification, and then separating to obtain clove bud oil;
the extraction device includes:
the container is used for containing the clove buds and the extracting solvent, and a heating device is arranged below the container;
the container mouth is connected with a three-way bent angle, a main pipe and a branch pipe of the three-way bent angle are respectively connected with a first condensing pipe and a second condensing pipe, and a collecting container is arranged at the outlet position of the second condensing pipe.
Firstly, preparing an extraction device, referring to fig. 1, fig. 1 is a schematic structural diagram of the extraction device of the clove bud oil for cigarettes; in the figure: 1-electric heating sleeve, 2-round bottom flask, 3-three-way bent angle, 4-condenser tube, 41-water inlet, 42-water outlet, 5-condenser tube, 51-water inlet, 52-water outlet, 6-oil-water mixture drop, 7-beaker, 8-magnetic stirrer and 9-magnetic stirrer.
Wherein, the container for holding the clove buds and the extracting solvent is preferably a round-bottom flask, and the mass of the clove bud raw material is not more than one tenth of the water mass of the maximum capacity of the round-bottom flask. In the invention, the volume of the round-bottomed flask is selected from one of 2000mL, 3000mL and 5000 mL.
A heating device is arranged below the container. The specific kind of the heating device is not particularly limited, and the heating device known to those skilled in the art may be used. In the present invention, an electric heating jacket is preferably used.
The container mouth is connected with a three-way bent angle, a main pipe and a branch pipe of the three-way bent angle are respectively connected with a first condensing pipe and a second condensing pipe, and a collecting container is arranged at the outlet position of the second condensing pipe.
The condensation is bidirectional condensation of oil-water mixed vapor, and comprises vertical reflux condensation (i.e. condensation through a condenser connected with a main pipe) and horizontal recovery condensation (i.e. condensation through a condenser connected with a branch pipe).
The liquid drops formed by condensation in the vertical direction reflux condensation is returned to the round bottom flask in the condensation pipe 4, the liquid drops formed by condensation in the horizontal direction condensation in the condensation pipe 5 are returned to the beaker 7, and the collection of clove bud oil is performed and meanwhile demulsification is also performed.
There is a collection container, preferably a beaker, provided at the outlet of the second condenser tube, and the present invention is not particularly limited to the collection container.
In the invention, the collecting container is arranged on a magnetic stirrer, and a magnetic stirrer is arranged in the collecting container.
After the extraction device is prepared, the clove buds and the extraction solvent are placed in the extraction device, then a condensation pipe and condensed water are connected, and a heating device is turned on to start heating extraction.
Wherein the extraction solvent is selected from water, and the mass ratio of the clove buds to the extraction solvent is 1: (5-9), preferably 1:5, 1:6, 1:7, 1:8, 1:9, or 1: any value between (5) and (9).
The extraction temperature is 100 ℃ and the time is 4-8 hours, preferably 4, 5, 6, 7, 8, or any value between 4 and 8.
The liquid drops formed by condensation in the vertical direction reflux condensation is returned to the round bottom flask in the condensation pipe 4, and the liquid drops formed by condensation in the horizontal direction condensation in the condensation pipe 5 are returned to the collection container 7, so that the clove bud oil is collected and demulsification is performed.
The collecting container is filled with water; and the collected liquid is collected, meanwhile, demulsification is carried out, and water is additionally added into a collecting container during demulsification. The water contained in the collecting container and the water added into the collecting container are used for demulsification of the collecting liquid of the oil-water mixture.
The mass ratio of the collecting liquid to the water is 1: (2-3), preferably 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, 1:3, or 1: any value between (2) and (3).
In the demulsification, the collected liquid and water are stirred at a rotation speed of 10 to 100rpm, preferably 10, 30, 50, 70, 90, 100, or any value between 10 and 100rpm for 1 to 10 minutes.
After the completion of stirring, the mixture is allowed to stand for a period of preferably 10 to 30 minutes, more preferably 10, 15, 20, 25, 30, or any value between 10 and 30 minutes. After standing, oil-water separation and delamination are achieved.
In the invention, oil-water separation is to separate the layered clove bud oil from water through a separating funnel. And after the separation is finished, obtaining the crude oil of the clove bud oil.
Finally, removing the moisture in the crude oil, wherein the moisture-removing substance is anhydrous sodium sulfate. The mass of the anhydrous sodium sulfate is 5-40% of the mass of the crude oil of the clove bud oil.
The invention also provides the clove bud oil extracted by the extraction method, and the yield of the clove bud oil is more than or equal to 9.9%.
According to the invention, the oil-water mixture of the clove bud oil is obtained by adopting a specific extraction device, and then the oil-water mixture is demulsified by adopting a specific demulsification method, so that the extraction method is simple and easy to implement, the applicability is strong, and the extraction efficiency of the essential oil is obviously improved.
In order to further understand the present invention, the following examples are provided to illustrate the bud oil of clove for cigarettes and the extraction method thereof, and the scope of the present invention is not limited by the following examples.
The extraction apparatus used in examples 1 to 4 and comparative example 3 below includes:
a round-bottom flask used for containing flos Caryophylli buds and extracting solvent, wherein an electric heating sleeve is arranged below the round-bottom flask;
the bottle mouth of the round bottom flask is connected with a three-way bent angle, a main pipe (vertical reflux condensation) and a branch pipe (horizontal reflux condensation) of the three-way bent angle are respectively connected with a first condenser pipe and a second condenser pipe, a beaker for collecting an oil-water mixture is arranged at the outlet position of the second condenser pipe, the beaker is arranged on a magnetic stirrer, and a magnetic stirrer is arranged in the beaker.
The extraction apparatus (structure see fig. 2) used in comparative examples 1 and 2 includes:
a round-bottom flask used for containing flos Caryophylli buds and extracting solvent, wherein an electric heating sleeve is arranged below the round-bottom flask; an oil-water separator is connected to the bottleneck of the round bottom flask, and the upper port of the oil-water separator is connected with a condensing tube.
Example 1:
(1) Weighing 400g of clove bud raw materials in a malaysia production place, and placing the clove buds in a 5000mL round-bottom flask;
(2) Adding 3500g deionized water into a round-bottom flask, heating at 100 ℃ by an electric heating sleeve, forming oil-water mixed vapor after 40min, and starting to reflux liquid drops;
(3) Condensing the oil-water mixed vapor into liquid drops after passing through a three-way bent angle and a horizontal condensing pipe, collecting the liquid drops into a beaker filled with 3000mL of deionized water, and demulsifying the liquid drops while collecting the liquid drops for about 4.5 hours to obtain 2345g of oil-water mixture;
(4) Complete demulsification of the oil-water mixture in the beaker: adding 2000g deionized water, stirring at 20rpm for 5min, standing for 15min, separating flos Caryophylli bud oil from water, layering, wherein the upper layer is water, and the lower layer is flos Caryophylli bud oil;
(5) Separating the layered clove bud oil from water by using a separating funnel to obtain 45.4g of crude clove bud oil;
(6) 15g anhydrous sodium sulfate is added into the crude oil of the clove bud oil, and the moisture in the essential oil is removed, so that 41.1g of the clove bud oil is obtained, and the oil yield of the clove bud oil is 10.27%.
Example 2:
(1) Weighing 500g of clove bud raw material in the Guangdong production area of China, and placing the clove buds into a 5000mL round bottom flask;
(2) Adding 4000g of deionized water into a round-bottom flask, heating at 100 ℃ by an electric heating sleeve, forming oil-water mixed vapor after 45min, and starting to reflux liquid drops;
(3) The oil-water mixed vapor is cooled into liquid drops after passing through a three-way bent angle and a horizontal condensing pipe, and is collected into a beaker filled with 3000mL deionized water, demulsified while being collected, and 2956g of oil-water mixture is obtained after about 5.1 h;
(4) The oil-water mixture in beaker 7 is completely demulsified: adding 3000g deionized water, stirring at 40rpm for 6min, standing for 10min, completely separating and layering flos Caryophylli bud oil and water, and collecting flos Caryophylli bud oil as lower layer;
(5) Separating the layered clove bud oil from water by using a separating funnel to obtain 64.7g of crude clove bud oil;
(6) 21g anhydrous sodium sulfate is added into the crude oil of the clove bud oil, and the moisture in the essential oil is removed, so that 61.7g of the clove bud oil is obtained, and the oil yield of the clove bud oil is 12.34%.
Example 3:
(1) Weighing 450g of clove bud raw material of a tank Sanya origin, and placing clove buds into a 5000mL round bottom flask;
(2) Adding 3600g of deionized water into a round-bottom flask, heating at 100 ℃ for 43min to form oil-water mixed vapor, and starting to reflux liquid drops;
(3) The oil-water mixed vapor is cooled into liquid drops after passing through a three-way bent angle, a horizontal condensing pipe and the bent angle, and is collected into a beaker filled with 4000mL of deionized water, demulsification is carried out while collection, and then 2711g of oil-water mixture is obtained about 4.8 h;
(4) The oil-water mixture in beaker 7 is completely demulsified: adding 2000g deionized water, stirring at 30rpm for 5min, standing for 15min, separating flos Caryophylli bud oil from water, and layering to obtain flos Caryophylli bud oil as the lower layer;
(5) Separating the layered clove bud oil from water by using a separating funnel to obtain 53.9g of crude clove bud oil;
(6) Adding 16g anhydrous sodium sulfate into crude oil of flos Caryophylli bud oil, and removing water in essential oil to obtain flos Caryophylli bud oil 50.5g with oil yield of 11.22%.
Example 4:
(1) Weighing 400g of clove bud raw materials of a production place of Hainan island in China, and placing the clove buds into a 5000mL round-bottom flask;
(2) Adding 3500g deionized water into a round-bottom flask, heating at 100 ℃ by utilizing an electric heating sleeve, forming oil-water mixed vapor after 41min, and starting liquid drop reflux;
(3) The oil-water mixed vapor is cooled into liquid drops after passing through a three-way bent angle and a horizontal condensing pipe, and is collected into a beaker filled with 5000mL of deionized water for about 4.4 hours, thus 2401g of oil-water mixture is obtained;
(4) Completely demulsifying the oil-water mixture in the beaker 7, adding 1000g of deionized water, stirring at 60rpm for 5min, standing for 15min, separating and layering the clove bud oil and water, wherein the lower layer is the clove bud oil;
(5) Separating the layered clove bud oil from water by using a separating funnel to obtain 43.6g of crude clove bud oil;
(6) 17g of anhydrous sodium sulfate is added into the crude oil of the clove bud oil, and the moisture in the essential oil is removed, so that 39.6g of the clove bud oil is obtained, and the oil yield of the clove bud oil is 9.9%.
Comparative example 1:
the extraction of clove bud oil was performed according to example 2 using the extraction method of a conventional oil-water separator device (structure see figure 2),
(1) Weighing 500g of clove bud raw material in the Guangdong production area of China, and placing the clove buds into a 5000mL round bottom flask;
(2) Adding 4000g of deionized water into a round-bottom flask, heating at 100 ℃ by an electric heating sleeve, forming oil-water mixed vapor after 45min, and starting to reflux liquid drops;
(3) Collecting the oil-water mixture of the oil collecting pipe in the oil-water separator for about 4.8 hours for multiple times to obtain 571g of emulsified oil-water mixture;
(4) Separating oil-water mixture, freezing at 4deg.C for 14 hr, separating oil from flos Caryophylli bud, and placing oil of flos Caryophylli bud on bottom layer;
(5) Separating the separated clove bud oil from water by using a separating funnel to obtain 5.2g of crude clove bud oil;
(6) 2g anhydrous sodium sulfate is added into the crude oil of the clove bud oil, and the moisture in the essential oil is removed, so that 4.6g of the clove bud oil is obtained, and the oil yield of the clove bud oil is 0.92%.
Comparative example 2:
the extraction of clove bud oil was performed according to example 2 using the extraction method of a conventional oil-water separator device (structure see figure 2),
(1) Weighing 500g of clove bud raw material in the Guangdong production area of China, and placing the clove buds into a 5000mL round bottom flask;
(2) Adding 3500g deionized water into a round-bottom flask, heating at 100 ℃ by an electric heating sleeve, forming oil-water mixed vapor after 40min, and starting to reflux liquid drops;
(3) Collecting oil-water mixture of an oil collecting pipe in the oil-water separator for about 4.9 hours to obtain 579g of emulsified oil-water mixture;
(4) Demulsification is carried out on the oil-water mixture, 1400g of deionized water is added, stirring is carried out for 5min at 70rpm, after standing for 14min, the clove bud oil is separated from water and layered, and the lower layer is the clove bud oil;
(5) Separating the separated clove bud oil from water by using a separating funnel to obtain 8.5g of clove bud oil crude oil;
(6) 2.5g anhydrous sodium sulfate is added into the crude oil of the clove bud oil, and the moisture in the essential oil is removed to obtain 8.2g of the clove bud oil, and the oil yield of the clove bud oil is 1.64%.
Comparative example 3:
according to the method and apparatus of example 2, extraction of clove bud oil was performed by changing only the frozen demulsification method,
(1) Weighing 500g of clove bud raw material in the Guangdong production area of China, and placing the clove buds into a 5000mL round bottom flask;
(2) Adding 4000g of deionized water into a round-bottom flask, heating at 100 ℃ by an electric heating sleeve, forming oil-water mixed vapor after 45min, and starting to reflux liquid drops;
(3) The oil-water mixed vapor is cooled into liquid drops after passing through a three-way bent angle and a horizontal condensing pipe, and is collected into a beaker filled with 3000mL deionized water, demulsified while being collected, and 2962g of oil-water mixture is obtained after about 5.3 h;
(4) Separating oil-water mixture, freezing at 4deg.C for 15 hr, separating oil from flos Caryophylli bud, and placing oil of flos Caryophylli bud on bottom layer;
(5) Separating the layered clove bud oil from water by using a separating funnel to obtain 41.3g of crude clove bud oil;
(6) 15g anhydrous sodium sulfate is added into the crude oil of the clove bud oil, and the moisture in the essential oil is removed, so that 36.7g of the clove bud oil is obtained, and the oil yield of the clove bud oil is 7.34%.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (6)
1. The extraction method of the clove bud oil for the cigarettes is characterized by comprising the following steps of:
the extraction device comprises:
the container is used for containing the clove buds and the extracting solvent, and a heating device is arranged below the container;
a three-way bent angle is connected at the container mouth, a main pipe and a branch pipe of the three-way bent angle are respectively connected with a first condensing pipe and a second condensing pipe, a collecting container is arranged at the outlet position of the second condensing pipe;
(1) Placing flos Caryophylli bud in a container of an extraction device;
(2) Adding water into the container for extraction to form oil-water mixed vapor, and starting the liquid drops to flow back;
(3) Condensing the oil-water mixed vapor into liquid drops after passing through a tee bend bent angle and a second condensing pipe, collecting the liquid drops in a collecting container containing water, and demulsifying while collecting to obtain an oil-water mixture;
(4) Adding water into the oil-water mixture for stirring, completely demulsifying the oil-water mixture in the collecting container, standing, separating the oil from water of the clove bud, layering, wherein the upper layer is water, and the lower layer is the oil of the clove bud;
(5) Separating the layered clove bud oil from water to obtain clove bud oil;
the water contained in the collecting container and the water added into the collecting container are used for demulsification of the collecting liquid of the oil-water mixture;
the mass ratio of the collecting liquid to the water is 1: (2-3), wherein the mass of water is the total amount of water contained in the collection container and water additionally added to the collection container.
2. The extraction method according to claim 1, wherein the extraction solvent is selected from water, and the mass ratio of the clove bud to the extraction solvent is 1: (5-9).
3. The extraction method according to claim 1, wherein the extraction temperature is 100 ℃ and the extraction time is 4-8 hours.
4. The method of extraction according to claim 1, wherein the container for containing clove bud oil and extraction solvent is selected from a round-bottom flask having a volume selected from one of 2000mL, 3000mL, 5000 mL.
5. The extraction method according to claim 1, wherein the stirring speed is 10-100 rpm and the stirring time is 1-10 min when demulsification is performed.
6. The method according to claim 1, further comprising a step of removing moisture after the separation, wherein the moisture-removing substance is anhydrous sodium sulfate.
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