CN114989896A - 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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- CN114989896A CN114989896A CN202210853616.8A CN202210853616A CN114989896A CN 114989896 A CN114989896 A CN 114989896A CN 202210853616 A CN202210853616 A CN 202210853616A CN 114989896 A CN114989896 A CN 114989896A
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- 239000001902 eugenia caryophyllata l. bud oil Substances 0.000 title claims abstract description 74
- 238000000605 extraction Methods 0.000 title claims abstract description 74
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 111
- 238000009833 condensation Methods 0.000 claims abstract description 39
- 230000005494 condensation Effects 0.000 claims abstract description 39
- 239000007788 liquid Substances 0.000 claims abstract description 35
- 235000019476 oil-water mixture Nutrition 0.000 claims abstract description 30
- 239000001353 eugenia caryophyllata l. Substances 0.000 claims abstract description 24
- 241000628997 Flos Species 0.000 claims abstract description 21
- 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 14
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 12
- 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 5
- 235000016639 Syzygium aromaticum Nutrition 0.000 claims description 5
- 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
- 239000003921 oil Substances 0.000 description 34
- 235000019198 oils Nutrition 0.000 description 33
- 239000008367 deionised water Substances 0.000 description 17
- 229910021641 deionized water Inorganic materials 0.000 description 17
- 238000010992 reflux Methods 0.000 description 12
- 238000005485 electric heating Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 239000010779 crude oil Substances 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 238000001816 cooling Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000839 emulsion Substances 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 239000000295 fuel oil 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
- 238000005034 decoration Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
Images
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
Abstract
The invention provides an extraction method of clove bud oil for cigarettes, which comprises the following steps: A) extracting and collecting flos Caryophylli buds in an extraction device to obtain oil-water mixture collecting solution; B) mixing the collected liquid with water to perform demulsification, and then separating to obtain clove bud oil; the extraction device includes: the device comprises a container for containing clove buds and an extraction solvent, wherein a heating device is arranged below the container; the container opening is connected with a three-way bend, a main pipe of the three-way bend and branch pipes are respectively connected with a first condensation pipe and a second condensation pipe, and a collection container is arranged at the outlet position of the second condensation pipe. According to the invention, the oil-water mixture of the clove bud oil is obtained by adopting the specific extraction device, and then the oil-water mixture is demulsified by adopting the 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 flavors, 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 plant essential oil, an oil-water separator device is generally adopted for extracting the natural essential oil. Natural essential oils are further divided into light oils and heavy oils, namely: light oil is lighter than water, heavy oil is heavier than water, and most of the essential oil belongs to light oil. The clove bud oil belongs to heavy oil, and is extracted by a steam distillation method at the lower layer of an oil collecting pipe of an oil-water separator, and the upper layer is water.
In the process of extracting essential oil from clove bud oil by using an oil-water separator in a steam distillation method, oil-water mixed steam formed by the clove bud oil and water is condensed to easily form emulsion to form a stable milky oil-water mixture, oil and water cannot be separated and layered, a series of processes of repeated reflux, heating, steam and condensation are performed, and an 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 clove bud is generally 10-20%, and the yield of clove bud oil extracted by a traditional oil-water separator by adopting a steam distillation method is about 1%, which is far lower than the oil content of clove bud. Therefore, a method for extracting clove bud oil is urgently needed at present, the yield of essential oil is improved, and the requirement of production on 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 a method for extracting clove bud oil for cigarettes, which comprises the following steps:
A) extracting and collecting flos Caryophylli buds in an extraction device to obtain oil-water mixture collecting solution;
B) mixing the collected liquid with water to perform demulsification, and then separating to obtain clove bud oil;
the extraction device comprises:
the device comprises a container for containing clove buds and an extraction solvent, wherein a heating device is arranged below the container;
the container opening is connected with a tee bend, a main pipe of the tee bend and branch pipes are respectively connected with a first condensation pipe and a second condensation pipe, and a collection container is arranged at the outlet of the second condensation 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 h.
Preferably, the container for containing the clove bud oil and the 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 step B), the mass ratio of the collection liquid to water is 1: (2-3).
Preferably, the collection container contains water;
and (3) demulsifying while collecting the collected liquid, wherein water is additionally added into the collecting container during demulsification.
Preferably, when demulsification is carried out, the collected liquid and water need to be stirred, the rotating speed of stirring is 10-100 rpm, and the stirring time is 1-10 min.
Preferably, the step B) further comprises a step of removing moisture after the separation, wherein the moisture-removing substance is anhydrous sodium sulfate.
The invention also provides clove bud oil extracted by the extraction method, wherein the yield of the clove bud oil is more than or equal to 9.9%.
Compared with the prior art, the invention provides an extraction method of clove bud oil for cigarettes, which comprises the following steps: A) extracting and collecting flos Caryophylli buds in an extraction device to obtain oil-water mixture collecting solution; B) mixing the collected liquid with water for demulsification, and then separating to obtain clove bud oil; the extraction device comprises: the device comprises a container for containing clove buds and an extraction solvent, wherein a heating device is arranged below the container; the container opening is connected with a three-way bend, a main pipe of the three-way bend and branch pipes are respectively connected with a first condensation pipe and a second condensation pipe, and a collection container is arranged at the outlet position of the second condensation pipe. According to the invention, the oil-water mixture of the clove bud oil is obtained by adopting the specific extraction device, and then the oil-water mixture is demulsified by adopting the 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 for clove bud oil for cigarettes provided by the invention;
in the figure: 1-an electric heating jacket, 2-a round bottom flask, 3-a three-way bend, 4-a condenser pipe, 41-a water inlet, 42-a water outlet, 5-a condenser pipe, 51-a water inlet, 52-a water outlet, 6-oil-water mixture drops, 7-a beaker, 8-a magnetic stirrer and 9-a magnetic stirrer;
fig. 2 is a schematic structural diagram of an extraction device of clove bud oil of the prior art and comparative examples 1 and 2.
In the figure: 1-electric jacket, 2-round flask, 3-oil-water separator, 31-oil collecting pipe, 32-valve, 4-condenser pipe, 41-water inlet, 42-water outlet.
Detailed Description
The invention provides a method for extracting clove bud oil for cigarettes, which comprises the following steps:
A) extracting and collecting flos Caryophylli buds in an extraction device to obtain oil-water mixture collecting solution;
B) mixing the collected liquid with water to perform demulsification, and then separating to obtain clove bud oil;
the extraction device includes:
the device comprises a container for containing clove buds and an extraction solvent, wherein a heating device is arranged below the container;
the container opening is connected with a three-way bend, a main pipe of the three-way bend and branch pipes are respectively connected with a first condensation pipe and a second condensation pipe, and a collection container is arranged at the outlet position of the second condensation pipe.
Firstly, preparing an extraction device, and referring to fig. 1, fig. 1 is a schematic structural diagram of the extraction device for clove bud oil for cigarettes provided by the invention; in the figure: 1-electric heating jacket, 2-round bottom flask, 3-three-way bend angle, 4-condenser pipe, 41-water inlet, 42-water outlet, 5-condenser pipe, 51-water inlet, 52-water outlet, 6-oil-water mixture drop, 7-beaker, 8-magnetic stirrer and 9-magnetic stirrer.
The container for containing the clove buds and the extraction solvent is preferably a round-bottom flask, and the mass of the raw material of the clove buds is not more than one tenth of the mass of water in the maximum capacity of the round-bottom flask. In the present invention, the volume of the round-bottom flask is selected from 2000mL, 3000mL, 5000 mL.
And a heating device is arranged below the container. The present invention is not particularly limited to the specific type of the heating device, and a 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 opening is connected with a three-way bend, a main pipe of the three-way bend and branch pipes are respectively connected with a first condensation pipe and a second condensation pipe, and a collection container is arranged at the outlet position of the second condensation pipe.
The condensation is the two-way condensation of oil-water mixed steam, and comprises vertical direction backflow condensation (namely condensation through a condenser connected with a main pipe) and horizontal direction recovery condensation (namely condensation through a condenser connected with a branch pipe).
The reflux condensation in the vertical direction is that liquid drops formed by condensation in the condensation pipe 4 reflux into the round-bottom flask, the liquid drops formed by condensation in the condensation pipe 5 in the horizontal direction enter the beaker 7, and the clove bud oil is collected and simultaneously emulsion breaking is carried out.
A collection container is provided at the outlet of the second condensation pipe, and the collection container is not particularly limited in the present invention, and is preferably a beaker.
In the invention, the collecting container is arranged on a magnetic stirrer, and a magnetic stirrer is arranged in the collecting container.
After preparing the extraction device, placing the clove buds and the extraction solvent in the extraction device, connecting a condensation pipe and condensed water, opening a heating device, and starting 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 to 9), preferably 1:5, 1:6, 1:7, 1:8, 1:9, or 1: (5-9).
The extraction temperature is 100 ℃, the extraction time is 4-8 h, and the extraction time is preferably 4, 5, 6, 7, 8 or any value between 4 and 8.
The reflux condensation in the vertical direction is that liquid drops formed by condensation in the condensation pipe 4 reflux into the round-bottom flask, the liquid drops formed by condensation in the condensation pipe 5 in the horizontal direction enter the collection container 7, and the clove bud oil is collected and simultaneously emulsion breaking is carried out.
The collecting container is filled with water; and (3) demulsifying while collecting the collected liquid, wherein water is additionally added into the collecting container during demulsification. Wherein the water contained in the collecting container and the additional water added into the collecting container are both used for demulsifying the collecting fluid of the oil-water mixture.
The mass ratio of the collecting liquid to the water is 1: (2 to 3), preferably 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, 1:3, or 1: (2-3) is arbitrary.
When demulsification is carried out, the collected liquid and water need to be stirred, the rotating speed of stirring is 10-100 rpm, preferably any value between 10, 30, 50, 70, 90 and 100 or 10-100 rpm, and the stirring time is 1-10 min.
And after stirring, standing for preferably 10-30 min, preferably 10, 15, 20, 25, 30 or any value between 10-30 min. After standing, oil-water separation and layering are achieved.
In the invention, oil-water separation is to separate the layered clove bud oil and water by a separating funnel. After the separation is finished, the crude oil of the clove bud oil is obtained.
Finally, removing water in the crude oil, wherein the water-removing substance is anhydrous sodium sulfate. The mass of the anhydrous sodium sulfate is 5-40% of that of the crude oil of the clove bud oil.
The invention also provides clove bud oil extracted by the extraction method, wherein 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 the specific extraction device, and then the oil-water mixture is demulsified by adopting the 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 clove bud oil for cigarette and the extraction method thereof, and the scope of the present invention is not limited by the following examples.
The extraction apparatus used in the following examples 1 to 4 and comparative example 3 included:
the round-bottom flask is used for containing clove buds and an extraction solvent, and an electric heating sleeve is arranged below the round-bottom flask;
be connected with the tee bend angle in round flask bottleneck department, the person in charge (vertical direction backward flow condensation) and branch pipe (horizontal direction backward flow condensation) punishment of tee bend angle do not are connected with first condenser pipe and second condenser pipe the exit position of second condenser pipe is provided with the beaker of collecting oil water mixture, and on magnetic stirrers was arranged in to the beaker, there was magnetic stirrers in the beaker.
The extraction apparatus used in comparative example 1 and comparative example 2 (structure see fig. 2) includes:
the round-bottom flask is used for containing clove buds and an extraction solvent, and an electric heating sleeve is arranged below the round-bottom flask; an oil-water separator is connected to the bottle mouth of the round-bottom flask, and a condenser pipe is connected to the upper port of the oil-water separator.
Example 1:
(1) weighing 400g of raw material of clove buds in Malaysia producing areas, and placing the clove buds into a 5000mL round-bottom flask;
(2) adding 3500g of deionized water into a round-bottom flask, heating by an electric heating jacket at 100 ℃, forming oil-water mixed steam after 40min, and starting reflux of liquid drops;
(3) condensing the oil-water mixed steam into liquid drops 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 while collecting for about 4.5 hours to obtain 2345g of an oil-water mixture;
(4) fully demulsifying the oil-water mixture in the beaker: adding 2000g of deionized water, stirring at 20rpm for 5min, standing for 15min, separating flos Caryophylli bud oil and water, and layering to obtain upper layer of water and lower layer of flos Caryophylli bud oil;
(5) separating the layered clove bud oil and water by using a separating funnel to obtain 45.4g of crude clove bud oil;
(6) adding 15g of anhydrous sodium sulfate into crude clove bud oil, and removing water in essential oil to obtain 41.1g of clove bud oil, wherein the oil yield of the clove bud oil is 10.27%.
Example 2:
(1) weighing 500g of raw material of clove buds from Guangdong origin in China, and placing the clove buds into a 5000mL round-bottom flask;
(2) adding 4000g of deionized water into a round-bottom flask, heating by an electric heating jacket at 100 ℃, forming oil-water mixed steam after 45min, and starting reflux of liquid drops;
(3) cooling the oil-water mixed steam into liquid drops after passing through a three-way bent angle and a horizontal condenser pipe, collecting the liquid drops into a beaker filled with 3000mL of deionized water, and demulsifying while collecting for about 5.1 hours to obtain 2956g of an oil-water mixture;
(4) and (3) completely demulsifying the oil-water mixture in the beaker 7: adding 3000g deionized water, stirring at 40rpm for 6min, standing for 10min to completely separate and layer flos Caryophylli bud oil and water, wherein the lower layer is flos Caryophylli bud oil;
(5) separating the layered clove bud oil and water by using a separating funnel to obtain 64.7g of crude clove bud oil;
(6) adding 21g of anhydrous sodium sulfate into crude clove bud oil, and removing water in essential oil to obtain 61.7g of clove bud oil, wherein the oil yield of the clove bud oil is 12.34%.
Example 3:
(1) weighing 450g of raw material of clove buds of a tanzania producing area, and placing the clove buds into a 5000mL round-bottom flask;
(2) adding 3600g of deionized water into a round-bottom flask, heating at 100 ℃, forming oil-water mixed steam after 43min, and starting liquid drop reflux;
(3) allowing the oil-water mixed steam to pass through a three-way bend, a horizontal condenser pipe and a bend angle, cooling the oil-water mixed steam into liquid drops, collecting the liquid drops into a beaker filled with 4000mL of deionized water, and demulsifying while collecting for about 4.8 hours to obtain 2711g of an oil-water mixture;
(4) and (3) completely demulsifying the oil-water mixture in the beaker 7: adding 2000g of deionized water, stirring at 30rpm for 5min, standing for 15min, separating flos Caryophylli bud oil and water, and layering to obtain lower layer flos Caryophylli bud oil;
(5) separating the layered clove bud oil and 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 from essential oil to obtain 50.5g flos Caryophylli bud oil with oil yield of 11.22%.
Example 4:
(1) weighing 400g of a clove bud raw material of a place where Hainan island is produced in China, and placing the clove bud in a 5000mL round-bottom flask;
(2) adding 3500g of deionized water into a round-bottom flask, heating at 100 ℃ by using an electrothermal sleeve, forming oil-water mixed steam after 41min, and starting liquid drop reflux;
(3) the oil-water mixed steam is cooled into liquid drops after passing through a three-way bent angle and a horizontal condensing tube, and the liquid drops are collected into a beaker filled with 5000mL of deionized water for about 4.4 hours to obtain 2401g of an oil-water mixture;
(4) completely demulsifying the oil-water mixture in the beaker 7, adding 1000g of deionized water, stirring at the rotating speed of 60rpm for 5min, standing for 15min, separating and layering clove bud oil and water, wherein the lower layer is the clove bud oil;
(5) separating the layered clove bud oil and water by using a separating funnel to obtain 43.6g of crude clove bud oil;
(6) adding 17g anhydrous sodium sulfate into crude oil of flos Caryophylli bud oil, and removing water from essential oil to obtain 39.6g flos Caryophylli bud oil with oil yield of 9.9%.
Comparative example 1:
the clove bud oil is extracted by the extraction method of the conventional oil-water separator device (the structure is shown in figure 2) according to the embodiment 2,
(1) weighing 500g of a raw material of clove buds produced in Guangdong province in China, and placing the clove buds into a 5000mL round-bottom flask;
(2) adding 4000g of deionized water into a round-bottom flask, heating by an electric heating jacket at 100 ℃, forming oil-water mixed steam after 45min, and starting reflux of liquid drops;
(3) collecting the oil-water mixture in an 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 the oil-water mixture, freezing at 4 deg.C for 14 hr to separate the clove bud oil and water, with the clove bud oil at the bottom layer;
(5) separating the separated clove bud oil and water by using a separating funnel to obtain 5.2g of crude clove bud oil;
(6) adding 2g anhydrous sodium sulfate into crude oil of flos Caryophylli bud oil, and removing water from essential oil to obtain 4.6g flos Caryophylli bud oil with oil yield of 0.92%.
Comparative example 2:
the clove bud oil is extracted by the extraction method of the conventional oil-water separator device (the structure is shown in figure 2) according to the embodiment 2,
(1) weighing 500g of raw material of clove buds from Guangdong origin in China, and placing the clove buds into a 5000mL round-bottom flask;
(2) adding 3500g of deionized water into a round-bottom flask, heating by an electric heating jacket at 100 ℃, forming oil-water mixed steam after 40min, and starting reflux of liquid drops;
(3) collecting the oil-water mixture in an oil collecting pipe in the oil-water separator for about 4.9 hours for multiple times to obtain 579g of emulsified oil-water mixture;
(4) demulsifying the oil-water mixture, adding 1400g of deionized water, stirring at 70rpm for 5min, standing for 14min, separating flos Caryophylli bud oil from water, and layering to obtain lower layer flos Caryophylli bud oil;
(5) separating the separated clove bud oil and water by using a separating funnel to obtain 8.5g of crude clove bud oil;
(6) adding 2.5g anhydrous sodium sulfate into crude oil of flos Caryophylli bud oil, and removing water from essential oil to obtain 8.2g flos Caryophylli bud oil with oil yield of 1.64%.
Comparative example 3:
according to the method and the device in the embodiment 2, the extraction of the clove bud oil is carried out only by changing the freezing demulsification method,
(1) weighing 500g of raw material of clove buds from Guangdong origin in China, and placing the clove buds into a 5000mL round-bottom flask;
(2) adding 4000g of deionized water into a round-bottom flask, heating by an electric heating jacket at 100 ℃, forming oil-water mixed steam after 45min, and starting reflux of liquid drops;
(3) cooling the oil-water mixed steam into liquid drops after passing through a three-way bent angle and a horizontal condenser pipe, collecting the liquid drops into a beaker filled with 3000mL of deionized water, and demulsifying while collecting for about 5.3 hours to obtain 2962g of an oil-water mixture;
(4) separating the oil-water mixture, freezing at 4 deg.C for 15 hr to separate the clove bud oil and water, with the clove bud oil at the bottom layer;
(5) separating the layered clove bud oil and water by using a separating funnel to obtain 41.3g of crude clove bud oil;
(6) adding 15g of anhydrous sodium sulfate into the crude clove bud oil, and removing water in the essential oil to obtain 36.7g of clove bud oil, wherein the oil yield of the clove bud oil is 7.34%.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. The method for extracting clove bud oil for cigarettes is characterized by comprising the following steps:
A) extracting and collecting flos Caryophylli buds in an extraction device to obtain oil-water mixture collecting solution;
B) mixing the collected liquid with water to perform demulsification, and then separating to obtain clove bud oil;
the extraction device comprises:
the device comprises a container for containing clove buds and an extraction solvent, wherein a heating device is arranged below the container;
the container opening is connected with a three-way bend, a main pipe of the three-way bend and branch pipes are respectively connected with a first condensation pipe and a second condensation pipe, and a collection container is arranged at the outlet position of the second condensation pipe.
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 h.
4. The extraction method as claimed in claim 1, wherein the container for containing clove bud oil and the extraction solvent is selected from round-bottomed flasks, and the volume of the round-bottomed flasks is selected from one of 2000mL, 3000mL and 5000 mL.
5. The extraction method according to claim 1, wherein in step B), the mass ratio of the collection liquid to water is 1: (2-3).
6. The extraction method according to claim 1, wherein the collection container contains water;
and (3) demulsifying while collecting the collected liquid, wherein water is additionally added into the collecting container during demulsification.
7. The extraction method according to claim 1, wherein the collection liquid and water are stirred during demulsification, wherein the stirring speed is 10-100 rpm, and the stirring time is 1-10 min.
8. The extraction method according to claim 1, wherein the step B) further comprises a step of removing moisture after the separation, wherein the moisture-removing substance is anhydrous sodium sulfate.
9. The clove bud oil extracted by the extraction method according to any one of claims 1 to 8, wherein the yield of the clove bud oil is more than or equal to 9.9%.
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| CN202210853616.8A CN114989896B (en) | 2022-07-11 | 2022-07-11 | Clove bud oil for cigarettes and extraction method thereof |
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| CN202210853616.8A CN114989896B (en) | 2022-07-11 | 2022-07-11 | Clove bud oil for cigarettes and extraction method thereof |
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Citations (10)
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