CN111617513A - Distillation and extraction device capable of automatically stopping and simultaneously extracting agilawood aroma components and method for extracting agilawood aroma components by distillation and extraction device - Google Patents
Distillation and extraction device capable of automatically stopping and simultaneously extracting agilawood aroma components and method for extracting agilawood aroma components by distillation and extraction device Download PDFInfo
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- CN111617513A CN111617513A CN202010568113.7A CN202010568113A CN111617513A CN 111617513 A CN111617513 A CN 111617513A CN 202010568113 A CN202010568113 A CN 202010568113A CN 111617513 A CN111617513 A CN 111617513A
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- 238000000605 extraction Methods 0.000 title claims abstract description 45
- 238000004821 distillation Methods 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims description 9
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 20
- 238000010992 reflux Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims description 6
- 229920006221 acetate fiber Polymers 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 235000013773 glyceryl triacetate Nutrition 0.000 claims description 3
- 239000001087 glyceryl triacetate Substances 0.000 claims description 3
- 229960002622 triacetin Drugs 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 229950005499 carbon tetrachloride Drugs 0.000 claims description 2
- 239000003205 fragrance Substances 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 2
- 238000002835 absorbance Methods 0.000 abstract description 3
- 230000007794 irritation Effects 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract 1
- 238000005457 optimization Methods 0.000 abstract 1
- 239000000779 smoke Substances 0.000 abstract 1
- 238000002474 experimental method Methods 0.000 description 9
- 230000004044 response Effects 0.000 description 6
- 239000004973 liquid crystal related substance Substances 0.000 description 5
- 238000012544 monitoring process Methods 0.000 description 4
- 239000012074 organic phase Substances 0.000 description 4
- 239000000523 sample Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000000944 Soxhlet extraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- 229930014626 natural product Natural products 0.000 description 2
- 238000012803 optimization experiment Methods 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 230000000391 smoking effect Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 241001533085 Aquilaria sinensis Species 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000013473 artificial intelligence Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0207—Control systems
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/04—Solvent extraction of solutions which are liquid
- B01D11/0484—Controlling means
-
- 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
- B01D3/40—Extractive distillation
-
- 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
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Wood Science & Technology (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Automation & Control Theory (AREA)
- Extraction Or Liquid Replacement (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a simultaneous distillation and extraction device capable of automatically stopping, which comprises a simultaneous distillation extractor (1), a heater (4), a chip controller (3) and an ultraviolet sensor (2), wherein a reflux capillary tube (11) is arranged in the simultaneous distillation extractor (1); the ultraviolet sensor (2) is positioned at the reflux capillary (11); the chip controller (3) can receive the signal of the ultraviolet sensor (2) and display the value detected by the ultraviolet sensor (2) in real time; a target value is set on the chip controller (3), and when the value detected by the ultraviolet sensor (2) is lower than the target value, the chip controller (3) controls the heater (4) to stop heating. The extracted agilawood extract is added into the cigarette filter stick, so that the aroma quality and the aroma quantity of smoke are effectively improved, and the irritation is reduced. The device can monitor the ultraviolet absorbance of the extraction liquid in real time, master the extraction degree of the target object in real time, avoid the optimization of extraction time, save experimental time and save manpower.
Description
Technical Field
The invention belongs to the technical field of extraction, and particularly relates to a distillation and extraction device capable of automatically stopping and a method for extracting agilawood fragrance components.
Background
The simultaneous distillation and extraction is realized by heating the sample solution and the organic phase simultaneously to generate steam. The water vapor brings the volatile or semi-volatile components in the sample to the condenser tube, meets with the organic phase vapor, and is condensed and reflows to the capillary tube at the lower end to complete phase separation. The organic phase with the extracted aroma components flows back to the organic phase bottle. The method has high extraction efficiency for volatile components.
However, the simultaneous distillation and extraction apparatuses commonly used in laboratories have certain disadvantages. When the Soxhlet extraction is carried out on a sample, the extraction condition is difficult to monitor in real time, in addition, the extraction degree of the sample is not known, the extraction is not stopped at any time, and the optimal experimental time can be obtained only through a series of time optimization experiments.
With the rapid development of science and technology, artificial intelligence gradually enters daily life. Therefore, the distillation and extraction device commonly used in the laboratory needs to be improved, intelligent equipment is developed, the experimental time is saved, and the labor is saved.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention aims to provide a simultaneous distillation and extraction device capable of automatically stopping; on the other hand, the application of the device capable of automatically stopping and simultaneously distilling and extracting in the extraction of natural products such as agilawood is provided.
The invention provides a simultaneous distillation extraction device capable of automatically stopping, which comprises a simultaneous distillation extractor 1, a heater 4, a chip controller 3 and an ultraviolet sensor 2, wherein a reflux capillary tube 11 is arranged in the simultaneous distillation extractor 1; the ultraviolet sensor 2 is positioned at the return capillary 11; the chip controller 3 is electrically connected with the ultraviolet sensor 2 and the heater 4 respectively.
Wherein, the ultraviolet sensor 2 can be a micro ultraviolet sensor, which is clamped at the reflux capillary 11 to facilitate the disassembly and replacement of the distillation extractor 1.
Preferably, the method for automatically stopping the distillation and extraction device at the same time comprises the following steps: the chip controller 3 can receive the signal of the ultraviolet sensor 2 and display the value detected by the ultraviolet sensor 2 in real time; a target value (for example, 450mAu) is set by the chip controller 3, and when the value detected by the ultraviolet sensor 2 is lower than the target value (450mAu), the chip controller 3 controls the heater 4 to stop heating.
Preferably, the chip controller 3 may be located inside the heater 4, that is, the heater 4 may be a heater with a smart chip, and may be a magnetic stirring heater with a smart chip, which has a liquid crystal display, and displays the value detected by the ultraviolet sensor 2 in real time through the liquid crystal display of the heater 4.
The second aspect of the invention provides an application of the device capable of automatically stopping and simultaneously distilling and extracting in extraction of natural products such as agilawood.
Extracting the agilawood by using an extraction solvent, setting a target value of 450mAU through the chip controller 3, and controlling the heater 4 to stop heating by the chip controller 3 when the value detected by the ultraviolet sensor 2 is lower than the target value to obtain the agilawood extract.
Preferably, the extraction solvent is one or more selected from petroleum ether, n-hexane, cyclohexane, chloroform, tetrachloromethane, dichloromethane and the like. The specific extraction experimental steps are as follows:
20g of agilawood was sliced and placed in a simultaneous distillation extractor, 350mL of water was added, 50mL of dichloromethane was added to the other bottle, and heating was stopped when the uv detector signal was set below 450mAU after the solvent started to reflux. The monitoring spectrum during the extraction experiment is shown in figure 2. At the beginning of heating, the solvent did not begin to reflux and there was no signal response. When the extraction solvent reflows, the micro ultraviolet sensor detects signal fluctuation. When the experiment is carried out for 3h, the extraction work is basically finished, the signal response is reduced, and when the signal response is lower than a set value, the system stops working.
Dissolving the agilawood extract in glyceryl triacetate to prepare 1-8% solution, adding the solution into acetate fiber tows according to 1-5% of the weight of the acetate fiber tows, and preparing the cigarette filter stick for cigarettes. Wherein the acetate fiber tows can be replaced by other raw materials of the cigarette filter stick.
Sensory evaluation personnel evaluate the cigarettes of the cigarette filter rods added with the agilawood extract and the cigarettes of the cigarette filter rods not added with the agilawood extract, and the results show that the cigarettes of the cigarette filter rods added with the agilawood extract prepared in the embodiment 1 have richer smoking feeling aroma, reduce offensive odor and reduce irritation.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the automatic-stopping simultaneous distillation and extraction device, the chip controller 3 can receive the signal of the ultraviolet sensor 2, display the value detected by the ultraviolet sensor 2 in real time, and monitor the progress of the Soxhlet extraction experiment in real time.
2. According to the automatic-stopping simultaneous distillation and extraction device, the chip controller 3 is used for setting the target value, when the value detected by the ultraviolet sensor 2 is lower than the target value, the chip controller 3 controls the heater 4 to stop heating, the experiment can be automatically stopped according to the extraction degree, and the device is a novel humanized experimental device, so that a series of time optimization experiments are avoided, and the experimental time and labor are saved.
Drawings
FIG. 1 is a schematic view of an automatic stop simultaneous distillation extractor according to the present invention;
FIG. 2 is a monitoring chart of the process of extracting Aquilaria sinensis by the simultaneous distillation and extraction device which can be automatically stopped in example 1;
the names of the reference numerals in the description of the drawings are: 1-simultaneous distillation extractor, 2-ultraviolet sensor, 3-chip controller, 4-heater, 11-reflux capillary.
Detailed Description
The invention is further illustrated by the following figures and examples, which are not intended to limit the invention in any way, and any alterations or substitutions based on the teachings of the invention are intended to fall within the scope of the invention.
Example 1
As shown in fig. 1, the automatic stop simultaneous distillation extraction device comprises a simultaneous distillation extractor 1, a heater 4, a chip controller 3, and an ultraviolet sensor 2, wherein the simultaneous distillation extractor 1 is provided with a reflux capillary 11; the ultraviolet sensor 2 is positioned at the return capillary 11; the chip controller 3 is electrically connected with the ultraviolet sensor 2 and the heater 4 respectively.
Wherein, the ultraviolet sensor 2 can be a micro ultraviolet sensor, which is clamped at the reflux capillary 11 to facilitate the disassembly and replacement of the distillation extractor 1.
The chip controller 3 is located inside the heater 4, that is, the heater 4 is a magnetic stirring heater with an intelligent chip, which has a liquid crystal display, the chip controller 3 can receive the signal of the ultraviolet sensor 2, and display the value detected by the ultraviolet sensor 2 in real time through the liquid crystal display of the heater 4 (the wavelength of ultraviolet light is selected, for example, 254nm, the maximum ultraviolet absorption signal is 1, and when there is no ultraviolet absorption signal, the signal value is 0 or a negative value), and in addition, the chip controller 3 sets a target value through the chip controller 3 by the heater 4, and when the value detected by the ultraviolet sensor 2 is lower than the target value, the chip controller 3 controls the heater 4 to stop heating.
When in work:
the substance to be extracted is placed in a simultaneous distillation extractor and the extraction solvent is poured into a bottom round bottom flask. The uv sensor was allowed to blank scan, and the environmental background was subtracted. After the solvent started to reflux, the target absorbance value (uv absorption spectrum) was set and the experiment was started. And monitoring the experiment progress according to the real-time measured value on the liquid crystal display screen of the heater. When the absorbance is lower than the set value, the experiment is automatically stopped.
The extraction device is used for extracting agilawood, and the specific operation steps are as follows: 20g of agilawood was sliced and placed in a simultaneous distillation extractor, 350mL of water was added, 50mL of dichloromethane was added to the other bottle, and heating was stopped when the uv detector signal was set below 450mAU after the solvent started to reflux. The monitoring spectrum during the extraction experiment is shown in fig. 2. At the beginning of the previous extraction, the solvent did not start refluxing and there was no signal response. When the extraction solvent reflows, the micro ultraviolet sensor detects signal fluctuation. When the experiment is carried out for 3h, the extraction work is basically finished, the signal response is reduced, and when the signal response is lower than the set value of 450mAU, the controller with the intelligent chip can automatically cut off the power supply of the heater.
Example 2
The agilawood extract extracted in the example 1 is dissolved in glyceryl triacetate to prepare a 5% solution, and the 5% solution is added into a cigarette filter stick according to 4% of the weight of the tows to prepare a cigarette. Sensory evaluation personnel evaluate the cigarettes of the cigarette filter rods added with the agilawood extract and the cigarettes of the cigarette filter rods not added with the agilawood extract, and the results show that the cigarettes of the cigarette filter rods added with the agilawood extract prepared in the embodiment 1 have richer smoking feeling aroma, reduce offensive odor and reduce irritation.
Claims (6)
1. The simultaneous distillation extraction device capable of automatically stopping is characterized by comprising a simultaneous distillation extractor (1), a heater (4), a chip controller (3) and an ultraviolet sensor (2), wherein a reflux capillary tube (11) is arranged in the simultaneous distillation extractor (1); the ultraviolet sensor (2) is positioned at the return capillary (11); the chip controller (3) is electrically connected with the ultraviolet sensor (2) and the heater (4) respectively.
2. The apparatus for simultaneous distillation and extraction capable of being automatically stopped according to claim 1, wherein the chip controller (3) can receive the signal of the ultraviolet sensor (2) and display the value detected by the ultraviolet sensor (2) in real time; a target value is set through the chip controller (3), and when the value detected by the ultraviolet sensor (2) is lower than the target value, the chip controller (3) controls the heater (4) to stop heating.
3. The apparatus for simultaneous distillation and extraction which can be automatically stopped according to claim 1, wherein the chip controller (3) is located inside the heater (4) and displays the value detected by the ultraviolet sensor (2) in real time through the heater (4).
4. A method for extracting agilawood fragrance components by using an automatic stop simultaneous distillation extraction device according to claim 2, wherein agilawood is extracted by using an extraction solvent, a target value is set by the chip controller (3), and when the value detected by the ultraviolet sensor (2) is lower than the target value, the chip controller (3) controls the heater (4) to stop heating to obtain agilawood extract.
5. The method as claimed in claim 4, wherein the extraction solvent is selected from one or more of petroleum ether, n-hexane, cyclohexane, chloroform, tetrachloromethane, dichloromethane, etc.
6. The application of the agilawood extract extracted by the method according to claim 4, wherein the agilawood extract is dissolved in glyceryl triacetate to prepare a 1-8% solution, and the solution is added into acetate fiber tows according to 1-5% of the weight of the acetate fiber tows to prepare a cigarette filter stick for cigarettes.
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| CN202010568113.7A CN111617513B (en) | 2020-06-19 | 2020-06-19 | Automatic-stopping simultaneous distillation extraction device and method for extracting agilawood aroma components by same |
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| CN202010568113.7A CN111617513B (en) | 2020-06-19 | 2020-06-19 | Automatic-stopping simultaneous distillation extraction device and method for extracting agilawood aroma components by same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113231118A (en) * | 2021-05-10 | 2021-08-10 | 海南医学院 | Fractionating device for organic chemistry experiment |
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