CN109280582A - A kind of high efficiency preparation method of the dried orange peel absolute oil for tobacco flavoring - Google Patents
A kind of high efficiency preparation method of the dried orange peel absolute oil for tobacco flavoring Download PDFInfo
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- CN109280582A CN109280582A CN201811098042.8A CN201811098042A CN109280582A CN 109280582 A CN109280582 A CN 109280582A CN 201811098042 A CN201811098042 A CN 201811098042A CN 109280582 A CN109280582 A CN 109280582A
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- Prior art keywords
- orange peel
- dried orange
- cigarette
- absolute oil
- tank
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- 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
Abstract
The invention discloses a kind of preparation methods of dried orange peel absolute oil, use following device: ultrasonic extraction tank (1)；Chromatographic column (2)；Air compressor machine (3)；Concentration tank (4)；Reversed resin column (5)；Condenser (6)；Vacuum pump (8)；Solvent recovery tank (7)；Step are as follows: 1. by dried orange peel raw material ultrasonic extraction；2. being purified by chromatographic column (2)；3. being concentrated；4. being purified by reversed resin column (5)；5. decompression arrives the dried orange peel absolute oil except ethyl alcohol.The device of the invention can efficiently be extracted and be purified to dried orange peel absolute oil, and obtained dried orange peel absolute oil is effectively promoted for changing cigarette, electronic cigarette or heating in the cigarette that do not burn and improves its and aspirate comfort.
Description
Technical field
The invention belongs to essence spice for cigarette preparation fields, and in particular to a kind of method for efficiently preparing dried orange peel absolute oil, with
And the dried orange peel absolute oil in cigarette, electronic cigarette and heats the application in the perfuming cigarette that do not burn.
Background technique
Perfuming cigarette is the core technology for strengthening cigarette style characteristic, especially in recent years, tobacco tar-reducing harm reduction work
It is lasting to promote, be gradually reduced releasing content of coke tar in cigarette, it is incident be cigarette flavor and it is jealous also decrease, this is often
The aesthetic quality for needing to ensure and promoted by blending means cigarette meets fragrance and jealous pursuit of the consumer to cigarette.
In addition, with electronic cigarette and the development for heating the new tobacco productses such as cigarette of not burning, the novel hot plant perfume ingredient in day is used for
Flavoring also has tight demand, substitutes the blending that synthetic perfume carries out tobacco product with natural this perfume ingredient, it is fragrant to improve product
Gas it is rich, demand of the consumer to different taste can be better met.
Dried orange peel is the mature pericarp of rutaceae orange and its variety, takes fruit, strips pericarp, dries in the shade or divulges information
It is dry.Pericarp is with Chen Zheliang, therefore named dried orange peel.Dried orange peel acrid flavour is bitter, warm-natured, has effects that warming stomach for dispelling cold, regulating qi-flowing for strengthening spleen, is suitble to stomach
The people of the symptoms such as portion's turgor, indigestion, loss of appetite, cough ant phlegm is edible.Dried orange peel contains volatile oil, hesperidine, vitamin
B, the ingredients such as C, the volatile oil contained by it have mild stimulation to gastrointestinal tract, can promote the secretion of digestive juice, and exclude in intestinal tube
Pneumatosis.Dried orange peel is conventional Chinese medicine simply, has effects that ventilate invigorating the spleen, eliminating dampness and eliminating phlegm, the greasy lasting of solution, stopping nausea and vomiting by lowering the adverse flow of QI.It is suitble to stomach
The people of the symptoms such as portion's turgor, indigestion, loss of appetite, cough ant phlegm is edible.
Extraction for effective component in dried orange peel has already appeared microwave abstracting, ultrasonic wave extraction, refluxing extraction of routine etc.
The yield of method, these method dried orange peel medicinal extract is higher, but the methods of ultrasonic wave extraction, microwave abstracting are easily destroyed the heat in dried orange peel
Quick property substance causes this perfume of dried orange peel impaired, reduces dried orange peel medicinal extract quality.In addition dried orange peel medicinal extract is vulnerable to medicinal extract state, dissolubility
Deng influence, be limited in scope in application process.At present for the extraction of effective component in dried orange peel, technique mainly mentioned with water, alcohol
It mentions, then the process being concentrated obtains.Time-consuming for these methods, and is easily destroyed the aroma component in dried orange peel, due to containing in dried orange peel
There are a large amount of pectin, cellulose etc., extract the flavonoids in dried orange peel, volatile oil cannot sufficiently, reduce quality.In addition existing
Some dried orange peel extracts are due to complicated component, in new tobacco products, influencing electronic cigarette and heating the cigarette that do not burn
Suction experience.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, devises a kind of side for using column chromatography and preparing dried orange peel absolute oil
Method.It is compared with traditional solvent extraction with molecularly distilled, production cost is significantly reduced, and the yield and quality of absolute oil obtain
It improves.Gained dried orange peel absolute oil is in addition to it can be used for traditional cigarette flavoring, it may also be used for new tobacco products (such as electronic cigarette or non-ignitable
Burn cigarette), effectively strengthen cigarette, electronic cigarette or the distinctive fragrant and sweet feature of dried orange peel for heating the cigarette that do not burn, improves the rich of fragrance
Richness and pleasant impression cover the miscellaneous gas of product suction, improve cigarette, electronic cigarette or the suction comfort for heating the cigarette that do not burn, mention
High flue gas quality gives consumer and preferably aspirates impression.
Technical scheme is as follows:
First aspect present invention discloses a kind of preparation method of dried orange peel absolute oil, uses following device:
Ultrasonic extraction tank 1, upper part have feed opening 11, and discharge port 14 is arranged at lower part, and filter screen is arranged at 14 top of discharge port
Plate 13；
Chromatographic column 2；
Air compressor machine 3；
Concentration tank 4；
Reversed resin column 5；
Condenser 6；
Vacuum pump 8；
Solvent recovery tank 7；
The connection type of each component is as follows:
The ultrasonic extraction tank 1 is connected to by its discharge port 14 with 2 upper inlet of chromatographic column, under the chromatographic column 2
Portion outlet is connected to 4 top of concentration tank；4 top of concentration tank is connected to the entrance of the condenser 6, the condenser 10
Upper end outlet is connected to the vacuum pump 8；Solvent recovery tank 7 described in the 10 lower end outlet of condenser；The air compressor machine 3 divides
It is not connected to 1 upper port of ultrasonic extraction tank and 4 upper port of the concentration tank；Described in 4 lower part outlet of the concentration tank connection
Reversed resin column 5；
Steps are as follows for the preparation method:
1. dried orange peel raw material is added in the ultrasonic extraction tank 1, feed opening and discharge port are sealed, dried orange peel raw material weight is added
The methyl acetate of 4-6 times of amount, the ultrasonic extraction 30-40min at 40-50 DEG C；
2. starting air compressor machine 3 after having extracted, to step, 1. the ultrasonic extraction tank 1 pressurizes, and allows extract liquor by going out
The filtering sieve plate 13 of material mouth 14 is entered in concentration tank 4 by chromatographic column 2；
3. concentration tank 4 is warming up to 75-85 DEG C, start vacuum pump 8 and condenser 6, extract liquor is concentrated under reduced pressure, until being evaporated
Methyl acetate obtains the paste of dried orange peel extraction；
4. the paste that the ethyl alcohol that 95wt% is added into concentration tank 4 obtains step 3. is completely dissolved, start air compressor machine 3
It pressurizes to concentration tank 4, liquid is allowed to pass through reversed resin column 5 completely；
5. 4. obtaining liquid to step is added 3-5 times of paste weight of the propylene glycol, it is evaporated under reduced pressure and removes ethyl alcohol, i.e.,
Obtain the dried orange peel absolute oil.
Preferably, the diameter of the chromatographic column 2: a height of 2:1, it is filled with silica gel particle and anhydrous sodium sulfate particle,
The partial size of the particle is 100-200 mesh；BOSHI reversed-phase resin is filled in the reversed resin column 5；The BOSHI reverse phase
The diameter of resin filling: a height of 1:2, partial size are 35~75 μm.
Preferably, the upper end of the ultrasonic extraction tank 1 is connected to the first pump B1；The upper end of the concentration tank 4 and the second pump
B2 connection；It is connected between each component by pipeline, has valve F on the pipeline.
Preferably, step further includes being carried out using methyl acetate to ultrasonic extraction tank 1 3. before the reduced pressure extract liquor
Then methyl acetate cleaning solution is entered 4 step of concentration tank by chromatographic column 2 by washing.
Preferably, step further includes the 1/4-5 using the paste weight before 5. the reduction vaporization removes ethyl alcohol
95wt% ethyl alcohol washs concentration tank 4, and ethanol washes are then carried out the decompression of step 5. by reversed resin column 5
Evaporating ethanol step.
Second aspect of the present invention discloses dried orange peel absolute oil made from the preparation method in cigarette, electronic cigarette or non-ignitable
Burn the purposes of flavoring in cigarette.
Illustrate the step of present invention produces dried orange peel absolute oil method with reference to the accompanying drawing, specific as follows:
A. the extraction of dried orange peel raw material
Extraction for fragrance component in dried orange peel raw material, common solvent have ethyl alcohol, petroleum ether, ethyl acetate etc., acetic acid
Ethyl ester polarity is moderate, can dissolve most fragrance component and its glycoside compounds, and the big saccharide compound of content is molten in dried orange peel
It is few out, it is ideal Extraction solvent, but ethyl acetate boiling point is high, up to 77.5 DEG C, energy consumption is high during sample concentration, and holds
Easily residual.Therefore, methyl acetate is used to replace ethyl acetate for Extraction solvent in the present invention, methyl acetate and ethyl acetate have
Very similar chemical property, but boiling point is only that 57.8 DEG C of energy consumptions that sample concentration is compared with ethyl acetate substantially reduce, and
Dissolvent residual will not be caused in the sample.
The dried orange peel raw material used is crushed to 15-20 mesh, shown in Fig. 1 using the dried orange peel for originating in Yunnan, dried orange peel sample drying
The feed opening 11 of thermostatic ultrasonic extractor 1 be added in ultrasonic extraction tank, seal feed opening and discharge port, the first pump of starting B1
The methyl acetate of 4-6 times of dried orange peel raw material weight is added, then the ultrasonic extraction 30-40min at 40-50 DEG C.Opening after having extracted
Valve F2 in Fig. 1, starting air compressor machine 3 pressurize to ultrasonic extraction tank 1, and dried orange peel extract is allowed to pass through the filtering on discharge port 14
Sieve plate 13 and the chromatographic column 2 for leading to the silica gel particle 22 with anhydrous sodium sulfate particle 21.
B. the purification of anhydrous sodium sulfate particle and silica gel particle composite chromatography column 2 to dried orange peel extract
Due to containing moisture in dried orange peel raw material, in dried orange peel absolute oil extraction process, the big polarity such as moisture and a small amount of carbohydrate at
Dividing can also be dissolved into dried orange peel extract.It is right using anhydrous sodium sulfate particle and silica gel particle composite chromatography column 2 in the present invention
The purification of extract liquor.
The diameter of chromatographic column 2: a height of 2:1, the size and dried orange peel sample of chromatographic column 2 feed intake flux matched, wherein silica gel particle
22 partial size is 100-200 mesh, and the loadings of silica gel particle 22 are the 1/50 of dried orange peel sample inventory, anhydrous sodium sulfate particle 21
Partial size is also 100-200 mesh, and the loadings of anhydrous sodium sulfate particle 21 are the 1/4 of silica gel.When extract liquor passes through chromatographic column 2,
Moisture in extract liquor is adsorbed and be removed by anhydrous sodium sulfate particle 21, and the big polar component such as sugar dissolved out on a small quantity is by silica gel
Grain 22 is adsorbed and is removed, and can reach the effect of extract liquor high-efficient purification by chromatographic column 2.By anhydrous sodium sulfate particle and silicon
The purified extract liquor of glue Particles dispersed chromatographic column is transferred in concentration tank 4.
C. the concentration of extract liquor
After extract liquor is gone in concentration tank, concentration tank is warming up to 75-85 DEG C, while starting and condenser pipe 6 and vacuum pump
8, extract liquor is concentrated under reduced pressure, until being evaporated methyl acetate, obtains the paste of dried orange peel extract.Solvent acetic acid methyl esters is cold again
Enter in solvent recovery tank 7 after condenser 6 is cooling, extracts and use for dried orange peel raw material next time.
D. dried orange peel raw material washs
The methyl acetate recycled after sample concentration again returns in ultrasonic extraction tank, the ultrasonic extraction 20- at 40-50 DEG C
30min according to the above method by chromatographic column 2, and is transferred in concentration tank 4.It is again started up concentration tank 4 and evaporated under reduced pressure acetic acid first
Ester obtains the paste of dried orange peel absolute oil.This concentration gained methyl acetate extracts for dried orange peel next time to be used.
E. the reversed-phase resin column chromatography purification of dried orange peel extract
Due to containing the small polarity unfavorable to cigarette sense organ such as a large amount of waxes, fatty acid in the methyl acetate extract of dried orange peel
Ingredient, extraction product also needs further with reversed-phase resin column chromatography purification removing wax and fatty acid impurities, net to improve gained
The quality of oil.In the present invention, the removing impurity such as wax and fatty acid are using the filling of 5 resin of BOSHI reversed-phase resin chromatographic column
Diameter: a height of 1:2, resin partial size are 35~75 μm, and the loadings of resin are the 1/2-1/3 of gained paste.
Reversed-phase resin column chromatography purification operation are as follows: concentration tank is warming up to 50-60 DEG C, by the second pump B2 in Fig. 1 toward dense
The ethyl alcohol of 95wt% is added in contracting tank 4, additive amount is that resulting paste can be made to be completely dissolved, and after being completely dissolved paste, is opened
Valve F4 is opened, starting air compressor machine 3 pressurizes to concentration tank, and Open valve F8 allows the dissolved ethanol solution of paste to pass through
Reversed-phase resin chromatographic column 5；It has crossed and 95wt% ethanol washing concentration tank is added after column into concentration tank 4 again, 95wt% ethyl alcohol
Additional amount is the 1/4-5 of first time additional amount, and cleaning solution is allowed to pass through reversed-phase resin chromatographic column 5.
In this step, the ethanol solution of paste 95w% crosses chromatographic column 5, and with 95wt% ethanol washing chromatographic column 5, old
Fragrance component in skin absolute oil does not retain on reversed resin chromatography column 5, and the impurity components such as wax and fatty acid can be retained in
On reversed-phase resin chromatographic column, it can effectively reach the effect that the fragrance component in dried orange peel absolute oil is separated with impurity such as wax and fatty acid
Fruit, to improve the quality of dried orange peel absolute oil.
Merge the ethanol solution of above-mentioned 95wt%, the propylene glycol of 3-5 times of paste of gained is then added into solution, and
It is evaporated under reduced pressure and removes ethyl alcohol to get the dried orange peel absolute oil is arrived.The purpose that propylene glycol is added can increase the mobility of dried orange peel absolute oil,
Has the function of stable dried orange peel absolute oil this perfume ingredient simultaneously.
The yield of gained dried orange peel absolute oil is 4.8-5.5%.Gained dried orange peel absolute oil be uniform bright yellow oily stream, band by
Strong dried orange peel is peculiar naturally fragrant, and elegant fragrance is comfortable；The favorable solubility in ethyl alcohol, propylene glycol equal solvent is ideal cigarette
Use additive.
F. the recycling of remaining methyl acetate
After sample extraction is complete, remain methyl acetate in the dried orange peel waste residue that extracted, the present invention can be to the part
Methyl acetate is recycled, and to reduce the environmental pollution in production process, and saves production consumption.Solvent recovery process are as follows: close
Valve closing door F1 and valve F5 seals feed opening 11, ultrasonic extraction tank 1 is warming up to 90-100 DEG C, allows methyl acetate in extractor
Evaporation, the methyl acetate steam after evaporation by anhydrous sodium sulfate and silica gel composite chromatography column and is transferred in concentration tank, through cold
Condenser condensing recovery enters in solvent recovery tank 7.In this process, methyl acetate steam is compound by anhydrous sodium sulfate and silica gel
After chromatographic column 2, methyl acetate remaining in chromatographic column 2 is also taken out of, has achieved the effect that effective recycling residual solvent.Recycling
Methyl acetate is for the use of dried orange peel sample extraction next time.
G. the regeneration of reversed-phase resin chromatographic column
In the present invention, anhydrous sodium sulfate and silica gel composite chromatography column are disposable, and next time needs weight when producing absolute oil
New filling replacement.BOSHI reversed-phase resin chromatographic column 5 can repeatedly use (at least 6000 times), used BOSHI reversed-phase resin
Chromatographic column 5 is eluted using 2-3 times of column volume of acetone, and regeneration can continue secondary make after removing the wax adsorbed on column and fatty acid
With.
H. application of the gained dried orange peel absolute oil in perfuming cigarette
A. dried orange peel absolute oil made from the above method is used in cigarette shreds, the dried orange peel absolute oil is pressed the ten of pipe tobacco weight
5/10000ths are added on cigarette shreds to the ratio of a ten thousandth, and cigarette finished product is made in pipe tobacco and is smoked panel test.The result shows that:
Dried orange peel absolute oil produced by the present invention can effectively assign cigarette dried orange peel natural feature perfume, the perfume quantity and flavouring essence quality of cigarette smoking
It is improved, moreover it is possible to which the miscellaneous gas for covering cigarette smoking improves the comfort of cigarette smoking, (this hair is not added better than control sample
The cigarette of bright obtained dried orange peel absolute oil).Or,
B. in cigarette filter forming process, the dried orange peel absolute oil that the present invention is obtained is by plasticizer triacetyl glycerine amount
1-1.5wt% amount is added in triacetyl glycerine, then being added to the triacetyl glycerine of dried orange peel absolute oil by filter tow weight
The 6-8wt% of amount is uniformly sprayed on filter tow, and filter stick is made, and volume then is made by conventional cigarette cigarette in the filter stick
Cigarette carries out sensory evaluation and smokes panel test.The result shows that: perfume quantity, the fragrance of the cigarette of dried orange peel absolute oil of the present invention are added in filter tip
Rich and refined spend is better than control cigarette, and the natural feature perfume (or spice) feature of dried orange peel is prominent, (of the invention obtain is not added better than control sample
The cigarette of the dried orange peel absolute oil arrived).
C. in cigarette paper preparation process, dried orange peel absolute oil of the present invention will be incited somebody to action this in 0.8-1.2 times of cigarette paper weight of ratio
It invents dried orange peel absolute oil obtained to be uniformly coated on cigarette paper, volume then is made in the cigarette paper roll for being coated with dried orange peel absolute oil
Cigarette carries out sensory evaluation and smokes panel test.The result shows that: the cigarette of dried orange peel absolute oil of the present invention is added in cigarette paper, dried orange peel is distinctive
It is very prominent to smell perfume, perfume quantity, flavouring essence quality and the comfort of cigarette smoking (are not added the present invention to obtain better than control sample
Dried orange peel absolute oil cigarette).
I. application of the gained dried orange peel absolute oil in electronic cigarette tobacco tar
In the tobacco juice process for preparation of electronic cigarette, dried orange peel absolute oil produced by the present invention is added to the ratio of 1-7wt%
In tobacco juice for electronic smoke, wherein preferred ratio is 5wt%.Dried orange peel absolute oil can also be in electronic cigarettes such as fruit dried orange peel, peppermint dried orange peels
It is used in liquid with the ratio of 0.1-3wt%.The result shows that: the total score of the electronic cigarette containing electronic cigarette tobacco tar of the present invention smoked panel test compared with
Height, is mainly manifested in that electronics smoke product dried orange peel is distinctive to smell that fragrant feature is prominent, aroma quality is good, and perfume quantity is sufficient；Next shows
Miscellaneous gas is light, and pleasant impression is cleaner, better than control sample (electronic cigarette for the dried orange peel absolute oil that the present invention obtains is not added).
J. gained dried orange peel absolute oil is heating the application in the cigarette that do not burn
Do not burn in cigarette manufacturing process in heating, by dried orange peel absolute oil obtained by the present invention with a ten thousandth to ten thousand/
Five ratio is added on the thin slice for heating the cigarette that do not burn, is added without dried orange peel absolute oil obtained by the present invention as control sample one
It rises and carries out sensory evaluating smoking.The result shows that: the heating for adding dried orange peel absolute oil of the invention does not burn that cigarette dried orange peel is distinctive to smell fragrant spy
Sign is very prominent, and perfume quantity is more sufficient, and suction quality is improved, and (obtained dried orange peel of the invention is not added better than control sample
The cigarette that do not burn of absolute oil).
Beneficial effects of the present invention:
1, the present invention uses methyl acetate for extractant.Methyl acetate polarity is moderate, can not only dissolve in tobacco sample
Most fragrance components, and the big polar component such as carbohydrate in dried orange peel is not extracted during the extraction process, obtained dried orange peel
Absolute oil purity is high.In addition methyl acetate low boiling point, readily volatilized, low energy consumption in sample concentration and solvent recovery process, is not easy
Dissolvent residual is caused, production cost and Product Safety are improved than other methods.
2, the device of the invention dexterously uses " anhydrous sodium sulfate-silica gel composite chromatography column " and " reversed-phase resin column chromatography "
High-efficient purification is carried out to dried orange peel absolute oil, anhydrous sodium sulfate-silica gel composite chromatography column can effectively remove moisture and big polar component, instead
Phase resin column chromatography can effectively remove the small polar component such as wax and fatty acid.Dried orange peel absolute oil is produced with traditional solvent extraction
It compares, operating process is simplified, and fragrance component loss is few in production process, and gained dried orange peel absolute oil yield significantly improves.And biography
The molecularly distilled of system is compared, and the method for the present invention can allow a large amount of nonvolatile fragrance component glycoside compounds in dried orange peel (i.e. latent fragrant
Compound) it is retained in dried orange peel absolute oil, the loss of such fragrance component is effectively prevented, these latent aroma compounds can be fired in tobacco
It is released during burning by glycosidic bond fracture, effectively improves the quality of flue gas.
3, there is reversed-phase resin column in the device of the invention, dried orange peel absolute oil can be refined using the chromatography reversed-phase resin column.
BOSHI reversed-phase resin is polystyrene-divinylbenzene copolymeric material, is set based on modern HPLC liquid chromatogram isolation technics
Meter, there is lesser particle and higher separating property, the present invention is used for the separation and purification purification of dried orange peel absolute oil for the first time.
Reversed resin is also able to maintain good column through regeneration reusable 6000 times or more and imitates, and is far below it for real cost of production
Its column chromatography for separation technique.
4, extraction element of the invention is compared using ultrasonic extraction process with existing extraction process, energy in extraction process
Consumption is reduced, and is extracted more complete.The device of the invention can realize the addition of solvent, chromatography column purification, sample concentration
Be automatically brought into operation, production procedure is easy to operate, human cost consumption is low.Furthermore the device of the invention is used, is used in each step
Solvent effective recycling and reusing can be obtained.Production process solvent consumption greatly reduces, while saving solvent cost, ring
Border pollution substantially reduces, and production operation safety significantly improves.
5, the dried orange peel absolute oil purity obtained using the device of the invention is higher, for cigarette or new tobacco products (such as electricity
Sub- cigarette cigarette or the cigarette that do not burn) in, effectively strengthen cigarette, electronic cigarette or heat the dried orange peel of cigarette this perfume feature of not burning, covers
The miscellaneous gas of product suction promotes and improves cigarette, electronic cigarette or the suction comfort for heating the cigarette that do not burn, gives consumer more
Good suction impression.
Detailed description of the invention
Fig. 1 is extraction of the invention and refining plant schematic diagram.
Appended drawing reference are as follows: 1, ultrasonic extraction tank；2, chromatographic column；3, air compressor machine；4, concentration tank；5, reversed resin column；6, cold
Condenser；7, solvent recovery tank；8, vacuum pump；11, feed opening；12, plant material；13, sieve plate is filtered；14, discharge port；21, nothing
Aqueous sodium persulfate particle；22, silica gel particle；B1, the first pump；B2, the second pump；F (F1-F8), valve.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under that premise of not paying creative labor
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
It extracts the dried orange peel that raw material uses and uses the dried orange peel for originating in Yunnan, dried orange peel sample drying is crushed to 20 mesh, and inventory is
200kg is added in ultrasonic extraction tank 1, seals feed opening and discharge port, and 5 times of dried orange peel example weight of methyl acetate is added,
Ultrasonic extraction 35min at 45 DEG C, starting air compressor machine pressurizes to ultrasonic extraction tank after having extracted, and extract liquor is allowed to pass through discharge port
Filtering sieve plate and lead to chromatography column purification.
After being gone in concentration tank by the extract liquor of chromatographic column, concentration tank is warming up to 80 DEG C, while starting vacuum pump, concentration
Extract liquor, until being evaporated methyl acetate.The methyl acetate recycled after sample concentration is again returned in ultrasonic extraction tank 1,
Ultrasonic extraction 25min raw material at 45 DEG C, cleaning solution are transferred in concentration tank again by chromatographic column；Evaporated under reduced pressure second again
Sour methyl esters, can be obtained paste.
Concentration tank is warming up to 55 DEG C, and the ethyl alcohol of 95wt% is added into concentration tank, and ethyl alcohol additive amount is that can make resulting cream
Shape object is completely dissolved；Then it is pressurizeed with air compressor machine to concentration tank, the ethyl alcohol dissolved matter of 95wt% is then allowed to pass through reverse phase tree
Rouge chromatographic column 5.It has crossed after column and the above-mentioned 1/4 95wt% ethanol washing that can be completely dissolved paste object amount is added into concentration tank again
Concentration tank, and cleaning solution is allowed to wash chromatographic column by reversed-phase resin chromatographic column.Merge ethanol solution, resulting paste weight is added
The propylene glycol of 4 times of amount is evaporated under reduced pressure and removes ethyl alcohol, and the dried orange peel absolute oil can be obtained, and the yield of dried orange peel absolute oil is 5.2%.
Bar absolute oil is uniform bright brown oil fluid, and band is molten in ethyl alcohol, propylene glycol equal solvent by strong dried orange peel characteristic perfume
Solution property is good, is ideal cigarette additive.
Embodiment 2
Dried orange peel absolute oil made from the above method is used in cigarette shreds, the dried orange peel absolute oil is pressed the 100000 of pipe tobacco weight
/ five ratio is added on cigarette shreds, and cigarette finished product is made in pipe tobacco and is smoked panel test.The result shows that: it is produced by the present invention
Dried orange peel absolute oil can effectively assign cigarette dried orange peel natural feature perfume, and the perfume quantity and flavouring essence quality of cigarette smoking are improved, also
The miscellaneous gas that cigarette smoking can be covered, improves the comfort of cigarette smoking, (obtained dried orange peel of the invention is not added better than control sample
The cigarette of absolute oil).Or,
In cigarette filter forming process, the dried orange peel absolute oil that the present invention is obtained is by plasticizer triacetyl glycerine amount
1wt% amount is added in triacetyl glycerine, then being added to the triacetyl glycerine of dried orange peel absolute oil by filter tow weight
7wt% is uniformly sprayed on filter tow, and filter stick is made, and cigarette then is made by conventional cigarette cigarette in the filter stick, into
Row sensory evaluation is smoked panel test.The result shows that: it is added to the distinctive naturally fragrant feature of dried orange peel of the present invention in filter tip and protrudes, perfume quantity,
The rich and refined degree of fragrance, better than control sample (cigarette for the dried orange peel absolute oil that the present invention obtains is not added).Or,
In cigarette paper preparation process, dried orange peel absolute oil of the present invention is made the present invention in 1.0 times of cigarette paper weight of ratio
The dried orange peel absolute oil obtained is uniformly coated on cigarette paper, and cigarette then is made in the cigarette paper roll for being coated with dried orange peel absolute oil, into
Row sensory evaluation is smoked panel test.The result shows that: the cigarette of dried orange peel absolute oil of the present invention is added in cigarette paper, dried orange peel is distinctive naturally fragrant
Feature is prominent, perfume quantity, flavouring essence quality and the comfort of cigarette smoking, better than control sample (be not added the present invention obtain it is old
The cigarette of skin absolute oil).
Embodiment 3
In the process for preparation of tobacco juice for electronic smoke, dried orange peel absolute oil of the present invention is added to the ratio of weight 5%
In dried orange peel taste tobacco juice for electronic smoke.The result shows that: the total score of dried orange peel absolute oil of the invention is higher, and advantage is mainly manifested in dried orange peel
Distinctive naturally fragrant feature is prominent, and aroma quality is good, and perfume quantity is sufficient；Next shows that miscellaneous gas is light, and pleasant impression is cleaner, better than control
(electronic cigarette for the dried orange peel absolute oil that the present invention obtains is not added) in sample.
Embodiment 4
In heating cigarette manufacturing process of not burning, dried orange peel absolute oil obtained by the present invention is added with the ratio of a ten thousandth
It is added on the thin slice for heating the cigarette that do not burn, is added without dried orange peel absolute oil obtained by the present invention as control sample and carries out sense organ together
It smokes panel test.The result shows that: the heating distinctive naturally fragrant feature of cigarette dried orange peel of not burning for adding dried orange peel absolute oil of the invention is prominent, fragrant
Tolerance is more sufficient, miscellaneous to be so incensed that cover, and irritation is reduced, and suction quality is improved, and (this is not added better than control sample
Invent the cigarette that do not burn of obtained dried orange peel absolute oil).
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of dried orange peel absolute oil, which is characterized in that use following device:
Ultrasonic extraction tank (1), upper part have feed opening (11), and lower part has discharge port (14), and discharge port (14) top had
Screen plate (13)；
Chromatographic column (2)；
Air compressor machine (3)；
Concentration tank (4)；
Reversed resin column (5)；
Condenser (6)；
Vacuum pump (8)；
Solvent recovery tank (7)；
The connection type of each component is as follows:
The ultrasonic extraction tank (1) is connected to by its discharge port (14) with the chromatographic column (2) upper inlet, the chromatographic column
(2) lower part outlet is connected to the concentration tank (4) top；Concentration tank (4) top is connected to the entrance of the condenser (6),
Condenser (10) upper end outlet is connected to the vacuum pump (8)；Solvent described in the outlet of condenser (10) lower end returns
Closed cans (7)；The air compressor machine (3) is connected to ultrasonic extraction tank (1) upper port and the concentration tank (4) upper port respectively；
Concentration tank (4) lower part outlet is connected to the reversed resin column (5)；
Steps are as follows for the preparation method:
1. dried orange peel raw material is added in the ultrasonic extraction tank (1), feed opening and discharge port are sealed, dried orange peel raw material weight is added
4-6 times of methyl acetate, the ultrasonic extraction 30-40min at 40-50 DEG C；
2. starting air compressor machine (3) after having extracted, to step, 1. the ultrasonic extraction tank (1) is pressurizeed, and allows extract liquor by going out
The filtering sieve plate (13) of material mouth (14) is entered in concentration tank (4) by chromatographic column (2)；
3. concentration tank (4) is warming up to 75-85 DEG C, start vacuum pump (8) and condenser (6), extract liquor is concentrated under reduced pressure, until steaming
Dry methyl acetate obtains the paste of dried orange peel extraction；
4. the paste for obtaining step 3. to the ethyl alcohol that 95wt% is added in concentration tank (4) is completely dissolved, start air compressor machine (3)
It pressurizes to concentration tank (4), liquid is allowed to pass through reversed resin column (5) completely；
5. 4. obtaining liquid to step is added 3-5 times of paste weight of the propylene glycol, it is evaporated under reduced pressure and removes ethyl alcohol to get arriving
The dried orange peel absolute oil.
2. preparation method according to claim 1, which is characterized in that the diameter of the chromatographic column (2): a height of 2:1, in
Filled with silica gel particle and anhydrous sodium sulfate particle, the partial size of the particle is 100-200 mesh；In the reversed resin column (5)
Filled with BOSHI reversed-phase resin；The diameter of the BOSHI reversed-phase resin filling: a height of 1:2, partial size are 35~75 μm.
3. preparation method according to claim 1, which is characterized in that the upper end of the ultrasonic extraction tank (1) and the first pump
(B1) it is connected to；The upper end of the concentration tank (4) is connected to the second pump (B2)；It is connected between each component by pipeline, the pipeline
On have valve (F).
4. preparation method according to claim 1, which is characterized in that 3. step before the reduced pressure extract liquor, is also wrapped
It includes and ultrasonic extraction tank (1) is washed using methyl acetate, then enter methyl acetate cleaning solution by chromatographic column (2) dense
Contracting tank (4) step.
5. preparation method according to claim 1, which is characterized in that 5. step before the reduction vaporization removing ethyl alcohol, is gone back
Including using the 95wt% ethyl alcohol of the 1/4-5 of the paste weight to wash concentration tank (4), then by ethanol washes
By reversed resin column (5), carries out the reduction vaporization of step 5. and remove ethanol Step.
6. dried orange peel absolute oil made from preparation method according to claim 1 is used for cigarette, electronic cigarette or the cigarette that do not burn
The purposes of middle flavoring.
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| CN110551576A (en) * | 2019-09-04 | 2019-12-10 | 江苏第二师范学院（江苏省教育科学研究院） | orange peel essential oil with fly killing effect and application thereof |
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