CN109123754A - A kind of high efficiency preparation method and purposes of jujube absolute oil - Google Patents
A kind of high efficiency preparation method and purposes of jujube absolute oil Download PDFInfo
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- CN109123754A CN109123754A CN201811097886.0A CN201811097886A CN109123754A CN 109123754 A CN109123754 A CN 109123754A CN 201811097886 A CN201811097886 A CN 201811097886A CN 109123754 A CN109123754 A CN 109123754A
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- jujube
- cigarette
- tank
- absolute oil
- concentration tank
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- 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
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for extraction
-
- 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
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
-
- 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
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
-
- 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
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a kind of preparation methods of jujube 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 jujube 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 jujube absolute oil except ethyl alcohol.The device of the invention can efficiently be extracted and be purified to jujube absolute oil, and obtained jujube 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 jujube absolute oil, with
And the jujube 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.
Jujube is Rhamnaceae jujube, is the ripening fruits of jujube tree.Jujube is a kind of traditional dry fruit full of nutrition, tool
It is higher there are many alimentary health-care function, especially sugar content, it is widely used in food compositions, food additives and flavouring essence for tobacco.
Mainly there are concentration jujube juice, jujube absolute oil, jujube tincture and jujube medicinal extract etc. with the flavouring essence for tobacco of red date as raw materials.Wherein jujube absolute oil
It is through jujube extraction, distills, miscellaneous taste is covered with its unique jujube perfume (or spice), increases the fragrant and sweet sense of tobacco.
Red date extract currently used for perfuming cigarette has medicinal extract, tincture, absolute oil, essential oil etc..Traditional jujube absolute oil system
Preparation Method has solvent extraction, supercritical extraction, molecularly distilled etc..These method high production cost, the yield of absolute oil are low.
In addition existing red date extract is not burnt due to complicated component in new tobacco products, influencing electronic cigarette and heating
The suction of cigarette is experienced.
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 jujube 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 jujube 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 jujube 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 jujube 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. jujube raw material is added in the ultrasonic extraction tank 1, feed opening and discharge port are sealed, jujube 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 jujube 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 jujube 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 port import of the ultrasonic extraction tank 1 is connected to the first pump B1；The upper port of the concentration tank 4
It is connected to the second pump B2；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 jujube 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 jujube absolute oil method with reference to the accompanying drawing, specific as follows:
A. the extraction of jujube raw material
Extraction for fragrance component in jujube 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 jujube
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 jujube raw material used uses Xinjiang Shule jujube, dry, pulverize 15-20 mesh after the stoning of jujube sample, from Fig. 1
Shown in the feed opening 11 of thermostatic ultrasonic extractor 1 be added in ultrasonic extraction tank, seal feed opening and discharge port, starting first
The methyl acetate that 4-6 times of jujube raw material weight is added in B1 is pumped, then the ultrasonic extraction 30-40min at 40-50 DEG C.After having extracted
Valve F2 in Fig. 1 is opened, starting air compressor machine 3 pressurizes to ultrasonic extraction tank 1, and jujube extract is allowed to pass through on discharge port 14
Filtering 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 jujube extract
Due to containing moisture in jujube raw material, in jujube absolute oil extraction process, the big polarity such as moisture and a small amount of carbohydrate at
Dividing can also be dissolved into jujube 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 jujube 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 jujube 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 jujube extract.Solvent acetic acid methyl esters is cold again
Enter in solvent recovery tank 7 after condenser 6 is cooling, extracts and use for jujube raw material next time.
D. jujube 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 jujube absolute oil.This concentration gained methyl acetate extracts for jujube next time to be used.
E. the reversed-phase resin column chromatography purification of jujube 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 jujube
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 4 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, red
Fragrance component in jujube 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 jujube absolute oil is separated with impurity such as wax and fatty acid
Fruit, to improve the quality of jujube 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 jujube absolute oil is arrived.The purpose that propylene glycol is added can increase the mobility of jujube absolute oil,
Has the function of stable jujube absolute oil this perfume ingredient simultaneously.
The yield of gained jujube absolute oil is 5.0-6.1%.Gained jujube absolute oil is uniform bright brown oil fluid, band
By strong jujube characteristic perfume, 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 jujube 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 jujube 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 jujube absolute oil in perfuming cigarette
A. jujube absolute oil made from the above method is used in cigarette shreds, the jujube 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:
Jujube absolute oil produced by the present invention effectively can have fragrant and sweet, the perfume quantity and fragrance of cigarette smoking for product imparting cigarette product jujube
Quality is improved, moreover it is possible to which the miscellaneous gas for covering cigarette smoking improves the comfort of cigarette smoking, (is not added better than control sample
The cigarette for the jujube absolute oil that the present invention obtains).Or,
B. in cigarette filter forming process, the jujube 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 jujube 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 jujube absolute oil of the present invention are added in filter tip
Rich and refined degree has graceful naturally jujube fragrant better than control cigarette, (is not added what the present invention obtained better than control sample
The cigarette of jujube absolute oil).
C. in cigarette paper preparation process, jujube 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 jujube absolute oil obtained to be uniformly coated on cigarette paper, volume then is made in the cigarette paper roll for being coated with jujube absolute oil
Cigarette carries out sensory evaluation and smokes panel test.The result shows that: the cigarette of jujube absolute oil of the present invention is added in cigarette paper, jujube feature
It smells perfume to protrude very much, perfume quantity, flavouring essence quality and the comfort of cigarette smoking are better than control sample, (are not added better than control sample
The cigarette for the jujube absolute oil that the present invention obtains).
I. application of the gained jujube absolute oil in electronic cigarette tobacco tar
In the tobacco juice process for preparation of electronic cigarette, jujube 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%.Jujube absolute oil can also be in electronic cigarettes such as fruit jujube, peppermint jujubes
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 fragrant and sweet feature is prominent, aroma quality is good, and perfume quantity is sufficient；Next shows that miscellaneous gas is light, and pleasant impression is cleaner, excellent
In control sample (electronic cigarette for the jujube absolute oil that the present invention obtains is not added).
J. gained jujube absolute oil is heating the application in the cigarette that do not burn
Do not burn in cigarette manufacturing process in heating, by jujube 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 jujube absolute oil obtained by the present invention as control sample one
It rises and carries out sensory evaluating smoking.The result shows that: heating the smelling for cigarette jujube feature of not burning for adding jujube absolute oil of the invention is fragrant non-
Often prominent, perfume quantity is more sufficient, and suction quality is improved, and (obtained jujube absolute oil of the invention is not added better than control sample
The cigarette that do not burn).
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 jujube is not extracted during the extraction process, obtained jujube
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 jujube 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.Jujube 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 jujube 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 jujube (i.e. latent fragrant
Compound) it is retained in jujube 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, jujube 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 jujube 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 jujube 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 jujube 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
Raw material is extracted using the jujube for originating in Xinjiang Shule, is dried after jujube stoning, is crushed to 18 mesh, inventory is
200kg is added in ultrasonic extraction tank 1, seals feed opening and discharge port, and 5 times of jujube 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 jujube absolute oil can be obtained, and the yield of jujube absolute oil is 6.0%.
Obtained jujube absolute oil is uniform bright brown oil fluid, and band is by strong jujube characteristic perfume, in ethyl alcohol, propylene glycol
Favorable solubility in equal solvent is ideal cigarette additive.
Embodiment 2
Jujube absolute oil made from the above method is used in cigarette shreds, the jujube 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
Jujube absolute oil can effectively strengthen the jujube of cigarette product this perfume feature, and the perfume quantity and flavouring essence quality of cigarette smoking are improved,
The miscellaneous gas that cigarette smoking can also be covered, improves the comfort of cigarette smoking, better than control sample (be not added the present invention obtain it is red
The cigarette of jujube absolute oil).Or,
In cigarette filter forming process, the jujube 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 jujube 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: perfume quantity, the fragrance that the cigarette of jujube absolute oil of the present invention is added in filter tip are rich
With refined degree, it is better than control sample (cigarette for the jujube absolute oil that the present invention obtains is not added).
In cigarette paper preparation process, jujube absolute oil of the present invention is made the present invention in 1.0 times of cigarette paper weight of ratio
The jujube absolute oil obtained is uniformly coated on cigarette paper, and cigarette then is made in the cigarette paper roll for being coated with jujube absolute oil, into
Row sensory evaluation is smoked panel test.The result shows that: the cigarette of jujube absolute oil of the present invention is added in cigarette paper, smelling for jujube feature is fragrant non-
Often prominent, better than control sample (obtained jujube of the invention is not added in perfume quantity, flavouring essence quality and the comfort of cigarette smoking
The cigarette of absolute oil).
Embodiment 3
In the process for preparation of tobacco juice for electronic smoke, jujube absolute oil of the present invention is added to the ratio of weight 5%
In red jujube taste tobacco juice for electronic smoke.The result shows that: the total score of jujube absolute oil of the invention is higher, and advantage is mainly manifested in jujube
Distinctive to bake fragrant and sweet feature protrusion, 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 jujube absolute oil that the present invention obtains is not added) in sample.
Embodiment 4
In heating cigarette manufacturing process of not burning, jujube 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 jujube absolute oil obtained by the present invention as control sample and carries out sense organ together
It smokes panel test.The result shows that: add jujube absolute oil of the invention heating do not burn cigarette jujube it is distinctive to bake fragrant and sweet feature prominent, it is fragrant
Tolerance is more sufficient, and suction quality is improved, and (volume that do not burn for the jujube absolute oil that the present invention obtains is not added better than control sample
Cigarette).
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)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811097886.0A CN109123754B (en) | 2018-09-20 | 2018-09-20 | Efficient preparation method and application of red date absolute |
Applications Claiming Priority (1)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112877138A (en) * | 2021-03-03 | 2021-06-01 | 郑州市鑫磊香料有限公司 | Red date absolute oil purification equipment and process |
| CN114532580A (en) * | 2022-03-30 | 2022-05-27 | 湖北中烟工业有限责任公司 | Preparation method of cigar tobacco leaves |
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| CN109123754B (en) | 2021-02-26 |
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