CN109852479A - A kind of floating oil method prepares the method and its application of flue-cured tobacco absolute oil - Google Patents
A kind of floating oil method prepares the method and its application of flue-cured tobacco absolute oil Download PDFInfo
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Abstract
The present invention relates to the method and its application that a kind of floating oil method prepares flue-cured tobacco absolute oil, belong to essence spice for cigarette technical field.This method includes extracting, being concentrated, refrigerating layering, secondary concentration, alcohol analysis, filtering, three times concentration, the obtained flue-cured tobacco absolute oil of molecular distillation series of processes, and flue-cured tobacco absolute oil is prepared into flavoring module, applied in cigarette.The present invention is using the ethyl alcohol of various concentration as extractant and extractant, the petroleum ether extraction of film filtering and conventional method is abandoned, and utilize water-oil separating principle, cleverly oily matter and the water-soluble substances in flue-cured tobacco extracting solution are separated, eliminate the macromoleculars water-soluble substances such as carbohydrate, protein, remain main aroma component in flue-cured tobacco to the greatest extent, this method is simple, safety, economy, absolute oil yield are high.Gained absolute oil is applied in cigarette, and tobacco aroma is abundant, cigarette perfume is natural, strong, elegant, and cigarette main aroma is greatly improved.
Description
Technical field
The invention belongs to essence spice for cigarette technical fields, and in particular to a kind of floating oil method prepare flue-cured tobacco absolute oil method and
It is applied.
Background technique
Molecular distillation technique is the novel liquid-liquid isolation technics rapidly developed in recent years, because it is particularly adapted to higher boiling, heat
Quick property and oxidizable material isolate and purify, while having the advantages that high vacuum, separation temperature are low etc., are widely used to eat
The fields such as product, medicine, daily use chemicals, fragrance have significant advantage in terms of the separation of natural products, can preferably be enriched with natural production
Object characteristic chicken flavor ingredient.But when using molecular distillation technique separating natural product, in high vacuum, high temperature environment, naturally
The macromolecular substances such as carbohydrate, pectin, protein in product can foam under a high vacuum, be carbonized at high temperature, cause to equipment
Greatly injury, and separative efficiency is seriously affected, therefore before doing molecular distillation, it is necessary to natural extract is located in advance
Reason, gets rid of the macromolecular substances such as carbohydrate, pectin, protein.
Flue-cured tobacco absolute oil is extracted from cured tobacco leaf or yanmo concrete using molecular distillation technique with this perfume of flue-cured tobacco
A kind of tobacco aromaticss can be with its advantage is that obtain tobacco aroma ingredient abundant while not introducing exogenous chemical substance
Cigarette is directly applied to, the flue-cured tobacco extract perfuming effect by processing purifying can be more ideal, can obtain flue-cured tobacco abundant
Cigarette perfume,.
Just because of the good application effect of flue-cured tobacco absolute oil and prospect, currently, preparing flue-cured tobacco absolute oil using flue-cured tobacco medicinal extract
Work is also gradually increasing, but in flue-cured tobacco absolute oil preparation process, a part is using traditional petroleum ether as extractant
Or extractant gets rid of the macromolecular substances such as the carbohydrate in tobacco, protein；Another part is then using modern membrane technology filtering
Fall macromolecular substances.There is its defect using two kinds of pre-treating methods, petroleum ether is a kind of highly volatile, inflammable, explosive molten
Agent, difficulty of processing is big, safety is low, pollution is big, and petroleum ether has kerosene taste, uses petroleum ether as extractant or extractant
The pure tobacco oil of preparation is applied in tobacco, will increase miscellaneous gas.A kind of patent ZL201810184517.9 " Sun cured tobacco molecular distillation
The preparation method of object " discloses a kind of preparation method of Sun cured tobacco molecular distillation object.The Sun cured tobacco molecular distillation object is to weigh
The ethanol solution of 20%-95% is added in Sun cured tobacco raw material, and refluxing extraction twice, merges extracting solution twice, and filter is collected by filtration
Liquid is concentrated under reduced pressure to give Sun cured tobacco medicinal extract after recycling 100nm ceramic membrane to be filtered, and the ethyl alcohol that concentration 95% is then added is molten
The sedimentation of liquid chamber temperature is concentrated under reduced pressure after taking supernatant that 100nm ceramic membrane filter is utilized to handle again and removes whole spirit solvents, obtains
To Sun cured tobacco absolute oil；Finally carry out fining to separate and collect light component being Sun cured tobacco using molecular distillation equipment Sun cured tobacco absolute oil
Molecular distillation object.The patent is exactly also not introduce miscellaneous gas, film although safety is protected using modern membrane technology
Processing is to retain substance according to the size of molecular weight, cannot extract the aroma component in tobacco to the greatest extent, and right
Equipment requirement is high, with high costs.
Patent 200910006909.7 " preparation method of wild Perilla leaf clean oil " discloses a kind of wild perillaseed absolute oil preparation side
Method, the preparation method of the open country Perilla leaf clean oil, including the wild perillaseed leaf powder of preparation, organic solvent refluxing extraction are concentrated, back dissolving is cold
The concentration of jelly suction filtration, molecular distillation isolate and purify, and obtain wild Perilla leaf clean oil, and why which, which passes through, is extracted, is concentrated, alcohol is analysed just
Have the condition of molecular distillation, is because protein, pectin, sugared content equal size are extremely low in wild perillaseed, it is only necessary to simple
Extracting concentration can be handled completely；However the substance that protein this for flue-cured tobacco, pectin, sugared content are high, party's rule
It is difficult to be applicable in.Therefore the problem of how overcome the deficiencies in the prior art is current essence spice for cigarette technical field urgent need to resolve.
Summary of the invention
It is an object of the present invention to solve the deficiency of the existing technology and provide one kind using ethyl alcohol as extractant and extractant,
According to the method that water-oil separating principle prepares flue-cured tobacco absolute oil, and it is applied in cigarette, improves cigarette smoking impression.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of method that floating oil method prepares flue-cured tobacco absolute oil, includes the following steps:
Step (1) is extracted: refluxing extraction twice carried out to cured tobacco leaf, is the 8-10 times of 60-90% ethyl alcohol measured of addition for the first time,
Refluxing extraction 2-3 hours at 80-100 DEG C；It is the 60-90% ethyl alcohol measured using 6-8 times for the second time, flows back at 80-100 DEG C
It extracts 2-3 hours；With the filtered through gauze of 200-500 mesh, combined extract；
Step (2), concentration: the extracting solution obtained at 60-70 DEG C of temperature to step (1) is concentrated, and is concentrated to density and is
1.1-1.2g/cm3, obtain concentrate；
Refrigeration layering: the concentrate refrigeration that step (2) obtains is layered, upper layer oily matter and lower layer are obtained for step (3)
Water-soluble substances；
Step (4), secondary concentration, alcohol analysis and filtering: at 60-70 DEG C of temperature, upper layer oily matter that step (3) is obtained into
Row vacuum concentration, obtains secondary concentration object；Ethyl alcohol is added into secondary concentration object and stands progress alcohol analysis, to which there is no Precipitations
Afterwards, precipitating is removed in filtering, obtains secondary concentration liquid；
Step (5) is concentrated three times: the secondary concentration liquid that step (4) obtains being concentrated in vacuo at 60-80 DEG C of temperature, is baked
Smoke-dipping paste；
Step (6) molecular distillation: carries out firsts and seconds molecular distillation to the flue-cured tobacco medicinal extract that step (5) obtains, merges resulting
Light component is to get flue-cured tobacco absolute oil.
It is further preferred that cured tobacco leaf described in step (1) is Hongda tobacco, K326, Yun yan85 and NC102
One or more of.
It is further preferred that the Hongda tobacco, K326, Yun yan85 and NC102 tobacco leaf sugar content be
18-25%, total nitrogen content are 1.5-2.5%, and nicotine content is 1.2-2.2%.
It is further preferred that in step (3), refrigeration be 5-8 DEG C in temperature at stand 18-24h.
It is further preferred that filtering first uses the filtered through gauze of 200-500 mesh in step (4), then de- using 3-5 layers
Rouge cotton is filtered.
It is further preferred that vacuum concentration described in vacuum concentration described in step (4) and step (5) is vacuum
Concentration is up to vacuum degree is until 1-5kpa, solvent-free spilling.
It is further preferred that the alcohol analysis is 5-8 times of 95% ethyl alcohol of addition into secondary concentration object in step (4),
There is Precipitation in lower layer after standing 4-8h at being 5-8 DEG C in temperature after stirring and dissolving.
It is further preferred that first order molecular distillation is in distillation pressure 1 × 10 in step (6)-4-1×10-3KPa,
It is carried out under the conditions of 50-80 DEG C of feeding temperature, 100-120 DEG C of vapo(u)rizing temperature, 30-45 DEG C of condensation temperature；
Secondary molecules distillation is in distillation pressure 1 × 10-4-1×10-3KPa, 50-80 DEG C of feeding temperature, vapo(u)rizing temperature 150-180
DEG C, it is carried out under the conditions of 55-65 DEG C of condensation temperature；
First order molecular is distilled into light component and secondary molecules distillation light component merging to get flue-cured tobacco absolute oil is arrived.
The present invention also provides a kind of flue-cured tobacco absolute oil flavoring modules, including following components composition in parts by weight: 30-
50 parts of flue-cured tobacco absolute oil, 0.1-0.5 parts of mentha piperita oils, the ethanol solution of 10% furanone of 1-5 part, 10% ethylmaltol of 6-15 part
Ethanol solution, 30-63 parts of propylene glycol；The flue-cured tobacco absolute oil is prepared for above-mentioned floating oil method and is baked made from the method for flue-cured tobacco absolute oil
Cigarette absolute oil.
Present invention simultaneously provides the applications of the flue-cured tobacco absolute oil flavoring module, and there are two types of application methods, the first be by
It is 0.5-1.0% that flavoring module, which is diluted to mass concentration with 95% ethyl alcohol, obtains flavoring module dilution；According to mass ratio 1:100
Flavoring module dilution is uniformly sprayed on pipe tobacco, cigarette is made in drying under temperature 50 C；
Second is to be added to flavoring module in electronics tobacco tar according to mass concentration 0.5 ‰ -1 ‰, as electronic cigarette additive.
Compared with prior art, the present invention has the advantages that:
1. the present invention is initiative using ethyl alcohol as extractant and extractant, in entire technique compared to petroleum ether extraction technique
In process, the present invention has only used the ethyl alcohol of various concentration as extractant and extractant, extracts, filters, concentration is also conventional
Technology can utmostly guarantee so that the technique does not introduce miscellaneous gas, easy to operate, safe and nontoxic harmless, low in cost
The stability of product quality.
2., using present invention process, almost all of oiliness causes in flue-cured tobacco compared with modern membrane filtration technique processing technique
Fragrant ingredient can be remained completely, into subsequent molecular distillation technique, so that the aroma component type of product is more
Abundant, amount is more sufficient, and fragrance is fuller.
3. initiative utilizes water-oil separating principle, oily matter and the water-soluble substances in extracting solution of suncuring tabacco are separated.
Wherein, primary concentration, refrigeration layering, secondary concentration, alcohol analysis are the core procedures of this technique, are the key that realization water-oil separating rings
Section, the basic principle is that ethyl alcohol almost evaporates in solution after extracting solution to be concentrated to certain density, is dissolved in ethyl alcohol
Oil components be gradually precipitated, remaining solvent is almost water.Again by refrigeration layering, oil components and water gradually divide
It opens, upper layer is oil components, and lower layer is water phase.Alcohol analysis is carried out after concentration, removes in oil components most of water-soluble big point
Sub- substance, up to purification medicinal extract after concentration.
4. it is higher than existing method using the yield that present invention process prepares flue-cured tobacco absolute oil, it is shown in Table 1.
1 different pre-treatments mode flue-cured tobacco absolute oil yield of table
After 5. flavoring module application to cigarette is made in gained absolute oil, personnel's progress sensory evaluation of smokeing panel test is organized, 2 and table 3 are shown in Table,
The result shows that tobacco aroma is abundant, cigarette perfume is natural, strong, elegant, cigarette after flue-cured tobacco absolute oil flavoring module is added in cigarette
Main aroma is greatly improved, and shows preferably application effect, to abundant cigarette brand, promotes cigarette industry health hair
Exhibition has positive effect.
2 Sensory Quality of Cigarette of table is smoked panel test table
Note: the cigarette of addition flue-cured tobacco absolute oil is labeled as A, and the cigarette of addition flavoring module is labeled as B, and 95 points and its above are conjunctions
Lattice.
The description of 3 major function of table
Note: CK is blank control, and the cigarette of addition flue-cured tobacco absolute oil is labeled as A, and the cigarette of addition flavoring module is labeled as B.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and it should not be regarded as limiting this hair
Bright range.In the examples where no specific technique or condition is specified, described technology or conditions according to the literature in the art
Or it is carried out according to product description.Production firm person is not specified in material therefor or equipment, is that can be obtained by purchase
Conventional products.
The present invention is unless otherwise stated, percentage sign is mass percent." times amount ", the quality multiple referred to " again ".
Embodiment 1
A kind of method that floating oil method prepares flue-cured tobacco absolute oil, includes the following steps:
Step (1) is extracted: being carried out refluxing extraction twice to cured tobacco leaf, is 60% ethyl alcohol for adding 8 times of amounts for the first time, at 80 DEG C
Lower refluxing extraction two hours；It is 60% ethyl alcohol measured using 6 times, refluxing extraction two hours at 80 DEG C for the second time；With 200 purposes
Filtered through gauze, combined extract；
Step (2), concentration: the extracting solution obtained under temperature 60 C to step (1) is concentrated, and being concentrated to density is 1.1g/
cm3, obtain concentrate；
Refrigeration layering: the concentrate refrigeration that step (2) obtains is layered, upper layer oily matter and lower layer are obtained for step (3)
Water-soluble substances；
Step (4), secondary concentration, alcohol analysis and filtering: under temperature 60 C, the upper layer oily matter that step (3) is obtained is carried out
Vacuum concentration, obtains secondary concentration object；Ethyl alcohol is added into secondary concentration object and stands progress alcohol analysis, to which there is no Precipitations
Afterwards, precipitating is removed in filtering, obtains secondary concentration liquid；
Step (5) is concentrated three times: the secondary concentration liquid that step (4) obtains is concentrated in vacuo under temperature 60 C, obtains flue-cured tobacco leaching
Cream；
Step (6) molecular distillation: carries out firsts and seconds molecular distillation to the flue-cured tobacco medicinal extract that step (5) obtains, merges resulting
Light component is to get flue-cured tobacco absolute oil.
The flue-cured tobacco absolute oil as made from 30 parts of the present embodiment, 0.1 part of mentha piperita oil, the ethanol solution of 1 part of 10% furanone, 6
The ethanol solution of 10% ethylmaltol of part, 30 parts of propylene glycol are prepared into flue-cured tobacco absolute oil flavoring module.
It is 1.0% that flavoring module, which is diluted to mass concentration with 95% ethyl alcohol, is uniformly sprayed according to solid-liquid ratio 1:100 and pipe tobacco
On, cigarette is made in drying under temperature 50 C.Professional sensory evaluating smoking's evaluation personnel reference examples blank cigarette sample is organized to carry out pair
Than evaluation of smokeing panel test.Evaluation result of smokeing panel test shows that after adding flue-cured tobacco absolute oil flavoring module, tobacco aroma is abundant, cigarette perfume is natural, dense
Strongly fragrant, elegant, cigarette main aroma is greatly improved, and shows preferably application effect.
Embodiment 2
A kind of method that floating oil method prepares flue-cured tobacco absolute oil, includes the following steps:
Step (1) is extracted: being carried out refluxing extraction twice to cured tobacco leaf, is 90% ethyl alcohol for adding 10 times of amounts for the first time, 100
Refluxing extraction 3 hours at DEG C；It is 90% ethyl alcohol measured using 8 times, refluxing extraction 3 hours at 100 DEG C for the second time；With 500 purposes
Filtered through gauze, combined extract；
Step (2), concentration: the extracting solution obtained under temperature 70 C to step (1) is concentrated, and being concentrated to density is 1.2g/
cm3, obtain concentrate；
Refrigeration layering: the concentrate that step (2) obtains is refrigerated at 8 DEG C and is stood and be layered for 24 hours, obtained by step (3)
Layer oily matter and lower layer's water-soluble substances；
Step (4), secondary concentration, alcohol analysis and filtering: under temperature 70 C, the upper layer oily matter that step (3) is obtained is carried out
Vacuum concentration, obtains secondary concentration object；Ethyl alcohol is added into secondary concentration object and stands progress alcohol analysis, to which there is no Precipitations
Afterwards, the filtered through gauze of 500 mesh is first used, then is filtered using 5 layers of absorbent cotton and removes precipitating, obtains secondary concentration liquid；
The alcohol analysis is 8 times of 95% ethyl alcohol of addition into secondary concentration object, after standing 8h at being 8 DEG C in temperature after stirring and dissolving
There is Precipitation in lower layer；
Step (5) is concentrated three times: the secondary concentration liquid that step (4) obtains is concentrated in vacuo at 80 DEG C of temperature, obtains flue-cured tobacco leaching
Cream；
Step (6) molecular distillation: carries out firsts and seconds molecular distillation to the flue-cured tobacco medicinal extract that step (5) obtains, first order molecular steams
Evaporate is in distillation pressure 1 × 10-3KPa is carried out under the conditions of 80 DEG C of feeding temperature, 120 DEG C of vapo(u)rizing temperature, 45 DEG C of condensation temperature；
Secondary molecules distillation is in distillation pressure 1 × 10-3KPa, 80 DEG C of feeding temperature, 180 DEG C of vapo(u)rizing temperature, condensation temperature 65
It is carried out under the conditions of DEG C；
First order molecular is distilled into light component and secondary molecules distillation light component merging to get flue-cured tobacco absolute oil is arrived.
Wherein, cured tobacco leaf described in step (1) is Hongda tobacco, and the sugar content of tobacco leaf is 18-25%, total nitrogen content
For 1.5-2.5%, nicotine content 1.2-2.2%.
Concentration is vacuum concentration up to vacuum degree is in 1- three times described in secondary concentration described in step (4) and step (5)
5kpa, until solvent-free spilling.
The flue-cured tobacco absolute oil as made from 50 parts of the present embodiment, 0.5 part of mentha piperita oil, 5 part of 10% furanone ethanol solution,
The ethanol solution of 15 part of 10% ethylmaltol, 63 parts of propylene glycol are prepared into flue-cured tobacco absolute oil flavoring module.
It is 0.8% that flavoring module, which is diluted to mass concentration with 95% ethyl alcohol, is uniformly sprayed according to solid-liquid ratio 1:100 and pipe tobacco
On, cigarette is made in drying under temperature 50 C.Professional sensory evaluating smoking's evaluation personnel reference examples blank cigarette sample is organized to carry out pair
Than evaluation of smokeing panel test.Evaluation result of smokeing panel test shows that after adding flue-cured tobacco absolute oil flavoring module, tobacco aroma is sufficient, cigarette perfume is strong, association
Tonality is good, main aroma is greatly improved, and shows preferably application effect.
Embodiment 3
A kind of method that floating oil method prepares flue-cured tobacco absolute oil, includes the following steps:
Step (1) is extracted: being carried out refluxing extraction twice to cured tobacco leaf, is 60% ethyl alcohol for adding 8 times of amounts for the first time, at 80 DEG C
Lower refluxing extraction 2.5 hours；It is 60% ethyl alcohol measured using 6 times, refluxing extraction 2.5 hours at 80 DEG C for the second time；With 200 mesh
Filtered through gauze, combined extract；
Step (2), concentration: the extracting solution obtained under temperature 60 C to step (1) is concentrated, and being concentrated to density is 1.1g/
cm3, obtain concentrate；
Refrigeration layering: the concentrate that step (2) obtains is refrigerated at 5 DEG C and stands 18h and be layered, obtained by step (3)
Layer oily matter and lower layer's water-soluble substances；
Step (4), secondary concentration, alcohol analysis and filtering: under temperature 60 C, the upper layer oily matter that step (3) is obtained is carried out
Vacuum concentration, obtains secondary concentration object；Ethyl alcohol is added into secondary concentration object and stands progress alcohol analysis, to which there is no Precipitations
Afterwards, the filtered through gauze of 200 mesh is first used, then is filtered using 3 layers of absorbent cotton and removes precipitating, obtains secondary concentration liquid；
The alcohol analysis is 5 times of 95% ethyl alcohol of addition into secondary concentration object, after standing 4h at being 5 DEG C in temperature after stirring and dissolving
There is Precipitation in lower layer；
Step (5) is concentrated three times: the secondary concentration liquid that step (4) obtains is concentrated in vacuo under temperature 60 C, obtains flue-cured tobacco leaching
Cream；
Step (6) molecular distillation: carries out firsts and seconds molecular distillation to the flue-cured tobacco medicinal extract that step (5) obtains, first order molecular steams
Evaporate is in distillation pressure 1 × 10-4KPa is carried out under the conditions of 50 DEG C of feeding temperature, 100 DEG C of vapo(u)rizing temperature, 30 DEG C of condensation temperature；
Secondary molecules distillation is in distillation pressure 1 × 10-4KPa, 50 DEG C of feeding temperature, 150 DEG C of vapo(u)rizing temperature, condensation temperature 55
It is carried out under the conditions of DEG C；
First order molecular is distilled into light component and secondary molecules distillation light component merging to get flue-cured tobacco absolute oil is arrived.
Wherein, cured tobacco leaf described in step (1) is K326 and Yun yan85 (mass ratio 1:1), two kinds of tobacco leaves containing sugar
Amount is 18-25%, and total nitrogen content is 1.5-2.5%, and nicotine content is 1.2-2.2%.
Concentration is vacuum concentration up to vacuum degree is in 1- three times described in secondary concentration described in step (4) and step (5)
5kpa, until solvent-free spilling.
The flue-cured tobacco absolute oil as made from 40 parts of the present embodiment, 0.3 part of mentha piperita oil, 3 part of 10% furanone ethanol solution,
The ethanol solution of 10 part of 10% ethylmaltol, 43 parts of propylene glycol are prepared into flue-cured tobacco absolute oil flavoring module.
Flavoring module is added in electronics tobacco tar according to mass concentration 0.5 ‰.Organize professional sensory evaluating smoking's evaluation personnel
Reference examples blank electronic tobacco tar sample compares evaluation of smokeing panel test.Evaluation result of smokeing panel test shows in addition flue-cured tobacco absolute oil flavoring mould
After block, flue-cured tobacco feature is fragrant obviously, cigarette perfume is mellow, harmony is preferable, main aroma is greatly improved, and shows preferably to answer
Use effect.
Embodiment 4
A kind of method that floating oil method prepares flue-cured tobacco absolute oil, includes the following steps:
Step (1) is extracted: being carried out refluxing extraction twice to cured tobacco leaf, is 75% ethyl alcohol for adding 9 times of amounts for the first time, at 95 DEG C
Lower refluxing extraction 2.3 hours；It is 80% ethyl alcohol measured using 7 times, refluxing extraction 2.7 hours at 90 DEG C for the second time；With 300 mesh
Filtered through gauze, combined extract；
Step (2), concentration: the extracting solution obtained at 65 DEG C of temperature to step (1) is concentrated, and being concentrated to density is 1.15g/
cm3, obtain concentrate；
Refrigeration layering: the concentrate that step (2) obtains is refrigerated at 7 DEG C and stands 20h and be layered, obtained by step (3)
Layer oily matter and lower layer's water-soluble substances；
Step (4), secondary concentration, alcohol analysis and filtering: at 66 DEG C of temperature, the upper layer oily matter that step (3) is obtained is carried out
Vacuum concentration, obtains secondary concentration object；Ethyl alcohol is added into secondary concentration object and stands progress alcohol analysis, to which there is no Precipitations
Afterwards, the filtered through gauze of 400 mesh is first used, then is filtered using 4 layers of absorbent cotton and removes precipitating, obtains secondary concentration liquid；
The alcohol analysis is 6 times of 95% ethyl alcohol of addition into secondary concentration object, after standing 6h at being 6 DEG C in temperature after stirring and dissolving
There is Precipitation in lower layer；
Step (5) is concentrated three times: the secondary concentration liquid that step (4) obtains is concentrated in vacuo under temperature 70 C, obtains flue-cured tobacco leaching
Cream；
Step (6) molecular distillation: carries out firsts and seconds molecular distillation to the flue-cured tobacco medicinal extract that step (5) obtains, first order molecular steams
Evaporate is in distillation pressure 5 × 10-4KPa is carried out under the conditions of 70 DEG C of feeding temperature, 110 DEG C of vapo(u)rizing temperature, 40 DEG C of condensation temperature；
Secondary molecules distillation is in distillation pressure 6 × 10-4KPa, 65 DEG C of feeding temperature, 160 DEG C of vapo(u)rizing temperature, condensation temperature 60
It is carried out under the conditions of DEG C；
First order molecular is distilled into light component and secondary molecules distillation light component merging to get flue-cured tobacco absolute oil is arrived.
Wherein, cured tobacco leaf described in step (1) is NC102, and the sugar content of tobacco leaf is 18-25%, total nitrogen content 1.5-
2.5%, nicotine content 1.2-2.2%.
Concentration is vacuum concentration up to vacuum degree is in 1- three times described in secondary concentration described in step (4) and step (5)
5kpa, until solvent-free spilling.
The flue-cured tobacco absolute oil as made from 35 parts of the present embodiment, 0.4 part of mentha piperita oil, the ethanol solution of 3 part of 10% furanone, 9
The ethanol solution of 10% ethylmaltol of part, 55 parts of propylene glycol are prepared into flue-cured tobacco absolute oil flavoring module.
Flavoring module is added in electronics tobacco tar according to mass concentration 1 ‰.Organize professional sensory evaluating smoking's evaluation personnel pair
Blank electronic tobacco tar sample compares evaluation of smokeing panel test as usual.Evaluation result of smokeing panel test shows in addition flue-cured tobacco absolute oil flavoring module
Afterwards, plentiful sufficient, strong mellow, slightly stimulation, the main aroma of flue gas of tobacco aroma is greatly improved, and shows preferably to answer
Use effect.
Embodiment 5
A kind of method that floating oil method prepares flue-cured tobacco absolute oil, includes the following steps:
Step (1) is extracted: being carried out refluxing extraction twice to cured tobacco leaf, is 90% ethyl alcohol for adding 8 times of amounts for the first time, at 85 DEG C
Lower refluxing extraction 2.4 hours；It is 80% ethyl alcohol measured using 6 times, refluxing extraction 2.5 hours at 90 DEG C for the second time；With 500 mesh
Filtered through gauze, combined extract；
Step (2), concentration: the extracting solution obtained at 65 DEG C of temperature to step (1) is concentrated, and being concentrated to density is 1.1g/
cm3, obtain concentrate；
Refrigeration layering: the concentrate that step (2) obtains is refrigerated at 5-6 DEG C and is stood and be layered, obtained by step (3)
Layer oily matter and lower layer's water-soluble substances；
Step (4), secondary concentration, alcohol analysis and filtering: under temperature 70 C, the upper layer oily matter that step (3) is obtained is carried out
Vacuum concentration, obtains secondary concentration object；Ethyl alcohol is added into secondary concentration object and stands progress alcohol analysis, to which there is no Precipitations
Afterwards, the filtered through gauze of 500 mesh is first used, then is filtered using 4 layers of absorbent cotton and removes precipitating, obtains secondary concentration liquid；
The alcohol analysis is 6 times of 95% ethyl alcohol of addition into secondary concentration object, after standing at being 5-6 DEG C in temperature after stirring and dissolving
There is Precipitation in lower layer；
Step (5) is concentrated three times: the secondary concentration liquid that step (4) obtains is concentrated in vacuo at 65 DEG C of temperature, obtains flue-cured tobacco leaching
Cream；
Step (6) molecular distillation: carries out firsts and seconds molecular distillation to the flue-cured tobacco medicinal extract that step (5) obtains, first order molecular steams
Evaporate is in distillation pressure 1 × 10-4×10-3KPa, under the conditions of 60 DEG C of feeding temperature, 110 DEG C of vapo(u)rizing temperature, 35 DEG C of condensation temperature into
Row；
Secondary molecules distillation is in distillation pressure 1 × 10-4KPa-1×10-3KPa, 70 DEG C of feeding temperature, 170 DEG C of vapo(u)rizing temperature,
It is carried out under the conditions of 63 DEG C of condensation temperature；
First order molecular is distilled into light component and secondary molecules distillation light component merging to get flue-cured tobacco absolute oil is arrived.
Wherein, cured tobacco leaf described in step (1) is 1kg Hongda tobacco.
Concentration is vacuum concentration up to vacuum degree is in 1- three times described in secondary concentration described in step (4) and step (5)
5kpa, until solvent-free spilling.
The flue-cured tobacco absolute oil as made from 40 parts of the present embodiment, 0.1 part of mentha piperita oil, 2 part of 10% furanone ethanol solution 10
The ethanol solution of 10% ethylmaltol of part, 46 parts of propylene glycol are prepared into flue-cured tobacco absolute oil flavoring module.
It is 1.0% that flavoring module, which is diluted to mass concentration with 95% ethyl alcohol, is uniformly sprayed according to solid-liquid ratio 1:100 and pipe tobacco
On, cigarette is made in drying under temperature 50 C.Professional sensory evaluating smoking's evaluation personnel reference examples blank cigarette sample is organized to carry out pair
Than evaluation of smokeing panel test.Evaluation result of smokeing panel test shows that after adding flue-cured tobacco absolute oil flavoring module, tobacco aroma enriches sufficient, smoke alcohol
It is thick, coordinate, the comfortable main aroma of pleasant impression is greatly improved, show preferably application effect.
Flavoring module is added in electronics tobacco tar according to mass concentration 0.8 ‰.Organize professional sensory evaluating smoking's evaluation personnel
Reference examples blank electronic tobacco tar sample compares evaluation of smokeing panel test.Evaluation result of smokeing panel test shows in addition flue-cured tobacco absolute oil flavoring mould
After block, tobacco aroma is obvious, cigarette perfume is naturally soft, main aroma is greatly improved, and shows preferably application effect.
In order to preferably be illustrated to the present invention, applicant has been done accordingly for core of the invention step to having a competition
(condition of other steps is consistent with claims in addition to the step listed by this table) is tested, the results are shown in Table 4.
The comparison of each test result after 4 core procedure of table changes
Note: "-" indicates to cancel the step
The basic principles, main features and advantages of the present invention have been shown and described above.The technical staff of the industry
It should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe the present invention
Principle, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these variation and
Improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent
Object defines.
Claims (10)
1. a kind of method that floating oil method prepares flue-cured tobacco absolute oil, which comprises the steps of:
Step (1) is extracted: refluxing extraction twice carried out to cured tobacco leaf, is the 8-10 times of 60-90% ethyl alcohol measured of addition for the first time,
Refluxing extraction 2-3 hours at 80-100 DEG C；It is the 60-90% ethyl alcohol measured using 6-8 times for the second time, flows back at 80-100 DEG C
It extracts 2-3 hours；With the filtered through gauze of 200-500 mesh, combined extract；
Step (2), concentration: the extracting solution obtained at 60-70 DEG C of temperature to step (1) is concentrated, and is concentrated to density and is
1.1-1.2g/cm3, obtain concentrate；
Refrigeration layering: the concentrate refrigeration that step (2) obtains is layered, upper layer oily matter and lower layer are obtained for step (3)
Water-soluble substances；
Step (4), secondary concentration, alcohol analysis and filtering: at 60-70 DEG C of temperature, upper layer oily matter that step (3) is obtained into
Row vacuum concentration, obtains secondary concentration object；Ethyl alcohol is added into secondary concentration object and stands progress alcohol analysis, to which there is no Precipitations
Afterwards, precipitating is removed in filtering, obtains secondary concentration liquid；
Step (5) is concentrated three times: the secondary concentration liquid that step (4) obtains being concentrated in vacuo at 60-80 DEG C of temperature, is baked
Smoke-dipping paste；
Step (6) molecular distillation: carries out firsts and seconds molecular distillation to the flue-cured tobacco medicinal extract that step (5) obtains, merges resulting
Light component is to get flue-cured tobacco absolute oil.
2. the method that floating oil method according to claim 1 prepares flue-cured tobacco absolute oil, which is characterized in that baked described in step (1)
Cigarette tobacco leaf is one or more of Hongda tobacco, K326, Yun yan85 and NC102.
3. the method that floating oil method according to claim 1 prepares flue-cured tobacco absolute oil, which is characterized in that the safflower great Jin
Member, K326, Yun yan85 and NC102 tobacco leaf sugar content be 18-25%, total nitrogen content is 1.5-2.5%, and nicotine content is
1.2-2.2%。
4. the method that floating oil method according to claim 1 prepares flue-cured tobacco absolute oil, which is characterized in that in step (3), refrigeration is
18-24h is stood at being 5-8 DEG C in temperature.
5. the method that floating oil method according to claim 1 prepares flue-cured tobacco absolute oil, which is characterized in that in step (4), filtering is first
It is filtered using the filtered through gauze of 200-500 mesh, then using 3-5 layers of absorbent cotton.
6. the method that floating oil method according to claim 1 prepares flue-cured tobacco absolute oil, which is characterized in that true described in step (4)
Vacuum concentration described in sky concentration and step (5) is vacuum concentration up to vacuum degree is until 1-5kpa, solvent-free spilling.
7. the method that floating oil method according to claim 1 prepares flue-cured tobacco absolute oil, which is characterized in that described in step (4)
Alcohol analysis is 5-8 times of 95% ethyl alcohol of addition into secondary concentration object, stands lower layer after 4-8h at being 5-8 DEG C in temperature after stirring and dissolving
There is Precipitation.
8. the method that floating oil method according to claim 1 prepares flue-cured tobacco absolute oil, which is characterized in that in step (6), a fraction
Son distillation is in distillation pressure 1 × 10-4-1×10-3KPa, 50-80 DEG C of feeding temperature, 100-120 DEG C of vapo(u)rizing temperature, condensation temperature
It is carried out under the conditions of 30-45 DEG C of degree；
Secondary molecules distillation is in distillation pressure 1 × 10-4-1×10-3KPa, 50-80 DEG C of feeding temperature, vapo(u)rizing temperature 150-180
DEG C, it is carried out under the conditions of 55-65 DEG C of condensation temperature；
First order molecular is distilled into light component and secondary molecules distillation light component merging to get flue-cured tobacco absolute oil is arrived.
9. a kind of flue-cured tobacco absolute oil flavoring module, which is characterized in that including following components composition in parts by weight: 30-50
Part flue-cured tobacco absolute oil, 0.1-0.5 parts of mentha piperita oils, the ethanol solution of 10% furanone of 1-5 part, 10% ethylmaltol of 6-15 part
Ethanol solution, 30-63 part propylene glycol；The flue-cured tobacco absolute oil is that the preparation of floating oil method described in claim 1-8 any one is roasting
Flue-cured tobacco absolute oil made from the method for cigarette absolute oil.
10. the application of flue-cured tobacco absolute oil flavoring module as claimed in claim 9, it is characterised in that: there are two types of application methods, the first
It is that flavoring module is diluted to mass concentration with 95% ethyl alcohol is 0.5-1.0%, obtains flavoring module dilution；According to mass ratio 1:
100 are uniformly sprayed on flavoring module dilution on pipe tobacco, and cigarette is made in drying under temperature 50 C；
Second is to be added to flavoring module in electronics tobacco tar according to mass concentration 0.5 ‰ -1 ‰.
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| CN109875104A (en) * | 2019-04-19 | 2019-06-14 | 云南磊然康科技有限公司 | A kind of preparation method for the electronic atomized liquid being enriched with tea aroma ingredient |
| CN111671131A (en) * | 2020-06-22 | 2020-09-18 | 福建中烟工业有限责任公司 | Electronic cigarette atomized liquid with flue-cured tobacco and tobacco taste and preparation method thereof |
| CN113826942A (en) * | 2021-10-29 | 2021-12-24 | 云南中烟新材料科技有限公司 | Preparation method of sun-cured tobacco extract with sweet characteristic and processing method of sun-cured tobacco |
| CN115067539A (en) * | 2022-05-27 | 2022-09-20 | 海南摩尔兄弟科技有限公司 | Aerosol generating substrate, tobacco extract and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109875104A (en) * | 2019-04-19 | 2019-06-14 | 云南磊然康科技有限公司 | A kind of preparation method for the electronic atomized liquid being enriched with tea aroma ingredient |
| CN111671131A (en) * | 2020-06-22 | 2020-09-18 | 福建中烟工业有限责任公司 | Electronic cigarette atomized liquid with flue-cured tobacco and tobacco taste and preparation method thereof |
| CN111671131B (en) * | 2020-06-22 | 2022-04-22 | 福建中烟工业有限责任公司 | Electronic cigarette atomized liquid with flue-cured tobacco and tobacco taste and preparation method thereof |
| CN113826942A (en) * | 2021-10-29 | 2021-12-24 | 云南中烟新材料科技有限公司 | Preparation method of sun-cured tobacco extract with sweet characteristic and processing method of sun-cured tobacco |
| CN113826942B (en) * | 2021-10-29 | 2022-06-21 | 云南中烟新材料科技有限公司 | Preparation method of sun-cured tobacco extract with sweet characteristic and processing method of sun-cured tobacco |
| CN115067539A (en) * | 2022-05-27 | 2022-09-20 | 海南摩尔兄弟科技有限公司 | Aerosol generating substrate, tobacco extract and preparation method thereof |
| CN115581310A (en) * | 2022-09-02 | 2023-01-10 | 江西中烟工业有限责任公司 | Preparation method of endogenous recombinant essence for flue-cured tobacco |
| CN115581310B (en) * | 2022-09-02 | 2023-09-19 | 江西中烟工业有限责任公司 | Preparation method of tobacco endogenous recombinant essence |
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