CN106962972B - A kind of counterextraction method for lifting discarded tobacco leaf quality - Google Patents
A kind of counterextraction method for lifting discarded tobacco leaf quality Download PDFInfo
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- CN106962972B CN106962972B CN201710166257.8A CN201710166257A CN106962972B CN 106962972 B CN106962972 B CN 106962972B CN 201710166257 A CN201710166257 A CN 201710166257A CN 106962972 B CN106962972 B CN 106962972B
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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
- A24B15/241—Extraction of specific substances
Abstract
The present invention relates to extraction and counterextraction field,Particularly relate to the motion for being extracted component in subcritical fluids,Optionally material is inversely diffused into inside material,The counterextraction method for lifting discarded tobacco leaf quality realized the change of material internal component or swap the composition in different material,Comprise the following steps,Pretreatment,Dry and breaking-wall cell is handled,Extraction,Pretreated sample is placed in extractor,Inject extractant and entrainer,Extracted under certain extraction conditions,Extraction obtains sample extraction thing after terminating,Sample extraction thing cleans,The sample extraction thing being purified after removal of impurities,Sample extraction thing after purification is together inserted in counterextraction tank with discarded tobacco leaf,Inject counterextraction solvent and entrainer,Counterextraction is carried out under the conditions of certain counterextraction,Counterextraction obtains the discarded tobacco leaf after counterextraction after terminating,The counterextraction method of the present invention,Technique is simple,It is effectively improved the quality of discarded tobacco leaf.
Description
Technical field
The present invention relates to extraction and counterextraction field, and in particular to the motion by extraction component in subcritical fluids is utilized,
Optionally material is inversely diffused into inside material, the change of material internal component is realized or enters the composition in different material
The counterextraction method for the lifting discarded tobacco leaf quality that row exchanges.
Background technology
Discarded tobacco leaf refers to middle yellow Pyatyi in GB2635-86, upper yellow level Four, each grade cigarette below bluish yellow two level
Leaf.This part tobacco leaf for its presentation quality, color is pale brown, it is yellowish-brown and with cyan, became uneven is even, blade construction is dredged
Pine, glossiness be weaker, more with obvious flower piece, residual hinder area is big and oil is insufficient etc.；For inherent sucking quality, fragrance
Shortcoming, aroma quality is rougher, hardship is peppery, excitant astringent taste is obvious, pleasant impression is not net, oral cavity tongue residue is more.Wherein miscellaneous gas is
Cause discarded tobacco leaf and influence the principal element of quality of tobacco, miscellaneous gas refers to make smoker feel displeased caused by tobacco leaf burning
Fast smell, mainly there are the miscellaneous gas of blue foreign smell, region and withered and burnt smell etc..China is tobacco planting and big producer, is planted at present
Area occupies first place in the world.In tobacco planting and production process, there is substantial amounts of discarded tobacco leaf to produce, constitute about tobacco leaf total output
25%.At present, discarded tobacco leaf is mainly used in expanded cut tobacco or thin slice in tobacco business, and only in four class cigarette and five class cigarette
Use, ratio is less than 10% mostly.However as the adjustment of market structure, the demand of medium-to-high grade cigarette is more and more big, high-quality
The acquisition of raw material has turned into the development priority of cigarette enterprise.Discarded tobacco leaf is faced with that level of comprehensive utilization is low, approach is few, the wasting of resources is non-
A series of problems, such as Chang Yanchong.In the case, existing tobacco leaf resource is made full use of, expands the output of medium-to-high grade cigarette,
The overall quality of discarded tobacco leaf raw material is lifted, its use value is improved and all has great importance to enterprise, to society.
A kind of " method that discarded tobacco leaf use value is improved using subcritical dry cleaning technology（CN2013104 41875.0）”
A kind of method that discarded tobacco leaf use value is improved using subcritical dry cleaning technology is disclosed, quick remove produces in discarded tobacco leaf
The precursor of miscellaneous gas, so as to lift the quality of discarded tobacco leaf raw material to a certain extent；Qi Kun researchs are found（Finished product tobacco leaf is conformal
The subcritical abstraction technique of lowering harm and decreasing coking, application number 201110076093.2）, nicotine and tar precursor thing energy are removed by extracting
Reach the purpose of lowering harm and decreasing coking.Both approaches are all just with subcritical technology, from sample tobacco leaf surface or inside to cigarette
Leaf is handled, and the nicotine in tobacco leaf or tar precursor thing are got rid of, so as to improve the quality of discarded tobacco leaf.
The content of the invention
There is provided that a kind of technique is simple, input is low, can it is an object of the invention to overcome the deficiencies in the prior art
Material, is optionally inversely diffused into material by motion of the utilization of industrialized production by extraction component in subcritical fluids
Portion, the inverse extraction for lifting discarded tobacco leaf quality realized the change of material internal component or swap the composition in different material
Take method.
The technical proposal of the invention is realized in this way：
A kind of counterextraction method for lifting discarded tobacco leaf quality, comprises the following steps：
Step 1）Pretreatment：The material samples for needing to be extracted are dried and breaking-wall cell is handled；
Step 2）Extraction：By step 1）Pretreated material samples are placed in closed extractor, are vacuumized until extraction
Take vacuum in tank to reach -100 kPa, then extraction is injected by the use of subcritical fluids as extractant into extractor, will locate in advance
Material samples after reason are totally submerged, and add ethanol solution as being extracted after entrainer；It is after extraction terminates, liquid is molten
Agent is pumped into evaporator, and constant temperature carrying out precipitation treatment is carried out respectively to material samples and liquid flux, that is, respectively obtains the material after extraction
Sample and sample extraction thing；
Step 3）Removal of impurities：The sample extraction thing of gained enters after impurity is more, it is necessary to carry out removal of impurities processing sometimes again after extraction
Row counterextraction, removal of impurities processing procedure is any of following, and sample extraction thing obtained by after a, extraction is with 10 times of 95% ethanol 50
Back dissolving is heated at DEG C, 24 h are freezed under the conditions of -30 DEG C, is filtered, the recovered solvent of gained supernatant produces the sample after purification
Extract；B, molecular distillation：The ml/min of charging rate 0.8~1.0, the Pa of vacuum 15~20,60 DEG C of heating-up temperature, cooling
10~12 DEG C of temperature, the r/min of rotating speed 260；C, gained sample extraction takes thing to be dissolved with 6 times of amount water, in the condition of temperature 45 C
Under, the h of magnetic agitation 1, stratification, supernatant liquid pours out from the suitable for reading of separatory funnel, and opening cock makes lower floor's liquid from liquid separation
Mouth is released under funnel, collects lower floor's liquid, is concentrated into the sample extraction thing that density produces purification for 1.2 g/ml；
Step 4）Counterextraction：By the sample extraction thing after purification and the discarded tobacco leaf for needing to carry out counterextraction by 1:1~
500 g/g mass ratio together inserts subcritical counterextraction tank, vacuumizes until vacuum reaches -100 kPa in counterextraction tank,
Then counterextraction is injected into counterextraction tank and is used as counterextraction solvent by the use of subcritical fluids, it would be desirable to carry out the low-quality tobacco of counterextraction
Leaf is totally submerged, and injects counterextraction with counterextraction is carried out after entrainer, after counterextraction terminates, is carried out constant temperature to counterextraction tank and is taken off
Molten processing, precipitation terminate to obtain the discarded tobacco leaf after counterextraction processing.
Step 1）Described in dried material samples moisture content below 10%.
Step 1）Described in breaking-wall cell processing be following processing procedure in one kind, a, microwave frequency measurment are dried
Tobacco leaf moistens water 25% by weight, and microwave treatment is carried out after the min of sealing and standing 40；Microwave condition be power 800 W, 30 s twice,
Per the s of minor tick 10；B, supersonic wave wall breaking, dried tobacco leaf moisten water 300%, ultrasound are carried out after the min of sealing and standing 60 by weight
Ripple processing；Ultrasonic Conditions are the W of power 500, the min of time 60；C, Terahertz broken wall, dried tobacco leaf moisten water by weight
Terahertz processing is carried out after 25%, the min of sealing and standing 40, Terahertz treatment conditions are 30 DEG C of temperature, the cm of distance 10, the time 10
min；D, broken wall is crushed, 100 mesh sieves are crossed after dried tobacco leaf is crushed.
Step 2）Described in pretreated material samples and extractant mass volume ratio be 1:10~20 g/
Ml, and volume is the 0~15% of material samples and extractant cumulative volume, concentration is 50~95% ethanol solution is added as extraction
Take entrainer, extraction time is 10~30 minutes, and temperature is 20~50 DEG C, and pressure is 0.25~0.9 Mpa, cycling extraction 3
~4 times.
Step 4）Described in sample extraction thing and need carry out counterextraction discarded tobacco leaf quality summation and counterextraction
The ratio of the volume of solvent is 1:20~40 g/ml, and add volume for material samples and counterextraction total solvent volume 0~
15%th, for the ethanol solution that concentration is 50~95% as counterextraction entrainer, the time is 30~40 minutes, and temperature is 20~50
DEG C, pressure is 0.25~0.9 Mpa.
Described material samples include chrysanthemum, tree moss, jujube, fennel seeds, dandelion, hawthorn, rose, raisins, cucurbit
Bar, one kind in the natural plants such as tobacco.
Described extractant is at least one of propane, butane, HFC-134a, dimethyl ether and liquefied ammonia.
Described counterextraction solvent is at least one of propane, butane, dimethyl ether and HFC-134a.
Liquid flux directly can be pumped into counterextraction tank and carry out inverse extraction without evaporating carrying out precipitation treatment after the completion of the extraction
Processing is taken, now counterextraction tank domestic demand places discarded tobacco leaf and is pumped through vacuum in advance.
The solvent gas evaporated in subcritical abstraction and counterextraction the process materials sample and liquid flux, through overvoltage
Contracting condensation, the solvent of liquid flow back to solvent storage tank, recycle.
The positive effect of the present invention is：
Subcritical abstraction technology is to utilize subcritical abstraction solvent, closed, anaerobic, low pressure extractor in, according to having
The similar principle to mix of machine thing, by extracting material and molecule diffusion process of the extractant in extraction process, make in material
Active skull cap components be transferred in the extractant of liquid, then by the process of reduction vaporization by extractant and purpose product
Separation, finally give a kind of novel extraction and isolation technics of purpose product.Subcritical abstraction technology compares other separation methods
There are many advantages:It is nontoxic, harmless, environmentally friendly, pollution-free, non-thermal technology, do not destroy Product Activity, anti-oxidation, production capacity is big, can
Industrialization large-scale production, energy-conservation, operating cost are low, are easy to separate with product, have very wide application prospect.
Subcritical counterextraction is the inverse process of subcritical abstraction, is referred under undercritical conditions, using by extraction component in Asia
Motion in critical fluids, optionally material is inversely diffused into inside material, realizes the change of material internal component or make
A kind of new technology that composition in different material swaps.Using subcritical counterextraction technology, discarded tobacco leaf one can be assigned
Determine the delicate fragrance of degree, the fragrance of a flower, cream perfume, fruity, herbal, bakee perfume, Xin Xiang, the fragrant and sweet and banksia rose so that discarded tobacco leaf is sample
Cigarette in aroma quality, perfume quantity, concentration, miscellaneous gas, strength, excitant, pleasant impression, flammability and grey etc., relatively control and
Lifting different degrees of Yan Junyou.
Embodiment
A kind of counterextraction method for lifting discarded tobacco leaf quality, comprises the following steps：
Step 1）Pretreatment：The material samples for needing to be extracted are dried and breaking-wall cell is handled；Material samples
Including one in the natural plants such as chrysanthemum, tree moss, jujube, fennel seeds, dandelion, hawthorn, rose, raisins, faenum graecum, tobacco
Kind, for the moisture content of dried material samples below 10%, breaking-wall cell processing is one kind in following processing procedure, a, micro-
Ripple broken wall, dried tobacco leaf moisten water 25%, microwave treatment are carried out after the min of sealing and standing 40 by weight；Microwave condition is power
800 W, 30 s twice, per minor tick 10 s；B, supersonic wave wall breaking, dried tobacco leaf moisten water 300%, sealing and standing by weight
Ultrasonication is carried out after 60 min；Ultrasonic Conditions are the W of power 500, the min of time 60；C, Terahertz broken wall, it is dried
Tobacco leaf moistens water 25% by weight, and Terahertz processing is carried out after the min of sealing and standing 40, and Terahertz treatment conditions are 30 DEG C of temperature, away from
From 10 cm, the min of time 10；D, broken wall is crushed, 100 mesh sieves are crossed after dried tobacco leaf is crushed；
Step 2）Extraction：By step 1）Pretreated material samples are placed in closed extractor, are vacuumized until extraction
Take vacuum in tank to reach -100 kPa, then extraction is injected by the use of subcritical fluids as extractant into extractor, will locate in advance
Material samples after reason are totally submerged, and add ethanol solution as being extracted after entrainer, and extraction conditions is extractant
For at least one of propane, butane, HFC-134a, dimethyl ether and liquefied ammonia, pretreated material samples and extractant
Mass volume ratio is 1:10~20 g/ml, and add volume be the 0~15% of material samples and extractant cumulative volume, concentration be
50~95% ethanol solutions are as extraction entrainer, and extraction time is 10~30 minutes, and temperature is 20~50 DEG C, and pressure is
0.25~0.9 Mpa, cycling extraction 3~4 times；After extraction terminates, liquid flux is pumped into evaporator, to material samples and liquid
Solvent carries out constant temperature carrying out precipitation treatment respectively, that is, respectively obtains material samples and sample extraction thing after extraction；
Step 3）Removal of impurities：The sample extraction thing of gained enters after impurity is more, it is necessary to carry out removal of impurities processing sometimes again after extraction
Row counterextraction, removal of impurities processing procedure is any of following, and sample extraction thing obtained by after a, extraction is with 10 times of 95% ethanol 50
Back dissolving is heated at DEG C, 24 h are freezed under the conditions of -30 DEG C, is filtered, the recovered solvent of gained supernatant produces the sample after purification
Extract；B, molecular distillation：The ml/min of charging rate 0.8~1.0, the Pa of vacuum 15~20,60 DEG C of heating-up temperature, cooling
10~12 DEG C of temperature, the r/min of rotating speed 260；C, gained sample extraction takes thing to be dissolved with 6 times of amount water, in 450 DEG C of condition of temperature
Under, the h of magnetic agitation 1, stratification, supernatant liquid pours out from the suitable for reading of separatory funnel, and opening cock makes lower floor's liquid from liquid separation
Mouth is released under funnel, collects lower floor's liquid, is concentrated into the sample extraction thing that density produces purification for 1.2 g/ml；
Step 4）Counterextraction：By the sample extraction thing after purification and the discarded tobacco leaf for needing to carry out counterextraction by 1:1~
500 g/g mass ratio together inserts subcritical counterextraction tank, vacuumizes until vacuum reaches -100 kPa in counterextraction tank,
Then counterextraction is injected into counterextraction tank and is used as counterextraction solvent by the use of subcritical fluids, it would be desirable to carry out the low-quality tobacco of counterextraction
Leaf is totally submerged, and is injected counterextraction with counterextraction, the condition of counterextraction is carried out after entrainer and be, counterextraction solvent be propane,
At least one of butane, dimethyl ether and HFC-134a, the quality of discarded tobacco leaf of the sample extraction thing with needing to carry out counterextraction
The ratio of summation and the volume of counterextraction solvent is 1:20~40 g/ml, and it is material samples and counterextraction solvent to add volume
Cumulative volume 0~15%, the ethanol solution that concentration is 50~95% be used as counterextraction entrainer, the time is 30~40 minutes, warm
Spend for 20~50 DEG C, pressure is 0.25~0.9 Mpa, and after counterextraction terminates, constant temperature carrying out precipitation treatment, precipitation are carried out to counterextraction tank
Terminate to obtain the discarded tobacco leaf after counterextraction processing.
Liquid flux directly can be pumped into counterextraction tank and carried out at counterextraction without evaporating carrying out precipitation treatment after the completion of extraction
Reason, now counterextraction tank domestic demand places discarded tobacco leaf and is pumped through vacuum in advance；Subcritical abstraction and counterextraction process materials sample
With the solvent gas evaporated in liquid flux, by compression condensation, the solvent of liquid flows back to solvent storage tank, recycles.
Embodiment 1
The g of chu chrysanthemum sample 50 is taken, 100 mesh sieves is crossed after drying and crushing, is placed in extractor, vacuumizes until vacuum in tank
Reach -100 kPa, subcritical fluids butane then injected into extractor as extractant, chu chrysanthemum sample is totally submerged,
The mass volume ratio 1 of chu chrysanthemum sample and subcritical fluids butane:10 g/ml, extraction entrainer are 95% ethanol water,
Entrainment 5%, extraction time are 20 min, and temperature is 25 DEG C, the Mpa of pressure 0.25, cycling extraction 3 times；After extraction terminates, by liquid
Body solvent is pumped into evaporator, carries out constant temperature carrying out precipitation treatment respectively to chu chrysanthemum sample and liquid flux, that is, obtains chu chrysanthemum extract.
Above-mentioned chu chrysanthemum extract is heated into back dissolving at 50 DEG C with 10 times of 95% ethanol, 24 h are freezed under the conditions of -30 DEG C,
Filtering, the recovered solvent of gained supernatant produce the chu chrysanthemum extract of purification；The chu chrysanthemum extract of the purification is detected through GC-MS and tied
Fruit is as shown in table 1, and the composition in the chu chrysanthemum extract of purification mainly includes alkenes, alcohols, ketone, esters and acids, content compared with
High material includes the borneol that content is 21.33%, 12.62% β-selinene and 11.46% gurjunene.
The GC-MS analysis results of the chu chrysanthemum essential oil of table 1
The chu chrysanthemum extract of the above-mentioned purifications of 1 g is taken, counterextraction tank is together inserted with 500 g BK31 discarded tobacco leafs, is taken out true
BK31 discarded tobacco leafs are totally submerged, chu chrysanthemum extract and BK31 are low by sky, injection subcritical fluids butane as counterextraction solvent
The mass volume ratio of hypo-tobacco leaf and counterextraction solvent is 1:20 g/ml, keeping temperature are 30 DEG C, 35 min are stood, to counterextraction
Tank carries out slow evaporation carrying out precipitation treatment, 30 DEG C of evaporating temperature, and precipitation terminates to obtain the BK31 discarded tobacco leafs after counterextraction.
The counterextraction tobacco leaf cigarette sensory evaluation of table 2
The Analyses Methods for Sensory Evaluation Results of tobacco leaf is as shown in table 2 after processing, and maximum standard degree is that 9,9 representatives are fine in table, and 8 represent
Good, 7 represent preferable, and 6 represent slightly good, and during 5 represent, 4 represent slightly worse, and 3 represent poor, and 2 represent poor, and 1 represents very poor, is seen by result
Aroma quality, perfume quantity, concentration, miscellaneous gas, strength, excitant, pleasant impression, flammability and the grey for going out cigarette after counterextraction relatively compare and
Lifting different degrees of Yan Junyou, especially perfume quantity and concentration all improve 2 grades than control.In addition, after counterextraction
It is more a certain degree of delicate fragrance when sample aspirates, the fragrance of a flower, cream perfume, fruity, herbal, baking perfume, Xin Xiang, fragrant and sweet
And the banksia rose, wherein delicate fragrance, fruity, baking perfume, Xin Xiang and fragrant and sweet note are more apparent.
Embodiment 2
The g of dandelion 100, microwave frequency measurment are taken, dried tobacco leaf moistens water 25%, carried out after the min of sealing and standing 40 by weight
Microwave treatment；Microwave condition twice, per the s of minor tick 10, is placed in extractor after microwave treatment, taken out for power 800 W, 30 s
Vacuum until in extractor vacuum reach -100 kPa, subcritical fluids dimethyl ether and tetrafluoro second are then injected into extractor
The volume ratio of alkane is 1:Dandelion is totally submerged, the mass body of dandelion and extractant by 1 mixed liquor as extractant
Product is than being 1:20 g/ml, entrainer are 200 ml 50% ethanol, and extraction time is 10 min, and temperature is 20 DEG C, pressure 0.60
Mpa, cycling extraction 3 times；After extraction terminates, liquid flux is pumped into evaporator, perseverance is carried out respectively to dandelion and liquid flux
Warm carrying out precipitation treatment, 20 DEG C of temperature, dandelion extract is produced after liquid flux precipitation.
Gained dandelion extract carries out molecular distillation：The ml/min of charging rate 1.0, the Pa of vacuum 20, heating-up temperature
60 DEG C, 10 DEG C of chilling temperature, the r/min of rotating speed 260, molecular distillation terminates the dandelion extract being purified, the purification
Dandelion extract detects through GC-MS, as a result as shown in table 3, main component in the dandelion extract of purification include aldehydes,
Ketone, alcohols, alkenes and ester type compound, the higher material of content include content be 10.32% octanoic acid, 9.48% it is trans-
2- decenals and 8.02% trans -2- heptenals.
The dandelion essential oil GC-MS testing results of table 3
The g of dandelion extract 1 purified obtained by molecular distillation and 400 g Luoyang B011 tobacco leaves are together inserted into counterextraction
Tank, vacuumize, the volume ratio for injecting subcritical fluids dimethyl ether and HFC-134a is 1:1 mixed liquor as counterextraction solvent,
Tobacco leaf is totally submerged by counterextraction solvent, and the mass volume ratio of tobacco leaf and counterextraction solvent is 1:30 g/ml, entrainer 75%
The ml of ethanol 600, keeping temperature be 20 DEG C, stand 30 min, the Mpa of pressure 0.55, to counterextraction tank carry out slow evaporation take off
Molten processing, 20 DEG C of evaporating temperature, precipitation terminate to obtain the B011 tobacco leaves after counterextraction.
The counterextraction tobacco leaf cigarette sensory evaluation of table 4
Tobacco leaf sense organ product are more as shown in table 4 than result, and maximum standard degree is 9,9 to represent fine in table, and 8 represent, 7 representatives compared with
Good, 6 represent slightly good, and during 5 represent, 4 represent slightly worse, and 3 represent poor, and 2 represent poor, and 1 represents very poor, is found out by result, counterextraction
The aroma quality of tobacco shred cigarette is significantly improved, miscellaneous gas is reduced, makes flue gas finer and smoother, soft, mellow and full, reduces oral area, throat, nose
Portion stimulates, in terms of perfume quantity, flue gas concentration is improved, improve hair property, strength, pleasant impression thoroughly, especially in terms of concentration and excitant,
It has been obviously improved effect.
Embodiment 3
The g of Zimbabwe's tobacco leaf 60, supersonic wave wall breaking are taken, dried tobacco leaf moistens water 300%, sealing and standing 60 by weight
Ultrasonication is carried out after min；Ultrasonic Conditions are the W of power 500, the min of time 60；Extraction is placed in after supersonic wave wall breaking processing
In tank, vacuumize until vacuum reaches -100 kPa in tank, subcritical fluids butane is then injected into extractor is used as extraction
Solvent is taken, Zimbabwe's tobacco leaf is totally submerged by extractant, and the mass volume ratio of Zimbabwe's tobacco leaf and extractant is 1:
15 g/ml, entrainer are the ml of 75% ethanol 50, and extraction time is 30 min, and temperature is 50 DEG C, and the Mpa of pressure 0.90, extraction follows
Number of rings 3 times；After extraction terminates, liquid flux is pumped into evaporator, constant temperature is carried out respectively to Zimbabwe's tobacco leaf and liquid flux
Carrying out precipitation treatment, 25 DEG C of temperature, leaf tobacco extract is produced after liquid flux precipitation.
Gained leaf tobacco extract cleans：Leaf tobacco extract is dissolved with 6 times of amount water, and under conditions of temperature 45 C, magnetic force stirs
1 h, stratification are mixed, supernatant liquid is poured out from the suitable for reading of separatory funnel, and opening cock makes lower floor's liquid mouth under separatory funnel
Release, collect lower floor liquid, it be 1.2 g/ml to be concentrated into density, that is, the leaf tobacco extract being purified, and the tobacco leaf of purification extracts
Thing detects through GC-MS, and as a result as shown in table 5, the main component in the leaf tobacco extract of purification includes ketone, esters, alcohols, alkene
Class and nicotine, the higher material of content include the neophytadiene that content is 64.98%, the nicotine that content is 21.35% and content and are
2.88% 7,10,13- hexadecatrienoic acid methyl esters.
The Zimbabwe's tobacco leaf essential oil GC-MS testing results of table 5
The leaf tobacco extract of the above-mentioned purifications of 0.5 g and Luoyang BK31 tobacco leaves are together inserted into counterextraction tank, vacuumized, is injected
Luoyang BK31 tobacco leaves are totally submerged, Luoyang BK31 tobacco leaves and counterextraction solvent by subcritical fluids butane as counterextraction solvent
Mass volume ratio be 1:32 g/ml, entrainer are the ml of 95% ethanol 16, and keeping temperature is 50 DEG C, the Mpa of pressure 0.60, is stood
40 min, slow evaporation carrying out precipitation treatment is carried out to counterextraction tank, 20 DEG C of evaporating temperature, precipitation terminates after obtaining counterextraction
BK31 tobacco leaves.
The counterextraction tobacco leaf cigarette sensory evaluation of table 6
Cigarette sense organ product are more as shown in table 6 than result, and maximum standard degree is 9,9 to represent fine in table, and 8 represent, 7 representatives compared with
Good, 6 represent slightly good, and during 5 represent, 4 represent slightly worse, and 3 represent poor, and 2 represent poor, and 1 represents very poor, is found out by result, counterextraction
Improve the aroma quality of cigarette, perfume quantity, concentration, the strength that improves, pleasant impression, reduce miscellaneous gas, increase thoroughly hair property, make flue gas more refinement
It is greasy, soft, mellow and full, oral area, throat, especially nose stimulation, cigarette concentration and miscellaneous gas are reduced, improves 2 grades.
Embodiment 4
The g of Zimbabwe's tobacco leaf 60, Terahertz broken wall are taken, dried tobacco leaf moistens water 25%, sealing and standing 40 by weight
Terahertz processing is carried out after min, Terahertz treatment conditions are 30 DEG C of temperature, the cm of distance 10, the min of time 10；Terahertz broken wall
It is placed in after processing in extractor, vacuumizes until vacuum reaches -100 kPa in tank, then injected into extractor subcritical
Zimbabwe's tobacco leaf is totally submerged by fluid butane as extractant, extractant, Zimbabwe's tobacco leaf and extractant
Mass volume ratio is 1:15 g/ml, entrainer are the ml of 75% ethanol 50, and extraction time is 30 min, and temperature is 50 DEG C, pressure
0.90 Mpa, extraction cycle number 3 times；After extraction terminates, liquid flux is pumped into evaporator, it is molten to Zimbabwe's tobacco leaf and liquid
Agent carries out constant temperature carrying out precipitation treatment respectively, 25 DEG C of temperature, and leaf tobacco extract is produced after liquid flux precipitation.
Gained leaf tobacco extract cleans：Leaf tobacco extract is dissolved with 6 times of amount water, and under conditions of temperature 45 C, magnetic force stirs
1 h, stratification are mixed, supernatant liquid is poured out from the suitable for reading of separatory funnel, and opening cock makes lower floor's liquid mouth under separatory funnel
Release, collect lower floor liquid, it is 1.2 g/ml to be concentrated into density, that is, the leaf tobacco extract being purified, by the above-mentioned purifications of 0.5 g
Leaf tobacco extract and Luoyang BK31 tobacco leaves together insert counterextraction tank, vacuumize, injection subcritical fluids butane is as inverse extraction
Solvent is taken, Luoyang BK31 tobacco leaves are totally submerged, the mass volume ratio of Luoyang BK31 tobacco leaves and counterextraction solvent is 1:40 g/
Ml, entrainer are the ml of 50% ethanol 16, and keeping temperature is 50 DEG C, the Mpa of pressure 0.60, stands 30 min, counterextraction tank is carried out
Slow evaporation carrying out precipitation treatment, 20 DEG C of evaporating temperature, precipitation terminate to obtain the BK31 tobacco leaves after counterextraction.
Embodiment 5
The g of dandelion 100, microwave frequency measurment are taken, dried tobacco leaf moistens water 25%, carried out after the min of sealing and standing 40 by weight
Microwave treatment；Microwave condition twice, per the s of minor tick 10, is placed in extractor after microwave treatment, taken out for power 800 W, 30 s
Vacuum until in extractor vacuum reach -100 kPa, subcritical fluids dimethyl ether and tetrafluoro second are then injected into extractor
The volume ratio of alkane is 1:Dandelion is totally submerged, the mass body of dandelion and extractant by 1 mixed liquor as extractant
Product is than being 1:20 g/ml, entrainer are 200 ml 50% ethanol, and extraction time is 10 min, and temperature is 20 DEG C, pressure 0.60
Mpa, cycling extraction 3 times；After extraction terminates, liquid flux is pumped into evaporator, perseverance is carried out respectively to dandelion and liquid flux
Warm carrying out precipitation treatment, 20 DEG C of temperature, dandelion extract is produced after liquid flux precipitation.
Gained dandelion extract carries out molecular distillation：The ml/min of charging rate 0.9, the Pa of vacuum 17, heating-up temperature
60 DEG C, 11 DEG C of chilling temperature, the r/min of rotating speed 260, molecular distillation terminates the dandelion extract being purified, molecule steamed
The g of dandelion extract 1 and 400 g Luoyang B011 tobacco leaves for evaporating gained purification together insert counterextraction tank, vacuumize, injection is sub-
The volume ratio of critical fluids dimethyl ether and HFC-134a is 1:1 mixed liquor is as counterextraction solvent, and counterextraction solvent is by tobacco leaf
It is totally submerged, the mass volume ratio of tobacco leaf and counterextraction solvent is 1:30 g/ml, entrainer are 75% ml of ethanol 600, are kept
Temperature is 20 DEG C, stands 30 min, the Mpa of pressure 0.9, and slow evaporation carrying out precipitation treatment, evaporating temperature 20 are carried out to counterextraction tank
DEG C, precipitation terminates to obtain the B011 tobacco leaves after counterextraction.
Embodiment 6
The g of chu chrysanthemum sample 50 is taken, 100 mesh sieves is crossed after drying and crushing, is placed in extractor, vacuumizes until vacuum in tank
Reach -100 KPa, subcritical fluids butane then injected into extractor as extractant, chu chrysanthemum sample is totally submerged,
The mass volume ratio 1 of chu chrysanthemum sample and subcritical fluids butane:10 g/ml, extraction entrainer are 95% ethanol water,
Entrainment 5%, extraction time are 20 min, and temperature is 25 DEG C, the Mpa of pressure 0.25, cycling extraction 3 times；After extraction terminates, by liquid
Body solvent is pumped into evaporator, carries out constant temperature carrying out precipitation treatment respectively to chu chrysanthemum sample and liquid flux, that is, obtains chu chrysanthemum extract.
Gained chu chrysanthemum extract carries out molecular distillation：The ml/min of charging rate 0.8, the Pa of vacuum 15, heating-up temperature 60
DEG C, 12 DEG C of chilling temperature, the r/min of rotating speed 260, molecular distillation terminates to produce the chu chrysanthemum extract of purification；Take the above-mentioned purifications of 1 g
Chu chrysanthemum extract, together insert counterextraction tank with 500 g BK31 discarded tobacco leafs, vacuumize, injection subcritical fluids butane is made
For counterextraction solvent, BK31 discarded tobacco leafs are totally submerged, the matter of chu chrysanthemum extract and BK31 discarded tobacco leafs and counterextraction solvent
It is 1 to measure volume ratio:20 g/ml, keeping temperature are 30 DEG C, the Mpa of pressure 0.25, stand 35 min, counterextraction tank are carried out slow
Carrying out precipitation treatment, 30 DEG C of evaporating temperature are evaporated, precipitation terminates to obtain the BK31 discarded tobacco leafs after counterextraction.
Claims (9)
- A kind of 1. counterextraction method for lifting discarded tobacco leaf quality, it is characterised in that comprise the following steps：Step 1）Pretreatment：The material samples for needing to be extracted are dried and breaking-wall cell is handled；Step 2）Extraction：By step 1）Pretreated material samples are placed in closed extractor, are vacuumized until extractor Interior vacuum reaches -100 kPa, then injects extraction by the use of subcritical fluids as extractant into extractor, after pretreatment Material samples be totally submerged, and add ethanol solution as being extracted after entrainer；After extraction terminates, liquid flux is taken out Enter evaporator, constant temperature carrying out precipitation treatment is carried out respectively to material samples and liquid flux, that is, respectively obtain the material samples after extraction With sample extraction thing；Step 3）Removal of impurities：Impurity is more, it is necessary to be carried out again after carrying out removal of impurities processing inverse sometimes for the sample extraction thing of gained after extraction Extraction, removal of impurities processing procedure is any of following, and sample extraction thing obtained by after a, extraction is with 10 times of 95% ethanol at 50 DEG C Back dissolving is heated, 24 h are freezed under the conditions of -30 DEG C, is filtered, the recovered solvent of gained supernatant produces the sample extraction after purification Thing；B, molecular distillation：The ml/min of charging rate 0.8~1.0, the Pa of vacuum 15~20,60 DEG C of heating-up temperature, chilling temperature 10~12 DEG C, the r/min of rotating speed 260；C, gained sample extraction takes thing to be dissolved with 6 times of amount water, under conditions of temperature 45 C, magnetic Power stirs 1 h, stratification, and supernatant liquid is poured out from the suitable for reading of separatory funnel, and opening cock makes lower floor's liquid from separatory funnel Lower mouth is released, and collects lower floor's liquid, is concentrated into the sample extraction thing that density produces purification for 1.2 g/ml；Step 4）Counterextraction：By the sample extraction thing after purification and the discarded tobacco leaf for needing to carry out counterextraction by 1:1~500 g/ G mass ratio together inserts subcritical counterextraction tank, vacuumizes until vacuum reaches -100 kPa, Ran Houxiang in counterextraction tank Injection counterextraction is used as counterextraction solvent by the use of subcritical fluids in counterextraction tank, it would be desirable to which the discarded tobacco leaf for carrying out counterextraction is complete Submergence, and counterextraction is injected with counterextraction is carried out after entrainer, after counterextraction terminates, counterextraction tank is carried out at constant temperature precipitation Reason, precipitation terminate to obtain the discarded tobacco leaf after counterextraction processing.
- 2. the counterextraction method of lifting discarded tobacco leaf quality according to claim 1, it is characterised in that：Step 1）Middle institute The moisture content for the dried material samples stated is below 10%.
- 3. the counterextraction method of lifting discarded tobacco leaf quality according to claim 1, it is characterised in that：Step 1）Middle institute The breaking-wall cell processing stated moistens water 25% by weight for one kind in following processing procedure, a, microwave frequency measurment, dried tobacco leaf, Microwave treatment is carried out after the min of sealing and standing 40；Microwave condition is the W of power 800, the s of microwave time 30, is repeated twice, often The s of minor tick 10；B, supersonic wave wall breaking, dried tobacco leaf moisten water 300%, ultrasonic wave are carried out after the min of sealing and standing 60 by weight Processing；Ultrasonic Conditions are the W of power 500, the min of time 60；C, Terahertz broken wall, dried tobacco leaf moisten water 25% by weight, Terahertz processing is carried out after the min of sealing and standing 40, Terahertz treatment conditions are 30 DEG C of temperature, the cm of distance 10, the min of time 10； D, broken wall is crushed, 100 mesh sieves are crossed after dried tobacco leaf is crushed.
- 4. the counterextraction method of lifting discarded tobacco leaf quality according to claim 1, it is characterised in that：Step 2）Middle institute The pretreated material samples and the mass volume ratio of extractant stated are 1:10~20g/ml, and it is material sample to add volume Product and extractant cumulative volume 0~15%, the ethanol solution that concentration is 50~95% be as extraction entrainer, extraction time 10~30 minutes, temperature was 20~50 DEG C, and pressure is 0.25~0.9 Mpa, cycling extraction 3~4 times.
- 5. the counterextraction method of lifting discarded tobacco leaf quality according to claim 1, it is characterised in that：Step 4）Middle institute The quality summation of discarded tobacco leaf of the sample extraction thing stated with needing to carry out counterextraction and the ratio of volume of counterextraction solvent are 1:20~40 g/ml, and add volume be the 0~15% of material samples and counterextraction total solvent volume, concentration be 50~95% For ethanol solution as counterextraction entrainer, the time is 30~40 minutes, and temperature is 20~50 DEG C, and pressure is 0.25~0.9 Mpa。
- 6. according to the counterextraction method of any described lifting discarded tobacco leaf qualities of claim 1-4, it is characterised in that：Described Material samples include one in chrysanthemum, tree moss, jujube, fennel seeds, dandelion, hawthorn, rose, raisins, faenum graecum, tobacco Kind.
- 7. the counterextraction method of the lifting discarded tobacco leaf quality according to claim 1 or 4, it is characterised in that：Described extraction Solvent is taken to include at least one of propane, butane, HFC-134a, dimethyl ether and liquefied ammonia.
- 8. the counterextraction method of discarded tobacco leaf quality is lifted according to claim 1 or 5, it is characterised in that：Described is inverse Extractant includes at least one of propane, butane, dimethyl ether and HFC-134a.
- 9. the counterextraction method of lifting discarded tobacco leaf quality according to claim 1, it is characterised in that：The subcritical extraction Take and counterextraction process materials sample and liquid flux in the solvent gas that evaporate, by compression condensation, the solvent stream of liquid Back dissolving developing agent storage tank, recycle.
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| CN107224750A (en) * | 2017-07-28 | 2017-10-03 | 寸洪明 | A kind of rose quintessence low-temperature extraction and rose quintessence ceramic membrane filter technique |
| CN108251218B (en) * | 2018-02-11 | 2021-06-15 | 安阳工学院 | Method for extracting artemisia vulgaris essential oil with high selectivity |
| CN108125277B (en) * | 2018-03-21 | 2021-03-05 | 福建中烟工业有限责任公司 | Electronic cigarette and manufacturing method thereof |
| CN109275947B (en) * | 2018-10-08 | 2021-10-15 | 浙江中烟工业有限责任公司 | Supercritical extraction treatment method suitable for tobacco shreds in heating and non-combustion state |
| CN109846076B (en) * | 2018-12-12 | 2022-09-13 | 云南中烟工业有限责任公司 | Method for improving quality of low-applicability tobacco leaves |
| CN112315016A (en) * | 2020-11-19 | 2021-02-05 | 河南中烟工业有限责任公司 | Method for processing selected raw tobacco |
| CN112369648A (en) * | 2020-12-03 | 2021-02-19 | 湖北中烟工业有限责任公司 | Method for leaching raw materials of paper-making reconstituted tobacco |
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Effective date of registration: 20210611 Address after: No.16, Yulin South Road, Zhengzhou, Henan 450000 Patentee after: CHINA TOBACCO HENAN INDUSTRIAL Co.,Ltd. Patentee after: Zhengzhou Zhengda medicine and food Health Research Institute Co.,Ltd. Address before: No.16, Yulin South Road, Zhengzhou, Henan 450000 Patentee before: CHINA TOBACCO HENAN INDUSTRIAL Co.,Ltd. Patentee before: Zhengzhou University |