CN105249526B - Method for extracting tobacco aroma component through water jet comminution and entrainment-type microwave distillation - Google Patents

Method for extracting tobacco aroma component through water jet comminution and entrainment-type microwave distillation Download PDF

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Publication number
CN105249526B
CN105249526B CN201510732476.9A CN201510732476A CN105249526B CN 105249526 B CN105249526 B CN 105249526B CN 201510732476 A CN201510732476 A CN 201510732476A CN 105249526 B CN105249526 B CN 105249526B
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nicotiana tabacum
aroma component
filter screen
microwave
clamping
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CN105249526A (en
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叶菁
胡汉华
孙春毅
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Wuhan Newway Pharmaceutical Machinery Co., Ltd.
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WUHAN NEWWAY CHENCHUANG TECHNOLOGY DEVELOPMENT Co Ltd
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Abstract

The invention relates to a method for extracting a tobacco aroma component through water jet comminution and entrainment-type microwave distillation. The method comprises the following steps: S1, adding comminuted raw materials used for extraction of the tobacco aroma component into a stirring tank, adding water, stirring the mixture, and conveying the stirred mixture to a centrifugal separator; S2, conveying a heavy component separated out from the mixture to a water jet mill for water jet milling; S3, conveying a light component solution obtained in step S2 to a feed opening in the upper end of a continuous entrainment-type thin-material-layer microwave evaporation device, and then conveying the light component solution through a microwave resonant cavity in a horizontal back-and-forth and layer-by-layer rising manner, wherein an upper filter screen belt-solid/liquid mixed material layer-lower filter screen belt wafer material layer structure is formed through two filter screen belts; S4, sucking a gas-phase aroma-source substance together with steam into a condenser, condensing the gas-phase aroma-source substance together with steam into a liquid, and then separating the gas-phase aroma-source substance from condensation water by utilizing the separator, so as to obtain the liquid tobacco aroma component. The method is a pure physical method capable of extracting the high-quality tobacco aroma component through cell disruption and distillation.

Description

The method that nappe flip length and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component
Technical field
The present invention relates to technical field of cigarette production, more particularly, it relates to a kind of nappe flip length and entrainment type micro-wave The method of distillation extraction Nicotiana tabacum L. aroma component.
Background technology
As people are gradually stepped up with health problem attention rate to smoking, and the continuous of dynamics that public place is banned on opium-smoking and the opium trade Increase, tobacco industry while reducing tar and reducing harm engineering is implemented starts to pay much attention to non-burning low temperature cigarette, electronic cigarette and mouth containing The novel tobacco such as cigarette product is researched and developed, and great as strategic, the of overall importance and long-range nature of relation industry value chain Problem is carried out.
Reducing tar and reducing harm engineering, makes the coal-tar middle oil content of Medicated cigarette constantly reduce, and the fragrance component in Nicotiana tabacum L. is also accordingly reduced, smoke It is thin out, the experience to smoking is affected, accordingly, it would be desirable to extract aroma component from Nicotiana tabacum L. effectively be mended to low-coke tar cigarette fragrance Repay;In novel tobacco product is constituted, Nicotiana tabacum L. this Studies of The Aromatic Substances is including including smog substrate, forming the peculiar fragrance institute of Nicotiana tabacum L. not The material that can or lack, needs extract aroma component from Nicotiana tabacum L.;On the other hand, the reconstituted tobacco course of processing of rising in recent years In, a part of this Studies of The Aromatic Substances of Nicotiana tabacum L. of loss is compensated by adding Nicotiana tabacum L. endogenouss spice, it is also desirable to extract from Nicotiana tabacum L. and cause Fragrant composition;Additionally, by the extraction to Nicotiana tabacum L. aroma component, can comprehensively utilize and dissolve Nicotiana tabacum L. accumulating and production of cigarettes process In a large amount of scraps for producing, scarp, cabo, tobacco cut, and abandon the appreciable discarded tobacco leaf in field every year, not only subtract Few pollution of the garbage to environment, while and can turn waste into wealth.
The alcohols main by contained by which of the distinctive aroma component of Nicotiana tabacum L., aldehydes, ketone, esters, acids, ethers, saccharide, terpene The Trace Volatile Organic Compounds composition of the Nicotiana tabacum L.s such as alkenes, amino acidses, alkaloid and heterocyclic compound.These volatile organic matters Typically based on primary metabolite such as cellulose, pectin, protein, hemicellulose etc., tobacco plant cell is distributed in In interior and intercellular substance, in dissolution, it is necessary to first could discharge through cell wall and cell membrane.But usual herbaceous plant vascular bundle The phloem tissue of the xylem in middle outside and inner side is tightr, solvent is difficult to permeate and is spread, and the aroma component of Nicotiana tabacum L. is difficult To be efficiently extracted.
In order to efficiently extract the aroma component of Nicotiana tabacum L., cell wall breaking process can be carried out to tobacco plant first, in order to These volatility perfume source materials being capable of smoothly dissolution in a solvent.
In order to realize, to tobacco plant cell breaking cellular wall purpose, in the art, various known methods being adopted:Such as, it is raw Substance treating method, is degraded to the cell wall of Nicotiana tabacum L. by enzyme or bacterium, it is understood that there may be problem be that alone enzyme is past Toward processing not thoroughly, can only Partial digestion cell wall;Alone bacterium process time is longer, cell wall thoroughly clear up and bacterium metabolite The quality of fragrant source material may be affected, the time is short and can not achieve the goal.
And for example, physical treatment method, makes cell wall breaking by method sides such as ultrasound wave, microwave, steam explosions.Wherein, surpass Sound wave cell wall breaking is that the cavitation Erosion that produced in liquid using high-frequency ultrasonic and size degradation effect crush cell wall, Possible problem is constrained to ultrasonic transducer power, and disposal ability is not big enough;Microwave frequency measurment is using the plant in microwave field During thing Absorption of Medium microwave energy, because intracellular molecular polarization produces dipole Action of Superhigh Frequency Vibration, friction and heat, work as liquid phase After absorbing enough latent heat gasifications, break through cell wall disengaged vapor and reach cell wall breaking purpose, possible problem is tobacco plant Fragrant source material deteriorate because overheated;Steam explosion be using with certain pressure steam enter plant cell in after, because dash forward So pressure release makes steam release cause cell wall breaking, possible problem to remain overheated.Physical treatment method processes intensity greatly, causes fragrant Component damages are larger.
For another example, chemical treatment method, is mainly processed by diluted acid, alkali, ozone, organic solvent and oxidation etc., makes cell wall Intensity decreases are cleared up, it is understood that there may be problem be these chemical composition later stage reluctant problems.
Another kind of solvent extraction method, can be under conditions of cell broken wall treatment not be done, using material dissolving in a solvent Sex differernce, that is, select to not needing dissolved element dissolubility little, and the solvent big to fragrant source Solubility of Substances, by solvent to thin The osmosiss of cell wall enter intracellular, dissolving solubility perfume source material, cause the concentration difference that cell is inside and outside, make intracellular Constantly to external diffusion, solvent is then constantly entered in cell concentrated solution, until when the inside and outside solution concentration of cell reaches dynamic equilibrium, Saturated solution is leached, novel solvent is added and is continued dissolution.Solvent can be highly polar water, or hydrophilic or lipophilic The organic solvent of property.Solvent extraction method is divided into two kinds of cold extraction method and hot lifting manipulation, common solvent extraction method relative poor, time Long, less efficient, aroma component relative amount is not high, and fragrance is not enough.
After cell makes fragrant source material dissolve in solvent because of breaking cellular wall or diffusion, then it is further desirable that the fragrant source of liquid phase Material is separated from solvent, i.e. distillation extraction.In the art, can be using various known methods:Such as, distillation extraction, It is different using each component boiling point (volatility) in mixing liquid, evaporate low boiling component, then it is whole to separate to be condensed into liquid Component.Wherein, the steam distillation with water as solvent, good economy performance, safe, strong operability, and to saccharide in Nicotiana tabacum L., The water solublity flavor matter such as amino acidses, phenols has a preferable extraction effect, but for low polarity, volatile organic acid, The key aroma component extraction effect such as terpenes, alcohols is not good, and needs higher evaporating temperature, and side reaction is more, may affect This fragrant effect of aroma component.
And for example, supercritical fluid CO2Extraction, the superpower solvability having using supercritical fluid make fragrant source material Dissolving, and the control by pressure and temperature, make CO2Solvent reaches critical point in extraction process, completes liquid phase to gas phase Hypercritical transition, and obtain the fragrant source material of liquid phase.The method purity is high, no solvent residue, is suitable for mostly non-in Nicotiana tabacum L. The extraction of the volatile aromatic composition of polarity or low pole, therefore in the existing more application in this area.But the method treating capacity is relatively low, Equipment investment is larger, relatively costly, low to the aromatic substance extraction yield of low volatility.
By above-mentioned analysis, the key technology for extracting aroma component from Nicotiana tabacum L. has at 2 points, and one is, realizes that cell breaks Wall;Two are, control when liquid-phase conversion is gas phase to evaporating temperature.The former is related to the dissolution of fragrant source material, the latter's relation To the quality of fragrant source material.
Nicotiana tabacum L. be Solanaceae herbaceous plant, can be used for extract Nicotiana tabacum L. aroma component tobacco-containing material be Nicotiana tabacum L. and root, stem etc., its In, Nicotiana tabacum L. is by arranging close flat epidermis cell, and the palisade tissue cell of mesophyll, spongy tissue cell and vascular bundle The parenchyma cells such as cell are constituted, and have collenchyma near epidermis;Rhizome is herb stem, and gather in stem many relatively tiny dimension pipes Beam, it is substantial amounts of parenchyma cell to be full of between vascular bundle, and in outer side, phloem is then distributed the xylem distribution in vascular bundle Inner side (this is just completely contrary with xylophyta).Therefore, if by the collenchyma of Nicotiana tabacum L. epidermis, and rhizome vascular bundle The phloem destruction of the xylem in outside and inner side, the breaking cellular wall of parenchyma cell is relative to be easier to realize.
In the art, the breaking cellular wall to tobacco plant cell, known method is by enzyme or bacterium as mentioned above Degradation, or acted on by the physical wall breaking of ultrasound wave, microwave, steam explosion, or the softening by soda acid solvent and clear up Effect is realized.In these methods, tobacco material is generally crushed to less than 5~20 mesh, that is, be smaller in size than 4000~830 μm with Under, minority is also crushed to below 100 mesh, i.e., 150 μm.Obviously, the crushing size of these tobacco materials is significantly larger than and generally plants The size range of the diameter of thing cell, i.e., 10~100 μm.Therefore, in existing Nicotiana tabacum L. aroma component extractive technique, to Nicotiana tabacum L. The crushing of raw material, does not produce the breaking cellular wall to cell and acts on.It is but by the degraded of above-mentioned enzyme or bacterium, or ultrasound wave, micro- The physical wall breaking of ripple, steam explosion, or cell wall breaking is made by the softening and the effect of clearing up of soda acid solvent, also thus cause phase The problem for answering cell wall breaking technique to bring, such as has that controllability is weaker, and sporoderm-broken rate is not high, or temperature is too high causes deterioration etc..
In the art, to the solution dissolved with Nicotiana tabacum L. perfume source material, the evaporating temperature control aspect of gas phase conversion is carried out, As mentioned above in known method, take including measures such as vapor distillation, normal-temperature distilled and vacuum distillations, but " of the same race Material has different saturated vapour pressures under not synthermal, and increases with the rising of temperature, and saturated vapour pressure value is higher, More be conducive to liquid phase to be changed into gas phase " evaporating principle and Nicotiana tabacum L. perfume source material " temperature is too high to cause deterioration " this association to contradiction In terms of tune, belong to mostly conventional technological balance, the principle in terms of relative shortage method and apparatus breaks through.
The patent below quoted from obtains certain success in terms of some method and apparatus wherein, but this can not be inevitably It is suitable to be construed to these existing technologies.
The Chinese patent CN 200610036630.X of Song Guangquan et al., disclose a kind of tobacco essence spice extracting method, Comprise the steps:Nicotiana tabacum L. is crushed or shredding, and is put into extractor;It is 1 by Nicotiana tabacum L. and solvent mass ratio:2~1:16, in extraction Solvent is added in taking tank;It it is 20~60 DEG C in temperature, vacuum is that decompression extract return method 1~8 is little under 0.020~0.098MPa When;80~500 mesh mesh screens of extract Jing or titanium rod core or ultrafiltration etc. separate, collect filtrate, vacuum be 0.020~ Under 0.098MPa, sample proportion d is evaporated to4 20For 1.1~1.4g/ml, tobacco essence spice is obtained final product.The invention is employed The closed circulating techniques such as low-temperature reduced-pressure liquid-solid extraction, gap flow stirring and concentrating under reduced pressure.
The Chinese patent CN 200680027774.7 of Philip Mirris Products Inc, discloses one kind and prepares containing cigarette The method of the solution of careless solute, including a kind of preferred extractant and supercritical fluid extraction tobacco solutes, is rich in being formed The Nicotiana tabacum L. of the extractant of tobacco solutes and depleted tobacco solutes, the extractant Jing entrapment solvents that will be enriched in tobacco solutes are rich in The solution of tobacco solutes is formed, wherein described tobacco solutes include nicotine and at least one tobacco flavor mixture and/or cigarette Careless aromatic.
The Chinese patent CN 200810237438.6 of Sun Deping et al., discloses a kind of tobacco sheets by paper making method production Extracting process, has following material in extract and its accounts for the percetage by weight of extract:Acid protease 0.02%~ 0.1%;Cellulase 0.01%~0.1%;Pectase 0.01%~0.1%;Enzyme activity accelerator 0.1%~1%.Acid egg White enzyme carries out liquid submerged fermentation and post processing, while using homemade enzyme activity accelerator.
The Chinese patent CN 200910027400.0 of yellow Wenhua et al., discloses a kind of preparation method of tobacco extract And its application, with Nicotiana tabacum L. as raw material, Jing enzymolysis, ultrasonic extraction, filtration, chromatography post separation, concentrating under reduced pressure step are obtained Nicotiana tabacum L. Extract;The tobacco extract ethanol of concentration 80% dissolves, and is added in tobacco shred using atomizing type spray.The invention is used Zymolysis technique and ultrasonic extraction, with reference to chromatography, Extracting temperature is low, and the time is short, and solvent load is few.
The Chinese patent CN 201110248504.1 of Wang Yuanliang et al., discloses a kind of using ultrasound wave alkalization pretreatment Continuous extraction nicotine, hemicellulose, lignin, the new method of cellulose from Nicotiana tabacum L., Nicotiana tabacum L. are ground into particle diameter no less than 20 mesh Powder, add the aqueous medium equivalent to 10~30 times of Nicotiana tabacum L. volume, adjust pH value to 9-13, and carry out ultrasonic pretreatment, surpass Acoustic power is no less than 20kHz, and ultrasonic pretreatment time is no less than 20 minutes, obtains ultrasonic pretreatment fluid, further extract cigarette Alkali, hemicellulose, lignin, cellulose.
The Chinese patent application publication No. CN 103126062A of Zhang Qi et al., discloses one and grows tobacco composition extracting method, Including:(1) 5~15 times of non-polar organic solvents are added by weight in Nicotiana tabacum L., stir, ultrasonic extraction 30~120 minutes, mistake Isolated extract is removed organic solvent and obtains oil-soluble tobacco extracts by filter;(2) to step (1) separating and extracting liquid Add 5~10 times of water in Nicotiana tabacum L. afterwards by weight, stir, ultrasonic extraction 30~60 minutes, filter, by isolated extraction Liquid removes water and obtains water solublity tobacco extracts, merges with the oil-soluble tobacco extracts of step (1).The method can be extracted The larger water-soluble components of polarity, can also extract the less oil soluble sexual element of polarity.
Yang Qian vivid et al. Chinese patent CN 201310177314.4, discloses and a kind of prepares cigarette perfume with tobacco chippings The method of material and the fragrance applications.By the use of tobacco chippings as raw material, tobacco extract is prepared by polar solvent extraction, by Nicotiana tabacum L. Extractum is mixed with macroporous resin and carries out static adsorption, after separating treatment, obtains unadsorbed latent fragrant component, by highly polar molten The flavor components of absorption are obtained after agent eluting macroporous resin.
The Chinese patent application publication No. CN 103462204A of Xu Qingquan et al., discloses a kind of including water extraction and super Critical CO2The reconstituted tobacco of compound tobacco flavor matter obtained in extraction, Nicotiana tabacum L. flavor matter are fixed from Nicotiana tabacum L. by water extraction To the polarity flavor matter and supercritical CO that extract2Extraction orients the nonpolar flavor matter of extraction from Nicotiana tabacum L. and constitutes, pole Property flavor matter and nonpolar flavor matter formula proportion be 1000:0.1~5.
The Chinese patent application publication No. CN 103484252A of Pan Xuesong et al., discloses a kind of Zimbabwe Nicotiana tabacum L. essence Extracting solution is prepared as concentrated extract, then adds glycerol to concentrated extract, finally carries out decompression steaming to which by the preparation method of oil Evaporate, liquid-liquid extraction and the step of concentration precipitation, obtain faint yellow Zimbabwe tobacco essential oil.
The Chinese patent application publication No. CN 103720031A of Tang Ziwen et al., discloses a kind of system of tobacco extract The application of Preparation Method and the extract in Medicated cigarette, takes tobacco material according to feed liquid mass ratio 1:5~1:10 ratio adds dense The ethanol of degree 70%~95%, adds the phosphoric acid or sulphuric acid of tobacco material quality 0.5%~3%, in 60~90 DEG C of bar Circumfluence distillation 1~3 hour under part;Products therefrom cools down supernatant after filtering, takes supernatant concentrating under reduced pressure, obtains extractum, i.e., For tobacco extract.
The Chinese patent application publication No. CN 103789090A of Yang Yaling et al., discloses the colored volatile matter that grows tobacco and carries Take and microcapsule preparation method, by Nicotiana tabacum L. chopping, weigh, add a certain amount of saliferous distilled water solution, soak certain hour, water Steam distillation is extracted, and is collected fraction, is obtained Nicotiana tabacum L. volatile matter.Again plus 95% ethanol dilution, and cyclodextrin and distilled water are added Mix homogeneously, grinds to form pastel, decompression sucking filtration with colloid mill, with absolute ethanol washing, the precipitation drying after sucking filtration.
The Chinese patent application publication No. CN 104138028A of Qu Yongsheng et al., discloses a kind of tobacco flavor composition and carries Method is taken, tobacco shred or Nicotiana tabacum L. is balanced into process or dried, is made sample moisture content uniform;By tobacco shred or Nicotiana tabacum L., it is put into After impregnating in Extraction solvent, cooling;Mixed liquor is put into into Ultrasonic Cell Disruptor, using ultrasonic grinding tobacco shred or Nicotiana tabacum L.;Crush cigarette After silk or Nicotiana tabacum L., sealing container, after continuing dipping, centrifugation removes solid formation, that is, obtain tobacco flavor constituents extraction liquid.
The Chinese patent application publication No. CN 104450186A of Liu Xinjian et al., discloses a kind of tobacco juice for electronic smoke cigarette Waste/hypo-tobacco leaf is placed in ultrasound-enhanced supercritical extraction equipment and is extracted by the preparation method of draft Studies of The Aromatic Substances, ultrasonic frequency 20KHz, ultrasonic power 100W, carbon dioxide flow are 10~20L/h, and extracting pressure is 15~25MPa, spends 40~55 DEG C, extraction The time is taken for 1.5~2h, entrainer is Propylene Glycol, ethanol, distillation water mixed solvent, and carbon dioxide is obtained with this Studies of The Aromatic Substances of Nicotiana tabacum L. Mixed liquor, then separated kettle separated, controls 45~60 DEG C of separation temperature, 7~12MPa of separating pressure, obtains Nicotiana tabacum L. this perfume Material.
Based on more than, analysis understands, in the art, does not still have a kind of wet grinding technique at present, its force side for crushing Formula not only has mill stripping and smashes effect, while having the direct broken cells of stretching action concurrently, and in the form of feed liquid film layer, leads to Cross microwave exposure heating, the method for carrying out distillation extraction Nicotiana tabacum L. aroma component.Accordingly, it is desired to provide a kind of by using to Nicotiana tabacum L. The suitable crushing force mechanism of plant material, makes tobacco plant cell obtain abundant breaking cellular wall, to improve the molten of Nicotiana tabacum L. perfume source material Xie Du;It is also expected to provide a kind of feed liquid for dissolved with Nicotiana tabacum L. perfume source material, using the equal material refining layer that continuously transports can be inverted, Microwave resonance intracavity returned the motion mode of rising in the past, under the bigger serface of multilamellar, by microwave exposure, to relatively thin material Layer carries out the vaporising device that body phase is uniformly heated, and realizes the high efficient cryogenic evaporation of Nicotiana tabacum L. aroma component.
The content of the invention
The technical problem to be solved in the present invention is, there is provided a kind of nappe flip length and strap-clamping-type microwave distillation extract Nicotiana tabacum L. The method of aroma component, realizes the high quality tobacco aroma component of cell wall breaking and distillation extraction with pure physical method.
The technical solution adopted for the present invention to solve the technical problems is:Construct a kind of nappe flip length and entrainment type micro-wave The method of distillation extraction Nicotiana tabacum L. aroma component, comprises the following steps:
S1, the extraction raw material of Nicotiana tabacum L. aroma component after crushing is added in agitator tank, after adding water stirring, delivers to centrifugation Seperator;
S2, the heavy thing after separation is delivered to into water fluid jet grind carries out nappe flip length;
S3, by step S2 obtain lightweight thing solution be delivered to the thin bed of material microwave evaporation device upper end of continuous strap-clamping-type Charge door, the microwave evaporation device, by two filter screen bands solid-liquid are mixed using the pinch upper roll and pinch under roll of a pair of revolutions Thing to being clipped between filter screen band, formed upper filter screen band, the solidliquid mixture bed of material and lower filter screen band to material folding Rotating fields, and with water The flat transfer ways for successively rising that come and go make the solidliquid mixture feed liquid in the layer to material folding, equal by microwave cavity Microwave energy is absorbed under even thin layer state and be heated evaporation;
S4, gas phase perfume source material are aspirated into condenser, and are condensed into liquid together with water vapour with steam Body;Make fragrant source material with condensed moisture from the Nicotiana tabacum L. aroma component of acquisition liquid by separator again.
In such scheme, water fluid jet grind makes Nicotiana tabacum L. by the impact of high-pressure water jet, water wedge tension force, cavitation denudation Mean diameter about < 5~l0 μm are reached with the superfine grinding granularity of the tobacco plant material such as root, stem, be beneficial to the pole of fragrant source material Property composition is soluble in water, meanwhile, under the violent turbulent flow emulsification of high-pressure water jet, it is also beneficial to the nonpolar of fragrant source material (oiliness or lipid) composition is soluble in water.
In such scheme, the water fluid jet grind and centrifugal separator, high-pressure plunger pump and delivery pump formed closed-circuit pulverization with Centrifugal separator detached heavy thing (containing coarse granule) is returned the water jet for plant superfine grinding by separating circuit Mill, carries out continuous circulation and crushes;By centrifugal separator detached lightweight thing solution (containing fragrant source material and fine tobacco plant Grain) high-pressure plunger pump is sent into, recycle as working media, until in the detached lightweight thing solution of centrifugal separator The lightweight thing solution, when granularity reaches mean diameter about < 5~l0 μm, is switched out closed-circuit pulverization and is separated back by subparticle Road, and be transported to next stage and be evaporated extraction.
In such scheme, cone of revolution video disc of the lightweight thing solution from the superiors, alternating flow to undermost solid During determining conical surface video disc, uniform film layer is successively formed, period is heated to Film Flow by microwave exposure, eliminate and add Incremental contribution of the vapourss to gas phase in vaporizer, while using the decompression of fluid speedup and the collaboration decompressing effect of vacuum draw, Make feed liquid be converted into gas phase at a lower temperature, the fragrant source material in the lightweight thing solution is evaporated to into gas phase, the heat is handed over Temperature is changed in the range of 25~80 DEG C, and evaporating temperature can be carried out more accurate by the Loading Control of microwave pulse irradiation Control.
In such scheme, by vacuum pump set, by the gas phase of the continuous strap-clamping-type thin bed of material microwave evaporation device evaporation Fragrant source material, is drawn into condenser and is condensed into liquid;Again by separator, make fragrant source material with condensed moisture from acquisition liquid The Nicotiana tabacum L. aroma component of state, the vacuum of vacuum pump set is 0.035~0.095MPa.
In such scheme, the extraction raw material of the Nicotiana tabacum L. aroma component such as Nicotiana tabacum L., root, stem is crushed to by plant pulverizer 10 mesh of granularity < (1.7mm), is added in agitator tank, then by solid-to-liquid ratio 1:(2~8) water is added, at normal temperatures impregnated raw material 30 ~60min, period agitator are accomplished continuously or intermittently stirred with 0.2~1m/s of linear velocity;Swelling good raw material will be impregnated, by slurry Delivery pump is delivered to the centrifugal separator, and the heavy thing after separation is transported to the water jet for plant superfine grinding Mill;Lightweight thing solution after separation, is transported to high-pressure plunger pump, recycles as working media.
In such scheme, separator is set at the discharge adapter of the water fluid jet grind for plant superfine grinding, will The tobacco plant aroma volatile produced during nappe flip length, is fed directly to thin positioned at the continuous strap-clamping-type In the condenser and separator of bed of material microwave evaporation device back segment, trapped with Nicotiana tabacum L. aroma component in the lump.
Implement the method that the nappe flip length and strap-clamping-type microwave distillation of the present invention extract Nicotiana tabacum L. aroma component, with following Beneficial effect:
The present invention carries out cell wall breaking crushing by water fluid jet grind to tobacco plant, to improve the dissolving of Nicotiana tabacum L. perfume source material Degree;And the thin bed of material microwave evaporation device of continuous strap-clamping-type is utilized, make the solution dissolved with Nicotiana tabacum L. perfume source material high at a lower temperature Effect evaporation, finally by efficient condenser and oil water separator, prepares and realizes that cell wall breaking and distillation are carried with pure physical method The high quality tobacco aroma component for taking.
Description of the drawings
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is the method technological process example that a kind of nappe flip length and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component Property sketch;
Fig. 2 is the main view profile of the thin bed of material microwave evaporation device of continuous strap-clamping-type;
Fig. 3 is the side cutaway view of the thin bed of material microwave evaporation device of continuous strap-clamping-type;
Fig. 4 is the top view of the thin bed of material microwave evaporation device of continuous strap-clamping-type;
Feeding structure local main view profiles of the Fig. 5 for Fig. 2 shown devices;
Fig. 6 is for the upper and lower nip rolls of Fig. 2 shown devices and to material folding Rotating fields local main view profile;
Discharging structure local main view profiles of the Fig. 7 for Fig. 1 shown devices;
Fig. 8 is the water fluid jet grind main view profile for plant superfine grinding;
Fig. 9 is the top view of the water fluid jet grind for plant superfine grinding;
Figure 10 is the A-A profiles in Fig. 8;
Figure 11 is the main view profile that top feeds hierarchy;
Figure 12 is the C direction views in Figure 11;
Figure 13 is the main view profile that lower nozzle crushes structure;
Figure 14 is the B direction views in Figure 13.
Specific embodiment
In order to be more clearly understood to the technical characteristic of the present invention, purpose and effect, now compare accompanying drawing and describe in detail The specific embodiment of the present invention.
As shown in figure 1, a kind of nappe flip length for providing of the present invention and entrainment type micro-wave temperature distillation extraction Nicotiana tabacum L. cause perfume into The method divided, its technological process and set device include:Agitator tank 0101, tobacco slurry delivery pump 0102, high-pressure plunger Pump 0103, for the water fluid jet grind 0104 of plant superfine grinding, crushes slurry delivery pump 0105, crushes slip separator 0106, Flow control valve 0107, centrifugal separator 0108, the thin bed of material microwave evaporation device 0109 of continuous strap-clamping-type, condenser 0110, point From device 0111, vacuum pump set 0112, handpiece Water Chilling Units 0113.
A kind of nappe flip length and entrainment type micro-wave temperature distillation extraction Nicotiana tabacum L. aroma component method processing step and Main technologic parameters are as follows:
Step 1:By the extraction raw material of the Nicotiana tabacum L. aroma component such as Nicotiana tabacum L., root, stem, granularity < is crushed to by plant pulverizer 10 mesh (1.7mm), are added in agitator tank 0101, then by solid-to-liquid ratio 1:(2~8) add water, at normal temperatures impregnated raw material 30~ 60min, period agitator are accomplished continuously or intermittently stirred with 0.2~1m/s of linear velocity;Swelling good raw material will be impregnated, by tobacco pulp Material conveying pump 0102 is delivered to centrifugal separator 0108, and the heavy thing (coarse granule containing raw material) after separation is transported to described being used for The water fluid jet grind 0104 of plant superfine grinding;Lightweight thing (containing fragrant source material and fine tobacco plant granule) solution after separation, High-pressure plunger pump 0103 is conveyed into, is recycled as working media.
Step 2:Heavy thing after separation is taken over via charging, into the water fluid jet grind for plant superfine grinding 0104 flat circular pipe type pulverizing chamber, carries out nappe flip length;Slurry after crushing passes through to crush slurry delivery pump 0105, via Discharge adapter is sucked discharges the water fluid jet grind 0104 for plant superfine grinding, then is delivered to centrifugal separator 0108 and enters Row is separated;By this process, the heavy thing after separating centrifugal separator 0108, by high-pressure plunger pump 0103, described for planting Closed-circuit pulverization and divide that the water fluid jet grind 0104 of thing superfine grinding, centrifugal separator 0108 and crushing slurry delivery pump 0105 are formed In loop, obtain continuous circulation and crush, until the subparticle in the light material liquid after being separated by centrifugal separator 0108, When granularity reaches the setting index of mean diameter about < 5~l0 μm, light material liquid is switched out by flow control valve 0107 Closed-circuit pulverization and separating circuit, and it is transported into the thin bed of material microwave evaporation device of continuous strap-clamping-type 0109.
The crushing pressure of the nozzle of the water fluid jet grind 0104 for plant superfine grinding is 5~20MPa, it is preferable that 7 ~12MPa, the back pressure of flat circular pipe type crushing chamber is in the range of 0.010~0.040MPa, it is preferable that 0.02~0.03MPa.
By crushing slip separator 0106, by 0104 crushing process of water fluid jet grind for plant superfine grinding The escaping gas of middle generation is fed directly to trap in the condenser 0110 and separator 0111 of vaporising device back segment.
Step 3:The light material liquid obtained by step 2, is transported to the thin bed of material microwave evaporation of the continuous strap-clamping-type Device 0109, by screw conveying feeding bed, and is turned round upper and lower nip rolls to being clipped between filter screen band, is come and gone with level and successively gone up The transfer ways for rising absorb microwave energy with thin uniform layer state, make contained cigarette by microwave cavity, the light material liquid Hay-scented source material is converted into gas phase at a lower temperature, and heat exchange temperature is in the range of 25~80 DEG C, and can pass through microwave pulse The Loading Control of irradiation, is more accurately controlled to evaporating temperature.
The Nicotiana tabacum L. perfume source material of gas phase, under the swabbing action of vacuum pump set 0112, discharges via upper end pump orifice described The thin bed of material microwave evaporation device 0109 of continuous strap-clamping-type, the vacuum of vacuum pump set 0112 is 0.035~0.095MPa.
The gas phase Nicotiana tabacum L. perfume source material of the thin bed of material microwave evaporation device of the continuous strap-clamping-type 0109 is discharged, is aspirated into Condenser 0110, and liquid is condensed into together with water vapour;Again by separator 0111, Nicotiana tabacum L. perfume source material and condensed moisture is made From the Nicotiana tabacum L. aroma component of acquisition liquid.
Solution after thin 0109 evaporation and concentration of bed of material microwave evaporation device of the continuous strap-clamping-type, can be used as producing cigarette The raw material of careless extractum is comprehensively utilized.
Handpiece Water Chilling Units 0113 are that condenser 0110 provides coolant, 0.5~8 DEG C of chilling temperature scope.
The water fluid jet grind and the thin bed of material microwave evaporation device of the continuous strap-clamping-type for plant superfine grinding, and Situ cleaning CIP devices and steam high temperature sterilize measure is configured with extraction system.
As shown in Fig. 2-Fig. 7, the thin bed of material microwave evaporation device of continuous strap-clamping-type 0109 includes:Boil-off gas discharge pipe 0901, infrared temperature measurement device 0902, lid 0903 on vaporizer, carrying roller 0904, modified roller 0905 draw conveying roller 0906, upper filter screen Band 0907, evaporator tube 0908, screw conveying feeding bed 0909, screw conveying feeding motor 09091, pinch upper roll 0910, on Pinch roller motor 09101, pinch under roll 0911, pinch under roll motor 09111, stone roller 0912, stone roller motor 09121, brush roll 0913, Brushroll motor 09131, upper separate roller 0914, upper separation roller motor 09141, upper scraping plate 0915, lower separate roller 0916, lower separate roller Motor 09161, lower scraping plate 0917, helical feed hopper 0918, lower filter screen band 0919, to material folding layer 0920, nozzle 0921, collection Liquid bucket 0922, circulation fluid drain connection 0923, microwave magnetron 0924.
As shown in Figure 2, Figure 3 and Figure 4, boil-off gas discharge pipe 0901 arranges the vertex of a cone centre bit of lid 0903 on an evaporator Put, by sealing flange or weld connection;Multiple infrared temperature measurement devices 0902 arrange lid 0903 and evaporator tube on an evaporator On 0908 folding face shape side wall, coupled by flange and bolt seal, infrared measurement of temperature hot spot runs through 0908 through hole of evaporator tube To vaporizer, the quantity of infrared temperature measurement device 0,902 5~9, the present embodiment are 5;Carrying roller 0904 is arranged on per layer to folder The lower section in 0920 stage casing of the bed of material, is contacted with the lower surface to material folding layer 0920, the upper filter screen of another horizontal direction band 0907 and lower filter The lower section in 0919 stage casing of guipure respectively arranges a carrying roller 0904;Modified roller 0905 has 2,1 therein, is arranged on vaporizer cylinder Position above body 0908 with 0910 homonymy of pinch upper roll, the location portability position in the horizontal direction of modified roller 0905 are solid by bolt It is fixed, to adjust upper filter screen with 0907 tension force.
Multiple traction conveying rollers 0906 are arranged on per layer of both sides to material folding layer 0920, so that it is defeated that material folding layer 0920 is altered course Send, and load-bearing solidliquid mixture;Traction 0906 roll surface of conveying roller with 0911 roll surface locating slot of pinch upper roll 0910 and pinch under roll The stopper slot of same size and structure, to prevent to material folding layer 0920 sideslip under transportation state;Stopper slot is along roll surface axis side To width, can be selected in the range of 500~5000mm according to the treating capacity of vaporizer, the present embodiment is 1600mm, is drawn defeated The quantity of roller 0906 is sent, can be determined according to evaporator specifications, it is larger to specification, can the configuration traction in traction conveying roller 0906 Motor 09061, to improve the tension distribution of filter screen band, the present embodiment arranges 10 traction conveying rollers 0906, from bottom to up Traction electric machine 09061 is configured on 6th traction conveying roller 0906.
Upper filter screen band 0907 and lower filter screen band 0919, are respectively slightly less than traction 0906 roll surface stopper slot of conveying roller for a width For no reason the filter screen band of 5~10mm of width, filter screen band are the nonmetallic materials of wave transparent, and such as thin cotton is weaved cotton cloth, or terylene filter cloth, Terylene filter screen, nylon leaching net etc., the present embodiment is weaved cotton cloth for cotton, and tape thickness λ scope is 0.5~2mm.
The basic configuration of evaporator tube 0908 is the rectangle housing of a setting, outer wall with structural steel frame structural strengthening, Used as microwave cavity, wherein, a pair opposite sides in plummet direction may be designed to folding face shape, the angle β scopes between folding face For 120 °~170 °, in the present embodiment, the refraction of microwave can be strengthened in β=116.15 °, these folding faces, advantageously form microwave humorous Shake field, and makes wave field be evenly distributed;Whole evaporator tube 0908 is with low electric damage value microwave reflection metallic conductor, such as stainless The materials such as steel, aluminum are constructed, and in the present embodiment, are rustless steel SUS304, and cylinder is highly 2950mm, width 2100/2500mm, thick Degree 2150mm.
Evaporator tube 0908, the various location of two folding face shape outer walls are provided with several microwave magnetrons 0924 and many Individual infrared temperature measurement device 0902, between microwave magnetron 0924 and infrared temperature measurement device 0902, by the pulsewidth with microwave pulse power supply Coupling with arteries and veins spacing is controlled, and makes microwave heating evaporating temperature in 25~100 DEG C of operated within range of setting;Evaporator tube At the 0908 feedback mouth of microwave magnetron 0924, closed with the polyfluortetraethylene plate of wave transparent.
The microwave frequency of microwave magnetron 0924 can select 2450MHz, or 915MHz, when solidliquid mixture electricity damage value it is larger Or evaporation capacity it is larger when, 915MHz can be matched, 2450MHz is typically matched;Microwave rated power is configured:2450MHz, 5.4~ 50kW;915MH, 20~120kW;In the present embodiment, the microwave frequency of microwave magnetron 0924 is 2450MHz, 12 0.9kW's Magnetron, the maximum rated power of configuration is 10.8kW, and according to different solidliquid mixtures and treating capacity, actual power is adjustable It is whole.
Pinch upper roll 0910 and pinch under roll 0911, are arranged on the lower section of evaporator tube 0908, with screw conveying feeding bed 0909 homonymy, respectively by pinch upper roll motor 09101 and the synchronous opposite driving of pinch under roll motor 09111, or can pass through a motor Via the synchronous opposite driving of belt wheel shunting, rotating speed can pass through servo or frequency conversion is adjusted;0911 roll surface of pinch upper roll 0910 and pinch under roll Locating slot is offered respectively, along the groove width of roll surface axis direction, can be according to the treating capacity of vaporizer, in 500~5000mm scopes Interior to select, the present embodiment is 1600mm;Groove depth δ scope is 5~15mm, and the present embodiment is 10mm.
Stone roller 0912 is arranged on 0911 upstream end of the pinch upper roll 0910 of revolution and pinch under roll, and axis horizontal distance range is 200~600mm, the present embodiment are 345mm;Stone roller 0912 is driven by stone roller motor 09121, and rotating speed can pass through servo or change Frequency modulation is whole.
Screw conveying feeding bed 0909 is arranged on the top of stone roller 0912, the feed opening pair of screw conveying feeding bed 0909 Claim the dead in line of projection and the stone roller 0912 of axis, the width of the feed opening of screw conveying feeding bed 0909 along axis, compared with Little 20~the 30mm of 0910 roll surface locating slot groove width 500~5000mm value ranges of pinch upper roll;The blanking of screw conveying feeding bed 0909 Opening's edge is 20~70mm to the width range of 0920 conveying direction of material folding layer, and the present embodiment is 35mm;Screw conveying feeding bed Gap between 0912 roll surface of 0909 feed opening and stone roller, by couple electric pushrod flashboard adjust, span of control be 5~ 25mm, the present embodiment are 12mm.
Screw conveying feeding bed 0909, by varying pitch, or becomes spiral shell gauge structure, and revolution speed of screw, makes solidliquid mixture Certain material seal pressure is formed in screw conveying feeding bed 0909, pressure reduction is produced at charging aperture, pressure differential range is 0.035~ 0.095MPa, can associate control by pressure transducer with helical feed servomotor or frequency conversion motor;Screw conveying feeding bed 0909 feed hopper is arranged on outside the microwave cavity of evaporator tube 0908;In evaporator tube 0908 adjacent to helical feed On the side wall of charging bed 0909, the observation window that can be had an X-rayed is set, window material is anti-microwave leakage glass.
Upper separate roller 0914 and lower separate roller 0916, are arranged on the top of evaporator tube 0908, with helical feed discharge Struggle against 0918 homonymy, respectively by upper separation roller motor 09141 and the synchronous opposite driving of lower separation roller motor 09161, or can pass through one Via the synchronous opposite driving of belt wheel shunting, rotating speed can pass through servo to platform motor or frequency conversion is adjusted.
Upper scraping plate 0915 and lower scraping plate 0917 are separately positioned at the surface of separate roller 0914 and lower separate roller 0916, with Corresponding upper filter screen band 0907 and lower filter screen band 0919 are contacted, and contact force size is adjustable;0917 material of upper scraping plate 0915 and lower scraping plate Expect for politef.
Brush roll 0913 is separately positioned on above separate roller 0914 with below lower separate roller 0916, makes the bristle of brush roll 0913 Contact with 0919 bandwidth direction with 0907 and lower filter screen along upper filter screen respectively;Brush roll 0913 is driven by brushroll motor 09131.
Helical feed hopper 0918 is arranged on the top of evaporator tube 0908, and 0914 homonymy of upper separate roller, and will Upper scraping plate 0915 and lower scraping plate 0917 and brush roll 0913 are dissolved in wherein, and make removing entirely falls in helical feed to material folding layer 0920 In hopper 0918, the conveyor screw of its underpart is by varying pitch, or becomes spiral shell gauge structure, and revolution speed of screw, makes material defeated Send and in pipe, form certain material envelope effect, produce pressure reduction at discharge gate, pressure differential range is 0.035~0.095MPa, can be passed through Helical feed motor speed is controlled;With on the side wall of 0918 corresponding evaporator tube 0908 of helical feed hopper, arrange The observation maintenance door that can be had an X-rayed, window material are anti-microwave leakage glass.
Another 1 in modified roller 0905, is arranged on below evaporator tube 0908, with 0914 homonymy of upper separate roller, changed course The location portability position in the horizontal direction of roller 0905, is bolted, to adjust lower filter screen with 0919 tension force.
Nozzle 0921 is stratified and set on, with 0914 homonymy of upper separate roller, orlop and time lower floor's traction conveying roller 0906 The top of roll surface, the liquid mist that nozzle 0921 is formed can uniformly be sprayed at the surface to material folding layer 0920, and the feed liquid sprayed is led to The outer compression pump matched somebody with somebody is crossed, is extracted from liquid collecting bucket 0922 via circulation fluid drain connection 0923.
Upper separate roller 0914, lower separate roller 0916 draw conveying roller 0906, pinch upper roll 0910, pinch under roll 0911 and stone The rotating speed of roller 0912, by PLC or the integrated control of industrial computer, makes upper filter screen equal with 0919 tension distribution with 0907 and lower filter screen It is even, and upper filter screen band 0907 and lower filter screen band 0919 is made, can respectively from upper separate roller 0914 and lower separate roller 0916, by changed course Roller 0905, successfully returns to pinch upper roll 0910 and pinch under roll 0911, is formed to the clip-on circulation transport structure of solidliquid mixture.
As shown in figure 8, the water fluid jet grind 0104 for plant superfine grinding includes:Top charging hierarchy 041, and under Portion's nozzle crushes structure 042, and top is fed hierarchy 041 and is connected by bolt seal with lower nozzle crushing structure 042, and Flat circular pipe type crushing chamber 0424 and blade classification 0414 structure of impact ring is formed, wherein, flat circular pipe type crushing chamber 0424 is wrapped Include multiinjector and converge disintegrating area, and uniform nozzle multiple spot tangential impact disintegrating area.
As shown in Fig. 8~Figure 14, the outer diameter of flat circular pipe type crushing chamber 0424 is D0, flat circular pipe type crushing chamber 0424 inner diameter be D1,0415 center circle diameter of feed opening be D2, lower substrate outside diameter be D3, blade classification impact ring 0414 internal diameter is D4, and 0411 internal diameter of charging adapter is Din, and discharge adapter internal diameter is Dout.
As shown in Fig. 8~Figure 12, top charging hierarchy 041, by charging adapter 0411, discharge adapter 0412, upper base Body 0413, blade is classified impact ring 0414 and feed opening 0415 is constituted, and wherein, blade is classified impact ring 0414 and is rushed by nozzle is converged Hit wall 0414a, uniform jet impact wall 0414b and tangential vane 0414c is constituted.
As shown in fig. 10 and fig. 12, feed adapter 0411 to be connected by bolt seal with upper matrix 0413, charging adapter 0411 position determined by 0415 center circle diameter D2 of feed opening, D2=(0.80~0.87) × D0, it is preferable that D=0.84D0;Enter Material 0411 diameter Din=(0.2~0.4) × (D0-D1) of adapter, it is preferable that Din=0.23 × (D0-D1), D0 spans 300~1160mm.
As shown in Fig. 8, Figure 13 and Figure 14, the inner diameter of flat circular pipe type crushing chamber 0424 be D1 be D1=(0.55~ 0.75) × D0, it is preferable that D1=0.64D0.
As is illustrated by figs. 11 and 12, discharge adapter 0412 is located at the center of the circle of upper matrix 0413, and with upper matrix by weldering Connect in succession, 0412 diameter Dout=(0.12~0.16) of discharge adapter × D0, it is preferable that Dout=0.13D0.
As shown in Figure 10, Figure 11 and Figure 12, it is overall structure that blade is classified impact ring 0414 and upper matrix 0413, blade point Level 0414 internal diameter D4=(0.45~0.65) of impact ring × D0, it is preferable that D4=0.54D0;In blade classification impact ring 0414 Converge 40 °~54 ° of the arc length angle of jet impact wall 0414a, it is preferable that 48 °, and from the convergences spray cut angle with different The axis of mouth 0423a, 0423b, 0423c and 0423d, is touched with wide-angle low-angle tangent;Blade is classified impact ring Uniform jet impact wall 0414b on 0414 is corresponding tangent with 0423 axis of uniform nozzle, uniform jet impact wall 0414b 16 °~20 ° of arc length angle, it is preferable that 18 °;Blade classification impact ring 0414 on tangential vane 0414c cut angle 25 °~ 50 °, it is preferable that 30 °, 42 ° of tangential vane 0414c setting areas arc length angle, the tangential vane 0414c close to feed opening 0415 sets Put 72 ° of area arc length angle;Tangential vane 0414c height h=(2.8~3.5) × (D0-D1), it is preferable that h=3.1 × (D0- D1);The blade passage gap width of the alternate composition of two tangential vane 0414c is 3~6mm, it is preferable that 4mm.
As shown in Figure 10, Figure 13 and Figure 14, lower nozzle crushes structure 042, by nozzle plug 0421, annular high voltage moisture Cloth room 0422, convergence nozzle 0423a, 0423b, 0423c and 0423d, uniform nozzle 0423, and flat circular pipe type crushing chamber 0424th, pressure transducer 0425, lower substrate 0426 and water under high pressure access tube 0427 are constituted.
As shown in Figure 10, it is 10 °~20 ° to converge nozzle 0423a with horizontal axis angle, it is preferable that 15 °, converges nozzle Neighbour angle between 0423b, 0423c and 0423d be 17 °~25 ° preferably, 20 °;Uniformly the tangential angle beta of nozzle 0423 is 50 °~75 °, it is preferable that 62 °;Nozzle and uniform nozzle is converged, is connected in lower substrate 0426 by thread seal;Water under high pressure Access tube 0427 is welded on 0426 cylindrical side wall of lower substrate, and is communicated with annular high voltage water distribution room 0422.
As shown in Fig. 8 and Figure 14, the cross section of fluid channel size of flat circular pipe type crushing chamber 0424:Width B=0.5 × (D0- D1), height H=(0.15~0.35) × (D0-D1), it is preferable that H=0.2 (D0-D1).
It is that 3~7 throat diameters are 0.7~2.5mm High pressure water jet nozzles to converge nozzle, it is preferable that it is 4 to converge nozzle High pressure water jet nozzle of the individual throat diameter for 1mm;Multiple uniform nozzles are the height that 4~9 throat diameters are 0.7~2.5mm Pressure water jet nozzle, it is preferable that it is that 4 throat diameters are 1mm High pressure water jet nozzles to converge nozzle.
The crushing pressure of High pressure water jet nozzle is 5~30MPa, it is preferable that 7~12MPa.
Discharge adapter is connected with suction pump, and swabbing pressure makes flat circular pipe type crushing chamber by suction pump Serve Motor Control Back pressure in the range of 0.080~0.040MPa, it is preferable that in the range of 0.02~0.03MPa.Due to described ultra-fine for plant The water fluid jet grind of crushing with water as working media, if in crushing process, by high-pressure plunger pump continuously from extraction system Outer supplementary work Jie water, then can cause to affect distillation efficiency to the excessively dilution of fragrant source material.In this regard, extraction system be configured with from Centrifugal separator, forms high-pressure plunger pump, the water fluid jet grind for plant superfine grinding, centrifugal separator and delivery pump and closes Road is crushed and separating circuit, will be used for plant superfine grinding described in centrifugal separator detached heavy thing (containing coarse granule) return Water fluid jet grind, carries out continuous circulation and crushes;By centrifugal separator detached lightweight thing (containing fragrant source material and fine tobacco plant Grain) send into high-pressure plunger pump, as working media recycle, until the detached lightweight thing of centrifugal separator granularity reach it is flat During particle diameter about < 5~l0 μm, heat exchanger preheating is transported in the form of wet colloidal sol, then is admitted to the thin material of continuous strap-clamping-type Layer microwave evaporation device upper end charge door is evaporated process.
The present invention utilizes the water fluid jet grind for plant superfine grinding to carry out cell wall breaking crushing to tobacco plant, to improve The dissolubility of Nicotiana tabacum L. perfume source material;And the thin bed of material microwave evaporation device of continuous strap-clamping-type is utilized, by dissolved with Nicotiana tabacum L. perfume source material Solidliquid mixture comes and goes the transfer ways for successively rising by microwave cavity to being clipped between filter screen band with level, and solid-liquid is mixed Compound feed liquid absorbs microwave energy with thin uniform layer state, contained Nicotiana tabacum L. perfume source material is evaporated at a lower temperature, meanwhile, lead to The loading again to isolating feed liquid is crossed, with circulating and evaporating, the solution dissolved with Nicotiana tabacum L. perfume source material is made under relatively low vacuum, by Liquid-phase conversion is gas phase.Also, by being specifically designed for the water fluid jet grind for plant superfine grinding and the continuous entrainment The coupling technique of the thin bed of material microwave evaporation device design of formula and auxiliary device configuration, form a set of Nicotiana tabacum L. aroma component and extract system System.
By the water fluid jet grind for plant superfine grinding, by the extraction raw material of Nicotiana tabacum L. aroma component, i.e. Nicotiana tabacum L. and Root, stem etc., under the impact and water wedge tension force and cavitation denudation of high-pressure water jet, superfine grinding to mean diameter about < 5 ~l0 μm, make diameter about in the cell wall damage of the various tobacco plant cells of 10~100 μ m in size scopes, not only contribute to perfume (or spice) The polar component of source material is soluble in water, and under the violent turbulent flow emulsification of high-pressure water jet, is also beneficial to fragrant source thing Nonpolar (the oiliness or lipid) composition of matter is soluble in water.
As the water fluid jet grind for plant superfine grinding is with water as working media, if in crushing process, by height Hydraulic plunger pump continuously supplements work Jie's water from outside extraction system, then can cause the excessively dilution to Nicotiana tabacum L. perfume source material and shadow Ring distillation efficiency.In this regard, extraction system is configured with centrifugal separator, high-pressure plunger pump is made, described for plant superfine grinding Water fluid jet grind, centrifugal separator and delivery pump form closed-circuit pulverization and separating circuit, and centrifugal separator detached heavy thing (is contained Coarse granule) water fluid jet grind for plant superfine grinding is returned, carry out continuous circulation and crush;Centrifugal separator is detached Lightweight thing (the solidliquid mixture feed liquid containing Nicotiana tabacum L. perfume source material and fine tobacco plant granule) sends into high-pressure plunger pump, used as work Make medium circulation use, until when the granularity of the detached lightweight thing of centrifugal separator reaches mean diameter about < 5~l0 μm, with solid The form of liquid mixture feed liquid is transported into the thin bed of material microwave evaporation device of continuous strap-clamping-type and is evaporated process.
As plant granule size contained in work Jie's water is small, and almost without abrasion, therefore high-pressure plunger is not resulted in Supercharging push rod abrasion of the pump with simple linear re-ciprocating motion as operation principle, and doping contact scar is produced to solution.Water-jet Stream grinds the very little that heats up in crushing process, will not produce heat affecting to Nicotiana tabacum L. perfume source material.
During nappe flip length, some in tobacco plant are easy to the aroma type molecule escaped from liquid phase, due to The impact of high-pressure water jet and cavitation and produce volatilization, therefore in the row of the water fluid jet grind for plant superfine grinding Separator is set at material adapter, this part volatile aroma is fed directly to into condensation and gas-liquid point positioned at vaporising device back segment In device, trapped with Nicotiana tabacum L. aroma component in the lump.
Nicotiana tabacum L. and root, stem of raw material etc. are extracted as Nicotiana tabacum L. aroma component, in the water-jet for plant superfine grinding Before stream pulverizing is broken, first water retting is used in agitator tank, produce Plant fiber certain swelling, so that water fluid jet grind is carried out efficiently Loosen crushing.
Crushed by a period of time cell wall breaking to the raw material such as Nicotiana tabacum L. and root, stem and the dissolution of fragrant source material is processed, Jing Filtering means dehydration device is admitted to by centrifugal separator detached heavy thing (containing coarse granule) carries out solid-liquid separation, and the slag charge of gained can It is integrated into utilizing, such as manufactures paper with pulp admixture as non-combustion type low-temperature cigarette sheathing paper, or as non-combustion type low-temperature cigarette combustion Carbonized stock of material element etc..
A kind of thin bed of material microwave evaporation device of continuous strap-clamping-type, using the pinch upper roll and pinch under roll of revolution, by upper What filter screen band and lower filter screen band were formed to clamping structure is inverted the uniform thin bed of material for continuously transporting, in microwave resonance intracavity with left and right The transfer ways for successively rising are come and gone, under microwave exposure, body phase is carried out to the thin bed of material and is uniformly heated, and by isolating feed liquid Nozzle CYCLIC LOADING, improve evaporation capacity.Liquid film layer is thinner, faster by thermal evaporation, and evaporation capacity increases.Meanwhile, film layer number Amount is more, and specific surface area is bigger, and evaporation capacity is also bigger.
A kind of thin bed of material microwave evaporation device of continuous strap-clamping-type, also by the sealing structure of charging and discharging, improves steaming The vacuum in device is sent out, Efficient Conversion is gas phase at a lower temperature to make feed liquid.Simultaneously as using the right of multilamellar transportation state Material folding layer, increases heat exchange specific surface area, and vaporising device is compact, and area utilization is high.
Due to the mode of heating of microwave exposure, instead of the heating steam being introduced directly in vaporizer, in vaporizer Gas phase is only the escaping gas produced by feed liquid evaporation, eliminates incremental contribution of the water vapour to gas phase in vaporizer, makes steaming Device is sent out under the swabbing action of vacuum pump set, also so that vacuum is significantly improved, contributes to reducing on thin bed of material gas-liquid interface Pressure, is beneficial to volatile component low-temperature evaporation in the range of 25~80 DEG C, can both improve the evaporation efficiency of feed liquid, reduce volatilization Property gas subsequent condensation gas-liquid separation load, also reduce it is possible cross impact of the heat effect to volatile component quality.
Using in microwave heating process, thermal inertia is little, the characteristic that controllability is good, by the pulsed irradiation loading control of microwave System, is more accurately controlled to evaporating temperature, further improves the quality of volatile component.
A kind of gas phase Nicotiana tabacum L. perfume source material of the thin bed of material microwave evaporation device of continuous strap-clamping-type is discharged, is drawn into cold Solidifying device and gas-liquid separation device, make Nicotiana tabacum L. perfume source material with condensed moisture from the Nicotiana tabacum L. aroma component of acquisition liquid.Condensation and Gas-liquid separation can adopt high-efficiency condensation well known in the art and segregation apparatuss, such as screw pipework condensation device, membrane separator, chromatography Post separation device, macroporous resin separator etc..
Solution after a kind of thin bed of material microwave evaporation device evaporation and concentration of the continuous strap-clamping-type, due to containing Fragrant source material with low saturated vapour pressure value, therefore can be comprehensively utilized as the raw material for producing tobacco extract.
Embodiments of the invention are described above in conjunction with accompanying drawing, but be the invention is not limited in above-mentioned concrete Embodiment, above-mentioned specific embodiment are only schematic, rather than restricted, one of ordinary skill in the art Under the enlightenment of the present invention, in the case of without departing from present inventive concept and scope of the claimed protection, can also make a lot Form, these are belonged within the protection of the present invention.

Claims (10)

1. a kind of method that nappe flip length and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component, it is characterised in that include with Lower step:
S1, the extraction raw material of Nicotiana tabacum L. aroma component after crushing is added in agitator tank, after adding water stirring, delivers to centrifugation Machine;
S2, the heavy thing after separation is delivered to into water fluid jet grind carries out nappe flip length;
S3, that the lightweight thing solution for separating acquisition after nappe flip length in step S2 is delivered to the thin bed of material of continuous strap-clamping-type is micro- Ripple vaporising device, pinch upper roll and pinch under roll of the microwave evaporation device using a pair of revolutions, by two filter screen bands, by solid-liquid Mixture to being clipped between filter screen band, formed upper filter screen band, the solidliquid mixture bed of material and lower filter screen band to material folding Rotating fields, and The transfer ways for successively rising are come and gone by microwave cavity with level, the solidliquid mixture feed liquid in the layer to material folding is made, Microwave energy is absorbed under thin uniform layer state and be heated evaporation;
S4, gas phase perfume source material are aspirated into condenser, and are condensed into liquid together with water vapour with steam;Again Make fragrant source material with condensed moisture from the Nicotiana tabacum L. aroma component of acquisition liquid by separator.
2. the method that nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component, its It is characterised by, in step S2, by high-pressure plunger pump, water fluid jet grind, centrifugal separator and the delivery pump connection of crushing slurry Closed-circuit pulverization and separating circuit, the raw material in agitator tank is formed, centrifugal separator is delivered to by tobacco slurry delivery pump, separated Heavy thing afterwards is transported to water fluid jet grind;Lightweight thing solution after separation, is conveyed into high-pressure plunger pump, as working media Recycle.
3. the method that nappe flip length according to claim 2 and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component, its It is characterised by, the slurry after crushing obtains continuous circulation in closed-circuit pulverization with separating circuit and crushes, until by centrifugal separator When the subparticle granularity in lightweight thing solution after separation reaches the setting index of mean diameter, will be light by flow control valve Matter thing solution switches out closed-circuit pulverization and separating circuit, and is transported to the upper and lower nip rolls of microwave evaporation device to being clipped in filter screen band Between.
4. the method that nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component, its It is characterised by, the volatile aroma produced in the water fluid jet grind crushing process is delivered to the condenser positioned at vaporising device back segment Middle trapping.
5. the method that nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component, its It is characterised by, the condenser is connected with handpiece Water Chilling Units.
6. the method that nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component, its It is characterised by, in step S1, the extraction raw material of Nicotiana tabacum L. aroma component is crushed to 10 mesh of granularity < by plant pulverizer, It is added in agitator tank, then by solid-to-liquid ratio 1:(2~8) water is added, at normal temperatures 30~60min of impregnated raw material, period agitator Accomplished continuously or intermittently stirred with 0.2~1m/s of linear velocity.
7. the method that nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component, its It is characterised by, in step S3, in microwave evaporation device, lightweight thing solution is in the range of 25~80 DEG C.
8. the method that nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component, its It is characterised by, the thin bed of material microwave evaporation device of the continuous strap-clamping-type includes evaporator tube, is provided with the evaporator tube The traction conveying roller that stone roller, pinch upper roll, pinch under roll and multiple layerings are crisscross arranged, arranges between pinch upper roll and pinch under roll and filters Guipure and lower filter screen band, the stone roller by solidliquid mixture be delivered between upper filter screen band and lower filter screen band and by pinch upper roll and Pinch under roll is pressed, and the traction conveying roller drives upper filter screen band and lower filter screen band to convey in evaporator tube, the vaporizer Cylinder is provided with microwave heating equipment.
9. the method that nappe flip length according to claim 8 and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component, its It is characterised by, the top of the evaporator tube is provided with separate roller and lower separate roller, and upper filter screen band and lower filter screen band are at upper point Separated away from roller and lower separate roller, the side of the upper separate roller is provided with upper scraping plate, and the side of the lower separate roller is provided with down Scraper plate.
10. the method that nappe flip length according to claim 8 and strap-clamping-type microwave distillation extract Nicotiana tabacum L. aroma component, its It is characterised by, the evaporator tube is connected with vacuum extractor.
CN201510732476.9A 2015-10-31 2015-10-31 Method for extracting tobacco aroma component through water jet comminution and entrainment-type microwave distillation Expired - Fee Related CN105249526B (en)

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