CN105251229B - A kind of method of nappe flip length and strap-clamping-type microwave distillation extraction effective component of chinese medicine - Google Patents
A kind of method of nappe flip length and strap-clamping-type microwave distillation extraction effective component of chinese medicine Download PDFInfo
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Abstract
The present invention relates to a kind of method of nappe flip length and strap-clamping-type microwave distillation extraction effective component of chinese medicine, comprise the following steps:S1, the extraction raw material of effective component of chinese medicine after crushing is added in agitator tank, centrifugal separator is delivered to after adding water stirring;S2, the heavy thing after separation is delivered to water fluid jet grind progress nappe flip length;S3, by the step S2 obtain lightweight thing solution be delivered to the thin bed of material microwave evaporation device upper end charge door of continuous strap-clamping-type, by two filter screen bands formation upper filter screen bands, the solidliquid mixture bed of material and lower filter screen band to material folding Rotating fields, and pass through microwave cavity with the horizontal transfer ways successively risen that come and go;S4, gas-phase activity material are aspirated into condenser, and liquid is condensed into together with water vapour with steam;Active material and condensed moisture are made from obtaining the effective component of chinese medicine of liquid by separator again.The present invention realizes breaking-wall cell and the high-quality effective component of chinese medicine of distillation extraction with pure physical method.
Description
Technical field
The present invention relates to field of traditional Chinese medicine pharmacy, more specifically to a kind of nappe flip length and strap-clamping-type microwave distillation
The method for extracting effective component of chinese medicine.
Background technology
With the raising of modern society's general level of the health, and approval of the people to " back to nature " theory, with natural plants
Increasingly paid attention to for the medicine of raw material, food, health care and skin care item etc., wherein, Chinese medicine is because with unique complete reason
By system, deep humanism connotation, curative effect affirmative, have no side effect and be loved by people.In inheriting tradition Chinese medicine processing technology
On the basis of preparation technique, extraction and application is carried out to effective component of chinese medicine using new method, new technology, is to improve Chinese medicine matter
Amount, the important channel for improving form of Chinese drug, rationally utilizing natural resources of Chinese medicinal materials.
Plant medicine is taken from root, rhizome, skin, leaf, flower, fruit, seed and natural gum of plant etc., its it is medicinal effectively into
Point, i.e., active material mainly includes:Alkaloid, glucoside, volatile oil, tannin, amino acid, ketone, alcohols, phenols, terpenes,
Glucoside, organic acid etc., these active materials are typically with metabolite, such as cellulose, chlorophyll, starch, protein, tree
Fat, natural gum, carbohydrate etc. are matrix, are distributed in intracellular and cytoplasm.In dissolution, it is necessary to first through cell membrane and cell
Film could discharge.But the cell tissue of usual plant is close, and cell membrane is also very thick, solvent is not easy to permeate and is spread, effectively into
Divide or DDGS is difficult to be come out by derect seething.
For the effective elements of the medicine in efficiently extracting, breaking-wall cell processing can be carried out to plant medicine first, so as to
Being capable of smooth dissolution in a solvent in these active materials.Research shows, if by plant medicine ultra-fine grinding to average grain diameter
About 5~l0 μm, its granularity is less than 10~100 μm of the diameter of general plant cell, cell-wall breaking ratio can be made to reach >=95%, in fact
Existing so-called breaking-wall cell crushes.Therefore, using superfine grinding method, it can greatly reduce the particle size of plant, specific surface area
Dramatically increase, plant medicine active component dissolution rate and recovery rate significantly improve, while also improve having for plant medicine
Imitate utilization rate.
In order to realize that the breaking-wall cell to plant medicine crushes purpose, in the art, various known sides can be used
Method:Such as utilize medium mill stripping class grinding device, including vibromill, Ball-stirring mill, planetary mills and colloid mill, this kind of superfine grinding method
There is frictional heating, the problems such as making active ingredient of Chinese herbs easily be lost by heat deterioration and volatile ingredient, also there is grinding medium
The problem of matter abrasion doping pollution.
And for example, using dry method mechanical impact comminution and air-flow crushing, but due to the toughness of string so that impact comminution
Efficiency is difficult to improve, simultaneously as the combustibility of string, there is the possibility of dust explosion in crushing process, makes crushing
System must use more complicated anti-riot technique, and the riot gear that deployment cost is higher.Though deep cooling crush can solve toughness plant
The crushing problem of fiber, but production cost is higher.
For another example, physical treatment method, breaking-wall cell is made by ultrasonic wave, microwave, steam blasting the methods of side.Wherein, surpass
Sound wave breaking-wall cell is that caused cavitation Erosion and size degradation effect crushes cell membrane in liquid using high-frequency ultrasonic,
The problem of possible, is constrained to ultrasonic transducer power, and disposal ability is not big enough;Microwave frequency measurment is to utilize 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 membrane disengaged vapor and reach breaking-wall cell purpose, it is possible the problem of be Chinese medicinal plant
Active material deteriorated because of overheat;Steam blasting is after utilizing the steam with certain pressure to enter in plant cell, because prominent
Right pressure release makes steam release cause breaking-wall cell, it is possible the problem of be still to overheat.It can be seen that at present at this kind of physical treatment method
Reason intensity is larger, and active ingredient loss is also larger.
Another solvent extraction method, the dissolving of material in a solvent can be utilized under conditions of cell broken wall treatment is not done
Sex differernce, that is, select to not needing dissolved element solubility small, and the solvent big to active agent solubility, by solvent to thin
The osmosis of cell wall enters into the cell, dissolves soluble active ingredients, causes the concentration difference that cell is inside and outside, make intracellular
Concentrated solution constantly then constantly enters in cell to external diffusion, solvent, until when the inside and outside solution concentration of cell reaches dynamic equilibrium,
Saturated solution is filtered out, novel solvent is added and continues dissolution.Solvent can be highly polar water or hydrophily or lipophilic
The organic solvent of property.Solvent extraction method is divided into two kinds of cold formulation and hot formulation, common solvent extraction method relative poor, time
Long, less efficient, the active ingredient relative amount of extraction is not high.
After cell makes active material dissolve in solvent because of broken wall or diffusion, then it is further desirable that the activity of liquid phase
Material separates from solvent, i.e. distillation extraction.In the art, various known methods can be used:Such as traditional extraction
Method, including decocting method, infusion process, percolation, reflux extraction, the way of distillation, steam distillation etc..Or more novel leaching
Extracting method, including supercritical fluid extraction, ultrasonic extraction, microwave loss mechanisms, charged extraction method, semi-bionic extraction, rotation
Flow extraction method, pressurized counter-flow extraction method, Enzymatic Extraction method etc..
Wherein, the way of distillation, it is different using each component boiling point (volatility) in mixing liquid, low boiling component is evaporated, then
Liquid is condensed into separate whole component.If using water as solvent, i.e. steam distillation is good economy performance, safe, operational
By force, and to water such as the semipolar alkaloid of plant medicine, tannin, amino acid, ketone, alcohols, glucoside, phenols, acylates
Soluble active substance has preferable extraction effect, but the volatile oil for low polarity, glucoside, organic acid, terpenes liposoluble
Property active component extraction effect it is bad, and need higher evaporating temperature, side reaction is more, may influence the activity of active ingredient.
And for example, supercritical fluid CO2Extraction, using superpower solvability possessed by supercritical fluid, makes active material
Dissolving, and by the control of pressure and temperature, make CO2Solvent reaches critical point in extraction process, completes liquid phase to gas phase
Hypercritical transition, and obtain the active material of liquid phase.This method purity is high, no solvent residue, is suitable in plant medicine
The extraction of most nonpolar or low pole volatile ingredient, therefore in the existing more application in this area.But this method treating capacity compared with
It is low, equipment investment is larger, cost is higher, low to the active material extraction yield of low volatility.
By above-mentioned analysis, the key technology for extracting active component from plant medicine has at 2 points, when, realize
Breaking-wall cell;Second, control when liquid-phase conversion is gas phase to evaporating temperature.The former is related to the dissolution rate of active material, after
Person is related to the quality of active material.
Analysis is understood according to more than, in the art, the breaking-wall cell of plant medicine is crushed known to method, mainly
Using dry method grinding process, its force mechanism crushed mainly grinds stripping and smashed, material institute corresponding with force mechanism
The resistant to breakage resistance of production is:Resistance to compression, shearing resistance, bending resistance and anti-impact force, that is, a tension reduction resistant force is lacked.And material
Mechanical strength rule is:Compression strength is maximum, and shearing strength is taken second place, and bending strength is smaller, and tensile strength is minimum.Therefore, planting
In method known to the crushing of species Chinese medicine breaking-wall cell, crush force mechanism and lacked a stretching that can improve material grindability
(or tension force) pulverization power, this is also the general character shortcoming of other dry method grinding processes.Further, since dry method grinding process is being ground
In stripping and fragmentation process, frictional heating phenomenon is produced.Thus the problem of having triggered corresponding breaking-wall cell process bands, such as there is
Sporoderm-broken rate it is not high and overheat caused by active Chinese drug component substance degradation the deficiencies of.
In the art, to the solution dissolved with active Chinese drug component material, the evaporating temperature control aspect of gas phase conversion is carried out,
As described above in known method, take including measures such as steam 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 rise of temperature, and saturated vapour pressure value is higher,
More be advantageous to liquid phase and be changed into gas phase " this association to contradiction of evaporating principle and active Chinese drug component material " temperature is too high to cause deterioration "
In terms of tune, belong to conventional technological balance mostly, the principle in terms of relative shortage method and apparatus breaks through.
Some method and apparatus aspects obtain certain success to the patent quoted from below wherein, but this can not be inevitably
These technologies for being construed to existing are suitable.
The Chinese patent CN 02149695.1 of Wei rattan children et al., disclose a kind of Microwave Pretreatment of effective ingredients in plant
Extracting method, dry plant is crushed first, adds and is sufficiently humidified so as on a small quantity containing ethanol water, it is then quick as being carried out in microwave field
Pretreatment, is eventually adding hot solvent agitator treating can and the extracts active ingredients in plant tissue is come out.
The Chinese patent CN 200510016832.3 of Yu Yongli et al., disclose a kind of active component in northern schisandra extraction
Method, step are:Fructus schisandrae is featured → crushing → heating → microwave treatment → refluxing extraction → filtering → high speed centrifugation point
From → it is dried in vacuo to obtain finished product.
Ma Feng et al. Chinese patent CN 200610044442.1, disclose it is a kind of for effective ingredients in plant extraction
Decompressed microwave extraction device and method, it is made up of micro-wave oven, extractor, condenser, separator and decompressor.Micro-wave oven is set
In extractor periphery, microwave generator is evenly arranged in it;Electric mixer is installed on extractor, sets and disappears at the top of extractor
Chinaware, extractor top are extraction cell, the solvent storage room of bottom setting activity, it is middle by with uniform solvent penetration hole every
Plate separates extraction cell and storage room.Depressurizing with microwave action, the condensed device of solvent evaporation is condensed into liquid solvent, by following
Endless tube returns to solvent storage room, and plant is after microwave irradiation, by the device for discharging discharging of extractor bottom.Due to being adopted in device
With decompression and solvent recycling apparatus, effective ingredients in plant extraction process caused by microwave irradiation is accelerated, while ensure plant
Because temperature is too high thermal metamorphism will not occur for active ingredient.
Zhao Ying et al. Chinese patent CN 200610104933.0, disclose a kind of extraction production of effective component of chinese medicine
Method, after traditional Chinese medicinal material raw materials removal of impurities, corresponding extract solution is added, through against oozing, extracting, supersonic oscillations hydrotropy, Fast Stripping is effective
Composition.Suitable for containing water-soluble, the Chinese medicine of alcohol-soluble active ingredient.
The Chinese patent CN 200810051150.X of Pan Yong qis, the invention discloses a kind of continuous normal temperature extraction Chinese medicine to have
The method and device of composition is imitated, solvent is well mixed with 30~100 mesh Chinese medicine materials mixed liquor is made, be transported to extractor
Separated among electrode, electrode voltage is 3~9 kilovolts, the KHz of frequency 3~9, is made in mixed liquor by 20~200 amperes
High frequency electric, the biomolecule of Chinese medicine material is polarized in the presence of high frequency electric and electric field force, shows electric polarity, produce
Concussion, intermolecular attraction is destroyed, the structure of matter occur it is loose, solvent can rapid osmotic to inside material, make active ingredient
It is rapidly dissolved among solvent, the dregs of a decoction and solvent separation is carried out after extraction, obtain the solution containing effective component of chinese medicine.
Qin Shengli et al. Chinese patent CN 200910022006.8, disclosing a kind of ultrasonic wave extraction natural plants has
The preparation technology of composition is imitated, is comprised the following steps:Clean dedusting;Crush;Dipping:By the natural plant raw material to be extracted after crushing
The material blending tank for being put into built-in agitator continue stirring, to be extracted natural into material blending tank in whipping process
Material mixture liquid is obtained after adding maceration extract and blended stirring in plant material;Ultrasonic wave extraction:In hydraulic circulation pump one
Under effect, material mixture liquid is circulated constantly by being connected to the circulating line between material blending tank and ultrosonic extractor
Inside ultrosonic extractor by and carry out continuous cycle type ultrasonic wave extraction;Filtering;It is concentrated under reduced pressure.
The Chinese patent CN 200910214229.4 of Yang good fortune et al., disclose a kind of supersonic synergic electrostatic field extraction and plant
The method and its device of thing active ingredient, including extractor are a cleaning groove type cylinder sound reactors, are set in extractor
Put contre electrode, electrostatic generator positive and negative electrode is electrically connected by controlling switch with contre electrode, the earth terminal of electrostatic generator with
The side wall electrical connection of extractor, realizes the extraction to polar component and nonpolarity element.
Zhang Zongquan et al. Chinese patent CN 201110143520.4, disclose a kind of electromagnetic force synergistic supersonic wave Chinese medicine
Extracts active ingredients device, set in the upper end of tank body and be machined with charge door, the downward work(of spoke side is provided with lid on tank body
Rate ultrasonic transducer, be provided with the spoke side of power ultrasonic transducer extend into tank body, lower end couples with ultrasonic radiation disk
Radial ultrasonic radiant tube, be machined with filter opening on ultrasonic radiation disk;In tank body between ultrasonic radiation disk and housing bottom in tank body
It is provided with plate shaped filter membrane on wall, is provided with magnetic stainless steel polyhedron in tank body on ultrasonic radiation disk, on the lateral wall of tank body
The coil being arranged on skeleton for being provided with by 6 or 12 and being connected with programmable controller.
The Chinese patent CN 201110233876.7 of Chen Hong chapters et al., disclose a kind of raising active components in medicinal plant
The raw material gas explosion preprocess method of dissolution rate:It will be placed in the material after water or aqueous solution preimpregnation in high-pressure bottle, seal, be passed through
Medium, temperature of charge is set to maintain 0.5~30min at 40~250 DEG C, then quick pressure releasing, the thing that will be handled in high-pressure container
Material is discharged into non-pressure vessel, that is, obtains the pretreated material of gas explosion;Described medium is air, carbon dioxide, ozone, liquid
Nitrogen, nitrogen, water vapour, supercritical CO2In one kind or any two kinds of combination.Based on active components in medicinal plant bioactivity
And selectivity fully ensures that material handles intensity, is not damaging using the combination of media gas explosion mode under a variety of low temperature, high pressure conditions
Under the premise of the activity for hindering active ingredient, active ingredient dissolution rate is improved.
The Chinese patent CN 201210230560.7 of Shen Zhi just et al., disclose and a kind of carried using high-pressure fog counter-current
The device and method of active ingredient of natural plant is taken, by natural plants impurity to be extracted, is crushed;Place into agitator tank and add immersion
Liquid, material suspension is obtained, Extraction solvent is added in extractor, the material suspension prepared is sprayed into the drop that nebulizes and entered
Row spraying extraction, then the extraction of high-pressure fog adverse current, finally removes solid impurity with centrifuge;It is concentrated under reduced pressure, it is dry using spraying
Dry, microwave drying or vacuum drying obtain product.
Zhao Wenchang et al. Chinese patent CN 201210502408.X, disclose a kind of traditional Chinese medicine extraction enrichment facility and carry
The method for taking concentration, extracting the structure of enrichment facility includes extraction unit and upgrading unit, and extraction unit includes extractor and medicine
Liquid storage tank, piston moving up and down is provided with extractor, when piston rod is in the presence of driving force, move up piston
With to the dregs of a decoction pressure further squeezing in upper compression chamber;Upgrading unit includes concentrate container, vavuum pump and for holding to concentration
The heater of device heating, is provided with the stair-stepping evaporator plate assembly to form decoction film in concentrate container, is recycled concentration.
Xu Yongping et al. Chinese patent CN 200510130852.3, discloses a kind of effective plant component extracting process,
I.e. after the mixture of mechanical crushing solid plant raw material and appropriate chemical assistant, from water or ethanol effective component extracting, utilize
Produce micro- shear between interface during mechanical crushing solid plant raw material, cell membrane is broken, and fresh section is exposed, chemical assistant with effectively
The principle of the mutual absorption or effect of cluster of grains or micel occurs between composition, changes the microcosmic property of effective ingredients in plant
Can, stripping quantity improves.
The Chinese patent application publication No. CN 101371854A of Li Qiao such as, disclose a kind of wet method of effective component of chinese medicine
Crush extracting method.Including step:Tcm and herbal slice or coarse powder are put in grinder, add the solvents (water, no of 4~20 times of amounts
Ethanol, acetone with concentration etc.), crushed 5~40 minutes at a high speed in 10000 revs/min, decoction is in 5000~10000 after crushing
Rev/min centrifugation 5~10 minutes, gained decoction is traditional Chinese medicine extyaction liquid.
It is worth noting that, in CN 101371854A, although and it is what crushes dress that described wet pulverizing, which is not known,
Put, but the feature that rotating speed is 5000~10000 revs/min is crushed based on it and judged, it should be small dimension colloid mill, i.e., by height
In the ring-type tapered narrow small gap formed between fast revolving body and fixation wall, because the strong shear of fluid boundary-layer acts on and returns
Turn the percussion of toothed surfaces, the solid material in liquid torn, be ground into fine particle.This powder to fibrous plants
Broken is a kind of preferable mode, but is generation of the crushing process along with heat the problem of exist, and this may cause some Chinese medicines
The inactivation or deterioration of bioactive ingredients.
Analysis is understood based on more than, in the art, at present still without a kind of wet grinding technique, its force side crushed
Formula not only has mill stripping and smashes effect, while has the direct broken cells of stretching action concurrently, and in the form of feed liquid film layer, leads to
Microwave irradiation heating is crossed, the method for carrying out distillation extraction effective component of chinese medicine.Accordingly, it is desired to provide one kind is by using to plant
The suitable crushing force mechanism of class Chinese medicine material, Chinese medicinal plant cell is set to obtain abundant broken wall, to improve active Chinese drug component material
Solubility;It is also expected to provide a kind of feed liquid being directed to dissolved with active Chinese drug component material, using the equal material refining layer that continuously transports can be inverted,
The motion mode of rising was returned in the past in microwave resonance intracavitary, under the bigger serface of multilayer, by microwave irradiation, to relatively thin
The bed of material carries out the vaporising device that body phase uniformly heats, and realizes the high efficient cryogenic evaporation of active Chinese drug component material.
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 extracts Chinese medicine
The method of active ingredient, breaking-wall cell and the high-quality effective component of chinese medicine of distillation extraction are realized 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 effective component of chinese medicine, comprises the following steps:
S1, the extraction raw material of effective component of chinese medicine after crushing is added in agitator tank, centrifugation is delivered to after adding water stirring
Seperator;
S2, the heavy thing after separation is delivered to water fluid jet grind progress nappe flip length;
S3, by the 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 use the pinch upper roll and pinch under roll of a pair of revolutions, by two filter screen bands, solid-liquid are mixed
Between thing is to being clipped in 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 successively risen 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 is heated evaporation;
S4, gas-phase activity material are aspirated into condenser, and liquid is condensed into together with water vapour with steam
Body;Active material and condensed moisture are made from obtaining the effective component of chinese medicine of liquid by separator again.
In such scheme, water fluid jet grind makes root, root by the impact of high-pressure water jet, water wedge tension force, cavitation denudation
The ultra-fine grinding granularity of the plant medicine raw material such as stem, skin, leaf, flower, fruit, seed reaches average grain diameter about < 5~l0 μm, with profit
It is soluble in water in the polar component of active Chinese drug component, meanwhile, under the violent turbulent flow emulsification of high-pressure water jet, in being also beneficial to
Nonpolar (the lipid or oiliness) composition of medicine activity is soluble in water.
In such scheme, water fluid jet grind forms closed-circuit pulverization with separating with centrifugal separator, high-pressure plunger pump and delivery pump
Loop, the heavy thing (containing coarse granule) of centrifugal separator separation is returned into the water fluid jet grind for being used for plant ultra-fine grinding, entered
The continuous circulation of row crushes;Light material liquid (material containing active Chinese drug component and the fine plant medicine that centrifugal separator is separated
The solidliquid mixture feed liquid of grain) high-pressure plunger pump is sent into, recycled as working media, until the institute of centrifugal separator separation
The subparticle in light material liquid is stated, when granularity reaches average grain diameter about < 5~l0 μm, the light material liquid is switched out
Closed-circuit pulverization and separating circuit, and be transported to next stage and be evaporated extraction.
In such scheme, the light material liquid (solidliquid mixture feed liquid) by screw conveying feeding bed, and revolution it is upper,
Between pinch under roll is to being clipped in filter screen band, pass through microwave cavity, the lightweight thing with the horizontal transfer ways successively risen that come and go
Feed liquid absorbs microwave energy with thin uniform layer state, contained active Chinese drug component material is converted into gas phase at a lower temperature, described
Heat exchange temperature can be carried out more in the range of 25~120 DEG C by the Loading Control of microwave pulse irradiation to evaporating temperature
Accurately control.
In such scheme, by vacuum pump set, by a kind of continuous thin bed of material microwave evaporation device evaporation of strap-clamping-type
Gas-phase activity material, it is drawn into condenser and is condensed into liquid;Again by separator, make active material and condensed moisture from obtaining
The effective component of chinese medicine of liquid is obtained, the vacuum of vacuum pump set is 0.035~0.095MPa.
In such scheme, the light material liquid, pass through the evaporation of the thin bed of material microwave evaporation device of the continuous strap-clamping-type
After concentration, then via enriching slurry cooler be cooled to normal temperature, the solution being concentrated by evaporation after cooling, through dehydrate can be used as it is micro-
The raw material of riceization Chinese medicine is used.
In such scheme, by the extraction raw material of the effective component of chinese medicine such as root, rhizome, skin, leaf, flower, fruit, seed, pass through plant
Thing pulverizer is crushed to the mesh of granularity < 10 (1.7mm), is added in agitator tank, then by solid-to-liquid ratio 1:(2~8) water is added, normal
Temperature descends 30~60min of impregnated raw material, and during which agitator is accomplished continuously or intermittently stirred with 0.2~1.5m/s of linear velocity;Dipping is swelled
Good raw material, the centrifugal separator is delivered to by slurry delivery pump, and the heavy thing after separation is transported to described for planting
The water fluid jet grind of thing ultra-fine grinding;Light material liquid after separation, is transported to high-pressure plunger pump, makes as working media circulation
With.
In such scheme, separator is set at the discharge adapter of the water fluid jet grind for plant ultra-fine grinding, will
The caused plant medicine volatile effective component during nappe flip length, it is fed directly to positioned at a kind of continuous folder
In the condenser and separator of the thin bed of material microwave evaporation device back segment of belt, trapped in the lump with effective component of chinese medicine.
Implement the method for the nappe flip length and strap-clamping-type microwave distillation extraction effective component of chinese medicine of the present invention, have following
Beneficial effect:
The present invention carries out breaking-wall cell crushing by water fluid jet grind to plant, to improve the solubility of active Chinese drug component material;
And the thin bed of material microwave evaporation device of continuous strap-clamping-type is utilized, make the solution high-efficiency evaporating at a lower temperature dissolved with active material,
Finally by efficient condenser and separator, prepare and realize that the Chinese medicine of breaking-wall cell and distillation extraction is effective with pure physical method
Composition.
Brief 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 effective component of chinese medicine
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;
Fig. 5 is the feeding structure part main view profile of 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 part main view profile;
Fig. 7 is the discharging structure part main view profile of Fig. 1 shown devices;
Fig. 8 is the water fluid jet grind main view profile for plant ultra-fine grinding;
Fig. 9 is the top view of the water fluid jet grind for plant ultra-fine 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.
Embodiment
In order to which technical characteristic, purpose and the effect of the present invention is more clearly understood, now compares accompanying drawing and describe in detail
The embodiment of the present invention.
As shown in figure 1, a kind of nappe flip length provided by the invention and entrainment type micro-wave temperature distillation extract Chinese medicine effectively into
The method divided, its technological process and set device include:Agitator tank 0101, Traditional Chinese medicine pulp material conveying pump 0102, high-pressure plunger
Pump 0103, for the water fluid jet grind 0104 of plant ultra-fine grinding, slurry delivery pump 0105 is crushed, crushes slurry separator 0106,
Flow control valve 0107, centrifugal separator 0108, the continuous thin bed of material microwave evaporation device 0109 of 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 extract effective component of chinese medicine method processing step and
Main technologic parameters are as follows:
Step 1:By the extraction raw material of the effective component of chinese medicine such as the root of plant, rhizome, skin, leaf, flower, fruit, seed, pass through plant
Thing pulverizer is crushed to the mesh of granularity < 10 (1.7mm), is added in agitator tank 0101, then by solid-to-liquid ratio 1:(2~8) water is added,
30~60min of impregnated raw material at normal temperatures, during which agitator accomplished continuously or intermittently stirred with 0.2~1.5m/s of linear velocity;Will dipping
The raw material being swelled, centrifugal separator 0108 is delivered to by plant pulp material conveying pump 0102, the heavy thing after separation (contains raw material
Coarse granule) it is transported to the water fluid jet grind 0104 for being used for plant ultra-fine grinding;Lightweight thing (thing containing active Chinese drug component after separation
The solidliquid mixture feed liquid of matter and fine plant medicine particle) solution, high-pressure plunger pump 0103 is conveyed into, is situated between as work
Matter recycles.
Step 2:Heavy thing after separation is taken over via charging, into the water fluid jet grind for plant ultra-fine grinding
0104 flat circular pipe type pulverizing chamber, carry out nappe flip length;Slurry after crushing by crushing slurry delivery pump 0105, via
Discharge adapter is sucked the discharge water fluid jet grind 0104 for plant ultra-fine grinding, then is delivered to centrifugal separator 0108 and enters
Row separation;By this process, make centrifugal separator 0108 separate after heavy thing, by high-pressure plunger pump 0103, described be used to plant
The closed-circuit pulverization that water fluid jet grind 0104, centrifugal separator 0108 and the crushing slurry delivery pump 0105 of thing ultra-fine grinding are formed is with dividing
Crushed from continuous circulation in loop, is obtained, until the subparticle in the lightweight thing solution after being separated by centrifugal separator 0108,
When granularity reaches average grain diameter about < 5~l0 μm setting index, 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 0109 of continuous strap-clamping-type.
The crushing pressure of the nozzle of the water fluid jet grind 0104 for plant ultra-fine 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 slurry separator 0106, by the crushing process of water fluid jet grind 0104 for plant ultra-fine grinding
In caused escaping gas be fed directly to trap in the condenser 0110 and separator 0111 positioned at vaporising device back segment.
Step 3:The light material liquid obtained by step 2, it is transported to the thin bed of material microwave evaporation of the continuous strap-clamping-type
Device 0109, by screw conveying feeding bed, and between the upper and lower nip rolls of revolution is to being clipped in filter screen band, come and gone with level on successively
For the transfer ways risen by microwave cavity, the light material liquid absorbs microwave energy with thin uniform layer state, make it is contained in
Pharmaceutically active substance is converted into gas phase at a lower temperature, and heat exchange temperature can pass through microwave pulse in the range of 25~120 DEG C
The Loading Control of irradiation, evaporating temperature is more accurately controlled.
The active material of gas phase, it is described continuous via the discharge of upper end pump orifice under the swabbing action of vacuum pump set 0112
The thin bed of material microwave evaporation device 0109 of strap-clamping-type, the vacuum of vacuum pump set 0112 is 0.035~0.095MPa.
The gas-phase activity material of the thin bed of material microwave evaporation device 0109 of the continuous strap-clamping-type is discharged, is aspirated into condensation
Device 0110, and liquid is condensed into together with water vapour;Again by separator 0111, make active material with condensed moisture from acquisition
The effective component of chinese medicine of liquid.
Solution after evaporation and concentration, arranged via the lower end of the thin bed of material microwave evaporation device 0109 of the continuous strap-clamping-type
Go out, then normal temperature be cooled to by enriching slurry cooler 0111, the solution being concentrated by evaporation after cooling, through dehydrate can be used as it is micro-
The raw material of riceization Chinese medicine is used.
Handpiece Water Chilling Units 0113 are that condenser 0110 provides coolant, 0.5~8 DEG C of cooling temperature range.
The water fluid jet grind and the thin bed of material microwave evaporation device of the continuous strap-clamping-type for plant ultra-fine grinding, and
Situ cleaning CIP devices and steam high-temperature sterilization measure are configured with extraction system.
As shown in Fig. 2-Fig. 7, the continuous thin bed of material microwave evaporation device 0109 of strap-clamping-type includes:Boil-off gas discharge pipe
0901, infrared temperature measurement device 0902, lid 0903 on evaporator, 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 sets the vertex of a cone centre bit of lid 0903 on an evaporator
Put, pass through sealing flange or weld connection;Multiple infrared temperature measurement devices 0902 set lid 0903 and evaporator tube on an evaporator
In 0908 folding face shape side wall, coupled by flange and bolt seal, infrared measurement of temperature hot spot runs through the through hole of evaporator tube 0908
To evaporator, the quantity of infrared temperature measurement device 0,902 5~9, the present embodiment is 5;Carrying roller 0904 is arranged on every layer to folder
The lower section in the stage casing of the bed of material 0920, contacted with to the lower surface of material folding layer 0920, the upper filter screen band 0907 of another horizontal direction and lower filter
The lower section in the stage casing of guipure 0919 respectively sets a carrying roller 0904;Modified roller 0905 has 2,1 therein, is arranged on evaporator cylinder
The top of body 0908 and the position of the homonymy of pinch upper roll 0910, the location portability position of modified roller 0905 in the horizontal direction, are consolidated by bolt
It is fixed, to adjust the tension force of upper filter screen band 0907.
Multiple traction conveying rollers 0906 are arranged on every 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;Drawing the roll surface of conveying roller 0906 has and pinch upper roll 0910 and the roll surface locating slot of pinch under roll 0911
The stopper slot of identical 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, the present embodiment 1600mm according to the treating capacity of evaporator, traction is defeated
The quantity of roller 0906 is sent, can be determined according to evaporator specifications, it is larger to specification, traction can be configured in conveying roller 0906 is drawn
Motor, to improve the tension distribution of filter screen band, the present embodiment, 10 traction conveying rollers 0906 are set, in the 6th from bottom to up
Traction electric machine is configured on traction conveying roller 0906.
Upper filter screen band 0907 and lower filter screen band 0919, respectively it is slightly less than the traction roll surface stopper slot of conveying roller 0906 for a width
5~10mm of width filter screen band for no reason, 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 scopes are 0.5~2mm.
The basic configuration of evaporator tube 0908 is a rectangle housing erect, outer wall with structural steel frame structural strengthening,
As microwave cavity, wherein, a pair of 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, β=116.15 °, these folding faces can strengthen the refraction of microwave, and it is humorous to advantageously form microwave
Shake field, and wave field is evenly distributed;Whole evaporator tube 0908 is such as stainless with low electric damage value microwave reflection metallic conductor
The materials such as steel, aluminium construct, and be stainless steel SUS304 in the present embodiment, and cylinder is highly 2950mm, width 2100/2500mm, thickness
Spend 2150mm.
Evaporator tube 0908, at the diverse location of two folding face shape outer walls, it is provided with several microwave magnetrons 0924 and more
Individual infrared temperature measurement device 0902, between microwave magnetron 0924 and infrared temperature measurement device 0902, pass through the pulsewidth with microwave pulse power supply
Coupling with arteries and veins spacing controls, and makes microwave heating evaporation temperature in 25~100 DEG C of operated within range of setting;Evaporator tube
0908 microwave magnetron 0924 is presented at mouth, is closed with the polyfluortetraethylene plate of wave transparent.
2450MHz, or 915MHz can be selected in the microwave frequency of magnetron 0924, when solidliquid mixture electricity damage value is larger or steams
When hair amount is larger, 915MHz can be matched, typically matches 2450MHz;Microwave rated power configures:2450MHz, 5.4~50kW;
915MH, 20~120kW;In the present embodiment, the microwave frequency of magnetron 0924 is 2450MHz, 12 0.9kW magnetron, is matched somebody with somebody
The maximum rated power put is 10.8kW, and according to different solidliquid mixture and treating capacity, actual power can adjust.
Pinch upper roll 0910 and pinch under roll 0911, the lower section of evaporator tube 0108 is arranged on, with screw conveying feeding bed
0909 homonymy, respectively by the synchronous opposite driving of pinch upper roll motor 09101 and pinch under roll motor 09111, or a motor can be passed through
Via the synchronous opposite driving of belt wheel shunting, rotating speed can be adjusted by servo or frequency conversion;Pinch upper roll 0910 and the roll surface of pinch under roll 0911
Locating slot is offered respectively, can be according to the treating capacity of evaporator, in 500~5000mm scopes along the groove width of roll surface axis direction
It is interior selected, the present embodiment 1600mm;Groove depth δ scopes are 5~15mm, the present embodiment 10mm.
Stone roller 0912 is arranged on the pinch upper roll 0910 of revolution and the upstream end of pinch under roll 0911, axis horizontal distance range are
200~600mm, the present embodiment 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
The projection of axis is claimed to be overlapped with the axis of stone roller 0912, the width of the feed opening of screw conveying feeding bed 0909 along axis, compared with
Small 20~the 30mm of roll surface locating slot groove width 500~5000mm value ranges of pinch upper roll 0910;The blanking of screw conveying feeding bed 0909
Opening's edge is 20~70mm, the present embodiment 35mm to the width range of the conveying direction of material folding layer 0920;Screw conveying feeding bed
Gap between 0909 feed opening and the roll surface of stone roller 0912, by couple electric pushrod flashboard adjust, control range be 5~
25mm, the present embodiment 12mm.
Screw conveying feeding bed 0909, by varying pitch, or become spiral shell gauge structure, and revolution speed of screw, make solidliquid mixture
Certain material seal pressure is formed in the screw conveying feeding bed 0909, produces pressure difference at charging aperture, pressure differential range is 0.035~
0.095MPa, control can be associated with helical feed servomotor or variable-frequency motor 09091 by pressure sensor;Spiral transferring is sent into
The feed hopper of material bed 0909 is arranged on outside the microwave cavity of evaporator tube 0908;In evaporator tube 0908 adjacent to spiral
In the side wall of conveying charging bed 0909, the observation window that can be had an X-rayed is set, and window material is anti-microwave leakage glass.
Upper separate roller 0914 and lower separate roller 0916, the top of evaporator tube 0908 is arranged on, 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
Platform motor shunts synchronous opposite driving via belt wheel, and rotating speed can be adjusted by servo or frequency conversion.
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 contact, and contact force size is adjustable;Upper scraping plate 0915 and the material of lower scraping plate 0917
Expect for polytetrafluoroethylene (PTFE).
Brush roll 0913 is separately positioned on the top of separate roller 0914 and the lower section of lower separate roller 0916, makes the bristle of brush roll 0913
Contacted respectively along the bandwidth direction of upper filter screen band 0907 and lower filter screen band 0919;Brush roll 0913 is driven by brushroll motor 09131.
Helical feed hopper 0918 is arranged on the top of evaporator tube 0908, and the upper homonymy of separate roller 0914, 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 certain material envelope effect is formed in pipe, pressure difference is produced at discharge gate, pressure differential range is 0.035~0.095MPa, can be passed through
Helical feed motor speed controls;In the side wall of evaporator tube 0908 corresponding with helical feed hopper 0918, set
The observation maintenance door that can be had an X-rayed, window material are anti-microwave leakage glass.
Another 1 in modified roller 0905, the lower section of evaporator tube 0908 is arranged on, with the upper homonymy of separate roller 0914, changed course
The location portability position of roller 0905 in the horizontal direction, is bolted, to adjust the tension force of lower filter screen band 0919.
Nozzle 0921 is stratified and set on, and with the upper homonymy of separate roller 0914, conveying roller 0906 draws in orlop and time lower floor
The top of roll surface, the liquid mist that nozzle 0921 is formed, the surface to material folding layer 0920 can be uniformly sprayed at, the feed liquid sprayed, is led to
The outer compression pump matched somebody with somebody is crossed, is extracted via circulation fluid drain connection 0923 from liquid collecting bucket 0922.
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, make the tension distribution of upper filter screen band 0907 and lower filter screen band 0919 equal
It is even, and make upper filter screen band 0907 and lower filter screen band 0919, modified roller can be passed through respectively from separate roller 0914 and lower separate roller 0916
0905, pinch upper roll 0910 and pinch under roll 0911 are successfully returned to, is formed to the clip-on circulation transport structure of solidliquid mixture.
As shown in figure 8, the water fluid jet grind 0108 for plant ultra-fine grinding includes:Top charging hierarchy 041, and under
Portion's nozzle crushes structure 042, and top feeds hierarchy 041 and is connected with lower nozzle crushing structure 042 by bolt seal, and
Flat circular pipe type crushing chamber 0424 and blade the classification structure of impact ring 0414 is formed, wherein, flat circular pipe type crushing chamber 0424 wraps
Include multiinjector convergence 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 is D1, and the center circle diameter of feed opening 0415 is D2, and lower substrate outside diameter is D3, and blade is classified impact ring
0414 internal diameter is D4, and the charging internal diameter of adapter 0411 is Din, and discharge adapter internal diameter is Dout.
As shown in Fig. 8~Figure 12, top charging hierarchy 041, by feeding adapter 0411, discharge adapter 0412, upper base
Body 0413, blade classification impact ring 0414 and feed opening 0415 are formed, wherein, blade classification impact ring 0414 is rushed by convergence nozzle
Hit wall 0414a, uniform jet impact wall 0414b and tangential vane 0414c is formed.
As shown in fig. 10 and fig. 12, charging adapter 0411 is connected with upper matrix 0413 by bolt seal, charging adapter
0411 position determines by the center circle diameter D2 of feed opening 0415, D2=(0.80~0.87) × D0, it is preferable that D=0.84D0;Enter
Expect diameter Din=(0.2~0.4) × (D0-D1) of adapter 0411, 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 upper matrix 0413 circle, and passes through weldering with upper matrix
Connect in succession, the diameter Dout=(0.12~0.16) of discharge adapter 0412 × D0, it is preferable that Dout=0.13D0.
As shown in Figure 10, Figure 11 and Figure 12, blade classification impact ring 0414 is overall structure with upper matrix 0413, and blade divides
Level impact ring 0414 internal diameter D4=(0.45~0.65) × D0, it is preferable that D4=0.54D0;In blade classification impact ring 0414
Converge jet impact wall 0414a 40 °~54 ° of arc length angle, it is preferable that 48 °, and sprayed from the different convergences to cut angle
Mouth 0423a, 0423b, 0423c and 0423d axis, the tangent of low-angle is touched with wide-angle;Blade is classified impact ring
Uniform jet impact wall 0414b and the uniform axis of nozzle 0423 on 0414 is corresponding tangent, 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 is set
Put 72 ° of area's 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 compositions 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 sensor 0425, lower substrate 0426 and water under high pressure access tube 0427 are formed.
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 β that cuts angle of nozzle 0423 is
50 °~75 °, it is preferable that 62 °;Nozzle and uniform nozzle are converged, is connected to by thread seal in lower substrate 0422;Water under high pressure
Access tube 0427 is welded in 0426 cylindrical side wall of lower substrate, and 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 convergence nozzle is 4
Individual throat diameter is 1mm High pressure water jet nozzle;Multiple uniform nozzles are the height that 4~9 throat diameters are 0.7~2.5mm
Pressure water jet nozzle, it is preferable that convergence nozzle is that 4 throat diameters are 1mm High pressure water jet nozzles.
The crushing pressure of High pressure water jet nozzle is 5~30MPa, it is preferable that 7~12MPa.
The present invention utilizes carries out breaking-wall cell crushing for the water fluid jet grind of plant ultra-fine grinding to plant medicine, to carry
The solubility of senior middle school's pharmaceutically active substance;And using the thin bed of material microwave evaporation device of continuous strap-clamping-type by dissolved with active Chinese drug component material
Between solidliquid mixture is to being clipped in filter screen band, mixed with the horizontal transfer ways successively risen that come and go by microwave cavity, solid-liquid
Compound feed liquid absorbs microwave energy with thin uniform layer state, contained active Chinese drug component material is evaporated at a lower temperature, meanwhile, lead to
The loading again to isolating feed liquid is crossed, with circulating and evaporating, makes the solution dissolved with active Chinese drug component material under relatively low vacuum, by
Liquid-phase conversion is gas phase.Also, by specifically for the water fluid jet grind for plant ultra-fine grinding and the continuous entrainment
The coupling technique of the thin bed of material microwave evaporation device design of formula and servicing unit configuration, form a set of traditional Chinese medicine extyaction system
System.
By the water fluid jet grind for plant ultra-fine grinding, by the extraction raw material of active ingredient of Chinese herbs, i.e., with one
Determine the root of plant medicine of size requirement, rhizome, skin, leaf, flower, fruit, seed etc., impact and water in high-pressure water jet
Under wedge tension force and cavitation denudation, ultra-fine grinding to average grain diameter about < 5~l0 μm, make diameter about in 10~100 μ m in size
The cell wall damage of the various Chinese medicinal plant cells of scope, it is soluble in water to not only contribute to the polar component of active material, and
Under the violent turbulent flow emulsification of high-pressure water jet, nonpolar (the lipid or oiliness) composition for being also beneficial to active material is dissolved in
In water.
Because the water fluid jet grind for plant ultra-fine grinding is using water as working media, if in crushing process, passing through height
Hydraulic plunger pump continuously supplements work Jie's water outside extraction system, then can cause that the excessively dilution of active material is influenceed to steam
Evaporate efficiency.On the other hand, extraction system is configured with centrifugal separator, make high-pressure plunger pump, the water-jet for plant ultra-fine grinding
Stream mill, centrifugal separator and delivery pump form closed-circuit pulverization and separating circuit, and (the heavy thing of centrifugal separator separation is contained into thick
Grain) water fluid jet grind for being used for plant ultra-fine grinding is returned, carry out continuous circulation and crush;The lightweight that centrifugal separator is separated
Thing (the solidliquid mixture feed liquid of material containing active Chinese drug component and fine plant medicine particle) is sent into high-pressure plunger pump, as work
Medium circulation uses, until when the granularity of the lightweight thing of centrifugal separator separation reaches average grain diameter about < 5~l0 μm, with solid-liquid
The form of mixture feed liquid is transported into the thin bed of material microwave evaporation device of continuous strap-clamping-type and is evaporated processing.
Because plant granule size contained in work Jie's water is small, and almost without abrasion, therefore high-pressure plunger will not be caused
Supercharging push rod of the pump using simple linear re-ciprocating motion as operation principle is worn, and doping contact scar is produced to solution.Water-jet
Stream grinds the very little that heated up in crushing process, will not produce heat affecting to active material.
During nappe flip length, some in Chinese medicinal plant are easy to the volatile molecules escaped from liquid phase, due to
Impact and the cavitation of high-pressure water jet and produce volatilization, therefore in the row of the water fluid jet grind for plant ultra-fine grinding
Expect to set separator at adapter, this part escaping gas is fed directly to the condensation positioned at vaporising device back segment and gas-liquid point
From in device, trapped in the lump with effective component of chinese medicine.
As the plant roots of traditional Chinese medicine extyaction raw material, rhizome, skin, leaf, flower, fruit, seed etc., it is used to plant described
Before the water fluid jet grind of thing ultra-fine grinding crushes, water retting is first used in agitator tank, string is produced certain swelling, so as to
Water fluid jet grind carries out crushing of efficiently loosening.
By to a period of time breaking-wall cell crushing of the raw materials such as plant roots, rhizome, skin, leaf, flower, fruit, seed and activity
The dissolution processing of material, the heavy thing (containing coarse granule) separated via centrifugal separator are admitted to filtering means dehydration device and carry out solid-liquid
Separation, the slag charge of gained can be integrated into utilizing, such as feed or degradable farm chemical carrier.
The thin bed of material microwave evaporation device of a kind 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 continuously transported, in microwave resonance intracavitary with left and right
The transfer ways successively risen are come and gone, under microwave irradiation, body phase is carried out to the thin bed of material and uniformly heated, and by isolating feed liquid
Nozzle CYCLIC LOADING, to improve evaporation capacity.Liquid film layer is thinner, faster by thermal evaporation, evaporation capacity increase.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, steamed to improve
The vacuum in device is sent out, making feed liquid, Efficient Conversion is gas phase at a lower temperature.Simultaneously as pair using multilayer transportation state
Material folding layer, increase heat exchange specific surface area, vaporising device is compact, and area utilization is high.
Due to the mode of heating of microwave irradiation, instead of the heating steam being introduced directly into evaporator, in evaporator
Gas phase is only escaping gas caused by feed liquid is evaporated, and eliminates incremental contribution of the water vapour to gas phase in evaporator, makes steaming
Device is sent out under the swabbing action of vacuum pump set, also vacuum is significantly improved, helps to reduce on thin bed of material gas-liquid interface
Pressure, in favor of volatile component in the range of 25~105 DEG C low-temperature evaporation, can both improve the evaporation efficiency of feed liquid, reduction is waved
The gas-liquid separation load of hair property gas subsequent condensation, also reduce the possible influence for crossing heat effect to volatile component quality.
Using the characteristic that in microwave heating process, thermal inertia is small, controllability is good, control is loaded by the pulsed irradiation of microwave
System, is more accurately controlled evaporating temperature, further improves the quality of volatile component.
A kind of gas-phase activity material of the thin bed of material microwave evaporation device of continuous strap-clamping-type is discharged, is drawn into condensation dress
Put and gas-liquid separation device, make active material and condensed moisture from obtaining the active ingredient of Chinese herbs of liquid.Condensation and gas-liquid separation
High-efficiency condensation well known in the art and separator can be used, such as screw pipework condensation device, membrane separator, chromatography post separation
Device, macroreticular resin separator etc..
Solution after evaporation and concentration, there is the active Chinese drug component material of low saturated vapour pressure value containing some, through dehydration
Drying can be used as the raw material of micronized Chinese medicine.
Embodiments of the invention are described above in conjunction with accompanying drawing, but the invention is not limited in above-mentioned specific
Embodiment, above-mentioned embodiment is only schematical, rather than restricted, one of ordinary skill in the art
Under the enlightenment of the present invention, in the case of present inventive concept and scope of the claimed protection is not departed from, it can also make a lot
Form, these are belonged within the protection of the present invention.
Claims (10)
1. a kind of nappe flip length and strap-clamping-type microwave distillation extraction effective component of chinese medicine method, it is characterised in that including with
Lower step:
S1, the extraction raw material of effective component of chinese medicine after crushing is added in agitator tank, centrifugation is delivered to after adding water stirring
Machine;
S2, the heavy thing after separation is delivered to water fluid jet grind progress nappe flip length;
S3, the lightweight thing solution obtained after nappe flip length in the step S2 is delivered to the thin bed of material microwave steam of continuous strap-clamping-type
Transmitting apparatus, the microwave evaporation device use the pinch upper roll and pinch under roll of a pair of revolutions, by two filter screen bands, solid-liquid are mixed
Between thing is to being clipped in 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 successively risen 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 is heated evaporation;
S4, gas-phase activity material are aspirated into condenser, and liquid is condensed into together with vapor with vapor;
Active material and condensed moisture are made from obtaining the effective component of chinese medicine of liquid by separator again.
2. the method for nappe flip length according to claim 1 and strap-clamping-type microwave distillation extraction effective component of chinese medicine, its
It is characterised by, in the step S2, high-pressure plunger pump, water fluid jet grind, centrifugal separator is connected with slurry delivery pump is crushed
Form closed-circuit pulverization and separating circuit, the raw material in agitator tank, centrifugal separator is delivered to by plant pulp material conveying 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 for nappe flip length according to claim 2 and strap-clamping-type microwave distillation extraction effective component of chinese medicine, its
It is characterised by, the slurry after crushing obtains continuous circulation in closed-circuit pulverization and separating circuit and crushed, until by centrifugal separator
, will be light by flow control valve when the subparticle granularity in lightweight thing solution after separation reaches the setting index of average grain diameter
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 for nappe flip length according to claim 1 and strap-clamping-type microwave distillation extraction effective component of chinese medicine, its
It is characterised by, caused Chinese medicine volatile effective component is delivered to after microwave evaporation device during the nappe flip length
Trapped in the condenser of section.
5. the method for nappe flip length according to claim 1 and strap-clamping-type microwave distillation extraction effective component of chinese medicine, its
It is characterised by, the condenser is connected with handpiece Water Chilling Units.
6. the method for nappe flip length according to claim 1 and strap-clamping-type microwave distillation extraction effective component of chinese medicine, its
It is characterised by, in the step S1, by the extraction raw material containing effective component of chinese medicine:Root, rhizome, skin, leaf, flower, fruit or seed,
The mesh of granularity < 10 is crushed to by plant pulverizer, is added in agitator tank, then by solid-to-liquid ratio 1:(2~8)Water is added, in normal temperature
30 ~ 60min of lower impregnated raw material, during which agitator accomplished continuously or intermittently stirred with 0.2 ~ 1.5m/s of linear velocity.
7. the method for nappe flip length according to claim 1 and strap-clamping-type microwave distillation extraction effective component of chinese medicine, its
It is characterised by, in the step S3, lightweight thing solution is in the range of 25 ~ 120 DEG C in microwave evaporation device.
8. the method for nappe flip length according to claim 1 and strap-clamping-type microwave distillation extraction effective component of chinese medicine, its
It is characterised by, the continuous thin bed of material microwave evaporation device of 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 staggered, set and filter between pinch upper roll and pinch under roll
Guipure and lower filter screen band, the stone roller solidliquid mixture is delivered between upper filter screen band and lower filter screen band and by pinch upper roll and
Pinch under roll presses, and the traction conveying roller drives upper filter screen band and lower filter screen band to be conveyed in evaporator tube, the evaporator
Cylinder is provided with microwave heating equipment.
9. the method for nappe flip length according to claim 8 and strap-clamping-type microwave distillation extraction effective component of chinese medicine, its
It is characterised by, the top of the evaporator tube is provided with upper separate roller and lower separate roller, and upper filter screen band and lower filter screen band are at upper point
From being separated at 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 for nappe flip length according to claim 8 and strap-clamping-type microwave distillation extraction effective component of chinese medicine, its
It is characterised by, the evaporator tube is connected with vacuum extractor.
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CN112246353B (en) * | 2020-09-27 | 2023-09-22 | 内蒙古北化浩绅科技有限公司 | Mixed grinding device for asphalt material production |
EP4163000B1 (en) * | 2021-02-19 | 2024-04-10 | Anhui Jinhe Industrial Co., Ltd. | Production apparatus and production method for sucrose-6-ester |
CN117282124B (en) * | 2023-11-16 | 2024-03-22 | 北京露华本草生物科技有限公司 | Plant raw juice extraction process and equipment based on infrared heating |
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CN201074948Y (en) * | 2007-07-04 | 2008-06-18 | 天水华圆制药设备科技有限责任公司 | Fluid materials drier |
CN101773555A (en) * | 2009-01-09 | 2010-07-14 | 苏州知微堂生物科技有限公司 | Anti-AIDS five-in-one nano-TCM and production method thereof |
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