CN105251229A - Method for extracting traditional Chinese medicine effective components by water jet comminuting and entrainment type microwave distillation - Google Patents
Method for extracting traditional Chinese medicine effective components by water jet comminuting and entrainment type microwave distillation Download PDFInfo
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Abstract
The invention relates to a method for extracting traditional Chinese medicine effective components by water jet comminuting and entrainment type microwave distillation. The method comprises the following steps of S1, adding smashed extracting materials of the traditional Chinese medicine effective components to a mixing tank, adding water, mixing, and then sending to a centrifuge; S2, conveying separated heavy components to a water jet mill for the water jet comminuting; S3, conveying a light component solution obtained from the step S2 to a charging opening in the upper end of a continuous entrainment type thin-layer microwave evaporation device, so as to form an opposite interlayer structure including an upper filter screen belt, a solid-liquid mixed material layer and a lower filter screen belt by virtue of two filter screen belts, and passing through a microwave cavity in a horizontal back-and-forth layer-by-layer rising conveying mode; S4, sucking gas-phase active materials and steam into a condenser, so as to be condensed into liquid together with water steam, and then separating the active materials from condensed water by a separator, so as to obtain the liquid traditional Chinese medicine effective components. According to the method, cell disruption and distillation extraction of the high-quality traditional Chinese medicine effective components are realized by using a pure physical method.
Description
Technical field
The present invention relates to field of traditional Chinese medicine pharmacy, more particularly, relate to a kind of method of nappe flip length and strap-clamping-type microwave distillation extraction Effective Component of Chinese Medicine.
Background technology
Along with the raising of modern society's general level of the health, and people are to the approval of " back to nature " theory, be that raw-material medicine, food, health care and skin care item etc. are more and more paid attention to natural plants, wherein, Chinese medicine is because having unique complete theoretical system, deep humanism connotation, curative effect affirmative, having no side effect and be loved by the people.On the basis of inheriting tradition Chinese medicine processing technology and preparation technique, adopt new method, new technology carries out extraction and application to Effective Component of Chinese Medicine, is the important channel of improving traditional Chinese medicine quality, improving form of Chinese drug, Appropriate application natural resources of Chinese medicinal materials.
Plant medicine be taken from the root of plant, rhizome, skin, leaf, flower, really, seed and natural gum etc., its effective medicinal components, namely active material mainly comprises: alkaloid, glucoside, volatile oil, tannin, amino acid, ketone, alcohols, phenols, terpenes, glucoside, organic acid etc., these active materials are normally with metabolite, if cellulose, chlorophyll, starch, protein, resin, natural gum, carbohydrate etc. are matrix, be distributed in cell and in cytoplasm.When stripping, must first could discharge through cell membrane and cell membrane.But the cell tissue of plant is tight usually, and cell membrane is also very thick, makes solvent not easily permeate and spread, active ingredient or DDGS are difficult to by derect seething out.
In order to the effective elements of the medicine in extraction efficiently, first can carry out breaking-wall cell process to plant medicine, so that these active materials can stripping smoothly in a solvent.Research shows, if by plant medicine ultra-fine grinding to average grain diameter about 5 ~ l0 μm, makes its granularity be less than the diameter 10 ~ 100 μm of general plant cell, can make cell-wall breaking ratio reach >=95%, realize so-called breaking-wall cell pulverize.Therefore, utilize superfine grinding method, the particle size of plant can be made greatly to reduce, and specific area significantly increases, and plant medicine active component dissolution rate and recovery rate significantly improve, and also improves the effective rate of utilization of plant medicine simultaneously.
In order to realize pulverizing object to the breaking-wall cell of plant medicine, in the art, various known method can be adopted: shell class grinding device as utilized medium mill, involving vibrations mill, Ball-stirring mill, planetary mills and colloid mill, this kind of superfine grinding method also exists frictional heating, make active ingredient of Chinese herbs be subject to the problems such as heat deterioration and volatile ingredient easily lose, also there is the problem that abrasive media wearing and tearing doping is polluted.
And for example, utilize dry method mechanical impact comminution and air-flow crushing, but due to the toughness of string, impact comminution efficiency is made to be difficult to improve, meanwhile, due to the combustibility of string, in crushing process, there is the possibility of dust explosion, crushing system is made to adopt more complicated anti-riot technique, and the riot gear that deployment cost is higher.Though deep cooling crush can solve the pulverizing problem of toughness vegetable fibre, production cost is higher.
For another example, physical treatment method, makes breaking-wall cell by method sides such as ultrasonic wave, microwave, steam blastings.Wherein, supersonic cell broken wall is that the cavitation Erosion that utilizes high-frequency ultrasonic to produce in liquid and size degradation effect make cell membrane broken, and possible problem is limited to ultrasonic transducer power, and disposal ability is large not; When microwave frequency measurment is the plant medium microwave energy absorbing utilized in microwave field, because intracellular molecular polarization produces dipole Action of Superhigh Frequency Vibration, friction and heat-dissipating, when after the latent heat gasification that liquid phase scrubbing is enough, break through cell membrane disengaged vapor and reach breaking-wall cell object, possible problem is that the active material of Chinese medicinal plant is because of overheated and deteriorated; Steam blasting utilizes the steam with certain pressure to enter after in plant cell, and cause breaking-wall cell because unexpected pressure release makes steam discharge, possible problem remains overheated.Visible, current this kind of physical treatment method process intensity is comparatively large, and active ingredient loss is also larger.
Another kind of solvent extraction method, can under the condition not doing cell broken wall treatment, utilize material dissolubility difference in a solvent, namely select not needing dissolved element solubility little, and the solvent large to active agent solubility, enter in cell by the osmosis of solvent to cell membrane, dissolve soluble active ingredients, cause the concentration difference that cell is inside and outside, make intracellular concentrated solution constantly to external diffusion, solvent then constantly enters in cell, until when the inside and outside solution concentration of cell reaches dynamic equilibrium, saturated solution is leached, then adds novel solvent continuation stripping.Solvent can be the water of strong polarity, also can be hydrophily or lipophilic organic solvent.Solvent extraction method is divided into cold formulation and hot formulation two kinds, common solvent extraction method relative poor, and the time is long, and efficiency is lower, and the active ingredient relative amount of extraction is not high.
When cell because broken wall or diffusion make active material dissolve in after in solvent, then need further the active material of liquid phase is separated from solvent, namely distill extraction.In the art, various known method can be adopted: as traditional leach extraction method, comprise decocting method, infusion process, percolation, reflux extraction, the way of distillation, steam distillation etc.Or comparatively novel leach extraction method, comprise supercritical fluid extraction, ultrasonic extraction, microwave loss mechanisms, charged extraction method, semi-bionic extraction, eddy flow extraction method, pressurized counter-flow extraction method, Enzymatic Extraction method etc.
Wherein, the way of distillation, utilizes each component boiling point (volatility) in mixing material different, low boiling component is evaporated, then is condensed into liquid to be separated whole component.If take water as solvent, i.e. steam distillation, good economy performance, security are high, strong operability, and to water-soluble actives such as the semipolar alkaloid of plant medicine, tannin, amino acid, ketone, alcohols, glucoside, phenols, acylates, there is good extraction effect, but it is not good for the volatile oil of low polarity, glucoside, organic acid, terpenes fat-soluble active ingredient extraction effect, and needing higher evaporating temperature, side reaction is more, may affect the activity of active ingredient.
And for example, supercritical fluid CO
2extraction, the superpower solvability utilizing supercritical fluid to have, makes active material dissolve, and by the control of pressure and temperature, makes CO
2solvent reaches critical point in extraction process, completes the hypercritical transition of liquid phase to gas phase, and obtains the active material of liquid phase.The method purity is high, no solvent residue, is suitable for the extraction to the volatile ingredient of nonpolar or low pole mostly in plant medicine, therefore has more application in this area.But the method treating capacity is lower, equipment investment is comparatively large, cost is higher, low to the active material extraction yield of low volatility.
Known by above-mentioned analysis, the key technology extracting active component from plant medicine has 2 points, and one is, realizes breaking-wall cell; Two are, to the control of evaporating temperature when liquid-phase conversion is gas phase.The former is related to the dissolution rate of active material, and the latter is related to the quality of active material.
Known according to above analysis, in the art, known method is pulverized to the breaking-wall cell of plant medicine, main employing be dry method grinding process, its force mechanism pulverized mainly grinds stripping and smashes, the resistant to breakage resistance that material corresponding with force mechanism is produced is: resistance to compression, shearing resistance, bending resistance and anti-impact force, has namely lacked a tension reduction resistant force.And the mechanical strength rule of material is: compression strength is maximum, shearing strength is taken second place, and bending strength is less, and tensile strength is minimum.Therefore, pulverize in known method at plant medicine breaking-wall cell, pulverize force mechanism and lacked stretching (or tension force) the pulverization power that one can be improved material grindability, this is also the general character shortcoming of other dry method grinding process.In addition, because dry method grinding process is in mill stripping and fragmentation process, frictional heating phenomenon is produced.Cause the problem that corresponding cell technology for broken wall brings thus, as there is the deficiencies such as the not high and overheated active Chinese drug component substance degradation caused of sporoderm-broken rate.
In the art, to the solution being dissolved with active Chinese drug component material, carry out the evaporating temperature control aspect of gas phase conversion, in known method described above, take and comprise steam distillation, the measures such as normal-temperature distilled and decompression distillation, but " material of the same race has different saturated vapour pressures under not synthermal, and increase along with the rising of temperature, saturated vapour pressure value is higher, more be conducive to liquid phase and become gas phase " evaporating principle and active Chinese drug component material " temperature is too high causes deterioration " this to the coordination aspect of contradiction, mostly belong to conventional technological balance, the principle of relative shortage method and apparatus aspect breaks through.
The patent below quoted from wherein some method and apparatus aspect obtains certain success, but this can not to be interpreted as these existing technology be inevitably suitable.
Wei rattan children waits the Chinese patent CN02149695.1 of people, disclose a kind of Microwave Pretreatment extracting method of effective ingredients in plant, first dry plant is pulverized, add a small amount of fully moistening containing ethanol water, then carry out Quick Pretreatment as in microwave field, finally adding hot solvent agitator treating just can the extracts active ingredients in plant tissue out.
The Chinese patent CN200510016832.3 of the people such as Yu Yongli, disclose a kind of extraction process of active component in northern schisandra, step is: fructus schisandrae obtains finished product through selected → pulverizing → heating → microwave treatment → refluxing extraction → filtration → high speed centrifugation separation → vacuum drying.
The Chinese patent CN200610044442.1 of the people such as Ma Feng, discloses a kind of decompressed microwave extraction device for effective ingredients in plant extraction and method, is made up of micro-wave oven, extractor, condenser, separator and decompressor.Micro-wave oven is arranged on extractor periphery, is evenly arranged microwave generator in it; Extractor is provided with electric mixer, and extractor top arranges demagnetizer, and extractor top is extraction cell, and bottom arranges movable solvent storage room, middle by being with the dividing plate in uniform solvent penetration hole that extraction cell and apotheca are separated.Decompression and microwave action under, solvent evaporation becomes liquid solvent through condenser condenses, turns back to solvent storage room by circulation pipe, plant after microwave irradiation, by the device for discharging discharging of extractor bottom.Owing to have employed decompression and solvent recycling apparatus in device, accelerate the effective ingredients in plant leaching process that microwave irradiation causes, ensure simultaneously effective ingredients in plant can not Yin Wendu too high and thermal metamorphism occurs.
The Chinese patent CN200610104933.0 of the people such as Zhao Ying, discloses a kind of extraction preparation method of Effective Component of Chinese Medicine, after traditional Chinese medicinal material raw materials removal of impurities, adds corresponding extract, through inverse to ooze, lixiviate, and supersonic oscillations hydrotropy, Fast Stripping effective ingredient.Be applicable to the Chinese medicine of containing water-soluble, alcohol soluble active principals.
The Chinese patent CN200810051150.X of Pan Yongqi, the invention discloses a kind of method and device of continuous extracting Chinese medicine effective ingredient at normal temperature, solvent is mixed with 30 ~ 100 order Chinese medicine materials and makes mixed liquor, the electrode centre being transported to extractor is separated, electrode voltage is 3 ~ 9 kilovolts, frequency 3 ~ 9 KHz, make the high frequency electric by 20 ~ 200 amperes in mixed liquor, under the effect of high frequency electric and electric field force, the biomolecule of Chinese medicine material is polarized, manifest electric polarity, produce concussion, intermolecular attraction is destroyed, the structure of matter occurs loose, solvent can rapid osmotic inner to material, active ingredient is made to be rapidly dissolved among solvent, the dregs of a decoction and separated from solvent is carried out after extraction, obtain the solution containing Effective Component of Chinese Medicine.
The Chinese patent CN200910022006.8 of the people such as Qin Shengli, discloses a kind of preparation technology of extracting active ingredient of natural plant by supersonic, comprises the following steps: cleaning dedusting; Pulverize; Dipping: the mixing of materials tank that the natural plant raw material to be extracted after pulverizing puts into built-in agitator is carried out Keep agitation, in whipping process, in the natural plant raw material to be extracted in mixing of materials tank, add maceration extract and after mix and blend, obtain mixing of materials liquid; Ultrasonic wave extracts: under the effect of hydraulic circulation pump one, circulate by mixing of materials liquid by being connected to circulating line between mixing of materials tank and ultrosonic extractor constantly passing through from ultrosonic extractor is inner and carries out the extraction of continuous cycle type ultrasonic wave; Filter; Reduced pressure concentration.
The Chinese patent CN200910214229.4 of the people such as Yang Fu, disclose a kind of method and device thereof of extracting effective components of plants by ultrasonic cooperating with electrostatic field, comprising extractor is a cleaning groove type cylinder sound reactor, in extractor, contre electrode is set, electrostatic generator positive and negative electrode is electrically connected with contre electrode by gauge tap, the earth terminal of electrostatic generator is electrically connected with the sidewall of extractor, realizes the extraction to polar component and nonpolarity element.
The Chinese patent CN201110143520.4 of the people such as Zhang Zongquan, disclose a kind of electromagnetic force synergistic supersonic wave traditional Chinese medicine extyaction device, arrange in the upper end of tank body and be processed with charge door, tank body covers and is provided with the downward power ultrasonic transducer of spoke side, the spoke side of power ultrasonic transducer is provided with and extend into the radial ultrasonic radiant tube that tank body is interior, lower end connects with ultrasonic radiation dish, ultrasonic radiation dish is processed with filter opening; Between ultrasonic radiation dish and housing bottom, inner tank wall is provided with plate shaped filter membrane in tank body, in tank body, ultrasonic radiation dish is provided with magnetic stainless steel polyhedron, the lateral wall of tank body is provided with by 6 or 12 and the coil be arranged on skeleton be connected with Programmable Logic Controller.
The Chinese patent CN201110233876.7 of the people such as Chen Hongzhang, disclose a kind of raw material gas explosion preprocess method improving active components in medicinal plant dissolution rate: be placed in high-pressure bottle by with the material after water or aqueous solution preimpregnation, sealing, pass into medium, temperature of charge is made to maintain 0.5 ~ 30min at 40 ~ 250 DEG C, then quick pressure releasing, is discharged in non-pressure vessel by the material processed in high-pressure container, namely obtains the pretreated material of gas explosion; Described medium is air, carbon dioxide, ozone, liquid nitrogen, nitrogen, water vapour, supercritical CO
2in a kind of or combination of any two kinds.Combination of media gas explosion mode based on active components in medicinal plant biologically active under the multiple low temperature of selective employing, high pressure conditions, fully ensures material process intensity, under the active prerequisite not damaging active ingredient, improves active ingredient dissolution rate.
Shen Zhi has just waited the Chinese patent CN201210230560.7 of people, discloses a kind of device and method utilizing high-pressure fog counter-current to extract active ingredient of natural plant, by natural plants impurity to be extracted, pulverizing; Put into agitator tank again and add soak, obtain material suspension, in extractor, add Extraction solvent, the material suspension prepared is sprayed the drop that nebulizes and carry out spraying extraction, then high-pressure fog counter-flow extraction, finally removes solid impurity with centrifuge; Reduced pressure concentration, adopts spraying dry, microwave drying or vacuum drying to obtain product.
The Chinese patent CN201210502408.X of the people such as Zhao Wenchang, disclose a kind of traditional Chinese medicine extraction enrichment facility and extract concentrated method, the structure extracting enrichment facility comprises extraction unit and upgrading unit, extraction unit comprises extractor and liquid storage tank, piston moving up and down is provided with in extractor, when under the effect of piston rod in driving force, piston is made to move up with squeezing further of exerting pressure to the dregs of a decoction in upper compression chamber; Upgrading unit comprises concentrate container, vavuum pump and the heater for heating to concentrate container, is provided with the stair-stepping evaporator plate assembly forming liquid film in concentrate container, capable of circulation concentrated.
The Chinese patent CN200510130852.3 of Xu Yong equality people, disclose a kind of effective plant component extracting process, after the mixture of i.e. mechanical crushing solid plant raw material and appropriate chemical assistant, select water or alcohol extract active ingredient, micro-shear is produced between interface when utilizing mechanical crushing solid plant raw material, cell membrane is broken, fresh tangent plane is exposed, the mutual absorption of cluster of grains or micel or the principle of effect is there is between chemical assistant and active ingredient, change the micro-property of effective ingredients in plant, stripping quantity improves.
The Chinese patent application publication No. CN101371854A of Li Qiaoru, discloses a kind of wet pulverizing extracting method of Effective Component of Chinese Medicine.Comprise step: put in grinder by tcm and herbal slice or meal, add the solvent (ethanol, acetone etc. of water, variable concentrations) of 4 ~ 20 times amount, pulverize 5 ~ 40 minutes at a high speed in 10000 revs/min, after pulverizing, liquid is centrifugal 5 ~ 10 minutes in 5000 ~ 10000 revs/min, and gained liquid is traditional Chinese medicine extyaction liquid.
It should be noted that, in CN101371854A, although not clear and definite described wet pulverizing is any reducing mechanism, but pulverize based on it feature judgement that rotating speed is 5000 ~ 10000 revs/min, it should be small dimension colloid mill, namely by the ring-type tapered narrow small gap formed between high-speed rotator and fixation wall, because of the strong shear effect of fluid boundary-layer and the percussion of revolution toothed surfaces, the solid material in liquid is made to tear, be ground into fine particle.This is a kind of mode preferably to the pulverizing of fibrous plants, but Problems existing is the generation of crushing process along with heat, and this may cause deactivation or the deterioration of some Chinese traditional medicine biology active component.
Known based on above analysis, in the art, still there is no a kind of wet grinding technique at present, its force mechanism pulverized not only has mill stripping and smashes effect, have the direct broken cells of stretching action concurrently simultaneously, and with the form of feed liquid rete, heated by microwave irradiation, carry out distilling the method extracting Effective Component of Chinese Medicine.Therefore, expecting to provide a kind of by adopting the pulverizing force mechanism suitable to plant medicine raw material, making Chinese medicinal plant cell obtain abundant broken wall, to improve the solubility of active Chinese drug component material; Also expect to provide a kind of feed liquid for being dissolved with active Chinese drug component material, utilization can be inverted the equal material refining layer transported continuously, with the motion mode of round rising in microwave cavity, under the bigger serface of multilayer, pass through microwave irradiation, the thinner bed of material is carried out to the vaporising device of body phase homogeneous heating, realize the high efficient cryogenic evaporation of active Chinese drug component material.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of nappe flip length and strap-clamping-type microwave distillation to extract the method for Effective Component of Chinese Medicine, realizes the high-quality Effective Component of Chinese Medicine of breaking-wall cell and distillation extraction with pure physical method.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method constructing nappe flip length and strap-clamping-type microwave distillation extraction Effective Component of Chinese Medicine, comprises the following steps:
S1, the extraction raw material of Effective Component of Chinese Medicine after pulverizing is joined in agitator tank, add after water stirs and deliver to centrifugal separator;
S2, the heavy thing after being separated is delivered to water fluid jet grind and carries out nappe flip length;
S3, the light materials solution that described step S2 obtains is delivered to continuous strap-clamping-type thin bed of material microwave evaporation device upper end charge door, described microwave evaporation device adopts a pair pivotal pinch upper roll and pinch under roll, by two filter screen bands, by solidliquid 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 come and go with level the transfer ways successively risen and pass through microwave cavity, make described to the solidliquid mixture feed liquid in material folding layer, microwave energy absorbing under thin uniform layer state and by heating evaporation;
S4, gas-phase activity material, with steam, are sucked and enter condenser, and be condensed into liquid together with water vapour; Again by separator make active material and condensed moisture from, obtain liquid Effective Component of Chinese Medicine.
In such scheme, water fluid jet grind is by the impact of high-pressure water jet, water wedge tension force, cavitation denudation, make root, rhizome, skin, leaf, flower, really, the ultra-fine grinding granularity of the plant medicine raw material such as seed reaches average grain diameter and be about < 5 ~ l0 μm, the polar component being beneficial to active Chinese drug component is soluble in water, simultaneously, under the turbulent flow emulsification that high-pressure water jet is violent, nonpolar (fat or the oiliness) composition being also conducive to active Chinese drug component is soluble in water.
In such scheme, water fluid jet grind and centrifugal separator, high-pressure plunger pump and delivery pump form closed-circuit pulverization and separating circuit, the heavy thing (containing coarse granule) that centrifugal separator is separated is returned the described water fluid jet grind for plant ultra-fine grinding, carries out continuous circulation pulverizing; Light material liquid (the solidliquid mixture feed liquid containing active Chinese drug component material and the fine plant medicine particle) high-pressure plunger pump of making a gift to someone that centrifugal separator is separated, recycle as working media, until the subparticle in the described light material liquid of centrifugal separator separation, granularity reaches average grain diameter when being about < 5 ~ l0 μm, described light material liquid is switched out closed-circuit pulverization and separating circuit, and is transported to next stage and carries out vaporize draw.
In such scheme, described light material liquid (solidliquid mixture feed liquid) is by screw conveying feeding bed, with the upper and lower nip rolls of revolution is to being clipped between filter screen band, come and go with level the transfer ways successively risen and pass through microwave cavity, described light material liquid is with thin uniform layer state microwave energy absorbing, contained active Chinese drug component material is made to be converted into gas phase at a lower temperature, described heat exchange temperature is within the scope of 25 ~ 120 DEG C, and by the Loading Control of microwave pulse irradiation, evaporating temperature is controlled comparatively accurately.
In such scheme, by vacuum pump set, by the gas-phase activity material that described a kind of continuous strap-clamping-type thin bed of material microwave evaporation device evaporates, suction enters condenser and is condensed into liquid; Again by separator, make active material and condensed moisture from, obtain liquid Effective Component of Chinese Medicine, the vacuum of vacuum pump set is 0.035 ~ 0.095MPa.
In such scheme, described light material liquid, after the evaporation and concentration by described continuous strap-clamping-type thin bed of material microwave evaporation device, then is cooled to normal temperature via enriching slurry cooler, the cooled solution of evaporation and concentration, is used through dehydrating the raw material that can be used as micronized Chinese medicine.
In such scheme, by root, rhizome, skin, leaf, flower, really, the extraction raw material of the Effective Component of Chinese Medicine such as seed, granularity < 10 order (1.7mm) is crushed to by plant pulverizer, join in agitator tank, again by solid-to-liquid ratio 1:(2 ~ 8) add water, impregnated raw material 30 ~ 60min at normal temperatures, period agitator with linear velocity 0.2 ~ 1.5m/s continuously or intermittent stirring; By the swelling good raw material of dipping, by slurry transferring transport pump to described centrifugal separator, the heavy thing after separation is transported to the described water fluid jet grind for plant ultra-fine grinding; Light material liquid after separation, is transported to high-pressure plunger pump, recycles as working media.
In such scheme, in discharge adapter place of the described water fluid jet grind for plant ultra-fine grinding, separator is set, by the plant medicine volatile effective component produced in nappe flip length process, directly be delivered to the condenser and separator that are arranged in described a kind of continuous strap-clamping-type thin bed of material microwave evaporation device back segment, trap in the lump with Effective Component of Chinese Medicine.
Implement the method for nappe flip length of the present invention and strap-clamping-type microwave distillation extraction Effective Component of Chinese Medicine, there is following beneficial effect:
The present invention carries out breaking-wall cell pulverizing by water fluid jet grind to plant, to improve the solubility of active Chinese drug component material; And utilize continuous strap-clamping-type thin bed of material microwave evaporation device, make the solution high-efficiency evaporating being at a lower temperature dissolved with active material, finally by efficient condenser and separator, prepare the Effective Component of Chinese Medicine realizing breaking-wall cell and distillation extraction with pure physical method.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is the method technological process exemplary schematic illustration that a kind of nappe flip length and strap-clamping-type microwave distillation extract Effective Component of Chinese Medicine;
Fig. 2 is the main pseudosection of continuous strap-clamping-type thin bed of material microwave evaporation device;
Fig. 3 is the side cutaway view of continuous strap-clamping-type thin bed of material microwave evaporation device;
Fig. 4 is the top view of continuous strap-clamping-type thin bed of material microwave evaporation device;
Fig. 5 is the main pseudosection in feeding structure local of Fig. 2 shown device;
Fig. 6 be Fig. 2 shown device upper and lower nip rolls and to material folding Rotating fields local main pseudosection;
Fig. 7 is the main pseudosection in discharging structure local of Fig. 1 shown device;
Fig. 8 is the main pseudosection of water fluid jet grind 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 profile in Fig. 8;
Figure 11 is the main pseudosection of top charging hierarchy;
Figure 12 is the C direction view in Figure 11;
Figure 13 is the main pseudosection that lower nozzle pulverizes structure;
Figure 14 is the B direction view in Figure 13.
Detailed description of the invention
In order to there be understanding clearly to technical characteristic of the present invention, object and effect, now contrast accompanying drawing and describe the specific embodiment of the present invention in detail.
As shown in Figure 1, the method of Effective Component of Chinese Medicine is extracted in a kind of nappe flip length provided by the invention and the distillation of strap-clamping-type microwave temperature, its technological process and set device comprise: 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, pulverize slurry transferring pump 0105, pulverize slip separator 0106, flow control valve 0107, centrifugal separator 0108, continuous strap-clamping-type thin bed of material microwave evaporation device 0109, condenser 0110, separator 0111, vacuum pump set 0112, handpiece Water Chilling Units 0113.
Method processing step and the main technologic parameters of described a kind of nappe flip length and strap-clamping-type microwave temperature distillation extraction Effective Component of Chinese Medicine are as follows:
Step 1: by the root of plant, rhizome, skin, leaf, flower, really, the extraction raw material of the Effective Component of Chinese Medicine such as seed, granularity < 10 order (1.7mm) is crushed to by plant pulverizer, join in agitator tank 0101, again by solid-to-liquid ratio 1:(2 ~ 8) add water, impregnated raw material 30 ~ 60min at normal temperatures, period agitator with linear velocity 0.2 ~ 1.5m/s continuously or intermittent stirring; By the swelling good raw material of dipping, be delivered to centrifugal separator 0108 by plant pulp material conveying pump 0102, the heavy thing (containing raw material coarse granule) after separation is transported to the described water fluid jet grind 0104 for plant ultra-fine grinding; Lightweight thing after separation (the solidliquid mixture feed liquid containing active Chinese drug component material and fine plant medicine particle) solution, is transferred people's high-pressure plunger pump 0103, recycles as working media.
Step 2: the heavy thing after separation is taken over via charging, enters the described tubular pulverizing chamber of flat ring for the water fluid jet grind 0104 of plant ultra-fine grinding, carries out nappe flip length, slurry after pulverizing, by pulverizing slurry transferring pump 0105, is sucked via discharge adapter and discharges the described water fluid jet grind 0104 for plant ultra-fine grinding, then is delivered to centrifugal separator 0108 and is separated, by this process, heavy thing after centrifugal separator 0108 is separated, by high-pressure plunger pump 0103, the described water fluid jet grind 0104 for plant ultra-fine grinding, centrifugal separator 0108 is with in the closed-circuit pulverization pulverizing the formation of slurry transferring pump 0105 and separating circuit, acquisition continuous circulation is pulverized, until the subparticle in lightweight thing solution after being separated by centrifugal separator 0108, granularity reaches average grain diameter when being about the setting index of < 5 ~ l0 μm, by flow control valve 0107, light material liquid is switched out closed-circuit pulverization and separating circuit, and be transported into continuous strap-clamping-type thin bed of material microwave evaporation device 0109.
The pulverizing pressure of the nozzle of the described water fluid jet grind 0104 for plant ultra-fine grinding is 5 ~ 20MPa, preferably, 7 ~ 12MPa, the back pressure of the tubular crushing chamber of flat ring within the scope of 0.010 ~ 0.040MPa, preferably, 0.02 ~ 0.03MPa.
By pulverizing slip separator 0106, will directly be delivered to the condenser 0110 and separator 0111 trapping that are arranged in vaporising device back segment at the described escaping gas being used for producing in water fluid jet grind 0104 crushing process of plant ultra-fine grinding.
Step 3: the light material liquid obtained by step 2, be transported to described continuous strap-clamping-type thin bed of material microwave evaporation device 0109, by screw conveying feeding bed, with in revolution, pinch under roll is to being clipped between filter screen band, come and go with level the transfer ways successively risen and pass through microwave cavity, described light material liquid is with thin uniform layer state microwave energy absorbing, contained active Chinese drug component material is made to be converted into gas phase at a lower temperature, heat exchange temperature is within the scope of 25 ~ 120 DEG C, and by the Loading Control of microwave pulse irradiation, evaporating temperature is controlled comparatively accurately.
The active material of gas phase, under the swabbing action of vacuum pump set 0112, discharge described continuous strap-clamping-type thin bed of material microwave evaporation device 0109 via upper end pump orifice, the vacuum of vacuum pump set 0112 is 0.035 ~ 0.095MPa.
Discharge the gas-phase activity material of described continuous strap-clamping-type thin bed of material microwave evaporation device 0109, be sucked and enter condenser 0110, and be condensed into liquid together with water vapour; Again by separator 0111, make active material and condensed moisture from, obtain liquid Effective Component of Chinese Medicine.
Solution after evaporation and concentration, lower end via described continuous strap-clamping-type thin bed of material microwave evaporation device 0109 is discharged, being cooled to normal temperature by enriching slurry cooler 0111 again, the cooled solution of evaporation and concentration, being used through dehydrating the raw material that can be used as micronized Chinese medicine.
Handpiece Water Chilling Units 0113 provides cooling fluid, chilling temperature scope 0.5 ~ 8 DEG C for condenser 0110.
The described water fluid jet grind for plant ultra-fine grinding and described continuous strap-clamping-type thin bed of material microwave evaporation device, and in extraction system, be configured with situ cleaning CIP device and the measure of steam high-temperature sterilization.
As shown in Fig. 2-Fig. 7, continuous strap-clamping-type thin bed of material microwave evaporation device 0109 comprises: boil-off gas discharge pipe 0901, infrared temperature measurement device 0902, evaporimeter upper cover 0903, carrying roller 0904, modified roller 0905, traction 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, pinch upper roll 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 separate 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, liquid collecting 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 is arranged on the vertex of a cone center of evaporimeter upper cover 0903, by sealing flange or weld connection; Multiple infrared temperature measurement device 0902 is arranged on the folding face shape sidewall of evaporimeter upper cover 0903 and evaporator tube 0908, connected by flange and bolt seal, it is inner to evaporimeter that infrared measurement of temperature hot spot runs through evaporator tube 0908 through hole, the quantity of infrared temperature measurement device 0,902 5 ~ 9, the present embodiment is 5; Carrying roller 0904 is arranged on every layer of below to material folding layer 0920 stage casing, contacts with to the lower surface of material folding layer 0920, and the upper filter screen band 0907 of another horizontal direction and the below in lower filter screen band 0919 stage casing respectively arrange a carrying roller 0904; Modified roller 0905 has 2, wherein 1, is arranged on the position with pinch upper roll 0910 homonymy above evaporator tube 0908, and modified roller 0905 location portability position in the horizontal direction, is bolted, to adjust the tension force of upper filter screen band 0907.
Multiple traction conveying roller 0906 is arranged on every layer of both sides to material folding layer 0920, carries to make to alter course to material folding layer 0920, and load-bearing solidliquid mixture; Traction conveying roller 0906 roll surface has the stopper slot with pinch upper roll 0910 and pinch under roll 0911 roll surface locating slot same size and structure, to prevent material folding layer 0920 sideslip under transportation state; Stopper slot is along the width of roll surface axis direction, can according to the treating capacity of evaporimeter, selected within the scope of 500 ~ 5000mm, the present embodiment is 1600mm, the quantity of traction conveying roller 0906, can determine according to evaporator specifications, larger to specification, traction electric machine can be configured in traction conveying roller 0906, to improve the tension distribution of filter screen band, the present embodiment, arranges 10 traction conveying rollers 0906, and the traction conveying roller 0906 of the 6th from bottom to up configures traction electric machine.
Upper filter screen band 0907 and lower filter screen band 0919, it is respectively the band of filter screen for no reason that a width is slightly less than traction conveying roller 0906 roll surface stopper slot width 5 ~ 10mm, filter screen band is the nonmetallic materials of wave transparent, cotton as thin is weaved cotton cloth, or terylene filter cloth, terylene filter screen, nylon leaching net etc., the present embodiment is that cotton is weaved cotton cloth, 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, as microwave cavity, wherein, a pair of plummet direction side in opposite directions, can be designed to folding face shape, the angle β scope between folding face is 120 ° ~ 170 °, in the present embodiment, β=116.15 °, the refraction of microwave can be strengthened in these folding faces, is conducive to forming microwave resonance field, and wave field is evenly distributed; Whole evaporator tube 0908 is with low electric damage value microwave reflection metallic conductor, and as the material structure such as stainless steel, aluminium, in the present embodiment, be stainless steel SUS304, cylindrical shell height is 2950mm, width 2100/2500mm, thickness 2150mm.
Evaporator tube 0908, the diverse location place of two folding face shape outer walls, be provided with several microwave magnetron 0924 and multiple infrared temperature measurement device 0902, between microwave magnetron 0924 and infrared temperature measurement device 0902, by controlling with being coupled of pulsewidth and arteries and veins spacing of microwave pulse power supply, make heating using microwave evaporating temperature at 25 ~ 100 DEG C of operated within range of setting; The microwave magnetron 0924 of evaporator tube 0908 presents mouth place, closes with the polyfluortetraethylene plate of wave transparent.
The microwave frequency of magnetron 0924 can select 2450MHz, or 915MHz, when solidliquid mixture electricity damage value is comparatively large or evaporation capacity is larger, can matches 915MHz, generally match 2450MHz; Microwave rated power configures: 2450MHz, 5.4 ~ 50kW; 915MH, 20 ~ 120kW; In the present embodiment, the microwave frequency of magnetron 0924 is the magnetron of 2450MHz, 12 0.9kW, and the maximum rated power of configuration is 10.8kW, according to different solidliquid mixtures and treating capacity, and actual power adjustable.
Pinch upper roll 0910 and pinch under roll 0911, be arranged on the below of evaporator tube 0108, with screw conveying feeding bed 0909 homonymy, respectively by pinch upper roll motor 09101 and pinch under roll motor 09111 locking phase to driving, or shunt locking phase to driving by a motor via belt wheel, rotating speed is by servo or frequency conversion adjustment; Pinch upper roll 0910 and pinch under roll 0911 roll surface offer locating slot respectively, along the groove width of roll surface axis direction, can according to the treating capacity of evaporimeter, and selected within the scope of 500 ~ 5000mm, the present embodiment is 1600mm; Groove depth δ scope is 5 ~ 15mm, and the present embodiment is 10mm.
Stone roller 0912 is arranged on pivotal pinch upper roll 0910 and pinch under roll 0911 upstream end, and axis horizontal distance range is 200 ~ 600mm, and the present embodiment is 345mm; Stone roller 0912 is driven by stone roller motor 09121, and rotating speed is by servo or frequency conversion adjustment.
Screw conveying feeding bed 0909 is arranged on the top of stone roller 0912, the projection of the feed opening axis of symmetry of screw conveying feeding bed 0909 and the dead in line of stone roller 0912, the feed opening of screw conveying feeding bed 0909 along the width of axis, compared with the little 20 ~ 30mm of pinch upper roll 0910 roll surface locating slot groove width 500 ~ 5000mm value range; The feed opening of screw conveying feeding bed 0909 is along being 20 ~ 70mm to the width range of material folding layer 0920 throughput direction, and the present embodiment is 35mm; Gap between screw conveying feeding bed 0909 feed opening and stone roller 0912 roll surface, adjusted by the flashboard connecting electric pushrod, control range is 5 ~ 25mm, and the present embodiment is 12mm.
Screw conveying feeding bed 0909, pass through varying pitch, or become spiral shell gauge structure, and revolution speed of screw, solidliquid mixture is made to form certain material seal pressure in screw conveying feeding bed 0909, produce pressure reduction at charging aperture place, pressure differential range is 0.035 ~ 0.095MPa, to associate control by pressure sensor with helical feed servomotor or variable-frequency motor 09091; The feed hopper of screw conveying feeding bed 0909 is arranged on outside the microwave cavity of evaporator tube 0908; On the sidewall of the contiguous screw conveying feeding bed 0909 of evaporator tube 0908, arrange the observation window that can have an X-rayed, window material is anti-microwave leakage glass.
Upper separate roller 0914 and lower separate roller 0916, be arranged on the top of evaporator tube 0908, with helical feed hopper 0918 homonymy, respectively by upper separate roller motor 09141 and lower separate roller motor 09161 locking phase to driving, or shunt locking phase to driving by a motor via belt wheel, rotating speed is by servo or frequency conversion adjustment.
Upper scraping plate 0915 and lower scraping plate 0917 are separately positioned on the surface of separate roller 0914 and lower separate roller 0916, and contact with lower filter screen band 0919 with corresponding upper filter screen band 0907, contact force size is adjustable; Upper scraping plate 0915 and lower scraping plate 0917 material are polytetrafluoroethylene (PTFE).
Brush roll 0913 to be separately positioned on above separate roller 0914 and below lower separate roller 0916, and the bristle of brush roll 0913 is contacted along the bandwidth direction of upper filter screen band 0907 with lower filter screen band 0919 respectively; Brush roll 0913 is driven by brushroll motor 09131.
Helical feed hopper 0918 is arranged on the top of evaporator tube 0908, with upper separate roller 0914 homonymy, and upper scraping plate 0915 and lower scraping plate 0917 and brush roll 0913 are dissolved in wherein, what make to remove all falls into helical feed hopper 0918 to material folding layer 0920, the conveyor screw of its underpart passes through varying pitch, or become spiral shell gauge structure, and revolution speed of screw, make material in carrier pipe, form certain material envelope effect, pressure reduction is produced at discharge gate place, pressure differential range is 0.035 ~ 0.095MPa, controls by helical feed motor speed; On the sidewall of the evaporator tube 0908 corresponding with helical feed hopper 0918, arrange the observation access door that can have an X-rayed, window material is anti-microwave leakage glass.
Another 1 in modified roller 0905, be arranged on below evaporator tube 0908, with upper separate roller 0914 homonymy, modified roller 0905 location portability position in the horizontal direction, is bolted, to adjust the tension force of lower filter screen band 0919.
Nozzle 0921 is stratified and set on, with upper separate roller 0914 homonymy, the top of orlop and time lower floor's traction conveying roller 0906 roll surface, the liquid mist that nozzle 0921 is formed, evenly can be sprayed at the surface to material folding layer 0920, the feed liquid sprayed, by the compression pump of joining outward, extracts from liquid collecting bucket 0922 via circulation fluid drain connection 0923.
Upper separate roller 0914, lower separate roller 0916, traction conveying roller 0906, pinch upper roll 0910, the rotating speed of pinch under roll 0911 and stone roller 0912, by PLC or industrial computer integrating control, make the tension distribution of upper filter screen band 0907 and lower filter screen band 0919 even, and make upper filter screen band 0907 and lower filter screen band 0919, can respectively from separate roller 0914 and lower separate roller 0916, by modified roller 0905, successfully turn back to pinch upper roll 0910 and pinch under roll 0911, formed the clip-on circulation transport structure of solidliquid mixture.
As shown in Figure 8, water fluid jet grind 0108 for plant ultra-fine grinding comprises: top charging hierarchy 041, structure 042 is pulverized with lower nozzle, top charging hierarchy 041 and lower nozzle are pulverized structure 042 and are connected by bolt seal, and form the tubular crushing chamber 0424 of flat ring and blade classification impact ring 0414 structure, wherein, the tubular crushing chamber 0424 of flat ring comprises multiinjector and converges disintegrating area, and uniform nozzle multiple spot tangential impact disintegrating area.
As shown in Fig. 8 ~ Figure 14, the outer diameter of the tubular crushing chamber 0424 of flat ring is D0, the inner diameter of the tubular crushing chamber 0424 of flat ring is D1, feed opening 0415 center circle diameter is D2, lower substrate outside diameter is D3, it is D4 that ring 0414 internal diameter is impacted in blade classification, and charging adapter 0411 internal diameter 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 matrix 0413, ring 0414 is impacted in blade classification and feed opening 0415 is formed, wherein, blade classification impact ring 0414 is made up of convergence jet impact wall 0414a, uniform jet impact wall 0414b and tangential vane 0414c.
As shown in fig. 10 and fig. 12, charging adapter 0411 is connected by bolt seal with upper matrix 0413, and charging adapter 0411 position is determined by feed opening 0415 center circle diameter D2, D2=(0.80 ~ 0.87) × D0, preferably, and D=0.84D0; Charging adapter 0411 diameter Din=(0.2 ~ 0.4) × (D0-D1), preferably, Din=0.23 × (D0-D1), D0 span 300 ~ 1160mm.
As shown in Fig. 8, Figure 13 and Figure 14, the inner diameter of the tubular crushing chamber 0424 of flat ring is D1 is D1=(0.55 ~ 0.75) × D0, preferably, and D1=0.64D0.
As is illustrated by figs. 11 and 12, discharge adapter 0412 is positioned at the center of matrix 0413 circle, and with upper matrix by being welded to connect, discharge adapter 0412 diameter Dout=(0.12 ~ 0.16) × D0, preferably, Dout=0.13D0.
As shown in Figure 10, Figure 11 and Figure 12, it is overall structure that blade classification impacts ring 0414 with upper matrix 0413, and ring 0414 internal diameter D4=(0.45 ~ 0.65) × D0 is impacted in blade classification, preferably, and D4=0.54D0; The arc length angle 40 ° ~ 54 ° of the convergence jet impact wall 0414a on ring 0414 is impacted in blade classification, preferably, 48 °, and from there is the axis of different convergence nozzle 0423a, 0423b, 0423c and 0423d of cutting angle, touch low-angle tangent with wide-angle; The uniform jet impact wall 0414b that blade classification is impacted on ring 0414 is corresponding tangent with uniform nozzle 0423 axis, uniform jet impact wall 0414b arc length angle 16 ° ~ 20 °, preferably, and 18 °; Tangential vane 0414c on blade classification impact ring 0414 cuts angle 25 ° ~ 50 °, preferably, 30 °, tangential vane 0414c setting area arc length angle 42 °, the tangential vane 0414c setting area arc length angle 72 ° of next-door neighbour's feed opening 0415; Tangential vane 0414c height h=(2.8 ~ 3.5) × (D0-D1), preferably, h=3.1 × (D0-D1); The blade passage gap width of two alternate formations of tangential vane 0414c is 3 ~ 6mm, preferably, and 4mm.
As shown in Figure 10, Figure 13 and Figure 14, lower nozzle pulverizes structure 042, by nozzle plug 0421, annular high voltage water distribution room 0422, converge nozzle 0423a, 0423b, 0423c and 0423d, uniform nozzle 0423, and the tubular crushing chamber 0424 of flat ring, pressure sensor 0425, lower substrate 0426 and water under high pressure access tube 0427 are formed.
As shown in Figure 10, converging nozzle 0423a and horizontal axis angle is 10 ° ~ 20 °, preferably, 15 °, the neighbour angle between convergence nozzle 0423b, 0423c and 0423d be 17 ° ~ 25 ° preferably, 20 °; The β that cuts angle of uniform nozzle 0423 is 50 ° ~ 75 °, preferably, and 62 °; Converge nozzle and uniform nozzle, be connected in lower substrate 0422 by thread seal; Water under high pressure access tube 0427 is welded on lower substrate 0426 cylindrical sidewall, and communicates with annular high voltage water distribution room 0422.
As shown in Fig. 8 and Figure 14, the cross section of fluid channel size of the tubular crushing chamber 0424 of flat ring: width B=0.5 × (D0-D1), height H=(0.15 ~ 0.35) × (D0-D1), preferably, H=0.2 (D0-D1).
Convergence nozzle is 3 ~ 7 throat diameters is 0.7 ~ 2.5mm High pressure water jet nozzle, and preferably, convergence nozzle is 4 throat diameters is the High pressure water jet nozzle of 1mm; Multiple uniform nozzle is 4 ~ 9 throat diameters is the High pressure water jet nozzle of 0.7 ~ 2.5mm, and preferably, convergence nozzle is 4 throat diameters is 1mm High pressure water jet nozzle.
The pulverizing pressure of High pressure water jet nozzle is 5 ~ 30MPa, preferably, and 7 ~ 12MPa.
The present invention utilizes the water fluid jet grind being used for plant ultra-fine grinding to carry out breaking-wall cell pulverizing to plant medicine, to improve the solubility of active Chinese drug component material; And utilize continuous strap-clamping-type thin bed of material microwave evaporation device to be dissolved with the solidliquid mixture of active Chinese drug component material to being clipped between filter screen band, come and go with level the transfer ways successively risen and pass through microwave cavity, solidliquid mixture feed liquid is with thin uniform layer state microwave energy absorbing, contained active Chinese drug component material is evaporated at a lower temperature, simultaneously, by the loading again to segregation feed liquid, with circulating and evaporating, making the solution being dissolved with active Chinese drug component material under lower vacuum, is gas phase by liquid-phase conversion.Further, by the special coupling technique for the described water fluid jet grind for plant ultra-fine grinding and described continuous strap-clamping-type thin bed of material microwave evaporation apparatus design and servicing unit configuration, a set of traditional Chinese medicine extyaction system is formed.
By the described water fluid jet grind for plant ultra-fine grinding, by the extraction raw material of active ingredient of Chinese herbs, namely there is the root of the plant medicine of certain particle size dimensional requirement, rhizome, skin, leaf, flower, really, seed etc., under the impact of high-pressure water jet and water wedge tension force and cavitation denudation, ultra-fine grinding to average grain diameter is about < 5 ~ l0 μm, make diameter about the cell wall damage of the various Chinese medicinal plant cells of 10 ~ 100 μm of size ranges, the polar component being not only conducive to active material is soluble in water, and under the violent turbulent flow emulsification of high-pressure water jet, also nonpolar (fat or the oiliness) composition being conducive to active material is soluble in water.
Because the described water fluid jet grind for plant ultra-fine grinding is working media with water, if in crushing process, from extraction system, supplement work Jie water continuously by high-pressure plunger pump, then can cause the too dilution of active material and affect distillation efficiency.To this, extraction system is configured with centrifugal separator, high-pressure plunger pump, the described water fluid jet grind for plant ultra-fine grinding, centrifugal separator and delivery pump is made to form closed-circuit pulverization and separating circuit, the heavy thing (containing coarse granule) that centrifugal separator is separated is returned the described water fluid jet grind for plant ultra-fine grinding, carries out continuous circulation pulverizing; Lightweight thing (the solidliquid mixture feed liquid containing active Chinese drug component material and the fine plant medicine particle) high-pressure plunger pump of making a gift to someone that centrifugal separator is separated, recycle as working media, until the granularity of lightweight thing that centrifugal separator is separated reaches average grain diameter when being about < 5 ~ l0 μm, be transported into continuous strap-clamping-type thin bed of material microwave evaporation device with the form of solidliquid mixture feed liquid and carry out evaporation process.
Because plant granule size contained in work Jie water is small, and almost without abrasion, therefore the supercharging push rod wearing and tearing that high-pressure plunger pump is operation principle with simple linear re-ciprocating motion can not be caused, and doping contact scar is produced to solution.Water fluid jet grind heats up very little in crushing process, can not produce heat affecting to active material.
In nappe flip length process, some in Chinese medicinal plant are easy to the volatile molecules of escaping from liquid phase, volatilization is produced due to the impact of high-pressure water jet and cavitation, therefore separator is set in discharge adapter place of the described water fluid jet grind for plant ultra-fine grinding, this part escaping gas is directly delivered to the condensation and gas-liquid separation device that are arranged in vaporising device back segment, traps in the lump with Effective Component of Chinese Medicine.
As the plant roots of traditional Chinese medicine extyaction raw material, rhizome, skin, leaf, flower, really, seed etc., before the described water fluid jet grind for plant ultra-fine grinding is pulverized, first in agitator tank with water retting, string is produced certain swelling, the pulverizing so that water fluid jet grind is efficiently loosened.
By to plant roots, rhizome, skin, leaf, flower, really, a period of time breaking-wall cell of the raw material such as seed pulverizes and the stripping process of active material, the heavy thing (containing coarse granule) be separated via centrifugal separator is admitted to filtering means dehydration device and carries out Separation of Solid and Liquid, the slag charge of gained can be fully utilized, as feed or degradable farm chemical carrier etc.
The continuous strap-clamping-type of described one thin bed of material microwave evaporation device, utilize pivotal pinch upper roll and pinch under roll, what formed clamping structure by upper filter screen band and lower filter screen band is inverted the even thin bed of material transported continuously, come and go the transfer ways successively risen with left and right in microwave cavity, under microwave irradiation, body phase homogeneous heating is carried out to the thin bed of material, and by the nozzle CYCLIC LOADING to segregation feed liquid, improves evaporation capacity.Liquid rete is thinner, faster by thermal evaporation, and evaporation capacity increases.Meanwhile, rete quantity is more, and specific area is larger, and evaporation capacity is also larger.
The continuous strap-clamping-type of described one thin bed of material microwave evaporation device, also by the hermetically-sealed construction of charging and discharging, improves the vacuum in evaporimeter, make feed liquid at a lower temperature Efficient Conversion be gas phase.Meanwhile, due to adopt multilayer transportation state to material folding layer, heat exchange specific area is increased, and vaporising device is compact, and area utilization is high.
Due to the mode of heating of microwave irradiation, instead of the heating steam directly imported in evaporimeter, gas phase in evaporimeter is only feed liquid and evaporates the escaping gas produced, eliminate the incremental contribution of water vapour to gas phase in evaporimeter, make evaporimeter under the swabbing action of vacuum pump set, also vacuum is made to significantly improve, contribute to reducing the pressure on thin bed of material gas-liquid interface, be beneficial to volatile component low-temperature evaporation within the scope of 25 ~ 105 DEG C, both the evaporation efficiency of feed liquid can have been improved, reduce the gas-liquid separation load of escaping gas subsequent condensation, also reduce possible heat effect excessively to the impact of volatile component quality.
Utilize in microwave heating process, thermal inertia be little, characteristic that controllability is good, by the pulsed irradiation Loading Control of microwave, evaporating temperature is controlled comparatively accurately, improves the quality of volatile component further.
Discharge the gas-phase activity material of described a kind of continuous strap-clamping-type thin bed of material microwave evaporation device, suction enters condensing unit and gas-liquid separation device, make active material and condensed moisture from, obtain the active ingredient of Chinese herbs of liquid state.Condensation and gas-liquid separation can adopt high-efficiency condensation well known in the art and separator, as screw pipework condensation device, membrane separator, chromatographic column separator, macroreticular resin separator etc.
Solution after evaporation and concentration, has the active Chinese drug component material of low saturated vapour pressure value containing some, be used through dehydrating the raw material that can be used as micronized Chinese medicine.
By reference to the accompanying drawings embodiments of the invention are described above; but the present invention is not limited to above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is only schematic; instead of it is restrictive; those of ordinary skill in the art is under enlightenment of the present invention; do not departing under the ambit that present inventive concept and claim protect, also can make a lot of form, these all belong within protection of the present invention.
Claims (10)
1. nappe flip length and strap-clamping-type microwave distillation extract a method for Effective Component of Chinese Medicine, it is characterized in that, comprise the following steps:
S1, the extraction raw material of Effective Component of Chinese Medicine after pulverizing is joined in agitator tank, add after water stirs and deliver to centrifugal separator;
S2, the heavy thing after being separated is delivered to water fluid jet grind and carries out nappe flip length;
S3, the light materials solution that described step S2 obtains is delivered to continuous strap-clamping-type thin bed of material microwave evaporation device, described microwave evaporation device adopts a pair pivotal pinch upper roll and pinch under roll, by two filter screen bands, by solidliquid 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 come and go with level the transfer ways successively risen and pass through microwave cavity, make described to the solidliquid mixture feed liquid in material folding layer, microwave energy absorbing under thin uniform layer state and by heating evaporation;
S4, gas-phase activity material, with steam, are sucked and enter condenser, and be condensed into liquid together with water vapour; Again by separator make active material and condensed moisture from, obtain liquid Effective Component of Chinese Medicine.
2. nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract the method for Effective Component of Chinese Medicine, it is characterized in that, in described step S2, high-pressure plunger pump, water fluid jet grind, centrifugal separator and pulverizing slurry transferring pump are connected to form closed-circuit pulverization and separating circuit, raw material in agitator tank, be delivered to centrifugal separator by plant pulp material conveying pump, the heavy thing after separation is transported to water fluid jet grind; Lightweight thing solution after separation, is transferred people's high-pressure plunger pump, recycles as working media.
3. nappe flip length according to claim 2 and strap-clamping-type microwave distillation extract the method for Effective Component of Chinese Medicine, it is characterized in that, slurry after pulverizing obtains continuous circulation and pulverizes in closed-circuit pulverization and separating circuit, until when the subparticle granularity in lightweight thing solution after being separated by centrifugal separator reaches the setting index of average grain diameter, by flow control valve, lightweight thing solution is switched out closed-circuit pulverization and separating circuit, and be transported to the upper and lower nip rolls of microwave evaporation device to being clipped between filter screen band.
4. nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract the method for Effective Component of Chinese Medicine, it is characterized in that, the aroma volatile produced in described water fluid jet grind crushing process is delivered to the condenser being arranged in vaporising device back segment and traps.
5. nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract the method for Effective Component of Chinese Medicine, and it is characterized in that, described condenser is connected with handpiece Water Chilling Units.
6. nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract the method for Effective Component of Chinese Medicine, it is characterized in that, in described step S1, by root, rhizome, skin, leaf, flower, really, the extraction raw material of the Effective Component of Chinese Medicine such as seed, granularity < 10 order is crushed to by plant pulverizer, join in agitator tank, again by solid-to-liquid ratio 1:(2 ~ 8) add water, impregnated raw material 30 ~ 60min at normal temperatures, period agitator with linear velocity 0.2 ~ 1.5m/s continuously or intermittent stirring.
7. nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract the method for Effective Component of Chinese Medicine, it is characterized in that, in described step S3, in low-temperature evaporation device in microwave evaporation device lightweight thing solution within the scope of 25 ~ 120 DEG C.
8. nappe flip length according to claim 1 and strap-clamping-type microwave distillation extract the method for Effective Component of Chinese Medicine, it is characterized in that, described continuous strap-clamping-type thin bed of material microwave evaporation device comprises evaporator tube, stone roller is provided with in described evaporator tube, pinch upper roll, the traction conveying roller that pinch under roll and multiple layering are crisscross arranged, upper filter screen band and lower filter screen band are set between pinch upper roll and pinch under roll, solidliquid mixture to be delivered between upper filter screen band and lower filter screen band and by pinch upper roll and pinch under roll pressing by institute's stone roller, described traction conveying roller drives upper filter screen band and lower filter screen band to carry in evaporator tube, described evaporator tube is provided with microwave heating equipment.
9. nappe flip length according to claim 8 and strap-clamping-type microwave distillation extract the method for Effective Component of Chinese Medicine, it is characterized in that, the top of described evaporator tube is provided with separate roller and lower separate roller, upper filter screen band and lower filter screen band upper separate roller and lower separate roller place separated, the side of described upper separate roller is provided with upper scraping plate, and the side of described lower separate roller is provided with lower scraping plate.
10. nappe flip length according to claim 2 and strap-clamping-type microwave distillation extract the method for Effective Component of Chinese Medicine, and it is characterized in that, described evaporator tube is connected with vacuum extractor.
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| CN108452542A (en) * | 2018-05-04 | 2018-08-28 | 美清科技（北京）有限公司 | Liquid vaporising unit and liquid evaporation technique |
| CN112246353A (en) * | 2020-09-27 | 2021-01-22 | 陈维元 | A mix grinder for pitch material production |
| CN113039001A (en) * | 2021-02-19 | 2021-06-25 | 安徽金禾实业股份有限公司 | Production equipment and production method of sucrose-6-ester |
| CN117282124A (en) * | 2023-11-16 | 2023-12-26 | 北京亚东生物制药有限公司 | 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108452542A (en) * | 2018-05-04 | 2018-08-28 | 美清科技（北京）有限公司 | Liquid vaporising unit and liquid evaporation technique |
| CN112246353A (en) * | 2020-09-27 | 2021-01-22 | 陈维元 | A mix grinder for pitch material production |
| 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 |
| CN113039001A (en) * | 2021-02-19 | 2021-06-25 | 安徽金禾实业股份有限公司 | Production equipment and production method of sucrose-6-ester |
| CN113039001B (en) * | 2021-02-19 | 2022-10-18 | 安徽金禾实业股份有限公司 | Production equipment and production method of sucrose-6-ester |
| CN117282124A (en) * | 2023-11-16 | 2023-12-26 | 北京亚东生物制药有限公司 | Plant raw juice extraction process and equipment based on infrared heating |
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