CN104083896B - A kind of ultrasonic Microwave Extraction technique that involves - Google Patents
A kind of ultrasonic Microwave Extraction technique that involves Download PDFInfo
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- CN104083896B CN104083896B CN201410277157.9A CN201410277157A CN104083896B CN 104083896 B CN104083896 B CN 104083896B CN 201410277157 A CN201410277157 A CN 201410277157A CN 104083896 B CN104083896 B CN 104083896B
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Abstract
The invention provides a kind of ultrasonic Microwave Extraction technique that involves, there is coordinated regulation device, collaborative adjusting device is first controlled microwave introduction device and is imported microwave, after certain hour, the first warning device sends alarm signal to coordinated regulation device, and coordinated regulation device control ultrasonic wave imports device and imports ultrasonic wave; After certain hour, Secondary Report alarm device sends alarm signal to coordinated regulation device, and coordinated regulation device control microwave introduction device and ultrasonic wave import device and successively change its operate power; The 3rd warning device imports device at microwave introduction device and ultrasonic wave and sends alarm signal to coordinated regulation device after with the operate power work certain hour after changing, coordinated regulation device is first controlled microwave introduction device and is quit work, and rear control ultrasonic wave imports device and quits work. Importing time, importing order, importing power and the shut-in time of this system to ultrasonic wave and microwave strictly controlled, thereby reaches the optimum Match effect of ultrasonic wave and microwave.
Description
Technical field
The present invention relates to a kind of ultrasonic Microwave Extraction technique that involves, belong to the abstraction technique neck of Chinese medicine useful componentTerritory.
Background technology
Active skull cap components in plant or Chinese medicine is in fields such as medicine, food, chemical industry, cosmetics, feedsIn have broad application prospects. The preparation of Chinese medical concrete, liquid extract or bioactivator in pharmaceuticals industryAnd in food, cosmetics, feed industry, the preparation of the functional additive of plant origin all needs to adopt and carriesTaking equipment; In chemical industry and chemical analysis field, the processes such as sample pre-treatments or sample preparation, chemical synthesisAlso may need to adopt clear up, extraction equipment or reactor.
It is emerging in recent years extractive technique that ultrasonic wave assisted extraction and Microwave-assisted Extraction are got. From dried materialExtract target compound and be roughly divided into two steps: the 1) infiltration of material, the i.e. expansion of material and aquation; 2)Solubility target compound is by diffusion, the mass transport process of infiltration from material to solvent. Research shows, ultrasonicRipple can make plant cell wall produce hole, is conducive to the stripping of target compound in cell, can promote to passMatter process. In addition, ultrasonic wave can also reduce raw meal particle size, thereby increases the contact area of material and solvent,Be conducive to the extraction of target compound. That ultrasonic wave assisted extraction has is easy to operate, with low cost, while extractingBetween short, be easy to amplify the advantage such as production. Conventional ultrosonic extractor comprises sonde-type extraction element at presentWith water-bath type extraction element. The former probe sphere of action is limited, is unfavorable for amplifying producing; The latter producesUltrasonic vibration can must just can be passed to sample by medium and sample bottle, this indirectly ul-trasonic irradiationMode may affect extraction efficiency.
Microwave can or be extracted material by intracellular polar water molecules and absorbs and produce amount of heat, makes thinIn born of the same parents, temperature rises rapidly, and the pressure that water vapor produces can break through cell membrane and cell membrane, forms largerMass transfer channel, thereby the extraction of promotion target compound. Microwave-assisted Extraction is got has short, solvent of extraction timeConsumption is few, extraction efficiency advantages of higher. Conventional Microwave Extraction device comprises sealed high pressure extraction tank at presentWith open atmospheric extraction device. The former intensity to extractor material and sealing requirements are very high, sample placeReason amount is little, and poor stability is expensive, and cool time that need to be longer. The latter often can not regulate and carryGet temperature, affected the optimization of extraction process, when excess Temperature, may cause some thermal instability targetedCompound degraded.
In recent years, in order to improve extraction efficiency, the patent documentation that ultrasonic wave and Microwave Extraction technology are combinedOf common occurrence, Chinese patent literature can make full use of void effect and both tools of microwave of ultrasonic vibrationThere is high energy effect, can overcome again some deficiency of conventional ultrasound and Microwave Extraction technology. Chinese patentCN2748147Y, CN1651896A.CN2773664Y.CN2822737Y, CN2880211Y discloses severalUltrasonic wave Microwave Extraction device, differs from one another.
But research shows, often there is following point in existing ultrasonic wave and Microwave Extraction device:
While utilizing existing above-mentioned ultrasonic wave Microwave Extraction device to extract, As time goes in sampleActivity substance content presents the trend that first low rear height then reduces again, especially in the middle and later periods of extracting, and inspectionThe amount of the bioactivator in the sample solution going out significantly reduces on the contrary, has greatly weakened ultrasonic wave and microwaveCollaborative work effect. In people's general idea, the importing time of ultrasonic wave and microwave, importing meritThe larger extraction effect of rate just should be better, but above-mentioned phenomenon and people's general idea consciousness is larger apart,In prior art, also do not find and produce the reason of above-mentioned phenomenon and the technological means addressing the above problem.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is to overcome the ultrasonic Microwave Extraction that involves of the prior artDevice causes the not good technological deficiency of synergy of ultrasonic wave and microwave, thus provide a kind of have higherCollaborative extraction effect, the ultrasonic wave Microwave Extraction technique that extraction efficiency is higher and energy loss is low.
Another technical problem that the present invention will solve is to overcome the ultrasonic microwave that involves of the prior art and carriesGet device and cause the not good technological deficiency of synergy of ultrasonic wave and microwave, thereby it is higher to provide one to haveCollaborative extraction effect, the ultrasonic wave Microwave Extraction system that extraction efficiency is higher and energy loss is low.
For this reason, the invention provides a kind of ultrasonic Microwave Extraction technique that involves, comprise the following steps of carrying out successively:
Step 1: open the upper cover of closed box, and be arranged in the sample solution device of described closed boxEntrance, is positioned over the solution of pre-configured sample to be extracted in described sample solution device, and closesDescribed entrance and described upper cover;
Step 2: open coordinated regulation device, described coordinated regulation device control microwave introduction device is opened, instituteState microwave introduction device and import continuous microwave in described sample solution device, described microwave introduction deviceInitial power is P1, and after certain hour t1, the first warning device of described coordinated regulation device is to described collaborativeRegulation device sends alarm signal, and described coordinated regulation device is controlled ultrasonic wave receiving after described alarm signalGatherer is opened, and imports ultrasonic wave in described sample solution device, described ultrasonic wave importing deviceInitial power is P2, the importing direction of described hyperacoustic importing direction and described microwave orthogonal vertical all the time,After certain hour t2, the Secondary Report alarm device of described coordinated regulation device is sent out to described coordinated regulation deviceGo out alarm signal, described coordinated regulation device is receiving that after described alarm signal, first controlling microwave introduction device subtractsSmall-power, after the certain hour of interval, controls described ultrasonic wave importing device and reduces power, makes both meritsRate is less than respectively its initial power P1, P2, described in the control of described coordinated regulation device ultrasonic wave import device andDescribed microwave introduction device is first controlled described microwave introduction device after with the Power operation certain hour t3 after reducingOut of service, it is out of service that the described ultrasonic wave of rear control imports device, and the sample solution in described step 1 isThe sample solution of Reishi sporule, time t1 is 2-6 minute, and time t2 is 4-5 minute, and time t3 is 0.5-1.0Minute.
The cavity that the described sample solution device adopting is cuboid, described microwave introduction device has the institute of being arranged onState the even number microwave entrance on sample solution device, even number microwave entrance is at the sample solution of described cavityCornerwise two ends in the space forming distribute in pairs with maximum distance.
The described microwave entrance adopting is the opening of rectangular shape or trapezoidal shape, is positioned at the same space diagonal angleTwo microwave entrances at line two ends, the minor face along continuous straight runs of one of them microwave entrance arranges, and another is micro-The minor face of ripple entrance vertically arranges, and the described microwave entrance that minor face vertically arranges is than minor face edgeThe seamed edge of the vertical direction of the more close described sample solution device of described microwave entrance that horizontal direction arranges; InstituteStating the length of microwave entrance and the ratio of width is 25/12-24/13.
Described microwave introduction device also comprises the introduction chamber of the trapezoid cross section being connected with described microwave entrance, described inThe osculum end of introduction chamber is connected with described microwave entrance, and both junctions arrange microwave and suppress lasso, described inThe big opening end of microwave introduction chamber is connected with magnetron, on the outer wall of described magnetron, cooler is set, described coldBut device comprises that socket is arranged on the mount pad of described anode of magnetron, arranges annular water flowing chamber on described mount padAnd the lug boss projecting upwards from described mount pad, described lug boss is divided into described annular water flowing chamberThe intake tunnel being connected with water inlet and the exhalant canal being connected with delivery port.
The described closed box inside adopting also comprises for making to extract first of halfway sample solution backflowReflux, described the first reflux comprise be inserted in below sample solution liquid level for having extractedThe liquor pump that sample solution bursts out, with the discharge nozzle that described liquor pump is connected, is arranged on going out of described discharge nozzleThe jet at mouth place, the corresponding feeder setting of described jet, the lower end of described feeder is by valve and sampleProduct solution device is communicated with or disconnects, and described jet is communicated with discharge nozzle by switch valve or disconnects, and also comprisesReturn duct, one end of described return duct is inserted in described sample solution device, the other end by check valve withDischarge nozzle is communicated with or disconnects.
The ultrasonic Microwave Extraction technique that involves provided by the invention, also comprises in the closed box of employing and is arranged on instituteState the whole liquid levels of sample solution device following and be communicated with described discharge nozzle by tube connector for molten to sampleThe disk-shaped tube that liquid stirs, arranges several bellmouths on described disk-shaped tube, the osculum end of described bellmouthTowards liquid level setting; One end that described tube connector is connected with described discharge nozzle is positioned at described sample solution deviceInner.
Also comprise and be arranged on the second backflow dress of described closed box inside for the sample solution of vaporization is refluxedPut, described the second reflux has the taper drainage hood that is inserted into described sample solution device inside, described inThe big opening end of taper drainage hood covers whole liquid level and is positioned at described liquid level the most close described sample solution dress aboveBe set up the position of end, the osculum end of described taper drainage hood connects condenser pipe, the outside socket of described condenser pipeThere is circulating water flow siphunculus, on described circulating water flow siphunculus, loop head and loop exit are set.
The cooling liquid outlet of cooling back installation is communicated with described loop head, described cooling liquid inlet and circulationOutlet is communicated with, and described cooling back installation comprises that laminating is arranged on stainless on described sample solution device outer wallSteel paster, and be vertically set on several deflectors that highly differ on described stainless steel paster, someIndividual described deflector forms corrugated fluid passage, along the height of the described deflector of fluid direction of advanceReduce gradually, the gap between adjacent baffle increases gradually, is positioned at the adjacent of fluid direction of advance forefrontGap between deflector is not more than between the adjacent baffle at the rear of fluid direction of advance gap0.5-0.8 doubly.
The ultrasonic Microwave Extraction system that involves provided by the invention, comprises the openable closed box of upper cover, arrangesIn the sample solution device with openable entrance of described closed box inside, be positioned at described sample solutionBetween device and described casing and the sidewall setting of the described sample solution device of fitting have cooling liquid inlet andThe cooling back installation of cooling liquid outlet, also comprises and is arranged on movably micro-on described sample solution deviceRipple gatherer, movably ultrasonic wave imports device and coordinated regulation device, described coordinated regulation deviceImport the position of device on described sample solution device by controlling described microwave introduction device and described ultrasonic wavePut described microwave introduction device is imported to microwave importing direction and described ultrasonic wave in sample solution deviceDevice is to the ultrasound waveguide Inbound orthogonal vertical all the time in described sample solution device, and, described collaborativeThe first warning device, Secondary Report alarm device and the 3rd warning device are set on regulation device, extract while beginning,Described in described collaborative adjusting device control, microwave introduction device imports microwave, after certain hour, and described the first reportAlarm device sends alarm signal to described coordinated regulation device, ultrasonic wave described in the control of described coordinated regulation deviceGatherer imports ultrasonic wave; After certain hour, described Secondary Report alarm device fills to described coordinated regulationPut and send alarm signal, after described coordinated regulation device is first controlled described microwave introduction device, ultrasonic wave imports dressPut and change respectively operate power, make operate power respectively lower than initial power separately; The described the 3rd reports to the police fillsPut at described microwave introduction device and described ultrasonic wave and import device with operate power work one timing after changingBetween backward described coordinated regulation device send alarm signal, described coordinated regulation device is first controlled described microwave and is ledEnter device and quit work, the described ultrasonic wave of rear control imports device and quits work.
The cavity that described sample solution device is cuboid, described microwave introduction device has and is arranged on described sampleEven number microwave entrance on product solution device, even number microwave entrance forms at the sample solution of described cavityCornerwise two ends in space distribute in pairs with maximum distance.
Described microwave entrance is the opening of rectangular shape or trapezoidal shape, is positioned at the same space diagonal two endsTwo microwave entrances, the minor face along continuous straight runs of one of them microwave entrance arranges, another microwave entranceMinor face vertically arrange, the described microwave entrance that minor face vertically arranges than minor face along level sideTo the seamed edge of vertical direction of the more close described sample solution device of described microwave entrance arranging; Described microwaveThe length of entrance and the ratio of width are 25/12-24/13.
Described microwave introduction device also comprises the introduction chamber of the trapezoid cross section being connected with described microwave entrance, described inThe osculum end of introduction chamber is connected with described microwave entrance, and both junctions arrange microwave and suppress lasso, described inThe big opening end of microwave introduction chamber is connected with magnetron, on the outer wall of described magnetron, cooler is set, described coldBut device comprises that socket is arranged on the mount pad of described anode of magnetron, arranges annular water flowing chamber on described mount padAnd the lug boss projecting upwards from described mount pad, described lug boss is divided into described annular water flowing chamberThe intake tunnel being connected with water inlet and the exhalant canal being connected with delivery port.
Technique scheme of the present invention has the following advantages compared to existing technology:
1. the ultrasonic Microwave Extraction technique that involves provided by the invention, by coordinated regulation device is set, to ultrasonicImporting time, importing order, importing power and the shut-in time of ripple and microwave are strictly controlled, first controlSystem imports microwave, and just starts to import ultrasonic wave after microwave imports certain hour, and this makes the heat of microwaveAmount can pass to sample solution better, thus guarantee microwave by sample solution be heated to certain hour andAfter degree, just carry out hyperacoustic importing, avoided importing in advance ultrasonic wave and sample causes when heatedThe waste of energy; After sample solution is heated to a certain degree, the heating of hyperacoustic cavitation and microwaveEffect is better merged, and hyperacoustic importing direction and microwave leads described in the control of coordinated regulation deviceInbound is vertical, makes ultrasonic wave carry out scissoring vibration to sample, for vibration shell-broken effect the best of sample,And ultrasonic wave is vertical with microwave, increase hyperacoustic scissoring vibration field intensity, expand hyperacoustic vibrationRegion, has the strong vibration of adding and makes the more uniform technique effect of vibration, thereby can improve extraction efficiency;Be adjustable because ultrasonic wave imports device and microwave introduction device, in the time that the height of sample solution is changed,Described ultrasonic wave be can adjust and device and the position of microwave introduction device on described sample solution device imported,Thereby the importing direction that makes described ultrasonic wave and microwave can remain vertical, makes the use of native systemScope is larger; In addition, due to the later stage in vibration, sample, probably all by broken wall treatment, is controlledThe power that ultrasonic wave imports device and microwave introduction device is less than initial power, can avoid from broken wallUnder the active material that in cell membrane, mass transfer goes out strong effect of vibration again, enter in damaged cell membrane, carryThe high extracted amount that extracts the later stage; And, extract the heat effect of later stage microwave for the effect of extracting notObviously, first out of service by coordinated regulation device control microwave introduction device, can further reduce energy consumption.
2. the ultrasonic Microwave Extraction technique that involves provided by the invention, the chamber that described sample solution device is cuboidBody, described microwave introduction device has the even number microwave entrance being arranged on described sample solution device, evenCornerwise two ends in the space that several microwave entrances form at the sample solution of described cavity become with maximum distanceTo distributing. Microwave entrance adopts the even number mode of design in pairs, and microwave entrance exists along sample solutionThe paired distribution in cornerwise two ends in the space forming in cavity, after this imports ultrasonic wave, from twoThe microwave that microwave entrance imports is crossing with ultrasonic wave respectively, and intersection point is positioned at conplane two opposite ends,After microwave is crossing with ultrasonic wave, hyperacoustic scissoring vibration effect is enhanced respectively at conplane two ends,And strengthen diffusion and mutually transmit along this plane, strengthened the vibration of ultrasonic wave in whole space brokenWall effect.
3. the ultrasonic Microwave Extraction technique that involves provided by the invention, described microwave entrance is rectangular shape or ladderThe opening of shape shape, is positioned at two microwave entrances at the same space diagonal two ends, one of them microwave entranceMinor face along continuous straight runs arrange, the minor face of another microwave entrance vertically arranges, minor face is along verticallyThe more close described sample of described microwave entrance that the described microwave entrance that direction arranges arranges than minor face along continuous straight runsThe seamed edge of the vertical direction of product solution device; The length of described microwave entrance and the ratio of width are25/12-24/13. The present invention adopts microwave incidence angle to become 0 degree angle with sample solution, makes microwave energy maximum limitDegree is absorbed by sample solution. Described in two, microwave entrance is pressed vertical and horizontal layout, and microwave energy is worn by waveguideAfter entering cavity, the component of the horizontal direction of leading wave field and the component of vertical direction form orthogonal in cavitySuperposition, has improved microwave field density, makes field strength distribution more even simultaneously, and sample solution is in high-strength completelyIn the radiation of degree microwave energy, improved the uniformity of heating using microwave and the intensity of heating using microwave, evidence is micro-This kind of particular design of ripple entrance, for the extraction with the same sample solution of amount, micro-in obvious reductionIn the situation of ripple heat time, the extraction efficiency of sample but obviously improves; Described sample solution device is rectangularThe cavity of body, this is farthest reflected microwave in this device, thereby makes the utilization of microwaveRate is greatly improved, and, between the microwave reflecting, can form the field intensity of orthogonal superposition, enter oneStep has increased heating using microwave efficiency.
4. the ultrasonic Microwave Extraction technique that involves provided by the invention, described microwave introduction device also comprises with describedThe introduction chamber of the trapezoid cross section that microwave entrance connects, described introduction chamber is waveguide cavity, the osculum of described introduction chamberEnd is connected with described microwave entrance, makes microwave in the time entering microwave entrance, obtain concentrating and strengthens, both companiesThe place of connecing arranges microwave and suppresses lasso, has prevented the leakage of microwave in junction, the large mouth of described microwave introduction chamberEnd is connected with magnetron, and magnetron is in generation when microwave, and the anode heat of magnetron constantly raises, byOn the outer wall of described magnetron, cooler is set, cooling for magnetron is carried out, can avoid magnetic control plumberThe time of doing is when larger, because heat is difficult to the burnout phenomenon that scatters and disappears and cause. Described cooler comprises socket peaceBe contained in the mount pad of described anode of magnetron, annular water flowing chamber be set and from described installation on described mount padThe lug boss projecting upwards on seat, described lug boss is divided into described annular water flowing chamber to be connected with water inletIntake tunnel and the exhalant canal being connected with delivery port, annular mount pad is directly socketed on described magnetron,Be convenient to install, and annular water flowing chamber is set on mount pad can makes magnetron obtain omnibearing heat radiation,More importantly, lug boss is set on mount pad, described lug boss by described annular water flowing chamber be divided intoThe intake tunnel that water inlet connects and the exhalant canal being connected with delivery port, this kind of design makes coolerStructure is very compact, and cooling effect is good.
5. the ultrasonic Microwave Extraction technique that involves provided by the invention, also comprises and is arranged on described closed box insideExtract for making the first reflux that halfway sample solution refluxes, described the first reflux comprises slottingEnter the liquor pump for the sample solution having extracted is burst out below sample solution liquid level, with described liquidThe discharge nozzle that pump connects, is arranged on the jet in the exit of described discharge nozzle, and described jet is corresponding to be collectedGroove arranges, and described jet is communicated with discharge nozzle by switch valve or disconnects, and also comprises return duct, described timeStream pipe one end be inserted in described sample solution device, the other end be communicated with discharge nozzle by check valve orDisconnect. After sample solution extracts, or in leaching process, need sample solution to pump and detectTime, open liquor pump 2 sample solution is pumped in described discharge nozzle, open switch valve, enter discharge nozzleIn a coating part enter jet, spray into feeder from described jet so that collect and detect,Now, because the pressure in described discharge nozzle is less, be less than the spring pressure of check valve, closed check valve,Sample solution can not be back in sample solution device by return duct, can carry out lasting pumping; TherewithMeanwhile, another part solution entering in described discharge nozzle enters in mixing component by tube connector, and from stirringThe bellmouth of mixing parts is spouting, and the solution of device bottom surface is dug, and has avoided viscosity largerSample solution is difficult to the problem of pumping. In the time not needing pumping, (for example sample solution detects rear discovery sample and carriesGet not thorough), switch valve cuts out, now, because liquor pump continues to pumping sample solution in discharge nozzle,Pressure in discharge nozzle constantly increases, in the time that the pressure in discharge nozzle is greater than the spring pressure of check valve, described inThe flap of check valve is opened, check valve is opened towards the inside of sample solution device, is positioned at discharge nozzleSample solution enters in return duct along check valve, is back to sample solution device from described return duct,Make sample solution carry out inner loop, prevent that the sample solution that viscosity is larger from producing the problem precipitating, auxiliaryHyperacoustic vibrating effect. After retrieval, find that sample extraction is thoroughly time, open the valve below feeder,Feeder is communicated with sample solution device, described sample is imported in described sample solution device again,Extract further, and described feeder can be used as the entrance of sample solution simultaneously. Of the present inventionAbove-mentioned design, by the pan feeding of sample solution, pumping, detection, again import and prevent the effect knot of precipitationBe integrated, while having avoided bottle that available technology adopting is general as sample solution device, pan feeding,Discharging and all need the sample bottle to take out from closed box while detecting and just can reduce operating efficiencyTechnological deficiency, and be particularly useful for the extraction of the sample solution that viscosity is larger, meanwhile, for the experimental stageThe extraction of sample solution, because researcher is immature for the research of experiment condition, usually can go outNow extract halfway situation, the defect of sample bottle has been avoided taking out frequently, has been packed in this kind of design, passes throughPumping can be understood the extraction situation of sample, has reduced working strength.
6. the ultrasonic Microwave Extraction technique that involves of Chinese medicine provided by the invention, also wraps in the closed box of employingDraw together and be arranged on the use that the whole liquid levels of described sample solution device are following and be communicated with described discharge nozzle by tube connectorIn the disk-shaped tube that sample solution is stirred, several bellmouths are set, described taper on described disk-shaped tubeHole is bellmouth, and the osculum end of described bellmouth is towards liquid level setting; Described tube connector and described discharge nozzle connectThe one end connecing is positioned at the inside of described sample solution device. Described liquor pump in needs pumping outward,Play the effect of pumping sample solution outward, in not needing outward pumping sample solution, by arrangingBellmouth on disk-shaped tube sprays the liquid level to sample solution device, thereby in described sample solution deviceSample solution produce and agitate, played the effect of stirring, effectively prevented precipitation, due to described liquidPump one pump is dual-purpose, just can stir by self circulation of sample solution, does not need to introduce shaft,Just can play good anti-precipitation. The osculum end of described bellmouth is towards liquid level setting. Bellmouth arrangesFor bellmouth and osculum end are towards liquid level setting, can make sample solution enter liquid level in the mode of jet,Strengthen stirring action, thereby improved sludge proof effect. The mixing component that dish type arranges increases stirring area,Further strengthen anti-sedimentation effect.
7. the ultrasonic Microwave Extraction technique that involves provided by the invention, also comprises for making in the closed box of employingThe second reflux that the sample solution of vaporization refluxes, described the second reflux has and is inserted into described sampleThe taper drainage hood of solution device inside, the big opening end of described taper drainage hood covers whole liquid level and is positioned at instituteThe position of stating liquid level the most close above described sample solution device upper end, the large end face of taper drainage hood covers wholeIndividual liquid level, and be positioned at the described liquid level position of the most close described sample solution device upper end above, make micro-The all gas producing in ripple heating process can enter in described taper drainage hood, in taper drainage hoodUnder the effect of wall, be condensed into liquid, and be back in sample solution along taper drainage hood; Described taper drainageThe osculum end of cover connects condenser pipe, and the outer cover of described condenser pipe is connected to circulating water flow siphunculus, draws by taperThe portion gas that the inwall of stream cover cannot carry out condensation, enters in condenser pipe by a bite end of taper drainage hood,The circulating water flow siphunculus of cooling effect by to(for) condenser pipe, this portion gas is condensed in condenser pipe, returnsFlow in sample solution.
8. the ultrasonic Microwave Extraction technique that involves provided by the invention, the cooling liquid outlet of cooling back installation and instituteState loop head be communicated with, described cooling liquid inlet is communicated with loop exit, for reflux cooling liquid withBe interconnected for the outer wall of sample solution device is carried out to cooling cooling back installation, thereby make thisThe cold of bright above-mentioned two cooling systems is reused, and has reduced energy consumption, and, dwindle this and beThe quantity of the extraneous chilled water system of system, makes structure compacter; And for the ease of rear circulating cooling liquid pairIn front circulating cooling pressurization but, described in several, deflector forms corrugated fluid passage, edgeThe height of the described deflector of fluid direction of advance reduces gradually, and the gap between adjacent baffle increases graduallyGreatly, the gap between the adjacent baffle of fluid direction of advance forefront is not more than and is positioned at the fluid side of advancingTo the 0.5-0.8 in gap between the adjacent baffle at rear doubly.
Brief description of the drawings
For content of the present invention is more likely to be clearly understood, below according to a particular embodiment of the inventionAnd by reference to the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 is the ultrasonic structural representation that involves Microwave Extraction system that embodiments of the invention 1 provide;
Fig. 2 is the coordinated regulation device of the extraction system that provides of embodiments of the invention 1 and the electricity of whole systemLearn connection diagram;
Fig. 3 is that the microwave entrance of the extraction system that provides of embodiments of the invention 2 is on sample solution deviceThe structural representation of set-up mode;
Fig. 4 is the structural representation of the cooler of the magnetron of the extraction system that provides of embodiments of the invention 3;
Fig. 5 is the first reflux and the sample solution device of the extraction system that provides of embodiments of the invention 4Scheme of installation;
Fig. 6 is the structural representation of the disk-shaped tube that provides of embodiments of the invention 4;
Fig. 7 is the structural representation of the cooling back installation of the extraction system that provides of embodiments of the invention 5.
In figure, Reference numeral is expressed as: 1-closed box, 2-sample solution device; 20-feeder; 21-liquidBody pump; 22-discharge nozzle; 23-jet; 24-switch valve; 25-return duct; 26-check valve; 27-connectsPipe; 28-disk-shaped tube; 29-bellmouth; 3-cooling-cycle device; 31-cooling liquid inlet; 32-cooling fluid goes outMouthful; 33-deflector; 5-microwave introduction device; 51-microwave entrance; 52-introduction chamber; 53-magnetron; 54-Cooler; 54a-mount pad; 54b-annular water flowing chamber; 54c-lug boss; 54d-water inlet; 54e-water outletMouthful; 54f-outer shroud; 54k-notch; The 54h-gap of circulating; 6-ultrasonic wave imports device; 7-coordinated regulation dressPut; 70-PLC; 71-the first warning device; 72-Secondary Report alarm device; 73-the 3rd warning device; 81-coneShape drainage hood; 82-condenser pipe; 83-circulating water flow siphunculus; 84-loop head; 85-loop exit; 10-Motor.
Detailed description of the invention
Embodiment 1
As shown in Figure 1, embodiment provides a kind of ultrasonic wave for Chinese medicine or active substance of plant extractionAnd Microwave Extraction system, comprise the openable closed box 1 of upper cover, be arranged at described closed box 1 insideThere is the sample solution device 2 of openable entrance, be positioned at described sample solution device 2 and described casing 1 itBetween and the sidewall setting of the described sample solution device 2 of fitting there is cooling liquid inlet 31 and cooling liquid outlet 32Cooling back installation 3, also comprise that the movably microwave that is arranged on described sample solution device 2 imports dressPut 5, movably ultrasonic wave imports device 6 and coordinated regulation device 7, and described coordinated regulation device 7 wrapsDraw together PLC controller 70 and can import device with PLC controller 70, microwave introduction device 5 and ultrasonic waveThe first warning device 71 of 6 feedback operation, Secondary Report alarm device 72, the 3rd warning device 73, at this, instituteStating the first warning device 71, Secondary Report alarm device 72 and the 3rd warning device 73 is those skilled in the artThe signalling means with time counting function generally adopting.
In the present embodiment, described microwave introduction device 5 comprise produce the magnetron 53 of microwave, for conductionThe introduction chamber 52 of the microwave that described magnetron 53 produces, described introduction chamber 52 is trapezoid cross section, wherein large mouthfulEnd is connected with magnetron 53, and osculum end is connected to microwave entrance 51, described in described microwave entrance 51 is arranged onIn the upright side walls of sample solution device 2, this microwave entrance 51 is oblong openings, and this oblong openings makesThe importing direction and the liquid level that obtain microwave are zero degree angle, make sample solution farthest heated. DescribedUltrasonic wave importing device 6 is positioned at the bottom of described sample solution device 2, hyperacoustic importing direction and microwaveImporting direction substantially vertical, thereby microwave heating action is produced for hyperacoustic shearing shell-broken effectHuge forward impact, has improved the destruction efficiency of ultrasonic wave for sample cell wall greatly.
Preferred as one, the importing direction of described ultrasonic wave and described microwave is orthogonal vertical, now, micro-Ripple heat effect not only can aggravate hyperacoustic shearing shell-broken effect, and, can produce larger stackBroken wall field intensity, is convenient to promote evenly carrying out of broken wall.
Import device 6 at described sample solution device 2 in order to control described microwave introduction device 5 and ultrasonic waveOn importing position, the same side of described sample solution device 2 arranges several microwave entrances 51, meanwhile,This sidewall is connected with described microwave introduction device 5 by baffle plate (not shown) movably, at needsWhile importing microwave to a certain microwave entrance 51, mobile described baffle plate makes described baffle plate not block this microwave entrance 51,In the time that needs change the entrance that imports microwave, mobile this baffle plate, makes baffle plate not need to import entering of microwaveMouth blocks, and so can realize the adjustment of baffle plate for microwave entrance 51, in the present embodiment, and described baffle plateThe screw that moves through realize electrodeless adjusting. In the present embodiment, in order to realize, described ultrasonic wave is imported to dressPut the control of 6 importing position, import device 6 at the described ultrasonic wave of installation of described sample solution device 2Sidewall on guide-track groove (not shown) is set, described ultrasonic wave imports on device 6 and is provided with described and leadsThe sidewall that rail groove matches, embeds described guide-track groove by described sidewall, can realize described ultrasonic by slidingThe movement of ripple gatherer 6 on described sample solution device 2, thus change ultrasonic wave imports device 6Ultrasonic vibration orientation.
In the present embodiment, in order to realize the Collaborative Control to ultrasound waveguide Inbound and microwave importing direction,Described ultrasonic wave imports and displacement transducer is set respectively (in figure not on device 5 and described microwave introduction device 6Illustrate), described displacement transducer is connected with the PLC controller 70 of described coordinated regulation device 7, Neng GouxiangDescribed PLC controller 70 transmits displacement signal and moves in the time receiving the action order of PLC controller 70Predefined position.
In the present embodiment, the meaning of described cooling back installation setting is: after system works long hours, produceRaw a large amount of heat, heat cannot shed service life of the system that affects, by described sample solution device 2With in the gap of described closed box 1, cooling back installation 3 is set, not only can will in system works, produceAmount of heat scatters and disappears, and cooling back installation 3 is arranged on and can makes system compacter between the two, workWhile work, import cooling fluid from cooling liquid inlet 31, cooling fluid makes the heat quilt of system for the conduction of coldCooling fluid is taken away, finally discharges from cooling liquid outlet 32, thus the system of making (especially sample solution device2) heat is dispersed, and improves the service life of system.
The above-mentioned ultrasonic Microwave Extraction system that involves of utilizing that the present embodiment provides is carried out the active material of sample and is extractedTime comprise following processing step:
Step 1: open the described upper cover of closed box 1, and the described entrance of sample solution device 2, willThe solution of pre-configured sample to be extracted is positioned in described sample solution device 2, and enters described in closingMouth and described upper cover;
Step 2: open described coordinated regulation device 7, as shown in Figure 2, the PLC of described coordinated regulation device 7Controller 70 is first to described microwave introduction device 5 and the first warning device 71 transmitted signals, described microwaveGatherer 5 is started working with initial power P1 immediately receiving after described signal, meanwhile, and described the first reportAlarm device 71 starts to carry out time counting receiving after described signal, after elapsed time t1, and described the first reportAlarm device 71 sends alarm signal to described PLC controller, and described PLC controller 70 is being received described reportAfter alert signal, import device 6 to described ultrasonic wave and send working signal, and simultaneously to described Secondary Report alarm device72 send working signal, and described ultrasonic wave imports device 71 and receiving after described working signal immediately with initial powerRate P2 starts working, and described Secondary Report alarm device 72 starts to carry out time counting receiving after working signal,After elapsed time t2, described Secondary Report alarm device 72 is to described PLC controller 70 transmitted signals, described PLCController is being received after described signal simultaneously to described microwave introduction device 5 and described ultrasonic wave importing device 6Send the signal that changes operating power, and send working signal to the 3rd warning device 73, described microwave importsDevice 5 and described ultrasonic wave import device 6 receiving that after this signal, priority changes its operating power, make workThe rate of doing work is less than respectively its initial power P1, P2, and described the 3rd warning device 73 is being received after this working signalStart to carry out time counting, after elapsed time t3, described the 3rd warning device 73 is to described PLC controller70 transmitted signals, described PLC controller 70 is first controlled described microwave introduction device receiving after described signal5 quit work, and the described ultrasonic wave of rear control imports device 6 and quits work.
The said extracted system of the present embodiment, has been realized described microwave has been imported to dress by coordinated regulation device 7Put 5 and described ultrasonic wave import device 6 job order, working time, operating power and stop suitableThe Comprehensive Control of order. First control and import microwave, and after microwave imports certain hour, just start to import ultrasonicRipple, this makes the heat of microwave can pass to better sample solution, thereby guarantees at microwave sample is moltenLiquid is heated to after certain hour and degree, just carries out hyperacoustic importing, avoided importing in advance ultrasonic wave andSample causes the waste of energy when not heated; After sample solution is heated to a certain degree, hyperacoustic skyThe heat effect of cavitation and microwave better merges, and coordinated regulation device 7 is controlled described ultrasonic waveImporting direction and the importing direction of microwave vertical, make ultrasonic wave carry out scissoring vibration to sample, for sampleVibration shell-broken effect the best of product, and ultrasonic wave is vertical with microwave, has increased hyperacoustic scissoring vibration fieldBy force, expand hyperacoustic vibration area, there is the strong vibration of adding and make the more uniform technique effect of vibration,Thereby can improve extraction efficiency; Be adjustable because ultrasonic wave imports device 6 and microwave introduction device 6,In the time that the height of sample solution is changed, can adjusts described ultrasonic wave and import device 6 microwave introduction devices 5Position on described sample solution device 2, thus the importing direction of described ultrasonic wave and microwave can be begunKeep eventually vertical, make the scope of application of native system larger; In addition, due to the later stage in vibration, sample veryMay be all by broken wall treatment, at the beginning of the power of control ultrasonic wave importing device and microwave introduction device is less thanBeginning power, can avoid active material that mass transfer has gone out from the cell membrane of broken wall in strong shaking againAction enters in damaged cell membrane under using, and improves the extracted amount that extracts the later stage; And, extract later stage microwaveHeat effect for extract effect not obvious, by coordinated regulation device control microwave introduction deviceFirst out of service, can further reduce energy consumption.
It should be noted that, utilize the said extracted system that the present embodiment provides to carry out carrying of bioactivatorWhile getting, the operate power after described time t1, t2, t3, initial power P1, P2 and change can basisThe different material extracting changes, and above-mentioned numerical value is in the time that extraction work starts, according to the different material extractingPre-set. In the present embodiment, said extracted system is used for the extraction to Reishi sporule, wherein, timeBetween t1 be 2-6 minute, time t2 is 4-5 minute, time t3 is 0.5-1.0 minute, has greatly improvedExtraction efficiency, initial power P1 is 50-200W, initial power P2 is 50-100W, greatly reduces energy consumption.
Embodiment 2
The present embodiment provides a kind of ultrasonic Microwave Extraction system that involves, and it is the change on embodiment 1 basisShape, as shown in Figure 3, the extraction system that the present embodiment provides is with respect to the improvement of embodiment 1: described inThe cavity that sample solution device 2 is cuboid, described microwave introduction device 5 has that to be arranged on described sample moltenEven number microwave entrance 51 on liquid device 2, even number microwave entrance 51 is the sample solution shape of described cavityCornerwise two ends in the space becoming distribute in pairs with maximum distance. The ultrasonic microwave that involves that the present embodiment providesExtraction system, the cavity that described sample solution device 2 is cuboid, described microwave introduction device 5 has to be establishedPut on described sample solution device 51, two described microwave entrances 51 of two microwave entrances at described cavityCornerwise two ends in the space that sample solution forms distribute in pairs with maximum distance. Microwave entrance 51 is along sampleThe paired distribution in cornerwise two ends in the space that product solution forms in cavity, after this imports ultrasonic wave,The microwave importing from two microwave entrances 51 is crossing with ultrasonic wave respectively, and intersection point is positioned at conplane twoIndividual opposite end, after microwave is crossing with ultrasonic wave, hyperacoustic scissoring vibration effect at conplane two ends respectivelyBe enhanced, and strengthen diffusion mutually transmit along this plane, strengthened ultrasonic wave in whole spaceInterior vibration shell-broken effect.
As the one distortion of the present embodiment, described microwave entrance 51 can also be set to other numbers, for example4,6,8 etc. even number numbers, the space that even number microwave entrance 51 forms along sample solutionCornerwise two ends distribute in pairs with maximum distance.
Improve as one, in the present embodiment, the opening that described microwave entrance 51 is rectangular shape, positionIn two microwave entrances 51 at the same space diagonal two ends, the minor face of one of them microwave entrance 51 is along levelDirection arranges, and the minor face of another microwave entrance 51 vertically arranges, and minor face vertically arrangesThe more close described sample of described microwave entrance 51 that described microwave entrance 51 arranges than minor face along continuous straight runs is moltenThe seamed edge of the vertical direction of liquid device 2; The length of described microwave entrance 51 and the ratio of width are25/12-24/13. Particularly, minor face vertically arranges described microwave entrance 51 is near being close toDistance between the vertical edges of the vertical seamed edge that described microwave resonance is strong and this vertical seamed edge is 75 millimeters, and shortThe described microwave entrance 51 of edge horizontal direction setting is near the strong vertical seamed edge of described microwave resonance being close toVertical edges and this vertical seamed edge between distance be 90 millimeters. The length of described microwave entrance 51 is 250Millimeter, width is 130 millimeters, the inside of described cavity has sample solution, the liquid level of described sample solutionWith the distance of the upper wall of described cavity be 120 millimeters.
The above-mentioned ultrasonic Microwave Extraction system that involves that the present embodiment provides, microwave incidence angle becomes 0 with sample solutionDegree angle, is absorbed microwave energy to greatest extent by sample solution. Described in two, microwave entrance 51 is pressed vertical and horizontalArrange, after making microwave energy penetrate cavity by waveguide, the component of the horizontal direction of leading wave field is with vertically squareTo component in cavity, form orthogonal superposition, improved microwave field density, make field strength distribution more equal simultaneouslyEven, sample solution is in the radiation of high-intensity microwave energy completely, has improved the uniformity of heating using microwave and micro-The intensity of ripple heating, this kind of particular design of evidence microwave entrance, for the same sample solution of same amountExtraction, in the situation that obviously reducing microwave heating time, the extraction efficiency of sample but obviously improves;The cavity that described sample solution device is cuboid, it is farthest anti-that this obtains microwave in this devicePenetrate, thereby the utilization rate of microwave is greatly improved, and, can shape between the microwave reflectingBe orthogonal stack field intensity, further increased heating using microwave efficiency.
As the one distortion of the present embodiment, described microwave entrance 51 can also be the opening of trapezoidal shape.
Embodiment 3
The present embodiment provides a kind of ultrasonic Microwave Extraction system that involves, and it is on embodiment 1 or 2 basesDistortion, in the present embodiment, as shown in Figure 4, described microwave introduction device 5 comprises magnetron 53, encouragesMagnetic system, reponse system (not shown) and cooler 54. Magnetron 53 output frequencies are 2450MHz,Output mean power 6kW, peak power output 10kw. Excitation system has two groups, and one group is that magnetron carriesElectromagnetism iron wire bag, another group be by enamel-covered wire around the electromagnetism iron wire bag that is enclosed within magnetron outside coil, thisTwo parts have special field power supply, and the electromagnetic electric current in electromagnetism iron wire bag is 8.0A left and right, and outer ledger lineIn circle, the large I of electric current is adjusted by coordinated regulation device 7. Reponse system has two parts, and a part is by sunElectrode current is input in one section of coil in magnet exciting coil and feeds back, a sampling of another part designResistance is connected in anode of magnetron loop, and anode current information is provided. Described cooler 54 comprises socket installationOn mount pad 54a described in the mount pad 54a of described magnetron 53 anodes, arrange annular water flowing chamber 54b andThe lug boss 54c projecting upwards from described mount pad 54a, described lug boss 54c is by described annular water flowing chamber54b is divided into the intake tunnel being connected with water inlet 54d and the exhalant canal being connected with delivery port 54e. ColdBut the concrete size of device 54 is pressed the size of magnetron 53 and is determined.
In the present embodiment, the integral piece that described cooler 54 is employing extrusion modling, thus make described coldBut device 54 sealings are best. On the outer wall of described annular water flowing chamber 54b, outer shroud 54f is set, described outer shroud 54fBe used for installing refrigerating gas, for the liquid of annular water flowing chamber 54b is dispelled the heat.
Lug boss 54c is as the watershed of annular water flowing chamber 54b in the present embodiment, in order to turnover currentShunting, makes annular water flowing chamber 54b become circulation runner. Lug boss 54c corresponding with annular water flowing chamber 54b go outForm circulation gap 54h, its effect is to make whole circumference in annular water flowing chamber 54b have water to flow through to deriveHeat, makes magnetron 53 anode perisporium heat radiations evenly. The endoporus of cooler 54 and the external diameter of anode of magnetronInterference fit. In the present embodiment, U-lag mouth is set on the lateral margin of described mount pad 54a, its effect isWhile installation for cooler, beat groove in order to fixing spiral shell for subsequent use, make it that rear magnetron is installed and be fixed in framework.
Embodiment 4
The present embodiment provides a kind of ultrasonic Microwave Extraction system that involves, and it is on embodiment 1 or 2 or 3 basesOn distortion, in the present embodiment, as shown in Figure 5, described extraction system also comprises and is arranged on described envelopeClose casing 1 inside for making to extract the first reflux that halfway sample solution refluxes, described first timeStream device comprises the liquor pump for the sample solution having extracted is burst out being inserted in below sample solution liquid level21, for driving the motor 10 of liquor pump 21, the discharge nozzle 22 with described liquor pump 21 is connected, is arranged onThe jet 23 in the exit of described discharge nozzle 22, the corresponding feeder 20 of described jet 23 arranges, described inThe lower end of feeder 20 is communicated with or disconnects with sample solution device 2 by valve, and described jet 23 passes throughSwitch valve 24 is communicated with or disconnects with discharge nozzle 22, also comprises return duct 25, and insert one end of described return duct 25Enter in described sample solution device 2, the other end is communicated with or disconnects with discharge nozzle 22 by check valve 26.Also comprise and be arranged on following tube connector 27 and the described discharge nozzle of also passing through of the whole liquid levels of described sample solution device 222 disk-shaped tubes 28 for sample solution is stirred that are communicated with, arrange several on described disk-shaped tube 28Bellmouth 29, described bellmouth 29 is bellmouth, the osculum end of described bellmouth is towards liquid level setting; DescribedOne end that tube connector 27 is connected with described discharge nozzle 22 is positioned at the inside of described sample solution device 2.
It should be noted that the check valve 26 in the present embodiment is check valves of a kind of spring, it is basicOperation principle is, in the time that switch valve 24 is opened, the pressure of spring is greater than the pressure in described discharge nozzle 22,The flap of check valve 26 is closed, and the sample solution in discharge nozzle 22 can not enter in described return duct 25, thisTime, carry out the normal pumping of sample solution; In the time not needing pumping sample solution, switch valve 24 cuts out, and goes outPressure in material pipe 22 increases gradually, in the time that the pressure in discharge nozzle 22 is greater than spring pressure, by check valve26 flap backs down, thereby check valve is opened towards the inside of described sample solution device 2, now,The liquid of discharge nozzle 22 enters in described return duct 25 along check valve 26, and is back to described sample solutionIn device 2.
It should be noted that, it arranges the check valve of mentioning in the present embodiment object and is mainly release, and energyEnough in the time that described switch valve 24 cuts out, open, make the sample in discharge nozzle 22 enter in return duct 25 and returnFlow in sample solution device 2; And in the time that described switch valve 24 is opened, described check valve 26 is closed, go outSample solution in material pipe 22 is injected into feeder 20 from described jet 23, sample in feeder 20Product solution is collected or is detected, if find after detection, sample solution does not extract completely, opens collectionValve between groove 20 and sample solution device 2, comes back in sample solution device sample solution.For realizing this main purpose, specifically arranging of described check valve can be various, except this realityExecute outside the spring check valve that example mentions, and can be set to gravity-held check valve, swing type check valve etc.
The above-mentioned design of the present embodiment, by the pan feeding of sample solution, pumping, detection, again import and anti-Only the effect of precipitation is combined as a whole, and has avoided the bottle that available technology adopting is general to fill as sample solutionWhile putting, in the time of pan feeding, discharging and detection, all need sample bottle to take out just and can fall from closed boxThe low technological deficiency of operating efficiency, and be particularly useful for the extraction of the sample solution that viscosity is larger, meanwhile,For the extraction of the sample solution of experimental stage, because researcher does not become for the research of experiment conditionRipe, usually there will be and extract halfway situation, this kind of design avoided taking out frequently, packing into sample bottleDefect, can understand the extraction situation of sample by pumping, reduced working strength.
Embodiment 5
The present embodiment provides a kind of ultrasonic Microwave Extraction system that involves, and it is at embodiment 1 or 2 or 3 or 4Distortion on basis, in the present embodiment, the cooling liquid outlet of described cooling back installation 3 32 with described inLoop head 84 is communicated with, and described cooling liquid inlet 31 is communicated with loop exit 85, described cooling back installation3 comprise that laminating is arranged on the stainless steel paster on described sample solution device 2 outer walls, and are vertically set on instituteState several deflectors 33 on stainless steel paster, described in several, to form corrugated fluid logical for deflector 33Road, as shown in Figure 7, along fluid direction of advance, the gap between adjacent baffle 33 increases gradually, positionGap between the adjacent baffle 33 of fluid direction of advance forefront is not more than and is positioned at fluid direction of advanceBetween the adjacent baffle 23 at rear, the 0.5-0.8 in gap doubly.
As further improvement of this embodiment, the height of several deflectors 33 can be set to highly differ,And the height that is positioned at the described deflector 33 of the same side reduces gradually along the flow direction of fluid.
Embodiment 6
The present embodiment provides a kind of ultrasonic Microwave Extraction system that involves, and it is at embodiment 1 or 2 or 3 or 4Or 5 further improvement on basis, in the present embodiment, as shown in Figure 1, described in also comprising and being arranged onInner the second reflux for the sample solution of vaporization is refluxed of closed box 1, described the second backflow dressPut and there is the taper drainage hood 81 that is inserted into described sample solution device inside, described taper drainage hood 81 largeMouth end covers whole liquid level and is positioned at the position of described liquid level the most close above described sample solution device 2 upper ends,The osculum end of described taper drainage hood 81 connects condenser pipe 82, and the outer cover of described condenser pipe 82 is connected to circulationCurrent siphunculus 83, arranges loop head 84 and loop exit 85 on described circulating water flow siphunculus 83.
Obviously, above-described embodiment is only for example is clearly described, and not to embodimentLimit. For those of ordinary skill in the field, can also make on the basis of the above description itThe variation that it is multi-form or variation. Here without also giving exhaustive to all embodiments. And byThe apparent variation that this extends out or variation are still among the protection domain in the invention.
Claims (5)
1. the ultrasonic Microwave Extraction technique that involves, comprises the following steps of carrying out successively:
Step 1: the upper cover of opening closed box (1), and be arranged in the entrance of the sample solution device (2) of described closed box (1), the solution of pre-configured sample to be extracted is positioned in described sample solution device (2), and closes described entrance and described upper cover;
Step 2: open coordinated regulation device (7), described coordinated regulation device (7) is controlled microwave introduction device (5) and is opened, described microwave introduction device (5) also imports continuous microwave in described sample solution device (2), the initial power of described microwave introduction device (5) is P1, after certain hour t1, the first warning device of described coordinated regulation device (7) sends alarm signal to described coordinated regulation device (7), described coordinated regulation device (7) is receiving that after described alarm signal, controlling ultrasonic wave imports device (6) unlatching, and import ultrasonic wave in described sample solution device (2), the initial power that described ultrasonic wave imports device (6) is P2, the importing direction of described hyperacoustic importing direction and described microwave orthogonal vertical all the time, after certain hour t2, the Secondary Report alarm device of described coordinated regulation device (7) sends alarm signal to described coordinated regulation device (7), described coordinated regulation device (7) is receiving that after described alarm signal, first controlling microwave introduction device (5) reduces power, after the certain hour of interval, control described ultrasonic wave importing device (6) and reduce power, make both power be less than respectively its initial power P1, P2, described coordinated regulation device (7) is controlled described ultrasonic wave and is imported device (6) and described microwave introduction device (5) first to control described microwave introduction device (5) after with the Power operation certain hour t3 after reducing out of service, it is out of service that the described ultrasonic wave of rear control imports device (6),
Sample solution in described step 1 is the sample solution of Reishi sporule, and time t1 is 2-6 minute, and time t2 is 4-5 minute, and time t3 is 0.5-1.0 minute.
2. the ultrasonic Microwave Extraction technique that involves according to claim 1, it is characterized in that: the cavity that the described sample solution device (2) of employing is cuboid, described microwave introduction device (5) has the even number microwave entrance (51) being arranged on described sample solution device (2), and cornerwise two ends in the space that even number microwave entrance (51) forms at the sample solution of described cavity distribute in pairs with maximum distance.
3. the ultrasonic Microwave Extraction technique that involves according to claim 2, it is characterized in that: the described microwave entrance (51) of employing is the opening of rectangular shape or trapezoidal shape, be positioned at two microwave entrances (51) at the same space diagonal two ends, the minor face along continuous straight runs of one of them microwave entrance (51) arranges, the minor face of another microwave entrance (51) vertically arranges, the seamed edge of the vertical direction of the more close described sample solution device of described microwave entrance (51) (2) that the described microwave entrance (51) that minor face vertically arranges arranges than minor face along continuous straight runs, the length of described microwave entrance (51) and the ratio of width are 25/12-24/13.
4. the ultrasonic Microwave Extraction technique that involves according to claim 3, it is characterized in that: described microwave introduction device (5) also comprises the introduction chamber (52) of the trapezoid cross section being connected with described microwave entrance (51), the osculum end of described introduction chamber (52) is connected with described microwave entrance (51), both junctions arrange microwave and suppress lasso, the big opening end of described introduction chamber (52) is connected with magnetron (53), cooler (54) is set on the outer wall of described magnetron (53), described cooler (54) comprises that socket is arranged on the mount pad (54a) of described magnetron (53) anode, the lug boss (54c) that annular water flowing chamber (54b) is set on described mount pad (54a) and projects upwards from described mount pad (54a), described annular water flowing chamber (54b) is divided into the intake tunnel being connected with water inlet (54d) and the exhalant canal being connected with delivery port (54e) by described lug boss (54c).
5. the ultrasonic Microwave Extraction technique that involves according to claim 4, it is characterized in that: inner also the comprising for making to extract the first reflux that halfway sample solution refluxes of described closed box (1) of employing, described the first reflux comprises the liquor pump (21) for the sample solution having extracted is burst out being inserted in below sample solution liquid level, the discharge nozzle (22) being connected with described liquor pump (21), be arranged on the jet (23) in the exit of described discharge nozzle (22), the corresponding feeder of described jet (23) (20) arranges, the lower end of described feeder (20) is communicated with or disconnects with sample solution device (2) by valve, described jet (23) is communicated with or disconnects with discharge nozzle (22) by switch valve (24), also comprise return duct (25), one end of described return duct (25) is inserted in described sample solution device (2), the other end is communicated with or disconnects with discharge nozzle (22) by check valve (26).
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