CN104083895A - Improved ultrasonic wave and microwave extraction system - Google Patents
Improved ultrasonic wave and microwave extraction system Download PDFInfo
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- CN104083895A CN104083895A CN201410277156.4A CN201410277156A CN104083895A CN 104083895 A CN104083895 A CN 104083895A CN 201410277156 A CN201410277156 A CN 201410277156A CN 104083895 A CN104083895 A CN 104083895A
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Abstract
The invention provides an improved ultrasonic wave and microwave extraction system. A sample solution apparatus is a cuboid cavity; a microwave introducing apparatus has an even number of microwave inlets arranged on the cavity, and the even number of microwave inlets are located at two ends of a diagonal of the space of the cavity and pairedly distributed according to farthest distance. According to the invention, since an even number of the microwave inlets are pairedly designed and the microwave inlets are pairedly distributed along two ends of the diagonal of the space formed by a sample solution in the cavity, microwaves introduced from two microwave inlets respectively intersect with ultrasonic waves when the ultrasonic waves are introduced and intersection points are located at two opposite ends of a same plane; after intersection of the microwaves and the ultrasonic waves, shear vibration effects of the ultrasonic waves are respectively enhanced at two ends of the same plane, and enhanced diffusion effects mutually transfer along the plane, which improves the vibration and wall breaking effects of the ultrasonic waves in the whole space.
Description
Technical field
The present invention relates to a kind of improved ultrasonic Microwave Extraction system that involves, belong to the abstraction technique field of Chinese medicine useful component.
Background technology
Active skull cap components in plant or Chinese medicine has broad application prospects in the fields such as medicine, food, chemical industry, cosmetics, feed.In pharmaceuticals industry, in the preparation of Chinese medical concrete, liquid extract or bioactivator and food, cosmetics, feed industry, the preparation of the functional additive of plant origin all needs to adopt extraction equipment; In chemical industry and chemical analysis field, the processes such as sample pre-treatments or sample preparation, chemical synthesis also 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 material, extract 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, ultrasonic wave can make plant cell wall produce hole, is conducive to the stripping of target compound in cell, can promote mass transport process.In addition, ultrasonic wave can also reduce raw meal particle size, thereby increases the contact area of material and solvent, is conducive to the extraction of target compound.That ultrasonic wave assisted extraction has is easy to operate, with low cost, extraction time is short, be easy to amplify the advantages such as production.Conventional ultrosonic extractor comprises sonde-type extraction element and water-bath type extraction element at present.The former probe sphere of action is limited, is unfavorable for amplifying producing; The ultrasonic vibration that the latter produces can must just can be passed to sample by medium and sample bottle, and this indirectly ul-trasonic irradiation mode may affect extraction efficiency.
Microwave can or be extracted material by intracellular polar water molecules and absorbs and produce amount of heat, make temperature in cell increase rapidly, the pressure that water vapor produces can break through cell membrane and cell membrane, forms larger mass transfer channel, thereby promotes the extraction of target compound.Microwave-assisted Extraction is got has that extraction time is short, solvent load is few, extraction efficiency advantages of higher.Conventional Microwave Extraction device comprises sealed high pressure extraction tank and open atmospheric extraction device at present.The former intensity to extractor material and sealing requirements are very high, and quantity of sample handling is little, and poor stability is expensive, and cool time that need to be longer.The latter often can not regulate extraction temperature, has affected the optimization of extraction process, may cause some thermal instability target compound degradeds when excess Temperature.
In recent years, in order to improve extraction efficiency, the patent documentation that ultrasonic wave and Microwave Extraction technology are combined is of common occurrence, void effect and microwave that Chinese patent literature can make full use of ultrasonic vibration had both had high energy effect, can overcome again some deficiency of conventional ultrasound and Microwave Extraction technology.Chinese patent CN2748147Y, CN1651896A.CN2773664Y.CN2822737Y, CN2880211Y discloses several ultrasonic wave Microwave Extraction devices, differs from one another.
But research shows, often there is following point in existing ultrasonic wave and Microwave Extraction device:
1) there is very large energy loss penetrating in microwave in process, single microwave entrance causes microwave near microwave entrance place and different away from the degree of heat of the sample at microwave entrance place, and, the form that Microwave Water is straight to be penetrated makes to exist in sample bottle the heating dead angle of sample, thereby cause the halfway technological deficiency of sample extraction, and the inhomogeneous phenomenon of above-mentioned heating cannot improve by extending microwave irradiating time simply;
2) the irradiation speed of microwave is very fast, and existing tank shape sample bottle makes microwave penetrate sample solution in moment, and after this, does not have lossy microwave energy to run off in vain, and the utilization rate of microwave energy is low, has extended microwave irradiating time, and energy loss is large.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is to overcome the ultrasonic Microwave Extraction device that involves of the prior art and causes the technological deficiency that sample extraction is inhomogeneous and then cause sample extraction rate to decline, thereby a kind of ultrasonic Microwave Extraction system that involves of the overall recovery rate that can improve sample is provided.
For this reason, the invention provides the ultrasonic Microwave Extraction system that involves of a kind of improved Chinese medicine, comprise the openable closed box of upper cover, be arranged at the sample solution device with openable entrance of described closed box inside, also comprise the movably microwave introduction device that is arranged on described sample solution device and movably ultrasonic wave import device, the cavity that described sample solution device is cuboid, described microwave introduction device has the even number microwave entrance being arranged on described sample solution device, cornerwise two ends in the space that even number microwave entrance forms at the sample solution of described cavity distribute in pairs with maximum distance, described microwave entrance is rectangular opening, the length of described microwave entrance and the ratio of width are 12/25-13/24.
Be positioned at two microwave entrances at the same space diagonal two ends, the minor face along continuous straight runs of one of them microwave entrance arranges, the minor face of another microwave entrance vertically arranges, the seamed edge of the vertical direction of the more close described sample solution device of described microwave entrance that the described microwave entrance that minor face vertically arranges arranges than minor face along continuous straight runs.
Described microwave introduction device also comprises the introduction chamber of the cross section reducing being connected with described microwave entrance, the osculum end of described introduction chamber is connected with described microwave entrance, both junctions arrange microwave and suppress lasso, the big opening end of described microwave introduction chamber is connected with magnetron, on the outer wall of described magnetron, cooler is set, described cooler comprises that socket is arranged on the mount pad of described anode of magnetron, the lug boss that annular water flowing chamber is set on described mount pad and projects upwards from described mount pad, described annular water flowing chamber is divided into the intake tunnel being connected with water inlet and the exhalant canal being connected with delivery port by described lug boss.
Also comprise and be arranged on described closed box inside for making to extract the first reflux that halfway sample solution refluxes, described the first reflux comprises the liquor pump for the sample solution having extracted is burst out being inserted in below sample solution liquid level, the discharge nozzle being connected with described liquor pump, be arranged on the jet in the exit of described discharge nozzle, the corresponding feeder setting of described jet, the lower end of described feeder is communicated with or disconnects with sample solution device by valve, described jet is communicated with discharge nozzle by switch valve or disconnects, also comprise return duct, one end of described return duct is inserted in described sample solution device, the other end is communicated with discharge nozzle by check valve or disconnects.
Also comprise and be arranged on the disk-shaped tube for sample solution is stirred that the whole liquid levels of described sample solution device are following and be communicated with described discharge nozzle by tube connector, several poke holes are set on described disk-shaped tube, described poke hole is bellmouth, and the osculum end of described bellmouth is towards liquid level setting; One end that described tube connector is connected with described discharge nozzle is positioned at the inside of described sample solution device.
Also comprise and be arranged on second reflux of described closed box inside for the sample solution of vaporization is refluxed, described the second reflux has the taper drainage hood that is inserted into described sample solution device inside, the big opening end of described taper drainage hood covers whole liquid level and is positioned at the position of described liquid level the most close above described sample solution device upper end, the osculum end of described taper drainage hood connects condenser pipe, the outer cover of described condenser pipe is connected to circulating water flow siphunculus, on described circulating water flow siphunculus, loop head and loop exit is set.
Also comprise coordinated regulation device, described coordinated regulation device imports the position of device on described sample solution device and makes described microwave introduction device import device to the ultrasound waveguide Inbound orthogonal vertical all the time in described sample solution device to the microwave importing direction in sample solution device and described ultrasonic wave by controlling described microwave introduction device and described ultrasonic wave, and, on described coordinated regulation device, the first warning device is set, Secondary Report alarm device and the 3rd warning device, extract while beginning, described in described collaborative adjusting device control, microwave introduction device imports microwave, after certain hour, described the first warning device sends alarm signal to described coordinated regulation device, described in the control of described coordinated regulation device, ultrasonic wave imports device and imports ultrasonic wave, after certain hour, described Secondary Report alarm device sends alarm signal to described coordinated regulation device, described coordinated regulation device is controlled respectively described microwave introduction device and ultrasonic wave and is imported device and change its operate power, makes operate power separately respectively lower than its initial power, described the 3rd warning device imports device at described microwave introduction device and described ultrasonic wave and sends alarm signal to described coordinated regulation device after with the operate power work certain hour after changing, described coordinated regulation device is first controlled described microwave introduction device and is quit work, and the described ultrasonic wave of rear control imports device and quits work.
Also comprise and be arranged on second reflux of described closed box inside for the sample solution of vaporization is refluxed, described the second reflux has the taper drainage hood that is inserted into described sample solution device inside, the big opening end of described taper drainage hood covers whole liquid level and is positioned at the position of described liquid level the most close above described sample solution device upper end, the osculum end of described taper drainage hood connects condenser pipe, the outer cover of described condenser pipe is connected to circulating water flow siphunculus, on described circulating water flow siphunculus, loop head and loop exit is set.
Technique scheme of the present invention has the following advantages compared to existing technology:
1. the ultrasonic Microwave Extraction system that involves provided by the invention, the cavity that described sample solution device is cuboid, described microwave introduction device has the even number microwave entrance being arranged on described sample solution device, and cornerwise two ends in the space that even number microwave entrance forms at the sample solution of described cavity distribute in pairs with maximum distance.Microwave entrance adopts the even number mode of design in pairs, and the paired distribution in cornerwise two ends in the space that microwave entrance forms in cavity along sample solution, after this imports ultrasonic wave, the microwave importing from two microwave entrances 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 shell-broken effect of ultrasonic wave in whole space.
2. the ultrasonic Microwave Extraction system that involves provided by the invention, described microwave entrance is the opening of rectangle or trapezoidal shape, be positioned at two microwave entrances at the same space diagonal two ends, the minor face along continuous straight runs of one of them microwave entrance arranges, the minor face of another microwave entrance vertically arranges, the seamed edge of the vertical direction of the more close described sample solution device of described microwave entrance that the described microwave entrance that minor face vertically arranges arranges than minor face along continuous straight runs; The length of described microwave entrance and the ratio of width are 12/25-13/24.The present invention adopts microwave incidence angle to become 0 degree angle with sample solution, and microwave energy is absorbed by sample solution to greatest extent.Described in two, microwave entrance is pressed vertical and horizontal layout, after making microwave energy penetrate cavity by waveguide, the component of the horizontal direction of leading wave field and the component of vertical direction form orthogonal superposition in cavity, improve microwave field density, make field strength distribution more even simultaneously, sample solution is in the radiation of high-intensity microwave energy completely, the uniformity of heating using microwave and the intensity of heating using microwave are improved, this kind of particular design of evidence microwave entrance, for the extraction with the same sample solution of amount, 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, this is farthest reflected microwave in this device, thereby the utilization rate of microwave is greatly improved, and, the field intensity that can form orthogonal superposition between the microwave reflecting, has further increased heating using microwave efficiency.
3. the ultrasonic Microwave Extraction system that involves provided by the invention, described microwave introduction device also comprises the introduction chamber of the cross section reducing being connected with described microwave entrance, described introduction chamber is waveguide cavity, the osculum end of described introduction chamber is connected with described microwave entrance, making microwave in the time entering microwave entrance, obtain concentrating strengthens, both junctions arrange microwave and suppress lasso, prevent the leakage of microwave in junction, the big opening end of described microwave introduction chamber is connected with magnetron, magnetron is in the time producing microwave, the anode heat of magnetron constantly raises, by cooler being set on the outer wall of described magnetron, for carrying out cooling to magnetron, can avoid the magnetron working time larger time, because heat is difficult to the burnout phenomenon that scatters and disappears and cause.Described cooler comprises that socket is arranged on the mount pad of described anode of magnetron, the lug boss that annular water flowing chamber is set on described mount pad and projects upwards from described mount pad, described annular water flowing chamber is divided into the intake tunnel being connected with water inlet and the exhalant canal being connected with delivery port by described lug boss, annular mount pad is directly socketed on described magnetron, be convenient to install, and annular water flowing chamber is set on mount pad can make magnetron obtain omnibearing heat radiation, be more importantly, lug boss is set on mount pad, described annular water flowing chamber is divided into the intake tunnel being connected with water inlet and the exhalant canal being connected with delivery port by described lug boss, this kind of design makes the structure of cooler very compact, and cooling effect is good.
4. the ultrasonic Microwave Extraction system that involves provided by the invention, also comprise and be arranged on described closed box inside for making to extract the first reflux that halfway sample solution refluxes, described the first reflux comprises the liquor pump for the sample solution having extracted is burst out being inserted in below sample solution liquid level, the discharge nozzle being connected with described liquor pump, be arranged on the jet in the exit of described discharge nozzle, the corresponding feeder setting of described jet, described jet is communicated with discharge nozzle by switch valve or disconnects, also comprise return duct, one end of described return duct is inserted in described sample solution device, the other end is communicated with discharge nozzle by check valve or disconnects.After sample solution extracts, or in leaching process, need sample solution to pump while detecting, opening liquor pump 2 is pumped into sample solution in described discharge nozzle, open switch valve, the coating part entering in discharge nozzle enters jet, spray into feeder so that collect and detect from described jet, 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; Meanwhile, another part solution entering in described discharge nozzle enters in mixing component by tube connector, and spouting from the poke hole of mixing component, the solution of device bottom surface is dug, the problem of having avoided sample solution that viscosity is larger to be difficult to pumping.For example, in the time not needing pumping (sample solution finds that sample extraction is not thorough after detecting), 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, the flap of described check valve is opened, check valve is opened towards the inside of sample solution device, the sample solution that is positioned at discharge nozzle enters return duct along check valve, be 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, the vibrating effect of auxiliary ultrasonic.While finding that after retrieval sample extraction is not thorough, 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.Above-mentioned design of the present invention, by the pan feeding of sample solution, pumping, detect, again the effect that imports and prevent precipitation is combined as a whole, while having avoided bottle that available technology adopting is general as sample solution device, at pan feeding, when discharging and detection, all need sample bottle to take out the technological deficiency that just can reduce operating efficiency from closed box, and be particularly useful for the extraction of the sample solution that viscosity is larger, simultaneously, for the extraction of the sample solution of experimental stage, because researcher is immature for the research of experiment condition, usually there will be the halfway situation of extracting, this kind of design avoided taking out frequently, pack the defect of sample bottle into, can understand the extraction situation of sample by pumping, reduce working strength.
5. the ultrasonic Microwave Extraction system that involves provided by the invention, also comprise and be arranged on the disk-shaped tube for sample solution is stirred that the whole liquid levels of described sample solution device are following and be communicated with described discharge nozzle by tube connector, several poke holes are set on described disk-shaped tube, described poke hole is bellmouth, and the osculum end of described bellmouth is towards liquid level setting; One end that described tube connector is connected with described discharge nozzle is positioned at the inside of described sample solution device.Described liquor pump is in needs pumping outward, play the effect of pumping sample solution outward, in not needing outward pumping sample solution, spray the liquid level to sample solution device by the poke hole being arranged on disk-shaped tube, thereby the sample solution in described sample solution device is produced and agitated, play the effect of stirring, effectively prevent precipitation, because described liquor pump one pump is dual-purpose, self circulation by sample solution just can be stirred, do not need to introduce shaft, just can play good anti-precipitation.Described poke hole is bellmouth, and the osculum end of described bellmouth is towards liquid level setting.Poke hole is set to bellmouth and osculum end towards liquid level setting, can make sample solution enter liquid level in the mode of jet, has strengthened stirring action, thereby improves sludge proof effect.The mixing component that dish type arranges increases stirring area, has further strengthened anti-sedimentation effect.
6. the ultrasonic Microwave Extraction system that involves provided by the invention, also comprise and be arranged on second reflux of described closed box inside for the sample solution of vaporization is refluxed, described the second reflux has the taper drainage hood that is inserted into described sample solution device inside, the big opening end of described taper drainage hood covers whole liquid level and is positioned at the position of described liquid level the most close above described sample solution device upper end, the large end face of taper drainage hood covers whole liquid level, and be positioned at the position of described liquid level the most close above described sample solution device upper end, the all gas producing in microwave heating process can be entered in described taper drainage hood, under the effect of the inwall of taper drainage hood, be condensed into liquid, and be back in sample solution along taper drainage hood, the osculum end of described taper drainage hood connects condenser pipe, the outer cover of described condenser pipe is connected to circulating water flow siphunculus, cannot carry out the portion gas of condensation by the inwall of taper drainage hood, a bite end by taper drainage hood enters in condenser pipe, the circulating water flow siphunculus of cooling effect by to(for) condenser pipe, this portion gas is condensed in condenser pipe, is back in sample solution.
7. the ultrasonic Microwave Extraction system that involves provided by the invention, the cooling liquid outlet of cooling back installation is communicated with described loop head, described cooling liquid inlet is communicated with loop exit, for refluxing cooling liquid and being interconnected for the outer wall of sample solution device is carried out to cooling cooling back installation, thereby the cold of above-mentioned two cooling systems of the present invention is reused, reduce energy consumption, and, dwindle the quantity of the extraneous chilled water system of native system, made structure compacter; And for the ease of rear circulating cooling liquid the pressurization for front circulating cooling, described in several, deflector forms corrugated fluid passage, height along the described deflector of fluid direction of advance reduces gradually, gap between adjacent baffle increases gradually, is not more than the 0.5-0.8 in gap between the adjacent baffle at the rear of fluid direction of advance doubly in the gap between the adjacent baffle of fluid direction of advance forefront.
8. the ultrasonic Microwave Extraction system that involves provided by the invention, by coordinated regulation device is set, importing time, importing order, importing power and shut-in time to ultrasonic wave and microwave are strictly controlled, first control and import microwave, and after importing certain hour, microwave just starts to import ultrasonic wave, this makes the heat of microwave can pass to better sample solution, thereby guarantee sample solution to be heated to after certain hour and degree at microwave, just carry out hyperacoustic importing, avoided importing in advance ultrasonic wave and sample causes the waste of energy when heated; After sample solution is heated to a certain degree, the heat effect of hyperacoustic cavitation and microwave better merges, and, described in the control of coordinated regulation device, the importing direction of hyperacoustic importing direction and microwave is vertical, make 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 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 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, make the scope of application of native system larger; In addition, due to the later stage in vibration, sample is probably all by broken wall treatment, the power of controlling ultrasonic wave importing device and microwave introduction device is less than initial power, can avoid entering in damaged cell membrane under active material that mass transfer has gone out from the cell membrane of broken wall strong effect of vibration again, improve the extracted amount that extracts the later stage; And the heat effect that extracts later stage microwave is not obvious for the effect of extracting, first out of service by coordinated regulation device control microwave introduction device, can further reduce energy consumption.
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 invention and 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 extraction system and the electricity connection diagram of whole system that embodiments of the invention 1 provide;
Fig. 3 is the structural representation of the microwave entrance of the extraction system that provides of embodiments of the invention 2 set-up mode on sample solution device;
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 of extraction system and the scheme of installation of sample solution device that embodiments of the invention 4 provide;
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-liquor pump; 22-discharge nozzle; 23-jet; 24-switch valve; 25-return duct; 26-check valve; 27-tube connector; 28-disk-shaped tube; 29-poke hole; 3-cooling-cycle device; 31-cooling liquid inlet; 32-cooling liquid outlet; 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-delivery port; 54f-outer shroud; 54k-notch; The 54h-gap of circulating; 6-ultrasonic wave imports device; 7-coordinated regulation device; 70-PLC; 71-the first warning device; 72-Secondary Report alarm device; 73-the 3rd warning device; 81-taper 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 Microwave Extraction system that involves for Chinese medicine or active substance of plant extraction, comprise the openable closed box 1 of upper cover, be arranged at the sample solution device 2 with openable entrance of described closed box 1 inside, between described sample solution device 2 and described casing 1 and the cooling back installation 3 with cooling liquid inlet 31 and cooling liquid outlet 32 of the sidewall setting of the described sample solution device 2 of fitting, also comprise the movably microwave introduction device 5 being arranged on described sample solution device 2, movably ultrasonic wave imports device 6 and coordinated regulation device 7, described coordinated regulation device 7 comprise PLC controller 70 and can with PLC controller 70, microwave introduction device 5 and ultrasonic wave import the first warning device 71 of device 6 feedback operation, Secondary Report alarm device 72, the 3rd warning device 73, at this, described the first warning device 71, the signalling means with time counting function that Secondary Report alarm device 72 and the 3rd warning device 73 generally adopt for those skilled in the art.
In the present embodiment, described microwave introduction device 5 comprise produce the magnetron 53 of microwave, for conducting the introduction chamber 52 of the microwave that described magnetron 53 produces, described introduction chamber 52 is reducing cross section, wherein big opening end is connected with magnetron 53, osculum end is connected to microwave entrance 51, described microwave entrance 51 is arranged in the upright side walls of described sample solution device 2, this microwave entrance 51 is rectangular aperture, this rectangular aperture makes the importing direction of microwave and liquid level be zero degree angle, makes sample solution farthest heated.Described ultrasonic wave importing device 6 is positioned at the bottom of described sample solution device 2, hyperacoustic importing direction is substantially vertical with the importing direction of microwave, thereby make microwave heating action produce huge forward impact for hyperacoustic shearing shell-broken effect, greatly improved the destruction efficiency of ultrasonic wave for sample cell wall.
Preferred as one, the importing direction of described ultrasonic wave and described microwave is orthogonal vertical, now, microwave heating action not only can be aggravated hyperacoustic shearing shell-broken effect, and, can produce larger stack broken wall field intensity, be convenient to promote evenly carrying out of broken wall.
Import the importing position of device 6 on described sample solution device 2 in order to control described microwave introduction device 5 and ultrasonic wave, the same side of described sample solution device 2 arranges several microwave entrances 51, simultaneously, this sidewall is connected with described microwave introduction device 5 by baffle plate (not shown) movably, in the time that needs import 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, make baffle plate not need the entrance that imports microwave to block, so can realize the adjustment of baffle plate for microwave entrance 51, in the present embodiment, the screw that moves through of described baffle plate is realized electrodeless adjusting.In the present embodiment, in order to realize the control that described ultrasonic wave is imported to the importing position of device 6, import at the described ultrasonic wave of the installation of described sample solution device 2 on the sidewall of device 6 guide-track groove (not shown) is set, described ultrasonic wave imports on device 6 and is provided with the sidewall matching with described guide-track groove, described sidewall is embedded to described guide-track groove, can realize described ultrasonic wave by sliding and import the movement of device 6 on described sample solution device 2, thereby change the ultrasonic vibration orientation of ultrasonic wave importing device 6.
In the present embodiment, in order to realize the Collaborative Control to ultrasound waveguide Inbound and microwave importing direction, described ultrasonic wave imports on device 5 and described microwave introduction device 6 displacement transducer (not shown) is set respectively, described displacement transducer is connected with the PLC controller 70 of described coordinated regulation device 7, can transmit displacement signal and in the time receiving the action order of PLC controller 70, move to predefined position to described PLC controller 70.
In the present embodiment, the meaning of described cooling back installation setting is: after system works long hours, produce a large amount of heats, heat cannot shed service life of the system that affects, by cooling back installation 3 being set in the gap of described sample solution device 2 and described closed box 1, not only the amount of heat producing in system works can be scattered and disappeared, cooling back installation 3 is arranged on and can makes system compacter between the two, when work, import cooling fluid from cooling liquid inlet 31, cooling fluid takes away the heat of the system liquid that is cooled for the conduction of cold, finally discharge from cooling liquid outlet 32, thereby the heat of the system of making (especially sample solution device 2) is dispersed, the service life of raising system.
The above-mentioned ultrasonic Microwave Extraction system that involves of utilizing that the present embodiment provides carries out comprising when the active material of sample extracts following processing step:
Step 1: open the described upper cover of closed box 1, and the described entrance of sample solution device 2, 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 described coordinated regulation device 7, as shown in Figure 2, the PLC controller 70 of described coordinated regulation device 7 is first to described microwave introduction device 5 and the first warning device 71 transmitted signals, described microwave introduction device 5 is started working with initial power P1 immediately receiving after described signal, simultaneously, described the first warning device 71 starts to carry out time counting receiving after described signal, after elapsed time t1, described the first warning device 71 sends alarm signal to described PLC controller, described PLC controller 70 imports device 6 to described ultrasonic wave and sends working signal receiving after described alarm signal, and send working signal to described Secondary Report alarm device 72 simultaneously, described ultrasonic wave imports device 71 and starts working with initial power P2 immediately receiving after described working signal, 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 PLC controller is receiving after described signal that the while sends to described microwave introduction device 5 and described ultrasonic wave importing device 6 signal that changes operating powers, and send working signal to the 3rd warning device 73, described microwave introduction device 5 and described ultrasonic wave import device 6 and are receiving that after this signal, priority changes its operating power, make operating power be less than respectively its initial power P1, P2, described the 3rd warning device 73 starts to carry out time counting receiving after this working signal, after elapsed time t3, described the 3rd warning device 73 is to described PLC controller 70 transmitted signals, described PLC controller 70 is first controlled described microwave introduction device 5 after described signal and is quit work receiving, the described ultrasonic wave of rear control imports device 6 and quits work.
The said extracted system of the present embodiment, has been realized to described microwave introduction device 5 and described ultrasonic wave is imported job order, working time, the operating power of device 6 and stop the Comprehensive Control of order by coordinated regulation device 7.First control and import microwave, and after importing certain hour, microwave just starts to import ultrasonic wave, this makes the heat of microwave can pass to better sample solution, thereby guarantee sample solution to be heated to after certain hour and degree at microwave, just carry out hyperacoustic importing, avoided importing in advance ultrasonic wave and sample causes the waste of energy when heated; After sample solution is heated to a certain degree, the heat effect of hyperacoustic cavitation and microwave better merges, and, it is vertical that coordinated regulation device 7 is controlled the importing direction of described hyperacoustic importing direction and microwave, make 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 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 adjust described ultrasonic wave and import the position on sample solution device 2 described in device 6 microwave introduction devices 5, thereby the importing direction that makes described ultrasonic wave and microwave can remain vertical, make the scope of application of native system larger; In addition, due to the later stage in vibration, sample is probably all by broken wall treatment, the power of controlling ultrasonic wave importing device and microwave introduction device is less than initial power, can avoid the active material that mass transfer has gone out from the cell membrane of broken wall to enter in damaged cell membrane under strong effect of vibration again, improve the extracted amount that extracts the later stage; And the heat effect that extracts later stage microwave is not obvious for the effect of extracting, first out of service by coordinated regulation device control microwave introduction device, can further reduce energy consumption.
It should be noted that, while utilizing said extracted system that the present embodiment provides to carry out the extraction of bioactivator, operate power after described time t1, t2, t3, initial power P1, P2 and change can change according to the different material extracting, above-mentioned numerical value is in the time that extraction work starts, pre-set according to the different material extracting.In the present embodiment, said extracted system is for the extraction to Reishi sporule, wherein time t1 is 1-3 minute, time t2 is 3-5 minute, and time t3 is 2-3 minute, thereby whole extraction time was controlled in 6-11 minute, greatly improve extraction efficiency, initial power P1 is 50-200W, and 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, it is the distortion on embodiment 1 basis, in the present embodiment, as shown in Figure 3, the cavity that described sample solution device 2 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.The ultrasonic Microwave Extraction system that involves that the present embodiment provides, the cavity that described sample solution device 2 is cuboid, described microwave introduction device 5 has the cornerwise two ends that are arranged on the space that 51, two described microwave entrances 51 of two microwave entrances on described sample solution device form at the sample solution of described cavity and distributes in pairs with maximum distance.The paired distribution in cornerwise two ends in the space that microwave entrance 51 forms in cavity along sample solution, 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 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 shell-broken effect of ultrasonic wave in whole space.
As the one distortion of the present embodiment, described microwave entrance 51 can also be set to other numbers, for example 4,6,8 etc. even number numbers, cornerwise two ends in the space that even number microwave entrance 51 forms along sample solution distribute in pairs with maximum distance.
Improve as one, in the present embodiment, described microwave entrance 51 is rectangular opening, 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 2 of described microwave entrance 51 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 12/25-13/24.Particularly, the described microwave entrance 51 that minor face vertically arranges is 75 millimeters near the distance between vertical edges and this vertical seamed edge of the strong vertical seamed edge of the described microwave resonance being close to, and the described microwave entrance 51 of minor face along continuous straight runs setting is 90 millimeters near the distance between vertical edges and this vertical seamed edge of the strong vertical seamed edge of the described microwave resonance being close to.The length of described microwave entrance 51 is 250 millimeters, and width is 130 millimeters, and the inside of described cavity has sample solution, and the distance of the liquid level of described sample solution and the upper wall of described cavity is 120 millimeters.
The above-mentioned ultrasonic Microwave Extraction system that involves that the present embodiment provides, microwave incidence angle becomes 0 degree angle with sample solution, microwave energy is absorbed by sample solution to greatest extent.Described in two, microwave entrance 51 is pressed vertical and horizontal layout, after making microwave energy penetrate cavity by waveguide, the component of the horizontal direction of leading wave field and the component of vertical direction form orthogonal superposition in cavity, improve microwave field density, make field strength distribution more even simultaneously, sample solution is in the radiation of high-intensity microwave energy completely, the uniformity of heating using microwave and the intensity of heating using microwave are improved, this kind of particular design of evidence microwave entrance, for the extraction with the same sample solution of amount, 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, this is farthest reflected microwave in this device, thereby the utilization rate of microwave is greatly improved, and, the field intensity that can form orthogonal superposition between the microwave reflecting, has 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.
As the another kind distortion of the present embodiment, it can not arrange coordinated regulation device 7.
Embodiment 3
The present embodiment provides a kind of ultrasonic Microwave Extraction system that involves, it is the distortion on embodiment 1 or 2 bases, in the present embodiment, as shown in Figure 4, described microwave introduction device 5 comprises magnetron 53, excitation 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, one group is the electromagnetism iron wire bag that magnetron carries, another group be by enamel-covered wire around the electromagnetism iron wire bag that is enclosed within magnetron outside coil, these two parts have special field power supply, electromagnetic electric current in electromagnetism iron wire bag is 8.0A left and right, and in additional coil, the large I of electric current is adjusted by coordinated regulation device 7.Reponse system has two parts, and a part is that anode current is input in one section of coil in magnet exciting coil and is fed back, and a sampling resistor of another part design is connected in anode of magnetron loop, and anode current information is provided.Described cooler 54 comprises that socket is arranged on the lug boss 54c that annular water flowing chamber 54b is set and projects upwards from described mount pad 54a on mount pad 54a described in the mount pad 54a of described magnetron 53 anodes, and 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.The concrete size of cooler 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 cooler 54 sealings best.On the outer wall of described annular water flowing chamber 54b, outer shroud 54f is set, described outer shroud 54f is used for installing refrigerating gas, for the liquid of annular water flowing chamber 54b is dispelled the heat.
Lug boss 54c, as the watershed of annular water flowing chamber 54b, in order to the shunting of turnover current, makes annular water flowing chamber 54b become circulation runner in the present embodiment.Lug boss 54c is corresponding with annular water flowing chamber 54b goes out to form circulation gap 54h, and its effect is to make whole circumference in annular water flowing chamber 54b have water to flow through to derive heat, makes magnetron 53 anode perisporiums heat radiations evenly.The external diameter interference fit of the endoporus of cooler 54 and anode of magnetron.In the present embodiment, U-lag mouth is set on the lateral margin of described mount pad 54a, its effect is to beat groove in order to fixing spiral shell for subsequent use while installing for cooler, it is installed after magnetron be fixed in framework.
Embodiment 4
The present embodiment provides a kind of ultrasonic Microwave Extraction system that involves, it is the distortion on embodiment 1 or 2 or 3 bases, in the present embodiment, as shown in Figure 5, described extraction system also comprises and is arranged on the first reflux refluxing for making to extract halfway sample solution in described closed box 1 inside, 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, for driving the motor 10 of liquor pump 21, 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 20 of described jet 23 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.Also comprise and be arranged on the disk-shaped tube 28 for sample solution is stirred that the whole liquid levels of described sample solution device 2 are following and be communicated with described discharge nozzle 22 by tube connector 27, several poke holes 29 are set on described disk-shaped tube 28, described poke hole 29 is bellmouth, and the osculum end of described bellmouth is towards liquid level setting; One end that described 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, check valve 26 in the present embodiment is check valves of a kind of spring, its basic operation 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, and the flap of check valve 26 is closed, and the sample solution in discharge nozzle 22 can not enter in described return duct 25, now, carry out the normal pumping of sample solution; In the time not needing pumping sample solution, switch valve 24 cuts out, pressure in discharge nozzle 22 increases gradually, in the time that the pressure in discharge nozzle 22 is greater than spring pressure, the flap of check valve 26 is backed 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 in described sample solution device 2.
It should be noted that, it arranges the check valve of mentioning in the present embodiment object and is mainly release, and can in the time that described switch valve 24 cuts out, open, and makes the sample in discharge nozzle 22 enter in return duct 25 and be back in sample solution device 2; And in the time that described switch valve 24 is opened, described check valve 26 is closed, sample solution in discharge nozzle 22 is injected into feeder 20 from described jet 23, in feeder 20, sample solution is collected or is detected, if find after detection, sample solution does not extract completely, open the valve between feeder 20 and sample solution device 2, sample solution come back in sample solution device.For realizing this main purpose, specifically arranging of described check valve can be various, except the spring check valve that the present embodiment is mentioned, 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, detect, again the effect that imports and prevent precipitation is combined as a whole, while having avoided bottle that available technology adopting is general as sample solution device, at pan feeding, when discharging and detection, all need sample bottle to take out the technological deficiency that just can reduce operating efficiency from closed box, and be particularly useful for the extraction of the sample solution that viscosity is larger, simultaneously, for the extraction of the sample solution of experimental stage, because researcher is immature for the research of experiment condition, usually there will be the halfway situation of extracting, this kind of design avoided taking out frequently, pack the defect of sample bottle into, can understand the extraction situation of sample by pumping, reduce working strength.
Embodiment 5
The present embodiment provides a kind of ultrasonic Microwave Extraction system that involves, it is the distortion on embodiment 1 or 2 or 3 or 4 bases, in the present embodiment, the cooling liquid outlet 32 of described cooling back installation 3 is communicated with described loop head 84, described cooling liquid inlet 31 is communicated with loop exit 85, described cooling back installation 3 comprises that laminating is arranged on the stainless steel paster on described sample solution device 2 outer walls, and be vertically set on several deflectors 33 on described stainless steel paster, described in several, deflector 33 forms corrugated fluid passage, as shown in Figure 7, along fluid direction of advance, gap between adjacent baffle 33 increases gradually, be not more than the 0.5-0.8 in gap between the adjacent baffle 23 at the rear of fluid direction of advance in the gap between the adjacent baffle 33 of fluid direction of advance forefront 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, it is the further improvement on embodiment 1 or 2 or 3 or 4 or 5 bases, in the present embodiment, as shown in Figure 1, also comprise and be arranged on second reflux of described closed box 1 inside for the sample solution of vaporization is refluxed, described the second reflux has the taper drainage hood 81 that is inserted into described sample solution device inside, the big opening end of described taper drainage hood 81 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, the outer cover of described condenser pipe 82 is connected to circulating water flow siphunculus 83, loop head 84 and loop exit 85 are set on described circulating water flow siphunculus 83.
Obviously, above-described embodiment is only for example is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all embodiments.And the apparent variation of being extended out thus or variation are still among the protection domain in the invention.
Claims (6)
1. the improved ultrasonic Microwave Extraction system that involves, comprise the openable closed box of upper cover (1), be arranged at the inner sample solution device (2) with openable entrance of described closed box (1), it is characterized in that: also comprise the movably microwave introduction device (5) that is arranged on described sample solution device (2) and movably ultrasonic wave import device (6), it is characterized in that: described sample solution device (2) is cuboid cavity, described microwave introduction device (5) has the even number microwave entrance (51) being arranged on described sample solution device (2), 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, described microwave entrance (51) is rectangular opening, the length of described microwave entrance (51) and the ratio of width are 12/25-13/24, 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.
2. the improved ultrasonic Microwave Extraction system that involves according to claim 1, it is characterized in that: described microwave introduction device (5) also comprises the introduction chamber (52) of the cross section reducing 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 microwave introduction chamber 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).
3. the improved ultrasonic Microwave Extraction system that involves according to claim 2, it is characterized in that: also comprise and be arranged on inner the first reflux that is used for making to extract halfway sample solution backflow of described closed box (1), 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).
4. the improved ultrasonic Microwave Extraction system that involves according to claim 3, it is characterized in that: also comprise and be arranged on all following disk-shaped tubes (28) for sample solution is stirred being also communicated with described discharge nozzle (22) by tube connector (27) of liquid level of described sample solution device (2), several poke holes (29) are set on described disk-shaped tube (28), described poke hole (29) is bellmouth, and the osculum end of described bellmouth is towards liquid level setting; One end that described tube connector (27) is connected with described discharge nozzle (22) is positioned at the inside of described sample solution device (2).
5. the improved ultrasonic Microwave Extraction system that involves according to claim 4, it is characterized in that: also comprise and be arranged on inner the second reflux for the sample solution of vaporization is refluxed of described closed box (1), described the second reflux has the taper drainage hood (81) that is inserted into described sample solution device inside, the big opening end of described taper drainage hood (81) covers whole liquid level and is positioned at the described liquid level position of the most close described sample solution device (2) upper end above, the osculum end of described taper drainage hood (81) connects condenser pipe (82), the outer cover of described condenser pipe (82) is connected to circulating water flow siphunculus (83), loop head (84) and loop exit (85) are set on described circulating water flow siphunculus (83).
6. according to the improved ultrasonic Microwave Extraction system that involves described in any one in claim 1-5, it is characterized in that: also comprise coordinated regulation device (7), described coordinated regulation device (7) imports the position of device (6) on described sample solution device (2) and makes the ultrasound waveguide Inbound all the time orthogonal vertical of described microwave introduction device (5) in to the microwave importing direction in sample solution device (2) and described ultrasonic wave importing device (6) to described sample solution device (2) by controlling described microwave introduction device (5) and described ultrasonic wave, and, on described coordinated regulation device (7), the first warning device is set, Secondary Report alarm device and the 3rd warning device, extract while beginning, described collaborative adjusting device (7) is controlled described microwave introduction device (5) and is imported microwave, after certain hour, described the first warning device sends alarm signal to described coordinated regulation device (7), described coordinated regulation device (7) is controlled described ultrasonic wave and is imported device (6) importing ultrasonic wave, after certain hour, described Secondary Report alarm device sends alarm signal to described coordinated regulation device, described coordinated regulation device (7) successively controls described microwave introduction device (5) and ultrasonic wave importing device (6) changes respectively its operate power, makes operate power separately respectively lower than its initial power, described the 3rd warning device sends alarm signal at described microwave introduction device (5) and described ultrasonic wave importing device (6) with the backward described coordinated regulation device of operate power work certain hour (7) after changing, described coordinated regulation device (7) is first controlled described microwave introduction device (5) and is quit work, and the described ultrasonic wave of rear control imports device (6) and quits work.
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Inventor after: Liao Hengbin Inventor after: Yin Yunfeng Inventor before: Jin Feng |
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| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170922 Address after: Xingye Road Industrial Park, Mayang Miao Autonomous County, Huaihua, Hunan, 418000 Patentee after: Hunan Li'Nong WuBeiZi Industry Development Co. Ltd. Address before: Yueqing City, Zhejiang province Yuecheng town Tadatoki outside No. 6 Lane 2 Patentee before: Jin Feng |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Improved ultrasonic wave and microwave extraction system Effective date of registration: 20171226 Granted publication date: 20160504 Pledgee: Hunan Mayang rural commercial bank Limited by Share Ltd Pledgor: Hunan Li'Nong WuBeiZi Industry Development Co. Ltd. Registration number: 2017430000120 |
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| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20200512 Granted publication date: 20160504 Pledgee: Hunan Mayang rural commercial bank Limited by Share Ltd Pledgor: HUNAN LINONG GALLNUT INDUSTRY DEVELOPMENT Co.,Ltd. Registration number: 2017430000120 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Improved ultrasonic wave and microwave extraction system Effective date of registration: 20200512 Granted publication date: 20160504 Pledgee: Hunan Mayang rural commercial bank Limited by Share Ltd Pledgor: HUNAN LINONG GALLNUT INDUSTRY DEVELOPMENT Co.,Ltd. Registration number: Y2020980002143 |