The ultrasonic Microwave Extraction system that involves of a kind of Chinese medicine
Technical field
The present invention relates to the ultrasonic Microwave Extraction system that involves of a kind of Chinese medicine, 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 is very high to the intensity of extractor material and sealing requirements, 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 during 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:
While utilizing existing above-mentioned ultrasonic wave Microwave Extraction device to extract, As time goes on, microwave heating action is constantly accumulated, liquid in sample solution device is much vaporized as gas, the gas of gasification is constantly accumulated in sample solution, thereby the top pressure of sample solution is constantly increased, and the increase of top pressure declines the ultrasonic vibration effect under condition of the same race, has reduced the extraction efficiency of sample.
Summary of the invention
Therefore, the technical problem to be solved in the present invention is to overcome the ultrasonic microwave heating equipment that involves of the prior art in the technological deficiency of processing later stage extraction efficiency reduction, thereby the ultrasonic Microwave Extraction system that involves that a kind of efficiency is higher is provided.
For this reason, the invention provides a kind of ultrasonic Microwave Extraction system that involves of Chinese medicine with reflux, comprise the openable closed box of upper cover, be arranged at the sample solution device with openable entrance of described closed box inside, the microwave introduction device and the ultrasonic wave that are fixedly installed on described sample solution device import 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 drainage hood of the cross section reducing that is inserted into described sample solution device inside, the big opening end of described 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 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 are set.
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 even number microwave entrance distributes with maximum distance in pairs at cornerwise two ends in the space of the sample solution formation of described cavity.
Described microwave entrance is the opening of rectangular shape 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 25/12-24/13.
Described microwave introduction device also comprises the introduction chamber of the trapezoid cross section 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 and projects upwards from described mount pad on described mount pad, described lug boss is divided into the intake tunnel being connected with water inlet and the exhalant canal being connected with delivery port by described annular water flowing chamber.
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.
The ultrasonic Microwave Extraction system that involves of Chinese medicine 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 bellmouths are set on described disk-shaped tube, 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 the cooling back installation being arranged between sample solution device and described closed box, the cooling liquid outlet of cooling back installation is communicated with described loop head, described cooling liquid inlet is communicated with loop exit, described cooling back installation comprises that laminating is arranged on the stainless steel paster on described sample solution device outer wall, and be vertically set on several deflectors that highly differ on described stainless steel paster, 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, in the gap between the adjacent baffle of fluid direction of advance forefront, be not more than the 0.5-0.8 in gap between the adjacent baffle at the rear of fluid direction of advance doubly.
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 orthogonal vertical all the time of the ultrasound waveguide Inbound 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 starting, described collaborative adjusting device is controlled described microwave introduction device and is imported microwave, after certain hour, described the first warning device sends alarm signal to described coordinated regulation device, described coordinated regulation device is controlled described ultrasonic wave and is imported device importing ultrasonic wave, after certain hour, described Secondary Report alarm device sends alarm signal to described coordinated regulation device, and described coordinated regulation device controls described microwave introduction device and ultrasonic wave importing device changes its operate power, makes operate power respectively lower than its initial power, described the 3rd warning device imports device at described microwave introduction device and described ultrasonic wave and to described coordinated regulation device, sends alarm signal 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.
Utilize that Chinese medicine described in above-mentioned any one is ultrasonic involves the extraction process that Microwave Extraction system is carried out Chinese medicine, comprise the following steps of carrying out successively:
Step 1: open the described upper cover of closed box, and the described entrance of sample solution device, the solution of pre-configured sample to be extracted is positioned in described sample solution device, and closes described entrance and described upper cover;
Step 2: open described coordinated regulation device, described coordinated regulation device is controlled described microwave introduction device and is opened, described microwave introduction device also imports continuous microwave in described sample solution device, the initial power of described microwave introduction device is P1, after certain hour t1, the first warning device of described coordinated regulation device sends alarm signal to described coordinated regulation device, described coordinated regulation device is controlled described ultrasonic wave and is imported device unlatching after receiving described alarm signal, and import ultrasonic wave in described sample solution device, the initial power that described ultrasonic wave imports device is P2, the importing direction of described hyperacoustic importing direction and described microwave is orthogonal vertical all the time, after certain hour t2, the Secondary Report alarm device of described coordinated regulation device sends alarm signal to described coordinated regulation device, described coordinated regulation device is controlled described ultrasonic wave importing device after receiving described alarm signal simultaneously and described microwave introduction device reduces power, make both power be less than respectively its initial power P1, P2, described coordinated regulation device is controlled described ultrasonic wave and is imported device and described microwave introduction device first to control described microwave introduction device 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.
Sample solution in described step 1 is the sample solution of Reishi sporule, and time t1 is 1-3 minute, and time t2 is 3-5 minute, and time t3 is 6-7 minute.
Technique scheme of the present invention has the following advantages compared to existing technology:
1. the ultrasonic Microwave Extraction system that involves of Chinese medicine provided by the invention, 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, reduce the air pressure of sample solution device top, improve ultrasonic vibration effect, 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, by the inwall of taper drainage hood, cannot carry out the portion gas of condensation, 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.
2. the ultrasonic Microwave Extraction system that involves of Chinese medicine provided by the invention, by coordinated regulation device is set, the importing time to ultrasonic wave and microwave, importing order, importing power and shut-in time 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 while not being heated, after sample solution is heated to a certain degree, the heat effect of hyperacoustic cavitation and microwave better merges, and, the importing direction of the coordinated regulation device described hyperacoustic importing direction of control and microwave is vertical, make ultrasonic wave carry out scissoring vibration to sample, vibration shell-broken effect for sample is best, and ultrasonic wave is vertical with microwave, increased hyperacoustic scissoring vibration field intensity, expanded hyperacoustic vibration area, there is the strong vibration of adding and make the more uniform technique effect of vibration, thereby can improve extraction efficiency, because ultrasonic wave imports device and microwave introduction device is adjustable, when 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, by coordinated regulation device, control microwave introduction device first out of service, can further reduce energy consumption.
3. the ultrasonic Microwave Extraction system that involves of Chinese medicine 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 even number microwave entrance distributes with maximum distance in pairs at cornerwise two ends in the space of the sample solution formation of described cavity.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 intersects with ultrasonic wave respectively, and intersection point is positioned at conplane two opposite ends, after microwave and ultrasonic wave intersect, 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.
4. the ultrasonic Microwave Extraction system that involves of Chinese medicine provided by the invention, described microwave entrance is the opening of rectangular shape 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 25/12-24/13.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 quadrature superposition in cavity, improved 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 have been 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, between the microwave reflecting, can form the field intensity of orthogonal superposition, further increase heating using microwave efficiency.
5. the ultrasonic Microwave Extraction system that involves of Chinese medicine provided by the invention, described microwave introduction device also comprises the introduction chamber of the trapezoid cross section 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 when entering microwave entrance, obtain concentrating strengthens, both junctions arrange microwave and suppress lasso, prevented the leakage of microwave in junction, the big opening end of described microwave introduction chamber is connected with magnetron, magnetron is when 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, in the time of can avoiding the magnetron working time larger, 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 and projects upwards from described mount pad on described mount pad, described lug boss is divided into the intake tunnel being connected with water inlet and the exhalant canal being connected with delivery port by described annular water flowing chamber, annular mount pad is directly socketed on described magnetron, be convenient to install, and annular water flowing chamber is set on mount pad can be so that magnetron obtains omnibearing heat radiation, be more importantly, lug boss is set on mount pad, described lug boss is divided into the intake tunnel being connected with water inlet and the exhalant canal being connected with delivery port by described annular water flowing chamber, this kind of design makes the structure of cooler very compact, and cooling effect is good.
6. the ultrasonic Microwave Extraction system that involves of Chinese medicine 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, from described jet, spray into feeder 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; Meanwhile, another part solution entering in described discharge nozzle enters in mixing component by tube connector, and spouting from the bellmouth 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, when 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, when 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, from described return duct, be back to sample solution device, 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, extraction for 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, the defect that packs sample bottle into, by pumping, can understand the extraction situation of sample, reduced working strength.
7. the ultrasonic Microwave Extraction system that involves of Chinese medicine 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 bellmouths are set on described disk-shaped tube, described bellmouth 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, when not needing outward pumping sample solution, by the bellmouth being arranged on disk-shaped tube, spray the liquid level to sample solution device, thereby the sample solution in described sample solution device is produced and agitated, played the effect of stirring, effectively prevented 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 bellmouth is bellmouth, and the osculum end of described bellmouth is towards liquid level setting.Bellmouth is set to bellmouth and osculum end towards liquid level setting, can, so that sample solution enters liquid level in the mode of jet, strengthen stirring action, thereby improve sludge proof effect.The mixing component that dish type arranges increases stirring area, has further strengthened anti-sedimentation effect.
8. the ultrasonic Microwave Extraction system that involves of Chinese medicine 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, reduced 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 the place ahead 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.
Accompanying drawing explanation
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 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-bellmouth; 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.
The specific embodiment
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 trapezoid 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 oblong openings, this oblong openings makes the importing direction of microwave and liquid level be zero degree angle, and sample solution is farthest heated.Described ultrasonic wave imports the bottom that device 6 is positioned at 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.
As a kind of preferred, 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.
In order to control described microwave introduction device 5 and ultrasonic wave, import the importing position of device 6 on described sample solution device 2, the same side of described sample solution device 2 arranges several microwave entrances 51, simultaneously, this sidewall passes through movably baffle plate (not shown) and is connected with described microwave introduction device 5, when needs import microwave to a certain microwave entrance 51, mobile described baffle plate makes described baffle plate not block this microwave entrance 51, when 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 baffle plate for the adjustment of 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, at the described ultrasonic wave of the installation of described sample solution device 2, import 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, by sliding, can realize described ultrasonic wave and import the movement of device 6 on described sample solution device 2, thereby change the ultrasonic vibration orientation that ultrasonic wave imports 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 and when receiving the action order of PLC controller 70, move to predefined position to described PLC controller 70 transmission displacement signals.
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 at 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 between the two can be so that system be compacter, during work, from cooling liquid inlet 31, import cooling fluid, cooling fluid takes away the heat of the system liquid that is cooled for the conduction of cold, finally from cooling liquid outlet 32, discharge, 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 after receiving described signal, simultaneously, described the first warning device 71 starts to carry out time counting after receiving 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 after receiving described alarm signal, and to described Secondary Report alarm device 72, send working signal simultaneously, described ultrasonic wave imports device 71 and with initial power P2, starts working immediately after receiving described working signal, described Secondary Report alarm device 72 starts to carry out time counting after receiving working signal, after elapsed time t2, described Secondary Report alarm device 72 is to described PLC controller 70 transmitted signals, described PLC controller imports to described microwave introduction device 5 and described ultrasonic wave the signal that device 6 sends change operating power after receiving described signal simultaneously, and send working signal to the 3rd warning device 73, described microwave introduction device 5 and described ultrasonic wave import device 6 and after receiving this signal, change respectively 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 after receiving 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 and is quit work after receiving described signal, 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 Comprehensive Control sequentially 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 while not being heated; After sample solution is heated to a certain degree, the heat effect of hyperacoustic cavitation and microwave better merges, and, the importing direction of the coordinated regulation device 7 described hyperacoustic importing directions of control and microwave is vertical, make ultrasonic wave carry out scissoring vibration to sample, vibration shell-broken effect for sample is best, and ultrasonic wave is vertical with microwave, increased hyperacoustic scissoring vibration field intensity, expanded hyperacoustic vibration area, there is the strong vibration of adding and make the more uniform technique effect of vibration, thereby can improve extraction efficiency; Because ultrasonic wave imports device 6 and microwave introduction device 6 is adjustable, when 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, by coordinated regulation device, control microwave introduction device first out of service, 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 when 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 improved 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, as shown in Figure 3, the extraction system that the present embodiment provides is with respect to the improvement of embodiment 1: described sample solution device 2 is the cavity of cuboid, described microwave introduction device 5 has the even number microwave entrance 51 being arranged on described sample solution device 2, and even number microwave entrance 51 distributes with maximum distance in pairs at cornerwise two ends in the space of the sample solution formation of described cavity.Two described microwave entrances 51 distribute with maximum distance in pairs at cornerwise two ends in the space of the sample solution formation of described cavity.After this imports ultrasonic wave, the microwave importing from two microwave entrances 51 intersects with ultrasonic wave respectively, and intersection point is positioned at conplane two opposite ends, after microwave and ultrasonic wave intersect, 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.
A kind of distortion as 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.
As a kind of improvement, in the present embodiment, the opening that described microwave entrance 51 is rectangular 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 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 25/12-24/13.Particularly, the described microwave entrance 51 that minor face vertically arranges is 75 millimeters near the vertical edges of the strong vertical seamed edge of the described microwave resonance being close to and the distance between this vertical seamed edge, and the described microwave entrance 51 of minor face along continuous straight runs setting is 90 millimeters near the vertical edges of the vertical seamed edge of the cavity being close to and the distance between this vertical seamed edge.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 quadrature superposition in cavity, improved field intensity, 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 have been 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, between the microwave reflecting, can form the field intensity of orthogonal superposition, further increase heating using microwave efficiency.
As a kind of 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, 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 lug boss 54c is divided into the intake tunnel being connected with water inlet 54d and the exhalant canal being connected with delivery port 54e by described annular water flowing chamber 54b.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 is as the watershed of annular water flowing chamber 54b in the present embodiment, and the shunting in order to turnover current, makes annular water flowing chamber 54b become circulation runner.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 in order to fixing standby spiral shell, to beat groove 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 bellmouths 29 are set on described disk-shaped tube 28, 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, when 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; When not needing pumping sample solution, switch valve 24 cuts out, pressure in discharge nozzle 22 increases gradually, when 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 when 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 when 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, extraction for 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, the defect that packs sample bottle into, by pumping, can understand the extraction situation of sample, reduced 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, in the gap between the adjacent baffle 33 of fluid direction of advance forefront, be not more than the 0.5-0.8 in gap between the adjacent baffle 23 at the rear of fluid direction of advance 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 exhaustive without also giving all embodiments.And the apparent variation of being extended out thus or change are still among the protection domain in the invention.