CN109420359A - A kind of ultrasound with reflux unit involves Microwave Extraction system - Google Patents

Abstract

The present invention provides Chinese medicine ultrasound and involves Microwave Extraction system, with coordinated regulation device, first warning device, the second warning device and third warning device are set on coordinated regulation device, corrdinated adjustment device controls first microwave introduction device and imports microwave, after a certain period of time, first warning device issues alarm signal to coordinated regulation device, and coordinated regulation device controls ultrasonic delivery device and imports ultrasonic wave；After after a certain period of time, the second warning device issues alarm signal to coordinated regulation device, and coordinated regulation device control microwave introduction device and ultrasonic delivery device change it and run power, and operation power is made to be respectively lower than its initial power；Third warning device issues alarm signal to coordinated regulation device after microwave introduction device and ultrasonic delivery device are with the operation power work certain time after changing, coordinated regulation device first controls microwave introduction device and stops working, and the rear ultrasonic delivery device that controls stops working.

Description

A kind of ultrasound with reflux unit involves Microwave Extraction system

Technical field

The present invention relates to a kind of ultrasounds of Chinese medicine to involve Microwave Extraction system and extraction process, belongs to Chinese medicine useful component Abstraction technique field.

Background technique

Active skull cap components in plant or Chinese medicine have wide in the fields such as medicine, food, chemical industry, cosmetics, feed Wealthy application prospect.Chinese medical concrete, the preparation of liquid extract or bioactive substance and food, cosmetics, feeding in pharmaceuticals industry The preparation of the functional additive of plant origin is required using extract equipment in material industry；In chemical industry and chemical analysis field In, the processes such as sample pre-treatments or sample preparation, chemical synthesis may also be needed using resolution, extraction equipment or reactor.

Ultrasonic wave assisted extraction and microwave radiation exaraction are extractive techniques emerging in recent years.Mesh is extracted from dried material Mark compound is roughly divided into two steps: the 1) infiltration of material, the i.e. expansion and aquation of material；2) Soluble target compound is logical Cross the mass transport process of diffusion, infiltration from material to solvent.Studies have shown that ultrasonic wave can make plant cell wall generate hole, have Conducive to the dissolution of target compound in cell, mass transport process can be promoted.In addition, ultrasonic wave can also reduce material size, from And increase the contact area of material and solvent, be conducive to the extraction of target compound.Ultrasonic wave assisted extraction have it is easy to operate, It is low in cost, extraction time is short, is easy to the advantages that amplifying production.Currently used ultrosonic extractor includes that sonde-type extracts Device and water-bath type extraction element.The former probe sphere of action is limited, is unfavorable for amplification production；The ultrasonic wave vibration that the latter generates Kinetic energy must can just be transferred to sample by medium and sample bottle, and this indirect ultrasonic wave mode of action may influence to extract effect Rate.

Microwave by intracellular polar water molecules or can be extracted material absorbing and generate amount of heat, make intracellular temperature It rises rapidly, the pressure that water vapor generates can break through cell membrane and cell wall, biggish mass transfer channel be formed, to promote mesh Mark the extraction of compound.Microwave radiation exaraction has many advantages, such as that extraction time is short, solvent usage is few, extraction efficiency is high.Often at present Microwave Extraction device includes sealed high pressure extraction tank and open atmospheric extraction device.The former is strong to extraction tank material Degree and sealing requirements are very high, and quantity of sample handling is small, and safety is poor, expensive, and need longer cooling time.The latter is past Toward Extracting temperature is not adjustable, the optimization of extraction process is affected, may cause some thermal instability targets when the temperature is excessively high Degradation.

In recent years, in order to improve extraction efficiency, the patent document that ultrasonic wave and microwave extraction technology combine is shown in not repeatly It is fresh, Chinese patent literature can make full use of the void effect of ultrasonic activation and microwave radiation not only had high energy effect but also Overcome certain deficiencies of conventional ultrasound and microwave extraction technology.Chinese patent CN2748147Y, CN1651896A.CN2773664Y.CN2822737Y, CN2880211Y disclose several ultrasonic microwave extraction elements, each to have Characteristic.

But studies have shown that existing ultrasonic wave and Microwave Extraction device often have the following problems:

When being extracted using existing above-mentioned ultrasonic microwave extraction element, over time, microwave heating action Constantly accumulation, the liquid in sample solution device are much gasified as gas, and the gas of gasification is constantly accumulated in sample solution, So that the top pressure of sample solution constantly increases, the increase of top pressure is so that the ultrasonic activation under the conditions of of the same race is imitated Fruit decline, reduces the extraction efficiency of sample.

Summary of the invention

Therefore, exist the technical problem to be solved in the present invention is that ultrasound in the prior art is overcome to involve microwave heating equipment The technological deficiency that later period extraction efficiency reduces is handled, so that providing a kind of higher ultrasound of efficiency involves Microwave Extraction system.

For this purpose, the present invention, which provides a kind of Chinese medicine ultrasound with reflux unit, involves Microwave Extraction system, including upper cover Openable closed box, the sample solution device with openable entrance being set to inside the closed box, setting Moveable microwave introduction device on the sample solution device, moveable ultrasonic delivery device further include setting For making the second reflux unit of the sample solution reflux of vaporization inside the closed box, second reflux unit has The big opening end of the taper drainage hood being inserted into inside the sample solution device, the taper drainage hood covers entire liquid level and position Near the position of sample solution device upper end more than the liquid level, the osculum end of the taper drainage hood connects condensation Pipe, the outside of the condenser pipe are socketed with circulating water flow siphunculus, and loop head is arranged on the circulating water flow siphunculus and recycles Mouthful.

The sample solution device is the cavity of cuboid, and the microwave introduction device, which has, to be arranged in the sample solution Even number microwave entrance on device, even number microwave entrance is in the cornerwise of the space that the sample solution of the cavity is formed Both ends are distributed in pairs with maximum distance.

The microwave entrance is the opening of rectangular shape or trapezoidal shape, positioned at two of the same space diagonal line both ends The short side of microwave entrance, one of microwave entrance is horizontally disposed, and the short side of another microwave entrance is along the vertical direction Setting, the microwave entrance that short side the is arranged along the vertical direction microwave entrance more horizontally disposed than short side closer to The seamed edge of the vertical direction of the sample solution device；This value of the length and width of the microwave entrance is 25/12-24/13.

The microwave introduction device further includes the introduction chamber for the trapezoid cross section connecting with the microwave entrance, the introduction chamber Osculum end connect with the microwave entrance, the junction of the two setting microwave inhibits lasso, the big mouth of the microwave introduction chamber End is connect with magnetron, and cooler is arranged on the outer wall of the magnetron, and the cooler includes that socket is mounted on the magnetic control The mounting base of tube anode, the lug boss that annular water flowing chamber is set in the mounting base and is projected upwards from the mounting base, The water outlet that the annular water flowing chamber is divided into the intake tunnel connecting with water inlet and connect with water outlet by the lug boss Channel.

It further include the first reflux being arranged in inside the closed box for making to extract halfway sample solution reflux Device, first reflux unit include being inserted in the sample solution liquid level sample solution below for that will extract to pass in and out Liquid pump, the discharge nozzle connecting with the liquid pump are mounted on the jet port in the exit of the discharge nozzle, the jet port pair Collecting tank is answered to be arranged, it further includes return pipe that the jet port, which is connected to or is disconnected with discharge nozzle by switch valve, the return pipe One end is inserted into the sample solution device, and the other end is connected to or is disconnected with discharge nozzle by check valve.

The ultrasound of Chinese medicine provided by the invention involves Microwave Extraction system, further includes being arranged in the sample solution device The disk-shaped tube for being stirred to sample solution being connected to below whole liquid levels and by connecting tube with the discharge nozzle, it is described Several bellmouths are set on disk-shaped tube, and the osculum end of the bellmouth is arranged towards liquid level；The connecting tube and the discharging One end of pipe connection is located at the inside of the sample solution device.

It further include being arranged in inside the closed box for making the second reflux unit of the sample solution reflux of vaporization, institute Stating the second reflux unit has the taper drainage hood being inserted into inside the sample solution device, the big mouth of the taper drainage hood End covers entire liquid level and is located at the liquid level or more near the position of sample solution device upper end, the taper drainage The osculum end of cover connects condenser pipe, and the outside of the condenser pipe is socketed with circulating water flow siphunculus, sets on the circulating water flow siphunculus Set loop head and loop exit.

It further include the cooling back installation being arranged between sample solution device and the closed box, cooling back installation Cooling liquid outlet be connected to the loop head, the cooling liquid inlet is connected to loop exit, the cooling back installation Including the stainless steel patch that fitting is arranged on the sample solution device outer wall, and impossible be arranged in the stainless steel patch of hanging down On several different deflectors of height, several described deflectors form wavy fluid channel, advance along fluid The height of the deflector in direction gradually decreases, and the gap between adjacent baffle is gradually increased, and is located at fluid direction of advance Gap between the adjacent baffle of forefront is not more than the gap between the adjacent baffle of fluid direction of advance rearmost 0.5-0.8 times.

It further include coordinated regulation device, the coordinated regulation device is by controlling the microwave introduction device and the ultrasound Position of the wave gatherer on the sample solution device makes the microwave introduction device micro- into sample solution device The ultrasonic delivery direction of wave importing direction and the ultrasonic delivery device into the sample solution device is orthogonal always to hang down Directly, also, on the coordinated regulation device first warning device, the second warning device and third warning device are set, extract When beginning, the corrdinated adjustment device controls the microwave introduction device and imports microwave, after a certain period of time, the first alarm dress It sets to the coordinated regulation device and issues alarm signal, the coordinated regulation device, which controls the ultrasonic delivery device and imports, to be surpassed Sound wave；After after a certain period of time, second warning device issues alarm signal to the coordinated regulation device, and the collaboration is adjusted Control device controls the microwave introduction device and ultrasonic delivery device changes it and runs power, and operation power is made to be respectively lower than it Initial power；The third warning device is in the microwave introduction device and the ultrasonic delivery device with the operation after changing Alarm signal is issued to the coordinated regulation device after power work certain time, the coordinated regulation device first controls described micro- Wave gatherer stops working, and controls the ultrasonic delivery device afterwards and stops working.

Involve the extraction process that Microwave Extraction system carries out Chinese medicine, packet using Chinese medicine ultrasound described in any of the above embodiments Include the following steps successively carried out:

Step 1: the upper cover of closed box and the entrance of sample solution device are opened, it will be pre-configured The solution of sample to be extracted be placed in the sample solution device, and close the entrance and the upper cover；

Step 2: the coordinated regulation device is opened, the coordinated regulation device controls the microwave introduction device and opens, The microwave introduction device simultaneously imports continuous microwave, the initial power of the microwave introduction device into the sample solution device For P1, after certain time t1, the first warning device of the coordinated regulation device issues alarm signal to the coordinated regulation device Number, the coordinated regulation device controls the ultrasonic delivery device after receiving the alarm signal and opens, and to the sample Ultrasonic wave is imported in product solution containment, the initial power of the ultrasonic delivery device is P2, the importing direction of the ultrasonic wave With the importing direction of microwave orthogonal vertical always, after certain time t2, the second alarm of the coordinated regulation device Device issues alarm signal, the coordinated regulation device same time control after receiving the alarm signal to the coordinated regulation device It makes the ultrasonic delivery device and the microwave introduction device reduces power, so that the power of the two is respectively smaller than its initial power Rate P1, P2, the coordinated regulation device control the ultrasonic delivery device and the microwave introduction device with the function after reducing It is out of service that the microwave introduction device is first controlled after rate operation certain time t3, is controlled the ultrasonic delivery device afterwards and is stopped Operation.

Sample solution in the step 1 is the sample solution of Reishi sporule, and time t1 is 1-3 minutes, and time t2 is 3-5 Minute, time t3 is 6-7 minutes.

Mutually this prior art has the advantage that above-mentioned technical proposal of the invention

1. Chinese medicine ultrasound provided by the invention involves Microwave Extraction system, by the way that coordinated regulation device is arranged, to ultrasound The importing time of wave and microwave, importing sequence import power and shut-in time progress strict control, and first control imports microwave, And it is imported in microwave and just starts to import ultrasonic wave after a certain period of time, this enables the heat of microwave preferably to pass to sample Solution, so that it is guaranteed that just carrying out the importing of ultrasonic wave after sample solution is heated to certain time and degree by microwave, avoiding The waste that energy is caused when ultrasonic wave and sample are not heated is imported in advance；After sample solution is heated to a certain degree, ultrasound The cavitation of wave is preferably merged with the heat effect of microwave, also, coordinated regulation device controls the importing of the ultrasonic wave The importing direction of direction and microwave is vertical, so that ultrasonic wave carries out scissoring vibration to sample, for the vibration shell-broken effect of sample Most preferably, and ultrasonic wave and microwave are vertical, increase the scissoring vibration field strength of ultrasonic wave, expand the vibration area of ultrasonic wave, With reinforcement vibration and to vibrate technical effect more evenly, so as to improve extraction efficiency；Since ultrasonic delivery fills It is adjustable for setting with microwave introduction device, when the height of sample solution is changed, the adjustable ultrasonic delivery device With position of the microwave introduction device on the sample solution device so that the importing direction energy of the ultrasonic wave and microwave Enough remain vertical, so that the use scope of this system is bigger；In addition, due to the later period in vibration, sample is likely to All by broken wall treatment, the power for controlling ultrasonic delivery device and microwave introduction device is less than initial power, can be to avoid Through entering in damaged cell wall under the active material strong effect of vibration again that mass transfer in the cell wall of broken wall goes out, mention Height extracts the extracted amount in later period；Also, the heat effect for extracting later period microwave is unobvious for the effect of extraction, passes through association It is first out of service with regulation device control microwave introduction device, energy consumption can be further decreased.

2. Chinese medicine ultrasound provided by the invention involves Microwave Extraction system, the sample solution device is the chamber of cuboid Body, the microwave introduction device have the even number microwave entrance being arranged on the sample solution device, and even number microwave enters Mouth is distributed at cornerwise both ends in the space that the sample solution of the cavity is formed with maximum distance in pairs.Microwave entrance uses The mode that even number designs in pairs, and cornerwise both ends in space that microwave entrance is formed in the cavity along sample solution Pairs of distribution, after this makes ultrasonic delivery, the microwave imported from two microwave entrances intersects with ultrasonic wave respectively, and hands over Point is located at conplane two opposite ends, and the scissoring vibration effect of ultrasonic wave is conplane after microwave intersects with ultrasonic wave Both ends respectively obtain enhancing, and enhanced diffustion effect is mutually transmitted along the plane, enhances ultrasonic wave in entire space Vibration shell-broken effect.

3. Chinese medicine ultrasound provided by the invention involves Microwave Extraction system, the microwave entrance is rectangular shape or ladder The opening of shape shape, two microwave entrances positioned at the same space diagonal line both ends, the short side of one of microwave entrance is along water Square to setting, the short side of another microwave entrance is arranged along the vertical direction, and the microwave that short side is arranged along the vertical direction enters The seamed edge of vertical direction of the mouth microwave entrance more horizontally disposed than short side closer to the sample solution device；Institute This value for stating the length and width of microwave entrance is 25/12-24/13.The present invention is using microwave incidence angle and sample solution at 0 degree Angle absorbs microwave energy by sample solution to greatest extent.Two microwave entrances are arranged by vertical and horizontal, keep microwave energy logical It crosses waveguide to penetrate after cavity, the component of the horizontal direction of leading wave field and the component of vertical direction form just be folded in the cavity Add, improve microwave field density, while making field strength distribution more uniform, sample solution is completely disposed in high-intensity microwave and can radiate In, the uniformity of microwave heating and the intensity of microwave heating are improved, test proves this kind of special designing of microwave entrance, right For the extraction of the same sample solution of same amount, in the case where being substantially reduced microwave heating time, the extraction efficiency of sample But it significantly improves；The sample solution device is the cavity of cuboid, this obtains microwave in the device to the greatest extent Reflection, so that the utilization rate of microwave is greatly improved, also, is capable of forming orthogonal superposition between reflected microwave Field strength, further increase microwave heating efficiency.

4. the ultrasound of Chinese medicine provided by the invention involves Microwave Extraction system, the microwave introduction device further includes and institute State microwave entrance connection trapezoid cross section introduction chamber, the introduction chamber be waveguide cavity, the osculum end of the introduction chamber with it is described Microwave entrance connection, so that microwave obtains concentrating enhancing when entering microwave entrance, the junction setting microwave of the two inhibits set Circle, it is therefore prevented that in the leakage of junction, the big opening end of the microwave introduction chamber connect microwave with magnetron, and magnetron is micro- in generation When wave, the anode heat of magnetron is constantly increased, by the way that cooler is arranged on the outer wall of the magnetron, for magnetron Cooled down, can to avoid the magnetron working time it is larger when, as heat be difficult to scatter and disappear and caused by burnout phenomenon.It is described cold But device includes that socket is mounted on the mounting base of the anode of magnetron, annular water flowing chamber is arranged in the mounting base and from described The annular water flowing chamber is divided into the water inlet connecting with water inlet and led to by the lug boss projected upwards in mounting base, the lug boss Road and the exhalant canal connecting with water outlet, annular mounting base is directly socketed on the magnetron, is easily installed, and pacifies Annular water flowing chamber is arranged on dress seat can make magnetron obtain comprehensive heat dissipation, be arranged in mounting base The annular water flowing chamber is divided into the intake tunnel connecting with water inlet and connect with water outlet by lug boss, the lug boss Exhalant canal, this kind design so that the structure of cooler is very compact, and cooling effect is excellent.

It further include being arranged in the closed box 5. the ultrasound of Chinese medicine provided by the invention involves Microwave Extraction system Portion is used to make to extract the first reflux unit of halfway sample solution reflux, and first reflux unit includes being inserted in sample The liquid pump of the liquid level of solution sample solution disengaging below for that will extract, the discharge nozzle being connect with the liquid pump, peace Jet port mounted in the exit of the discharge nozzle, the jet port correspond to collecting tank setting, and the jet port passes through switch valve It is connected to or disconnects with discharge nozzle, further include return pipe, one end of the return pipe is inserted into the sample solution device, another End is connected to or is disconnected with discharge nozzle by check valve.After sample solution extracts, or needed during the extraction process by sample Product solution pumps out when being detected, and opens liquid pump 2 and sample solution is pumped into the discharge nozzle, turn on the switch valve, enter Coating a part in discharge nozzle enters jet port, sprays into collecting tank from the jet port in order to collect and detect, at this point, Since the pressure in the discharge nozzle is smaller, less than the spring pressure of check valve, closed check valve, sample solution will not be by returning Flow tube flows back into sample solution device, can carry out lasting pumping；At the same time, into another portion in the discharge nozzle Solution is divided to enter in mixing component by connecting tube, and spouting from the bellmouth of mixing component, so that device bottom surface is molten Liquid is dug, and is avoided the biggish sample solution of viscosity and is difficult to the problem of pumping.When not needing pumping (such as sample solution Find that sample extraction is not thorough after detection), switch valve is closed, at this point, since liquid pump continues the pumping samples into discharge nozzle Solution, the pressure in discharge nozzle constantly increase, when the pressure in discharge nozzle is greater than the spring pressure of check valve, the check valve Flap be opened, check valve towards sample solution device inside open, the sample solution in discharge nozzle is along unidirectional Valve enters in return pipe, is back in sample solution device from the return pipe, so that sample solution carries out internal circulation, prevents Only the biggish sample solution of viscosity leads to the problem of precipitating, the vibrating effect of auxiliary ultrasonic.Sample extraction is found after retrieval When being not thorough, opens the valve below collecting tank and import the sample again so that collecting tank is connected to sample solution device It in the sample solution device, is further extracted, and the collecting tank can simultaneously serve as the entrance of sample solution. Above-mentioned design of the invention, by the pan feeding of sample solution, pumping, detection, again import and prevent precipitating effect be combined into One, when avoiding in the prior art using general bottle body as sample solution device, all in pan feeding, discharging and detection It needs from closed box to take out sample bottle just and can be carried out the technological deficiency for reducing working efficiency, and be particularly suitable for gluing Spend the extraction of biggish sample solution, meanwhile, for the extraction of the sample solution of experimental stage, due to researcher for The research of experiment condition is immature, usually will appear and extracts halfway situation, this kind design avoids frequent taking-up, is packed into The defect of sample bottle, by pumping can the extraction situation to sample understand, reduce working strength.

It further include that setting is filled in the sample solution 6. the ultrasound of Chinese medicine provided by the invention involves Microwave Extraction system The disk-shaped tube for being stirred to sample solution setting whole liquid levels or less and being connected to by connecting tube with the discharge nozzle, institute It states and several bellmouths is set on disk-shaped tube, the bellmouth is bellmouth, and the osculum end of the bellmouth is arranged towards liquid level； One end that the connecting tube is connect with the discharge nozzle is located at the inside of the sample solution device.The liquid pump is past in needs When outer pumping, play the role of pumping samples solution outward, when not needing pumping samples solution outward, by setting It sets the bellmouth on disk-shaped tube and sprays liquid level to sample solution device, thus molten to the sample in the sample solution device Liquid generates surge, plays the role of stirring, effectively prevents precipitating, and since the liquid pump one pumps dual-purpose, passes through sample The circulation of itself of solution can be carried out stirring, and not need to introduce agitating shaft, can play good anti-precipitation.It is described Bellmouth is bellmouth, and the osculum end of the bellmouth is arranged towards liquid level.Bellmouth is set as bellmouth and osculum end direction Liquid level setting, can make sample solution enter liquid level in a manner of jet stream, enhance stirring action, to improve sludge proof Effect.The mixing component of dish type setting increases mixing area, further enhances anti-sedimentation effect.

It further include being arranged in the closed box 7. the ultrasound of Chinese medicine provided by the invention involves Microwave Extraction system Portion is used to make the second reflux unit of the sample solution reflux of vaporization, and second reflux unit is molten with the sample is inserted into Taper drainage hood inside liquid device, the big opening end of the taper drainage hood cover entire liquid level and are located at the liquid level or more most Close to the position of sample solution device upper end, the large end face of taper drainage hood covers entire liquid level, and is located at the liquid More than face near the position of sample solution device upper end, so that all gas generated in microwave heating process can be into Enter in the taper drainage hood, liquid is condensed under the action of the inner wall of taper drainage hood, and flow back along taper drainage hood Into sample solution；The osculum end of the taper drainage hood connects condenser pipe, and the outside of the condenser pipe is socketed with circulating water flow Siphunculus, the portion gas that can not be condensed by the inner wall of taper drainage hood are entered cold by a bite end of taper drainage hood In solidifying pipe, the cooling effect by circulating water flow siphunculus for condenser pipe, the portion gas is condensed in condenser pipe, flows back into In sample solution.

8. the ultrasound of Chinese medicine provided by the invention involves Microwave Extraction system, the cooling liquid outlet of cooling back installation with Loop head connection, the cooling liquid inlet be connected tos with loop exit, that is, the liquid that is used to flow back cooling and are used for sample The outer wall of product solution containment carries out cooling cooling back installation and is interconnected, so that above-mentioned two cooling system of the invention The cooling capacity of system is reused, and energy consumption is reduced, also, reduces the quantity of the extraneous chilled water system of this system, so that knot Structure is more compact；It is led and for the ease of rear circulating cooling liquid for the pressurization of front circulating cooling, described in several Flowing plate forms wavy fluid channel, gradually decreases along the height of the deflector of fluid direction of advance, adjacent guide Gap between plate is gradually increased, and the gap between the adjacent baffle of fluid direction of advance forefront, which is not more than, is located at stream 0.5-0.8 times of gap between the adjacent baffle of body direction of advance rearmost.

9. the ultrasound of Chinese medicine provided by the invention involves Microwave Extraction technique, because using extraction described in any of the above embodiments System and have the advantages that described in any of the above embodiments.

Detailed description of the invention

In order to make the content of the present invention more clearly understood, it below according to specific embodiments of the present invention and combines Attached drawing, the present invention is described in further detail, wherein

Fig. 1 is the structural schematic diagram that the ultrasound that the embodiment of the present invention 1 provides involves Microwave Extraction system；

Fig. 2 is the coordinated regulation device of extraction system and being electrically connected for whole system that the embodiment of the present invention 1 provides Schematic diagram；

Fig. 3 is setting side of the microwave entrance for the extraction system that the embodiment of the present invention 2 provides on sample solution device The structural schematic diagram of formula；

Fig. 4 is the structural schematic diagram of the cooler of the magnetron for the extraction system that the embodiment of the present invention 3 provides；

Fig. 5 is the installation of the first reflux unit and sample solution device for the extraction system that the embodiment of the present invention 4 provides Schematic diagram；

Fig. 6 is the structural schematic diagram for the disk-shaped tube that the embodiment of the present invention 4 provides；

Fig. 7 is the structural schematic diagram of the cooling back installation for the extraction system that the embodiment of the present invention 5 provides.

Appended drawing reference indicates in figure are as follows: 1- closed box, 2- sample solution device；20- collecting tank；21- liquid pump；22- Discharge nozzle；23- jet port；24- switch valve；25- return pipe；26- check valve；27- connecting tube；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 enters Mouthful；52- introduction chamber；53- magnetron；54- cooler；54a- mounting base；54b- annular water flowing chamber；54c- lug boss；54d- into The mouth of a river；54e- water outlet；54f- outer ring；54k- notch；54h- passage gaps；6- ultrasonic delivery device；7- coordinated regulation dress It sets；70-PLC；The first warning device of 71-；The second warning device of 72-；73- third warning device；81- taper drainage hood；82- is cold Solidifying pipe；83- circulating water flow siphunculus；84- loop head；85- loop exit；10- motor.

Specific embodiment

Embodiment 1

As shown in Figure 1, embodiment, which provides a kind of ultrasound extracted for Chinese medicine or active substance of plant, involves microwave Extraction system, including the openable closed box 1 of upper cover, being set to inside the closed box 1 has openable entrance Sample solution device 2, between the sample solution device 2 and the cabinet 1 and be bonded the sample solution device 2 The cooling back installation 3 with cooling liquid inlet 31 and cooling liquid outlet 32 of side wall setting further includes being arranged in the sample Moveable microwave introduction device 5 on solution containment 2, moveable ultrasonic delivery device 6 and coordinated regulation device 7, The coordinated regulation device 7 includes PLC controller 70 and can be with PLC controller 70, microwave introduction device 5 and ultrasound waveguide Enter the first warning device 71, the second warning device 72, third warning device 73 of 6 feedback operation of device, here, first report Alarm device 71, the second warning device 72 and third warning device 73 have time meter for what those skilled in the art generallyd use The signalling means of number function.

In the present embodiment, the microwave introduction device 5 includes the magnetron 53 for generating microwave, for conducting the magnetic control The introduction chamber 52 for the microwave that pipe 53 generates, the introduction chamber 52 are trapezoid cross section, and wherein big opening end is connect with magnetron 53, osculum End is connected to microwave entrance 51, and the microwave entrance 51 is arranged in the upright side walls of the sample solution device 2, which enters Mouth 51 is oblong openings, and the importing direction and liquid level which makes microwave are in zero degree angle, so that sample solution Farthest it is heated.The ultrasonic delivery device 6 is located at the bottom of the sample solution device 2, the importing of ultrasonic wave The importing direction of direction and microwave is substantially vertical, so that microwave heating action generates the shearing shell-broken effect of ultrasonic wave Huge positive influence, substantially increases ultrasonic wave for the destruction efficiency of sample cell wall.

As a preference, the importing direction of the ultrasonic wave and the microwave is orthogonal vertical, at this point, microwave heating is made With can not only aggravate the shearing shell-broken effect of ultrasonic wave, and it is possible to biggish superposition broken wall field strength be generated, convenient for promoting to break The uniform progress of wall.

In order to control the microwave introduction device 5 and ultrasonic delivery device 6 leading on the sample solution device 2 Entering position, several microwave entrances 51 are arranged in the same side of the sample solution device 2, meanwhile, which passes through moveable Baffle (not shown) is connect with the microwave introduction device 5, mobile when needing to import microwave to a certain microwave entrance 51 The baffle makes the baffle not block the microwave entrance 51, and when needing to change the entrance for importing microwave, the mobile baffle makes It obtains baffle to block the entrance for not needing to import microwave, adjustment of the baffle for microwave entrance 51 so can be realized, in this reality It applies in example, the movement of the baffle realizes electrodeless adjustment by screw.In the present embodiment, in order to realize to the ultrasound waveguide The control for entering the importing position of device 6, on the side wall of the installation ultrasonic delivery device 6 of the sample solution device 2 Guide-track groove (not shown) is set, is provided with the side wall to match with the guide-track groove on the ultrasonic delivery device 6, it will The side wall is embedded in the guide-track groove, and the ultrasonic delivery device 6 can be realized in the sample solution device 2 by sliding On movement, to change the ultrasonic activation orientation of ultrasonic delivery device 6.

In the present embodiment, described super in order to realize the Collaborative Control to ultrasonic delivery direction and microwave importing direction Displacement sensor (not shown), the displacement sensing are respectively set on sound wave gatherer 5 and the microwave introduction device 6 Device is connect with the PLC controller 70 of the coordinated regulation device 7, can to the PLC controller 70 transmit displacement signal and It is moved at preset position when receiving the action order of PLC controller 70.

In the present embodiment, the meaning of the cooling back installation setting is: system generates a large amount of after working long hours Heat, heat can not shed the service life for the system that influences, by the sample solution device 2 and the closed box 1 Gap in cooling back installation 3 is set, system can not only be worked in the amount of heat that generates scatter and disappear, circulating cooling is filled Setting 3 and being arranged between can make system more compact, when work, import coolant liquid, coolant liquid from cooling liquid inlet 31 So that the heat of system is cooled, liquid band is walked for conduction for cooling capacity, is finally discharged from cooling liquid outlet 32, so that system The heat of (especially sample solution device 2) is dissipated, and the service life of system is improved.

Packet when being extracted using the active material that above-mentioned ultrasound provided in this embodiment involves Microwave Extraction system progress sample Include following processing step:

Step 1: opening the upper cover of closed box 1 and the entrance of sample solution device 2, will be pre-configured with The solution of good sample to be extracted is placed in the sample solution device 2, and closes the entrance and the upper cover；

Step 2；The coordinated regulation device 7 is opened, as shown in Fig. 2, the PLC controller 70 of the coordinated regulation device 7 Signal is sent to the microwave introduction device 5 and the first warning device 71 first, the microwave introduction device 5 is receiving the letter Immediately with initial power P1 start-up operation after number, meanwhile, first warning device 71 starts to carry out after receiving the signal Time counting, after time t1, first warning device 71 sends alarm signal, the PLC control to the PLC controller Device 70 processed sends working signal to the ultrasonic delivery device 6 after being connected to the alarm signal, and simultaneously to described second Warning device 72 sends working signal, and the ultrasonic delivery device 71 is after receiving the working signal immediately with initial power P2 starts to work, and second warning device 72 starts to carry out time counting after receiving working signal, after time t2, Second warning device 72 to the PLC controller 70 send signal, the PLC controller after receiving the signal simultaneously The signal for changing operating power is sent to the microwave introduction device 5 and the ultrasonic delivery device 6, and is alarmed and filled to third 73 transmission working signals are set, the microwave introduction device 5 and the ultrasonic delivery device 6 change respectively after receiving the signal Its operating power, so that operating power is respectively smaller than its initial power P1, P2, the third warning device 73 is receiving the work Start to carry out time counting after signal, after time t3, the third warning device 73 is sent to the PLC controller 70 to be believed Number, the PLC controller 70 first controls the microwave introduction device 5 after receiving the signal and stops working, and controls institute afterwards Ultrasonic delivery device 6 is stated to stop working.

The said extracted system of the present embodiment, realized by coordinated regulation device 7 to the microwave introduction device 5 and The job order of the ultrasonic delivery device 6, the working time, operating power and stopping sequence comprehensively control.First control Import microwave, and microwave import after a certain period of time just start import ultrasonic wave, this enable microwave heat preferably Sample solution is passed to, so that it is guaranteed that just carrying out ultrasonic wave after sample solution is heated to certain time and degree by microwave It imports, avoids the waste for importing cause energy when ultrasonic wave and sample are not heated in advance；Sample solution is heated to centainly After degree, the cavitation of ultrasonic wave is preferably merged with the heat effect of microwave, also, coordinated regulation device 7 control it is described The importing direction of ultrasonic wave and the importing direction of microwave are vertical, so that ultrasonic wave carries out scissoring vibration to sample, for sample It is best to vibrate shell-broken effect, and ultrasonic wave and microwave are vertical, increase the scissoring vibration field strength of ultrasonic wave, expand ultrasonic wave Vibration area, have and reinforce vibration and to vibrate technical effect more evenly, so as to improve extraction efficiency；Due to super Sound wave gatherer 6 and microwave introduction device 6 be it is adjustable, it is adjustable described super when the height of sample solution is changed Position on sample solution device 2 described in 6 microwave introduction device 5 of sound wave gatherer, so that the ultrasonic wave and microwave Importing direction can remain vertically so that the use scope of this system is bigger；In addition, due to the later period in vibration, sample Product are likely to all by broken wall treatment, and the power for controlling ultrasonic delivery device and microwave introduction device is less than initial power Rate can enter under strong effect of vibration again broken to avoid the active material gone out from mass transfer in the cell wall of broken wall In the cell wall of damage, the extracted amount for extracting the later period is improved；Also, extract later period microwave heat effect for extraction effect It is first out of service by coordinated regulation device control microwave introduction device through unobvious, energy consumption can be further decreased.

It should be noted that when carrying out the extraction of bioactive substance using said extracted system provided in this embodiment, Operation power after the time t1, t2, t3, initial power P1, P2 and change can be carried out according to the different material of extraction Change, above-mentioned numerical value is pre-set according to the different material of extraction when extraction work starts.In the present embodiment, above-mentioned Extraction system is for the extraction to Reishi sporule, and wherein time t1 is 1-3 minutes, and time t2 is 3-5 minutes, and time t3 is 2-3 Minute, so that entire extraction time controlled in 6-11 minutes, extraction efficiency is substantially increased, initial power P1 is 50-200W, initial power P2 are 50-100W, greatly reduce energy consumption.

Embodiment 2

The present embodiment provides a kind of ultrasounds to involve Microwave Extraction system, is the deformation on 1 basis of embodiment, such as schemes Shown in 3, extraction system provided in this embodiment is relative to the improvement of embodiment 1: the sample solution device 2 is cuboid Cavity, the microwave introduction device 5 has the even number microwave entrance 51 that is arranged on the sample solution device 2, even number A microwave entrance 51 is distributed at cornerwise both ends in the space that the sample solution of the cavity is formed with maximum distance in pairs.Two A microwave entrance 51 is divided at cornerwise both ends in the space that the sample solution of the cavity is formed with maximum distance in pairs Cloth.After this makes ultrasonic delivery, the microwave imported from two microwave entrances 51 intersects with ultrasonic wave respectively, and intersection point is located at Conplane two opposite ends, the scissoring vibration effect of ultrasonic wave is at conplane both ends point after microwave intersects with ultrasonic wave Do not enhanced, and enhanced diffustion effect is mutually transmitted along the plane, enhances vibration of the ultrasonic wave in entire space Shell-broken effect.

As a kind of deformation of the present embodiment, the microwave entrance 51 may be arranged as other numbers, such as 4,6 A, 8 etc. even number numbers, cornerwise both ends in the space that even number microwave entrance 51 is formed along sample solution are with farthest Distance distribution in pairs.

As an improvement in the present embodiment, the microwave entrance 51 is the opening of rectangular shape, it is located at same sky Between diagonal line both ends two microwave entrances 51, the short side of one of microwave entrance 51 is horizontally disposed, another is micro- The short side of wave entrance 51 is arranged along the vertical direction, this short side of the microwave entrance 51 that short side is arranged along the vertical direction is along level side To setting the microwave entrance 51 closer to the sample solution device 2 vertical direction seamed edge；The microwave entrance 51 Length and width this value be 25/12-24/13.Specifically, the microwave entrance 51 that short side is arranged along the vertical direction is close The strong vertical seamed edge of the neighbouring microwave resonance vertical edges and the distance between the vertical seamed edge be 75 millimeters, and short side Vertical edges and the vertical seamed edge of the horizontally disposed microwave entrance 51 close to the vertical seamed edge of neighbouring cavity The distance between be 90 millimeters.The length of the microwave entrance 51 is 250 millimeters, and width is 130 millimeters, the inside of the cavity With sample solution, the liquid level of the sample solution is 120 millimeters at a distance from the upper wall of the cavity.

Above-mentioned ultrasound provided in this embodiment involves Microwave Extraction system, microwave incidence angle and sample solution into 0 degree of angle, Absorb microwave energy by sample solution to greatest extent.Two microwave entrances 51 are arranged by vertical and horizontal, pass through microwave energy Waveguide penetrates after cavity, and the component of the horizontal direction of leading wave field and the component of vertical direction form just be folded in the cavity Add, improve field strength, while making field strength distribution more uniform, sample solution is completely disposed in during high-intensity microwave can radiate, and is mentioned The high uniformity of microwave heating and the intensity of microwave heating, test proves this kind of special designing of microwave entrance, for same For the extraction for measuring same sample solution, in the case where being substantially reduced microwave heating time, the extraction efficiency of sample is bright It is aobvious to improve；The sample solution device is the cavity of cuboid, this reflects microwave to the greatest extent in the device, So that the utilization rate of microwave is greatly improved, also, the field of orthogonal superposition is capable of forming between reflected microwave By force, microwave heating efficiency is further increased.

As a kind of deformation of the present embodiment, the microwave entrance 51 can also be the opening of trapezoidal shape.

Embodiment 3

The present embodiment provides a kind of ultrasounds to involve Microwave Extraction system, is the deformation on embodiment 1 or 2 bases, In the present embodiment, as shown in figure 4, the microwave introduction device 5 include magnetron 53, excitation system, feedback system (in figure not Show) and cooler 54.53 output frequency of magnetron is 2450MHz, exports mean power 6kW, peak power output 10kw.It encourages Magnetic system has two groups, and one group is the included electromagnetism iron wire packet of magnetron, another group be by enameled wire around the electricity covered in magnetron Coil outside magnet wire packet, this two parts have special field power supply, and the electromagnetic electric current in electromagnetism iron wire packet is 8.0A or so, And the size of electric current can be adjusted by coordinated regulation device 7 in additional coil.Feedback system has two parts, and a part is by anode electricity Stream, which is input in one section of coil being wound in magnet exciting coil, to be fed back, and another part designs a sampling resistor and connects in magnetron In anode loop, anode current information is provided.The cooler 54 includes the installation that socket is mounted on 53 anode of magnetron The lug boss that annular water flowing chamber 54b is set and is projected upwards from the mounting base 54a on mounting base 54a described in seat 54a 54c, the lug boss 54c by the annular water flowing chamber 54b be divided into the water inlet 54d intake tunnel connecting and with water outlet The exhalant canal of mouth 54e connection.Depending on the specific size of cooler 54 is by the size of magnetron 53.

In the present embodiment, the cooler 54 is the integral piece using extrusion forming, so that the cooler 54 Leakproofness is best.Outer ring 54f is set on the outer wall of the annular water flowing chamber 54b, the outer ring 54f is used to install cooling gas, For radiating to the liquid in annular water flowing chamber 54b.

Lug boss 54c is made as the watershed of annular water flowing chamber 54b with the shunting of benefit disengaging water flow in the present embodiment Annular water flowing chamber 54b becomes circulation runner.Lug boss 54c is corresponding with annular water flowing chamber 54b to be gone out to form passage gaps 54h, Effect is that whole circumference in annular water flowing chamber 54b is made to have water to flow through to export heat, keeps the heat dissipation of 53 anode peripheral wall of magnetron equal It is even.The inner hole of cooler 54 and the outer diameter of anode of magnetron are interference fitted.In the present embodiment, the lateral margin of the mounting base 54a Upper setting U-lag mouth beats slot to fixed spare spiral shell when effect is for cooler installation, magnetron quilt after installing it It is fixed in frame.

Embodiment 4

The present embodiment provides a kind of ultrasounds to involve Microwave Extraction system, is the change on embodiment 1 or 2 or 3 bases Shape, in the present embodiment, as shown in figure 5, the extraction system further includes being arranged inside the closed box 1 for making to extract First reflux unit of halfway sample solution reflux, first reflux unit include being inserted in sample solution liquid level or less For that will extract sample solution disengaging liquid pump 21, for driving the motor 10 of liquid pump 21, with the liquid pump The discharge nozzle 22 of 21 connections is mounted on the jet port 23 in the exit of the discharge nozzle 22, the corresponding collecting tank of the jet port 23 The lower end of 20 settings, the collecting tank 20 is connected to or is disconnected with sample solution device 2 by valve, and the jet port 23 is by opening It closes valve 24 to be connected to or disconnect with discharge nozzle 22, further includes return pipe 25, it is molten that one end of the return pipe 25 is inserted into the sample In liquid device 2, the other end is connected to or is disconnected with discharge nozzle 22 by check valve 26.It further include that setting is filled in the sample solution The dish type for being stirred to sample solution setting 2 whole liquid levels or less and being connected to by connecting tube 27 with the discharge nozzle 22 Pipe 28, several bellmouths 29 are arranged on the disk-shaped tube 28, and the osculum end of the bellmouth is arranged towards liquid level；The connection One end that pipe 27 is connect with the discharge nozzle 22 is located at the inside of the sample solution device 2.

It is worth noting that, the check valve 26 in the present embodiment is a kind of check valve of spring, basic work is former Reason is, when switch valve 24 is opened, the pressure of spring is greater than the pressure in the discharge nozzle 22, and the flap of check valve 26 is closed, Sample solution in discharge nozzle 22 not can enter in the return pipe 25, at this point, carrying out the normal pumping of sample solution；When being not required to When wanting pumping samples solution, switch valve 24 is closed, and the pressure in discharge nozzle 22 is gradually increased, when the pressure in discharge nozzle 22 is greater than When spring pressure, the flap of check valve 26 is opened, so that the inside of check valve towards the sample solution device 2 is beaten It opens, at this point, the liquid of discharge nozzle 22 enters in the return pipe 25 along check valve 26, and is back to the sample solution device In 2.

It should be noted that its setting purpose of the check valve referred in the present embodiment essentially consists in release, and can be in institute Opening when switch valve 24 is closed is stated, so that the sample in discharge nozzle 22 enters in return pipe 25 and is back to sample solution device 2 It is interior；And when the switch valve 24 is opened, the check valve 26 is closed, and the sample solution in discharge nozzle 22 is from the jet port 23 It is injected into collecting tank 20, sample solution is collected or detected in collecting tank 20, if discovery sample solution does not have after sensing There is extraction then to open the valve between collecting tank 20 and sample solution device 2 completely, so as to come back to sample molten for sample solution In liquid device, for realizing for this main purpose, the specific setting of the check valve can be multiplicity, in addition to this implementation Except the spring check valve that example refers to, and can be set to gravity-held check valve, swing type check valve etc..

The above-mentioned design of the present embodiment by the pan feeding of sample solution, pumping, detection, imports and prevents again precipitating Effect is combined as a whole, avoid in the prior art using general bottle body as sample solution device when, pan feeding, discharge with And it requires from closed box to take out sample bottle just when detection and can be carried out the technological deficiency for reducing working efficiency, and is outstanding It is suitable for the extractions of the biggish sample solution of viscosity, meanwhile, for the extraction of the sample solution of experimental stage, due to grinding It is immature for the research of experiment condition to study carefully personnel, usually will appear and extract halfway situation, this kind design avoids frequently Taking-up, be packed into sample bottle defect, by pumping can the extraction situation to sample understand, reduce working strength.

Embodiment 5

The present embodiment provides a kind of ultrasounds to involve Microwave Extraction system, is on embodiment 1 or 2 or 3 or 4 bases Deformation, in the present embodiment, the cooling liquid outlet 32 of the cooling back installation 3 is connected to the loop head 84, described cold But liquid import 31 is connected to loop exit 85, and the cooling back installation 3 includes that fitting is arranged outside the sample solution device 2 Stainless steel patch on wall, and several deflectors 33 being vertically set on the stainless steel patch are led described in several Flowing plate 33 forms wavy fluid channel, as shown in fig. 7, the gap along fluid direction of advance, between adjacent baffle 33 It is gradually increased, the gap between the adjacent baffle 33 of fluid direction of advance forefront, which is not more than, is located at fluid direction of advance 0.5-0.8 times of gap between the adjacent baffle 23 of rearmost.

As further improvement of this embodiment, the height of several deflectors 33 can be set to height it is different, and Height positioned at the deflector 33 of the same side is gradually decreased along the flow direction of fluid.

Embodiment 6

The present embodiment provides a kind of ultrasounds to involve Microwave Extraction system, is on embodiment 1 or 2 or 3 or 4 or 5 bases On further improvement, in the present embodiment, as shown in Figure 1, further including being arranged inside the closed box 1 for making to vaporize Sample solution reflux the second reflux unit, second reflux unit have is inserted into inside the sample solution device Taper drainage hood 81, the big opening end of the taper drainage hood 81 cover entire liquid level and are located at the liquid level or more near described The position of 2 upper end of sample solution device, the osculum end of the taper drainage hood 81 connect condenser pipe 82, the condenser pipe 82 it is outer Portion is socketed with circulating water flow siphunculus 83, and loop head 84 and loop exit 85 is arranged on the circulating water flow siphunculus 83.

Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or It changes still within the protection scope of the invention.

Claims (2)

1. a kind of ultrasound with reflux unit involves Microwave Extraction system, including the openable closed box of upper cover (1), setting In the internal sample solution device (2) with openable entrance of the closed box (1), setting is filled in the sample solution Set the moveable microwave introduction device (5) on (2), moveable ultrasonic delivery device (6), it is characterised in that: further include The second reflux unit for making the sample solution reflux of vaporization, second reflux are set inside the closed box (1) Device has the taper drainage hood (81) being inserted into inside the sample solution device, the big opening end of the taper drainage hood (81) It covers entire liquid level and is located at the liquid level or more near the position of sample solution device (2) upper end, the taper is drawn The osculum end of stream cover (81) connects condenser pipe (82), and the outside of the condenser pipe (82) is socketed with circulating water flow siphunculus (83), institute It states and loop head (84) and loop exit (85) is set on circulating water flow siphunculus (83)；The ultrasound with reflux unit involves Microwave Extraction system further include setting inside the closed box (1) for making to extract the of halfway sample solution reflux One reflux unit, first reflux unit include being inserted in the sample solution liquid level sample solution below for that will extract The liquid pump (21) of disengaging, the discharge nozzle (22) connecting with the liquid pump (21), is mounted on the outlet of the discharge nozzle (22) The jet port (23) at place, the jet port (23) corresponding collecting tank (20) setting, the lower end of the collecting tank (20) passes through valve It is connected to or disconnects with sample solution device (2), the jet port (23) connects on-off by switch valve (24) and discharge nozzle (22) It opens, further includes return pipe (25), one end of the return pipe (25) is inserted into the sample solution device (2), and the other end is logical Check valve (26) is crossed to be connected to or disconnect with discharge nozzle (22).

2. the ultrasound according to claim 1 with reflux unit involves Microwave Extraction system, it is characterised in that: further include The disk for being arranged below the whole liquid levels of the sample solution device (2) and being connected to by connecting tube (27) with the discharge nozzle (22) Shape pipe (28), is arranged several bellmouths (29) on the disk-shaped tube (28), and the osculum end of the bellmouth (29) is towards liquid level Setting；One end that the connecting tube (27) connect with the discharge nozzle (22) is located at the inside of the sample solution device (2).