CN104759112A - Extracting assembly for bioactive substances and ultrasonic-microwave combined extracting method - Google Patents
Extracting assembly for bioactive substances and ultrasonic-microwave combined extracting method Download PDFInfo
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Abstract
The invention discloses an extracting assembly for bioactive substances and an ultrasonic-microwave combined extracting method, and belongs to the bioactive substance extracting technology. The extracting assembly is formed by connecting two or three of an ultrasonic-microwave extracting unit, an ultrasonic extracting unit and a microwave extracting unit in series. The extracting assembly is high in integration degree, small in occupied space and capable of realizing ultrasonic-microwave modularization, the microwave head and the ultrasonic head are separated in space, so that mutual interferences between the ultrasonic and the microwaves are reduced, and work can be simultaneously or independently performed according to the material properties; on the condition that the quantity or power of the microwave heads is not increased, the complete processing of an extracting feed liquid by microwaves is achieved without a dead corner, so that a few materials can be processed, and a large number of materials can be processed; a microwave processing mode in the prior art is changed into a short-time mobile continuous processing mode, so that bioactive substances sensitive to heat can be effectively protected.
Description
Technical field
The invention belongs to bioactivator extractive technique.
Background technology
In bioactivator extraction, large quantity research display, ultrasonic extraction and Microwave Extraction have many-sided advantage.
Ultrasonic have: 1. mechanical effect.Hyperacoustic mechanism can facilitate the dispersion of the emulsification of liquid, the liquefaction of gel and solid.2. cavitation.Ul-trasonic irradiation can produce a large amount of minute bubbles when liquid.A reason is that in liquid, local occurs tension and forms negative pressure, and the reduction of pressure makes the dissolved gas supersaturation being originally dissolved in liquid, and from liquid effusion, becomes minute bubbles; Another reason is that powerful tension " tears " a cavity liquid, is called cavitation.Being liquid vapors or the another kind of gas being dissolved in liquid in cavity, may be even vacuum.The minute bubbles formed because of cavitation constantly can move with the vibration of surrounding medium, grow up or vanish suddenly.When vanishing, surrounding liquid pours bubble suddenly and produces high temperature, high pressure, produces shock wave simultaneously.Rub and can form electric charge in accompanying with cavitation, and produce luminescence phenomenon in the electric discharge of bubble internal cause.The technology of carrying out ultrasonic process is in a liquid mostly relevant with cavitation.3. fuel factor.Because ultrasonic frequency is high, energy is large, can be produced significant fuel factor by during Absorption of Medium.4. chemical effect.Hyperacoustic effect can impel generation or accelerate some chemical reaction.
The principle of microwave abstracting: 1. microwave process is that frequency electromagnetic waves penetrates the arrival microtubule fasolculus of internal batch of (biology) spe medium and the process of glandular cell's system.Owing to absorbing microwave energy, the temperature of cell interior will rise rapidly, thus the ability making the pressure of cell interior exceed cell wall expansion to can bear, result cell rupture, active ingredient in it freely flows out, and is dissolved at a lower temperature in spe medium.2. the speed that the molecule that the electromagnetic field that microwave produces can accelerate to be extracted component is spread to solid liquid interface by solid interior.3. because the frequency dependence of micro-wave frequency and molecule rotation connects, therefore microwave energy is a kind of rotation by Ion transfer and dipole and causes the non-ionising radiation energy of molecular motion, when it acts on a point period of the day from 11 p.m. to 1 a.m, molecule rotation can be promoted, if molecule has certain polarity, instantaneous polarization can be produced under the effect of microwave field, and do reversal campaign with the speed of 24.5 hundred million times/s, thus produce key vibration, tear and interparticle friction and collision, and produce a large amount of heat energy rapidly, impel cell rupture, cellular content is overflowed and diffuses in solvent.
Although, there are some problems in ultrasonic or Microwave Extraction device existing single on market.Such as fixed ultrasonic head limits the adaptation to the change of material treating capacity of device.Such as name is called the Chinese patent (ZL200520001353.X) of " ultrasonic extraction device " again, owing to carrying out Agitation and mixing by gas to material, may be different to the mixture homogeneity of different material, thus the material extraction efficiency different to proportion can be different.What prior art had is located at ultrasonic head or microwave head on extractor outer wall, or is located at extractor center of inside, and such one is complex structure, and circuit distribution is wide, and terminal is many, repairs and change element trouble; Two is have requirement to volume of material, if material can not cover ultrasonic in tank or microwave head less completely, and operation of just can not starting shooting.Also have one be Vltrasonic device to be linear array, short then several meters, long then tens meters, such extraction system takes up space too greatly, and comprehensive cost is high.
In ultrasonic-microwave combination extraction, existing three kinds of products in the market: the CW-2000 type that Shanghai Xintuo Analytical Instruments Technology Co.ltd produces and CW-2000A type, its microwave power 10-800W (adjustable arbitrarily); Frequency 2450MHz; Ultrasonic power/frequency is 50W/40KHz; Sample accommodating: standard configuration 100mL, 250mL, 500mL.A kind of furnace chamber volume is had to be the CW-2000A type of 65L in addition.Its microwave power and ultrasonic power/frequency are also the same with CW-2000 type, and just maximum sample amount is increased to 1000ml.Therefore, this comprehensive extraction element is only suitable for doing laboratory sample process.Also has the ultrasonic microwave composite reaction system of Nanjing Xian Ou instrument manufacturing Co., Ltd and Nanjing, Nanjing following current Instrument Ltd..Microwave power is 0-900W to 0-3500W, and microwave power is 0-700 to 0-5000W.Treating capacity is that 0.5-500ml arrives maximum 1-12L.Therefore, said system is laboratory sample process or 10L level treating capacity.Suitability for industrialized production cannot be used for.
Application number is propose in the Chinese patent document of 201010116211.3 " a kind of ultrasound/microwave continuous countercurrent extraction device and method thereof ", and its device is setting arranged in a straight line, and ultrasonic and microwave portions has larger space interval, and device takes up room larger.
Application number be 200610114487.1 Chinese patent document in propose " a kind of method of integrated extraction and isolation Effective Component of Chinese Medicine and device ", essential core component is expansion bed, although mentioned the one in extractor, ultrasonic extraction device, Microwave Extraction device and the semi-bionic extraction method device that extraction element is band heating jacket in literary composition, do not provide any structure of ultrasonic-microwave device; In addition, from embodiment, the extraction sample size done, from 5g to 50g, can not carry out industrialized extraction.
Application number is the Chinese patent document " a kind of Chinese medicine ultrasonic and Microwave Extraction system " announced of 201410277304.2, without agitating device; The material of fixed volume can only be processed; Need external cooling device; Flexibility is lacked to the Volume Changes of material handling.
Publication number is " resonance device that microwave/ultrasonic composite reinforced sample is cleared up/extracted " that the Chinese patent document of CN1651896A is announced; Microwave head and ultrasonic head are concentrated in a drum, can process sample simultaneously, but process in batches only.Publication number is the one Microwave Extraction device capable of circulation that the Chinese patent document of CN2822737Y is announced; microwave generator scatters in different directions in metal coating shell, but exist microwave to other generators produce point discharge and to nonmetallic materials accessory heat and the possibility of causing danger.Publication number is that the Chinese patent document of CN2880211 discloses can quantity-produced microwave and ultrasonic extraction device, but does not mention microwave and ultrasonic actual installation structure.
Publication number is triple-frequency ultrasonic extraction device and the using method thereof of the Chinese patent document announcement of CN100479898C, the ultrasonic probe of different frequency is adopted to be fixed in the hexahedron vibrator of extractor central authorities, although can produce the ultrasonic vibration of different frequency like this, the ultrasonic vibration of different frequency simultaneously also can offset a part the ability of ultrasonic shake plate.In addition, Vltrasonic device requires to be immersed in material liquid, and such fixed volume pattern just cannot process the tailing of small size.
Summary of the invention
The object of the invention is the shortcoming overcoming prior art, a kind of extraction assembly and ultrasonic-microwave combination extraction process of bioactivator are provided.
The present invention extracts assembly by ultrasonic-Microwave Extraction unit, and in ultrasonic extraction unit and Microwave Extraction unit two or three is in series,
The structure of ultrasonic extraction unit is: by a left side, right ultrasonic shake plate and front and back wallboard are encircled into a vertical material cavity, this material cavity is again by the central longitudinal dividing plate in it and one or more diaphragm plate be separated into multiple extraction cell be close to up and down, the Flow of Goods and Materials hole that material can be allowed to flow through each extraction cell is from top to bottom had on the relevant position of midfeather and diaphragm plate, one of feed pipe and the top is extracted cell and is connected, the mouth of pipe rises to the discharge nozzle of material cavity upper position and of bottom and extracts cell and connect (this design is in order to ensure it is completely fluid material in chamber when opening ultrasonic system), ultrasonic shake plate is provided with ultrasonic head at the correspondence position of each extraction cell,
The structure of Microwave Extraction unit is: be provided with two or more microwave cavity in a vertical housing, microwave head is provided with in microwave cavity, microwave cavity surrounding establishes Flow of Goods and Materials chamber, the wall in Flow of Goods and Materials chamber has and material can be allowed to flow through each Flow of Goods and Materials chamber from top to bottom and the Flow of Goods and Materials hole of microwave leakage can be prevented, feed pipe is established in the Flow of Goods and Materials chamber at top, the Flow of Goods and Materials chamber of bottom establishes the mouth of pipe to rise to the discharge nozzle (this design is in order to ensure when opening microwave system to be completely fluid material in chamber) of housing upper position, discharge nozzle exit is provided with temperature sensor,
The structure of ultrasonic-Microwave Extraction unit is: be provided with two or more microwave cavity in a vertical housing, microwave head is provided with in microwave cavity, microwave cavity surrounding establishes Flow of Goods and Materials chamber, the wall in Flow of Goods and Materials chamber has and material can be allowed to flow through each Flow of Goods and Materials chamber from top to bottom and the Flow of Goods and Materials hole of microwave leakage can be prevented, feed pipe is established in the Flow of Goods and Materials chamber at top, the Flow of Goods and Materials chamber of bottom establish the mouth of pipe rise to housing upper position discharge nozzle (this design in order to ensure open ultrasonic-microwave system time chamber in be completely fluid material), discharge nozzle exit is provided with temperature sensor, ultrasonic head and ultrasonic shake plate is established between Flow of Goods and Materials chamber and inner walls,
The inventive method is:
The device used comprises extraction assembly, this extraction assembly is by ultrasonic-Microwave Extraction unit, in ultrasonic extraction unit and Microwave Extraction unit two or three is in series, include the first material in addition and store blending tank and the second material storage blending tank, EGR, heater, cooling device, press filtration device and switch board;
The structure of ultrasonic extraction unit is: by a left side, right ultrasonic shake plate and front and back wallboard are encircled into a vertical material cavity, this material cavity is again by the central longitudinal dividing plate in it and one or more diaphragm plate be separated into multiple extraction cell be close to up and down, the Flow of Goods and Materials hole that material can be allowed to flow through each extraction cell is from top to bottom had on the relevant position of midfeather and diaphragm plate, one of feed pipe and the top is extracted cell and is connected, the mouth of pipe rises to the discharge nozzle of material cavity upper position and of bottom and extracts cell and connect (this design is in order to ensure it is completely fluid material in chamber when opening ultrasonic system), ultrasonic shake plate is provided with ultrasonic head at the correspondence position of each extraction cell,
The structure of Microwave Extraction unit is: be provided with two or more microwave cavity in a vertical housing, microwave head is provided with in microwave cavity, microwave cavity surrounding establishes Flow of Goods and Materials chamber, the wall in Flow of Goods and Materials chamber has and material can be allowed to flow through each Flow of Goods and Materials chamber from top to bottom and the Flow of Goods and Materials hole of microwave leakage can be prevented, feed pipe is established in the Flow of Goods and Materials chamber at top, the Flow of Goods and Materials chamber of bottom establishes the mouth of pipe to rise to the discharge nozzle (this design is in order to ensure when opening microwave system to be completely fluid material in chamber) of housing upper position, discharge nozzle exit is provided with temperature sensor,
The structure of ultrasonic-Microwave Extraction unit is: be provided with two or more microwave cavity in a vertical housing, microwave head is provided with in microwave cavity, microwave cavity surrounding establishes Flow of Goods and Materials chamber, the wall in Flow of Goods and Materials chamber has and material can be allowed to flow through each Flow of Goods and Materials chamber from top to bottom and the Flow of Goods and Materials hole of microwave leakage can be prevented, feed pipe is established in the Flow of Goods and Materials chamber at top, the Flow of Goods and Materials chamber of bottom establish the mouth of pipe rise to housing upper position discharge nozzle (this design in order to ensure open ultrasonic-microwave system time chamber in be completely fluid material), discharge nozzle exit is provided with temperature sensor, ultrasonic head and ultrasonic shake plate is established between Flow of Goods and Materials chamber and inner walls,
First material stores blending tank and the second material storage blending tank is isometric sandwich stainless steel tank body, water or conduction oil medium is filled with in interlayer, interlayer is provided with medium entrance and outlet, material stores blending tank and is provided with agitating device, material stores blending tank top charging aperture, and discharging opening is established in bottom;
The discharging opening that first thing material stores blending tank is connected with the feed end extracting assembly by centrifugal pump; Extract and first add water before operation or other solvents store in blending tank to the first material, open heating system, open agitating device, then add and treat extract material; The first material mixing of materials liquid stored in blending tank is sent into by centrifugal pump and is extracted assembly, active ingredient stripping is carried out in the process of continuous-flow, return the first material material and store blending tank, through being no less than the above-mentioned circulation of twice to complete leaching process; After circulation leaching process completes, material is imported by Steering valve and filters crimping section, carries out filtering and extruding; After completing this step, extract enters the second material by Steering valve and stores blending tank; Until the extract that all first materials store blending tank enters the second material store blending tank; The material slag produced in the process is trapped within and filters in pressurizing unit the interior liquid and extruding is slagged tap, and is then taken out by crushed material slag; In tapping process, first material is imported the first material and store blending tank or short time Break-Up System work; Store blending tank at material and extract assembly discharge end and be equipped with temperature monitoring system, after temperature exceeds design temperature, the extraction unit extracted in assembly can stop microwave or ultrasound works, also material can be imported cooling device, by air-cooled reduction temperature of charge, temperature in whole leaching process is made to remain in the scope of setting; After completing extraction circulation, enter the second material storage blending tank by the extract of extruding slagging-off by Steering valve and deposit, at this moment can carry out again the extraction of new material.
The present invention compared to the prior art tool has the following advantages and beneficial effect:
1. device involved by integrates ultrasonic and microwave, and intensive degree is high, and institute takes up space few.
2. can realize ultrasonic-microwave mode blocking, be convenient to manufacture, change, repair.
3. the module number by increasing and decreasing extraction unit improves or reduces disposal ability, realizes task performance optimization.
4. involved by, device microwave head is spatially separated with ultrasonic head, both can reduce the mutual interference between ultrasonic and microwave, can carry out work separately at the same time or separately again according to material properties.
5., when not increasing microwave head quantity or power, reaching microwave to the process completely of extracting feed liquid, not staying dead angle.
6. both can process a small amount of material, a large amount of material can be processed again; The high-power short time can be used during material handling, the long mode of small-power also can be used to carry out; For a large amount of material, the mode extending extraction time or increase extraction module can be adopted to reach the object increasing handled thing doses.
7. the mode of microwave treatment in prior art is changed into short time mobility to process continuously; material in microwave field only less than a minutes; and at microwave material exit set temperature sensor; once temperature reaches setting value; microwave head just quits work, so just can available protecting to heat sensitive bioactivator.
8. can according to circumstances use cooling system flexibly to keep the temperature stabilization extracting the later stage.
Accompanying drawing illustrates:
Fig. 1 is that the master of ultrasonic extraction unit in embodiment 1 equipment therefor looks cross-sectional view.
Fig. 2 is that the master of Microwave Extraction unit in embodiment 1 equipment therefor looks cross-sectional view.
Fig. 3 is that the master of ultrasonic in embodiment 1 equipment therefor-Microwave Extraction unit looks cross-sectional view.
Fig. 4 is the structural representation of embodiment 1 equipment therefor.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1.
The structure of ultrasonic extraction unit is shown in Fig. 1: be encircled into a vertical material cavity by left and right ultrasonic shake plate 1 and front and back wallboard (can't see in figure), and this material cavity is separated into eight by the central longitudinal dividing plate 2 in it and three pieces of diaphragm plates 3 again and extracts cell.The Flow of Goods and Materials hole (in figure, arrow represents Flow of Goods and Materials direction) that material can be allowed to flow through each extraction cell is from top to bottom had on the relevant position of midfeather 2 and diaphragm plate 3.Feed pipe 4 extracts cell with one of the top and connects.The mouth of pipe 5 rises to the discharge nozzle 6 of material cavity upper position and extracts cell with of bottom and connect.Ultrasonic shake plate 1 is provided with ultrasonic head 7 at the correspondence position of each extraction cell.In Fig. 1,8 is ultrasonic head-shield, and 9 is bottom Butterworth Hatch, and 10 is cleaning valve, and 11 is removable cover, and 12 is the hand-tight wing nut of cover plate.
The structure of Microwave Extraction unit is shown in Fig. 2: one vertical housing 13 and is provided with two microwave cavities 14, microwave head 26 is provided with in microwave cavity 25, microwave cavity 14 surrounding is Flow of Goods and Materials chamber 16, the wall in Flow of Goods and Materials chamber 16 has material can be allowed to flow through Flow of Goods and Materials hole that each Flow of Goods and Materials chamber 16 can prevent again microwave leakage from top to bottom, feed pipe 17 is established in the Flow of Goods and Materials chamber at top, the Flow of Goods and Materials chamber of bottom establishes the mouth of pipe to rise to the discharge nozzle 18 of housing 13 upper position, and outlet 19 place of discharge nozzle 18 is provided with temperature sensor 9 (not shown); In Fig. 2,20 is bottom Butterworth Hatch, and 21 is valve, and 22 is removable cover, and 23 is the hand-tight wing nut of cover plate 22.
The structure of ultrasonic-Microwave Extraction unit is shown in Fig. 3: one vertical housing 24 and is provided with two microwave cavities 25, microwave head 26 is provided with in microwave cavity 25, microwave cavity 25 surrounding establishes Flow of Goods and Materials chamber 28, on the wall in Flow of Goods and Materials chamber 28, relevant position has material can be allowed to flow through Flow of Goods and Materials hole that each Flow of Goods and Materials chamber 28 can prevent again microwave leakage from top to bottom, feed pipe 29 is established in the Flow of Goods and Materials chamber at top, the Flow of Goods and Materials chamber of bottom establishes the mouth of pipe 30 to rise to the discharge nozzle 31 of housing 24 upper position, outlet 30 place of discharge nozzle 31 is provided with temperature sensor (not shown), ultrasonic head 32 and ultrasonic shake plate 33 is established between the inwall of Flow of Goods and Materials chamber 28 and housing 24, in Fig. 3,34 is bottom Butterworth Hatch, and 35 is valve, and 36 is removable cover, and 37 is the hand-tight wing nut of cover plate 36.
The structural representation of whole equipment is shown in Fig. 4.The device used includes extraction assembly, this extraction assembly is by a ultrasonic extraction unit 51, a ultrasonic-Microwave Extraction unit 52 and a Microwave Extraction unit 53 are in series successively, include the first material in addition and store blending tank 38 and the second material storage blending tank 39, circulating conveyor, heater, cooling device, press filtration device and switch board 54.
First material stores blending tank 38 and the second material storage blending tank 39 is isometric sandwich stainless steel tank body, water or conduction oil medium is filled with in interlayer, interlayer is provided with medium entrance and outlet, material stores blending tank and is provided with agitating device 40, material stores blending tank top charging aperture, and discharging opening is established in bottom;
The discharging opening that first material stores blending tank 38 is connected with the feed end extracting assembly by centrifugal pump; Extract and first add water before operation or other solvents store in blending tank 38 to the first material, open heating system, open corresponding agitating device 40, then add and treat extract material; The first material mixing of materials liquid stored in blending tank 38 is sent into by centrifugal pump and is extracted assembly, active ingredient stripping is carried out in the process of continuous-flow, return the first material material and store blending tank 38, through being no less than the above-mentioned circulation of twice to complete leaching process; After circulation leaching process completes, material is imported by Steering valve and filters pressurizing unit 42, carries out filtering and extruding; After completing this step, extract enters the second material by Steering valve and stores blending tank 39; Until the extract that all first materials store blending tank 38 enters the second material store blending tank 39; The material slag produced in the process is trapped within and filters in pressurizing unit 42 and squeeze out liquid, is then taken out by crushed material slag; In tapping process, first material is imported the first material and store blending tank 38 or short time Break-Up System work; Store blending tank at material and extract assembly discharge end and be equipped with temperature monitoring and control system, after temperature exceeds design temperature, extract stopping microwave or the ultrasound works of the extraction unit in assembly, also material can be imported cooling device, by air-cooled reduction temperature of charge, temperature in whole leaching process is made to remain in the scope of setting; After completing extraction circulation, enter the second material storage blending tank by the extract of extruding slagging-off by Steering valve and deposit, at this moment can carry out again the extraction of new material.41 and 48 is centrifugal pump, and 43 is extract heater, and 44 is extract drain pipe, and 45 is interlayer liquid heater, and 46 is interlayer liquid drain pipe, and 47 is extract feed tube, and 49 is fluid reservoir interlayer, and 50 is fluid reservoir stirring motor.
In other words, operating process is as follows: for needing to carry out the material that extracts, first the first material is stored the canned water of mixing or solvent to the amount needed, then opens the related valve of heater, startup heating system.The object that circulating-heating reaches water or Extraction solvent in all even Fast Heating first material storage blending tank is carried out by storing liquid in blending tank interlayer to the first material.After completing extract heating, will meet the requirements of and Powderedly treat that extract adds from tank top, sealing top blind flange.Then the stirring motor starting this material storage blending tank top stirs, and internal circulation of liquid system in interlayer of can simultaneously opening in the process carries out the insulation of feed liquid, and after material reaches predetermined temperature, system can close heating and circulating pump automatically.Agitating device work can be stopped after mixing of materials is even.At this moment open the valve leading to and extract assembly, feed liquid is entered under the promotion of circular centrifugal pump and enters each extraction unit successively.Ultrasonic and microwave can be opened processed material after feed liquid is full of extraction unit.According to the number of feed liquid, the processing time is 20-40min.After completing process, feed liquid is imported and filters pressurizing unit expecting that slag filtration is removed.Filtered fluid imports fluid reservoir or other containers complete extraction.General when room ambient conditions is higher, the heat that in leaching process, ultrasonic and Microwave Extraction unit produces at work can maintain the Extracting temperature of 50-60 degree Celsius.If because using extraction unit more, and when making temperature of charge rise to more than design temperature, one is that system can stop heating automatically, can open deflecting valve in addition, make material enter cooling system, be lowered the temperature by air-cooled.
Embodiment 2.
The extraction of kidney bean bean powder active material is carried out by the device of embodiment 1.Store blending tank to the first material to add water, open heating system and interlayer and pot liquid are heated, then add bean powder on demand, open agitating device and mix.After completing batch mixing can Open valve make feed liquid enter extract assembly carry out circulation extraction, filter after completing extraction.Filtered fluid enters the second material by conduit and stores blending tank storage tank, now completes the extraction of a tank material, and the first material stores mixing tank storage and vacates, and can add material again and extract next time.
Embodiment 3.
The extraction of kidney bean bean powder active material is carried out by the device of embodiment 1.Kidney bean bean powder active material extracts.Store blending tank to the first material to add water, open heating system and interlayer and pot liquid are heated, then add bean powder on demand, open agitating device and mix.After completing batch mixing can Open valve make feed liquid enter extract assembly carry out circulation extraction, open the ultrasonic part in ultrasonic extraction unit power supply and ultrasonic-Microwave Extraction unit, close microwave power supply, at this moment adopt simple ultrasonic process, but in two extraction units, supersonic frequency is different.Filter after completing extraction through the ultrasonic process of different frequency.Filtered fluid enters the second emptying material by conduit and stores blending tank.First material stores blending tank and vacates, and can add material again and extract next time.
Embodiment 4.
The extraction of cassia seed powder active material is carried out by the device of embodiment 1.First material is stored blending tank add water, open heating system and interlayer and pot liquid are heated, then add cassia seed on demand, open agitating device and mix.Feed liquid can be entered extract assembly to carry out circulation to extract, open the microwave portions in ultrasonic extraction unit power supply and ultrasonic-Microwave Extraction unit, close ultrasound portion independent power source, at this moment adopt the ultrasonic processing mode extraction adding microwave by Open valve after completing batch mixing.Microwave heating is utilized to make to change dissociated anthraquinone in conjunction with grace quinone in cassia seed.Filtered fluid enters the second emptying material by conduit and stores blending tank, and the first material stores blending tank and vacates, and can add material again and extract next time.
Embodiment 5 is comparison example.
Get 10kg herb powder and pour storage tank first material storage blending tank into, add extract by 1:6-12, open heating and stirring device, when temperature of charge reaches setting value, open discharge valve, select single ultrasonic tupe, namely material only enters ultrasonic extraction unit and processes.Then pump into the second material by circulating pump and store blending tank, complete and once circulate, ultrasonic setting process 10-30 minute.Respectively in 10,20 of process, within 30 minutes, carry out the rear sampling and measuring of process of slagging tap.If temperature increases to over setting value in leaching process, then can open cooling tube valve and make material enter cooling device cooling.Then slag tap by filtering pressurizing unit.Filtered fluid is squeezed into the second material by centrifugal pump and is stored blending tank.
Get 10kg herb powder, add extract by 1:6-1:12, open heating and stirring device, when temperature of charge reaches setting value, maintain stirring and reach 30 minutes.Then slagged tap by filter.Filtered fluid is squeezed into the second material by centrifugal pump and is stored blending tank.
Take out extract, carry out active principle assay.Result shows, and after only using 30 minutes constant temperature to stir extraction, active constituent content is the 70-80% of ultrasonic process.And ultrasonic process after 10 minutes active principle content just can reach the ultrasonic extraction 90%-93% of 30 minutes.Ultrasonic 20 minutes reach the ultrasonic process 95-96% of 30 minutes.Therefore ultrasonic and circulated extraction method has significant extraction efficiency.
Embodiment 6.
Mung bean phytolectin protein extraction is carried out by the device of embodiment 1.Get 50kg mung bean flour respectively, be divided into 5 parts, every part of 10kg, pour storage tank 13 into, add water as extract by 1:10, mixing.Extracting temperature is 45-50 DEG C.
Method 1: only with stirring, every 5 minutes 1 time, each stirring 1 minute, extract 30 minutes, then extruding is slagged tap, and gets 1L filtered fluid, 62 DEG C are heated 40 minutes, and 4000 leave the heart 20 minutes, adopt the protein concentration of biuret method spectrophotometer measurement supernatant.
Method 2: heat with method 1, but open stirring simultaneously, opens centrifugal pump and ultrasonic extraction device 10 minutes, and after 30 minutes, extruding is slagged tap, and gets 1L filtered fluid centrifugal, adopts the protein concentration of biuret method spectrophotometer measurement supernatant.
Method 3: heat with method 1, ultrasonic 10 minutes, microwave 2 minutes, press filtration after 30 minutes, measured the protein concentration of supernatant by method 1.
Method 4: heat with method 1, ultrasonic process 18 minutes, microwave 2 minutes, measures the protein concentration extracting supernatant with method 1 after 20 minutes.
The protein content determination result of each supernatant:
As shown above, use ultrasonic process within 18 minutes, to add microwave treatment and can obtain maximum extracted rate in 2 minutes, the time also shortens 1/3rd to result.
Claims (3)
1. an extraction assembly for bioactivator, is characterized in that:
By ultrasonic-Microwave Extraction unit, in ultrasonic extraction unit and Microwave Extraction unit two or three is in series;
The structure of ultrasonic extraction unit is: by a left side, right ultrasonic shake plate and front and back wallboard are encircled into a vertical material cavity, this material cavity is again by the central longitudinal dividing plate in it and one or more diaphragm plate be separated into multiple extraction cell be close to up and down, the Flow of Goods and Materials hole that material can be allowed to flow through each extraction cell is from top to bottom had on the relevant position of midfeather and diaphragm plate, one of feed pipe and the top is extracted cell and is connected, the mouth of pipe rises to the discharge nozzle of material cavity upper position and of bottom and extracts cell and connect, ultrasonic shake plate is provided with ultrasonic head at the correspondence position of each extraction cell,
The structure of Microwave Extraction unit is: be provided with two or more microwave cavity in a vertical housing, microwave head is provided with in microwave cavity, microwave cavity surrounding establishes Flow of Goods and Materials chamber, the wall in Flow of Goods and Materials chamber has and material can be allowed to flow through each Flow of Goods and Materials chamber from top to bottom and the Flow of Goods and Materials hole of microwave leakage can be prevented, feed pipe is established in the Flow of Goods and Materials chamber at top, the Flow of Goods and Materials chamber of bottom establishes the mouth of pipe to rise to the discharge nozzle of housing upper position, and discharge nozzle exit is provided with temperature sensor;
The structure of ultrasonic-Microwave Extraction unit is: be provided with two or more microwave cavity in a vertical housing, microwave head is provided with in microwave cavity, microwave cavity surrounding establishes Flow of Goods and Materials chamber, the wall in Flow of Goods and Materials chamber has and material can be allowed to flow through each Flow of Goods and Materials chamber from top to bottom and the Flow of Goods and Materials hole of microwave leakage can be prevented, feed pipe is established in the Flow of Goods and Materials chamber at top, the Flow of Goods and Materials chamber of bottom establishes the mouth of pipe to rise to the discharge nozzle of housing upper position, discharge nozzle exit is provided with temperature sensor, establishes ultrasonic head and ultrasonic shake plate between Flow of Goods and Materials chamber and inner walls; The device used comprises extraction assembly, this extraction assembly is by ultrasonic-Microwave Extraction unit, in ultrasonic extraction unit and Microwave Extraction unit two or three is in series, include the first material in addition and store blending tank and the second material storage blending tank, EGR, heater, cooling device, press filtration device and switch board.
2. the extraction assembly of bioactivator as claimed in claim 1, it is characterized in that: by a ultrasonic extraction unit, a ultrasonic-Microwave Extraction unit and a Microwave Extraction unit are in series successively.
3. a bioactivator ultrasonic-microwave combination extraction process, is characterized in that:
The device used comprises extraction assembly, this extraction assembly is by ultrasonic-Microwave Extraction unit, in ultrasonic extraction unit and Microwave Extraction unit two or three is in series, include the first material in addition and store blending tank and the second material storage blending tank, EGR, heater, cooling device, press filtration device and switch board;
The structure of ultrasonic extraction unit is: by a left side, right ultrasonic shake plate and front and back wallboard are encircled into a vertical material cavity, this material cavity is again by the central longitudinal dividing plate in it and one or more diaphragm plate be separated into multiple extraction cell be close to up and down, the Flow of Goods and Materials hole that material can be allowed to flow through each extraction cell is from top to bottom had on the relevant position of midfeather and diaphragm plate, one of feed pipe and the top is extracted cell and is connected, the mouth of pipe rises to the discharge nozzle of material cavity upper position and of bottom and extracts cell and connect, ultrasonic shake plate is provided with ultrasonic head at the correspondence position of each extraction cell,
The structure of Microwave Extraction unit is: be provided with two or more microwave cavity in a vertical housing, microwave head is provided with in microwave cavity, microwave cavity surrounding establishes Flow of Goods and Materials chamber, the wall in Flow of Goods and Materials chamber has and material can be allowed to flow through each Flow of Goods and Materials chamber from top to bottom and the Flow of Goods and Materials hole of microwave leakage can be prevented, feed pipe is established in the Flow of Goods and Materials chamber at top, the Flow of Goods and Materials chamber of bottom establishes the mouth of pipe to rise to the discharge nozzle of housing upper position, and discharge nozzle exit is provided with temperature sensor;
The structure of ultrasonic-Microwave Extraction unit is: be provided with two or more microwave cavity in a vertical housing, microwave head is provided with in microwave cavity, microwave cavity surrounding establishes Flow of Goods and Materials chamber, the wall in Flow of Goods and Materials chamber has and material can be allowed to flow through each Flow of Goods and Materials chamber from top to bottom and the Flow of Goods and Materials hole of microwave leakage can be prevented, feed pipe is established in the Flow of Goods and Materials chamber at top, the Flow of Goods and Materials chamber of bottom establishes the mouth of pipe to rise to the discharge nozzle of housing upper position, discharge nozzle exit is provided with temperature sensor, establishes ultrasonic head and ultrasonic shake plate between Flow of Goods and Materials chamber and inner walls;
First material stores blending tank and the second material storage blending tank is isometric sandwich stainless steel tank body, water or conduction oil medium is filled with in interlayer, interlayer is provided with medium entrance and outlet, material stores blending tank and is provided with agitating device, material stores blending tank top charging aperture, and discharging opening is established in bottom;
The discharging opening that first thing material stores blending tank is connected with the feed end extracting assembly by centrifugal pump; Extract and first add water before operation or other solvents store in blending tank to the first material, open heating system, open agitating device, then add and treat extract material; The first material mixing of materials liquid stored in blending tank is sent into by centrifugal pump and is extracted assembly, active ingredient stripping is carried out in the process of continuous-flow, return the first material material and store blending tank, through being no less than the above-mentioned circulation of twice to complete leaching process; After circulation leaching process completes, material is imported by Steering valve and filters crimping section, carries out filtering and extruding; After completing this step, extract enters the second material by Steering valve and stores blending tank; Until the extract that all first materials store blending tank enters the second material store blending tank; The material slag produced in the process is trapped within and filters in pressurizing unit the interior liquid and extruding is slagged tap, and is then taken out by crushed material slag; In tapping process, first material is imported the first material and store blending tank or short time Break-Up System work; Store blending tank at material and extract assembly discharge end and be equipped with temperature monitoring system, after temperature exceeds design temperature, the extraction unit extracted in assembly can stop microwave or ultrasound works, also material can be imported cooling device, by air-cooled reduction temperature of charge, temperature in whole leaching process is made to remain in the scope of setting; After completing extraction circulation, enter the second material storage blending tank by the extract of extruding slagging-off by Steering valve and deposit, at this moment can carry out again the extraction of new material.
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| CN105132118A (en) * | 2015-09-25 | 2015-12-09 | 海南大学 | Coconut oil extraction method |
| CN114232107A (en) * | 2021-12-17 | 2022-03-25 | 沪本新材料科技（上海）有限公司 | Preparation device of wormwood extract and production method of wormwood chinlon polyester fiber |
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| CN101530674A (en) * | 2009-03-16 | 2009-09-16 | 王艺瑾 | Process for extracting active ingredients of traditional Chinese medicine in unit and combined type and device thereof |
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| CN104759112B (en) | 2016-04-06 |
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