CN104923137A - Method for enhancing fluid mixing in micro-reactor - Google Patents
Method for enhancing fluid mixing in micro-reactor Download PDFInfo
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- CN104923137A CN104923137A CN201410102972.1A CN201410102972A CN104923137A CN 104923137 A CN104923137 A CN 104923137A CN 201410102972 A CN201410102972 A CN 201410102972A CN 104923137 A CN104923137 A CN 104923137A
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Abstract
The invention relates to a method for enhancing the mixing of multiple fluids in a micro-reactor. In the provided method, bubbles are continuously introduced into the fluids from one or more air inlets arranged in a micro-channel, at the same time ultrasonic waves with a specific frequency and power are applied on the fluids, the cavatition effect of ultrasonic waves can fiercely vibrate and move the bubbles, strong turbulence can be triggered in the multiple fluids, thus the mixing among fluids is enhanced, and the obstruction is prevented and evacuated.
Description
Technical field
The invention belongs to the fields such as chemical industry intensifying method, chemical industry equipment, applications of ultrasound, specifically a kind of method utilizing the mixing of ultrasound-enhanced microchannel inner fluid, prevention and dredge blockage.
Background technology
Microreactor refers to that inner structural features size is at the several microns of chemical industry equipments to number mm-scale.This internal structure is usually also referred to as microchannel.Relative to traditional large chemical equipment, microreactor has that specific surface is high, heat and mass speed is fast, handling safety, be easy to amplify, take up an area the advantages such as space is little, makes microreactor become one of the most promising Chemical Engineering Technology.
But microreaction technology also presents some new problem demanding prompt solutions on stream.Because microchannel size is little, flowing is usually in laminar condition and surface tension effects is remarkable, makes the mixed intensified more difficult of multiple fluid in microchannel.At present conventional way is that microchannel is designed to the structures such as bending, obstacle, collision, is locally causing eddy current or chaotic flow to strengthen mixing, little between the operating space of this microreactor, pressure drop ratio is larger.In addition, because the microchannel size in microreactor is little, at structure places such as these bending, obstacle, collisions, passage is easily blocked by impurity or process fluid, particularly when processing containing solid or generating solid or the very large fluid of viscosity.
Solve the mixed intensified difficulty of multiple fluid in microreactor, susceptible to plugging problem, need to introduce external energy in microreactor, to prevent and to dredge its blocking, its mixing of strengthening further.Having the advantages such as penetrability is good, energy density is high, safe and reliable due to ultrasonic, introduced by ultrasonic wave in microchannel, is a kind of very effective method that simultaneously can solve the problems such as mixed intensified difficulty and blocking.
Ultrasound-enhanced fluid chemical field, prevention and dredge blockage mainly rely on ultrasonic cavitation, namely the cavitation bubble growth under ultrasonication in fluid, periodic vibration, to collapse, and producing violent shock wave, acoustic streaming etc. in fluid near bubble, disturbance fluid is with strengthening fluid mixing, mass transfer.In addition, disturbance caused by the vibration of microchannel wall and gas liquid film high vibration under ultrasonication, can destroy the gathering between solid in fluid or dope or the adhesion at microchannel wall, thus prevention and dredge blockage.(Ultrasound andMicrostructures-A Promising Combination such as S.Hubner, ChemSusChem2012,5,279 – 288) directly pass in microreactor by ultrasonic, find that ultrasonic cavitation effectively can promote the mixing between profit, improve the yield of p-nitrobenzene amyl acetate hydrolysis.(the A Teflon microreactor with integrated piezoelectric actuator to handlesolid forming reactions such as Simon Kuhn, Lab Chip, 2011,11,2488 – 2492) be incorporated in the microchannel of microreactor inside by ultrasonic, find that ultrasonic cavitation effectively can destroy the blocking of products sodium chloride crystal grain in microchannel in carbon nitrogen coupling reaction.
Because the liquid volume in microchannel is little, contained cavitation bubble number ratio tradition large scale equipment is few; In addition because microchannel inner fluid speed is often higher, the cavitation bubble formed is easy to be washed away by fluid, thus cavitation bubble total quantity when causing actual motion in microchannel is fewer, and ultrasonic cavitation effect is poor relative to legacy equipment.In order to improve the effect of the mixing of multiple fluid in ultrasound-enhanced microchannel, mass transfer and prevention and dredge blockage further, needing the quantity of artificial increase micro channel hollow bubble, thus strengthening ultrasonic cavitation.(the Lateral cavity acoustic transducer such as Armando R.Tovar, Lab Chip, 2009,9,41 – 43) propose the concept of " chamber, side acoustic driver " first, namely, at the artificial process cavity of microchannel sidewall or groove, after liquid enters microchannel, some air is bound in chamber or groove and forms bubble; When applying certain frequency ultrasonic to microchannel, these bubbles produce violent vibration and acoustic streaming under ultrasonic effect, thus can fluid-mixing (flow 0.8 μ l/min) or Fluid Motion Driven By Moving.(the A fast microfluidicmixer based on acoustically driven sidewall-trapped microbubbles such as Daniel Ahmed, Microfluid Nanofluid, 2009, 7, 727 – 731 and A millisecond micromixervia single-bubble-based acoustic streaming, Lab Chip, 2009, 9, 2738 – 2741) adopt the method for " chamber, side acoustic driver " on the sidewall of microchannel or in passage, process some long 90-240 μm, wide 60-90 μm, the groove of dark 155 μm, when applying 70-82 KHz ultrasonic to whole microreactor, bubble in groove produces violent vibration under ultrasonic effect, and form violent acoustic streaming whirlpool in its vicinity to promote mixing, incorporation time can be reduced to 7-120 millisecond when flow 6-16 μm of l/min.
In sum, the method cavitation bubble total amount only by ultrasound-enhanced mixing in microchannel is few, easily runs off under high flow rate.The method that " chamber, side acoustic driver " strengthens the mixing of microchannel inner fluid and prevention and dredge blockage can reach reasonable effect under certain condition, but the method is only applicable to the lower and occasion that microchannel wall hydrophobicity is stronger of velocity ratio.When flow-rate ratio is higher, the bubble of the structure such as chamber, groove constraint is equally easily washed away by fluid, and when particularly the hydrophobicity of microchannel wall is poor, the constraint effect of the structure such as chamber, groove to bubble is more weak.In addition, when high flow rate, the ultrasound-enhanced weak effect of limited quantity bubble, needs to process the ultrasound-enhanced effects of structure guarantee such as a large amount of chambers, groove at microchannel wall, processing cost is high, and the isostructural size of chamber, groove just cannot adjust after processing again.In addition, the ultrasound-enhanced effect of this method is difficult to long-time steady operation.Because the bubble that the structure such as chamber, groove fetters may shake broken under long-time ultrasonication, or is diminished by absorption of fluids, or depart under the acting in conjunction of ultrasonic vibration and liquid flow.
Summary of the invention
In order to solve the problem, present inventor has performed further investigation.Find: if arrange one or several gas accesses in microchannel, then gas is passed into, then can produce bubble that is a large amount of, size uniform constantly in microchannel, now, in microchannel, apply the ultrasonic of certain frequency, utilize cavitation that is ultrasonic and gas phase, make the gas phase high vibration in microchannel and motion, and cause disturbance and acoustic streaming in a liquid, thus the mixing of energy efficient hardening liquid.The ultrasonic sound intensity of input is larger, and fluid chemical field strengthening effect is better.Under certain sound intensity, when the horizontal equivalent diameter of supersonic frequency f and gas phase meets specific matching relationship, ultrasonicly reach resonance with gas phase, now gas phase vibration and most motion intense, significantly, therefore mixed intensified effect is best for the disturbance caused in a fluid and acoustic streaming.Under other matching relationship, ultrasonicly can not reach resonance with gas phase, now gas-liquid interface vibration and motion more weak, strengthening effect is poor.The quantity of bubble and size control by the gas flow of gas access, when fluid flow is higher in microchannel, improve the bubble that gas flow just can obtain requirement and size accordingly.
Therefore, this method be applicable to high flow rate occasion, can long-time steady operation, MCA simple, be a kind of method of simple and efficient strengthening microchannel inner fluid mixing, prevention and dredge blockage.
The present invention is based on above-mentioned research and resolve and propose following technical scheme:
Importing gas phase continuously by being arranged in more than the two kinds fluids in microchannel of the gas access of more than or two in microchannel, forming gas-liquid polyphase flow, the horizontal equivalent diameter of regulation and control gas phase is 10-5000 μm; Apply frequency is the ultrasonic of 16-600kHz simultaneously, makes gas phase high vibration and motion under ultrasonic cavitation.
In technique scheme, the stream shape of described gas-liquid polyphase flow is the one in bubble flow, slug flow, bullet shape annular flow, stirring stream and annular flow.Be preferably the one in bubble flow or slug flow.The stream shape of gas-liquid polyphase flow is a known concept in field of chemical engineering.Gas phase in this patent is formed in the liquid phase to the situation of multiphase flow, when stream shape refers to that gas-liquid polyphase flow enters microreactor, gas phase is placed in the shape of liquid phase.In microreactor, bubble flow, slug flow, bullet shape annular flow, stirring stream and annular flow are modal several heterogeneous shaped flow streams.
Described apply in gas-liquid microreactor ultrasonic, the matching relationship of supersonic frequency f and the horizontal equivalent diameter d of gas phase is f*d=1-40mmkHz.Both are preferably f*d=4-30mmkHz by product value.
The horizontal equivalent diameter of described gas phase be in gas-liquid flow shape gas phase perpendicular to the cross section equivalent diameter on flow direction.When biphase gas and liquid flow shape is bubble flow, cross section equivalent diameter is the diameter of bubble; Bubble diameter and quantity can be regulated and controled by the flow velocity of gas-liquid two-phase; When biphase gas and liquid flow shape be slug flow, play shape annular flow time, the cross section equivalent diameter of gas phase regulates and controls primarily of the cross sectional dimensions of microchannel; When biphase gas and liquid flow shape is for stirring stream and annular flow, the lateral cross section equivalent diameter of gas phase is regulated and controled by the cross sectional dimensions of microchannel and the flow velocity of gas-liquid two-phase simultaneously.
In described gas-liquid microreactor, ultrasonic transducer can be bonded in microreactor outer surface, make ultrasonic conducting enter microreactor; Also ultrasonic transducer can be integrated in microreactor inside, make ultrasonic direct conduction enter microchannel; Whole microreactor can also be put into ultrasonic cleaning tank.
This method, under bubble flow or slug flow, adopts frequency to be that 16-600kHz and the sound intensity are higher than 0.5W/cm
2the ultrasonic operation carrying out the course of reaction relating to solid.
This method can be applied to the mixed process between the various fluid of strengthening, the such as mixed process of two kinds of aqueous solution that dissolve each other, the emulsion process etc. of water-oil phase.Also may be used for the strengthening of various chemical reaction process, particularly relate to the course of reaction of solid.What is called relates to the course of reaction of solid, has referred to that solid participates in reaction as reactant, catalyst etc., or in generation product, some is the course of reaction of solid.
The present invention under bubble flow and slug flow, by importing bubble continuously, and when supersonic frequency is higher than 16 KHz, efficient hardening liquid-liquid diphase mixed effect.Only under bubble flow, in supersonic frequency higher than 20 KHzs, sound intensity 1.5W/cm
2time, can carry out the reaction of liquid liquid precipitate continuously in the microchannel that equivalent diameter is 667 μm, for material preparation, process is without blocking.
Accompanying drawing explanation
Fig. 1 is embodiment 1 ~ 3 MCA schematic diagram used.Wherein, 1 is liquid one access road, and 2 is liquid two access road, and 3 is gas entrance passage, and 4 is main channel.
Fig. 2 is the mixing situation of water and ink when not adding ultrasonic in embodiment 1.
Fig. 3 is the mixing situation of water and ink when adding ultrasonic in embodiment 1.
Fig. 4 is the mixing situation of water and ink when not adding ultrasonic in embodiment 2.
Fig. 5 is the mixing situation of water and ink when adding ultrasonic in embodiment 2.
Fig. 6 is the change in pressure drop curve of microchannel in embodiment 3.
Detailed description of the invention
The present invention is further illustrated below by embodiment.
Micro passage reaction involved by following embodiment 1 ~ 3 is single channel microreactor, and MCA as shown in Figure 1.1 and 2 access roades being respectively two kinds of liquid, dark and are widely 500 μm, and 3 is gas entrance passage, dark 500 μm wide 200 μm.4 is main channel, dark 500 μm wide 1000 μm.
Fluid mixing process strengthening under embodiment 1, bubble flow
The present embodiment carrys out strengthening fluid with importing bubble flow bubble continuous in microreactor and is mixed into example.In order to observe the effect of ultrasound-enhanced mixing, at the solution that two liquid inlet channels 1 and 2 of microchannel pass into deionized water respectively and are made into deionized water ink, flow is 5ml/min; In gas entrance passage 3, pass into air, flow be 1ml/min as shown in Figure 2, the air passed into forms bubble flow in main channel 4, bubble lateral dimension about 300 μm.When not adding ultrasonic, ink and water flow along the both sides of passage 4, mix poor.When applying 20 KHzs in microreactor, the sound intensity is 1.5W/cm
2ultrasonic after, namely the product of the horizontal equivalent diameter d of supersonic frequency f and gas phase is f*d=6mmkHz, and in passage 4, water and ink mix immediately, see Fig. 3.
Fluid mixing process strengthening under embodiment 2, slug flow
The present embodiment carrys out strengthening fluid with importing slug flow bubble continuous in microreactor and is mixed into example.At the solution that two liquid inlet channels 2 and 1 of microchannel pass into deionized water respectively and are made into deionized water ink, flow is 1ml/min; In gas entrance passage 3, pass into air, flow is 2ml/min.As shown in Figure 4, the air passed into forms slug flow in main channel 4, the lateral dimension of bubble about 1000 μm.When not adding ultrasonic, ink and water flow along the both sides of passage 4, mix poor.When apply in microreactor ultrasonic after, in passage 4, water and ink mixed effect obviously strengthen, and see Fig. 5.Fig. 5 is supersonic frequency 18 KHz, the sound intensity is 1.5W/cm
2the mixed effect of Shi Shui and ink, the product of supersonic frequency f now and the horizontal equivalent diameter d of gas phase is f*d=18mmkHz.
Embodiment 3, liquid liquid precipitate course of reaction are strengthened
The present embodiment imports bubble flow bubble continuously to prevent and dredges microchannel blocking in microreactor by gas access.Pass into zinc nitrate solution and sodium carbonate liquor respectively at two liquid inlet channels 1 and 2 of microchannel, two strands of solution mix after entering main channel 4 and react generation zinc carbonate solid particle.The flow of zinc nitrate solution and sodium carbonate liquor is 50ml/min, and concentration is 0.5mol/L; In gas entrance passage 3, pass into the air that flow is 10ml/min, the air passed into forms bubble flow in main channel 4, bubble lateral dimension about 300 μm.The change curve of pressure drop time when Fig. 6 is reactor operation.When not adding ultrasonic, the zinc carbonate solids particles precipitate generated in microchannel 4 at channel wall, and is passed cumulative in time, and pressure drop increases gradually.After about 10 minutes, passage 4 blocks, and pressure is elevated to 4.75MPa, and reactor outlet does not have fluid to flow out.Now, apply frequency 20 KHz to reactor, the sound intensity is 1.5W/cm
2ultrasonic, can calculate, the product of the horizontal equivalent diameter d of supersonic frequency f and gas phase is f*d=6mmkHz, and now, the pressure drop of reactor drops to 0.25MPa immediately, and reactor outlet has fluid to flow out immediately.Under the effect that this is ultrasonic, reactor runs 2 hours continuously and has no obvious pressure oscillation, and pressure is always at 0.25-0.5MPa.Visible, the method can make the reaction of the liquid liquid precipitate in microchannel continous-stable carry out, and can effectively prevent and dredge microchannel blocking.
Claims (6)
1. strengthen the method for multiple fluid mixing in microreactor for one kind, it is characterized in that: import gas phase continuously by being arranged in more than the two kinds fluids in microchannel of the gas access of more than or two in microchannel, form gas-liquid polyphase flow, the horizontal equivalent diameter of regulation and control gas phase is 10-5000 μm; Apply frequency is the ultrasonic of 16-600kHz simultaneously, makes gas phase high vibration and motion under ultrasonic cavitation.
2. method according to claim 1, is characterized in that: the stream shape of described gas-liquid polyphase flow is the one in bubble flow, slug flow, bullet shape annular flow, stirring stream and annular flow.
3. method according to claim 1 and 2, is characterized in that: the stream shape of described gas-liquid polyphase flow is the one in bubble flow or slug flow.
4. method according to claim 1, is characterized in that: described apply in gas-liquid microreactor ultrasonic, the matching relationship of supersonic frequency f and the horizontal equivalent diameter d of gas phase is f*d=1-40mmkHz.
5. method according to claim 4, is characterized in that: described apply in gas-liquid microreactor ultrasonic, the matching relationship of supersonic frequency f and the horizontal equivalent diameter d of gas phase is f*d=4-30mmkHz.
6. the arbitrary described method of right 1 ~ 5, is characterized in that: under bubble flow or slug flow, adopts frequency to be that 16-600kHz and the sound intensity are higher than 0.5W/cm
2the ultrasonic operation carrying out the course of reaction relating to solid.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104162395A (en) * | 2014-03-21 | 2014-11-26 | 中国科学院大连化学物理研究所 | Method for enhancing gas-liquid process in micro-reactor |
| CN109020811A (en) * | 2018-09-19 | 2018-12-18 | 张家港瀚康化工有限公司 | The method for preparing propionic ester using microreactor |
| CN111773993A (en) * | 2020-07-01 | 2020-10-16 | 西安交通大学 | Counter-flow jet cold and hot fluid mixer under action of external field |
| CN113003852A (en) * | 2020-11-13 | 2021-06-22 | 四川全息生态环境技术产业有限公司 | Ultrasonic wave and H2O2And micro-channel advanced oxidation method and device |
| CN113527109A (en) * | 2021-07-08 | 2021-10-22 | 南京先进生物材料与过程装备研究院有限公司 | Method for preparing perfluoroalkyl aniline by micro-flow field reaction technology |
| CN114733415A (en) * | 2022-03-01 | 2022-07-12 | 中国科学院大连化学物理研究所 | Ultrasonic micro mixer with millisecond mixing performance |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104162395A (en) * | 2014-03-21 | 2014-11-26 | 中国科学院大连化学物理研究所 | Method for enhancing gas-liquid process in micro-reactor |
| CN109020811A (en) * | 2018-09-19 | 2018-12-18 | 张家港瀚康化工有限公司 | The method for preparing propionic ester using microreactor |
| CN111773993A (en) * | 2020-07-01 | 2020-10-16 | 西安交通大学 | Counter-flow jet cold and hot fluid mixer under action of external field |
| CN111773993B (en) * | 2020-07-01 | 2021-10-19 | 西安交通大学 | Counter-flow jet cold and hot fluid mixer under action of external field |
| CN113003852A (en) * | 2020-11-13 | 2021-06-22 | 四川全息生态环境技术产业有限公司 | Ultrasonic wave and H2O2And micro-channel advanced oxidation method and device |
| CN113527109A (en) * | 2021-07-08 | 2021-10-22 | 南京先进生物材料与过程装备研究院有限公司 | Method for preparing perfluoroalkyl aniline by micro-flow field reaction technology |
| CN114733415A (en) * | 2022-03-01 | 2022-07-12 | 中国科学院大连化学物理研究所 | Ultrasonic micro mixer with millisecond mixing performance |
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