CN106669556B - A method of millimeter grade particles are prepared using transformation microfluidic channel - Google Patents
A method of millimeter grade particles are prepared using transformation microfluidic channel Download PDFInfo
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- B01J13/02—Making microcapsules or microballoons
Abstract
The present invention provides a kind of methods for preparing millimeter grade particles using transformation microfluidic channel, and the described method comprises the following steps: a. prepares the basic channel of micro-fluidic chip；B. the tubular fitting in the basic channel of micro-fluidic chip is prepared；C. tubular fitting is assembled in the basic channel of micro-fluidic chip；D. particle is prepared.Method of the invention obtains more complicated different type microfluidic channel structure using simple processing and packaging technology; required specific aim flow field is provided for different magnitude of particle preparation; it is changeable to realize a core; one core is multi-purpose; have the characteristics that channel geometry can degree of change be big, controllability wide using size range is strong and low-consumption high-efficiency, can be used for monodisperse particles or drop that steady and continuous batch obtains hundred microns to several millimeters partial sizes.
Description
Technical field
The invention belongs to micro-/milli fluidics application fields, and in particular to a kind of to utilize transformation microfluidic channel preparation milli
The method of scale particles.
Background technique
Micro-capsule and laser fusion target fuel are loaded in microreactor, realizing controlled-release drug and catalyst carrier, bioactivity kind
In the fields such as container, hundred microns to several millimeters particles/drops are widely used.Traditional stirring, the emulsification of spraying and film etc. " from
Top is downward " material and chemical method be difficult to batch and prepare that monodisperse degree is high and bulky grain/drop of structure-controllable, and it is past
More, the time and effort consuming toward step.Over the past decade, micro-/milli fluidics be biology, chemistry and the application of the various fields such as material and
One of hot spot of research.Successively developed T-type channel (T-shaped junction), focus channel (Flow-focusing) and
The microchannel of the three basic forms of it such as co-flow pathway (Co-flowing), these three basic channel designs decide three kinds of basic flows
Type, flow pattern feature, miniflow bulk-mode and drop forming mechanism have obtained extensive research, in microring array and micron particles/liquid
Dripping is standby etc. to be widely used.Compare, the micro-/milli fluidics of " bottom-up " for particle/drop partial size with it is several
What regulation has unique advantage, furthers investigate its application technology in terms of millimeter magnitude particle/drop preparation with important
Realistic meaning.
Compared with micro/nano level particle/drop preparation, the preparation of millimeter grade particles/drop need to usually face large volume flow
The fluctuation of bring flow velocity, big lotion itself rheological characteristic, thermodynamic phase and buoyancy effect etc. caused by great risk and
Uncontrollability.To prepare grade polymer microballoon and microcapsules, three nozzle milk particles of American National ignition center development occur
Device technology, Zeng Yidu is a kind of classical way of related fields, but its assembly precision requires height, is gradually substituted.Chinese engineering
Physical study institute has successively developed double-T shaped, double ten types, double-Y shaped and dual coflow declines flow control passage technology.In contrast, double Y
It is possible to prevente effectively from hydrodynamics stationary point, flow field is more steady in type channel, control and entire drop body for different phase fluids
Long-pending ability of regulation and control is stronger, is advantageously implemented the accurate customization of size and particle geometric.Furthermore W. Engl et al. focuses commercial quantities
Change and reduce cost, " tubular type milli flow control " is utilized to prepare millimeter particles and drop, and emphasized development the relevant technologies have compared with
Big prospect and practical significance.However, micro-fluidic chip channel geometry is that continuous-stable forms drop and effectively controls its knot
The key of structure and size.Currently, a chip is applicable in, target size range is relatively narrow, and channel geometry is fixed, and user is difficult to root
It is multi-purpose according to one core of practical application request.Meanwhile the preparation processing technology of micro-fluidic chip is complicated, the bonding and photoetching skill of microchannel
Art threshold is higher, expensive, assembling not easy to disassemble, and inconvenience cleaning, the reuse rate of chip is low, and service life is shorter.Especially
It is that conventional method production complex pipeline is extremely difficult, even the laser direct-writing and 3D printing technique of developed recently, in chip
All there is severe bottleneck in the application in preparation, printing has particular/special requirement to material, and process is slow, it is difficult to realize fine and close bubble-free,
Optical clarity is very poor.
Currently, need to develop it is a kind of prepare millimeter grade particles/drop method using transformation microfluidic channel, using simple
Processing and packaging technology obtain more complicated different type microfluidic channel, and low-consumption high-efficiency, a core is changeable, and a core is multi-purpose, surely
Determine continuous batch and obtains the broader monodisperse particles/drop of size range.
Summary of the invention
Millimeter grade particles are prepared using transformation microfluidic channel technical problem to be solved by the invention is to provide a kind of
Method.
It is of the invention using transformation microfluidic channel prepare millimeter grade particles method the following steps are included:
A. the basic channel of micro-fluidic chip is prepared；
B. the tubular fitting in the basic channel of micro-fluidic chip is prepared；
C. tubular fitting is assembled in the basic channel of micro-fluidic chip；
D. particle is prepared.
The step a the following steps are included:
A1. the sheet glass of rectangular shape is lain in a horizontal plane in above aluminium foil, aluminium foil is upward along the side of sheet glass
Four sides of package sheet glass are folded, sheet glass is rolled into the hollow cuboid an of upper opening, obtains mold by aluminium foil
Performed polymer container defines length, height, the wide respectively X, Y, Z axis of hollow cuboid；
A2. surface is smooth, along the x axis the stepped increase of radius, stainless steel I with the straight sections such as N sections
Horizontal through mold performed polymer container, the horizontal symmetrical center line of stainless steel I is lower than the horizontal symmetrical of mold performed polymer container
Center line；In the horizontal symmetrical plane of stainless steel I, stainless steel is symmetrically fixed in the equal straight sections two sides of the second of stainless steel I
II and stainless steel III, stainless steel IV and stainless steel V, stainless steel are symmetrically fixed in the straight sections such as third of stainless steel I two sides
Stainless steel M-1 and stainless steel M is symmetrically fixed in the straight sections two sides such as the N of bar I, by fixed stainless steel, obtains required
The basic channel template of micro-fluidic chip；
Along X-axis negative direction, the angle between stainless steel II and stainless steel III is 120 °, stainless steel IV and stainless steel
Angle between bar V is 120 °, until the angle between stainless steel M-1 and stainless steel M is 120 °；N >=5, M >=5；
A3. polymer and curing agent are uniformly mixed, form prepolymer solution, prepolymer solution is evacuated to
Bubble-free is poured into mold performed polymer container made of step a1, again takes out the prepolymer solution in mold performed polymer container
Mold performed polymer container is put in a vacuum drying oven to bubble-free, solidifies 2 ~ 3h at 70 DEG C, micro-fluidic chip is made by vacuum
Basic channel die；
A4. the basic channel die of micro-fluidic chip is ultrasonically treated 30min, removes the aluminium foil of die surface and the glass of lower section
The stainless steel of mould inside is rotated and is extracted by glass piece, obtains micro-fluidic chip blank, cuts micro-fluidic chip blank shape,
The basic channel of micro-fluidic chip is obtained, the channel that stainless steel I is formed is channel I, and the channel that stainless steel II is formed is channel
II, the channel that stainless steel III is formed is channel III, and the channel that stainless steel IV is formed is channel IV, what stainless steel V was formed
Channel is channel V, until the channel that stainless steel M is formed is channel M.
The step b the following steps are included:
B1. tubular fitting I is prepared, tubular fitting I is hollow circular tube, and the outer diameter of hollow circular tube is less than the interior of I entrance of channel
Diameter；
B2. tubular fitting II is prepared, tubular fitting II is the conical pipe of hollow circle, and the outside diameter of conical pipe is stainless
The internal diameter of the straight sections such as I third ladder of steel pole；
B3. tubular fitting III is prepared, tubular fitting III is the conical pipe of hollow circle, and the outside diameter of conical pipe is stainless
The internal diameter of the straight sections such as I fourth order ladder of steel pole；
B4. tubular fitting IV is prepared, tubular fitting IV is the conical pipe of hollow circle, and the outside diameter of conical pipe is stainless
The internal diameter of the straight sections such as the 5th ladder of steel pole I；
B5. continue to prepare tubular fitting, until the outside diameter of the conical pipe of tubular fitting is I N ladder of stainless steel
The internal diameter of equal straight sections.
The step c the following steps are included:
C1. tubular fitting I is inserted into channel I, one end of tubular fitting I is fixed on the inlet in channel I, the other end
X-axis positive direction horizontal extension along channel I；
C2., the big end of the conical pipe of tubular fitting II is inserted into channel I, tubular fitting at the straight sections such as the N in channel I
The small end of II conical pipe is towards X-axis positive direction, and tubular fitting II is along the Forward of X-axis negative direction until the big end card of tubular fitting II
On the straight sections such as third, obtain focusing and coflow combined type channel；
C3., the big end of the conical pipe of tubular fitting III is inserted into channel I, tubular fitting at the straight sections such as the N in channel I
The small end of III conical pipe is towards X-axis positive direction, and tubular fitting III is along the Forward of X-axis negative direction until big end, which is stuck in the 4th, waits straight sections
On, obtain positive double focusing channel；
Or the small end of the conical pipe of tubular fitting VI is inserted into channel I, tubular fitting at the straight sections such as the N in channel I
The big end of VI conical pipe is towards X-axis positive direction, and tubular fitting VI is along the Forward of X-axis negative direction until big end, which is stuck in the 5th, waits straight sections
On, obtain reversed double focusing channel；
C4. continue that tubular fitting is installed, until obtaining required channel.
The step d the following steps are included:
D1. fluid I is passed through in tubular fitting I；
D2. it is passed through fluid II simultaneously in channel II and channel III, the fluid II and fluid I are immiscible；
D3. it is passed through fluid III simultaneously in channel VI and channel V, the fluid III and fluid II are immiscible；
D4. it collects to obtain milk particle at the straight sections such as N；
D5. milk particle is solidified, obtains particle.
The equal straight sections outer diameter of the stainless steel I is millimeter magnitude.
The polymer is dimethyl silicone polymer, and curing agent is polymethyl methacrylate, and the performed polymer is molten
The mass ratio of dimethyl silicone polymer and polymethyl methacrylate in liquid is 10:1.
The stainless steel stainless steel tube, stainless steel sleeve pipe, glass rod, glass tube, teflon rod or poly- four
The replacement of one of fluoride tubes.
The stainless steel passes through the gap left on aluminium foil when aluminium foil and is sealed with silicon mud；
The stainless steel I punches in advance, by stainless steel II, stainless steel III, stainless steel IV, stainless steel V
It is fixed until stainless steel M is inserted directly into corresponding hole.
The material of the tubular fitting is one of polyfluortetraethylene pipe, glass tube or stainless steel tube.
The method for preparing millimeter grade particles using transformation microfluidic channel of the invention, uses sheet glass, aluminium foil, stainless steel
The materials such as tube rod, stainless steel tube, glass rod, glass tube, teflon rod or polyfluortetraethylene pipe, material is cheap, can basis
It needs voluntarily to process, quick detachable and assembling is easy to clean, can repeatedly use, and is easy to be assembled into various all kinds of different complicated journeys
The micro-fluidic pipeline of degree.
The method for preparing millimeter grade particles using transformation microfluidic channel of the invention, according to different magnitude of target size
Demand carries out the transformation of channel geometry and size, and the target size of wider range is obtained using the same micro-fluidic chip,
Controllable space is big, realizes that a core is multi-purpose, often solves the matter of great urgency at the crucial moment of needs.Of the invention utilizes transformation miniflow
Only it is several that channel need to can be realized to the simple reduction and assembling of common materials and original part in the method that control channel prepares millimeter grade particles
The preparation of what complicated multiplicity and durable handy professional droplet generator, it is not necessary to different channels are prepared for different use demands,
Greatly reduce and avoid research user and repeats and extra labour.Meanwhile conventional method production complex pipeline is more difficult, packet
Nearest laser direct-writing and 3D printing technique are included, application in the chips all has severe bottleneck, and printing has special want to material
It asks, process is slow, it is difficult to realize fine and close bubble-free, optical clarity extreme influence.Of the invention utilizes transformation microfluidic channel
The method for preparing millimeter grade particles can produce complex pipeline channel using simple technique, not only greatly reduce miniflow
The threshold difficulty for controlling chip manufacturing and repacking, has been greatly reduced experimental cost, to greatly improve the reality of micro-fluidic chip
Application benefit.
The method for preparing millimeter grade particles using transformation microfluidic channel of the invention, for millimeter grade particles or drop system
Standby middle large volume flow bring flow velocity fluctuates, and rheological characteristic, thermodynamic phase and the buoyancy of big partial size lotion itself
Great risk caused by effect etc. and uncontrollability, using the flow field that double-Y shaped channel is more stable, by specific to channel interior
The transformation of geometry realizes that a core is changeable, and a core is multi-purpose, and steady and continuous batch prepares hundred microns to several millimeters and waits not same amount
The particle or drop of grade partial size.
The method for preparing millimeter grade particles using transformation microfluidic channel of the invention, core are intended to through simple process pair
The transformation of micro-fluidic chip channel geometry prepares specific aim for different sized particles and provides required flow field, realizes that a core is more
Become, a core is multi-purpose, and the particle or drop of hundred microns to several millimeters partial sizes are prepared for steady and continuous batch.
Detailed description of the invention
Fig. 1 is a kind of the double-Y shaped micro- of method preparation that millimeter grade particles are prepared using transformation microfluidic channel of the invention
The basic channel design schematic diagram of fluidic chip；
Fig. 2 is a kind of the poly- of the embodiment 1 of method that millimeter grade particles are prepared using transformation microfluidic channel of the invention
Burnt and coflow combined type channel design schematic diagram；
Fig. 3 is prepared by a kind of embodiment 1 of method that millimeter grade particles are prepared using transformation microfluidic channel of the invention
Double emulsion optical microscope photograph figure；
Fig. 4 be a kind of embodiment 2 of method that millimeter grade particles are prepared using transformation microfluidic channel of the invention just
To double focusing channel design schematic diagram；
Fig. 5 is prepared by a kind of embodiment 2 of method that millimeter grade particles are prepared using transformation microfluidic channel of the invention
Double emulsion optical microscope photograph figure；
Fig. 6 is a kind of the anti-of the embodiment 3 of method that millimeter grade particles are prepared using transformation microfluidic channel of the invention
To double focusing channel design schematic diagram；
Fig. 7 is prepared by a kind of embodiment 3 of method that millimeter grade particles are prepared using transformation microfluidic channel of the invention
Double emulsion optical microscope photograph figure.
In figure, 1. channel, I 2. channel, II 3. channel, III 4. channel, IV 5. channel, V 6. tubular fitting, I 7. tubulose
II 8. tubular fitting of accessory, III 9. tubular fitting IV.
Specific embodiment
The present invention is discussed in detail with reference to the accompanying drawings and examples.
It is of the invention using transformation microfluidic channel prepare millimeter grade particles method the following steps are included:
A. the basic channel of micro-fluidic chip is prepared；
B. the tubular fitting in the basic channel of micro-fluidic chip is prepared；
C. tubular fitting is assembled in the basic channel of micro-fluidic chip；
D. particle is prepared.
The step a the following steps are included:
A1. the sheet glass of rectangular shape is lain in a horizontal plane in above aluminium foil, aluminium foil is upward along the side of sheet glass
Four sides of package sheet glass are folded, sheet glass is rolled into the hollow cuboid an of upper opening, obtains mold by aluminium foil
Performed polymer container defines length, height, the wide respectively X, Y, Z axis of hollow cuboid；
A2. surface is smooth, along the x axis the stepped increase of radius, stainless steel I with the straight sections such as N sections
Horizontal through mold performed polymer container, the horizontal symmetrical center line of stainless steel I is lower than the horizontal symmetrical of mold performed polymer container
Center line；In the horizontal symmetrical plane of stainless steel I, stainless steel is symmetrically fixed in the equal straight sections two sides of the second of stainless steel I
II and stainless steel III, stainless steel IV and stainless steel V, stainless steel are symmetrically fixed in the straight sections such as third of stainless steel I two sides
Stainless steel M-1 and stainless steel M is symmetrically fixed in the straight sections two sides such as the N of bar I, by fixed stainless steel, obtains required
The basic channel template of micro-fluidic chip；
Along X-axis negative direction, the angle between stainless steel II and stainless steel III is 120 °, stainless steel IV and stainless steel
Angle between bar V is 120 °, until the angle between stainless steel M-1 and stainless steel M is 120 °；N >=5, M >=5；
A3. polymer and curing agent are uniformly mixed, form prepolymer solution, prepolymer solution is evacuated to
Bubble-free is poured into mold performed polymer container made of step a1, again takes out the prepolymer solution in mold performed polymer container
Mold performed polymer container is put in a vacuum drying oven to bubble-free, solidifies 2 ~ 3h at 70 DEG C, micro-fluidic chip is made by vacuum
Basic channel die；
A4. the basic channel die of micro-fluidic chip is ultrasonically treated 30min, removes the aluminium foil of die surface and the glass of lower section
The stainless steel of mould inside is rotated and is extracted by glass piece, obtains micro-fluidic chip blank, cuts micro-fluidic chip blank shape,
The basic channel of micro-fluidic chip is obtained, the channel that stainless steel I is formed is channel I 1, and the channel that stainless steel II is formed is channel
II 2, the channel that stainless steel III is formed is channel III 3, and the channel that stainless steel IV is formed is channel IV 4, V shape of stainless steel
At channel be channel V 5, until stainless steel M formed channel be channel M.
The step b the following steps are included:
B1. tubular fitting I 6 is prepared, tubular fitting I is hollow circular tube, and the outer diameter of hollow circular tube is less than I 1 entrance of channel
Internal diameter；
B2. tubular fitting II 7 is prepared, tubular fitting II is the conical pipe of hollow circle, and the outside diameter of conical pipe is stainless
The internal diameter of the straight sections such as I third ladder of steel pole；
B3. tubular fitting III 8 is prepared, tubular fitting III is the conical pipe of hollow circle, and the outside diameter of conical pipe is stainless
The internal diameter of the straight sections such as I fourth order ladder of steel pole；
B4. tubular fitting IV 9 is prepared, tubular fitting IV is the conical pipe of hollow circle, and the outside diameter of conical pipe is stainless
The internal diameter of the straight sections such as the 5th ladder of steel pole I；
B5. continue to prepare tubular fitting, until the outside diameter of the conical pipe of tubular fitting is I N ladder of stainless steel
The internal diameter of equal straight sections.
The step c the following steps are included:
C1. tubular fitting I 6 is inserted into channel I 1, one end of tubular fitting I 6 is fixed on the inlet in channel I 1, separately
X-axis positive direction horizontal extension of the one end along channel I 1；
C2., the big end of the conical pipe of tubular fitting II 7 is inserted into channel I 1 at the straight sections such as the N in channel I 1, tubulose is matched
The small end of the conical pipe of part II 7 is towards X-axis positive direction, and tubular fitting II 7 is along the Forward of X-axis negative direction up to tubular fitting II 7
Big end is stuck on the straight sections such as third, obtains focusing and coflow combined type channel；
C3., the big end of the conical pipe of tubular fitting III 8 is inserted into channel I 1 at the straight sections such as the N in channel I 1, tubulose is matched
The small end of the conical pipe of part III 8 is towards X-axis positive direction, and tubular fitting III 8 is along the Forward of X-axis negative direction until big end is stuck in 4th etc.
On straight section, positive double focusing channel is obtained；
Or the small end of the conical pipe of tubular fitting VI 9 is inserted into channel I 1 at the straight sections such as the N in channel I 1, tubulose is matched
The big end of the conical pipe of part VI 9 is towards X-axis positive direction, and tubular fitting VI 9 is along the Forward of X-axis negative direction until big end is stuck in 5th etc.
On straight section, reversed double focusing channel is obtained；
C4. continue that tubular fitting is installed, until obtaining required channel.
The step d the following steps are included:
D1. fluid I is passed through in tubular fitting I 6；
D2. it is passed through fluid II simultaneously in channel II and channel III, the fluid II and fluid I are immiscible；
D3. it is passed through fluid III simultaneously in channel VI and channel V, the fluid III and fluid II are immiscible；
D4. it collects to obtain milk particle at the straight sections such as N；
D5. milk particle is solidified, obtains particle.
The equal straight sections outer diameter of the stainless steel I is millimeter magnitude.
The polymer is dimethyl silicone polymer, and curing agent is polymethyl methacrylate, and the performed polymer is molten
The mass ratio of dimethyl silicone polymer and polymethyl methacrylate in liquid is 10:1.
The stainless steel stainless steel tube, stainless steel sleeve pipe, glass rod, glass tube, teflon rod or poly- four
The replacement of one of fluoride tubes.
The stainless steel passes through the gap left on aluminium foil when aluminium foil and is sealed with silicon mud；
The stainless steel I punches in advance, by stainless steel II, stainless steel III, stainless steel IV, stainless steel V
It is fixed until stainless steel M is inserted directly into corresponding hole.
The material of the tubular fitting is one of polyfluortetraethylene pipe, glass tube or stainless steel tube.
Experimental method used in following embodiments is conventional method unless otherwise specified.Institute in following embodiments
The material used, reagent etc. commercially obtain unless otherwise specified.
Test parameters in embodiment is shown in Table 1.
Embodiment 1
Embodiment 1 is to prepare double Y made of the method for millimeter grade particles using transformation microfluidic channel using of the invention
Type micro-fluidic chip focuses and coflow combined type channel design and its double emulsion and hollow sphere application and preparation example.
The sheet glass of rectangular shape is lain in a horizontal plane in above aluminium foil, aluminium foil is folded up along the side of sheet glass
Four sides of sheet glass are wrapped up, sheet glass is rolled into the hollow cuboid an of upper opening, obtains mold pre-polymerization by aluminium foil
Body container defines length, height, the wide respectively X, Y, Z axis of hollow cuboid；Surface is smooth, along the x axis radius be in ladder
It is that shape increases, with punching forms stainless steel I in advance on the straight sections such as the stainless steel second of the straight sections such as five sections and third, five sections
Equal straight sections radius is respectively 1.15mm, 2mm, 2.5mm, 3mm and 3.5mm；Stainless steel I is held horizontal through mold performed polymer
Device, the horizontal symmetrical center line of stainless steel I are lower than the horizontal symmetrical center line of mold performed polymer container；In stainless steel I
In horizontal symmetrical plane, stainless steel II and stainless steel III, stainless steel are symmetrically fixed in the equal straight sections two sides of the second of stainless steel I
Stainless steel IV and stainless steel V are symmetrically fixed in the straight sections such as third of bar I two sides；Along X-axis negative direction, stainless steel II and not
Angle between rust steel pole III is 120 °, and the angle between stainless steel IV and stainless steel V is 120 °, and it is negative to form X-axis in the same direction
The double-Y shaped template of direction opening.Stainless steel II, stainless steel III, stainless steel IV and V radius of stainless steel are
1.15mm is inserted directly on stainless steel I in corresponding hole fixed.When passing through aluminium foil with silicon mud sealing stainless steel on aluminium foil
The gap left.
Dimethyl silicone polymer is uniformly mixed with polymethyl methacrylate 10:1 in mass ratio, it is molten to form performed polymer
Liquid is evacuated to bubble-free, pours into mold performed polymer container, is evacuated to bubble-free again, is integrally placed on vacuum oven
In, solidify 2h at 70 DEG C, the basic channel die of micro-fluidic chip is made, the channel that stainless steel I is formed is channel I 1, stainless
The channel that steel pole II is formed is channel II 2, and the channel that stainless steel III is formed is channel III 3, the channel that stainless steel IV is formed
For channel IV 4, the channel that stainless steel V is formed is channel V 5；Mold is ultrasonically treated 30min, removes the aluminium of die surface
The stainless steel of mould inside is rotated and is extracted, obtains micro-fluidic chip blank by the sheet glass of foil and lower section；Cut micro-fluidic core
Piece blank shape obtains the basic channel of double-Y shaped micro-fluidic chip, sees Fig. 1.
The syringe needle for choosing outer diameter 1.28mm, internal diameter 0.9mm, is cut into the needle tubing of length 2.5cm, and section is repaired
It is whole smooth, obtain tubular fitting I 6；The polytetrafluoroethylene (PTFE) conical pipe of hollow circle is chosen, is trimmed, obtaining portlet internal diameter is
1.5mm, outer diameter 2.3mm, large port outer diameter are the nozzle of 5mm, form tubular fitting II 7；Tubular fitting I 6 is inserted into channel I
In 1, one end of tubular fitting I 6 is fixed on the inlet in channel I 1, and horizontal direction of the other end along channel I 1 extends；By tubulose
The big end of the conical pipe of accessory II 7 is inserted into channel I 1 at the 5th equal straight sections in channel I 1, along the Forward of X-axis negative direction until big end
It is stuck on the straight sections such as third, obtains focusing and coflow combined type channel design, see Fig. 2.
With the pure water (H of volume ratio 100:342O) with heavy water (D2O mixed solution) is fluid I；By divinylbenzene
(DVB) ratio of monomer and solvent dibutyl phthalate (DBP) 1:5 by volume are uniformly mixed, with mass fraction 0.8%
Sorbitan oleate (SPAN80) be emulsifier and mass fraction 3% phenyl it is bis- (2,4,6- trimethylbenzoyl)
Phosphine oxide (BAPO) is initiator, stirs 10 minutes and is uniformly mixed under conditions of logical argon gas protection, gained mixed solution is fluid
Ⅱ；With polyvinyl alcohol (PVA, the M of mass fraction 5%w=88000 g/mol) aqueous solution be fluid III；It will with micro-injection pump
Fluid I is passed through tubular fitting I (6), and fluid II is passed through channel II and channel III simultaneously, and fluid III is passed through channel VI and channel simultaneously
Ⅴ；Adjusting fluid I, fluid II and III volume flow rate of fluid is respectively 4.17 μ L/s, 1.36 μ L/s and 45.01 μ L/s, continuous steady
It is fixed that dual drop (W is prepared in batches1/O/W2), milk particle is collected in weighing bottle at the 5th equal straight sections, will collect milk particle
Weighing bottle is placed in test size under optical microscopy, outer diameter 5.457mm, and wall thickness is 465 μm, size standard deviation less than 1 ‰,
See Fig. 3.
Above-mentioned milk particle is transported in the cylindrical bottle of rate level rotation of 5rpm through glass pipe, choosing wavelength is
365nm, intensity of illumination are 3.7 W/cm3Ultraviolet lamp drop is irradiated, keep cylindrical bottle continue keep 5rpm rate
It is rotated horizontally；Multiple drop becomes milky from transparent, continues illumination and was allowed to be fully cured to 45 minutes；By wet gel ball
It is transferred in ethanol solution and carries out displacement 3-5 days, change an ethanol solution daily；Gel ball after displacement is put into CO2It is super to face
Boundary's drying equipment is dried to arrive complete polydivinylbenezene (PDVB) hollow sphere, outer diameter 5.411mm, wall thickness
461 μm, with batch product ball size standard deviation less than 2 ‰.
Embodiment 2
Embodiment 2 is to prepare double Y made of the method for millimeter grade particles using transformation microfluidic channel using of the invention
Type micro-fluidic chip forward direction double focusing channel and its double emulsion and hollow sphere application and preparation example.
Embodiment 2 and the embodiment of embodiment 1 are essentially identical, and the main distinction is, obtain in embodiment 1 double-Y shaped
On micro-fluidic chip combined type channel base, increase tubular fitting III 8.Refer specifically to choose the polytetrafluoroethylene (PTFE) taper of hollow circle
Pipe, trimming, obtaining portlet internal diameter is 2.5mm, and outer diameter 3.3mm, large port outer diameter is the nozzle of 6mm, forms tubular fitting
Ⅲ8；The big end of the conical pipe of tubular fitting III 8 is inserted into channel I 1 at the 5th equal straight sections in channel I 1, before X-axis negative direction
It moves and is waited on straight sections up to big end is stuck in the 4th, obtain positive double focusing channel design, see Fig. 4.
Using the method in similar embodiment 1, above-mentioned gained forward direction double focusing channel is used for continuous-stable batch and is prepared
Partial size is less than the millimeter grade particles of gained milk particle and microballoon in embodiment 1.Adjust fluid I, III volume flow rate of fluid II and fluid
Dual drop (W is prepared in respectively 4.17 μ L/s, 1.36 μ L/s and 25.11 μ L/s, continuous-stable batch1/O/W2),
Milk particle is collected in weighing bottle at five equal straight sections, the weighing bottle for collecting milk particle is placed in test size under optical microscopy, outer diameter
For 3.255mm, wall thickness is 185 μm, and size standard deviation is shown in Fig. 5 less than 1.5 ‰.After cured, displacement and drying, gathered
Divinylbenzene (PDVB) hollow sphere, outer diameter 3.223mm, are less than with batch product ball size standard deviation by 184 μm of wall thickness
2.5‰。
Embodiment 3
Embodiment 3 is to prepare double Y made of the method for millimeter grade particles using transformation microfluidic channel using of the invention
The reversed double focusing channel of type micro-fluidic chip and its double emulsion and hollow sphere application and preparation example.
Embodiment 3 and the embodiment of embodiment 1 are essentially identical, and the main distinction is, by the syringe needle in embodiment 1
Head changes outer diameter 0.7mm, internal diameter 0.5mm into, obtains being similar to double-Y shaped micro-fluidic chip combined type channel obtained in embodiment 1
Structure, and on this basis, increase tubular fitting IV 9.It refers specifically to choose the polytetrafluoroethylene (PTFE) conical pipe of hollow circle, trims, obtain
It is 1mm to portlet internal diameter, large port outer diameter is the nozzle of 7mm, forms tubular fitting IV 9；By the conical pipe of tubular fitting IV 9
Small end be inserted into channel I 1 at the 5th equal straight sections in channel I 1, along the Forward of X-axis negative direction until big end is stuck in the 5th equal straight sections
On, reversed double focusing channel design is obtained, sees Fig. 6.
Using the method in similar embodiment 1, the reversed double focusing channel of above-mentioned gained is used for continuous-stable batch and is prepared
Submillimeter/millimeter grade particles of the partial size much smaller than gained milk particle and microballoon in embodiment 1.Adjust fluid I, fluid II and fluid III
Volume flow rate is respectively 4.17 μ L/s, 1.36 μ L/s and 8.3 μ L/s, and dual drop (W is prepared in continuous-stable batch1/O/
W2), milk particle is collected in weighing bottle at the 5th equal straight sections, and the weighing bottle for collecting milk particle is placed under optical microscopy and tests ruler
Very little, outer diameter 0.812mm, wall thickness is 86 μm, and size standard deviation is shown in Fig. 7 less than 4 ‰.After cured, displacement and drying, obtain
To polydivinylbenezene (PDVB) hollow sphere, outer diameter 0.806mm, 84 μm of wall thickness, with criticizing, product ball size standard deviation is small
In 5 ‰.
Stainless steel I, syringe needle tube and polytetrafluoroethylene (PTFE) conical pipe bore in above-described embodiment can be according to target liquid
Drop or particle size accordingly increase or reduce, complete using the basic channel of gained micro-fluidic chip, simple operations in embodiment 1
It is converted at channel design, is advantageously used in the preparation of the particle/drop of hundred microns to several millimeters grade sizes.In above-described embodiment not
Become rusty steel pole I and stainless steel II, III, IV and V available stainless steel tube, stainless steel sleeve pipe, glass rod, glass tube, polytetrafluoroethyl-ne
Alkene bar or polyfluortetraethylene pipe replacement.
The present invention is not limited to above-mentioned specific embodiment, person of ordinary skill in the field from the above idea,
Without creative labor, made various transformation are within the scope of the present invention.
Claims (6)
1. a kind of method for preparing millimeter grade particles using transformation microfluidic channel, which is characterized in that this method includes following step
It is rapid:
A. the basic channel of micro-fluidic chip is prepared；
B. the tubular fitting in the basic channel of micro-fluidic chip is prepared；
C. tubular fitting is assembled in the basic channel of micro-fluidic chip；
D. particle is prepared；
The step a the following steps are included:
A1. the sheet glass of rectangular shape is lain in a horizontal plane in above aluminium foil, aluminium foil is folded up along the side of sheet glass
Four sides of sheet glass are wrapped up, sheet glass is rolled into the hollow cuboid an of upper opening, obtains mold pre-polymerization by aluminium foil
Body container defines length, height, the wide respectively X, Y, Z axis of hollow cuboid；
A2. surface is smooth, along the x axis the stepped increase of radius, stainless steel with the straight sections such as N sections I it is horizontal
Across mold performed polymer container, the horizontal symmetrical center line of stainless steel I is lower than the horizontal symmetrical center of mold performed polymer container
Line；In the horizontal symmetrical plane of stainless steel I, II He of stainless steel is symmetrically fixed in the equal straight sections two sides of the second of stainless steel I
Stainless steel IV and stainless steel V, stainless steel I are symmetrically fixed in stainless steel III, the straight sections such as third of stainless steel I two sides
The straight sections two sides such as N symmetrically fix stainless steel M-1 and stainless steel M, by fixed stainless steel, obtain required miniflow
Control the basic channel template of chip；
Along X-axis negative direction, the angle between stainless steel II and stainless steel III is 120 °, stainless steel IV and stainless steel V
Between angle be 120 °, until angle between stainless steel M-1 and stainless steel M is 120 °；N >=5, M >=5；
A3. polymer and curing agent are uniformly mixed, form prepolymer solution, prepolymer solution is evacuated to no gas
Bubble, pours into mold performed polymer container made of step a1, again vacuumizes the prepolymer solution in mold performed polymer container
To bubble-free, mold performed polymer container is put in a vacuum drying oven, solidifies 2 ~ 3h at 70 DEG C, it is basic that micro-fluidic chip is made
Channel die；
A4. the basic channel die of micro-fluidic chip is ultrasonically treated 30min, removes the aluminium foil of die surface and the glass of lower section
The stainless steel of mould inside is rotated and is extracted by piece, obtains micro-fluidic chip blank, is cut micro-fluidic chip blank shape, is obtained
To the basic channel of micro-fluidic chip, the channel that stainless steel I is formed is channel I (1), and the channel that stainless steel II is formed is channel
II (2), the channel that stainless steel III is formed are channel III (3), and the channel that stainless steel IV is formed is channel IV (4), stainless steel
The channel that bar V is formed is channel V (5), until the channel that stainless steel M is formed is channel M；
The step b the following steps are included:
B1. tubular fitting I (6) is prepared, tubular fitting I is hollow circular tube, and the outer diameter of hollow circular tube is less than channel I (1) entrance
Internal diameter；
B2. tubular fitting II (7) is prepared, tubular fitting II is the conical pipe of hollow circle, and the outside diameter of conical pipe is stainless steel
The internal diameter of the straight sections such as I third ladder of bar；
B3. tubular fitting III (8) is prepared, tubular fitting III is the conical pipe of hollow circle, and the outside diameter of conical pipe is stainless steel
The internal diameter of the straight sections such as I fourth order ladder of bar；
B4. tubular fitting IV (9) is prepared, tubular fitting IV is the conical pipe of hollow circle, and the outside diameter of conical pipe is stainless steel
The internal diameter of the straight sections such as the 5th ladder of bar I；
B5. continue to prepare tubular fitting, until the outside diameter of the conical pipe of tubular fitting is that I N ladder of stainless steel etc. is straight
The internal diameter of section；
The step c the following steps are included:
C1. tubular fitting I (6) is inserted into channel I (1), one end of tubular fitting I (6) is fixed on the entrance in channel I (1)
Place, X-axis positive direction horizontal extension of the other end along channel I (1)；
C2., the big end of the conical pipe of tubular fitting II (7) is inserted into channel I (1), tubulose at the straight sections such as the N in channel I (1)
The small end of the conical pipe of accessory II (7) is towards X-axis positive direction, and tubular fitting II (7) is along the Forward of X-axis negative direction until tubular fitting
The big end of II (7) is stuck on the straight sections such as third, obtains focusing and coflow combined type channel；
C3., the big end of the conical pipe of tubular fitting III (8) is inserted into channel I (1), tubulose at the straight sections such as the N in channel I (1)
The small end of the conical pipe of accessory III (8) is towards X-axis positive direction, and tubular fitting III (8) is along the Forward of X-axis negative direction until big end is stuck in
On 4th equal straight sections, positive double focusing channel is obtained；
Or the small end of the conical pipe of tubular fitting VI (9) is inserted into channel I (1), tubulose at the straight sections such as the N in channel I (1)
The big end of the conical pipe of accessory VI (9) is towards X-axis positive direction, and tubular fitting VI (9) is along the Forward of X-axis negative direction until big end is stuck in
On 5th equal straight sections, reversed double focusing channel is obtained；
C4. continue that tubular fitting is installed, until obtaining the channel with the straight sections such as N sections；
The step d the following steps are included:
D1. fluid I is passed through in tubular fitting I (6)；
D2. it is passed through fluid II simultaneously in channel II and channel III, the fluid II and fluid I are immiscible；
D3. it is passed through fluid III simultaneously in channel VI and channel V, the fluid III and fluid II are immiscible；
D4. it collects to obtain milk particle at the straight sections such as N；
D5. milk particle is solidified, obtains particle.
2. the method according to claim 1 for preparing millimeter grade particles using transformation microfluidic channel, which is characterized in that institute
The equal straight sections outer diameter for the stainless steel I stated is millimeter magnitude.
3. the method according to claim 1 for preparing millimeter grade particles using transformation microfluidic channel, which is characterized in that institute
The polymer stated is dimethyl silicone polymer, and curing agent is polymethyl methacrylate, poly- two in the prepolymer solution
The mass ratio of methylsiloxane and polymethyl methacrylate is 10:1.
4. the method according to claim 1 for preparing millimeter grade particles using transformation microfluidic channel, which is characterized in that institute
In stainless steel stainless steel tube, stainless steel sleeve pipe, glass rod, glass tube, teflon rod or the polyfluortetraethylene pipe stated
A kind of replacement.
5. the method according to claim 1 for preparing millimeter grade particles using transformation microfluidic channel, which is characterized in that institute
The stainless steel stated passes through the gap left on aluminium foil when aluminium foil and is sealed with silicon mud；
The stainless steel I punches in advance, by stainless steel II, stainless steel III, stainless steel IV, stainless steel V until
Stainless steel M is inserted directly into corresponding hole fixed.
6. the method according to claim 1 for preparing millimeter grade particles using transformation microfluidic channel, which is characterized in that institute
The material for the tubular fitting stated is one of polyfluortetraethylene pipe, glass tube or stainless steel tube.
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| CN110787846B (en) * | 2019-11-05 | 2021-04-16 | 华中科技大学 | One-step double-layer micro-droplet generation device and method |
| CN112569878B (en) * | 2020-01-21 | 2021-09-28 | 苏州恒瑞宏远医疗科技有限公司 | Equipment for preparing polyvinyl alcohol embolism microsphere with uniform grain diameter and production process thereof |
| CN111504406B (en) * | 2020-05-15 | 2022-03-29 | 大连理工大学 | Flow detection chip and detection method for ultramicro small-flow liquid |
| CN111569798B (en) * | 2020-05-27 | 2021-08-17 | 中山大学 | Degradable core-shell calcium alginate oxide gel microspheres and preparation method and application thereof |
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| CN104531519A (en) * | 2015-01-30 | 2015-04-22 | 中国科学院苏州生物医学工程技术研究所 | Microfluidic detection chip based on droplet experiments |
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| JP5072057B2 (en) * | 2005-08-22 | 2012-11-14 | 東ソー株式会社 | Microcapsule manufacturing method using microchannel structure |
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