CN106669556A - Method for preparing millimeter-scale granules by changing microfluidic channels - Google Patents
Method for preparing millimeter-scale granules by changing microfluidic channels Download PDFInfo
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Abstract
The invention provides a method for preparing millimeter-scale granules by changing microfluidic channels. The method comprises the following steps: a. preparing a microfluidic chip basic channel; b. preparing tubular parts of the microfluidic chip basic channel; c. assembling the tubular parts in the microfluidic chip basic channel; d. preparing the granules. After the method is used, different types of more complicated microfluidic channel structures are obtained by utilizing a simple processing and assembling technology, so that targeted flow fields are provided for preparation of granules of different magnitudes, and the fact that one core is varied and multifunctional is realized; the method has the characteristics of high in channel geometry transformation degree, wide application size range, high controllability, low consumption, efficiency and the like, thus being used for stably and continuously obtaining mono-dispersed granules or droplets with particle sizes of hundred microns to several millimeters in batches.
Description
Technical field
The invention belongs to micro-/milli fluidics application field, and in particular to one kind prepares milli using microfluidic channel is converted
The method of scale particles.
Background technology
Micro-capsule and laser fusion target fuel are loaded in microreactor, realizing controlled-release medicine and catalyst carrier, bioactivity kind
In the fields such as container, hundred microns to several millimeters particles/drop are widely used.Traditional stirring, spraying and film emulsification etc. " from
Top is downward " material and chemical method be difficult to batch and prepare that single dispersing degree is high and bulky grain/drop of structure-controllable, it is and past
More, the time and effort consuming toward step.It is near during the last ten years, micro-/milli fluidics be the various fields applications such as biological, chemistry and material and
One of focus of research.Successively T-shaped passage is developed（T-shaped junction）, focus channel（Flow-focusing）With
Co-flow pathway（Co-flowing）Deng the microchannel of three basic forms of it, these three basic channel designs decide three kinds of basic flows
Type, its flow pattern feature, miniflow bulk-mode and drop forming mechanism have obtained widely studied, in microring array and micron particles/liquid
Dripping is standby etc., and aspect is widely used.Compare, the micro-/milli fluidics of " bottom-up " for particle/drop particle diameter with it is several
What regulation and control have unique advantage, further investigate its application technology in terms of millimeter magnitude particle/drop preparation have it is important
Realistic meaning.
Compared with prepared by micro/nano level particle/drop, the preparation of millimeter grade particles/drop need to generally face large volume flow
Great risk that flow velocity fluctuation, the rheological characteristic of big emulsion itself, thermodynamic phase and buoyancy effect for bringing etc. are caused and
Uncontrollability.To prepare grade polymer microballoon and microcapsules, three nozzle milk particles of American National ignition center development occur
Device technology, had once been once a kind of classical way of association area, but the requirement of its assembly precision is high, is gradually substituted.Chinese engineering
Physical study institute has successively developed double-T shaped, double ten types, the double-Y shaped and dual micro-fluidic passage technology of coflow formula.In contrast, double Y
It is possible to prevente effectively from hydrodynamics stationary point, flow field is more sane, control and whole drop body for different phase fluids for type passage
Long-pending ability of regulation and control is stronger, is advantageously implemented the accurate customization of size and particle geometric.In addition W. Engl et al. focus on commercial quantities
Change and reduces cost, utilize " tubular type milli stream control " to prepare millimeter particles and drop, and emphasized development correlation technique have compared with
Big prospect and practical significance.However, micro-fluidic chip channel geometry is continuous-stable and forming drop and effectively controlling it to tie
The key of structure and size.At present, an applicable target size range of chip is narrower, and channel geometry is fixed, and user is difficult to root
It is multiplex according to the core of practical application request one.Meanwhile, the preparation processing technology of micro-fluidic chip is complicated, the bonding and photoetching skill of microchannel
Art threshold is higher, costly, assembling not easy to remove, and inconvenience cleaning, the repeat usage of chip is low, and service life is shorter.Especially
It is that conventional method making 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, development is needed badly a kind of using the method that microfluidic channel prepares millimeter grade particles/drop is converted, using simple
Processing and packaging technology obtain complex different type microfluidic channel, and low-consumption high-efficiency a, core is changeable, and a core is multiplex, surely
Determine continuous batch and obtain the broader monodisperse particles/drop of size range.
The content of the invention
The technical problems to be solved by the invention are to provide and a kind of prepare millimeter grade particles using converting microfluidic channel
Method.
It is of the invention to be comprised the following steps using converting microfluidic channel and prepare the method for millimeter grade particles：
A. the basic passage of micro-fluidic chip is prepared；
B. the tubular fitting of the basic passage of micro-fluidic chip is prepared；
C. tubular fitting is assembled in the basic passage of micro-fluidic chip；
D. particle is prepared.
Described step a is comprised the following steps：
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 a hollow cuboid for upper opening, obtains mould pre-polymerization by aluminium foil
Body container, defines length, height, the respectively X, Y, Z axis wide of hollow cuboid；
A2. by surface it is smooth, along the stepped increase of X-direction radius, with the level of the stainless steel of straight section I such as N sections
Through mould performed polymer container, the horizontal symmetrical center of the horizontal symmetrical center line less than mould performed polymer container of stainless steel I
Line；In the horizontal symmetrical plane of stainless steel I, the He of stainless steel II is symmetrically fixed in the second grade straight section both sides of stainless steel I
Stainless steel IV and stainless steel V, stainless steel I are symmetrically fixed in stainless steel III, the third straight section both sides of stainless steel I
The straight section both sides such as N symmetrically fix stainless steel M-1 and stainless steel M, by fixed stainless steel, obtain required miniflow
The control basic passage 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 the angle between stainless steel M-1 and stainless steel M is 120 °；N >=5, M >=5；
A3. polymer is uniformly mixed with curing agent, forms prepolymer solution, prepolymer solution is evacuated to without gas
Bubble, pours into the mould performed polymer container that step a1 is made, and again vacuumizes the prepolymer solution in mould performed polymer container
To bubble-free, mould performed polymer container is placed in vacuum drying chamber, 2 ~ 3h is solidified at 70 DEG C, be made micro-fluidic chip basic
Channel die；
A4. by the micro-fluidic chip ultrasonically treated 30min of basic channel die, the aluminium foil of die surface and the glass of lower section are removed
Piece, the stainless steel of mould inside is rotated and is extracted, and obtains micro-fluidic chip blank, cuts micro-fluidic chip blank shape, is obtained
To the basic passage of micro-fluidic chip, the passage that stainless steel I is formed is passage I, and the passage that stainless steel II is formed is passage II,
The passage that stainless steel III is formed is passage III, and the passage that stainless steel IV is formed is passage IV, and it is logical that stainless steel V is formed
Road is passage V, until the passage that stainless steel M is formed is passage M.
Described step b is comprised the following steps：
B1. tubular fitting I is prepared, tubular fitting I is hollow circular tube, the internal diameter of the external diameter less than the entrance of passage I of hollow circular tube；
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 steel I
The internal diameter of the straight sections such as the 3rd ladder；
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 steel I
The internal diameter of the straight sections such as fourth order ladder；
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 steel I
The internal diameter of the straight sections such as the 5th ladder；
B5. continue to prepare tubular fitting, until the outside diameter of the conical pipe of tubular fitting is straight N ladders of stainless steel I etc.
The internal diameter of section.
Described step c is comprised the following steps：
C1. in tubular fitting I being inserted into passage I, one end of tubular fitting I is fixed on the porch of passage I, and the other end is along logical
The X-axis positive direction in road I is horizontal-extending；
C2. passage I is inserted into the big end of the conical pipe of tubular fitting II at the straight section such as N of passage I, tubular fitting II
Towards X-axis positive direction, tubular fitting II is along the reach of X-axis negative direction until the big end of tubular fitting II is stuck in for the small end of conical pipe
On third straight section, obtain focusing on and coflow combined type passage；
C3. passage I is inserted into the big end of the conical pipe of tubular fitting III at the straight section such as N of passage I, tubular fitting III
The small end of conical pipe is stuck on fourth class straight section along the reach of X-axis negative direction towards X-axis positive direction, tubular fitting III until holding greatly,
Obtain positive double focusing passage；
Or the small end of the conical pipe of tubular fitting VI is inserted into passage I at the straight section such as N of passage I, tubular fitting VI
The big end of conical pipe is stuck on the 5th grade straight section along the reach of X-axis negative direction towards X-axis positive direction, tubular fitting VI until holding greatly,
Obtain reverse double focusing passage；
C4. continue that tubular fitting is installed, until obtaining required passage.
Described step d is comprised the following steps：
D1. it is passed through fluid I in tubular fitting I；
D2. fluid II is passed through simultaneously in passage II and passage III, described fluid II is immiscible with fluid I；
D3. fluid III is passed through simultaneously in passage VI and passage V, described fluid III is immiscible with fluid II；
D4. collected at the straight sections such as N and obtain milk particle；
D5. milk particle is solidified, is obtained particle.
The straight section external diameter that waits of described stainless steel I is millimeter magnitude.
Described polymer is dimethyl silicone polymer, and curing agent is polymethyl methacrylate, and described performed polymer is molten
Dimethyl silicone polymer and the mass ratio of polymethyl methacrylate in liquid are 10:1.
Described stainless steel stainless steel tube, stainless steel sleeve pipe, glass rod, glass tube, teflon rod or poly- four
A kind of replacement in fluoride tubes.
Described stainless steel passes through the gap left on aluminium foil during aluminium foil to be sealed with silicon mud；
Described stainless steel I punches in advance, by stainless steel II, stainless steel III, stainless steel IV, stainless steel V until
Stainless steel M is fixed in being inserted directly into corresponding hole.
The material of described tubular fitting is the one kind in polyfluortetraethylene pipe, glass tube or stainless steel tube.
Of the invention utilization converts the method that microfluidic channel prepares millimeter grade particles, 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
Need voluntarily to process, quick detachable and assembling is easy to clean, can repeatedly use, be easily assembled into various all kinds of different complexity journeys
The micro-fluidic pipeline of degree.
Of the invention utilization converts the method that microfluidic channel prepares millimeter grade particles, according to different magnitude of target size
Demand carries out the conversion of channel geometry and size, and the target size of wider range is obtained using same micro-fluidic chip,
Controllable space is big, realizes that a core is multiplex, often solves the matter of great urgency at the crucial moment for needing.Of the invention utilization converts miniflow
The method that control passage prepares millimeter grade particles only need to be to the simple reduction and assembling of common materials and original paper, you can realize that passage is several
The preparation of what complicated various and durable handy professional droplet generator, it is not necessary to for different use demands prepare different passages,
Greatly reduce and avoid research user to repeat and unnecessary work.Meanwhile, conventional method making complex pipeline is more difficult, bag
Nearest laser direct-writing and 3D printing technique is included, application in the chips all has severe bottleneck, and printing has special wanting to material
Ask, process is slow, it is difficult to realize fine and close bubble-free, optical clarity extreme influence.Of the invention utilization converts microfluidic channel
The method for preparing millimeter grade particles, complex pipeline passage can be produced using simple technique, not only greatly reduce miniflow
Control chip manufacturing and the threshold difficulty of repacking, have been greatly reduced experimental cost, so as to greatly improve the reality of micro-fluidic chip
Application benefit.
Of the invention utilization converts the method that microfluidic channel prepares millimeter grade particles, for millimeter grade particles or drop system
The flow velocity that standby middle large volume flow brings fluctuates, and the rheological characteristic of particle diameter emulsion itself, thermodynamic phase and buoyancy greatly
Great risk and uncontrollability that effect etc. is caused, using the flow field that double-Y shaped passage is more stable, by specific to channel interior
The conversion of geometry, realizes that a core is changeable, and a core is multiplex, and steady and continuous batch prepares hundred microns to the not same amount such as several millimeters
The particle or drop of level particle diameter.
Of the invention utilization converts the method that microfluidic channel prepares millimeter grade particles, and core is intended to by simple process pair
The conversion of micro-fluidic chip channel geometry, for different sized particles prepare flow field needed for specific aim is provided, realizes that a core is more
Become, a core is multiplex, hundred microns of particles or drop to several millimeters particle diameter are prepared for steady and continuous batch.
Brief description of the drawings
Fig. 1 be it is of the invention it is a kind of using convert microfluidic channel prepare millimeter grade particles method prepare it is double-Y shaped micro-
The basic channel design schematic diagram of fluidic chip；
Fig. 2 be it is of the invention it is a kind of using convert microfluidic channel prepare millimeter grade particles method embodiment 1 focusing and
Coflow combined type channel design schematic diagram；
Fig. 3 be it is of the invention it is a kind of using the embodiment 1 for converting the method that microfluidic channel prepares millimeter grade particles prepare it is double
Gravity emulsion optical microscope photograph figure；
Fig. 4 is that a kind of forward direction for utilizing the embodiment 2 for converting the method that microfluidic channel prepares millimeter grade particles of the invention is double
Focus channel structural representation；
Fig. 5 be it is of the invention it is a kind of using the embodiment 2 for converting the method that microfluidic channel prepares millimeter grade particles prepare it is double
Gravity emulsion optical microscope photograph figure；
Fig. 6 be it is of the invention it is a kind of using convert microfluidic channel prepare millimeter grade particles method embodiment 3 it is reverse double
Focus channel structural representation；
Fig. 7 be it is of the invention it is a kind of using the embodiment 3 for converting the method that microfluidic channel prepares millimeter grade particles prepare it is double
Gravity emulsion optical microscope photograph figure.
In figure, the 1. tubulose of I 2. passage of passage, II 3. passage, III 4. passage, IV 5. passage, V 6. tubular fitting I 7.
The tubular fitting IV of II 8. tubular fitting of accessory III 9..
Specific embodiment
The present invention is discussed in detail with reference to the accompanying drawings and examples.
It is of the invention to be comprised the following steps using converting microfluidic channel and prepare the method for millimeter grade particles：
A. the basic passage of micro-fluidic chip is prepared；
B. the tubular fitting of the basic passage of micro-fluidic chip is prepared；
C. tubular fitting is assembled in the basic passage of micro-fluidic chip；
D. particle is prepared.
Described step a is comprised the following steps：
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 a hollow cuboid for upper opening, obtains mould pre-polymerization by aluminium foil
Body container, defines length, height, the respectively X, Y, Z axis wide of hollow cuboid；
A2. by surface it is smooth, along the stepped increase of X-direction radius, with the level of the stainless steel of straight section I such as N sections
Through mould performed polymer container, the horizontal symmetrical center of the horizontal symmetrical center line less than mould performed polymer container of stainless steel I
Line；In the horizontal symmetrical plane of stainless steel I, the He of stainless steel II is symmetrically fixed in the second grade straight section both sides of stainless steel I
Stainless steel IV and stainless steel V, stainless steel I are symmetrically fixed in stainless steel III, the third straight section both sides of stainless steel I
The straight section both sides such as N symmetrically fix stainless steel M-1 and stainless steel M, by fixed stainless steel, obtain required miniflow
The control basic passage 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 the angle between stainless steel M-1 and stainless steel M is 120 °；N >=5, M >=5；
A3. polymer is uniformly mixed with curing agent, forms prepolymer solution, prepolymer solution is evacuated to without gas
Bubble, pours into the mould performed polymer container that step a1 is made, and again vacuumizes the prepolymer solution in mould performed polymer container
To bubble-free, mould performed polymer container is placed in vacuum drying chamber, 2 ~ 3h is solidified at 70 DEG C, be made micro-fluidic chip basic
Channel die；
A4. by the micro-fluidic chip ultrasonically treated 30min of basic channel die, the aluminium foil of die surface and the glass of lower section are removed
Piece, the stainless steel of mould inside is rotated and is extracted, and obtains micro-fluidic chip blank, cuts micro-fluidic chip blank shape, is obtained
To the basic passage of micro-fluidic chip, the passage that stainless steel I is formed is passage I 1, and the passage that stainless steel II is formed is passage II
2, the passage that stainless steel III is formed is passage III 3, and the passage that stainless steel IV is formed is passage IV 4, and stainless steel V is formed
Passage be passage V 5, until stainless steel M formed passage be passage M.
Described step b is comprised the following steps：
B1. tubular fitting I 6 is prepared, tubular fitting I is hollow circular tube, and the external diameter of hollow circular tube is interior less than the entrance of passage I 1
Footpath；
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 the 3rd ladders；
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；
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 I the 5th ladders；
B5. continue to prepare tubular fitting, until the outside diameter of the conical pipe of tubular fitting is straight N ladders of stainless steel I etc.
The internal diameter of section.
Described step c is comprised the following steps：
C1. by the insertion passage I 1 of tubular fitting I 6, one end of tubular fitting I 6 is fixed on the porch of passage I 1, the other end
X-axis positive direction along passage I 1 is horizontal-extending；
C2. passage I 1, tubular fitting II are inserted into the big end of the conical pipe of tubular fitting II 7 at the straight section such as N of passage I 1
, towards X-axis positive direction, tubular fitting II 7 is along the reach of X-axis negative direction until the big end of tubular fitting II 7 for the small end of 7 conical pipe
It is stuck on third straight section, obtains focusing on and coflow combined type passage；
C3. passage I 1, tubular fitting III are inserted into the big end of the conical pipe of tubular fitting III 8 at the straight section such as N of passage I 1
, towards X-axis positive direction, tubular fitting III 8 is along the reach of X-axis negative direction until big end is stuck in fourth class straight section for the small end of 8 conical pipe
On, obtain positive double focusing passage；
Or the small end of the conical pipe of tubular fitting VI 9 is inserted into passage I 1, tubular fitting VI at the straight section such as N of passage I 1
Towards X-axis positive direction, tubular fitting VI 9 is along the reach of X-axis negative direction until big end is stuck in the 5th grade straight section at the big end of 9 conical pipe
On, obtain reverse double focusing passage；
C4. continue that tubular fitting is installed, until obtaining required passage.
Described step d is comprised the following steps：
D1. it is passed through fluid I in tubular fitting I 6；
D2. fluid II is passed through simultaneously in passage II and passage III, described fluid II is immiscible with fluid I；
D3. fluid III is passed through simultaneously in passage VI and passage V, described fluid III is immiscible with fluid II；
D4. collected at the straight sections such as N and obtain milk particle；
D5. milk particle is solidified, is obtained particle.
The straight section external diameter that waits of described stainless steel I is millimeter magnitude.
Described polymer is dimethyl silicone polymer, and curing agent is polymethyl methacrylate, and described performed polymer is molten
Dimethyl silicone polymer and the mass ratio of polymethyl methacrylate in liquid are 10:1.
Described stainless steel stainless steel tube, stainless steel sleeve pipe, glass rod, glass tube, teflon rod or poly- four
A kind of replacement in fluoride tubes.
Described stainless steel passes through the gap left on aluminium foil during aluminium foil to be sealed with silicon mud；
Described stainless steel I punches in advance, by stainless steel II, stainless steel III, stainless steel IV, stainless steel V until
Stainless steel M is fixed in being inserted directly into corresponding hole.
The material of described tubular fitting is the one kind in polyfluortetraethylene pipe, glass tube or stainless steel tube.
Experimental technique used in following embodiments is conventional method unless otherwise specified.Institute in following embodiments
The material for using, reagent etc., unless otherwise specified, commercially obtain.
Test parameters in embodiment is shown in Table 1.
Embodiment 1
Embodiment 1 is using of the invention double-Y shaped micro- using convert that microfluidic channel prepares that the method for millimeter grade particles is made
Fluidic chip is focused on and coflow combined type channel design and its double emulsion and hollow ball 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 a hollow cuboid for upper opening, obtains mould pre-polymerization by aluminium foil
Body container, defines length, height, the respectively X, Y, Z axis wide of hollow cuboid；By surface it is smooth, along X-direction radius be in ladder
Shape increase, with the stainless steels of straight section second such as five sections and third straight section in advance punching form stainless steel I, five sections
1.15mm, 2mm, 2.5mm, 3mm and 3.5mm are respectively Deng straight section radius；Stainless steel I is held horizontal through mould performed polymer
Device, the horizontal symmetrical center line of the horizontal symmetrical center line less than mould performed polymer container of stainless steel I；In stainless steel I
In horizontal symmetrical plane, stainless steel II and stainless steel III, stainless steel are symmetrically fixed in the second grade straight section both sides of stainless steel I
Stainless steel IV and stainless steel V are symmetrically fixed in the third straight section both sides of bar I；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 °, forms X-axis in the same direction and bears
The double-Y shaped template of direction opening.Stainless steel II, stainless steel III, stainless steel IV and the radius of stainless steel V are
1.15mm, is inserted directly on stainless steel I fixation in corresponding hole.With silicon mud seal stainless steel pass through aluminium foil when on aluminium foil
The gap for leaving.
By dimethyl silicone polymer and polymethyl methacrylate in mass ratio 10:1 is well mixed, and forms performed polymer molten
Liquid, is evacuated to bubble-free, pours into mould performed polymer container, and bubble-free is evacuated to again, is integrally placed on vacuum drying chamber
In, solidify 2h at 70 DEG C, the basic channel die of micro-fluidic chip is made, the passage that stainless steel I is formed is passage I 1, stainless
The passage that steel pole II is formed is passage II 2, and the passage that stainless steel III is formed is passage III 3, the passage that stainless steel IV is formed
It is passage IV 4, the passage that stainless steel V is formed is passage V 5；By the ultrasonically treated 30min of mould, the aluminium of die surface is removed
Paper tinsel and the sheet glass of lower section, the stainless steel of mould inside are rotated and are extracted, and obtain micro-fluidic chip blank；Cut micro-fluidic core
Piece blank shape, obtains the basic passage of double-Y shaped micro-fluidic chip, sees Fig. 1.
External diameter 1.28mm, the syringe needle of internal diameter 0.9mm are chosen, the needle tubing of length 2.5cm is cut into, and section is repaiied
It is whole smooth, obtain tubular fitting I 6；The polytetrafluoroethylene (PTFE) conical pipe of hollow circle is chosen, is pruned, obtaining portlet internal diameter is
1.5mm, external diameter is 2.3mm, and large port external diameter is the nozzle of 5mm, forms tubular fitting II 7；Tubular fitting I 6 is inserted into passage I
In 1, one end of tubular fitting I 6 is fixed on the porch of passage I 1, and the other end extends along the horizontal direction of passage I 1；By tubulose
Passage I 1 is inserted at the big end of the conical pipe of accessory II 7 at the 5th grade straight section of passage I 1, along the reach of X-axis negative direction until big end
It is stuck on third straight section, obtains focusing on and coflow combined type channel design, sees Fig. 2.
With volume ratio 100：34 pure water（H2O）With heavy water（D2O）Mixed solution be fluid I；By divinylbenzene
（DVB）Monomer and solvent dibutyl phthalate（DBP）By volume 1：5 ratio is well mixed, with mass fraction 0.8%
Sorbitan oleate（SPAN80）For the phenyl of emulsifying agent and mass fraction 3% is double (2,4,6- trimethylbenzoyls)
Phosphine oxide（BAPO）It is initiator, stirring is well mixed for 10 minutes under conditions of leading to argon gas protection, and gained mixed solution is fluid
Ⅱ；With the polyvinyl alcohol of mass fraction 5%（PVA, Mw= 88000 g/mol）The aqueous solution is fluid III；Will with micro-injection pump
Fluid I is passed through tubular fitting I（6）, fluid II is passed through passage II and passage III simultaneously, and fluid III is passed through passage VI and passage simultaneously
Ⅴ；Adjustment fluid I, fluid II and the volume flow rate of fluid III are respectively 4.17 L/s, 1.36 L/s and 45.01 L/s, continuous steady
It is fixed to prepare dual drop in batches（W1/O/W2）, milk particle is collected at the 5th grade straight section in measuring cup, milk particle will be collected
Measuring cup is placed in test size under light microscope, and external diameter is 5.457mm, and wall thickness is 465 m, and size standard deviation is less than 1 ‰,
See Fig. 3.
Above-mentioned milk particle is transported in the cylindrical bottle of the rate level rotation of 5rpm through glass pipe, choosing wavelength is
365nm, intensity of illumination is 3.7 W/cm3Uviol lamp drop is irradiated, keep cylindrical bottle continue keep 5rpm speed
Horizontally rotated；Multiple drop is changed into 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 enters line replacement 3-5 days, an ethanol solution is changed daily；Gel ball after displacement is put into CO2It is super to face
Boundary's drying equipment is dried, that is, obtain complete polydivinylbenezene（PDVB）Hollow ball, external diameter 5.411mm, wall thickness
461 m, 2 ‰ are less than with batch product ball size standard deviation.
Embodiment 2
Embodiment 2 is using of the invention double-Y shaped micro- using convert that microfluidic channel prepares that the method for millimeter grade particles is made
Fluidic chip forward direction double focusing passage and its double emulsion and hollow ball application and preparation example.
Embodiment 2 is essentially identical with the implementation method of embodiment 1, differs primarily in that, embodiment 1 obtain it is 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, prunes, and obtains portlet internal diameter for 2.5mm, and external diameter is 3.3mm, and large port external diameter is the nozzle of 6mm, forms tubular fitting
Ⅲ8；Passage I 1 is inserted at the big end of the conical pipe of tubular fitting III 8 at the 5th grade straight section of passage I 1, before X-axis negative direction
Move and be stuck on fourth class straight section until holding greatly, obtain positive double focusing channel design, see Fig. 4.
Using the method in similar embodiment 1, above-mentioned gained forward direction double focusing passage is used for continuous-stable batch and is prepared
Millimeter grade particles of the particle diameter less than gained milk particle and microballoon in embodiment 1.Adjustment fluid I, fluid II and the volume flow rate of fluid III
Respectively 4.17 L/s, 1.36 L/s and 25.11 L/s, continuous-stable batch prepare dual drop（W1/O/W2）,
Milk particle is collected at five grade straight sections in measuring cup, the measuring cup for collecting milk particle is placed in test size, external diameter under light microscope
It is 3.255mm, wall thickness is 185 m, and size standard deviation is less than 1.5 ‰, sees Fig. 5.After cured, displacement and drying, gathered
Divinylbenzene（PDVB）Hollow ball, external diameter 3.223mm, the m of wall thickness 184 are less than with batch product ball size standard deviation
2.5‰。
Embodiment 3
Embodiment 3 is using of the invention double-Y shaped micro- using convert that microfluidic channel prepares that the method for millimeter grade particles is made
The reverse double focusing passage of fluidic chip and its double emulsion and hollow ball application and preparation example.
Embodiment 3 is essentially identical with the implementation method of embodiment 1, differs primarily in that, by the syringe needle in embodiment 1
Head changes external diameter 0.7mm, internal diameter 0.5mm into, obtains similar to the double-Y shaped micro-fluidic chip combined type passage obtained in embodiment 1
Structure, and on this basis, increase tubular fitting IV 9.Refer specifically to choose the polytetrafluoroethylene (PTFE) conical pipe of hollow circle, prune, obtain
It is 1mm to portlet internal diameter, large port external diameter is the nozzle of 7mm, forms tubular fitting IV 9；By the conical pipe of tubular fitting IV 9
Small end passage I 1 is inserted at the 5th grade straight section of passage I 1, along the reach of X-axis negative direction until big end is stuck in the 5th grade straight section
On, reverse double focusing channel design is obtained, see Fig. 6.
Using the method in similar embodiment 1, the reverse double focusing passage of above-mentioned gained is used for continuous-stable batch and is prepared
Submillimeter/millimeter grade particles of the particle diameter much smaller than gained milk particle and microballoon in embodiment 1.Adjustment fluid I, fluid II and fluid III
Volume flow rate is respectively 4.17 L/s, 1.36 L/s and 8.3 L/s, and continuous-stable batch prepares dual drop（W1/O/
W2）, milk particle is collected at the 5th grade straight section in measuring cup, the measuring cup for collecting milk particle is placed under light microscope and tests chi
Very little, external diameter is 0.812mm, and wall thickness is 86 m, and size standard deviation is less than 4 ‰, sees Fig. 7.After cured, displacement and drying, obtain
To polydivinylbenezene（PDVB）Hollow ball, external diameter 0.806mm, the m of wall thickness 84 are small with batch product ball size standard deviation
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 are accordingly increased or reduced, and using the gained basic passage of micro-fluidic chip in embodiment 1, simple operations are complete
Into channel design conversion, hundred microns of particle/drops to several millimeters level size are advantageously used in the preparation of.In above-described embodiment not
Rust steel pole I and stainless steel II, III, IV and V can use stainless steel tube, stainless steel sleeve pipe, glass rod, glass tube, polytetrafluoroethyl-ne
Alkene bar or polyfluortetraethylene pipe are replaced.
The present invention is not limited to above-mentioned specific embodiment, person of ordinary skill in the field from above-mentioned design,
Without performing creative labour, done a variety of conversion are within the scope of the present invention.
Claims (10)
1. a kind of utilization converts the method that microfluidic channel prepares millimeter grade particles, it is characterised in that the method includes following step
Suddenly：
A. the basic passage of micro-fluidic chip is prepared；
B. the tubular fitting of the basic passage of micro-fluidic chip is prepared；
C. tubular fitting is assembled in the basic passage of micro-fluidic chip；
D. particle is prepared.
2. according to claim 1 utilization converts the method that microfluidic channel prepares millimeter grade particles, it is characterised in that institute
The step of stating a is comprised the following steps：
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 a hollow cuboid for upper opening, obtains mould pre-polymerization by aluminium foil
Body container, defines length, height, the respectively X, Y, Z axis wide of hollow cuboid；
A2. by surface it is smooth, along the stepped increase of X-direction radius, with the level of the stainless steel of straight section I such as N sections
Through mould performed polymer container, the horizontal symmetrical center of the horizontal symmetrical center line less than mould performed polymer container of stainless steel I
Line；In the horizontal symmetrical plane of stainless steel I, the He of stainless steel II is symmetrically fixed in the second grade straight section both sides of stainless steel I
Stainless steel IV and stainless steel V, stainless steel I are symmetrically fixed in stainless steel III, the third straight section both sides of stainless steel I
The straight section both sides such as N symmetrically fix stainless steel M-1 and stainless steel M, by fixed stainless steel, obtain required miniflow
The control basic passage 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 the angle between stainless steel M-1 and stainless steel M is 120 °；N >=5, M >=5；
A3. polymer is uniformly mixed with curing agent, forms prepolymer solution, prepolymer solution is evacuated to without gas
Bubble, pours into the mould performed polymer container that step a1 is made, and again vacuumizes the prepolymer solution in mould performed polymer container
To bubble-free, mould performed polymer container is placed in vacuum drying chamber, 2 ~ 3h is solidified at 70 DEG C, be made micro-fluidic chip basic
Channel die；
A4. by the micro-fluidic chip ultrasonically treated 30min of basic channel die, the aluminium foil of die surface and the glass of lower section are removed
Piece, the stainless steel of mould inside is rotated and is extracted, and obtains micro-fluidic chip blank, cuts micro-fluidic chip blank shape, is obtained
To the basic passage of micro-fluidic chip, the passage that stainless steel I is formed is passage I（1）, the passage that stainless steel II is formed is passage
Ⅱ（2）, the passage that stainless steel III is formed is passage III（3）, the passage that stainless steel IV is formed is passage IV（4）, stainless steel
The passage that bar V is formed is passage V（5）, until the passage that stainless steel M is formed is passage M.
3. according to claim 1 utilization converts the method that microfluidic channel prepares millimeter grade particles, it is characterised in that institute
The step of stating b is comprised the following steps：
B1. tubular fitting I is prepared（6）, tubular fitting I is hollow circular tube, and the external diameter of hollow circular tube is less than passage I（1）Entrance
Internal diameter；
B2. tubular fitting II is prepared（7）, 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 the ladder of bar I the 3rd；
B3. tubular fitting III is prepared（8）, 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 the fourth order ladder of bar I；
B4. tubular fitting IV is prepared（9）, 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 ladder of bar I the 5th；
B5. continue to prepare tubular fitting, until the outside diameter of the conical pipe of tubular fitting is straight N ladders of stainless steel I etc.
The internal diameter of section.
4. according to claim 1 utilization converts the method that microfluidic channel prepares millimeter grade particles, it is characterised in that institute
The step of stating c is comprised the following steps：
C1. by tubular fitting I（6）Insertion passage I（1）In, tubular fitting I（6）One end be fixed on passage I（1）Entrance
Place, the other end is along passage I（1）X-axis positive direction it is horizontal-extending；
C2. by tubular fitting II（7）Conical pipe big end in passage I（1）The straight section such as N at insert passage I（1）, tubulose
Accessory II（7）Conical pipe small end towards X-axis positive direction, tubular fitting II（7）Along the reach of X-axis negative direction until tubular fitting
Ⅱ（7）Big end be stuck on third straight section, obtain focus on and coflow combined type passage；
C3. by tubular fitting III（8）Conical pipe big end in passage I（1）The straight section such as N at insert passage I（1）, tubulose
Accessory III（8）Conical pipe small end towards X-axis positive direction, tubular fitting III（8）Along the reach of X-axis negative direction until big end is stuck in
On fourth class straight section, positive double focusing passage is obtained；
Or by tubular fitting VI（9）Conical pipe small end in passage I（1）The straight section such as N at insert passage I（1）, tubulose
Accessory VI（9）Conical pipe big end towards X-axis positive direction, tubular fitting VI（9）Along the reach of X-axis negative direction until big end is stuck in
On 5th grade straight section, reverse double focusing passage is obtained；
C4. continue that tubular fitting is installed, until obtaining required passage.
5. according to claim 1 utilization converts the method that microfluidic channel prepares millimeter grade particles, it is characterised in that institute
The step of stating d is comprised the following steps：
D1. tubular fitting I（6）In be passed through fluid I；
D2. fluid II is passed through simultaneously in passage II and passage III, described fluid II is immiscible with fluid I；
D3. fluid III is passed through simultaneously in passage VI and passage V, described fluid III is immiscible with fluid II；
D4. collected at the straight sections such as N and obtain milk particle；
D5. milk particle is solidified, is obtained particle.
6. according to claim 2 utilization converts the method that microfluidic channel prepares millimeter grade particles, it is characterised in that institute
The straight section external diameter that waits of the stainless steel I stated is millimeter magnitude.
7. according to claim 2 utilization converts the method that microfluidic channel prepares millimeter grade particles, it is characterised in that institute
The polymer stated is dimethyl silicone polymer, and curing agent is polymethyl methacrylate, in described prepolymer solution poly- two
Methylsiloxane is 10 with the mass ratio of polymethyl methacrylate:1.
8. according to claim 2 utilization converts the method that microfluidic channel prepares millimeter grade particles, it is characterised 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.
9. according to claim 2 utilization converts the method that microfluidic channel prepares millimeter grade particles, it is characterised in that institute
The stainless steel stated passes through the gap left on aluminium foil during aluminium foil to be sealed with silicon mud；
Described stainless steel I punches in advance, by stainless steel II, stainless steel III, stainless steel IV, stainless steel V until
Stainless steel M is fixed in being inserted directly into corresponding hole.
10. according to claim 3 utilization converts the method that microfluidic channel prepares millimeter grade particles, it is characterised in that
The material of described tubular fitting is the one kind in polyfluortetraethylene pipe, glass tube or stainless steel tube.
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| CN111569798A (en) * | 2020-05-27 | 2020-08-25 | 中山大学 | Degradable core-shell calcium alginate oxide gel microspheres and preparation method and application thereof |
| CN112569878A (en) * | 2020-01-21 | 2021-03-30 | 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 |
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