CN107159072B - A kind of regulatable drop drives the preparation method of microreactor certainly - Google Patents
A kind of regulatable drop drives the preparation method of microreactor certainly Download PDFInfo
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- CN107159072B CN107159072B CN201710325224.3A CN201710325224A CN107159072B CN 107159072 B CN107159072 B CN 107159072B CN 201710325224 A CN201710325224 A CN 201710325224A CN 107159072 B CN107159072 B CN 107159072B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
Abstract
The invention discloses the preparation methods that a kind of regulatable drop drives microreactor certainly, comprising the following steps: (1) prepares coating liquid；(2) mask plate is prepared；(3) preparation has multistage gradient body structure surface flexible；(4) shutter is prepared；(5) surface that preparation chemical gradient is combined with flexible multilevel gradient-structure；(6) surface for combining at least 3 chemical gradients as made from step (1) to (5) with flexible multilevel gradient-structure, according to surface pillar by dredging close sequence, the surface of at least 3 above structures is arranged in " Y " font from top to bottom, is assembled into a microreactor；At least two reacting fluids can first come together in intersection reaction, flow to vertical runner again later.For the present invention on the basis of flexible multilevel gradient-structure surface, the chemical property for combining material surface changes the chemical gradient to be formed, and enhances the ability of material surface driving drop orientation transport.
Description
Technical field
The invention belongs to macromolecule material preparation areas more particularly to a kind of regulatable drop to drive microreactor certainly
Preparation method.
Background technique
Microreactor is the micromation chemical reaction system that a kind of unit process interface width is micron dimension, is the nineties
The micro- Chemical Engineering Technology risen.It refers to react as the main purpose, based on one or more microreactors, while being also possible to wrap
Microring array, micro- heat exchange, differential are included from one of the key components such as auxiliary devices and microsensors and microactuators such as, micro-extraction
Micro- reaction system.Specifically, what microreactor generally referred to manufacture by micro-processing technology and precision processing technology has micro-
The consersion unit of structure, fluid channel or dispersion scale in microreactor are in micron dimension, and the treating capacity of microreactor
Then the difference according to the purpose of its application reaches from several microlitres of scales annual to tens of thousands of cubic meters per minute.In recent years, it is based on
Requirement of certain specific reactions to runner surface wettability, surface wettability are initially introduced into microreactor, utilize profit
It is moist effectively to regulate and control movement of the fluid in runner.
Traditional micro- reaction system mainly passes through the method for photoetching, etching and machining in silicon wafer, glass, poly dimethyl
It is made on the materials such as siloxanes and polymethyl methacrylate, but these preparation methods were prepared there is Preparation equipment valuableness
The disadvantages of journey is complicated, and runner precision is inaccurate, and it is most of need external aids to provide power, greatly limit micro- anti-
Answer the process of industrialization of device.Wetability is combined in microreactor, makes the microreactor runner with wetting gradient, Ke Yishi
Existing drop drives certainly, to reduce the demand for needing external auxiliary.There are making apparatus valuableness, systems for current micro- reaction system
Standby process is complicated, runner precision inaccuracy, the problems such as can not regulating and controlling, need external auxiliary, and in the market will wetting gradient with it is micro-
The research that reactor combines is fewer and fewer, for the drop that can regulate and control from the research of driving microreactor almost without.
Summary of the invention
To solve the above-mentioned problems, the present invention provides a kind of preparation method of oneself driving microreactor of regulatable drop,
In view of the deficiencies of the prior art, the driving certainly and its regulation for realizing microfluid, greatly reduce fluid driving regulation and control cost, tool
There is the features such as portable, economic, quick, efficient, realizes and be widely applied.
Adopt the following technical scheme that thus: a kind of regulatable drop drives the preparation method of microreactor certainly, special
Sign be the following steps are included:
Step (1) prepares coating liquid: the ratio by the prepolymer of dimethyl silicone polymer and crosslinking agent with quality for 10:1
It is mixed evenly, places extract 20min with vacuum pump in a vacuum drying oven later, remove the bubble in solution, be made poly-
The coating liquid of dimethyl siloxane；
Step (2) prepares mask plate: taking the silicon template of a length of a film 50mm, width 25mm, thickness 1mm, utilizes three-dimensional drawing software
Gradient-structure layout viewing is drawn out, it is 10 μm that the gradient-structure layout viewing, which is with diameter, deep 40 μm of cell orifice is in template
Distribution gradient, the gradient distribution mode is subject to along template long side, with unit pitch of holes in the distance of first 1mm for 10
μm, unit pitch of holes increases to 20 μm and so in the distance of second 1mm；Then with the gradient-structure layout viewing of drafting
For reference, engraving processing is carried out to silicon template；The substrate of selection is substrate of glass, and carries out prerinse to it, i.e., by glass base
Successively 10~20min of ultrasound in acetone, absolute alcohol, deionized water, supersonic frequency are 50~100Hz at bottom, are washed with water later
Only it and is dried；Then the silicon template handled well is fitted tightly on the glass basic surface after prerinse；It will step
Suddenly for uniform fold in silicon template surface, the spin coating number of specific spin coating mode is 1 to the coating liquid of (1) preparation by way of spin coating
It is secondary, first with 1500 turns per minute of rate spin coating 5s, then with 8000 turns per minute of rate spin coating 20s, finally with per minute
Spin coating is had the silicon template of coating liquid with temperature for 75 DEG C of dry 20min, thus in silicon mould by 1500 turns of rate spin coating 5s later
The film of coating liquid is formed in plate surface；
Step (3) preparation has multistage gradient body structure surface flexible: preparing with a thickness of 1mm, the VHB glue that width is 25mm
Band, first by VHB Tape Pull, and maintain 50% dependent variable, then have coating liquid thin mask plate spin coating made from step (2)
The one side of film is fitted closely with the VHB adhesive tape after stretching, and 2 hours are handled in the baking oven that temperature is 80 DEG C；Later by glass
Substrate is taken off with silicon template, and the coating liquid film for replicating silicon template gradient-structure is just fitted closely with VHB adhesive tape；Finally discharge
To the pulling force of VHB adhesive tape, be tightly attached to polydimethylsiloxanefilm film on VHB tape surface just due to convergent force on the surface thereof
Generate the multilevel structure that buckling is combined with gradient；
Step (4) prepares shutter: going out an antiparallelogram using three-dimensional drawing Software on Drawing, trapezoidal upper short side is long
25mm, lower long side length 82.8mm, two waists and upper following angle are respectively 120 ° and 60 °, take a thickness 0.3mm, size with it is above-mentioned
Copper sheet is allowed to angle in 90 ° along trapezoidal high fold, that is, is converted into the shutter of a wedge shape by the identical copper sheet of antiparallelogram；
The surface that step (5) preparation chemical gradient is combined with flexible multilevel gradient-structure: it will be blocked made from step (4)
The triangle long edge position of plate be covered on step (3) preparation have multistage gradient body structure surface flexible on, the wedge shape of shutter
Opening direction is the direction that pillar is more dense on VHB adhesive tape；It places it in Surface Treatment with Plasma machine after handling 60min and takes
Out, the surface that chemical gradient is combined with flexible multilevel gradient-structure is obtained after shutter being removed；
Step (6) mutually ties at least 3 chemical gradients as made from step (1) to (5) with flexible multilevel gradient-structure
The surface of at least 3 above structures is arranged in one according to surface pillar by dredging close sequence by the surface of conjunction from top to bottom
" Y " font is assembled into a microreactor；At least two reacting fluids can first come together in intersection reaction, flow to again later perpendicular
Straight runner.
A kind of regulatable drop of preparation method preparation according to the present invention drives microreactor certainly, more in flexibility
On the basis of grade gradient-structure surface, the chemical property for combining material surface changes the chemical gradient to be formed, and further enhances
The ability of material surface driving drop orientation transport.The physical structure and chemical structure of material are changed simultaneously: in buckling
From left to right its change of gradient is close by dredging to column structure, to cause the hydrophobicity of material from left to right by dying down by force；Through
Material after crossing plasma treatment is due to the effect of shutter, and from left to right its change of gradient is by small to the extent of reaction being subject to
To big, material sheet can become hydrophily as hydrophobicity after treatment, to cause the hydrophobicity of material from left to right by strong
It dies down.The combination of the two greatly improves material for the directed driven ability of drop, and after lining up " Y " font, two kinds are reacted
Fluid can first come together in intersection reaction, flow to vertical runner again later.And due to being using VHB adhesive tape flexible as substrate
The multilevel structure of preparation, can also be by the variation stretched to realize multilevel structure arranging density to substrate, thus realization pair
The control of drop directed driven speed, thus to regulate and control the rate that reaction carries out.
The beneficial effects of the present invention are:
1) combine the physics gradient of material with chemical gradient, the energy of the material directed driven drop further increased
Power.
2) to change the hydrophobic of material surface by the arrangement density for changing gradient-structure to the stretching of flexible substrates
Property degree, it is easy to operate so as to regulate and control to reacting fluid flow rate, be not necessarily to external accessory.
3) drop can be made to be sufficiently mixed and fast transportation by design, to improve microreactor efficiency.
4) preparation method economy, it is convenient to operate.
Detailed description of the invention
Fig. 1 is to prepare schematic diagram, figure label with multistage gradient body structure surface flexible are as follows: 1 is VHB adhesive tape, and 2 are
Coating liquid film, 3 be silicon template, and 4 be substrate of glass, 5 multilevel structures combined for buckling with gradient.
Fig. 2 is multilevel structure surface plasma processing schematic, wherein 6 be shutter.
Specific embodiment
The present invention is further illustrated with reference to the accompanying drawing.
Referring to attached drawing.1 the present embodiment of embodiment the following steps are included:
Step (1) prepares coating liquid: the prepolymer and 0.5g crosslinking agent of 5g dimethyl silicone polymer (PDMS) coating liquid are mixed
Conjunction stirs evenly, and places extract 20min with vacuum pump in a vacuum drying oven later, removes the bubble in solution, is made poly- two
The coating liquid of methylsiloxane；
Step (2) prepares mask plate: taking the silicon template 3 of a length of a film 50mm, wide 25mm, thickness 1mm, utilizes three-dimensional drawing software
Gradient-structure layout viewing is drawn out, it is 10 μm that the gradient-structure layout viewing, which is with diameter, deep 40 μm of cell orifice is in template
Distribution gradient, the gradient distribution mode is subject to along template long side, with unit pitch of holes in the distance of first 1mm for 10
μm, unit pitch of holes increases to 20 μm and so in the distance of second 1mm；Then with the gradient-structure layout viewing of drafting
For reference, engraving processing is carried out to silicon template；The substrate of selection is substrate of glass, and carries out prerinse to it, i.e., by glass base
Successively 10~20min of ultrasound in acetone, absolute alcohol, deionized water, supersonic frequency are 50~100Hz at bottom, are washed with water later
Only it and is dried；Then the silicon template handled well is fitted tightly on the glass basic surface after prerinse；It will step
Suddenly for uniform fold in silicon template surface, the spin coating number of specific spin coating mode is 1 to the coating liquid of (1) preparation by way of spin coating
It is secondary, first with 1500 turns per minute of rate spin coating 5s, then with 8000 turns per minute of rate spin coating 20s, finally with per minute
Spin coating is had the silicon template of coating liquid with temperature for 75 DEG C of dry 20min, thus in silicon mould by 1500 turns of rate spin coating 5s later
Coating liquid film 2 is formed on 3 surface of plate；
Step (3) preparation has multistage gradient body structure surface flexible: preparing with a thickness of 1mm, the VHB adhesive tape that width is 25mm
1, first by VHB Tape Pull, and maintain 50% dependent variable, then have coating liquid thin mask plate spin coating made from step (2)
The one side of film 2 is fitted closely with the VHB adhesive tape after stretching, and 2 hours are handled in the baking oven that temperature is 80 DEG C；Later by glass
Substrate is taken off with silicon template, and the coating liquid film for replicating silicon template gradient-structure is just fitted closely with VHB adhesive tape；Finally discharge
To the pulling force of VHB adhesive tape, be tightly attached to polydimethylsiloxanefilm film on VHB tape surface just due to convergent force on the surface thereof
Generate the multilevel structure 5 that buckling is combined with gradient；
Step (4) prepares shutter 6: going out an antiparallelogram using three-dimensional drawing Software on Drawing, trapezoidal upper short side is long
25mm, lower long side length 82.8mm, two waists and upper following angle are respectively 120 ° and 60 °, take a thickness 0.3mm, size with it is above-mentioned
Copper sheet is allowed to angle in 90 ° along trapezoidal high fold, that is, is converted into the shutter of a wedge shape by the identical copper sheet of antiparallelogram；
The surface that step (5) preparation chemical gradient is combined with flexible multilevel gradient-structure: it will be blocked made from step (4)
The triangle long edge position of plate be covered on step (3) preparation have multistage gradient body structure surface flexible on, the wedge shape of shutter
Opening direction is the direction that pillar is more dense on VHB adhesive tape；It places it in Surface Treatment with Plasma machine after handling 60min and takes
Out, the surface that chemical gradient is combined with flexible multilevel gradient-structure is obtained after shutter being removed.
Step (6) combines 3 chemical gradients as made from step (1) to (5) with flexible multilevel gradient-structure
The surface of 3 above structures is arranged in " Y " font according to surface pillar by dredging close sequence by surface from top to bottom,
It is assembled into a microreactor；" Y " the font arrangement, is the microreactor of two kinds of liquid reactant mixtures, can be optionally
It is further added by required runner.Reaction liquid flows first to " Y " font middle and collects mixing, then flows to the end of " Y " font again
End.
2 the present embodiment of embodiment difference from example 1 is that: suitably substrate is stretched, material can be made
Material surface pillar arrangement becomes more sparse, to slightly change the hydrophobicity of material surface, and then to the flowing of fluid speed
Degree has an impact.
A kind of regulatable drop of this method preparation has buckling structure on material surface from microreactor is driven,
On buckling structure also with distribution gradient column structure, and material surface have chemical gradient, wetability by hydrophobicity by
Fade to hydrophily.Contact angle is different on different length direction on the surface of the material for liquid, to be dropped in the anti-of " Y " font upper end
Displacement occurs for the driving for answering fluid to will receive surface tension, the reaction of " Y " font intersection is come together in, finally in vertical runner
Upper outflow.
Claims (1)
1. the preparation method that a kind of regulatable drop drives microreactor certainly, it is characterised in that the following steps are included:
Step (1) prepares coating liquid: the prepolymer of dimethyl silicone polymer and crosslinking agent are mixed with quality for the ratio of 10:1
It stirs evenly, places extract 20min with vacuum pump in a vacuum drying oven later, remove the bubble in solution, poly- diformazan is made
The coating liquid of radical siloxane；
Step (2) prepares mask plate: taking the silicon template of a length of a film 50mm, width 25mm, thickness 1mm, utilizes three-dimensional drawing Software on Drawing
Gradient-structure layout viewing out, the gradient-structure layout viewing are that the cell orifice for being 10 μm, deeply 40 μm with diameter is in ladder in template
Degree distribution, the gradient distribution mode is subject to along template long side, with unit pitch of holes in the distance of first 1mm for 10 μm,
Unit pitch of holes increases to 20 μm and so in the distance of second 1mm；Then it is with the gradient-structure layout viewing of drafting
Reference carries out engraving processing to silicon template；The substrate of selection is substrate of glass, and carries out prerinse to it, i.e., by substrate of glass
Successively 10~20min of ultrasound in acetone, absolute alcohol, deionized water, supersonic frequency are 50~100Hz, are eluted with water later
And it is dried；Then the silicon template handled well is fitted tightly on the glass basic surface after prerinse；By step
(1) for uniform fold in silicon template surface, the spin coating number of specific spin coating mode is 1 to the coating liquid prepared by way of spin coating
It is secondary, first with 1500 turns per minute of rate spin coating 5s, then with 8000 turns per minute of rate spin coating 20s, finally with per minute
Spin coating is had the silicon template of coating liquid with temperature for 75 DEG C of dry 20min, thus in silicon mould by 1500 turns of rate spin coating 5s later
The film of coating liquid is formed in plate surface；
Step (3) preparation has multistage gradient body structure surface flexible: preparing with a thickness of 1mm, the VHB adhesive tape that width is 25mm, first
By VHB Tape Pull, and maintain 50% dependent variable, mask plate spin coating made from step (2) is then had into coating liquid film
It is fitted closely on one side with the VHB adhesive tape after stretching, 2 hours is handled in the baking oven that temperature is 80 DEG C；Later by substrate of glass
It is taken off with silicon template, the coating liquid film for replicating silicon template gradient-structure is just fitted closely with VHB adhesive tape；Finally release pair
The pulling force of VHB adhesive tape, the polydimethylsiloxanefilm film being tightly attached on VHB tape surface is just since convergent force produces on the surface thereof
The multilevel structure that raw buckling is combined with gradient；
Step (4) prepares shutter: go out an antiparallelogram using three-dimensional drawing Software on Drawing, the trapezoidal upper long 25mm of short side, under
Long side length 82.8mm, two waists and upper following angle are respectively 120 ° and 60 °, take a thickness 0.3mm, size and above-mentioned antiparallelogram
Copper sheet is allowed to angle in 90 ° along trapezoidal high fold, that is, is converted into the shutter of a wedge shape by identical copper sheet；
The surface that step (5) preparation chemical gradient is combined with flexible multilevel gradient-structure: by shutter made from step (4)
Triangle long edge position be covered on step (3) preparation have multistage gradient body structure surface flexible on, the wedge-like opening of shutter
Direction is the direction that pillar is more dense on VHB adhesive tape；It places it in Surface Treatment with Plasma machine after handling 60min and takes out,
The surface that chemical gradient is combined with flexible multilevel gradient-structure is obtained after shutter is removed；
Step (6) combines at least 3 chemical gradients as made from step (1) to (5) with flexible multilevel gradient-structure
The surface of at least 3 above structures is arranged in one " Y " according to surface pillar by dredging close sequence by surface from top to bottom
Font is assembled into a microreactor；At least two reacting fluids can first come together in intersection reaction, and it is vertical to flow to again later
Runner.
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| CN105833814A (en) * | 2016-04-27 | 2016-08-10 | 浙江工业大学 | Method for manufacturing liquid drop self-driven microreactor and microreactor manufactured through method |
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| CN1654311A (en) * | 2005-03-09 | 2005-08-17 | 吉林大学 | Method for constructing non-close packing colloid balls ordered arrangement using soft-graving technology |
| CN102515091A (en) * | 2011-12-22 | 2012-06-27 | 哈尔滨工业大学 | Plastic functional micro-structured surface soft-lithography duplicating method used in plastic functional micro-structured surface batch production |
| WO2015038767A1 (en) * | 2013-09-12 | 2015-03-19 | Western Michigan University Research Foundation | Microfluidic systems with microchannels and a method of making the same |
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