CN103908935B - A kind of capillary glass tube microfluidic devices and use this device to prepare there is the method for the polymer microballoon of multi-stage artery structure - Google Patents
A kind of capillary glass tube microfluidic devices and use this device to prepare there is the method for the polymer microballoon of multi-stage artery structure Download PDFInfo
- Publication number
- CN103908935B CN103908935B CN201410109418.6A CN201410109418A CN103908935B CN 103908935 B CN103908935 B CN 103908935B CN 201410109418 A CN201410109418 A CN 201410109418A CN 103908935 B CN103908935 B CN 103908935B
- Authority
- CN
- China
- Prior art keywords
- tube
- injection
- polymer microballoon
- stage artery
- microfluidic devices
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The present invention relates to a kind of capillary glass tube microfluidic devices and use this device to prepare the method with the polymer microballoon of multi-stage artery structure, solve the technical problem of the non-constant width of Size Distribution of porous microsphere polymeric material prepared by existing method.This preparation method adopts pore-foaming agent method and emulsion template method to combine, and in the capillary glass tube microfluidic devices of self assembly, preparation has the polymer microballoon of multi-stage artery structure.The scantling that the inventive method prepares is evenly distributed, have the polymer microballoon of the multi-stage artery structure that nanoscale duct and micron order duct are interconnected.This preparation method obtains the pore structure of nano-scale by adding pore-foaming agent, obtain micron-scale pore structure by emulsion template, the duct that the material finally obtained has larger specific area, is interconnected.
Description
Technical field
The present invention relates to a kind of capillary glass tube microfluidic devices and use this device to prepare and there is the method for the polymer microballoon of multi-stage artery structure, be specifically related to a kind of method of polymer microballoon of the multi-stage artery structure using capillary glass tube microfluidic devices to prepare to have nanoscale duct and micron order duct to be interconnected.
Background technology
Porous polymer refers to that inside includes the macromolecular material of a large amount of tortuous pore structure be interconnected.This material is prepared at present mainly through pore-foaming agent method and emulsion template method.The standby material of pore-foaming agent legal system has nano level hole dimension usually, and material prepared by emulsion template method normally has the overall bulk material of micrometer grade hole size.But poromeric pore structure prepared by above-mentioned two kinds of preparation methods is all more single.
At present, the preparation of hierarchical porous structure material focuses mostly in inorganic material, the rarely seen report of the preparation about the macromolecular material of hierarchical porous structure.2013, the people such as Sai to prepare the macromolecule block materials of hierarchical porous structure by Self-Assembling of Block Copolymer at Science magazine ran.The people such as Schofield have prepared the multilevel hierarchy polymeric membrane of the nano-pore with cyclodextrin, emulsion template micron openings and non-woven fabrics super big hole.But traditional parting material normally exists with microspheres form, the people such as Ning is with Fe for this reason
3o
4nano particle is stabilizing agent, by adding pore-foaming agent in the oil phase in Pickering double emulsion, has prepared porous microsphere material, and wherein emulsion template forms macropore, and pore-foaming agent forms relatively little hole, and this material is successfully applied to dye separation.The non-constant width but the Microsphere Size regrettably prepared by this method distributes.
Summary of the invention
The present invention is the technical problem of the non-constant width of Size Distribution solving porous microsphere polymeric material prepared by existing method, provides a kind of capillary glass tube microfluidic devices and uses this device to prepare the method with the polymer microballoon of multi-stage artery structure.
In order to solve the problems of the technologies described above, technical scheme of the present invention is specific as follows:
A kind of capillary glass tube microfluidic devices, described microfluidic devices comprises injection-tube, outer tube, collecting pipe and receiving tube;
Described injection-tube is arranged on inside outer tube one end, described collecting pipe is arranged on inside the outer tube other end, the spacing of described collecting pipe and injection-tube conical head is 0.08mm-0.15mm, described injection-tube, outer tube and collecting pipe are coaxially placed and are fixed with epoxy glue, and the other end of described collecting pipe is inserted in described receiving tube;
The external diameter of described injection-tube is 0.76mm, internal diameter is 0.58mm, and injection-tube conical head internal diameter is 0.05mm-0.1mm;
The internal diameter of described outer tube is 1.0mm;
The external diameter of described collecting pipe is 0.76mm, internal diameter is 0.58mm.
Use the preparation of capillary glass tube microfluidic devices to have the method for the polymer microballoon of multi-stage artery structure, the method specifically comprises the following steps:
(1) water-in-oil emulsion preparation
Measure GMA, ethylene glycol dimethacrylate, pore-foaming agent, emulsifying agent and dimethoxybenzoin, obtain mixed solution, being joined by this mixed solution is equipped with in three mouthfuls of round-bottomed flasks of agitating device again, constant speed dropwise adds with mixed solution isopyknic calcium chloride water under stirring again, continue to stir 5-10 minute, obtain water-in-oil emulsion;
(2) there is the polymer microballoon preparation of multi-stage artery structure
The water-in-oil emulsion that step (1) obtains is poured in injector syringe, driven in the injection-tube of water-in-oil emulsion implantation glass capillary microfluidic devices by syringe pump, driven by syringe pump in gap polyvinyl alcohol water solution is injected between injection-tube and outer tube, W/O/W double emulsion droplet is formed at injection-tube tip, this droplet flows through collecting pipe end and forms solids through ultra violet lamp, obtains the polymer microballoon with multi-stage artery structure.
In technique scheme, described pore-foaming agent is dibutyl phthalate, diethyl phthalate or dioctyl phthalate.
In technique scheme, the addition of described pore-foaming agent is 0.3-0.7 milliliter.
In technique scheme, the injection speed of described polyvinyl alcohol water solution is 2-8 ml/hour.
In technique scheme, described emulsifying agent is class 80 of department.
A kind of capillary glass tube microfluidic devices provided by the invention and the advantage using the preparation of this device to have the method for the polymer microballoon of multi-stage artery structure are:
The present invention adopts pore-foaming agent method and emulsion template method to combine, and prepares even size distribution, has the micro polymer ball material of the multi-stage artery structure that nanoscale duct and micron order duct are interconnected in the capillary glass tube microfluidic devices of self assembly.This preparation method obtains the pore structure of nano-scale by adding pore-foaming agent, obtain micron-scale pore structure by emulsion template, the duct that the material finally obtained has larger specific area, is interconnected.
Preparation method provided by the invention, by the control of adjustment pore-foaming agent consumption realization to material hole structure, can also realize the control to Microsphere Size by the injection speed of adjustment polyvinyl alcohol water solution.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Fig. 1 is capillary glass tube microfluidic devices schematic diagram.
Fig. 2 is the scanning electron microscope diagram with the polymer microballoon of hierarchical porous structure prepared by embodiment 1.
Fig. 3 is the mercury injection method resolution chart with the polymer microballoon of hierarchical porous structure prepared by embodiment 1.
Detailed description of the invention
As shown in Figure 1: capillary glass tube microfluidic devices provided by the invention comprises injection-tube, outer tube, collecting pipe and receiving tube; Described injection-tube is arranged on inside outer tube one end, described collecting pipe is arranged on inside the outer tube other end, the spacing of described collecting pipe and injection-tube conical head is 0.08mm-0.15mm, described injection-tube, outer tube and collecting pipe are coaxially placed and are fixed with epoxy glue, and the other end of described collecting pipe is inserted in described receiving tube; The external diameter of described injection-tube is 0.76mm, internal diameter is 0.58mm, and injection-tube conical head internal diameter is 0.05mm-0.1mm; The internal diameter of described outer tube is 1.0mm; The external diameter of described collecting pipe is 0.76mm, internal diameter is 0.58mm.
Use the preparation of capillary glass tube microfluidic devices to have the method for the polymer microballoon of multi-stage artery structure, concrete steps are as follows:
(1) water-in-oil emulsion preparation
Measure GMA, ethylene glycol dimethacrylate, pore-foaming agent, class of department 80 and dimethoxybenzoin, obtain mixed solution, being joined by this mixed solution is equipped with in three mouthfuls of round-bottomed flasks of agitating device again, constant speed dropwise adds with mixed solution isopyknic calcium chloride water under stirring again, continue to stir 5-10 minute, obtain water-in-oil emulsion; Described pore-foaming agent is dibutyl phthalate, diethyl phthalate or dioctyl phthalate, and the addition of described pore-foaming agent is 0.3-0.7 milliliter;
(2) there is the polymer microballoon preparation of multi-stage artery structure
The water-in-oil emulsion that step (2) obtains is poured in injector syringe, driven in the injection-tube of water-in-oil emulsion implantation glass capillary microfluidic devices by syringe pump, driven by syringe pump in gap polyvinyl alcohol water solution is injected between injection-tube and outer tube, injection speed is 2-8 ml/hour, W/O/W double emulsion droplet is formed at injection-tube tip, this droplet flows through collecting pipe end and forms solids through ultra violet lamp, obtains the polymer microballoon with multi-stage artery structure.
Embodiment 1
Measure 1.02 milliliters of GMAs, 0.68 milliliter of ethylene glycol dimethacrylate, 0.3 milliliter of dibutyl phthalate, 0.3 milliliter of class 80 of department, dimethoxybenzoin 0.17 gram, joins and is equipped with in three mouthfuls of round-bottomed flasks of agitating device, dropwise adds containing 2w/v% calcium chloride water 2 milliliters under 400 revs/min of constant agitation speed, drip off rear continuation stirring 5 minutes, obtain homogeneous milky water-in-oil emulsion.Above-mentioned emulsion is poured in syringe, and by the injection-tube of syringe pump implantation glass capillary microfluidic devices, injection speed is 0.3 ml/hour.2w/v% polyvinyl alcohol water solution passes through in the gap between the injection-tube of syringe pump Driver injection capillary glass tube microfluidic devices and outer tube, injection speed is 2 mls/hour, W/O/W double emulsion droplet is formed at tip place, mean droplet size is 470 microns, drop formation frequency be 120 drops/minute, droplet, through ultraviolet light irradiation initiated polymerization, obtains the polymer microballoon with hierarchical porous structure.Accompanying drawing 2 is for having the scanning electron microscope diagram of the polymer microballoon of hierarchical porous structure, and this figure shows that inside particles comprises circular opening, is communicated with between hole by window, and macromolecular scaffold inside comprises nano pore.Accompanying drawing 3 is for having the mercury injection apparatus method resolution chart of the polymer microballoon of hierarchical porous structure, and this figure shows that window average-size is 1 micron, and duct average-size is 32 nanometers.The specific area of nitrogen adsorption methods test material is 32 meters squared per gram.
Embodiment 2
Measure 1.02 milliliters of GMAs, 0.68 milliliter of ethylene glycol dimethacrylate, 0.5 milliliter of diethyl phthalate, 0.3 milliliter of class 80 of department, dimethoxybenzoin 0.17 gram, joins and is equipped with in three mouthfuls of round-bottomed flasks of agitating device, dropwise adds containing 2w/v% calcium chloride water 2 milliliters under 400 revs/min of constant agitation speed, drip off rear continuation stirring 10 minutes, obtain homogeneous milky water-in-oil emulsion.Above-mentioned emulsion is poured in syringe, and by the injection-tube of syringe pump implantation glass capillary microfluidic devices, injection speed is 0.3 ml/hour.2w/v% polyvinyl alcohol water solution passes through in the gap between the injection-tube of syringe pump Driver injection capillary glass tube microfluidic devices and outer tube, injection speed is 4 mls/hour, W/O/W double emulsion droplet is formed at tip place, mean droplet size is 410 microns, drop formation frequency be 200 drops/minute, droplet, through ultraviolet light irradiation initiated polymerization, obtains the polymer microballoon with hierarchical porous structure.Scanning electron microscope diagram shows that inside particles comprises circular opening, is communicated with between hole by window, and macromolecular scaffold inside comprises nano pore.Mercury injection apparatus method test window average-size is 1 micron, and duct average-size is 66 nanometers, and the specific area of nitrogen adsorption methods test material is 40 meters squared per gram.
Embodiment 3
Measure 1.02 milliliters of GMAs, 0.68 milliliter of ethylene glycol dimethacrylate, 0.7 milliliter of dioctyl phthalate, 0.3 milliliter of class 80 of department, dimethoxybenzoin 0.17 gram, joins and is equipped with in three mouthfuls of round-bottomed flasks of agitating device, dropwise adds containing 2w/v% calcium chloride water 2 milliliters under 400 revs/min of constant agitation speed, drip off rear continuation stirring 5 minutes, obtain homogeneous milky water-in-oil emulsion.Above-mentioned emulsion is poured in syringe, and by the injection-tube of syringe pump implantation glass capillary microfluidic devices, injection speed is 0.3 ml/hour.2w/v% polyvinyl alcohol water solution passes through in the gap between the injection-tube of syringe pump Driver injection capillary glass tube microfluidic devices and outer tube, injection speed is 8 mls/hour, W/O/W double emulsion droplet is formed at tip place, mean droplet size is 320 microns, drop formation frequency be 450 drops/minute, droplet, through ultraviolet light irradiation initiated polymerization, obtains the polymer microballoon with hierarchical porous structure.Scanning electron microscope diagram shows that inside particles comprises circular opening, is communicated with between hole by window, and macromolecular scaffold inside comprises nano pore.Mercury injection apparatus method test window average-size is 0.8 micron, and duct average-size is 63 nanometers, and the specific area of nitrogen adsorption methods test material is 50 meters squared per gram.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of extending out or variation be still among the protection domain of the invention.
Claims (6)
1. a capillary glass tube microfluidic devices, is characterized in that, described microfluidic devices comprises injection-tube, outer tube, collecting pipe and receiving tube;
Described injection-tube is arranged on inside outer tube one end, described collecting pipe is arranged on inside the outer tube other end, the spacing of described collecting pipe and injection-tube conical head is 0.08mm-0.15mm, described injection-tube, outer tube and collecting pipe are coaxially placed and are fixed with epoxy glue, and the other end of described collecting pipe is inserted in described receiving tube;
The external diameter of described injection-tube is 0.76mm, internal diameter is 0.58mm, and injection-tube conical head internal diameter is 0.05mm-0.1mm;
The internal diameter of described outer tube is 1.0mm;
The external diameter of described collecting pipe is 0.76mm, internal diameter is 0.58mm.
2. use the preparation of the microfluidic devices described in claim 1 to have the method for the polymer microballoon of multi-stage artery structure, it is characterized in that, the method specifically comprises the following steps:
(1) water-in-oil emulsion preparation
Measure GMA, ethylene glycol dimethacrylate, pore-foaming agent, emulsifying agent and dimethoxybenzoin, obtain mixed solution, being joined by this mixed solution is equipped with in three mouthfuls of round-bottomed flasks of agitating device again, constant speed dropwise adds with mixed solution isopyknic calcium chloride water under stirring again, continue to stir 5-10 minute, obtain water-in-oil emulsion;
(2) there is the polymer microballoon preparation of multi-stage artery structure
The water-in-oil emulsion that step (1) obtains is poured in injector syringe, driven in the injection-tube of water-in-oil emulsion implantation glass capillary microfluidic devices by syringe pump, driven by syringe pump in gap polyvinyl alcohol water solution is injected between injection-tube and outer tube, W/O/W double emulsion droplet is formed at injection-tube tip, this droplet flows through collecting pipe end and forms solids through ultra violet lamp, obtains the polymer microballoon with multi-stage artery structure.
3. preparation according to claim 2 has the method for the polymer microballoon of multi-stage artery structure, it is characterized in that, described pore-foaming agent is dibutyl phthalate, diethyl phthalate or dioctyl phthalate.
4. preparation according to claim 3 has the method for the polymer microballoon of multi-stage artery structure, it is characterized in that, the addition of described pore-foaming agent is 0.3-0.7 milliliter.
5. preparation according to claim 2 has the method for the polymer microballoon of multi-stage artery structure, it is characterized in that, the injection speed of described polyvinyl alcohol water solution is 2-8 ml/hour.
6. preparation according to claim 2 has the method for the polymer microballoon of multi-stage artery structure, it is characterized in that, described emulsifying agent is class 80 of department.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410109418.6A CN103908935B (en) | 2014-03-21 | 2014-03-21 | A kind of capillary glass tube microfluidic devices and use this device to prepare there is the method for the polymer microballoon of multi-stage artery structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410109418.6A CN103908935B (en) | 2014-03-21 | 2014-03-21 | A kind of capillary glass tube microfluidic devices and use this device to prepare there is the method for the polymer microballoon of multi-stage artery structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103908935A CN103908935A (en) | 2014-07-09 |
| CN103908935B true CN103908935B (en) | 2016-02-10 |
Family
ID=51035119
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410109418.6A Active CN103908935B (en) | 2014-03-21 | 2014-03-21 | A kind of capillary glass tube microfluidic devices and use this device to prepare there is the method for the polymer microballoon of multi-stage artery structure |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103908935B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861129B (en) * | 2015-04-27 | 2017-07-25 | 中国科学院长春应用化学研究所 | The preparation method and device of polymer Giant Vesicles |
| CN108980623B (en) * | 2018-06-22 | 2021-01-08 | 东莞理工学院 | Kinetic inhibition oil-water emulsion responding to hydrate and preparation method and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006000008A1 (en) * | 2004-06-29 | 2006-01-05 | Technische Universität Wien | Methods for the production of polymer carrier materials based on carbon hydrate-bis-(meth)acryl- amides |
| CN101073714A (en) * | 2007-04-06 | 2007-11-21 | 武汉大学 | Method for producing solid-phase microextraction capillaries |
| CN101735414A (en) * | 2009-12-18 | 2010-06-16 | 中国科学院化学研究所 | Porous polymer whole separating material and preparation method thereof |
| CN102026725A (en) * | 2008-03-14 | 2011-04-20 | 科隆迪亚戈有限公司 | Assays |
| CN103508411A (en) * | 2013-09-10 | 2014-01-15 | 上海交通大学 | Preparation method of microfluidic monolithic column chip and application of chip in raman detection |
-
2014
- 2014-03-21 CN CN201410109418.6A patent/CN103908935B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006000008A1 (en) * | 2004-06-29 | 2006-01-05 | Technische Universität Wien | Methods for the production of polymer carrier materials based on carbon hydrate-bis-(meth)acryl- amides |
| CN101073714A (en) * | 2007-04-06 | 2007-11-21 | 武汉大学 | Method for producing solid-phase microextraction capillaries |
| CN102026725A (en) * | 2008-03-14 | 2011-04-20 | 科隆迪亚戈有限公司 | Assays |
| CN101735414A (en) * | 2009-12-18 | 2010-06-16 | 中国科学院化学研究所 | Porous polymer whole separating material and preparation method thereof |
| CN103508411A (en) * | 2013-09-10 | 2014-01-15 | 上海交通大学 | Preparation method of microfluidic monolithic column chip and application of chip in raman detection |
Non-Patent Citations (1)
| Title |
|---|
| Synthesis and applications of emulsion-templated porous materials;Haifei Zhang，Andrew I. Cooper;《Soft Matter》;20050531;第107-1113页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103908935A (en) | 2014-07-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Yu et al. | Coaxial electrospinning with organic solvent for controlling the size of self-assembled nanoparticles | |
| CN104436760B (en) | A kind of magnetic response high efficiency oil-water separation tunica fibrosa and preparation method thereof | |
| Jeong et al. | Controlled generation of submicron emulsion droplets via highly stable tip-streaming mode in microfluidic devices | |
| Homaeigohar et al. | Novel compaction resistant and ductile nanocomposite nanofibrous microfiltration membranes | |
| CN106040117B (en) | The method that monodispersity calcium alginate microsphere is prepared based on emulsion liquid membrane mass transfer | |
| US20060063882A1 (en) | Process for preparing microrods using liquid-liquid dispersion | |
| CN103866492A (en) | Efficient oil and water separation composite fiber film and preparation method thereof | |
| CN100547131C (en) | The preparation of coaxial spinning technology has the method for hierarchical organization hollow molecules sieve fiber | |
| Wang et al. | Plugging properties and profile control effects of crosslinked polyacrylamide microspheres | |
| Zhang et al. | A microfluidic approach to fabricate monodisperse hollow or porous poly (HEMA–MMA) microspheres using single emulsions as templates | |
| CN103374141B (en) | Method for preparing faveolate polymer microsphere on basis of micro-fluidic chip | |
| CN103908935B (en) | A kind of capillary glass tube microfluidic devices and use this device to prepare there is the method for the polymer microballoon of multi-stage artery structure | |
| Dong et al. | Preparation of 10 μm scale monodispersed particles by jetting flow in coaxial microfluidic devices | |
| Fan et al. | Annealing effect on electrospun polymer fibers and their transformation into polymer microspheres | |
| CN102757012B (en) | Method for preparing micro-solution storage and multi-phase heterogenous microparticles | |
| CN106757516A (en) | The method that micro-fluidic electrostatic spinning prepares multilevel hierarchy high molecular superfine fiber | |
| CN104909326B (en) | Microparticle with micron/nanometer hierarchical pores and preparation method thereof | |
| CN106917189B (en) | A kind of CS/PLA water-oil separating nano fibrous membrane and preparation method thereof that hole is controllable | |
| Chen et al. | Janus membrane emulsification for facile preparation of hollow microspheres | |
| CN102697727B (en) | Method for preparing self-assembly ketoprofen liposome by electrostatic spinning technology | |
| CN105780299B (en) | Preparation method of supermolecule adsorption filter screen | |
| Schramm | Nano-and Microtechnology from A-Z: From Nanosystems to Colloids and Interfaces | |
| CN115155472B (en) | Method for preparing polymer microsphere by adopting phase inversion method | |
| CN104072788B (en) | Method of preparing cellulose microspheres by multichannel microflow device | |
| CN105326809A (en) | Preparation method for composite natural polymer microcapsules containing CaCO3 particles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |