CN101844406A - Device and method for manufacturing micro-nano porous structure - Google Patents
Device and method for manufacturing micro-nano porous structure Download PDFInfo
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- CN101844406A CN101844406A CN 201010160736 CN201010160736A CN101844406A CN 101844406 A CN101844406 A CN 101844406A CN 201010160736 CN201010160736 CN 201010160736 CN 201010160736 A CN201010160736 A CN 201010160736A CN 101844406 A CN101844406 A CN 101844406A
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Abstract
The invention discloses a device and a method for manufacturing a micro-nano porous structure, and relates to a micro-nano porous structure. The device is provided with an electric spinning solution tube, an injection pump, a perfusion tube, an electric spinning spray head, a device bracket, upper and lower rotating motors, a heater, a collecting belt, a skeleton solution tank and a lifting platform. The collecting belt is wound between rotating shafts of the upper and lower rotating motors, the electric spinning spray head is positioned above the upper rotating motor, the lifting platform is positioned on a base of the device bracket, and skeleton solution is just contacted with the lowest part of the collecting belt. During preparation, electric spinning nano fibers can be uniformly deposited on the surface of the collecting belt along with the rotation of the collecting belt, the skeleton solution forms a coat on the surface of the collecting belt, and then a multilayer film structure formed by alternative nano fiber films and solution coats is obtained. The multilayer film structure is taken down from the collecting belt, the edge of the multilayer structure is cut to remove the nano fiber films on the partial skeleton solution coats, then the multilayer structure is soaked into selective solution to remove the nano fiber films and heated to form the porous structure, and the aperture is between 100 and 800 nanometers.
Description
Technical field
The present invention relates to a kind of micro-nano porous structure, especially relate to a kind of micro-nano porous structure manufacturing installation and manufacture method based on electrostatic spinning.
Background technology
Porous material has excellent performance such as big specific area, good adsorption, permeability, damping shock absorption, impact energy absorption, sound absorption, electromagnetic shielding, has all demonstrated huge application potential at aspects such as prevention and cure of pollution, cooling integrated, Industrial Catalysis, chromatography filtration, Aero-Space lightweight protective materials, construction equipments.And polymer porous structure with its good biological compatibility, be easy to advantages such as integrated modification and all have its special advantages at aspects such as biological medicine, micro-nano mechanical-electronic system, little energy systems, be subjected to day by day paying close attention to widely, become the research focus of porous material.Develop a kind of efficient, convenient, polymer porous structure preparation method that can realize industrial applications, become the key point of present industrialization process.
For example, document [1] adopts with stainless steel wire as skeleton, skin is coated with absorbable polyester material (Poly (L-lactide-co-D, L-lactide) 70:30), in soya-bean oil, soak the decomposition of heating realization to Celogen Az, above steel-wire carcass, form loose structure, have good compression strength and high porosity and be good material as bionical skeleton, but preparation process comparatively complexity be unfavorable for mass production.Phase separation method is the main preparation methods of organic micro-nano porous structure, reported that as document [2] use high-solidification point solvent cryogenic quick freezing prepares polylactic acid/hydroxy acetate (poly (D, L-lactic-co-glycolic acid), PLGA) method of nanostructured, this kind micro-nano structure has good bio-compatibility, sticking, breeding and moving and have a significant effect polymer porous structure average pore size 50 μ m for cell.The same method that is separated that adopts of document [3] has been prepared 85/15poly (D, L-lactide-co-gly-colide) foam-like loose structure, aperture 30～100 μ m, has biological degradability preferably, can be applied to fields such as biological tissue's skeleton, utilize the loose structure aperture of phase disengagement method preparation to be unfavorable for further promoting performance and its range of application of expansion more greatly.Document [4] adopts the surface-treated method to carry out the preparation of nanostructured, and the roughness that has improved material surface by chemical surface treatment makes it be applicable to biologic bracket materials such as artificial tubes, but chemical method for treating surface is difficult to realize the preparation of three-dimensional micro-nano structure.Suspension polymerization [5] often is used to prepare the porous polymer microsphere structure, and the microballoon sphere diameter can be controlled 100～200 μ m.Seed swelling method [6] is the another kind of porous polymer microsphere structure preparation method commonly used, porous ball sphere diameter can be reduced to 3～15 μ m, these two kinds of methods can prepare micrometer level porous structure preferably, wouldn't be suitable for building of industrialization production and three-dimensional framework but the preparation method is complicated.
Electrostatic spinning is a kind of emerging nanostructured preparation method, have that nanofiber diameter is little, specific area is big, handiness is simple, material source is extensive, controlled, the pure physical process of nanofiber surface apertures is not destroyed advantages such as material character, all have important development prospect at aspects such as organic flexible electronic, biological skeletons.At present, the electrostatic spinning nano fiber applications has been become a research focus in biomedicine field, electro spinning nano fiber has been used to prepare the biological skeleton material as document [7].But the selective deposition of electrospinning silk nanofiber, industrialization production and three-dimensional structure are still the electrostatic spinning technique development problem, and have become the key factor of restriction electrostatic spinning technique development and application.
List of references:
[1]S.P.Lin，T.H.Barrows，S.H.Cartmell，et?al.，Biomaterials，2003，24：481-489。
[2] Yin Dezheng, Xiong Zhuo, Zhang Renji, etc. material Leader, 2006,20,393-396.
[3]Lakhwant?Singha，Vipin?Kumara，Buddy?D?Ratner.Biomaterials，2004，25：2611-2617。
[4]Miller?D?C，Thapa?A.Haberst?roh?K?M，et?al..Biomaterials，2004，25(1)：53-61。
[5]Macintyre.F.S，Sherrington.D.C.Macromolecules，2004，37(20)：7628-7636。
[6]Tuncel?A，Tuncel?M，and?Ergun?B，et?al.Colloids?Surf.，A，2002，197(1～3)：79-94。
[7]K.M.Woo，V.J.Chen，P.X.Ma，J.Biomed.Mater.Res.Part?A，2003，67A：531-537。
Summary of the invention
The object of the present invention is to provide a kind of micro-nano porous structure manufacturing installation and manufacture method that can prepare loose structure continuously.
Micro-nano porous structure manufacturing installation of the present invention is provided with electrospinning silk solution memotron, syringe pump, power supply, woven hose, electrospinning silk shower nozzle, appliance stand, goes up electric rotating machine, heater, collecting belt, lower rotating electrical machine, skeleton solution tank, hoistable platform.Electrospinning silk solution is stored in the electrospinning silk solution memotron; Electrospinning silk solution memotron is installed on the syringe pump, and electrospinning silk solution memotron is connected with electrospinning silk shower nozzle through woven hose; Positive source is electrically connected with electrospinning silk shower nozzle, and power cathode links to each other with appliance stand and collecting belt; Electrospinning silk shower nozzle is positioned at the electric rotating machine top, and the nanofiber that electrospinning silk shower nozzle sprays can be deposited on the collecting board upper top; Appliance stand be provided with from top to down successively the shower nozzle installing rack, on cantilever is installed, middle cantilever is installed, down cantilever is installed; Last electric rotating machine is installed on to be installed on the cantilever, installs on the cantilever in the middle of heater is installed on, and lower rotating electrical machine is installed on down installs on the cantilever; Heater is provided with left heating clamber and right heating clamber, and left heating clamber and right heating clamber carry out temperature control respectively; Collecting belt is wound between electric rotating machine and lower rotating electrical machine two turning cylinders, can be with the rotation campaign of motor; The collecting belt right-hand member passes through the right heating clamber heating region of heater, and the collecting belt left end passes through the left heating clamber heating region of heater; Hoistable platform is placed on the base of appliance stand; The skeleton solution tank places on the hoistable platform, holds skeleton solution in the skeleton solution tank.The at the uniform velocity rotation of motor has guaranteed the uniformity of nano fibrous membrane and skeleton solution coatings thickness.
Described collecting belt preferably adopts flexible collecting belt, and described flexible collecting belt can be fexible conductor film or insulator film, and the thickness of described fexible conductor film can be 0.1～2mm, and the thickness of described insulator film can be 0.1～2mm.
The manufacture method of porous micro nano structure of the present invention adopts described micro-nano porous structure manufacturing installation, and its manufacture method may further comprise the steps:
1) platform falls in adjusting, makes skeleton solution just in time contact the collecting belt lowest part;
2) electrospinning silk solution is injected electrospinning silk solution memotron, and electrospinning silk solution memotron is installed on the syringe pump, start syringe pump and regulate liquid supply speed;
3) electric rotating machine and lower rotating electrical machine in the startup drive collecting belt and rotate;
4) treat that electrospinning silk solution droplets appears in electrospinning silk shower nozzle place after, start DC high-voltage power supply, regulate DC high-voltage power supply voltage, solution stretcher strain under the electric field force effect produces jet, forms nanofiber and is deposited on the collecting belt;
5), will form the alternately multilayer membrane structure of stack of nano fibrous membrane and skeleton solution coatings on the collecting belt with the rotation of electric rotating machine;
6) the multilayer membrane structure is taken off from collecting belt, the edge is advanced cutting removal part skeleton coating expose nano fibrous membrane;
7) the multilayer membrane structure after the cutting is soaked in the selective dissolution liquid;
8) treat that nano fibrous membrane dissolving is removed after, the multilayer membrane structure is taken out, carry out heat drying and obtain micro-nano porous structure.
Last electric rotating machine equates that with lower rotating electrical machine rotating shaft rotational line speed rotating shaft rotational line speed is 0.1～2m/s.
Left heating clamber and right heating clamber can carry out temperature control respectively in the heater, and temperature controlling range is a room temperature to 80 ℃.
When making the porous micro nano structure, at first carry out the preparation of sandwich construction, regulate hoistable platform, make skeleton solution just in time contact the collecting belt lowest part, along with rotary electric machine rotates, can be coated with the even skeleton solution film of last layer on the collection surface; Open syringe pump, polymeric solution is transported to electrospinning silk shower nozzle by woven hose; Power-on, the solution at the electrospinning silk shower nozzle place generation jet that deforms under the effect of high voltage electric field, the nano fibrous membrane of formation is deposited on the collecting belt; Nano fibrous membrane heats its curing rate of raising and difficult drop-off after being deposited on collecting belt; Along with the motor rotation, the collecting belt that deposits nano fibrous membrane turns to lowest part and contacts with skeleton solution, forms layer of even skeleton solution coatings on the nano fibrous membrane surface; The flexible collecting belt that scribbles skeleton solution heats through heating clamber, and the skeleton solution coatings is solidified; When the flexible collecting belt that is solidified with the skeleton solution coatings rotates to highest point once more, new nano fibrous membrane will be arranged at skeleton solution coatings surface deposition, and so carry out repeatedly and will on flexible collecting belt, obtain the multilayer membrane structure that electro spinning nanometer fiber membrane and skeleton solution coatings replace.
The nano fibrous membrane dissolving is removed then, the multilayer membrane structure that electro spinning nanometer fiber membrane and skeleton solution coatings are replaced is taken into from collecting belt, to the marginal portion cutting, remove the unnecessary skeleton solution coatings in edge, multilayer membrane structure after the cutting is immersed in the selective dissolution solution, electro spinning nanometer fiber membrane is removed in dissolving, obtains micro-nano porous structure thereby carry out heat drying.
The present invention adopts the electrostatic spinning nano tunica fibrosa as sacrifice layer, realizes that by electric spinning equipment and rotating mechanism the alternately stack of layers of nanofibers and skeleton solution coatings obtains the multilayer membrane structure; The multilayer membrane structure is removed nanofiber by soaking selective dissolution liquid, thereby forms loose structure through heat drying again, and the aperture pore-size distribution is in 100～800nm in the loose structure.
Description of drawings
Fig. 1 is the structural representation of micro-nano porous structure manufacturing installation of the present invention.
Fig. 2 is the electron microscope picture that utilizes one of the micro-nano porous structure of described micro-nano porous structure manufacturing installation preparation.In Fig. 2, scale is 0.1 μ m.
Fig. 3 is two the electron microscope picture that utilizes the micro-nano porous structure of described micro-nano porous structure manufacturing installation preparation.In Fig. 3, scale is 0.1 μ m.
For micro-nano porous structure manufacturing installation involved in the present invention is described better, now in conjunction with the accompanying drawings:
As shown in Figure 1, micro-nano porous structure manufacturing installation involved in the present invention comprise electrospinning silk solution memotron 1, syringe pump 2, DC high-voltage power supply 3, woven hose 4, shower nozzle installing rack 5, electrospinning silk shower nozzle 6, appliance stand 7, on cantilever 8 be installed, gone up electric rotating machine 9, middle cantilever 10, heater 11, flexible collecting belt 12 be installed, down main parts size such as cantilever 13, lower rotating electrical machine 14, skeleton liquid solution groove 15, accurate hoistable platform 16 be installed.
Electrospinning silk solution is stored in the electrospinning silk solution memotron 1; Electrospinning silk solution memotron 1 is installed on the syringe pump 2; Solution can at the uniform velocity be delivered to electrospinning silk shower nozzle 6 through woven hose 4 in the electrospinning silk solution memotron 1.DC high-voltage power supply 3 can provide static to spin needed high direct voltage, and its positive pole is realized being electrically connected by lead and electrospinning silk shower nozzle 6, and negative pole joins by lead and appliance stand 7 and flexible collecting belt 12.Electrospinning silk shower nozzle 6 is positioned at electric rotating machine 9 tops.Appliance stand 7 have from top to down successively shower nozzle installing rack 5, on cantilever 8 is installed, middle cantilever 10 is installed, down cantilever 13 is installed; Electrospinning silk shower nozzle 6 is installed on shower nozzle installing rack 5, go up electric rotating machine 9 is installed on and installs that cantilever 8, heater 11 are installed cantilever 10 in the middle of being installed on, lower rotating electrical machine 14 is installed on down installation cantilever 13.Two heating clambers about heater 11 has, two heating clambers can carry out temperature control respectively; Flexible collecting belt 12 is wound between electric rotating machine 9 and 14 liang of motor rotation axis of lower rotating electrical machine, and can rotate along with the rotation of two motors; The flexible collecting belt 12 in right side passes through heater 11 right heating clamber heating regions; Flexible 12 bands of collecting in left side pass through heater 11 left heating clamber heating regions.On accurate hoistable platform 16 apparatus for placing supports 7 bases; Skeleton solution tank 15 places on the accurate hoistable platform 16, can accurately adjust the height of skeleton solution tank; Fill skeleton solution in the skeleton solution tank 15.
Adopt mass percent be 18% polyethylene glycol oxide (the PolyEthylene Oxide PEO) aqueous solution as electrospinning silk solution, adopt polyimides (PI Polyimide) liquid as skeleton solution, adopt deionized water as selective dissolution liquid.The supreme electric rotating machine of electrospinning silk shower nozzle top 120mm, DC high-voltage power supply applies voltage 10kV, electrospinning silk solution liquid supply speed 250 μ l/h, adopt thickness be the copper film of 0.gmm as flexible collecting belt, flexible collecting belt rotational line speed 1m/s.Collecting belt is for rotating counterclockwise 30 ℃ of the left heating clamber temperature of heater, 35 ℃ of right heating clamber temperature during rotation.After collecting 30min, take off the multilayer membrane structure, be soaked in the deionized water and take out behind the 36h, be heated to 40 ℃ of dry 24h from collecting belt.Utilize electron microscope to observe, loose structure that must be shown in Fig. 2 and 3, aperture 100～250nm.
During manufacturing, carry out according to the following steps:
A) regulate accurate hoistable platform 16, make skeleton solution just in time contact flexible collecting belt 12 lowest parts;
B) electrospinning silk solution is injected electrospinning silk solution memotron 1, be installed on the syringe pump 2, start syringe pump 2 and regulate liquid supply speed;
C) electric rotating machine 9 and lower rotating electrical machine 14 in the startup drive flexible collecting belt 12 and rotate;
D) treat that electrospinning silk solution droplets appears in electrospinning silk shower nozzle 6 places after, start DC high-voltage power supply 3, regulate DC high-voltage power supply 3 voltages, solution stretcher strain under the electric field force effect produces jet, forms nanofiber and is deposited on the flexible collecting belt 12;
E), will form the alternately multilayer membrane structure of stack of nano fibrous membrane and skeleton solution coatings on the flexible collecting belt 12 with the rotation of electric rotating machine;
F) the multilayer membrane structure is taken off from collecting belt 12, the edge is advanced cutting removal part skeleton coating expose nano fibrous membrane;
G) the multilayer membrane structure after the cutting is soaked in the selective dissolution liquid;
H) treat that nano fibrous membrane dissolving is removed after, the multilayer membrane structure is taken out, carry out heat drying and obtain micro-nano porous structure.
Last electric rotating machine 9 equates rotating shaft rotational line speed 0.1m/s to 2m/s with lower rotating electrical machine 14 rotating shaft rotational line speed.
Left heating clamber and right heating clamber can carry out temperature control respectively in the heater 11, and temperature controlling range is a room temperature to 80 ℃.
The sacrifice layer that adopts high-pressure electrostatic stretching formulations prepared from solutions nanofiber to make as loose structure.
The sandwich construction that soaks after the selective dissolution liquid can direct drying in air, also can add protective gas at airtight condition and carry out heat drying.
Chemical reaction can not take place in electrospinning silk solution and skeleton solution; The solid nano fiber can not dissolve in skeleton solution; Solid-state skeleton coating can not dissolved in selective dissolution liquid, and solid-state electro spinning nano fiber can dissolve after soaking in selective dissolution liquid fully.
Claims (4)
1. micro-nano porous structure manufacturing installation, it is characterized in that being provided with electrospinning silk solution memotron, syringe pump, power supply, woven hose, electrospinning silk shower nozzle, appliance stand, go up electric rotating machine, heater, collecting belt, lower rotating electrical machine, skeleton solution tank, hoistable platform, electrospinning silk solution is stored in the electrospinning silk solution memotron; Electrospinning silk solution memotron is installed on the syringe pump, and electrospinning silk solution memotron is connected with electrospinning silk shower nozzle through woven hose; Positive source is electrically connected with electrospinning silk shower nozzle, and power cathode links to each other with appliance stand and collecting belt; Electrospinning silk shower nozzle is positioned at the electric rotating machine top; Appliance stand be provided with from top to down successively the shower nozzle installing rack, on cantilever is installed, middle cantilever is installed, down cantilever is installed; Last electric rotating machine is installed on to be installed on the cantilever, installs on the cantilever in the middle of heater is installed on, and lower rotating electrical machine is installed on down installs on the cantilever; Heater is provided with left heating clamber and right heating clamber; Collecting belt is wound between electric rotating machine and lower rotating electrical machine two turning cylinders, and the collecting belt right-hand member passes through the right heating clamber heating region of heater, and the collecting belt left end passes through the left heating clamber heating region of heater; Hoistable platform is placed on the base of appliance stand; The skeleton solution tank places on the hoistable platform, holds skeleton solution in the skeleton solution tank.
2. a kind of micro-nano porous structure manufacturing installation as claimed in claim 1 is characterized in that described collecting belt is flexible collecting belt.
3. a kind of micro-nano porous structure manufacturing installation as claimed in claim 2, it is characterized in that described flexible collecting belt is fexible conductor film or insulator film, the thickness of described fexible conductor film is 0.1～2mm, and the thickness of described insulator film is 0.1～2mm.
4. the manufacture method of porous micro nano structure as claimed in claim 1 adopts micro-nano porous structure manufacturing installation according to claim 1, and its manufacture method may further comprise the steps:
1) platform falls in adjusting, makes skeleton solution just in time contact the collecting belt lowest part;
2) electrospinning silk solution is injected electrospinning silk solution memotron, and electrospinning silk solution memotron is installed on the syringe pump, start syringe pump and regulate liquid supply speed;
3) electric rotating machine and lower rotating electrical machine in the startup drive collecting belt and rotate;
4) treat that electrospinning silk solution droplets appears in electrospinning silk shower nozzle place after, start DC high-voltage power supply, regulate DC high-voltage power supply voltage, solution stretcher strain under the electric field force effect produces jet, forms nanofiber and is deposited on the collecting belt;
5), will form the alternately multilayer membrane structure of stack of nano fibrous membrane and skeleton solution coatings on the collecting belt with the rotation of electric rotating machine;
6) the multilayer membrane structure is taken off from collecting belt, the edge is advanced cutting removal part skeleton coating expose nano fibrous membrane;
7) the multilayer membrane structure after the cutting is soaked in the selective dissolution liquid;
8) treat after nano fibrous membrane dissolving is removed the multilayer membrane structure to be taken out, carry out heat drying and obtain micro-nano porous structure.
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| CN102776582A (en) * | 2012-05-24 | 2012-11-14 | 东华大学 | Automatic control multi-spray-head electrostatic spinning equipment |
| CN102922891A (en) * | 2012-10-26 | 2013-02-13 | 厦门大学 | Electro-hydraulic jet printing device of metal micro-nanometer structure |
| CN102978719A (en) * | 2012-12-21 | 2013-03-20 | 厦门大学 | Vacuum electro-spinning device |
| CN103255485A (en) * | 2013-05-20 | 2013-08-21 | 江苏菲特滤料有限公司 | Tip-end type needle-free electrostatic spinning equipment |
| CN103556240A (en) * | 2013-11-22 | 2014-02-05 | 苏州大学张家港工业技术研究院 | Electrostatic spinning device for preparing nano-porous fibers |
| CN103596751A (en) * | 2011-04-06 | 2014-02-19 | 约翰逊控制技术公司 | Seat cushion having an electrospun nonwoven polymer layer |
| CN109338598A (en) * | 2018-11-12 | 2019-02-15 | 清华大学 | A kind of methods and applications forming film |
| CN109929128A (en) * | 2019-01-28 | 2019-06-25 | 厦门大学 | Near field direct write based on PEO electrospinning film substrate focuses and micro- pattern is detached from method |
| CN110528090A (en) * | 2019-09-05 | 2019-12-03 | 南京工业职业技术学院 | A kind of preparation facilities and preparation method of high porosity porous fibrous structure |
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| CN103596751A (en) * | 2011-04-06 | 2014-02-19 | 约翰逊控制技术公司 | Seat cushion having an electrospun nonwoven polymer layer |
| CN102776582A (en) * | 2012-05-24 | 2012-11-14 | 东华大学 | Automatic control multi-spray-head electrostatic spinning equipment |
| CN102922891A (en) * | 2012-10-26 | 2013-02-13 | 厦门大学 | Electro-hydraulic jet printing device of metal micro-nanometer structure |
| CN102922891B (en) * | 2012-10-26 | 2014-08-06 | 厦门大学 | Electro-hydraulic jet printing device of metal micro-nanometer structure |
| CN102978719A (en) * | 2012-12-21 | 2013-03-20 | 厦门大学 | Vacuum electro-spinning device |
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| CN103556240B (en) * | 2013-11-22 | 2016-08-17 | 苏州大学张家港工业技术研究院 | For preparing the electrostatic spinning apparatus of nano-porous fiber |
| CN109338598A (en) * | 2018-11-12 | 2019-02-15 | 清华大学 | A kind of methods and applications forming film |
| CN109929128A (en) * | 2019-01-28 | 2019-06-25 | 厦门大学 | Near field direct write based on PEO electrospinning film substrate focuses and micro- pattern is detached from method |
| CN110528090A (en) * | 2019-09-05 | 2019-12-03 | 南京工业职业技术学院 | A kind of preparation facilities and preparation method of high porosity porous fibrous structure |
| CN110528090B (en) * | 2019-09-05 | 2024-02-02 | 南京工业职业技术学院 | Preparation device and preparation method of high-porosity porous structure fiber |
| CN111389472A (en) * | 2020-03-23 | 2020-07-10 | 南京工业职业技术学院 | Device and method for preparing electrospinning direct-writing multilayer microfluidic chip |
| CN114016208A (en) * | 2021-10-22 | 2022-02-08 | 武汉纺织大学 | Preparation method of high-insulation high-strength polyimide fiber paper |
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