CN103225115A - Method for preparing nano porous material by utilizing electrostatic spinning technique - Google Patents
Method for preparing nano porous material by utilizing electrostatic spinning technique Download PDFInfo
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- CN103225115A CN103225115A CN2013101511029A CN201310151102A CN103225115A CN 103225115 A CN103225115 A CN 103225115A CN 2013101511029 A CN2013101511029 A CN 2013101511029A CN 201310151102 A CN201310151102 A CN 201310151102A CN 103225115 A CN103225115 A CN 103225115A
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Abstract
The invention discloses a method for preparing a nano porous material by utilizing the electrostatic spinning technique. The method comprises the following steps: trichloromethane and isopropyl alcohol are mixed according to a mass ratio of 9:1 to obtain a mixed solution as a solvent; 12% poly butylenes succinate and 2% Yunnan Baiyao are dissolved in the mixed solution, and the container containing the mixed solution is sealed; the temperature of the solvent is adjusted at 25 DEG C and kept constant, and after stirring for 3-6 hours, a uniform and transparent solution is obtained; under the conditions of room temperature and relative humidity of 50%-80%, electrostatic spinning is performed to the uniform and transparent solution obtained, wherein the distance between a dash receiver and a spinneret is 10-20 cm, and the voltage is 8-15 kw, the flow rate is 1.5-8 ml/h, and the nano porous material is directly obtained through the electrostatic spinning technique without any further treatment. The method provided by the invention has the advantages that the structure is simple, the operation is convenient, the control is simple and the technological process is short, and provides a raw material ratio and experiment conditions, which are most suitable for preparing the nano porous material.
Description
Technical field
The present invention relates to the electrostatic spinning field, relate in particular to a kind of method of utilizing electrostatic spinning technique to prepare nano-porous materials.
Background technology
Nano-porous materials has characteristics such as superelevation absorption, high surface energy, high surface, can be used for filtration, obstruct, diffusion barrier, dress materials, bio-medical material and novel light composite etc., demonstrated great application prospect at aspects such as biology, medicine, the energy, environment, advanced manufacturing technology and national defence.The method for preparing nano-porous materials roughly has sol-gel process, hydrothermal synthesis method and electrostatic spinning technique etc.
Rise along with nanosecond science and technology, people give to prepare the method for electrostatic spinning of continuous micro nanometer fiber with great concern, method of electrostatic spinning is the important method that the electric field force strained polymer solution that produces by HV generator or melt prepare superfine fibre, is a kind of method of easy and simple to handle, applied widely, spinning nanofiber that production efficiency is higher relatively.This method has become the focus of exploitation nano material, and the potential application of having opened up nanofiber.
The various particular performances that static spins nano-porous materials can be applicable to photon structure, microfluid channel, catalyst, medical science, pharmacy, drug delivery, hidden apparatus (for example: stealth aircraft, contact clothing), radiation protection, organizational engineering, liquid storage and conveying, electrode material or reactor etc.
In the electrostatic spinning process, influence several important parameters of electrostatic spinning process, comprise polymer solution mass fraction, spinning voltage, receiving range, shower nozzle aperture and ambient temperature and humidity.The change of finding these parameters under study for action is very big to the influence of fibre diameter and morphosis thereof, so when utilizing electro-spinning to be equipped with nano-porous materials, its parameter has played crucial effects to the pore-forming of nanoporous.
Because, the pore-creating character of nano-porous materials is determining the effect of nano-porous materials, for this reason, we wish can avoid some troubles utilizing electrostatic spinning technique to prepare in the process of nano-porous materials, can directly prepare high-quality nano-porous materials, further promote the application of nano-porous materials.
Therefore, at above-mentioned technical problem, be necessary to provide a kind of new method of utilizing electrostatic spinning technique to prepare nano-porous materials, to solve the problems of the prior art.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of preparation method that just can prepare nanoscale porous material without pore creating material.
For achieving the above object, the invention provides following technical scheme:
A kind of method of utilizing electrostatic spinning technique to prepare nano-porous materials, it comprises the steps:
S1: is the proportioning mixing of 9:1 with chloroform and isopropyl alcohol by mass ratio, and the mixed liquor that obtains is as solvent;
S2: poly butylene succinate with 12% and 2% Yunnan Baiyao are dissolved in the mixed liquor among the step S1, will fill the seal of vessel of mixed liquor then;
S3: solution temperature is adjusted in 25 ℃, constant temperature and magnetic agitation 3-6 hour, until the solution that obtains transparent and homogeneous;
S4: in room temperature and relative humidity is under the condition of 55%-80%, and the polymer solution of the transparent and homogeneous that step S3 is obtained carries out electrostatic spinning and directly obtains nano-porous materials;
Among the described step S4, the polymer solution of transparent and homogeneous is carried out electrostatic spinning specifically comprise step: the polymer solution of transparent and homogeneous is added in the liquid storage tank, high voltage power supply device is connected on the spinning head, dash receiver is by ground power line ground connection, open high voltage power supply device, between spinning head and dash receiver, formed an electric field, make the polymer solution of the transparent and homogeneous in spinning head exit under the effect of high pressure, form solid jet, jet is collected nano-porous materials at last through swing, evaporation, fine process on dash receiver.
Preferably, utilize in the method that electrostatic spinning technique prepares nano-porous materials above-mentioned, when carrying out electrostatic spinning among the described step S4, the distance adjustment scope between dash receiver and the spinning head is 10-20cm.
Preferably, utilize in the method that electrostatic spinning technique prepares nano-porous materials above-mentioned, when carrying out electrostatic spinning among the described step S4, the voltage-regulation scope is 8-15kv.
Preferably, utilize in the method that electrostatic spinning technique prepares nano-porous materials above-mentioned, when carrying out electrostatic spinning among the described step S4, the flow velocity setting range is 1.5-8ml/h.
From technique scheme as can be seen, the invention provides proportioning raw materials and experiment condition that optimum prepares nano-porous materials, utilize direct preparation nano-porous materials of electrostatic spinning technique one step then, simple in structure, easy to operate, control is simple, technological process is short.
Description of drawings
In order to be illustrated more clearly in the embodiment of the invention or technical scheme of the prior art, to do to introduce simply to the accompanying drawing of required use in embodiment or the description of the Prior Art below, apparently, accompanying drawing relevant of the present invention in describing below only is some embodiments of the present invention, for those of ordinary skills, under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Fig. 1 is that the present invention utilizes electrostatic spinning technique to prepare the flow chart of the method for nano-porous materials.
The specific embodiment
The invention discloses a kind of preparation method that just can prepare nanoscale porous material without pore creating material.
Below in conjunction with the accompanying drawing in the embodiment of the invention, the technical scheme in the embodiment of the invention is described in detail, obviously, described embodiment only is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, the every other embodiment that those of ordinary skills are obtained under the prerequisite of not making creative work belongs to the scope of protection of the invention.
As shown in Figure 1, the method for utilizing electrostatic spinning technique to prepare nano-porous materials disclosed by the invention, it comprises the steps:
S1: is the proportioning mixing of 9:1 with chloroform and isopropyl alcohol by mass ratio, and the mixed liquor that obtains is as solvent;
S2: poly butylene succinate with 12% and 2% Yunnan Baiyao are dissolved in the mixed liquor among the step S1, will fill the seal of vessel of mixed liquor then;
S3: solution temperature is adjusted in 25 ℃, constant temperature and magnetic agitation 3-6 hour, until the solution that obtains transparent and homogeneous;
S4: in room temperature and relative humidity is under the condition of 55%-80%, and the polymer solution of the transparent and homogeneous that step S3 is obtained carries out electrostatic spinning and directly obtains nano-porous materials.
Among the described step S4, the polymer solution of transparent and homogeneous is carried out electrostatic spinning specifically comprise step: the polymer solution of transparent and homogeneous is added in the liquid storage tank, high voltage power supply device is connected on the spinning head, dash receiver is by ground power line ground connection, open high voltage power supply device, between spinning head and dash receiver, formed an electric field, make the polymer solution of the transparent and homogeneous in spinning head exit under the effect of high pressure, form solid jet, jet is collected nano-porous materials at last through swing, evaporation, fine process on dash receiver.
When carrying out electrostatic spinning among the described step S4, the distance adjustment scope between dash receiver and the spinning head is 10-20cm, and the voltage-regulation scope is 8-15kv, and the flow velocity setting range is 1.5-8ml/h.
The invention provides proportioning raw materials and experiment condition that optimum prepares nano-porous materials, utilize direct preparation nano-porous materials of electrostatic spinning technique one step then, simple in structure, easy to operate, control is simple, technological process is short.
Below in conjunction with several specific embodiments the method for utilizing electrostatic spinning technique to prepare nano-porous materials of the present invention is further set forth.
Embodiment 1
The first step: is the proportioning mixing of 9:1 with chloroform and isopropyl alcohol by mass ratio, and the mixed liquor that obtains is as solvent;
Second step: poly butylene succinate with 12% and 2% Yunnan Baiyao (a kind of Chinese traditional Chinese medicine medicament) are dissolved in the mixed liquor, will fill the seal of vessel of mixed liquor then;
The 3rd step: solution temperature is adjusted in 25 ℃, and constant temperature and magnetic agitation 4 hours are until the solution that obtains transparent and homogeneous;
The 4th step: in room temperature and relative humidity is under the condition of 55%-80%, the polymer solution of the transparent and homogeneous that obtains is above carried out electrostatic spinning, distance adjustment between dash receiver and the spinning head is 10-20cm, voltage 8kv when regulating spinning, flow velocity is set at 1.5ml/h, need not post processing by electrostatic spinning technique and can directly obtain nano-porous materials.
Embodiment 2
The first step: is the proportioning mixing of 9:1 with chloroform and isopropyl alcohol by mass ratio, and the mixed liquor that obtains is as solvent;
Second step: poly butylene succinate with 12% and 2% Yunnan Baiyao (a kind of Chinese traditional Chinese medicine medicament) are dissolved in the mixed liquor, will fill the seal of vessel of mixed liquor then;
The 3rd step: solution temperature is adjusted in 25 ℃, and constant temperature and magnetic agitation 4 hours are until the solution that obtains transparent and homogeneous;
The 4th step, in room temperature and relative humidity is under the condition of 55%-80%, the polymer solution of the transparent and homogeneous that obtains is above carried out electrostatic spinning, distance adjustment between dash receiver and the spinning head is 10-20cm, voltage 8kv when regulating spinning, flow velocity is set at 3ml/h, need not post processing by electrostatic spinning technique and can directly obtain nano-porous materials.
Embodiment 3
The first step: is the proportioning mixing of 9:1 with chloroform and isopropyl alcohol by mass ratio, and the mixed liquor that obtains is as solvent;
Second step: poly butylene succinate with 12% and 2% Yunnan Baiyao (a kind of Chinese traditional Chinese medicine medicament) are dissolved in the mixed liquor, will fill the seal of vessel of mixed liquor then;
The 3rd step: solution temperature is adjusted in 25 ℃, and constant temperature and magnetic agitation 4 hours are until the solution that obtains transparent and homogeneous;
The 4th step: in room temperature and relative humidity is under the condition of 55%-80%, the polymer solution of the transparent and homogeneous that obtains is above carried out electrostatic spinning, distance adjustment between dash receiver and the spinning head is 10-20cm, voltage 8kv when regulating spinning, flow velocity is set at 5ml/h, need not post processing by electrostatic spinning technique and can directly obtain nano-porous materials.
Embodiment 4
The first step: is the proportioning mixing of 9:1 with chloroform and isopropyl alcohol by mass ratio, and the mixed liquor that obtains is as solvent;
Second step: poly butylene succinate with 12% and 2% Yunnan Baiyao (a kind of Chinese traditional Chinese medicine medicament) are dissolved in the mixed liquor, will fill the seal of vessel of mixed liquor then;
The 3rd step: solution temperature is adjusted in 25 ℃, and constant temperature and magnetic agitation 4 hours are until the solution that obtains transparent and homogeneous;
The 4th step: in room temperature and relative humidity is under the condition of 55%-80%, the polymer solution of the transparent and homogeneous that obtains is above carried out electrostatic spinning, distance adjustment between dash receiver and the spinning head is 10-20cm, voltage 8kv when regulating spinning, flow velocity is set at 8ml/h, need not post processing by electrostatic spinning technique and can directly obtain nano-porous materials.
Embodiment 5
The first step: is the proportioning mixing of 9:1 with chloroform and isopropyl alcohol by mass ratio, and the mixed liquor that obtains is as solvent;
Second step: poly butylene succinate with 12% and 2% Yunnan Baiyao (a kind of Chinese traditional Chinese medicine medicament) are dissolved in the mixed liquor, will fill the seal of vessel of mixed liquor then;
The 3rd step: solution temperature is adjusted in 25 ℃, and constant temperature and magnetic agitation 4 hours are until the solution that obtains transparent and homogeneous;
The 4th step: in room temperature and relative humidity is under the condition of 55%-80%, the polymer solution of the transparent and homogeneous that obtains is above carried out electrostatic spinning, distance adjustment between dash receiver and the spinning head is 10-20cm, voltage 10kv when regulating spinning, flow velocity is set at 3ml/h, need not post processing by electrostatic spinning technique and can directly obtain nano-porous materials.
Embodiment 6
The first step: is the proportioning mixing of 9:1 with chloroform and isopropyl alcohol by mass ratio, and the mixed liquor that obtains is as solvent;
Second step: poly butylene succinate with 12% and 2% Yunnan Baiyao (a kind of Chinese traditional Chinese medicine medicament) are dissolved in the mixed liquor, will fill the seal of vessel of mixed liquor then;
The 3rd step: solution temperature is adjusted in 25 ℃, and constant temperature and magnetic agitation 4 hours are until the solution that obtains transparent and homogeneous;
The 4th step: in room temperature and relative humidity is under the condition of 55%-80%, the polymer solution of the transparent and homogeneous that obtains is above carried out electrostatic spinning, distance adjustment between dash receiver and the spinning head is 10-20cm, voltage 12kv when regulating spinning, flow velocity is set at 3ml/h, need not post processing by electrostatic spinning technique and can directly obtain nano-porous materials.
Embodiment 7
The first step: is the proportioning mixing of 9:1 with chloroform and isopropyl alcohol by mass ratio, and the mixed liquor that obtains is as solvent;
Second step: poly butylene succinate with 12% and 2% Yunnan Baiyao (a kind of Chinese traditional Chinese medicine medicament) are dissolved in the mixed liquor, will fill the seal of vessel of mixed liquor then;
The 3rd step: solution temperature is adjusted in 25 ℃, and constant temperature and magnetic agitation 4 hours are until the solution that obtains transparent and homogeneous;
The 4th step: in room temperature and relative humidity is under the condition of 55%-80%, the polymer solution of the transparent and homogeneous that obtains is above carried out electrostatic spinning, distance adjustment between dash receiver and the spinning head is 10-20cm, voltage 15kv when regulating spinning, flow velocity is set at 3ml/h, need not post processing by electrostatic spinning technique and can directly obtain nano-porous materials.
The invention provides optimum quality proportioning between the experimental raw, this proportioning can so that to the pore-creating character of nano-porous materials reach best.
The present invention utilizes direct preparation nano-porous materials of electrostatic spinning technique one step, and is simple in structure, easy to operate, control is simple, technological process is short, the proportioning raw materials and the experiment condition that provide optimum to prepare nano-porous materials.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and under the situation that does not deviate from spirit of the present invention or essential characteristic, can realize the present invention with other concrete form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims rather than above-mentioned explanation, therefore is intended to include in the present invention dropping on the implication that is equal to important document of claim and all changes in the scope.Any Reference numeral in the claim should be considered as limit related claim.
In addition, be to be understood that, though this specification is described according to embodiment, but be not that each embodiment only comprises an independently technical scheme, this narrating mode of specification only is for clarity sake, those skilled in the art should make specification as a whole, and the technical scheme among each embodiment also can form other embodiments that it will be appreciated by those skilled in the art that through appropriate combination.
Claims (4)
1. a method of utilizing electrostatic spinning technique to prepare nano-porous materials is characterized in that: comprise the steps:
S1: is the proportioning mixing of 9:1 with chloroform and isopropyl alcohol by mass ratio, and the mixed liquor that obtains is as solvent;
S2: poly butylene succinate with 12% and 2% Yunnan Baiyao are dissolved in the mixed liquor among the step S1, will fill the seal of vessel of mixed liquor then;
S3: solution temperature is adjusted in 25 ℃, constant temperature and magnetic agitation 3-6 hour, until the solution that obtains transparent and homogeneous;
S4: in room temperature and relative humidity is under the condition of 55%-80%, and the polymer solution of the transparent and homogeneous that step S3 is obtained carries out electrostatic spinning and directly obtains nano-porous materials;
Among the described step S4, the polymer solution of transparent and homogeneous is carried out electrostatic spinning specifically comprise step: the polymer solution of transparent and homogeneous is added in the liquid storage tank, high voltage power supply device is connected on the spinning head, dash receiver is by ground power line ground connection, open high voltage power supply device, between spinning head and dash receiver, formed an electric field, make the polymer solution of the transparent and homogeneous in spinning head exit under the effect of high pressure, form solid jet, jet is collected nano-porous materials at last through swing, evaporation, fine process on dash receiver.
2. the method for utilizing electrostatic spinning technique to prepare nano-porous materials according to claim 1 is characterized in that: when carrying out electrostatic spinning among the described step S4, the distance adjustment scope between dash receiver and the spinning head is 10-20cm.
3. the method for utilizing electrostatic spinning technique to prepare nano-porous materials according to claim 1 is characterized in that: when carrying out electrostatic spinning among the described step S4, the voltage-regulation scope is 8-15kv.
4. the method for utilizing electrostatic spinning technique to prepare nano-porous materials according to claim 1 is characterized in that: when carrying out electrostatic spinning among the described step S4, the flow velocity setting range is 1.5-8ml/h.
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Cited By (6)
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| 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 |
| CN103638561A (en) * | 2013-11-29 | 2014-03-19 | 苏州大学 | Preparation method of micro-nano bioactive porous material |
| CN105755676A (en) * | 2016-04-20 | 2016-07-13 | 徐海涛 | Method for producing gas filtration material with needleless electrospinning technology and application of gas filtration material |
| CN105780151A (en) * | 2016-04-20 | 2016-07-20 | 徐海涛 | Method for producing gas filtering material by melt electrospinning technology and application thereof |
| CN107157959A (en) * | 2017-03-29 | 2017-09-15 | 苏州大学 | A kind of mouth mask and preparation method for carrying medicine porous microsphere nano fibrous membrane |
| CN108998841A (en) * | 2017-06-07 | 2018-12-14 | 南京理工大学 | A kind of preparation method of porous polypropylene nitrile nanofibre |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| CN103638561A (en) * | 2013-11-29 | 2014-03-19 | 苏州大学 | Preparation method of micro-nano bioactive porous material |
| CN105755676A (en) * | 2016-04-20 | 2016-07-13 | 徐海涛 | Method for producing gas filtration material with needleless electrospinning technology and application of gas filtration material |
| CN105780151A (en) * | 2016-04-20 | 2016-07-20 | 徐海涛 | Method for producing gas filtering material by melt electrospinning technology and application thereof |
| CN107157959A (en) * | 2017-03-29 | 2017-09-15 | 苏州大学 | A kind of mouth mask and preparation method for carrying medicine porous microsphere nano fibrous membrane |
| CN108998841A (en) * | 2017-06-07 | 2018-12-14 | 南京理工大学 | A kind of preparation method of porous polypropylene nitrile nanofibre |
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