CN102776706A - Method for preparing polyetherimide amphipathic composite nano-scale fiber membrane - Google Patents
Method for preparing polyetherimide amphipathic composite nano-scale fiber membrane Download PDFInfo
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- CN102776706A CN102776706A CN2012102380650A CN201210238065A CN102776706A CN 102776706 A CN102776706 A CN 102776706A CN 2012102380650 A CN2012102380650 A CN 2012102380650A CN 201210238065 A CN201210238065 A CN 201210238065A CN 102776706 A CN102776706 A CN 102776706A
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Abstract
The invention relates to a method for preparing a polyetherimide amphipathic composite nano-scale fiber membrane, comprising the following steps: (1) mixing dichloromethane with N,N-dimethylacetamide to prepare a mixed solvent; adding polyetherimide and polyvinylpyrrolidone (PVP) into the mixed solvent; and oscillating for 8 to 24h till complete dissolution to obtain a spinning solution; and (2) adopting the spinning solution for electrostatic spinning, and finally drying to obtain the composite nano-scale fiber membrane. The preparation method is simple; the condition is mild; the evenly-mixed composite nano fiber membrane can be prepared in a single step; the prepared fiber has a smooth surface and is even in fineness; and in addition, the diameter distribution of the fiber is in a range of 400 nm to 1500nm.
Description
Technical field
The invention belongs to the preparation field of composite nano-fiber membrane, particularly a kind of preparation method of PEI amphiphilic composite nanometer level tunica fibrosa.
Background technology
Nano composite material is the new material of development in recent years; Since the size of nano composite material between molecule and body mutually between; Belong to Jie's sight system; Therefore show and molecule and the mutually different special nature of body, have tangible skin effect, quantum size effect, small-size effect and macro quanta tunnel effect, present many good physics and chemical characteristic.And the common methods of preparation nano composite material is a lot, for example: intercalation compounding, sol-gel process, situ aggregation method, supercritical ultrasonics technology, chemical dispersion additive method, blending method high polymeric solution direct insertion method, blending method high polymer fusion direct insertion method etc.
Owing to the upsurge of nanometer technology, the report that the applying high voltage electrostatic spinning technique prepares functional nano-fiber gets more and more in recent years.The researcher attempts various polymeric materials (comprising natural with synthetic macromolecule, protein even micromolecule etc.) to be prepared nano fibrous membrane through electrostatic spinning process, the function usefulness of performance material under nanoscale.These nanofibers carry out the common-sense application in various fields such as medicine, separation purification, the energy, environmental protection, catalytic reactions simultaneously.
The high-voltage electrostatic spinning technology is a kind of top-down nano-fabrication technique; The surface tension of liquid and the viscoelastic power of making every effort to overcome clothes shower nozzle capillary tip drop through extra electric field form jet; Under electrostatic repulsion, Coulomb force and surface tension acting in conjunction; Liquid jet after being atomized is crooked by high frequency, draw, divide, and drafted thousands of times in a few tens of milliseconds obtains nano-scale fiber through solvent evaporates or melt cooling at receiving terminal.This technical matters process is simple, control conveniently, select that material ranges is extensive, controllability strong and can have the nanofiber of microstructure characteristic through the sprinkler design preparation, is considered to have a kind of method that possibility realizes the continuous nano-fibre suitability for industrialized production.Should there be this technology to prepare functional nano-fiber and has good prospect prediction.And blended electro spinning prepares in the research of composite nano fiber; Some problems have been produced; Limited dissolving altogether/co-blended spinning of different material; These problems comprise the solvent that is difficult to obtain having simultaneously the difference in functionality material good solubility, and perhaps these well are total to broad dose and can not guarantee that polymeric material can form nanofiber under the electrostatic spinning process condition.Therefore, electrostatic spinning process research is still shouldered heavy responsibilities.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of PEI amphiphilic composite nanometer level tunica fibrosa; This preparation method is simple, and preparation condition is gentle, gained tunica fibrosa smooth surface; Fiber thickness is even, and distribution of fiber diameters is between 400-1000nm.
The preparation method of a kind of PEI amphiphilic composite nanometer level tunica fibrosa of the present invention comprises the following steps:
(1) preparing spinning solution: with carrene (DCM) and N; The mixed mixed solvent that gets of N-dimethylacetylamide (DMAC); PEI PEI and polyvinylpyrrolidone PVP are joined in the above-mentioned mixed solvent, vibration 8-24h to dissolve fully spinning solution;
(2) carrying out electricity spins: adopt above-mentioned spinning solution to carry out electrostatic spinning, final drying promptly gets composite Nano level tunica fibrosa.
The weight ratio of PEI described in the step (1) and polyvinylpyrrolidone is 1.0:1.0-5.0.
Polyvinylpyrrolidone PVP described in the step (1) is polyvinylpyrrolidone PVPK90.
The volume ratio of carrene and DMAC N,N is 5.0-6.0:1.0 in the described mixed solvent of step (1).
Adopt the 5mL syringe as the solution storage storage in the electrostatic spinning described in the step (2); The syringe needle that employing is scabbled is as the capillary that sprays thread; Described syringe needle is No. 5 stainless steel syringe needles; Internal diameter 0.5mm; The high pressure generator that is connected is the ZGF2000 type; Shanghai Su Te Electrical Appliances Co., Ltd, the spinning solution flow adopts the dull and stereotyped fiber that receives of aluminium foil by micro-injection pump (U.S.
company) control.
Electric spinning process parameter described in the step (2) does, advances speed 1.0-2.0mL/h, dash receiver from spinning nozzle apart from 10-25cm, voltage 12-16kv, environment temperature is 20-25 ℃, ambient humidity 67 ± 4%.
Distribution of fiber diameters is at 400-1000nm in the composite Nano level tunica fibrosa that obtains in the step (2).
Beneficial effect:
(1) preparation method of the present invention is simple, mild condition, but the composite nano-fiber membrane that the single step preparation mixes;
(2) gained fiber surface of the present invention is smooth, even thickness, and distribution of fiber diameters is between 400-1500nm.
Description of drawings
Fig. 1 is the high-voltage electrostatic spinning artwork;
PEI when Fig. 2 is electrostatic spinning high pressure 12kv/polyvinylpyrrolidone composite nano fiber ESEM picture;
PEI when Fig. 3 is electrostatic spinning high pressure 15kv/polyvinylpyrrolidone composite nano fiber ESEM picture;
PEI when Fig. 4 is electrostatic spinning high pressure 16kv/polyvinylpyrrolidone composite nano fiber ESEM picture.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The preparation of PEI/polyvinylpyrrolidone composite nano fiber, concrete steps are following:
(1) allotment of spinning solution
With carrene (DCM) 6mL, N; N-dimethylacetylamide (DMAC) 1mL packs in the tool plug triangular pyramidal bottle; Place constant-temperature shaking shaking table (25 ℃) vibration 10min; Polyether acid imide (PEI) 0.2000g and polyvinylpyrrolidone (PVP) 0.4000g are added in the solvent constant-temperature shaking 24h.
(2) electricity spins
With the above-mentioned spinning solution solution storage storage of packing into; The syringe needle that employing is scabbled (No. 5 stainless steel syringe needles; Internal diameter 0.5mm) as the capillary that sprays thread; Connect high pressure generator (ZGF2000 type; Shanghai Su Te Electrical Appliances Co., Ltd), the spinning solution flow adopts the aluminium foil flat board to accept fiber by micro-injection pump (U.S.
company) control.Electricity spinning process parameter: advance speed 1.0mL/h, dash receiver leaves spinning nozzle apart from 15cm, voltage 12kv.Other conditions: environment temperature is 25 ℃, ambient humidity 67 ± 4%.
(3) collect fiber, and be put in the dry 2d of vacuum drying chamber (37 ℃ of constant temperature), the back is through sem test such as Fig. 2.
Embodiment 2
The preparation of PEI/polyvinylpyrrolidone composite nano fiber, concrete steps are following:
(1) allotment of spinning solution: with carrene (DCM) 5mL, N; N-dimethylacetylamide (DMAC) 1mL packs in the tool plug triangular pyramidal bottle; Place constant-temperature shaking shaking table (25 ℃) vibration 10min; Polyether acid imide (PEI) 0.2000g and polyvinylpyrrolidone (PVP) 0.4000g are added in the solvent constant-temperature shaking 24h.。
(2) electricity spins: with the above-mentioned spinning solution solution storage storage of packing into; The syringe needle that employing is scabbled (No. 5 stainless steel syringe needles; Internal diameter 0.5mm) as the capillary that sprays thread; Connect high pressure generator (ZGF2000 type; Shanghai Su Te Electrical Appliances Co., Ltd), the spinning solution flow adopts the aluminium foil flat board to accept fiber by micro-injection pump (U.S.
company) control.
Electricity spinning process parameter: advance speed 1.0mL/h, dash receiver leaves spinning nozzle apart from 20cm, voltage 15kv.Other conditions: environment temperature is 25 ℃, ambient humidity 67 ± 4%.
(3) collect fiber, and be put in the dry 2d of vacuum drying chamber (37 ℃ of constant temperature), the back is through sem test such as Fig. 3.
Embodiment 3
The preparation of PEI/polyvinylpyrrolidone composite nano fiber, concrete steps are following:
(1) allotment of spinning solution
With carrene (DCM) 6mL, N; N-dimethylacetylamide (DMAC) 1mL packs in the tool plug triangular pyramidal bottle; Place constant-temperature shaking shaking table (25 ℃) vibration 10min; Polyether acid imide (PEI) 0.2000g and polyvinylpyrrolidone (PVP) 0.4000g are added in the solvent constant-temperature shaking 24h.
(2) electricity spins
With the above-mentioned spinning solution solution storage storage of packing into; The syringe needle that employing is scabbled (No. 5 stainless steel syringe needles; Internal diameter 0.5mm) as the capillary that sprays thread; Connect high pressure generator (ZGF2000 type; Shanghai Su Te Electrical Appliances Co., Ltd), the spinning solution flow adopts the aluminium foil flat board to accept fiber by micro-injection pump (U.S.
company) control.Electricity spinning process parameter: advance speed 1.0mL/h, dash receiver leaves spinning nozzle apart from 15cm, voltage 16kv.Other conditions: environment temperature is 25 ℃, ambient humidity 67 ± 4%.
(3) collect fiber, and be put in the dry 2d of vacuum drying chamber (37 ℃ of constant temperature), the back is through sem test such as Fig. 4.
Claims (7)
1. the preparation method of a PEI amphiphilic composite nanometer level tunica fibrosa comprises the following steps:
(1) with carrene and DMAC N,N mixed mixed solvent, PEI and polyvinylpyrrolidone PVP are joined in the above-mentioned mixed solvent, vibration 8-24h extremely dissolve fully spinning solution;
(2) adopt above-mentioned spinning solution to carry out electrostatic spinning, final drying promptly gets composite Nano level tunica fibrosa.
2. the preparation method of a kind of PEI amphiphilic composite nanometer level tunica fibrosa according to claim 1 is characterized in that: the weight ratio of PEI described in the step (1) and polyvinylpyrrolidone is 1.0:1.0-5.0.
3. the preparation method of a kind of PEI amphiphilic composite nanometer level tunica fibrosa according to claim 1 is characterized in that: the polyvinylpyrrolidone PVP described in the step (1) is polyvinylpyrrolidone PVPK90.
4. the preparation method of a kind of PEI amphiphilic composite nanometer level tunica fibrosa according to claim 1 is characterized in that: the volume ratio of carrene and DMAC N,N is 5.0-6.0:1.0 in the described mixed solvent of step (1).
5. the preparation method of a kind of PEI amphiphilic composite nanometer level tunica fibrosa according to claim 1 is characterized in that: adopt the 5mL syringe as the solution storage storage in the electrostatic spinning described in the step (2); The syringe needle that employing is scabbled is as the capillary that sprays thread, and described syringe needle is No. 5 stainless steel syringe needles, internal diameter 0.5mm; The spinning solution flow is controlled by micro-injection pump; Adopt the dull and stereotyped fiber that receives of aluminium foil.
6. the preparation method of a kind of PEI amphiphilic composite nanometer level tunica fibrosa according to claim 1; It is characterized in that: the electric spinning process parameter described in the step (2) is: advance speed 1.0-2.0mL/h; Dash receiver leaves spinning nozzle apart from 10-25cm; Voltage 12-16kv, environment temperature is 20-25 ℃, ambient humidity 67 ± 4%.
7. the preparation method of a kind of PEI amphiphilic composite nanometer level tunica fibrosa according to claim 1 is characterized in that: distribution of fiber diameters is at 400-1000nm in the composite Nano level tunica fibrosa that obtains in the step (2).
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Cited By (7)
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| CN103343423A (en) * | 2013-06-27 | 2013-10-09 | 北京化工大学常州先进材料研究院 | Crosslinking polyether imide fibrous membrane capable of being used as lithium ion battery separator and preparation thereof |
| CN108532025A (en) * | 2018-05-05 | 2018-09-14 | 程桂平 | A method of preparing composite fibre |
| CN108754872A (en) * | 2018-05-29 | 2018-11-06 | 郑州豫力新材料科技有限公司 | The production method of Static Spinning PLGA superfine fibre films |
| CN108807800A (en) * | 2018-08-08 | 2018-11-13 | 哈尔滨理工大学 | A kind of organo-mineral complexing lithium ion battery separator and preparation method thereof |
| CN110280229A (en) * | 2019-06-28 | 2019-09-27 | 东南大学 | Petrin class compound selective separation enrichment material preparation and application method |
| CN111910265A (en) * | 2020-07-17 | 2020-11-10 | 湖南工程学院 | Electrostatic spinning injection device with liquid preparation function |
| CN115369517A (en) * | 2022-08-30 | 2022-11-22 | 烟台民士达特种纸业股份有限公司 | Preparation method and application of polyether-ether-ketone nanofiber membrane |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103343423A (en) * | 2013-06-27 | 2013-10-09 | 北京化工大学常州先进材料研究院 | Crosslinking polyether imide fibrous membrane capable of being used as lithium ion battery separator and preparation thereof |
| CN103343423B (en) * | 2013-06-27 | 2016-04-13 | 北京化工大学常州先进材料研究院 | A kind of crosslinked polyethers imide fiber film and preparation thereof that can be used as lithium electric separator |
| CN108532025A (en) * | 2018-05-05 | 2018-09-14 | 程桂平 | A method of preparing composite fibre |
| CN108754872A (en) * | 2018-05-29 | 2018-11-06 | 郑州豫力新材料科技有限公司 | The production method of Static Spinning PLGA superfine fibre films |
| CN108754872B (en) * | 2018-05-29 | 2021-09-10 | 郑州豫力新材料科技有限公司 | Production method of electrostatic spinning PLGA superfine fiber membrane |
| CN108807800A (en) * | 2018-08-08 | 2018-11-13 | 哈尔滨理工大学 | A kind of organo-mineral complexing lithium ion battery separator and preparation method thereof |
| CN110280229A (en) * | 2019-06-28 | 2019-09-27 | 东南大学 | Petrin class compound selective separation enrichment material preparation and application method |
| CN110280229B (en) * | 2019-06-28 | 2022-03-11 | 东南大学 | Preparation and application method of pterin compound selective separation enrichment material |
| CN111910265A (en) * | 2020-07-17 | 2020-11-10 | 湖南工程学院 | Electrostatic spinning injection device with liquid preparation function |
| CN115369517A (en) * | 2022-08-30 | 2022-11-22 | 烟台民士达特种纸业股份有限公司 | Preparation method and application of polyether-ether-ketone nanofiber membrane |
| CN115369517B (en) * | 2022-08-30 | 2023-09-01 | 烟台民士达特种纸业股份有限公司 | Preparation method and application of polyether-ether-ketone nanofiber membrane |
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Application publication date: 20121114 |