CN103498211A - Migratory phase separation method for preparing core-shell structure nanofibers - Google Patents

Migratory phase separation method for preparing core-shell structure nanofibers Download PDF

Info

Publication number
CN103498211A
CN103498211A CN201310489285.5A CN201310489285A CN103498211A CN 103498211 A CN103498211 A CN 103498211A CN 201310489285 A CN201310489285 A CN 201310489285A CN 103498211 A CN103498211 A CN 103498211A
Authority
CN
China
Prior art keywords
solution
electrostatic spinning
shell structure
room temperature
spinning
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.)
Pending
Application number
CN201310489285.5A
Other languages
Chinese (zh)
Inventor
马贵平
王美策
方大为
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changzhou Institute for Advanced Materials Beijing University of Chemical Technology
Original Assignee
Changzhou Institute for Advanced Materials Beijing University of Chemical Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Changzhou Institute for Advanced Materials Beijing University of Chemical Technology filed Critical Changzhou Institute for Advanced Materials Beijing University of Chemical Technology
Priority to CN201310489285.5A priority Critical patent/CN103498211A/en
Publication of CN103498211A publication Critical patent/CN103498211A/en
Pending legal-status Critical Current

Links

Images

Landscapes

  • Artificial Filaments (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The invention relates to a migratory phase separation method for preparing core-shell structure nanofibers. The method includes dissolving fluoropolymer and associative polymer in an organic solution, heating and stirring till being dissolved completely, and mixing the two solutions by a certain mass proportion to obtain an electrostatic spinning solution; utilizing the electrostatic spinning solution to spin electrostatically, collecting fibers on a receiver, processing the obtained fibers in a vacuum oven with the constant temperature of 30 DEG C for 24 hours, and obtained the core-shell structure nanofibers. The invention aims to provide a preparing method of the core-shell structure nanofibers, the low surface of fluorine can allow the fluoropolymer to migrate to the surface rapidly during electric spinning, the core-shell structure nanofibers with clear phases are prone to forming, the preparing process is simple and easy to operate, the requirements on equipment is low, energy consumption is low, and preparing cost is also low.

Description

Migration-type is separated and prepares the method for nuclear shell structure nano fiber
Technical field
The present invention relates to a kind of migration-type is separated and prepares the method for nuclear shell structure nano fiber.
Background technology
Nanofiber comprises the superfine fibre that fibre diameter is nanometer scale in broad terms, also comprises nano particle is filled into to the fiber that in general fibre, it is carried out modification.Larger specific area is the characteristics of nanofiber maximum, this makes it have larger surface energy and active, thereby produce small-size effect, surface or interfacial effect, quantum size effect, macro quanta tunnel effect etc., in chemistry, physics (heat, light, electromagnetism etc.) properties, show excellent specific property.The performance of nanofiber uniqueness makes it in fields such as membrane material, filter medium, catalyst, electronic product, optics, biological medicine and composite reinforcing materials, have huge market potential.
In order to adapt to the productive life instructions for use, widen the range of application of nanofiber, people study and have prepared the nanofiber with special construction, and the nuclear shell structure nano fiber is exactly one of them.The nuclear shell structure nano fiber is composite, the good performance in conjunction with two or more materials of energy, can form the performance that the one-component polymer fiber can not have concurrently thus, prepare the nanofiber with specific function, can, according to different choice difference stratum nucleares, the Shell Materials of its Application Areas, meet the needs of practical application.As aspect the dentistry casting resin, Shell Materials is generally with resin matrix has the polymer of being combined in good interface, and the stratum nucleare material makes material have excellent mechanical property for strengthening the polymer of resin matrix.
Prepare the nuclear shell structure nano fiber following several method is arranged usually: chemical cladding process, surface chemistry combined techniques, coaxial electrostatic spinning method and blend method of electrostatic spinning.It is a kind of simple physical method that chemistry applies, and can only be applied on the top layer of tunica fibrosa, can not evenly be coated on the interior every fiber of film; Surface chemistry, in conjunction with being functional materials to be grafted to a kind of method of modifying of fiber surface, can affect the mechanical performance of fiber in implementation process, and in film, the modification ratio of profound fiber is more difficult; The coaxial electrostatic spinning method is to utilize a kind of method of the directly continuous machining functions nanofiber of coaxial electrostatic spinning equipment, and this processing method is had relatively high expectations to equipment, complicated operation.The blend method of electrostatic spinning is the method that 2 kinds or two or more material are carried out to simple physical mixed spinning, simple to operate, but requires phase process rapid, and not so the line of demarcation of nucleocapsid structure can be fuzzy, and phase-splitting is not thorough.
Summary of the invention
Requirement for the blend method of electrostatic spinning to phase-splitting speed, the object of the present invention is to provide a kind of preparation method that can obtain clear nuclear shell structure nano fiber.In this preparation method's process, phase-splitting is rapid, step is simple to operation, and preparation cost is cheap.
The purpose of this invention is to provide a kind of animal migration and be separated and prepare the method for nuclear shell structure nano fiber, specifically comprise the steps:
(1) fluoropolymer is joined to the mixed liquor that organic solution forms, the heating stirring and dissolving, be cooled to room temperature, and obtaining percentage by weight is 6~30wt% fluoropolymer electrostatic spinning solution;
(2) composite polymer is joined to the mixed liquor that organic solution forms, the heating stirring and dissolving, be cooled to room temperature, and obtaining percentage by weight is the composite polymer electrospun solution of 5~40wt%;
(3) electrostatic spinning solution in step (1), (2) is mixed with the certain mass ratio, heating stirs, and is cooled to room temperature, in Ultrasound Instrument, after standing ultrasonic half an hour, obtains electrostatic spinning solution;
(4) electrostatic spinning prepares the nuclear shell structure nano fiber: the spinning solution of step (3) gained is carried out to electrostatic spinning, collect fiber on receiver, the fiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, obtained phase-splitting nuclear shell structure nano fiber clearly;
Compared with prior art, the inventive method has the following advantages:
1, the high polymer nanometer fiber that prepared by this inventive method has special nucleocapsid structure, and wherein stratum nucleare is composite polymer, and shell is hydrophobic fluoropolymer;
2, the fluoropolymer of this nuclear shell structure nano fiber shell makes it have the performance of many excellences such as stronger corrosion-resistant and swellability, antioxygen, ultra-violet radiation resisting;
3, in fluoropolymer, the low-surface-energy of fluorine element makes fluoropolymer have the performance to surperficial fast transferring in the Electrospun process, thereby forms the nuclear shell structure nano fiber;
4, this inventive method preparation process is simple to operation, low for equipment requirements, energy consumption is little, and preparation cost is cheap.
The accompanying drawing explanation
The scanning electron microscope (SEM) photograph of the PVDF/PVP nanofiber sample that Fig. 1 is embodiment 1 preparation.
The scanning electron microscope (SEM) photograph of the PVDF/PAN nanofiber sample that Fig. 2 is embodiment 2 preparations.
The transmission electron microscope picture of the PVDF/PVP nanofiber sample that Fig. 3 is embodiment 1 preparation.
The transmission electron microscope picture of the PVDF/PAN nanofiber sample that Fig. 4 is embodiment 2 preparations.
The contact angle that the PVDF/PVP nanofiber sample that Fig. 5 is embodiment 4 preparations and water record.
The specific embodiment
Embodiment 1:
(1), under 25 ℃ of conditions of room temperature, PVDF is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2; Be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 75 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVDF solution that to obtain percentage by weight be 18wt%;
(2) under 25 ℃ of conditions of room temperature, PVP is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2, be placed on magnetic stirring apparatus, the rotating speed with 120rpm under 50 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVP solution that to obtain percentage by weight be 12wt%;
(3) mixing of both electrostatic spinning solutions: the part by weight by the electrostatic spinning solution in step (1), (2) with 1:3 mixes, and is placed on magnetic stirring apparatus, and the rotating speed with 120rpm under 50 ℃ of conditions is uniformly mixed, until solution mixes; Be cooled to room temperature, by solution standing ultrasonic half an hour in Ultrasound Instrument, bubble all separated out, finally obtain electrostatic spinning solution;
(4) under 25 ℃ of room temperatures, humidity 50% condition, the flow velocity by spinning solution in step (3) with 0.5mL/h is input on spinning head, applies 10.5kV voltage simultaneously and carry out electrostatic spinning and prepare the nuclear shell structure nano fiber on spinning head; Spun fiber collecting is on aluminium film receiver, and the distance between receiver and spinning head is 15cm; After spinning process completes, the PVDF/PVP nanofiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, finally obtained phase-splitting nuclear shell structure nano fiber clearly;
Embodiment 2:
(1), under 25 ℃ of conditions of room temperature, PVDF is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2; Be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 75 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVDF solution that to obtain percentage by weight be 18wt%;
(2) under 25 ℃ of conditions of room temperature, PAN is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2, be placed on magnetic stirring apparatus, the rotating speed with 120rpm under 50 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PAN solution that to obtain percentage by weight be 7wt%;
(3) by the electrostatic spinning solution in step (1), (2), the part by weight with 1:3 mixes, and is placed on magnetic stirring apparatus, and the rotating speed with 120rpm under 50 ℃ of conditions is uniformly mixed, until solution mixes; Be cooled to room temperature, by solution standing ultrasonic half an hour in Ultrasound Instrument, bubble all separated out, finally obtain electrostatic spinning solution;
(4) under 25 ℃ of room temperatures, humidity 50% condition, the flow velocity by spinning solution in step (3) with 0.5mL/h is input on spinning head, applies 11kV voltage simultaneously and carry out electrostatic spinning and prepare the nuclear shell structure nano fiber on spinning head; Spun fiber collecting is on aluminium film receiver, and the distance between receiver and spinning head is 15cm; After spinning process completes, the PVDF/PAN nanofiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, finally obtained phase-splitting nuclear shell structure nano fiber clearly;
Embodiment 3:
(1), under 25 ℃ of conditions of room temperature, PVF is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2; Be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 75 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVF solution that to obtain percentage by weight be 20wt%;
(2) under 25 ℃ of conditions of room temperature, PVP is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2, be placed on magnetic stirring apparatus, the rotating speed with 120rpm under 50 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVP solution that to obtain percentage by weight be 12wt%;
(3) mixing of both electrostatic spinning solutions: the part by weight by the electrostatic spinning solution in step (1), (2) with 1:3 mixes, and is placed on magnetic stirring apparatus, and the rotating speed with 120rpm under 50 ℃ of conditions is uniformly mixed, until solution mixes; Be cooled to room temperature, by solution standing ultrasonic half an hour in Ultrasound Instrument, bubble all separated out, finally obtain electrostatic spinning solution;
(4) under 25 ℃ of room temperatures, humidity 40% condition, the flow velocity by spinning solution in step (3) with 0.5mL/h is input on spinning head, applies 11.5kV voltage simultaneously and carry out electrostatic spinning and prepare the nuclear shell structure nano fiber on spinning head; Spun fiber collecting is on aluminium film receiver, and the distance between receiver and spinning head is 15cm; After spinning process completes, the PVF/PVP nanofiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, finally obtained phase-splitting nuclear shell structure nano fiber clearly;
Embodiment 4:
(1), under 25 ℃ of conditions of room temperature, PVDF is dissolved in the mixed solvent that the DMF/THF mass ratio is 8:2; Be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 75 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVDF solution that to obtain percentage by weight be 18wt%;
(2) under 25 ℃ of conditions of room temperature, PVP is dissolved in the mixed solvent that the DMF/THF mass ratio is 8:2, is placed on magnetic stirring apparatus, the rotating speed with 120rpm under 50 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVP solution that to obtain percentage by weight be 10wt%;
(3) mixing of both electrostatic spinning solutions: the part by weight by the electrostatic spinning solution in step (1), (2) with 1:1 mixes, and is placed on magnetic stirring apparatus, and the rotating speed with 120rpm under 50 ℃ of conditions is uniformly mixed, until solution mixes; Be cooled to room temperature, by solution standing ultrasonic half an hour in Ultrasound Instrument, bubble all separated out, finally obtain electrostatic spinning solution;
(4) under 25 ℃ of room temperatures, humidity 40% condition, the flow velocity by spinning solution in step (3) with 0.5mL/h is input on spinning head, applies 12kV voltage simultaneously and carry out electrostatic spinning and prepare the nuclear shell structure nano fiber on spinning head; Spun fiber collecting is on aluminium film receiver, and the distance between receiver and spinning head is 15cm; After spinning process completes, the PVDF/PVP nanofiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, finally obtained phase-splitting nuclear shell structure nano fiber clearly;
Embodiment 5:
(1), under 25 ℃ of conditions of room temperature, PVDF is dissolved in to the NMP/ acetone quality than in the mixed solvent for 8:2; Be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 75 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVDF solution that to obtain percentage by weight be 18wt%;
(2) under 25 ℃ of conditions of room temperature, PVP is dissolved in to the NMP/ acetone quality than in the mixed solvent for 8:2, be placed on magnetic stirring apparatus, the rotating speed with 120rpm under 50 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVP solution that to obtain percentage by weight be 12wt%;
(3) mixing of both electrostatic spinning solutions: the part by weight by the electrostatic spinning solution in step (1), (2) with 1:3 mixes, and is placed on magnetic stirring apparatus, and the rotating speed with 120rpm under 50 ℃ of conditions is uniformly mixed, until solution mixes; Be cooled to room temperature, by solution standing ultrasonic half an hour in Ultrasound Instrument, bubble all separated out, finally obtain electrostatic spinning solution;
(4) under 25 ℃ of room temperatures, humidity 50% condition, the flow velocity by spinning solution in step (3) with 0.5mL/h is input on spinning head, applies 10.5kV voltage simultaneously and carry out electrostatic spinning and prepare the nuclear shell structure nano fiber on spinning head; Spun fiber collecting is on aluminium film receiver, and the distance between receiver and spinning head is 15cm; After spinning process completes, the PVDF/PVP nanofiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, finally obtained phase-splitting nuclear shell structure nano fiber clearly;
Embodiment 6:
(1), under 25 ℃ of conditions of room temperature, PVDF is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2; Be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 75 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVDF solution that to obtain percentage by weight be 18wt%;
(2) under 25 ℃ of conditions of room temperature, PMMA is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2, be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 50 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVP solution that to obtain percentage by weight be 20wt%;
(3) mixing of both electrostatic spinning solutions: the part by weight by the electrostatic spinning solution in step (1), (2) with 1:1 mixes, and is placed on magnetic stirring apparatus, and the rotating speed with 100rpm under 50 ℃ of conditions is uniformly mixed, until solution mixes; Be cooled to room temperature, by solution standing ultrasonic half an hour in Ultrasound Instrument, bubble all separated out, finally obtain electrostatic spinning solution;
(4) under 25 ℃ of room temperatures, humidity 50% condition, the flow velocity by spinning solution in step (3) with 0.5mL/h is input on spinning head, applies 12kV voltage simultaneously and carry out electrostatic spinning and prepare the nuclear shell structure nano fiber on spinning head; Spun fiber collecting is on aluminium film receiver, and the distance between receiver and spinning head is 15cm; After spinning process completes, the PVDF/PMMA nanofiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, finally obtained phase-splitting nuclear shell structure nano fiber clearly;
Embodiment 7:
(1), under 25 ℃ of conditions of room temperature, PVDF is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2; Be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 75 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVDF solution that to obtain percentage by weight be 25wt%;
(2) under 25 ℃ of conditions of room temperature, PVP is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2, be placed on magnetic stirring apparatus, the rotating speed with 120rpm under 50 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVP solution that to obtain percentage by weight be 12wt%;
(3) mixing of both electrostatic spinning solutions: the part by weight by the electrostatic spinning solution in step (1), (2) with 1:3 mixes, and is placed on magnetic stirring apparatus, and the rotating speed with 120rpm under 50 ℃ of conditions is uniformly mixed, until solution mixes; Be cooled to room temperature, by solution standing ultrasonic half an hour in Ultrasound Instrument, bubble all separated out, finally obtain electrostatic spinning solution;
(4) under 25 ℃ of room temperatures, humidity 50% condition, the flow velocity by spinning solution in step (3) with 1mL/h is input on spinning head, applies 10kV voltage simultaneously and carry out electrostatic spinning and prepare the nuclear shell structure nano fiber on spinning head; Spun fiber collecting is on aluminium film receiver, and the distance between receiver and spinning head is 15cm; After spinning process completes, the PVDF/PVP nanofiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, finally obtained phase-splitting nuclear shell structure nano fiber clearly;
Embodiment 8:
(1), under 25 ℃ of conditions of room temperature, PVDF is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2; Be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 75 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVDF solution that to obtain percentage by weight be 18wt%;
(2) under 25 ℃ of conditions of room temperature, PAN is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2, be placed on magnetic stirring apparatus, the rotating speed with 120rpm under 50 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PAN solution that to obtain percentage by weight be 10wt%;
(3) by the electrostatic spinning solution in step (1), (2), the part by weight with 1:2 mixes, and is placed on magnetic stirring apparatus, and the rotating speed with 120rpm under 50 ℃ of conditions is uniformly mixed, until solution mixes; Be cooled to room temperature, by solution standing ultrasonic half an hour in Ultrasound Instrument, bubble all separated out, finally obtain electrostatic spinning solution;
(4) under 25 ℃ of room temperatures, humidity 60% condition, the flow velocity by spinning solution in step (3) with 1mL/h is input on spinning head, applies 13kV voltage simultaneously and carry out electrostatic spinning and prepare the nuclear shell structure nano fiber on spinning head; Spun fiber collecting is on aluminium film receiver, and the distance between receiver and spinning head is 10cm; After spinning process completes, the PVDF/PAN nanofiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, finally obtained phase-splitting nuclear shell structure nano fiber clearly;
Embodiment 9:
(1), under 25 ℃ of conditions of room temperature, PVDF is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2; Be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 75 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVDF solution that to obtain percentage by weight be 20wt%;
(2) under 25 ℃ of conditions of room temperature, PVP is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2, be placed on magnetic stirring apparatus, the rotating speed with 120rpm under 50 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVP solution that to obtain percentage by weight be 10wt%;
(3) mixing of both electrostatic spinning solutions: the part by weight by the electrostatic spinning solution in step (1), (2) with 1:3 mixes, and is placed on magnetic stirring apparatus, and the rotating speed with 120rpm under 50 ℃ of conditions is uniformly mixed, until solution mixes; Be cooled to room temperature, by solution standing ultrasonic half an hour in Ultrasound Instrument, bubble all separated out, finally obtain electrostatic spinning solution;
(4) under 25 ℃ of room temperatures, humidity 50% condition, the flow velocity by spinning solution in step (3) with 0.5mL/h is input on spinning head, applies 13kV voltage simultaneously and carry out electrostatic spinning and prepare the nuclear shell structure nano fiber on spinning head; Spun fiber collecting is on aluminium film receiver, and the distance between receiver and spinning head is 15cm; After spinning process completes, the PVDF/PVP nanofiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, finally obtained phase-splitting nuclear shell structure nano fiber clearly;
Embodiment 10:
(1), under 25 ℃ of conditions of room temperature, PVF is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2; Be placed on magnetic stirring apparatus, the rotating speed with 100rpm under 75 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVF solution that to obtain percentage by weight be 20wt%;
(2) under 25 ℃ of conditions of room temperature, PVP is dissolved in to the DMF/ acetone quality than in the mixed solvent for 8:2, be placed on magnetic stirring apparatus, the rotating speed with 120rpm under 50 ℃ of conditions carries out stirring and dissolving, until obtain clear solution; Be cooled to room temperature, the PVP solution that to obtain percentage by weight be 15wt%;
(3) mixing of both electrostatic spinning solutions: the part by weight by the electrostatic spinning solution in step (1), (2) with 1:2 mixes, and is placed on magnetic stirring apparatus, and the rotating speed with 120rpm under 50 ℃ of conditions is uniformly mixed, until solution mixes; Be cooled to room temperature, by solution standing ultrasonic half an hour in Ultrasound Instrument, bubble all separated out, finally obtain electrostatic spinning solution;
(4) under 25 ℃ of room temperatures, humidity 70% condition, the flow velocity by spinning solution in step (3) with 0.5mL/h is input on spinning head, applies 14kV voltage simultaneously and carry out electrostatic spinning and prepare the nuclear shell structure nano fiber on spinning head; Spun fiber collecting is on aluminium film receiver, and the distance between receiver and spinning head is 15cm; After spinning process completes, the PVF/PVP nanofiber that obtains 30 ℃ of vacuum constant temperatures in vacuum drying oven are processed 24 hours, finally obtained phase-splitting nuclear shell structure nano fiber clearly.

Claims (5)

1. a migration-type is separated and prepares the method for nuclear shell structure nano fiber, it is characterized in that, comprises the following steps:
(1) fluoropolymer is joined to the mixed liquor that organic solution forms, the heating stirring and dissolving, be cooled to room temperature, and obtaining percentage by weight is 6~30wt% fluoropolymer electrostatic spinning solution;
(2) composite polymer is joined to the mixed liquor that organic solution forms, the heating stirring and dissolving, be cooled to room temperature, and obtaining percentage by weight is the composite polymer electrospun solution of 5~40wt%;
(3) electrostatic spinning solution in step (1), (2) is mixed with the certain mass ratio, heating stirs, and is cooled to room temperature, in Ultrasound Instrument, after standing ultrasonic half an hour, obtains electrostatic spinning solution;
(4) spinning solution of step (3) gained is carried out to electrostatic spinning, the electrostatic spinning condition is: spinning voltage is 10~15kV, temperature is 10~35 ℃, relative humidity is 30%~70%, spinning distance is 8~20cm, the flow velocity of spinning head spinning solution is 0.2~1.0mL/h, and 30 ℃ of the vacuum constant temperatures in vacuum drying oven of the fiber on receiver are processed 24 hours, obtains phase-splitting nuclear shell structure nano fiber clearly.
2. according to the preparation method of claim 1, it is characterized in that fluoropolymer described in step (1) is one or more mixture in polyvinyl fluoride (PVF), Kynoar (PVDF), vinylidene-TFE copolymer (VDF-TFE), vinylidene fluoride-hexafluoropropylene copolymer (VDF-HFP) and ethylene-tetrafluoroethylene copolymer (E-TFE).
3. according to the preparation method of claim 1, it is characterized in that the organic solvent described in step (1), (2) is one or more the mixture in DMF (DMF), oxolane (THF), 1-METHYLPYRROLIDONE (NMP), dimethyl sulfoxide (DMSO) (DMSO), acetone, hexafluoroisopropanol, tetramethylurea and methyl ethyl ketone.
4. according to the preparation method of claim 1, it is characterized in that the composite polymer described in step (2) is polyacrylonitrile (PAN), polyvinylpyrrolidine (PVP), poly(ethylene oxide) (PEO), polymethyl methacrylate (PMMA), Merlon (PC), polyvinyl alcohol (PVA), cellulose acetate (CA), polyacrylamide (PAM), PLA (PLA) or polyvinyl chloride (PVC).
5. according to the preparation method of claim 1, it is characterized in that the mixed proportion between the middle fluoropolymer electrostatic spinning solution of step (3) and two kinds of solution of composite polymer electrospun solution is 0.1~10.
CN201310489285.5A 2013-10-17 2013-10-17 Migratory phase separation method for preparing core-shell structure nanofibers Pending CN103498211A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310489285.5A CN103498211A (en) 2013-10-17 2013-10-17 Migratory phase separation method for preparing core-shell structure nanofibers

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310489285.5A CN103498211A (en) 2013-10-17 2013-10-17 Migratory phase separation method for preparing core-shell structure nanofibers

Publications (1)

Publication Number Publication Date
CN103498211A true CN103498211A (en) 2014-01-08

Family

ID=49863462

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310489285.5A Pending CN103498211A (en) 2013-10-17 2013-10-17 Migratory phase separation method for preparing core-shell structure nanofibers

Country Status (1)

Country Link
CN (1) CN103498211A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104264248A (en) * 2014-09-16 2015-01-07 北京化工大学 Preparation method for controllable core-shell structure nanofiber
CN105924585A (en) * 2016-04-29 2016-09-07 永保化工(香港)有限公司 Core-shell type fluorine-containing nanometer emulsion, and preparation method and application thereof
WO2017088818A1 (en) * 2015-11-27 2017-06-01 广州迈普再生医学科技有限公司 Tissue repair fiber membrane, preparation method and application thereof, and tissue repair product
CN107447496A (en) * 2017-07-31 2017-12-08 安徽工程大学 A kind of super hydrophilic nucleocapsid Kynoar hexafluoropropene/cupric oxide nano piece film, preparation method and applications
CN112899817A (en) * 2021-01-27 2021-06-04 泉州师范学院(石狮)生态智能织物工程技术研究院 Self-assembly core-sheath temperature-sensitive fiber based on electrostatic spinning and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005105483A (en) * 2003-09-30 2005-04-21 Kureha Chem Ind Co Ltd Vinylidene fluoride resin monofilament and method for producing the same
CN101586268A (en) * 2009-06-25 2009-11-25 天津大学 Kynoar/the polycarbonate superfine fiber of core-shell structure and preparation method
CN102140706A (en) * 2011-04-28 2011-08-03 天津工业大学 Perfluoro polymer fiber and preparation method thereof
CN102817105A (en) * 2012-08-24 2012-12-12 上海交通大学 Preparation method of core-shell structured synthetic polymer-natural polymer composite fiber
CN102861355A (en) * 2012-10-12 2013-01-09 中国人民解放军第三军医大学 Functional wound dressing capable of accelerating wound healing and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005105483A (en) * 2003-09-30 2005-04-21 Kureha Chem Ind Co Ltd Vinylidene fluoride resin monofilament and method for producing the same
CN101586268A (en) * 2009-06-25 2009-11-25 天津大学 Kynoar/the polycarbonate superfine fiber of core-shell structure and preparation method
CN102140706A (en) * 2011-04-28 2011-08-03 天津工业大学 Perfluoro polymer fiber and preparation method thereof
CN102817105A (en) * 2012-08-24 2012-12-12 上海交通大学 Preparation method of core-shell structured synthetic polymer-natural polymer composite fiber
CN102861355A (en) * 2012-10-12 2013-01-09 中国人民解放军第三军医大学 Functional wound dressing capable of accelerating wound healing and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王美策等: "电纺丝法制备含氟聚合物核壳结构纳米纤维膜", 《2013年中国化工学会年会论文集》, 23 September 2013 (2013-09-23) *
王美策等: "电纺丝法制备含氟聚合物核壳结构纳米纤维膜", 《2013年全国高分子学术论文报告会论文摘要集—主题H:医用高分子》, 12 October 2013 (2013-10-12) *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104264248A (en) * 2014-09-16 2015-01-07 北京化工大学 Preparation method for controllable core-shell structure nanofiber
WO2017088818A1 (en) * 2015-11-27 2017-06-01 广州迈普再生医学科技有限公司 Tissue repair fiber membrane, preparation method and application thereof, and tissue repair product
CN105924585A (en) * 2016-04-29 2016-09-07 永保化工(香港)有限公司 Core-shell type fluorine-containing nanometer emulsion, and preparation method and application thereof
CN105924585B (en) * 2016-04-29 2018-11-23 永保化工(香港)有限公司 A kind of fluorine-containing nanoemulsions of core-shell type and its preparation method and application
CN107447496A (en) * 2017-07-31 2017-12-08 安徽工程大学 A kind of super hydrophilic nucleocapsid Kynoar hexafluoropropene/cupric oxide nano piece film, preparation method and applications
CN112899817A (en) * 2021-01-27 2021-06-04 泉州师范学院(石狮)生态智能织物工程技术研究院 Self-assembly core-sheath temperature-sensitive fiber based on electrostatic spinning and preparation method thereof

Similar Documents

Publication Publication Date Title
CN103498211A (en) Migratory phase separation method for preparing core-shell structure nanofibers
CN102242464B (en) Polymer-ceramic compound nanometer fibrous membrane as well as preparation method and application thereof
CN106149199B (en) A kind of preparation method of automatically cleaning membrane material, its product and purposes
CN104562292B (en) Preparation method of porous micro-nano PET fibers
CN106835304B (en) A kind of electrostatic spinning-electrical painting device and its application
CN108589048A (en) Orientation capillary power drive is prepared using electrostatic spinning large area efficiently to catchment the methods of hydrophobic/hydrophilic Janus composite cellulosic membranes
CN102561037B (en) Benzoxazine-modified super-hydrophobic nano fiber membrane and preparation method thereof
CN102733000B (en) Preparation method for hollow polymer nanofibers
CN107119346B (en) A kind of preparation method of carbon nano tube/graphene composite fibre
CN104746149B (en) The method that electrostatic spinning combination double solvents technology prepares porous nano-fibre
CN106222767A (en) A kind of coaxial eccentricity device for spinning and method
CN107195894A (en) A kind of metal carbon nano-fiber composite material and its preparation method and application
CN102268745B (en) Method for preparing porous polyacrylonitrile (PAN) nano fibres by electrospinning method
CN108187503A (en) A kind of preparation method of the enhanced chitosan multiple cellulose acetate film of montmorillonite
CN103757742B (en) A kind of preparation method of nuclear shell structure nano fiber of fluorine-contained surface
CN110387588A (en) A method of preparing the micro nanometer fiber film of core-shell structure using Janus syringe needle electrostatic spinning arranged side by side
CN106978671A (en) One kind prepares transparent VO using electrostatic spinning technique2The method of thermocolour smart membranes
CN105086454A (en) High-temperature resistance polyether sulfone nano-porous microspheres and preparation method thereof
CN109023706A (en) A kind of poly(N-isopropylacrylamide)/graphene composite material preparation method with photothermal response
CN103993382A (en) Method for improving pre-oxidation speed of polyacrylonitrile fiber through physical blending
CN109166960A (en) A kind of preparation method of fiber base flexible piezoelectric sensors
CN105261722B (en) It is orientated modified fibre homogeneity enhancing fluorine resin base barrier film
CN105803679A (en) Preparation method of pH response type multi-scale structure polyvinylidene fluoride nanofiber membrane
CN113235227B (en) Preparation method and application of composite film
CN104098084A (en) Preparation method of carbon nano tube paper with controllable shape and controllable size

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C02 Deemed withdrawal of patent application after publication (patent law 2001)
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20140108