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CN108998841A - A kind of preparation method of porous polypropylene nitrile nanofibre - Google Patents

A kind of preparation method of porous polypropylene nitrile nanofibre Download PDF

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Publication number
CN108998841A
CN108998841A CN201710424085.XA CN201710424085A CN108998841A CN 108998841 A CN108998841 A CN 108998841A CN 201710424085 A CN201710424085 A CN 201710424085A CN 108998841 A CN108998841 A CN 108998841A
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China
Prior art keywords
polyacrylonitrile
preparation
electrostatic spinning
porous polypropylene
polypropylene nitrile
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Pending
Application number
CN201710424085.XA
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Chinese (zh)
Inventor
冯章启
袁旭
史传梅
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Nanjing University of Science and Technology
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Nanjing University of Science and Technology
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Priority to CN201710424085.XA priority Critical patent/CN108998841A/en
Publication of CN108998841A publication Critical patent/CN108998841A/en
Pending legal-status Critical Current

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Classifications

    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4282—Addition polymers
    • D04H1/43—Acrylonitrile series
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/55—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Nonwoven Fabrics (AREA)
  • Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)

Abstract

The invention discloses a kind of preparation methods of porous polypropylene nitrile nanofibre film.The method ultrasonic disperse first prepares nanometer α-Fe2O3N,N-Dimethylformamide dispersion liquid, then polyacrylonitrile is added in dispersion liquid, is uniformly mixed obtained polyacrylonitrile/α-Fe2O3Nano fibrous membrane is finally immersed in dilution heat of sulfuric acid and sufficiently reacts by electrostatic spinning preparation doped with the polyacrylonitrile nanofiber film of iron oxide by electrostatic spinning liquid, removes α-Fe2O3Up to porous polypropylene nitrile nanofibre film.The specific surface area and porosity of polyacrylonitrile nanofiber can be dramatically increased in the present invention, simultaneously because there is the cyano that is easily modified in polyacrylonitrile structure, when fibre modification can greatly improve the conversion ratio of cyano in fiber, can be used as heavy-metal adsorption material.

Description

A kind of preparation method of porous polypropylene nitrile nanofibre
Technical field
The invention belongs to electrostatic spinning technique fields, are related to a kind of preparation method of porous polypropylene nitrile nanofibre film.
Background technique
Electrostatic spinning technique is evaporated or molten by rheology occurring under high voltage electrostatic field to form jet stream through solvent Body cooling and solidifying, obtains nanofiber.The nano fibrous membrane of electrostatic spinning preparation has high-ratio surface compared with traditional fiber The characteristics of product, high porosity.
Currently, mainly Electrospun nano-fibers are selectively removed by fast evaporating solvents or from blend polymer One component prepares porous fibre based on mutually separation.However, the above method usually requires to handle as-spun fibre, or Need time-consuming dissolution polymer.McCann etc. changes the reception medium of electrostatic spinning, receiver board is immersed in liquid nitrogen, fiber Occur Thermal inactive during electrostatic spinning, form solvent-rich phase and polymer-rich phase, be removed in vacuum solvent obtain it is more Hole superfine fibre (McCann J T, et al.J Am Chem Soc, 2006,128 (5): 1436~1437).Yu etc. is using poly- Acrylonitrile/N, N'- dimethylformamide/water ternary system are spinning solution, pass through non-solvent induction poly- third during electrostatic spinning The generation of alkene nitrile solution mutually separates, and has obtained the porous superfine fibre of polyacrylonitrile.Above two method wants control of temperature and humidity Ask very stringent, and spinning solution Miscibility it is poor (Yu X L, et al.Mater Lett, 2010,64 (22): 2407~ 2409)。
Summary of the invention
It is harsh for existing porous polypropylene nitrile nanofibre preparation process conditional, spinning solution Miscibility difference Problem, the present invention provides a kind of preparation methods of porous polypropylene nitrile nanofibre.
Technical scheme is as follows:
A kind of preparation method of porous polypropylene nitrile nanofibre, is obtained by electrostatic spinning doped with ferric oxide nano Ferric oxide nanometer particle, is then dissolved in dilute sulfuric acid to obtain porous polypropylene nitrile nanometer by the polyacrylonitrile nanofiber of grain Fiber, the specific steps are as follows:
Step 1, nanometer α-Fe2O3The preparation of dispersion liquid:
By nanometer α-Fe2O3It is added in n,N-Dimethylformamide, is obtained after 60~90min of ultrasonic treatment at room temperature dense Degree is the uniform α-Fe of 0.03~0.05g/mL2O3Nanoparticulate dispersion；
Step 2, the preparation of electrostatic spinning liquid:
Polyacrylonitrile is added to α-Fe2O3It in nanoparticulate dispersion, is stirred at room temperature uniformly mixed, obtains poly- third Alkene nitrile/α-Fe2O3Electrostatic spinning liquid；
Step 3, the preparation of porous polypropylene nitrile nanofibre film:
By polyacrylonitrile/α-Fe2O3Electrostatic spinning liquid carries out electrostatic spinning, using the metal needle of internal diameter 0.5mm, 1~3mL/ The fltting speed of h, the spinning voltage of 14~16kV, the reception distance of 10~15cm prepare the polyacrylonitrile doped with iron oxide Polyacrylonitrile nanofiber film doped with iron oxide is immersed in the dilution heat of sulfuric acid of 0.05~0.1mol/L by nano fibrous membrane In, it sufficiently reacts, is washed to neutrality, is drying to obtain porous polypropylene nitrile nanofibre film.
Preferably, in step 2, the quality volume fraction that the polyacrylonitrile accounts for electrostatic spinning liquid is 10~15%.
Preferably, in step 3, drying temperature is 40~60 DEG C.
Compared with prior art, the invention has the advantages that
(1) specific surface area, porosity of polyacrylonitrile nanofiber produced by the present invention significantly improve；
(2) the method for the present invention is to the of less demanding of control of temperature and humidity, nanofiber even thickness obtained；
Detailed description of the invention
Fig. 1 is the scanning of porous polypropylene nitrile nanofibre (A) and the polyacrylonitrile nanofiber film (B) without iron oxide Electron microscope.
Fig. 2 is the flow diagram of the preparation method of porous polypropylene nitrile nanofibre of the invention.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
Embodiment 1
(1) by the α-Fe of 0.09mg2O3Nanometer powder is added in 3mL n,N dimethylformamide, ultrasonic 80min, is made Concentration is the α-Fe of 0.03g/mL2O3Uniform dispersion.
(2) polyacrylonitrile for weighing 0.45g is added to α-Fe2O3In dispersion liquid, at 25 DEG C, it is in uniform for stirring to solution, It is centrifuged 1min under 1000r/min, removes the bubble in electrostatic spinning liquid, obtains polyacrylonitrile/α-Fe2O3Electrostatic spinning liquid.
(3) be arranged electrospinning parameters: metal internal diameter be 0.5mm, the fltting speed of 1.4mL/h, spinning voltage 15kV, receive away from From 12cm, the polyacrylonitrile nanofiber film doped with iron oxide will be obtained in nanofiber electrospinning to aluminium-foil paper.
(4) dilution heat of sulfuric acid for configuring 0.05mol/L, will be immersed in doped with the polyacrylonitrile nanofiber film of iron oxide It is sufficiently reacted in dilution heat of sulfuric acid.Nanofiber after reaction deionization is rinsed several times, until washing lotion at neutrality, finally exists Porous polypropylene nitrile nanofibre film obtained by drying in 40 DEG C of drying boxes.
Embodiment 2
(1) by the α-Fe of 0.12mg2O3Nanometer powder is added in the n,N dimethylformamide of 3mL, ultrasonic 80min, system Obtain the α-Fe that concentration is 0.04g/mL2O3Uniform dispersion.
(2) polyacrylonitrile for weighing 0.45g is added to α-Fe2O3In nanoparticulate dispersion, at 25 DEG C, stir to molten Liquid is centrifuged 1min in uniform under 1000r/min, remove the bubble in electrostatic spinning liquid, obtain polyacrylonitrile/α-Fe2O3Static Spinning Silk liquid.
(3) be arranged electrospinning parameters: metal internal diameter be 0.5mm, the fltting speed of 1.4mL/h, spinning voltage 15kV, receive away from From 12cm, the polyacrylonitrile nanofiber film doped with iron oxide will be obtained in nanofiber electrospinning to aluminium-foil paper.
(4) dilution heat of sulfuric acid for configuring 0.1mol/L, will be immersed in doped with the polyacrylonitrile nanofiber film of iron oxide It is sufficiently reacted in dilution heat of sulfuric acid.Nanofiber after reaction deionization is rinsed several times, until washing lotion at neutrality, finally exists Porous polypropylene nitrile nanofibre film obtained by drying in 40 DEG C of drying boxes.
The flow diagram of the preparation method of porous polypropylene nitrile nanofibre of the invention is as shown in Figure 2.It is obtained more The SEM figure of hole polyacrylonitrile nanofiber film is as shown in Fig. 1 (A).From Fig. 1 (A) as can be seen that after acid dissolution, polypropylene Specific surface area, the porosity of polyacrylonitrile nanofiber is dramatically increased in nitrile nanofibre surface irregularity.
Embodiment 3
(1) by the α-Fe of 0.15mg2O3Nanometer powder is added in the n,N dimethylformamide of 3mL, ultrasonic 80min, system Obtain the α-Fe that concentration is 0.05g/mL2O3Uniform dispersion.
(2) polyacrylonitrile for weighing 0.45g is added to α-Fe2O3In nanoparticulate dispersion, at 25 DEG C, stir to molten Liquid is centrifuged 1min in uniform under 1000r/min, remove the bubble in electrostatic spinning liquid, obtain polyacrylonitrile/α-Fe2O3Static Spinning Silk liquid.
(3) electrospinning parameters are arranged: metal internal diameter is 0.51mm, the fltting speed of 1.4mL/h, spinning voltage 15kV, reception Distance 12cm will obtain the polyacrylonitrile nanofiber film doped with iron oxide in nanofiber electrospinning to aluminium-foil paper.
(4) dilution heat of sulfuric acid for configuring 0.1mol/L, will be immersed in doped with the polyacrylonitrile nanofiber film of iron oxide It is sufficiently reacted in dilution heat of sulfuric acid.Nanofiber after reaction deionization is rinsed several times, until washing lotion at neutrality, finally exists Porous polypropylene nitrile nanofibre film obtained by drying in 40~60 DEG C of drying boxes.
Comparative example 1
This comparative example is substantially the same manner as Example 1, unique the difference is that α-Fe2O3The concentration of dispersion liquid is 0g/mL, is obtained Polyacrylonitrile nanofiber film, shown in scanning electron microscope such as Fig. 1 (B).From Fig. 1 (B) it can be seen that fiber surface is smooth, slightly Carefully uniformly occur without any beading phenomenon.
Comparative example 2
This comparative example is substantially the same manner as Example 1, unique the difference is that α-Fe2O3The concentration of dispersion liquid is 0.06g/mL.It should Under concentration polyacrylonitrile nanofiber can not be prepared by electrostatic spinning.
By embodiment and comparative example it is found that α-Fe2O3The concentration of dispersion liquid influences porous polypropylene nitrile nanofibre film Preparation, only α-Fe2O3The concentration of dispersion liquid is just able to achieve porous polypropylene nitrile nanofibre film in 0.03~0.05g/mL Electrostatic spinning.

Claims (3)

1. a kind of preparation method of porous polypropylene nitrile nanofibre, which is characterized in that specific step is as follows:
Step 1, nanometer α-Fe2O3The preparation of dispersion liquid:
By nanometer α-Fe2O3It is added in n,N-Dimethylformamide, obtaining concentration after 60~90min of ultrasonic treatment at room temperature is Uniform α-the Fe of 0.03~0.05g/mL2O3Nanoparticulate dispersion；
Step 2, the preparation of electrostatic spinning liquid:
Polyacrylonitrile is added to α-Fe2O3In nanoparticulate dispersion, be stirred at room temperature it is uniformly mixed, obtain polyacrylonitrile/ α-Fe2O3Electrostatic spinning liquid；
Step 3, the preparation of porous polypropylene nitrile nanofibre film:
By polyacrylonitrile/α-Fe2O3Electrostatic spinning liquid carries out electrostatic spinning, using the metal needle of internal diameter 0.5mm, 1~3mL/h's Fltting speed, the spinning voltage of 14~16kV, the reception distance of 10~15cm prepare the polyacrylonitrile nano doped with iron oxide Tunica fibrosa will be immersed in the dilution heat of sulfuric acid of 0.05~0.1mol/L doped with the polyacrylonitrile nanofiber film of iron oxide, Sufficiently reaction, is washed to neutrality, is drying to obtain porous polypropylene nitrile nanofibre film.
2. preparation method according to claim 1, which is characterized in that in step 2, the polyacrylonitrile accounts for electrostatic spinning The quality volume fraction of liquid is 10~15%.
3. preparation method according to claim 1, which is characterized in that in step 3, drying temperature is 40~60 DEG C.
CN201710424085.XA 2017-06-07 2017-06-07 A kind of preparation method of porous polypropylene nitrile nanofibre Pending CN108998841A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111501110A (en) * 2020-04-16 2020-08-07 西北工业大学 Preparation method of large-aperture electrostatic spinning nanofiber material
CN112226912A (en) * 2020-09-28 2021-01-15 北京碳阳科技有限公司 Porous polyacrylonitrile nanofiber membrane and preparation method thereof
CN113151981A (en) * 2021-04-09 2021-07-23 南通大学 Arsenic removal membrane for drinking water and preparation method thereof
CN113559929A (en) * 2021-08-16 2021-10-29 南昌航空大学 Cobaltosic oxide supported membrane catalyst and preparation method and application thereof

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US20110250256A1 (en) * 2007-08-10 2011-10-13 Genic Co, Ltd. Dissolvable Nano Web Porous Film and Method of Preparing the Same
CN103011778A (en) * 2012-12-14 2013-04-03 山东大学 Porous alumina nano fiber and preparation method thereof
CN103225115A (en) * 2013-04-26 2013-07-31 苏州大学 Method for preparing nano porous material by utilizing electrostatic spinning technique
KR20140012517A (en) * 2012-07-20 2014-02-03 한국과학기술원 Metal oxide nanofiber with nanopore, fabrication method for preparing the same and apparatus comprising the same
CN103590132A (en) * 2013-11-25 2014-02-19 扬州大学 Preparation method for electrostatic spinning nano-fiber adopting porous structure
CN106757538A (en) * 2016-11-14 2017-05-31 天津工业大学 A kind of electrical spinning method prepares porous carbon fiber preparation method
CN107354516A (en) * 2017-06-19 2017-11-17 西安科技大学 The method that porous silica Electrostatic spinning of fibres liquid and method of electrostatic spinning prepare porous silica silica fibre
CN107611434A (en) * 2017-09-08 2018-01-19 浙江大学 A kind of preparation method and applications of flexible self-supporting porous carbon nanofiber electrode

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040098023A1 (en) * 2002-11-15 2004-05-20 Scimed Life Systems, Inc. Embolic device made of nanofibers
US20110250256A1 (en) * 2007-08-10 2011-10-13 Genic Co, Ltd. Dissolvable Nano Web Porous Film and Method of Preparing the Same
KR20140012517A (en) * 2012-07-20 2014-02-03 한국과학기술원 Metal oxide nanofiber with nanopore, fabrication method for preparing the same and apparatus comprising the same
CN103011778A (en) * 2012-12-14 2013-04-03 山东大学 Porous alumina nano fiber and preparation method thereof
CN103225115A (en) * 2013-04-26 2013-07-31 苏州大学 Method for preparing nano porous material by utilizing electrostatic spinning technique
CN103590132A (en) * 2013-11-25 2014-02-19 扬州大学 Preparation method for electrostatic spinning nano-fiber adopting porous structure
CN106757538A (en) * 2016-11-14 2017-05-31 天津工业大学 A kind of electrical spinning method prepares porous carbon fiber preparation method
CN107354516A (en) * 2017-06-19 2017-11-17 西安科技大学 The method that porous silica Electrostatic spinning of fibres liquid and method of electrostatic spinning prepare porous silica silica fibre
CN107611434A (en) * 2017-09-08 2018-01-19 浙江大学 A kind of preparation method and applications of flexible self-supporting porous carbon nanofiber electrode

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111501110A (en) * 2020-04-16 2020-08-07 西北工业大学 Preparation method of large-aperture electrostatic spinning nanofiber material
CN112226912A (en) * 2020-09-28 2021-01-15 北京碳阳科技有限公司 Porous polyacrylonitrile nanofiber membrane and preparation method thereof
CN113151981A (en) * 2021-04-09 2021-07-23 南通大学 Arsenic removal membrane for drinking water and preparation method thereof
CN113151981B (en) * 2021-04-09 2022-04-01 南通大学 Arsenic removal membrane for drinking water and preparation method thereof
CN113559929A (en) * 2021-08-16 2021-10-29 南昌航空大学 Cobaltosic oxide supported membrane catalyst and preparation method and application thereof

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