CN106400205A - Preparation method of hollow magnetic iron oxide nanofiber - Google Patents
Preparation method of hollow magnetic iron oxide nanofiber Download PDFInfo
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- CN106400205A CN106400205A CN201611029130.3A CN201611029130A CN106400205A CN 106400205 A CN106400205 A CN 106400205A CN 201611029130 A CN201611029130 A CN 201611029130A CN 106400205 A CN106400205 A CN 106400205A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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Abstract
The invention relates to a preparation method of hollow magnetic iron oxide nanofiber. The preparation method comprises the following steps: heating and dissolving polyvinyl alcohol (PVA) in an aqueous solution of acetic acid, wherein the concentration of PVA is 1-20wt%, and the concentration of acetic acid is 1-50wt%; performing electrostatic spinning to obtain a PVA nanofiber membrane, wherein the spinning voltage is 10-20kv, and the curing distance is 5-20cm; performing heat treatment of the PVA nanofiber membrane, wherein the temperature is 150-250 DEG C, and the time is 1-30min; dissolving trivalent iron salt and bivalent iron salt in water to obtain a mixed solution, wherein the concentration of the trivalent iron salt is 1.5-8wt%, and the concentration of the bivalent iron salt is 0.5-3wt%; putting the PVA nanofiber membrane after the heat treatment into the mixed solution of iron salt, and performing hydrothermal synthesis in N2 atmosphere at the temperature of 50-90 DEG C; dropwise adding an alkaline solution with concentration of 1-10wt% to obtain a PVA nanofiber membrane coated with Fe3O4 nanoparticles; and finally, performing high-temperature calcination at the temperature of 500-900 DEG C to obtain AZO hollow nanofiber. According to the preparation method, the prepared magnetic nanofiber with a hollow structure has the advantages of low cost and uniform morphology.
Description
Technical field
The present invention relates to a kind of preparation method of hollow magnetic ferric oxide nano fiber, belong to chemical technology field.
Background technology
Magnetic Nano material is a kind of nano material with unique physico-chemical property, because it can be used as excellent height
Density magnetic recording material, electromagnetic wave absorbent material, biology and medical science functional material, so the research of magnetic Nano material has been drawn
Play the highest attention of scholars.Especially magnetic Nano fiber and nanometer filamentary material have high draw ratio, big ratio
The series of advantages such as surface area and enjoy the favor of researcher to be considered as constitute the functional materials such as following Novel electric, magnetic important
Assembly.The method preparing nanofiber at present has many kinds, such as:AAO template, hydro-thermal method, phase separation method etc., although these sides
Method has been able to prepare pattern and the good magnetic Nano fiber of magnetic, but they have complex operation, the lacking of high cost
Point.Electrostatic spinning becomes and prepares a kind of topmost method of magnetic Nano fiber in recent years, and this method can be prepared continuously
Uniformly, diameter is adjustable, possess the magnetic Nano fiber of multilevel hierarchy.
By electrostatic spinning technique, people have prepared CoFe2O4, NiFe2O4, (Ni, Zn) Fe2O4Etc. multiple magnetic Nanos
Fiber.Through retrieval, Chinese invention patent：CN102251305B, is related to a kind of cobalt nickel ferrite/Polyvinylpyrrolidone and is combined magnetic
The preparation method of property nanofiber, by modified Co1-xNixFe2O4Nano-particle is added in PVP ethanol solution, as spinning
Stock solution carries out electrostatic spinning, obtains final product cobalt nickel ferrite/Polyvinylpyrrolidone composite magnetic nanofiber.But magnetic nano particle
Son is easily reunited, and can reduce the viscosity of spinning liquid, leads to the discontinuous of spinning process, and the inhomogeneity of nanofiber diameter increases
Greatly.Hollow magnetic nanofiber has hollow structure, has bigger specific surface area, has at aspects such as wastewater treatments and potentially should
With.The present invention prepares α-Fe by the method that electrostatic spinning, Hydrothermal Synthesiss and high-temperature calcination combine2O3Hollow magnetic nanometer
Fiber, process is simple, and equipment requirements are low to producing, prepared magnetic fibre diameter Distribution uniformly, and has good magnetic
Energy.
Content of the invention
The purpose of the present invention be overcome existing prepare present in magnetic Nano fibre technology not enough, a kind of hollow magnetic is provided
Property ferric oxide nano fiber preparation method, the hollow magnetic ferric oxide nano pulp freeness obtaining is big, have hollow knot
Structure, with low cost, pattern are uniform.
The technical scheme providing according to the present invention, a kind of preparation method of hollow magnetic ferric oxide nano fiber, feature is,
Comprise the following steps：
(1) polyvinyl alcohol (PVA) is dissolved in the distilled water that with the addition of acetic acid, obtains mixed solution A；Mixed solution A
The concentration of middle PVA is 1-20wt%, and the concentration of acetic acid is 1-50wt%；
(2) A is carried out electrostatic spinning, regulation spinning voltage is 10-20kv, the distance of adjusting shower nozzle to cylinder is 5-
20cm, obtains PVA nano fibrous membrane；
(3) PVA nano fibrous membrane is put into baking oven and carry out heat treatment, adjust temperature and be 150-250 DEG C, heat treatment time is
1-30min, obtains the PVA nano fibrous membrane after heat treatment；
(4) trivalent iron salt and divalent iron salt are dissolved in distilled water and obtain mixed solution B, wherein the concentration of trivalent iron salt
For 1.5-8wt%, the concentration of divalent iron salt is 0.5-3wt%；PVA nano fibrous membrane after heat treatment is put in mixed solution B,
Using N2Protection, carries out hydrothermal synthesis reaction, sets 50-90 DEG C of bath temperature, and instillation concentration is 1-10wt%'s thereto
Aqueous slkali, obtains the PVA nano fibrous membrane having coated ferriferrous oxide nano-particle；
(5) the PVA nano fibrous membrane having coated ferroso-ferric oxide is put into calcining a period of time, calcining heat in tube furnace
For 500-900 DEG C, obtain described hollow magnetic ferric oxide nano fiber.
In step (1), the alcoholysis degree 96-100% of described PVA, degree of polymerization 1700-10000.
In step (4), described trivalent iron salt is iron chloride, iron sulfate and ferric nitrate.Described divalent iron salt is chlorine
Change ferrous iron, ferrous sulfate and ferrous nitrate.
In step (4), described aqueous slkali is sodium carbonate liquor, sodium bicarbonate solution, sodium hydroxide solution and potassium hydroxide
Solution.
In step (5), described calcination time is 30～120 minutes.Calcination atmosphere is air.
The hollow magnetic ferric oxide nano fiber of present invention preparation has the structure of hollow because of it, and specific surface area is larger, tool
Have the advantages that good magnetic, with low cost, form are excellent.
Brief description
Fig. 1 is the stereoscan photograph of the hollow ferrum nanofiber of embodiment 1 preparation.
Fig. 2 is the stereoscan photograph of the hollow ferrum nanofiber of embodiment 2 preparation.
Fig. 3 is the stereoscan photograph of the hollow ferrum nanofiber of embodiment 3 preparation.
Specific embodiment
With reference to concrete drawings and Examples, the invention will be further described.
Embodiment 1：A kind of preparation method of hollow magnetic ferric oxide nano fiber, comprises the following steps：
(1) PVA (degree of polymerization 2000, alcoholysis degree 96%) powder is added in the distilled water that with the addition of glacial acetic acid, mixed
Close solution A；In mixed solution A, the concentration of PVA is 12wt%, and the concentration of acetic acid is 5wt%, and mixed solution A is placed on constant temperature magnetic
Heated and stirred on power agitator, so as to abundant dissolve, adjusts heating-up temperature and is 80 DEG C, and stir speed (S.S.) is 10r/min；
(2) clear solution obtaining step (1) is poured in needle tubing, starts electrostatic spinning, and regulation spinning voltage is 12kv,
The distance of syringe pump to collecting board is 10cm, obtains the PVA nano fibrous membrane of white, white PVA nano fibrous membrane is put into
Baking oven carries out heat treatment, adjusts temperature and is 150 DEG C, heat treatment time is 30min, obtains the PVA nano fibrous membrane of yellow；
(3) iron chloride and ferrous chloride are dissolved in distilled water and obtain mixed solution B, and mixed solution B is put into super
Carry out fully dispersed in sound separating apparatus, wherein the concentration of iron chloride is 5wt%, the concentration of ferrous chloride is 1.5wt%；By yellow
PVA nano fibrous membrane put in mixed solution B, using N2Protection, carries out water-bath, sets 60 DEG C of bath temperature, and to
Wherein instill the aqueous slkali that concentration is 2wt%, obtain having coated Fe3O4The PVA nano fibrous membrane of magnetic nano-particle；
(4) the PVA nano fibrous membrane having coated magnetic nano-particle is put into calcining under air atmosphere in tube furnace, calcining
Temperature is 600 DEG C, calcination time 45min, obtains described hollow magnetic ferric oxide nano fiber.
Embodiment 2：A kind of preparation method of hollow magnetic ferric oxide nano fiber, comprises the following steps：
(1) PVA (degree of polymerization 3200, alcoholysis degree 98%) powder is added in the distilled water that with the addition of glacial acetic acid, mixed
Close solution A；In mixed solution A, the concentration of PVA is 6wt%, and the concentration of acetic acid is 4wt%, and mixed solution A is placed on constant temperature magnetic force
Heated and stirred on agitator, so as to abundant dissolve, adjusts heating-up temperature and is 90 DEG C, and stir speed (S.S.) is 90r/min；
(2) clear solution obtaining step (1) is poured in needle tubing, starts electrostatic spinning, and regulation spinning voltage is 15kv,
The distance of syringe pump to collecting board is 12cm, obtains the PVA nano fibrous membrane of white, white PVA nano fibrous membrane is put into
Baking oven carries out heat treatment, adjusts temperature and is 180 DEG C, heat treatment time is 10min, obtains the PVA nano fibrous membrane of yellow；
(3) iron sulfate and ferrous sulfate are dissolved in distilled water and obtain mixed solution B, and mixed solution B is put into super
Carry out fully dispersed in sound separating apparatus, wherein the concentration of iron chloride is 1.5wt%, the concentration of ferrous chloride is 0.5wt%；By Huang
The PVA nano fibrous membrane of color is put in mixed solution B, using N2Protection, carries out water-bath, sets 50 DEG C of bath temperature, and
Instill the aqueous slkali that concentration is 1wt% thereto, obtain having coated Fe3O4The PVA nano fibrous membrane of magnetic nano-particle；
(4) the PVA nano fibrous membrane having coated magnetic nano-particle is put into calcining under air atmosphere in tube furnace, calcining
Temperature is 500 DEG C, calcination time 30min, obtains described hollow magnetic ferric oxide nano fiber.
Embodiment 3：A kind of preparation method of hollow magnetic ferric oxide nano fiber, comprises the following steps：
(1) PVA (degree of polymerization 8000, alcoholysis degree 99%) powder is added in the distilled water that with the addition of glacial acetic acid, mixed
Close solution A；In mixed solution A, the concentration of PVA is 3wt%, and the concentration of acetic acid is 50wt%, and mixed solution A is placed on constant temperature magnetic
Heated and stirred on power agitator, so as to abundant dissolve, adjusts heating-up temperature and is 95 DEG C, and stir speed (S.S.) is 100r/min；
(2) clear solution obtaining step (1) is poured in needle tubing, starts electrostatic spinning, and regulation spinning voltage is 10kv,
The distance of syringe pump to collecting board is 10cm, obtains the PVA nano fibrous membrane of white, white PVA nano fibrous membrane is put into
Baking oven carries out heat treatment, adjusts temperature and is 150 DEG C, heat treatment time is 30min, obtains the PVA nano fibrous membrane of yellow；
(3) ferric nitrate and ferrous nitrate are dissolved in distilled water and obtain mixed solution B, and mixed solution B is put into super
Carry out fully dispersed in sound separating apparatus, wherein the concentration of ferric nitrate is 8wt%, the concentration of ferrous nitrate is 3wt%；By yellow
PVA nano fibrous membrane is put in mixed solution B, using N2Protection, carries out water-bath, sets 80 DEG C of bath temperature, and to it
Middle instillation concentration is the aqueous slkali of 5wt%, obtains having coated magnetic Fe3O4The PVA nano fibrous membrane of nanoparticle；
(4) the PVA nano fibrous membrane having coated magnetic nano-particle is put into calcining under air atmosphere in tube furnace, calcining
Temperature is 800 DEG C, calcination time 120min, obtains described hollow magnetic ferric oxide nano fiber.
The hollow magnetic ferric oxide nano fiber that the present invention obtains has hollow structure, increases the specific surface area of fiber.
The hollow magnetic ferric oxide nano fiber of the present invention, using pattern uniform PVA nanofiber as matrix, size can be passed through
The thickness of the diameter of PVA nanofiber and clad, to adjust, overcomes the deficiencies in the prior art.As shown in FIG. 1 to 3, in
The stereoscan photograph of empty magnetic ferric oxide nano fiber shows that its pattern is uniform, form is excellent.
Claims (5)
1. a kind of preparation method of hollow magnetic ferric oxide nano fiber, is characterized in that, comprise the following steps：
(1) polyvinyl alcohol (PVA) is dissolved in the distilled water that with the addition of acetic acid, obtains mixed solution A；PVA in mixed solution A
Concentration be 1-20wt%, the concentration of acetic acid is 1-50wt%；
(2) A is carried out electrostatic spinning, regulation spinning voltage is 10-20kv, the distance of adjusting shower nozzle to cylinder is 5-20cm, obtains
To PVA nano fibrous membrane；
(3) PVA nano fibrous membrane is put into baking oven and carry out heat treatment, adjust temperature and be 150-250 DEG C, heat treatment time is 1-
30min, obtains the PVA nano fibrous membrane after heat treatment；
(4) trivalent iron salt and divalent iron salt are dissolved in distilled water and obtain mixed solution B, the concentration of wherein trivalent iron salt is
1.5-8wt%, the concentration of divalent iron salt is 0.5-3wt%；PVA nano fibrous membrane after heat treatment is put in mixed solution B, adopts
Use N2Protection, carries out hydrothermal synthesis reaction, sets 50-90 DEG C of bath temperature, and instills the alkali that concentration is 1-10wt% thereto
Solution, obtains the PVA nano fibrous membrane having coated ferriferrous oxide nano-particle；
(5) the PVA nano fibrous membrane having coated ferroso-ferric oxide is put into calcining a period of time in tube furnace, calcining heat is
500-900 DEG C, obtain described hollow magnetic ferric oxide nano fiber.
2. a kind of preparation method of hollow magnetic ferric oxide nano fiber as claimed in claim 1, is characterized in that：Step (1)
In, the alcoholysis degree 96-100% of described PVA, degree of polymerization 1700-10000.
3. a kind of preparation method of hollow magnetic ferric oxide nano fiber as claimed in claim 1, is characterized in that：Step (4)
In, described trivalent iron salt is iron chloride, iron sulfate and ferric nitrate.Described divalent iron salt is ferrous chloride, ferrous sulfate and nitric acid
Ferrous.
4. a kind of preparation method of hollow magnetic ferric oxide nano fiber as claimed in claim 1, is characterized in that：Step (4)
In, described aqueous slkali is sodium carbonate liquor, sodium bicarbonate solution, sodium hydroxide solution and potassium hydroxide solution.
5. the preparation method of hollow magnetic ferric oxide nano fiber as claimed in claim 1, is characterized in that：In step (5), institute
Stating calcination time is 30～120 minutes.Calcination atmosphere is air.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611029130.3A CN106400205A (en) | 2016-11-21 | 2016-11-21 | Preparation method of hollow magnetic iron oxide nanofiber |
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| CN201611029130.3A CN106400205A (en) | 2016-11-21 | 2016-11-21 | Preparation method of hollow magnetic iron oxide nanofiber |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541078A (en) * | 2017-09-17 | 2018-01-05 | 钱景 | A kind of silk fibre composite of graphene oxide parcel and preparation method thereof |
| CN107556762A (en) * | 2017-09-17 | 2018-01-09 | 钱景 | A kind of titanic oxide/zinc oxide/silk/salix monogolica composite and preparation method |
| CN108411405A (en) * | 2018-04-03 | 2018-08-17 | 青岛大学 | A kind of Fe2O3/TiO2Composite nano fiber and preparation method thereof |
| CN108753251A (en) * | 2018-06-14 | 2018-11-06 | 山东大学 | A kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material and preparation method thereof |
| CN113952845A (en) * | 2021-11-05 | 2022-01-21 | 岭东核电有限公司 | Membrane filter material, preparation method thereof and application of membrane filter material in treating aerosol |
| CN115838521A (en) * | 2022-06-20 | 2023-03-24 | 宁德时代新能源科技股份有限公司 | Hollow fiber composite, method for producing same, electrode sheet, battery module, battery pack, and device |
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| CN1851070A (en) * | 2006-05-16 | 2006-10-25 | 苏州大学 | Polyvinyl alcohol electrostatic spinning solution |
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| CN1851070A (en) * | 2006-05-16 | 2006-10-25 | 苏州大学 | Polyvinyl alcohol electrostatic spinning solution |
Non-Patent Citations (2)
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| 王新月 等: ""α-Fe2O3中空磁性纳米纤维的制备研究"", 《功能材料》 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107541078A (en) * | 2017-09-17 | 2018-01-05 | 钱景 | A kind of silk fibre composite of graphene oxide parcel and preparation method thereof |
| CN107556762A (en) * | 2017-09-17 | 2018-01-09 | 钱景 | A kind of titanic oxide/zinc oxide/silk/salix monogolica composite and preparation method |
| CN108411405A (en) * | 2018-04-03 | 2018-08-17 | 青岛大学 | A kind of Fe2O3/TiO2Composite nano fiber and preparation method thereof |
| CN108753251A (en) * | 2018-06-14 | 2018-11-06 | 山东大学 | A kind of ZnO/Co composite Nanos hollow fibre electromagnetic wave absorbent material and preparation method thereof |
| CN108753251B (en) * | 2018-06-14 | 2020-04-14 | 山东大学 | ZnO/Co composite nano hollow fiber electromagnetic wave absorbing material and preparation method thereof |
| CN113952845A (en) * | 2021-11-05 | 2022-01-21 | 岭东核电有限公司 | Membrane filter material, preparation method thereof and application of membrane filter material in treating aerosol |
| CN113952845B (en) * | 2021-11-05 | 2022-07-15 | 岭东核电有限公司 | Membrane filter material, preparation method thereof and application of membrane filter material in treating aerosol |
| CN115838521A (en) * | 2022-06-20 | 2023-03-24 | 宁德时代新能源科技股份有限公司 | Hollow fiber composite, method for producing same, electrode sheet, battery module, battery pack, and device |
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Application publication date: 20170215 |