CN103789876A - Synthetic method of strip porous lanthanum ferrite nano fibers - Google Patents
Synthetic method of strip porous lanthanum ferrite nano fibers Download PDFInfo
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- CN103789876A CN103789876A CN201410032901.9A CN201410032901A CN103789876A CN 103789876 A CN103789876 A CN 103789876A CN 201410032901 A CN201410032901 A CN 201410032901A CN 103789876 A CN103789876 A CN 103789876A
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Abstract
The invention relates to a synthetic method of strip porous lanthanum ferrite nano fibers. The method comprises the following steps: dissolving Fe salt and La salt in mixed liquor of ethanol and acetic acid, and stirring at room temperature to form mixed liquor A; then, dissolving polyvinylpyrrolidone or polyvinyl alcohol in ethanol, and stirring at room temperature to form liquor B; slowing adding the mixed liquor A into the liquor B, and stirring at room temperature to form precursor liquor C; and electrostatically spinning the precursor liquor C to dry and roast the collected compound fibers. The strip porous lanthanum ferrite nano fibers are prepared by adopting an electrostatic spinning method. The strip porous lanthanum ferrite nano fibers have a stable and uniform structure, a large specific surface area, a high aspect ratio and an opened porous structure, so that the many active sites are formed, and performances such as catalysis and adsorption are remarkably improved.
Description
Technical field
The present invention relates to the synthetic method of nanometer ferrous acid lanthanum, particularly the method for the synthetic banded porous iron acid of high-voltage electrostatic spinning law technology lanthanum nanofiber.
Background technology
Nanofiber refers to line (pipe) the shape material of bidimensional in nanoscale on the three dimensions yardstick of material, mainly comprises nano silk, nano wire, nanometer rods, nanotube, nanobelt, nano-cable etc.The feature of nanofiber maximum is exactly that specific area is large, cause surface to increase with active, produce small-size effect, surface or interfacial effect, quantum size effect, macro quanta tunnel effect etc., gone out good specificity on surfaces, aspect such as light, sound, electricity, magnetic, heat.
The method that tradition is prepared nanofiber reel off raw silk from cocoons method, template synthetic method, split-phase method, self-assembly method, Using Gas Evaporation Method etc., but said method all cannot be produced the controlled nanofiber of size homogeneous.Electrostatic spinning rule can be avoided above-mentioned deficiency, becomes the technical way of the outer researcher's synthesis of nano fiber of Present Domestic.
The easy inactivation of ferrous acid lanthanum nano particle, easily cohesion, difficult recovery that traditional citric acid method is prepared, this has just reduced specific area, thereby has reduced the performance such as catalysis and absorption.Be nano silk and nanotube mostly and utilize the synthetic ferrous acid lanthanum nanofiber of method of electrostatic spinning, specific area is not very high, and then affects its some Practical Performances.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of synthetic method of banded porous ferrous acid lanthanum nanofiber, and synthetic ferrous acid lanthanum nanofiber has larger specific area.
A synthetic method for banded porous ferrous acid lanthanum nanofiber, comprises step:
(1) the Fe salt that is 1:1 by mol ratio or and La salt be dissolved in organic solvent or water, at room temperature stir form mixed solution A, described Fe salt is Fe (NO
3)
39H
2o or C
15h
21feO
6, La salt is La (NO
3)
36H
2o or La (CH
3cOO)
31.5H
2o;
(2) high polymer is dissolved in ethanol again, at room temperature stirs and form solution B, the quality of high polymer is 4 times of gross mass of Fe salt and La salt, and described high polymer is polyvinylpyrrolidone or polyvinyl alcohol;
(3) mixed solution A is slowly joined in solution B, and at room temperature stir formation precursor solution C;
(4) precursor solution C carries out electrostatic spinning, the composite fibre collected is dried to roasting and get final product.
As preferred scheme, in step (1), described organic solution is the mixed solution that ethanol and acetic acid are mixed to form with the volume ratio of 1:3-1:0.5, have this volume ratio stable system, in spinning process, can form stable taylor cone.
As preferred scheme, in step (1), described organic solution is acetic acid, dimethyl formamide (DMF).
The impact that is formed with on solution viscosity and fiber of Fe salt and La salt content, when Fe salt and La salt content are larger, difficulty in spinning, only have little fiber, and fiber is discontinuous on receiver; Fe salt and La salt content hour, have a large amount of droplets agglomerate on receiver, can only observe the fiber of minute quantity on receiver; When Fe salt and La salt content are suitable, can spray continuously a large amount of fibers, and the fiber of collecting on receiver is more level and smooth, therefore, as preferred scheme, in step (1), Fe salt and La salt are dissolved in organic solvent or water with the input amount of 0.2-0.3g/mL.
Polyvinylpyrrolidone and polyvinyl alcohol, as synthesizing water-solubility macromolecular compound, have the general aspects of water-soluble high-molecular compound, both water-soluble, are dissolved in again that majority of organic solvent, toxicity are very low, physiology intermiscibility is good.The concentration of solution is larger, and its viscosity is just larger.The viscosity of precursor solution is the important factor in order of electrostatic spinning process, the pattern of major effect composite fibre.When viscosity is suitable, the level and smooth and diameter of the fiber surface collected on receiver is evenly distributed.Therefore,, as preferred scheme, in step (2), polyvinylpyrrolidone or polyvinyl alcohol are dissolved in ethanol with the input amount of 0.35-0.45g/mL.
The present invention adopts method of electrostatic spinning to prepare the ferrous acid lanthanum nanofiber of banded porous, and this band shape porous nano-fibre has Stability Analysis of Structures, even, bigger serface, and high aspect ratio and open pore structure, and make avtive spot more.The specific area of synthetic banded porous ferrous acid lanthanum nanofiber is at 41.25-136.68m
2/ g, compared with citric acid complex method, sintetics specific area of the present invention increases more than three times, the performances such as catalysis and absorption be improved significantly.
In addition, synthesis technique of the present invention is simple, easy to operate, and cost is low, is easy to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the banded porous LaFeO of embodiment 1
3the SEM figure of nanobelt fiber.
Fig. 2 is the banded porous LaFeO of embodiment 1
3the TEM figure of nanobelt fiber.
The specific embodiment
Below specific embodiment of the invention method is further detailed, those skilled in the art is reading after this specific embodiment, can realize technical scheme of the present invention, and meanwhile, advantage of the present invention and good effect also can be embodied.
Embodiment 1
Fe (the NO that is 1:1 by 0.5g mol ratio
3)
39H
2o and La (NO
3)
36H
2o is dissolved in the mixed solution of 1mL ethanol and 1mL acetic acid, at room temperature stirs 1h form mixed solution A with magnetic stirring apparatus.Again 2g polyvinylpyrrolidone is dissolved in 5mL ethanol, at room temperature stirs 2h and form solution B.Finally mixed solution A is slowly joined in solution B with dropping funel, and at room temperature stir 6h, form precursor solution C.Precursor solution is joined in syringe, and the negative pole of high voltage source connects receiver, and positive pole connects the stainless steel syringe needle of syringe, carries out spinning.The composite fibre of collecting is dried to roasting.
Embodiment 2
The C that is 1:1 by 0.4g mol ratio
15h
21feO
6and La (CH
3cOO)
31.5H
2o is dissolved in 2mL acetic acid, at room temperature stirs 1h form mixed solution A with magnetic stirring apparatus.Again 1.75g polyvinylpyrrolidone is dissolved in 5mL ethanol, at room temperature stirs 2h and form solution B.Finally mixed solution A is slowly joined in solution B with dropping funel, and at room temperature stir 6h, form precursor solution C.Precursor solution is joined in syringe, and the negative pole of high voltage source connects receiver, and positive pole connects the stainless steel syringe needle of syringe, carries out spinning.The composite fibre of collecting is dried to roasting.
Embodiment 3
The C that is 1:1 by 0.6g mol ratio
15h
21feO
6and La (NO
3)
36H
2o is dissolved in 2mL distilled water, at room temperature stirs 1h form mixed solution A with magnetic stirring apparatus.Again 2.25g polyvinylpyrrolidone is dissolved in 5mL ethanol, at room temperature stirs 2h and form solution B.Finally mixed solution A is slowly joined in solution B with dropping funel, and at room temperature stir 6h, form precursor solution C.Precursor solution is joined in syringe, and the negative pole of high voltage source connects receiver, and positive pole connects the stainless steel syringe needle of syringe, carries out spinning.The composite fibre of collecting is dried to roasting.
Embodiment 4
Fe (the NO that is 1:1 by 0.5g mol ratio
3)
39H
2o and La (NO
3)
36H
2o is dissolved in dimethyl formamide (DMF), at room temperature stirs 1h form mixed solution A with magnetic stirring apparatus.Again 2g polyvinyl alcohol is dissolved in 5mL ethanol, at room temperature stirs 2h and form solution B.Finally mixed solution A is slowly joined in solution B with dropping funel, and at room temperature stir 6h, form precursor solution C.Precursor solution is joined in syringe, and the negative pole of high voltage source connects receiver, and positive pole connects the stainless steel syringe needle of syringe, carries out spinning.The composite fibre of collecting is dried to roasting.
Embodiment 5
With the difference of the embodiment 1 Fe (NO that to be only 0.5g mol ratio be 1:1
3)
39H
2o and La (NO
3)
36H
2o is dissolved in the mixed solution of 0.5mL ethanol and 1.5mL acetic acid.
Embodiment 6
With the difference of embodiment 2 C that to be only 0.6g mol ratio be 1:1
15h
21feO
6and La (CH
3cOO)
31.5H
2o is dissolved in the mixed solution of 2mL ethanol and 1mL acetic acid.
Claims (5)
1. a synthetic method for banded porous ferrous acid lanthanum nanofiber, comprises step:
(1) the Fe salt that is 1:1 by mol ratio or and La salt be dissolved in organic solvent or water, at room temperature stir form mixed solution A, described Fe salt is Fe (NO
3)
39H
2o or C
15h
21feO
6, La salt is La (NO
3)
36H
2o or La (CH
3cOO)
31.5H
2o;
(2) high polymer is dissolved in ethanol again, at room temperature stirs and form solution B, the quality of high polymer is 4 times of gross mass of Fe salt and La salt, and described high polymer is polyvinylpyrrolidone or polyvinyl alcohol;
(3) mixed solution A is slowly joined in solution B, and at room temperature stir formation precursor solution C;
(4) precursor solution C carries out electrostatic spinning, the composite fibre collected is dried to roasting and get final product.
2. method according to claim 1, is characterized in that: in step (1), described organic solvent is the mixed solution that ethanol and acetic acid are mixed to form with the volume ratio of 1:3-1:0.5.
3. method according to claim 1, is characterized in that: in step (1), described organic solvent is acetic acid, dimethyl formamide (DMF).
4. according to the method described in claim 1 or 2 or 3, it is characterized in that: in step (1), Fe salt and La salt are dissolved in organic solvent or water with the input amount of 0.2-0.3g/mL.
5. according to the method described in claim 1 or 2 or 3, it is characterized in that: in step (2), polyvinylpyrrolidone or polyvinyl alcohol are dissolved in ethanol with the input amount of 0.35-0.45g/mL.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828870A (en) * | 2015-03-27 | 2015-08-12 | 中国石油大学(北京) | Rare earth ferrite with macropore mesopore grading channel structure and manufacturing method and application thereof |
| CN106186079A (en) * | 2016-06-28 | 2016-12-07 | 郑州轻工业学院 | The preparation method of Ca-Ti ore type lanthanium complex oxide nanotube |
| CN107237008A (en) * | 2017-06-01 | 2017-10-10 | 赵云飞 | Preparation method, electrode and the electrochemical sensor of porous nano-fibre |
| CN110790317A (en) * | 2019-11-11 | 2020-02-14 | 东北大学 | Quadrature-phase yttrium ferrite nanofiber and preparation method thereof |
| CN113249824A (en) * | 2021-05-27 | 2021-08-13 | 陕西师范大学 | Preparation method of flexible carbon/lanthanum ferrite composite fiber membrane material |
| CN114751738A (en) * | 2022-03-08 | 2022-07-15 | 东华大学 | Strip-shaped ceramic fiber and preparation method and application thereof |
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| CN102502882A (en) * | 2011-10-10 | 2012-06-20 | 长春理工大学 | Method for preparing La2Fe2S5 submicron rod |
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2014
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| CN102268783A (en) * | 2011-06-20 | 2011-12-07 | 东华大学 | Method for preparing polyvinylidene fluoride (PVDF) porous nanofiber membrane with high ion migration number |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104828870A (en) * | 2015-03-27 | 2015-08-12 | 中国石油大学(北京) | Rare earth ferrite with macropore mesopore grading channel structure and manufacturing method and application thereof |
| CN104828870B (en) * | 2015-03-27 | 2016-06-08 | 中国石油大学(北京) | There is the rare earth ferrite of the mesoporous classification pore passage structure of macropore and method for making thereof and application |
| CN106186079A (en) * | 2016-06-28 | 2016-12-07 | 郑州轻工业学院 | The preparation method of Ca-Ti ore type lanthanium complex oxide nanotube |
| CN106186079B (en) * | 2016-06-28 | 2017-06-06 | 郑州轻工业学院 | The preparation method of Ca-Ti ore type lanthanium complex oxide nanotube |
| CN107237008A (en) * | 2017-06-01 | 2017-10-10 | 赵云飞 | Preparation method, electrode and the electrochemical sensor of porous nano-fibre |
| CN110790317A (en) * | 2019-11-11 | 2020-02-14 | 东北大学 | Quadrature-phase yttrium ferrite nanofiber and preparation method thereof |
| CN113249824A (en) * | 2021-05-27 | 2021-08-13 | 陕西师范大学 | Preparation method of flexible carbon/lanthanum ferrite composite fiber membrane material |
| CN113249824B (en) * | 2021-05-27 | 2022-11-18 | 陕西师范大学 | Preparation method of flexible carbon/lanthanum ferrite composite fiber membrane material |
| CN114751738A (en) * | 2022-03-08 | 2022-07-15 | 东华大学 | Strip-shaped ceramic fiber and preparation method and application thereof |
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