CN102041584A - Magnetic self-assembled mesoporous fiber and preparation method thereof - Google Patents
Magnetic self-assembled mesoporous fiber and preparation method thereof Download PDFInfo
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Abstract
The invention provides a magnetic self-assembled mesoporous fiber and a preparation method thereof. The preparation method comprises the following steps of: assembling magnetic matters on a mesoporous fiber in situ by adopting a sol-gel process, wherein the assembling quantity of the magnetic matters on the fiber accounts for 5-60 percent of the total weight; respectively dissolving metal salt and silicon sources into a solvent to prepare a metal-salt-containing solution of a certain concentration and a silicon-containing solution of a certain concentration; mixing the two solutions in proportion; adding a few of modifying agent, evenly mixing; aging for a certain period, and obtaining a magnetic composite silicon oxide fiber through a spinning technology or a fiber throwing technology; and sintering at high temperature to obtain a magnetic SiO2 mesoporous self-assembled fiber. The preparation method is simple for operation; the prepared magnetic SiO2 mesoporous self-assembled fiber has a regular shape; and fine magnetic particles are evenly distributed in pores of the mesoporous fiber and have controllable and adjustable assembling quantity.
Description
Technical field
The invention belongs to field of functional materials, be specifically related to a kind of magnetic self assembly mesoporous fiber and preparation method thereof.
Background technology
In the last few years, the mesoporous assembled material that can manually design was because its important basic research meaning and huge potential using value became one of all multidisciplinary forward position research fields such as crossing over physics, chemistry, material science, information science and life science.Mesoporous material can be used for the carrier of artificial heterogeneous assembly system, thereby produces various new-type functional material.Mesoporous material is because its specific area is big, voidage is high, pore-size distribution is narrow; and structurally have short distance orderly characteristics of sight level that are that atomic level is unordered, long-range promptly is situated between; its aperture is controlled easily simultaneously; thereby catalysis and separation science and light, electricity, magnetic, sensor, environmental protection, biological aspect numerous areas such as (fixing, identification such as enzyme, protein, the transmission of medicine etc.) very important application prospects is arranged.
Mesoporous magnetic composite is magnetic-particle to be assembled in the duct of mesoporous solid be composited, this new material is because the interaction at hole wall-granular boundary place, thereby have not available, the corresponding not available a series of properties of body phase material especially of magnetic-particle and mesoporous solid, greatly expanded application in magnetic fields.Magnetic-particle is assembled in the mesoporous silicon oxide, can obtains having the Transparent Magnetic Materials of applications well prospect, compare with the transparent polymer magnetic material, they have the better transparency, stronger magnetic, better photo and thermal stability and mechanical strength.Usually, the heterogeneous assembling of mesoporous material comprises the synthetic and post-modification method of original position.In-situ synthesis adopts template agent, silicon source and source of iron, under certain pH, and the mesopore silicon oxide material of the synthetic iron content of original position.The post-modification method is to introduce molysite to the hole of mesoporous material by methods such as liquid deposition, vapour deposition or solid phase doping on the basis of synthesizing ordered mesoporous material; by adding thermal bake-out molysite is decomposed then, thereby form iron oxide particle or iron oxygen bunch at hole surface.The research of mesoporous magnetic composite concentrates on (Huang Xianghui, Chen Zhenhua, the preparation of γ-Fe2O3/SiO2 composite nano-powder on the mesoporous magnetic composite powder mostly, Journal of Inorganic Materials, 2005,20 (3): 685-681), seldom (Wang Yin emits galactic equator, Wang Deyan and to the research of mesoporous magnetic laminated film and coating, Hu Xiaoya, self-assembling method prepare orderly microporous membrane, chemical progress, 2008,20 (1): 105-116),, be in blank especially for preparation magnetic self assembly mesoporous fiber.
Fiber is its block materials relatively, marked change has taken place in physical property, as Shi Yejian (TDK company), the U.S. A.H.Goldberg of Japan, R.C.Pullar, the Ц м у т и н И of synthetic polymer research institute of the academy of sciences of Russia of Britain. А. wait studies show that, the ferrite fibre material is changed significantly at the magnetic conductivity of microwave section, draw ratio is that its magnetic conductivity of staple fibre of 50: 1 will be 50 times with the volume bulk material, and material fiberization is remarkable to the raising of magnetic conductivity.Magnetic-particle is self-assembled in the meso-porous titanium dioxide silica fibre; not available a series of properties of Dui Ying body phase material especially; in fields such as magnetic recording, magnetic-optic devices, electromagnetic shielding, radar-wave absorbings huge potential using value is arranged, but also may be applied in other fields such as chemical industry catalysis, environmental protection, biomedicines.
Summary of the invention
The invention provides a kind of magnetic self assembly mesoporous fiber and preparation method thereof.The inventive method is simple to operate, and the mesoporous magnetic assembling of the SiO2 of preparation fibrous appearance is regular, and magnetic-particle is tiny, be uniformly distributed in the hole of mesoporous fiber, and magnetic-particle assembling amount controllable adjustment.
A kind of magnetic self assembly mesoporous fiber is to be assembled with magnetisable material in the mesoporous fiber duct, and wherein the assembling amount of magnetisable material in the fiber duct is 5～60% of both gross weights.Described mesoporous fiber is a silicon dioxide fibre.
Described magnetisable material is a kind of or their mixture in the compound of iron, manganese, copper, barium, cobalt, nickel, zinc.The compound of described iron, manganese, copper, barium, cobalt, nickel, zinc comprises metallic iron, manganese-zinc ferrite, cu ferrite, Zn ferrite, barium ferrite, CoZ ferrite, Mn ferrite, Ni ferrite, nickel Conjugate ferrite, Conjugate ferrite, nickel-copper ferrite or nickel-zinc ferrite.
A kind of preparation method of magnetic self assembly mesoporous fiber may further comprise the steps:
(1) preparation of colloidal sol
Respectively slaine and silicon source are dissolved in the solvent, be mixed with the siliceous solution of 10-200g/L metalline solution and 5-50g/L, above-mentioned two kinds of solution are pressed mass ratio 0.1～10 fully to be mixed, obtain mixed solution, get the mixed solution of 95～100 components by weight percent again, add the modifier of 0～5 components by weight percent, mix, stir 10～120min down at 30～80 ℃,, obtain the combined oxidation Ludox 20～80 ℃ of following ageings;
(2) preparation of spinning solution
Add 0～10 components by weight percent spinning-aid agent and mix in 90～100 components by weight percent combined oxidation Ludox, being concentrated into viscosity through 20～300 ℃ of constant temperature is 0.01～200pas, obtains spinning solution;
(3) spinning or get rid of silk
The spinning solution vacuum is deviate from bubble fully, extrude at the porous spinnerets of 10～500 μ m through diameter, one or more in the mode that stretches with static stretching, mechanical stretching or magnetic field orientating, total draw ratio is 3～300, obtains continuous gelatinous fibre; Or get rid of silk and obtain a staple fibre through getting rid of silk dish, get rid of silk dish rotating speed a 1000～10000r/min, the long 1cm～5cm of staple fibre;
(4) sintering
With above-mentioned gained fiber at H
2Or N
2Or heat treatment under both mixed atmospheres, 350～900 ℃ of temperature, time 1hr～4hr, obtain magnetic self assembly mesoporous fiber.
Described slaine is one or more mixing in ferric sulfate, ferric nitrate, iron chloride, frerrous chloride, ethanol iron, ferric acetate, ferrocene, ferric acetyl acetonade, iron pentacarbonyl, cobalt chloride, cobaltous sulfate, cobalt nitrate, pentacarbonyl cobalt, cobalt acetate, acetylacetone cobalt, nickel chloride, nickelous sulfate, nickel nitrate, nickel acetate, pentacarbonyl nickel, nickel acetylacetonate, barium chloride, barium nitrate, zinc chloride, zinc sulfate, zinc nitrate, manganese chloride, manganese sulfate, manganese nitrate, copper chloride, the copper sulphate.
Described silicon source is meant methyl silicate, ethyl orthosilicate, positive silicic acid propyl ester, butyl silicate or sodium metasilicate.
Described solvent is one or more the mixing of water, methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol, n-butanol, sec-butyl alcohol, isobutanol, amylalcohol, formic acid, acetate, benzene, acetonitrile, chloroform, pentane, hexane, benzinum, cyclohexane, carrene, ethyl acetate, carbon tetrachloride.
Described modifier is: hexadecyltrimethylammonium chloride, formamide, triethylamine, acetylacetone,2,4-pentanedione or ethyl acetoacetate.
Described spinning-aid agent comprises polyvinyl alcohol, polyethylene glycol, polyethylene glycol oxide, polyvinyl butyral resin or polyvinylpyrrolidone.
The present invention has compared following characteristics with other magnetic mesoporous assembled material:
(1) magnetic-particle is assembled in the duct of mesoporous fiber, magnetic mesoporous fiber is its block materials relatively, marked change has taken place in physical property, thereby have not available, the corresponding not available a series of properties of body phase material especially of magnetic-particle and mesoporous solid, huge potential using value is arranged in fields such as magnetic recording, magnetic-optic devices, electromagnetic shielding, radar-wave absorbings;
(2) magnetic-particle is adopted the sol-gel technology original position self-assemble in the duct of mesoporous fiber, technological operation is simple;
(3) magnetic component is more in the magnetic mesoporous composite fibre, magnetic-particle assembling amount controllable adjustment.
The inventive method is simple to operate, the SiO of preparation
2Mesoporous magnetic assembling fibrous appearance is regular, and magnetic-particle is tiny, be uniformly distributed in the hole of mesoporous fiber, and magnetic-particle assembling amount controllable adjustment.
Description of drawings
Fig. 1 is the ESEM picture of the mesoporous magnetic self assembly of the present invention fiber;
Fig. 2 is the XRD figure spectrum of the mesoporous magnetic self assembly of the present invention fiber;
Fig. 3 is the magnetic hysteresis tropic of the mesoporous magnetic self assembly of the present invention fiber.
The specific embodiment
Be intended to further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
Embodiment 1:
97 weight portion methyl silicates (TMOS) are mixed with 22.5 weight portion distilled water, regulate pH=5 with nitric acid, electromagnetic agitation is added drop-wise to 200 weight portion hexadecyltrimethylammonium chloride (CTAC after 2 hours, CTAC and TMOS mol ratio are 1: 4) solution in, 271 weight portion iron chloride are dissolved in the 1000 weight portion distilled water, then two kinds of solution are mixed, refluxed 1 hour in 60 ℃ under the electromagnetic agitation, place 80 ℃ of water-baths to heat 7 hours again, form pregel to the viscosity increase.Pregel is extruded (bore dia is 500 μ m) through the porous spinnerets, forms gelatinous fibre by the mechanical stretching effect, obtains continuous fibers 130 ℃ of dryings after 2 hours again.Continuous fibers is placed sintering furnace, pass to hydrogen, be warming up to 600 ℃ of calcinations 2 hours with 1 ℃/minute speed, magnetizing 0.1～2 minute under magnetic field intensity 12000 Gausses in the cooling back, promptly obtains continuous magnetic mesoporous assembling silicon dioxide fibre.
Embodiment 2:
233 weight portion ethyl orthosilicates are dissolved in the 118 weight portion absolute ethyl alcohols, 75 weight portion ferric nitrates are dissolved in 118 weight portion absolute ethyl alcohols, then two kinds of solution are mixed, add 50 weight portion formamides again, use the nitre acid for adjusting pH value, after the electromagnetic agitation 0.5 hour, uncovered 60 ℃ of water-baths heating 4 hours to the viscosity that places increases, and forms compound pregel.Compound pregel is extruded (bore dia is 20 μ m) through the porous spinnerets, applies 2 * 10 simultaneously
5The high-voltage electrostatic field of V/m stretches, and obtains continuous mesoporous silicon oxide composite fibre after the drying.Fiber is placed sintering furnace, pass to hydrogen, be warming up to 600 ℃ of calcinations 2 hours with 1 ℃/minute speed, magnetizing 0.1～2 minute under magnetic field intensity 12000 Gausses in the cooling back, promptly obtains continuous magnetic mesoporous assembling silicon dioxide fibre.
Embodiment 3:
50 weight portion cobalt nitrates are dissolved in the 200 weight portion absolute ethyl alcohols, add 100 weight portion ethyl orthosilicates simultaneously, place 90 ℃ of oil baths to reflux 72 hours, form pregel to the viscosity increase.Adding mass fraction at pregel is 0.04% polyvinyl alcohol (PVA, 1750), extrudes (bore dia is 500 μ m) through the porous spinnerets, forms gelatinous fibre by the mechanical stretching effect, promptly obtains continuous fibers after the drying.Continuous fibers is placed sintering furnace, pass to hydrogen, be warming up to 800 ℃ of calcinations 1 hour with 1 ℃/minute speed, magnetizing 0.1～2 minute under magnetic field intensity 12000 Gausses in the cooling back, promptly obtains continuous magnetic mesoporous assembling silicon dioxide fibre.
Embodiment 4:
50 weight portion nickel chlorides are dissolved in the 200 weight portion absolute ethyl alcohols, add 100 weight portion ethyl orthosilicates simultaneously, place 90 ℃ of oil baths to reflux 72 hours, form pregel to the viscosity increase.Adding mass fraction at pregel is 0.04% polyvinyl alcohol (PVA, 1750), extrudes (bore dia is 500 μ m) through the porous spinnerets, forms gelatinous fibre by the mechanical stretching effect, promptly obtains continuous fibers after the drying.Continuous fibers is placed sintering furnace, pass to hydrogen, be warming up to 800 ℃ of calcinations 1 hour with 1 ℃/minute speed, magnetizing 0.1～2 minute under magnetic field intensity 12000 Gausses in the cooling back, promptly obtains continuous magnetic mesoporous assembling silicon dioxide fibre.
Embodiment 5:
50 weight portion ferric acetyl acetonades are dissolved in 300 methyl alcohol, add 150 weight portion acetylacetone,2,4-pentanediones, under 0 ℃ of ice bath, dropwise add 3 weight portion triethylamines while stirring, add 200 weight portion methyl silicates then, dropwising the recession deicing bathes, at room temperature continue to stir 2 hours again, place ageing oven to be aged to certain viscosity in 40 ℃ solution, obtain pregel.Pregel is extruded (bore dia is 50 μ m) through the porous spinnerets, and the high-voltage electrostatic field that applies 2 * 105V/m simultaneously stretches, and obtains continuous mesoporous silicon oxide composite fibre after the drying.Fiber is placed sintering furnace, pass to hydrogen, be warming up to 900 ℃ of calcinations 2 hours with 1 ℃/minute speed, magnetizing 0.1～2 minute under magnetic field intensity 12000 Gausses in the cooling back, promptly obtains continuous magnetic mesoporous assembling silicon dioxide fibre.
Claims (10)
1. a magnetic self assembly mesoporous fiber is characterized in that, is to be assembled with magnetisable material in the mesoporous fiber duct, and wherein the assembling amount of magnetisable material in the fiber duct is 5～60% of both gross weights.
2. magnetic self assembly mesoporous fiber according to claim 1 is characterized in that described mesoporous fiber is a silicon dioxide fibre.
3. magnetic self assembly mesoporous fiber according to claim 1 is characterized in that, described magnetisable material is a kind of or their mixture in the compound of iron, manganese, copper, barium, cobalt, nickel, zinc.
4. magnetic self assembly mesoporous fiber according to claim 3, it is characterized in that the compound of described iron, manganese, copper, barium, cobalt, nickel, zinc comprises metallic iron, manganese-zinc ferrite, cu ferrite, Zn ferrite, barium ferrite, CoZ ferrite, Mn ferrite, Ni ferrite, nickel Conjugate ferrite, Conjugate ferrite, nickel-copper ferrite or nickel-zinc ferrite.
5. the preparation method of a magnetic self assembly mesoporous fiber is characterized in that, may further comprise the steps:
(1) preparation of colloidal sol
Respectively slaine and silicon source are dissolved in the solvent, be mixed with the siliceous solution of 10-200g/L metalline solution and 5-50g/L, above-mentioned two kinds of solution are pressed mass ratio 0.1～10 fully to be mixed, obtain mixed solution, get the mixed solution of 95～100 components by weight percent again, add the modifier of 0～5 components by weight percent, mix, stir 10～120min down at 30～80 ℃,, obtain the combined oxidation Ludox 20～80 ℃ of following ageings;
(2) preparation of spinning solution
Add 0～10 components by weight percent spinning-aid agent and mix in 90～100 components by weight percent combined oxidation Ludox, being concentrated into viscosity through 20～300 ℃ of constant temperature is 0.01～200pas, obtains spinning solution;
(3) spinning or get rid of silk
The spinning solution vacuum is deviate from bubble fully, extrude at the porous spinnerets of 10～500 μ m, one or more in the mode that stretches with static stretching, mechanical stretching or magnetic field orientating, total draw ratio through diameter
Be 3～300,Obtain continuous gelatinous fibre; Or get rid of silk and obtain a staple fibre through getting rid of silk dish, get rid of silk dish rotating speed a 1000～10000r/min, the long 1cm～5cm of staple fibre;
(4) sintering
With the heat treatment under H2 or N2 or both mixed atmospheres, 350～900 ℃ of temperature, time 1hr～4hr of above-mentioned gained fiber, obtain magnetic self assembly mesoporous fiber.
6. the preparation method of magnetic self assembly mesoporous fiber according to claim 5, it is characterized in that described slaine is a ferric sulfate, ferric nitrate, iron chloride, frerrous chloride, ethanol iron, ferric acetate, ferrocene, ferric acetyl acetonade, iron pentacarbonyl, cobalt chloride, cobaltous sulfate, cobalt nitrate, the pentacarbonyl cobalt, cobalt acetate, acetylacetone cobalt, nickel chloride, nickelous sulfate, nickel nitrate, nickel acetate, pentacarbonyl nickel, nickel acetylacetonate, barium chloride, barium nitrate, zinc chloride, zinc sulfate, zinc nitrate, manganese chloride, manganese sulfate, manganese nitrate, copper chloride, one or more mixing in the copper sulphate.
7. the preparation method of magnetic self assembly mesoporous fiber according to claim 5 is characterized in that, described silicon source is meant methyl silicate, ethyl orthosilicate, positive silicic acid propyl ester, butyl silicate or sodium metasilicate.
8. the preparation method of magnetic self assembly mesoporous fiber according to claim 5, it is characterized in that described solvent is one or more the mixing of water, methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol, n-butanol, sec-butyl alcohol, isobutanol, amylalcohol, formic acid, acetate, benzene, acetonitrile, chloroform, pentane, hexane, benzinum, cyclohexane, carrene, ethyl acetate, carbon tetrachloride.
9. the preparation method of magnetic self assembly mesoporous fiber according to claim 5 is characterized in that, described modifier is: hexadecyltrimethylammonium chloride, formamide, triethylamine, acetylacetone,2,4-pentanedione or ethyl acetoacetate.
10. the preparation method of magnetic self assembly mesoporous fiber according to claim 5 is characterized in that described spinning-aid agent comprises polyvinyl alcohol, polyethylene glycol, polyethylene glycol oxide, polyvinyl butyral resin or polyvinylpyrrolidone.
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| CN102623125A (en) * | 2012-03-28 | 2012-08-01 | 东华大学 | Preparation method for Fe3O4/SiO2 nanometer particle containing multiple magnetism cores |
| CN103311510A (en) * | 2013-05-19 | 2013-09-18 | 吉林大学 | Method for preparing zinc ferrite coated by graphene |
| CN103409851A (en) * | 2013-08-23 | 2013-11-27 | 厦门大学 | Preparation method of cobalt containing silicon carbide fiber |
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| CN103409851A (en) * | 2013-08-23 | 2013-11-27 | 厦门大学 | Preparation method of cobalt containing silicon carbide fiber |
| CN103409851B (en) * | 2013-08-23 | 2015-07-15 | 厦门大学 | Preparation method of cobalt containing silicon carbide fiber |
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| CN105442098A (en) * | 2015-12-31 | 2016-03-30 | 东华大学 | Preparation method of ductile SiO2 aerogel fiber coated with PVP (polyvinylpyrrolidone) |
| CN105442098B (en) * | 2015-12-31 | 2018-01-02 | 东华大学 | A kind of toughness SiO of PVP coatings2The preparation method of airsetting glue fiber |
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| CN106567156B (en) * | 2016-11-08 | 2019-06-18 | 华南理工大学 | The silica three-dimensional fiber material and preparation method thereof of cobalt load |
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| CN106607095B (en) * | 2017-01-03 | 2019-03-01 | 重庆理工大学 | The method that evaporation-induced self-assembly prepares magnetic hierarchical porous structure composite material |
| CN111187424A (en) * | 2020-02-14 | 2020-05-22 | 山东大学 | Lanthanide rare earth-organic polymer precursor, lanthanide rare earth oxide fiber, and preparation method and application thereof |
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