CN103551094B - Preparation method of core-shell structured Fe3O4@MCM-41 magnetic nano material - Google Patents
Preparation method of core-shell structured Fe3O4@MCM-41 magnetic nano material Download PDFInfo
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- CN103551094B CN103551094B CN201310594852.3A CN201310594852A CN103551094B CN 103551094 B CN103551094 B CN 103551094B CN 201310594852 A CN201310594852 A CN 201310594852A CN 103551094 B CN103551094 B CN 103551094B
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Abstract
The invention provides a preparation method of a core-shell structured Fe3O4@MCM-41 magnetic nano material, and relates to a method for synthesizing Fe3O4 magnetic nano material from a vesicle phase. The preparation method of the core-shell structured Fe3O4@MCM-41 magnetic nano material aims to solve the problems of uneven core-shell structure and small specific surface area of the magnetic nano material. The preparation method comprises the following steps of: 1, preparing a vesicle phase solution from hexadecyl trimethyl ammonium bromide and sodium dodecyl benzene sulfonate; 2, dissolving FeCl3 and FeSO4 in secondary distilled water, and then adding the vesicle phase solution to the obtained iron salt solution, adding quadrol to adjust the pH value of the system after ultrasonic treatment to obtain a black suspension; and 3, adding hexadecyl trimethyl ammonium bromide and TEOS (Tetra Ethyl Ortho Silicate) to the black suspension, carrying out a crystallization reaction after pH adjustment, washing and drying the solid-phase crystals and then roasting the solid-phase crystals to obtain the magnetic nano material. The preparation method of the core-shell structured Fe3O4@MCM-41 magnetic nano material is characterized in that the vesicles formed by compounding an anionic surfactant with a cationic surfactant are taken as micro-reactors, the thermodynamic performance of the system is stable, and in the meantime, the specific surface area of the magnetic nano material is large.
Description
Technical field
The present invention relates to a kind of vesica and be combined to Fe
3o
4the method of magnetic Nano material.
Background technology
Magnetic nano-particle has wide application space in research fields such as magnetic fluid, drug targeting release, catalysis, medical imaging, treatment of cancer, isolation technics, biochemical microreactor design and spectral detection.But pure magnetic nano-particle due to himself unstability, difficult to modify, high chemism and the shortcoming such as oxidizable be difficult to realize industrial applications.In order to solve this difficult problem, researcher passes through, at the different parcel shell of magnetic nano-particle surface construction, so as to reducing its agglomeration, to improve the stability of magnetic nano-particle to a great extent.Therefore the research of magnetic core-shell structure nano particle becomes a focus of technical field of material chemistry in recent years.
Common Shell Materials has metal material (gold, silver), and Inorganic Non-metallic Materials (silicon, carbon) and organic material (surfactant, polymer) etc., researcher can build suitable magnetic core-shell nano particle according to different Research Requirements.The magnetic silicon oxide of nucleocapsid structure, because of the magnetic response ability of the function uniqueness of its compound kernel and shell, hypotoxicity and surface chemical modification, gives it at the great application potential of every field.Bibliographical information in recent years about magnetic core-shell structural silica dioxide microballoon is more, particle size generally between 200-500nm, favorable dispersibility in specific solvent.The preparation method of hud typed material is a lot, main Problems existing is that the target product free degree is large, the yardstick of wayward nano particle, pattern, the defect of the uneven first-class aspect of coated shell structurre, this just makes researcher seek new breakthrough in synthetic method.
The composite system of cationic-anionic surfactants (C-A), due to its with opposite charges ion head base between strong electrostatic interaction, there is strong cooperative effect and high surface, abundant microstructure can be formed in aqueous, show complicated phase behavior, all have specific characteristics in the impact of, temperature charged on adsorption, surface and ionic strength effects on surface character and Micelle formation etc.The composite system of C-A can form spherical, bar-shaped, worm shape micella in aqueous, stratiform, sheet, plate-like, band shape, six sides, cubic liquid crystal phase, vesica, precipitation etc.Wherein vesica is the interested especially a kind of microstructures of people, and reason is that it can be used as model, the pharmaceutical carrier and microreactor etc. of cell membrane, has broad application prospects in fields such as biology, pharmacy, material, catalysis.The vesica that positive and negative surfactant compound is formed is a kind of thermodynamic stable system, can be used for nano materials as microreactor.
Though vesica phase is the metastable state system of the spontaneous formation of surfactant, but still belongs to thermodynamic unstable system, along with the minor variations of external condition, interference, the system pH of such as foreign ion change, the rising etc. of temperature all can impel vesica phase transformation.Research shows, gradually heat cell foam system, and the process changed from gel state to liquid crystal state has appearred in the hydrocarbon chain in vesicle bilayer film, and now, system creates larger enthalpy change.This transition temperature is called phase transition temperature (phase transition temperature), and also someone is called chain melting temperatur (chain melting tmperature).Therefore the formation of vesica is the change of the product of external condition, external condition, is easy to mutual conversion between vesica and liquid crystalline phase, lamellar phase.
Summary of the invention
The present invention seeks to the Fe obtained to solve existing method
3o
4the problem that magnetic Nano material nucleocapsid structure is uneven and specific area is little, and nucleocapsid structure Fe is provided
3o
4the preparation method of MCM-41 magnetic Nano material.
Nucleocapsid structure Fe of the present invention
3o
4the preparation method of MCM-41 magnetic Nano material follows these steps to realize:
One, 1.0:(1.5 ~ 3.0 in molar ratio) softex kw (CTAB) and neopelex (SDBS) are dissolved in redistilled water, obtained anion/cation surfactant mixed liquor, anion/cation surfactant mixed liquor is left standstill 24 ~ 48h under 25 ~ 35 DEG C of conditions, obtains vesica phase solution;
Two, be that 2.0:1.0 is by FeCl in molar ratio
3and FeSO
4be dissolved in the redistilled water of letting nitrogen in and deoxidizing process, obtain iron salt solutions, in iron salt solutions, add the vesica phase solution of step one, to add pH value to 9 ~ 10 of ethylenediamine regulation system after 25 ~ 35 DEG C of ultrasonic 2 ~ 3h, obtain black suspension;
Three, in the black suspension of step 2, softex kw (CTAB) is added, ethyl orthosilicate (TEOS) is added again when stirring, drip pH to 11 ~ 12 that ammoniacal liquor regulates black suspension, reaction 5 ~ 7h, with 48 ~ 52 DEG C of crystallization 24 ~ 36h, collect solid crystalline, solid crystalline absolute ethyl alcohol and redistilled water filter washing to neutral, then white solid powder is obtained through vacuum drying, then white solid powder is put into muffle furnace with 548 ~ 552 DEG C of roasting 10 ~ 12h, obtain nucleocapsid structure Fe
3o
4mCM-41 magnetic Nano material.
The nucleocapsid structure Fe that the present invention obtains
3o
4the kernel of MCM-41 magnetic Nano material is ferroferric oxide magnetic nanocrystal body, and particle diameter is less than 100nm, and shell is the regular MCM-41 layer of texture structure, Fe
3o
4mCM-41 magnetic Nano material particle diameter is less than 200nm, and average pore size is 6.28nm.
The vesica phase that the present invention is formed by positive and negative surfactant, liquid crystalline phase are microreactor synthesis of nano oxide structure unit, and by regulation and control vesica phase morphology, formed liquid crystal templated, the Thermodynamically stable of system, the orderly self assembly realizing binary oxide nano super-lattice forms the homogeneous Fe of shell structurre
3o
4mCM-41 magnetic Nano material, the specific area of magnetic Nano material can reach 513.9m simultaneously
2/ g.
Accompanying drawing explanation
Fig. 1 is the nucleocapsid structure Fe that embodiment one obtains
3o
4the transmission electron microscope picture of MCM-41 magnetic Nano material;
Fig. 2 is the nucleocapsid structure Fe that embodiment two obtains
3o
4the transmission electron microscope picture of MCM-41 magnetic Nano material;
Fig. 3 is nucleocapsid structure Fe
3o
4the XRD figure of MCM-41 magnetic Nano material and contrast sample MCM-41, wherein a-contrast sample MCM-41 curve, b-nucleocapsid structure Fe
3o
4the curve of MCM-41 magnetic Nano material;
Fig. 4 is the nucleocapsid structure Fe that embodiment one obtains
3o
4the projection Electronic Speculum figure of MCM-41 magnetic Nano material;
Fig. 5 is the nucleocapsid structure Fe that embodiment two obtains
3o
4the high power projection Electronic Speculum figure of MCM-41 magnetic Nano material local;
Fig. 6 is the nucleocapsid structure Fe that embodiment two obtains
3o
4the N of MCM-41 magnetic Nano material
2the curve of adsorption-desorption figure, a-contrast sample MCM-41, b-nucleocapsid structure Fe
3o
4the curve of MCM-41 magnetic Nano material;
Fig. 7 is the nucleocapsid structure Fe that embodiment two obtains
3o
4the graph of pore diameter distribution of MCM-41 magnetic Nano material, the pore-size distribution of a-contrast sample MCM-41, b-nucleocapsid structure Fe
3o
4the pore-size distribution of MCM-41 magnetic Nano material;
Fig. 8 is nucleocapsid structure Fe
3o
4the VSM figure of MCM-41 magnetic Nano material, the nucleocapsid structure Fe that a-embodiment one obtains
3o
4the curve of MCM-41 magnetic Nano material, the nucleocapsid structure Fe that b-embodiment two obtains
3o
4the curve of MCM-41 magnetic Nano material.
Detailed description of the invention
Detailed description of the invention one: present embodiment nucleocapsid structure Fe
3o
4the preparation method of MCM-41 magnetic Nano material follows these steps to implement:
One, 1.0:(1.5 ~ 3.0 in molar ratio) softex kw (CTAB) and neopelex (SDBS) are dissolved in redistilled water, obtained anion/cation surfactant mixed liquor, anion/cation surfactant mixed liquor is left standstill 24 ~ 48h under 25 ~ 35 DEG C of conditions, obtains vesica phase solution;
Two, be that 2.0:1.0 is by FeCl in molar ratio
3and FeSO
4be dissolved in the redistilled water of letting nitrogen in and deoxidizing process, obtain iron salt solutions, in iron salt solutions, add the vesica phase solution of step one, to add pH value to 9 ~ 10 of ethylenediamine regulation system after 25 ~ 35 DEG C of ultrasonic 2 ~ 3h, obtain black suspension;
Three, in the black suspension of step 2, softex kw (CTAB) is added, ethyl orthosilicate (TEOS) is added again when stirring, drip pH to 11 ~ 12 that ammoniacal liquor regulates black suspension, reaction 5 ~ 7h, with 48 ~ 52 DEG C of crystallization 24 ~ 36h, collect solid crystalline, solid crystalline absolute ethyl alcohol and redistilled water filter washing to neutral, then white solid powder is obtained through vacuum drying, then white solid powder is put into muffle furnace with 548 ~ 552 DEG C of roasting 10 ~ 12h, obtain nucleocapsid structure Fe
3o
4mCM-41 magnetic Nano material.
Present embodiment adopts the vesica of the spontaneous formation of anionic-cationic surfactant mixed system to be microreactor, obtains the magnetic Nano kernel that yardstick is homogeneous, and adjustment solution morphology is formed liquid crystal templated, one-step synthesis nucleocapsid structure Fe
3o
4mCM-41 magnetic Nano material.
Detailed description of the invention two: present embodiment and detailed description of the invention one are 0.028 ~ 0.032mol/L unlike the total concentration of softex kw (CTAB) and neopelex (SDBS) in step one anion/cation surfactant mixed liquor.Other step and parameter identical with detailed description of the invention one.
Detailed description of the invention three: present embodiment and detailed description of the invention one or two are 0.25 ~ 0.32mol/L unlike the concentration of Fe ion in step 2 iron salt solutions.Other step and parameter identical with detailed description of the invention one or two.
Detailed description of the invention four: one of present embodiment and detailed description of the invention one to three add softex kw (CTAB) unlike step 3 in the black suspension in step 2, makes CTAB total concentration in black suspension be 0.05 ~ 0.06moL/L.Other step and parameter identical with one of detailed description of the invention one to three.
Detailed description of the invention five: one of present embodiment and detailed description of the invention one to four add ethyl orthosilicate unlike step 3 again when stirring, and the speed wherein stirred is 500 ~ 1000r/min.Other step and parameter identical with one of detailed description of the invention one to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention one to five add ethyl orthosilicate (TEOS) unlike step 3 again when stirring, and the addition of ethyl orthosilicate makes n(TEOS in black suspension): n(Fe)=(5.0 ~ 10.0): 1.0.Other step and parameter identical with one of detailed description of the invention one to five.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention one to six are carry out drying at 200 DEG C unlike the vacuum drying described in step 3.Other step and parameter identical with one of detailed description of the invention one to six.
Embodiment one: the present embodiment nucleocapsid structure Fe
3o
4the preparation method of MCM-41 magnetic Nano material follows these steps to implement:
One, the softex kw (CTAB) of 0.36g and the neopelex (SDBS) of 0.697g are dissolved in 100mL redistilled water, obtained anion/cation surfactant mixed liquor, anion/cation surfactant mixed liquor is left standstill 24h under 30 DEG C of conditions, obtains vesica phase solution;
Two, by 1.7g(0.01moL) FeCl
3and 0.76g(0.005moL) FeSO
4be dissolved in the redistilled water of letting nitrogen in and deoxidizing process, obtain iron salt solutions, in iron salt solutions, add the vesica phase solution of step one, to add the pH value to 10 of ethylenediamine regulation system after 30 DEG C of ultrasonic 3h, obtain black suspension;
Three, in the black suspension of step 2,6g softex kw (CTAB) is added, 20mL(0.08moL is added again in intensively stirred situation) ethyl orthosilicate (TEOS), drip the pH to 11 that ammoniacal liquor regulates black suspension, reaction 7h, with 50 DEG C of crystallization 24h, collect solid crystalline, solid crystalline absolute ethyl alcohol and redistilled water filter washing to neutral, then white solid powder is obtained through vacuum drying, then white solid powder is put into muffle furnace with 550 DEG C of roasting 10h, obtain nucleocapsid structure Fe
3o
4mCM-41 magnetic Nano material.
Embodiment two: the present embodiment and embodiment one add 30mL(0.13moL unlike step 3 in intensively stirred situation) ethyl orthosilicate.Other step and parameter identical with embodiment one.
To the nucleocapsid structure Fe obtained
3o
4the crystal formation of MCM-41 magnetic nano-particle and surface nature thereof are characterized by X-ray diffractometer (RigakuD/max-II, Japan Ricoh) and Fourier infrared spectrograph (PE1600, Perkin Elmer company of the U.S.) respectively; Domain size distribution adopts Malvern nanometer particle size analyzer (ZEN3600, Malvern Instrument Ltd. of Britain) to analyze; Pattern and microstructure adopt transmission electron microscope (H-7650 FDAC) to characterize; Chemical composition x-ray photoelectron power spectrum (250Xi, U.S. Thermo Fisher ESCALAB) is analyzed; The magnetic property of magnetic nano-particle adopts vibrating specimen magnetometer (HH-15, Nanjing Univ. Instrument Factory) to measure; And the aperture of magnetic nano particle sub-surface and hole area analyze with BEL-Cat specificity of catalyst analyzer (BELCAT-M, Dutch Ankersmid Co., Ltd).
The nucleocapsid structure Fe that embodiment one and embodiment two obtain
3o
4the transmission electron microscope picture of MCM-41 magnetic Nano material is shown in Fig. 1 and Fig. 2 respectively, the particle diameter of core-shell structure magnetic nano particle is generally within the scope of 80-200nm as we can see from the figure, and along with adding the increase outer casing thickness increase of TEOS amount, particle radii become large, and shell structurre is homogeneous.
Nucleocapsid structure Fe
3o
4as shown in Figure 3, the characteristic peak of contrast sample MCM-41 mesopore molecular sieve generally appears near 2 θ=2 ° the XRD figure of MCM-41 magnetic Nano material.Known by comparative analysis, a occurs that in 2 θ=2.42 ° diffraction maximum is the hexagonal mesoporous structure diffraction peak of MCM-41, and b occurs diffraction maximum in 2 θ=2.38 °, and peak position slightly offsets 0.4 ° to low-angle relative to former powder, and magnetic core-shell Fe is described
3o
4the shell of MCM-41 nanoparticle still remains the hexagonal mesoporous structure of rule, and wherein MCM-41 mesopore molecular sieve is prepared by the method related in 2005 " applied chemistry " the 4th phase " aluminium lanthanum modifies the synthesis of hexagonal mesoporous silica, sign and the catalytic performance in ethoxylation ".
Fe can be found out by the high multiple projection Electronic Speculum figure of Fig. 4 and Fig. 5
3o
4the surface of MCM-41 magnetic nano-particle has mesoporous framework, and pore distribution is even, and have Hexagonal array crystal structure, as shown in Figure 5, magnetic nano-particle has clear striped, consistent with XRD result.
The means of testing that BET characterizes as mesoporous material, not only can pass through sample adsorption N
2content is how many and obtain the value of specific area, can also obtain the data of aperture, pore volume and pore passage structure type aspect, and the relation between the stuctures and properties of therefore mesoporous material can obtain more deep analysis.The NOVA-2000e type physical adsorption appearance that this experiment have employed Kang Ta company of the U.S. carrys out definite kernel shell structure Fe
3o
4the aperture of MCM-41 magnetic nano particle subshell MCM-41, and the specific area calculating shell with BET equation.
Magnetic core-shell Fe
3o
4as shown in Figure 6, graph of pore diameter distribution as shown in Figure 7 for the isothermal nitrogen adsorption desorption curve of MCM-41 nano particle.According to the classification of IUPAC, the adsorpting type of this nano particle belongs to IV type.A is contrast sample MCM-41 mesopore molecular sieve curve, and specific area is 966.9m
2/ g, pore volume is 0.5636mL/g, and aperture is 2.998nm; B is magnetic core-shell Fe
3o
4the shell MCM-41 curve of MCM-41 nano particle, specific area is 513.9m
2/ g, pore volume 0.307mL/g, aperture 6.281nm.Diminish from the shell MCM-41 specific area the known core-shell particles of above data, pore volume, aperture increases.
Fig. 8 is nucleocapsid structure Fe
3o
4the VSM figure of MCM-41 magnetic Nano material, as we know from the figure along with the increase of TEOS amount, Fe
3o
4the saturation magnetisation value of MCM-41 magnetic nano-particle reduces, and along with the addition of TEOS is from 20 ml to 30ml, saturation magnetisation value is reduced to 25emu/g from 33emu/g, does not have the Fe of coated MCM-41 shell
3o
4the saturation magnetisation value of nano particle is 54.19emu/g, the known coated Fe of shell data
3o
4mCM-41 nano particle saturation magnetisation value weakens, and along with the increase of thickness of the shell, the degree weakened strengthens, but still has certain magnetic response ability.
Claims (4)
1. nucleocapsid structure Fe
3o
4the preparation method of MCM-41 magnetic Nano material, is characterized in that nucleocapsid structure Fe
3o
4the preparation method of MCM-41 magnetic Nano material follows these steps to realize:
One, 1.0:(1.5 ~ 3.0 in molar ratio) softex kw and neopelex are dissolved in redistilled water, obtained anion/cation surfactant mixed liquor, anion/cation surfactant mixed liquor is left standstill 24 ~ 48h under 25 ~ 35 DEG C of conditions, obtains vesica phase solution;
Two, be that 2.0:1.0 is by FeCl in molar ratio
3and FeSO
4be dissolved in the redistilled water of letting nitrogen in and deoxidizing process, obtain iron salt solutions, in iron salt solutions, add the vesica phase solution of step one, to add pH value to 9 ~ 10 of ethylenediamine regulation system after 25 ~ 35 DEG C of ultrasonic 2 ~ 3h, obtain black suspension;
Three, softex kw is added in the black suspension of step 2, softex kw total concentration in black suspension is made to be 0.05 ~ 0.06moL/L, ethyl orthosilicate is added again when stirring, drip pH to 11 ~ 12 that ammoniacal liquor regulates black suspension, reaction 5 ~ 7h, with 48 ~ 52 DEG C of crystallization 24 ~ 36h, collect solid crystalline, solid crystalline absolute ethyl alcohol and redistilled water filtering and washing are to neutral, then white solid powder is obtained through vacuum drying, then white solid powder is put into Muffle furnace with 548 ~ 552 DEG C of roasting 10 ~ 12h, obtain nucleocapsid structure Fe
3o
4mCM-41 magnetic Nano material,
Wherein in step one anion/cation surfactant mixed liquor, the total concentration of softex kw and neopelex is 0.028 ~ 0.032mol/L.
2. nucleocapsid structure Fe according to claim 1
3o
4the preparation method of MCM-41 magnetic Nano material, is characterized in that the concentration of Fe ion in step 2 iron salt solutions is 0.25 ~ 0.32mol/L.
3. nucleocapsid structure Fe according to claim 1
3o
4the preparation method of MCM-41 magnetic Nano material, it is characterized in that step 3 adds ethyl orthosilicate again when stirring, the speed wherein stirred is 500 ~ 1000r/min.
4. nucleocapsid structure Fe according to claim 1
3o
4the preparation method of MCM-41 magnetic Nano material, is characterized in that the vacuum drying described in step 3 carries out drying at 200 DEG C.
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