CN103585955A - Preparation method of C/Fe3O4 porous nanometer coral ball composite material - Google Patents

Preparation method of C/Fe3O4 porous nanometer coral ball composite material Download PDF

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CN103585955A
CN103585955A CN201310574004.6A CN201310574004A CN103585955A CN 103585955 A CN103585955 A CN 103585955A CN 201310574004 A CN201310574004 A CN 201310574004A CN 103585955 A CN103585955 A CN 103585955A
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preparation
fe3o4
porous nano
coral ball
ball composite
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CN103585955B (en
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莫尊理
王博
张春
蒋彩弟
朱小波
赵国平
郭瑞斌
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Northwest Normal University
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Abstract

The invention provides a preparation method of a C/Fe3O4 porous nanometer coral ball composite material, and belongs to the technical field of nanometer materials. C/Fe3O4 nanometer particles in core shell structure are prepared through low-temperature carbonization of the traditional hydrothermal method by adopting cane sugar as a carbon source and Fe3O4 as an iron source; the coral composite material C/Fe3O4 with hole drapes on the surface is formed through low-temperature carbonization and acid etching by using small-particle Fe3O4 as pore forming agent. In the low-temperature carbonization process, the product particle size and the surface morphology can be controlled through changing the adding quantity of the carbon source, the carbonization time and the adding quantity of the pore forming agent. The coral composite material C/Fe3O4 prepared by the method has the advantages of no poison, no harm, strong biological affinity, large specific surface area, strong adsorption capacity and wide foreground in the application aspect of targeting drug carriers.

Description

A kind of C/Fe 3o 4the preparation method of porous nano coral ball composite
Technical field
The invention belongs to technical field of nano material, relate to a kind of C/Fe 3o 4the preparation method of nano composite material, relates in particular to a kind of C/Fe 3o 4the preparation method of porous nano coral ball composite.
Background technology
Along with magnetic target drugs with function carrier is incorporated into medical domain, the research of targeting pharmaceutical carrier is more and more subject to people's concern and attention.In cancer patient's therapeutic process, medicine can kill cancer cell, but is applied to each position of health simultaneously, and the cell of health is also caused to infringement to a certain degree.The advantage that targeting drug material has is, compares it can control rapidly medication with conventional medicament, by externally-applied magnetic field, medicine removed.Medicine is discharged by kidney in vivo in time, and reduction medicine is piled up the time in vivo, reduces danger.The pharmaceutical carrier with magnetic particle, can directly show by technology such as nuclear-magnetisms, can control intuitively pharmaceutical carrier, operates more accurate.
Spherical carbon back Fe 3o 4composite, as pharmaceutical carrier, has the advantage of the following aspects: spherical hypergeometric surface area, high drug load are faster for absorption and the rate of release of medicine; Fe 3o 4nano particle has good magnetic, to organism nonhazardous, and can utilize magnetic feature to control medication; Carbon material surface is coated, and protection tri-iron tetroxide, not by organism inner acidic environmental corrosion, makes carrier have more stability.Experiment shows, spherical carbon back Fe 3o 4composite is as pharmaceutical carrier, and its specific area is larger, and the adsorbance of medicine is larger, and drug releasing rate is faster, therefore, prepares a kind of carbon back Fe 3o 4the spherical composite of coral, carries acting body aspect as targeted drug and has a good application prospect.
Summary of the invention
The object of this invention is to provide a kind of C/Fe 3o 4the preparation method of porous nano coral ball composite.
One, C/Fe 3o 4the preparation of porous nano coral ball composite
C/Fe of the present invention 3o 4the preparation method of porous nano coral ball composite, comprises following processing step:
1, spherical nanometer C/Fe 3o 4preparation
By FeCl 36H 2o and anhydrous sodium acetate are fully dissolved in ethylene glycol with the mass ratio of 1:2.5～1:3.0, in 190～200 ℃ of reaction 8～10h; Black product, by washing for several times with distilled water, ethanol after Magnetic Isolation, obtains Fe 3o 4nano particle; Again by Fe 3o 4nano particle joins in sucrose solution, mechanical agitation 20～30min, ultrasonic processing 10～20min; Then carburizing reagent 4～5h under the condition of 150～160 ℃, makes the spherical nanometer C/Fe of nucleocapsid structure 3o 4.The concentration of above-mentioned sucrose solution is 50～70g/L; In sucrose solution, sucrose and FeCl 36H 2the mass ratio of O is 1:0.9～1:1.5.
2, small particle diameter Fe 3o 4preparation
By FeCl 36H 2o and FeSO 47H 2o is dissolved in distilled water with the mass ratio of 1:0.5～1:1.6, and mechanical agitation 10～20min slowly adds ammoniacal liquor, generates black precipitate; Use magnet precipitation and separation, after washing for several times, ultrasonic 10～20min makes the Fe of shape irregularity 3o 4nano particle disperses completely, obtains the Fe that particle diameter is not more than 30nm 3o 4nano particle.The concentration of above-mentioned ammoniacal liquor is 35～75g/L; Ammoniacal liquor and FeCl 36H 2o/FeSO 47H 2o total mass ratio is 1:0.5～1:2.0.
3, C/Fe 3o 4the preparation of porous nano coral ball
By above-mentioned small particle diameter Fe 3o 4nano particle and spherical nanometer C/Fe 3o 4mass ratio with 1:0.6～1:0.8 joins in sucrose solution, mechanical agitation 20～30min, ultrasonic processing 20～30min, then carburizing reagent 4～5h under the condition of 140～150 ℃; Carbonized product with distilled water washing for several times, immerses standing 24～48h in nitration mixture, makes target product C/Fe 3o 4porous nano coral ball.The concentration of described sucrose solution is 50～70g/L; In sucrose solution, the quality of sucrose and small particle diameter Fe 3o 4nano particle, spherical nanometer C/Fe 3o 4the ratio of gross mass is 1:2.0～1:3.0.
Consisting of of described nitration mixture: 2～5mL concentrated sulfuric acid, 0.2～0.5gNaNO 3, 0.5～1gKMnO 4carry out proportioning.
Two, C/Fe 3o 4the pattern of porous nano coral ball composite
Below by ESEM, transmission electron microscope, XRD, infrared spectrogram, thermogravimetric analysis, BET, analyze C/Fe prepared by the present invention 3o 4structure and the pattern of porous nano coral ball composite carry out analytic explanation.
1, electronic microscope photos
Fig. 1 is C/Fe prepared by the present invention 3o 4the Electronic Speculum figure of porous nano coral ball composite under different multiplying.Wherein Fig. 1 a records C/Fe under 100,000 times of conditions 3o 4the scanning electron microscope (SEM) photograph of porous nano coral ball composite.From Fig. 1 a, can see C/Fe 3o 4the chondritic of porous nano coral ball is obvious, and is coralliform stacked arrangement, and particle diameter is generally at 200～280nm.Fig. 1 c records C/Fe under 200,000 times of conditions 3o 4the scanning electron microscope (SEM) photograph of porous nano coral ball composite.As seen from Figure 2. the aperture in chondritic, pore shape irregularity, this is owing to utilizing interface legal system for Fe 3o 4when (～30nm), drip ammoniacal liquor at the Fe of generation of interfaces 3o 4out-of-shape causes.Chondritic surface pore fold phenomenon is obvious, and hole fold diameter is between 4～6nm.
Fig. 1 b is 200,000 times of C/Fe under condition 3o 4the transmission electron microscope picture of porous nano coral ball composite.As can be seen from the figure, C/Fe 3o 4porous nano coral ball composite presents nucleocapsid structure: Fe 3o 4in core is coated on completely by carbon-coating, surperficial burr show that carbon-coating surface exists obvious hole pleated structure, and this point is mutually corresponding with SEM.Fig. 1 d is single C/Fe 3o 4the transmission electron microscope figure of porous nano coral ball composite.Can find out C/Fe 3o 4composite material surface burr are many and close, and C/Fe is described 3o 4porous nano coral ball composite material surface hole pleated structure close-packed arrays, this point is corresponding with ESEM.
2, infrared analysis
Fig. 2 is respectively Fe 3o 4nano particle and C/Fe 3o 4the infrared spectrum of porous nano coral ball composite.579cm in figure -1there is stronger Fe-O key vibrations peak in place; At 1591cm -1and 1690cm -1be respectively the vibrations peak of C=C and C=O; At 3398cm -1place is hydroxyl vibration peak; C/Fe 3o 4the relative Fe of porous nano coral ball composite material line 3o 4nano particle line possesses more functional group peak, but due to low-temperature carbonization reaction, the thinner infrared spectrum analysis of carbon layer on surface is slightly not obvious, but its still can show compound after at Fe 3o 4by carbon-coating, be coated togather.
3, VSM analyzes
Fig. 3 is Fe under room temperature 3o 4nano particle (a) and C/Fe 3o 4the hysteresis curve figure of porous nano coral ball composite (b).Visible, C/Fe 3o 4porous nano coral ball composite shows typical superparamagnetic structure, and coercivity and residual magnetism can be ignored.Due to low-temperature carbonization course of reaction, Fe 3o 4the coated one deck carbon in surface, covers Fe 3o 4part magnetic, make Fe 3o 4the saturation magnetization of core is reduced to 18.16emu/g by 46.23emu/g, and this shows Fe 3o 4nanoparticle surface is coated by carbon-coating.
4, thermogravimetric analysis
Fig. 4 is C/Fe 3o 4the hot weightless picture of porous nano coral ball composite.The de-mistake that in figure, 30～150 ℃ is moisture, due to C/Fe 3o 4porous nano coral ball composite is prepared by the method for acid etching, has large amount of organic functional group on surface; 150～480 ℃ is surface organic matter decomposition weightlessness; Curve 480～700 ℃ all the time phenomenon to be that carbon layer on surface decomposes weightless, what curve became subsequently is smooth, shows residual F e 3o 4existence.C/Fe in curve and document in Fig. 5 3o 4spherical porous nanometer material is similar, also shows that product is successfully prepared.
5, X-ray diffraction analysis
Fig. 5 is C/Fe 3o 4the contrast spectrogram of the XRD of porous nano coral ball composite.Fig. 5 a is Fe 3o 4nano particle, its characteristic peak mainly appears at 2 θ=29.91 °, 35.41 °, 43.11 °, locates, shows Fe for 57.21 ° and 62.81 ° 3o 4nano particle is good cubic spinel magnet structure.Fig. 5 b is C/Fe 3o 4the XRD of porous nano coral ball composite, ° wider peak of increase by 2 θ=20.55, and do not observe other obvious peaks.Show that carbonized structure is unformed structure.On image, significantly observe and contain and C and Fe 3o 4the similar peak value of nano flower, this shows that carbonization is a coated process, Fe 3o 4nano flower surface is being coated unformed carbon.
6, BET analyzes
In Fig. 6,7, be respectively C/Fe 3o 4the nitrogen adsorption desorption isotherm figure (BET) of porous nano coral ball composite and pore size distribution curve figure (BJH).The IV type isotherm plots that the adsorption isotherm of Fig. 6 presents, and present H3 type hysteresis loop, according to determining of IUPAC (IUPAC), in material, there is the gap structure of 2～50 nanometers to exist.In addition, can significantly find out the higher relative pressure of hysteresis loop tendency deflection, show that the space that has size to be greater than 50nm exists.Aperture can not be by nitrogen at 100～150nm the analytical method of adsorption/desorption learn.Fig. 7 is for to record C/Fe by BJH method 3o 4relation between the average pore size of porous nano coral ball composite and pore volume.Fig. 7 shows that aperture is maximum at the pore volume of 4～6nm.According to Fig. 6,7, obtain C/Fe 3o 4specific area, aperture, the pore volume of porous nano coral ball composite are respectively 185.2～192.01m 2g -1, 6.08～7.44nm, 0.293～0.313cm 3/ g, these features make C/Fe 3o 4porous nano coral ball composite has application prospect at Drug absorbability targeting carrier.
The present invention has the following advantages with respect to prior art:
1, the present invention adopts sucrose as carbon source, with Fe 3o 4for source of iron, by traditional hydro-thermal method low-temperature carbonization, make nucleocapsid structure C/Fe 3o 4nano particle, and utilize small particle diameter Fe 3o 4as pore creating material, by low-temperature carbonization, acid etching forms the coralliform composite C/Fe that surface band has hole fold 3o 4, it is nontoxic, biocompatible ability is strong, and specific area is large, high adsorption capacity, in targeting pharmaceutical carrier application aspect, has prospect;
2, the present invention adopts hydrothermal reaction at low temperature to prepare C/Fe 3o 4porous nano coral ball composite, reaction temperature is low, and covered effect is good, surface uniform; In low-temperature carbonization process, by change add carbon source amount, reaction time, add the conditions such as pore-creating dosage, can realize particle diameter and the surface topography of product;
3, the present invention is with low cost, and preparation technology is simple, and reaction condition is gentle, and convenient and reliable operation, is easy to industrialization.
Accompanying drawing explanation
Fig. 1 is the C/Fe under different multiplying 3o 4the Electronic Speculum figure of porous nano coral ball composite.
Fig. 2 is that hydro-thermal method is prepared Fe 3o 4core and C/Fe 3o 4porous nano coral ball composite infrared spectrum.
Fig. 3 is that hydro-thermal method is prepared Fe 3o 4core and C/Fe 3o 4the hysteresis curve figure of porous nano coral ball composite.
Fig. 4 is C/Fe 3o 4porous nano coral ball composite is at 25～1000 ℃, 10 ℃/min, N 2thermogravimetric analysis figure under protection.
Fig. 5 is pure Fe 3o 4nanosphere (a) and C/Fe 3o 4the XRD analysis figure of porous nano coral ball composite (b).
Fig. 6 is C/Fe 3o 4the nitrogen adsorption desorption isotherm figure of porous nano coral ball composite.
Fig. 7 is C/Fe 3o 4the pore size distribution curve figure of porous nano coral ball composite.
The specific embodiment
Below by specific embodiment to C/Fe of the present invention 3o 4preparation, structure, the pattern of porous nano coral ball composite are further described.
Embodiment mono-
(1) Fe 3o 4(200nm) preparation of nano particle: by 0.675gFeCl 36H2O mixes and adds 35mL ethylene glycol with 1.8g anhydrous sodium acetate, keep 200 ℃ of reactions 8～10 hours after evenly mixing in reactor, by black in reactor distilled water, ethanol washing several product for, obtains Fe 3o 4(200nm) nano particle.
(2) spherical C/Fe 3o 4preparation: take 0.5g sucrose and be dissolved in 20mL distilled water, by sucrose solution and Fe 3o 4(200nm) nano particle mixes, mechanical agitation 20～30min, ultrasonic processing 10～20min.Mixed liquor is put into reactor and is kept 155 ℃ of temperature, and carburizing reagent makes spherical C/Fe for 4 hours 3o 4.
(3) pore creating material Fe 3o 4(30nm) preparation of nano particle: by 0.27gFeCl 36H 2o and 0.14gFeSO 47H 2o mixing is dissolved in 50mL distilled water, and mechanical agitation 20min, slowly drips 10mL(36g/L in solution surface) ammoniacal liquor, generate black precipitate, with magnet separated and washing by black precipitate, ultrasonic 20min makes the Fe of shape irregularity 3o 4nano particle disperses completely, makes Fe 3o 4(30nm) nano particle.
(4) C/Fe 3o 4the preparation of porous nano coral ball: take 0.5g sucrose and be dissolved in 20mL distilled water, add above-mentioned 0.83gFe 3o 4(30nm) nano particle and 0.6gC/Fe 3o 4nanosphere, mechanical agitation 20～30min, ultrasonic processing 20～30min, puts into reactor and keeps 145 ℃ of temperature, carburizing reagent 4 hours; Carbonized product is taken out with distilled water washing for several times, add nitration mixture (2～5mL concentrated sulfuric acid, 0.5gNaNO 3, 1gKMnO 4) standing 24～48 hours, make C/Fe 3o 4porous nano coral ball.Particle size were 200～240nm, surface pore fold comparatively dense.
Embodiment bis-
(1) Fe 3o 4(200nm) preparation of nano particle: with embodiment 1.
(2) spherical C/Fe 3o 4preparation: with embodiment 1.
(3) pore creating material Fe 3o 4(30nm) preparation of nano particle: drip 10mL(54g/L) ammoniacal liquor, the other the same as in Example 1.
(4) C/Fe 3o 4the preparation of porous nano coral ball: the carburizing reagent time is 4.5h, the other the same as in Example 1.Make C/Fe 3o 4porous nano coral ball particle size were 220～260nm, surface pore fold is intensive.
Implement three
(1) Fe 3o 4(200nm) preparation of nano particle: with embodiment 1.
(2) spherical C/Fe 3o 4preparation: the other the same as in Example 1.
(3) pore creating material Fe 3o 4(30nm) preparation of nano particle: add 10mL(72g/L) ammoniacal liquor, the other the same as in Example 1.
(4) C/Fe 3o 4the preparation of porous nano coral ball: dosage of sucrose is 0.55g, the carburizing reagent time is 5h, the other the same as in Example 1.Finally make C/Fe 3o 4particle diameter 240～the 280nm of porous nano coral ball, surface pore fold is intensive.
Embodiment tetra-
(1) Fe 3o 4(200nm) preparation of nano particle: with embodiment 1.
(2) spherical C/Fe 3o 4preparation: dosage of sucrose 0.55g, the carburizing reagent time is 4.5h, the other the same as in Example 1.
(3) pore creating material Fe 3o 4(30nm) preparation of nano particle: FeCl 36H 2the consumption 0.41g of O, FeSO 47H 2the consumption of O is 0.14g, drips 10mL(54g/L) ammoniacal liquor, the other the same as in Example 1.
(4) C/Fe 3o 4the preparation of porous nano coral ball: the other the same as in Example 1.Finally make C/Fe 3o 4porous nano coral ball.Particle size were 220～260nm, surface pore fold is tight.
Embodiment five
(1) Fe 3o 4(200nm) preparation of nano particle: with embodiment 1.
(2) spherical C/Fe 3o 4preparation: dosage of sucrose is 0.6g, and the carburizing reagent time is 5h, the other the same as in Example 1.
(3) pore creating material Fe 3o 4(30nm) preparation of nano particle: FeCl 36H 2o consumption is 0.54g, FeSO 47H 2o consumption is 0.14g, drips 10mL(72g/L) ammoniacal liquor, the other the same as in Example 1.
(4) C/Fe 3o 4the preparation of porous nano coral ball: dosage of sucrose is 0.6g, the carburizing reagent time is 4.5 hours, the other the same as in Example 1.Finally make C/Fe 3o 4porous nano coral ball.Particle size were 240～280nm, surface pore fold comparatively dense.

Claims (5)

1. a C/Fe 3o 4the preparation method of porous nano coral ball composite, comprises following processing step:
(1) spherical nanometer C/Fe 3o 4preparation
By FeCl 36H 2o and anhydrous sodium acetate are fully dissolved in ethylene glycol with the mass ratio of 1:2.5 ~ 1:3.0, in 190 ~ 200 ℃ of reaction 8 ~ 10h; Black product, by washing for several times with distilled water, ethanol after Magnetic Isolation, obtains Fe 3o 4nano particle; Again by Fe 3o 4nano particle joins in sucrose solution, mechanical agitation 20 ~ 30min, ultrasonic processing 10 ~ 20min; Then carburizing reagent 4 ~ 5h under the condition of 150 ~ 160 ℃, makes the spherical nanometer C/Fe of nucleocapsid structure 3o 4;
(2) small particle diameter Fe 3o 4preparation
By FeCl 36H 2o and FeSO 47H 2o is dissolved in distilled water with the mass ratio of 1:0.3 ~ 1:0.6, and mechanical agitation 10 ~ 20min slowly adds ammoniacal liquor, generates black precipitate; Use magnet precipitation and separation, washing is for several times to remove residual ammoniacal liquor in solution, and ultrasonic 10 ~ 20min makes the Fe of shape irregularity 3o 4nano particle disperses completely, finally obtains the Fe that particle diameter is not more than 30nm 3o 4nano particle;
(3) C/Fe 3o 4the preparation of porous nano coral ball
By above-mentioned small particle diameter Fe 3o 4nano particle and spherical nanometer C/Fe 3o 4mass ratio with 1:0.6 ~ 1:0.8 joins in sucrose solution, mechanical agitation 20 ~ 30min, ultrasonic processing 20 ~ 30min, then carburizing reagent 4 ~ 5h under the condition of 140 ~ 150 ℃; Carbonized product with distilled water washing for several times, immerses standing 24 ~ 48h in nitration mixture, makes target product C/Fe 3o 4porous nano coral ball.
2. C/Fe as claimed in claim 1 3o 4the preparation method of porous nano coral ball composite, is characterized in that: the concentration of step (1) sucrose solution is 50 ~ 70g/L; In sucrose solution, sucrose and FeCl 36H 2the mass ratio of O is 1:0.9 ~ 1:1.5.
3. C/Fe as claimed in claim 1 3o 4the preparation method of porous nano coral ball composite, is characterized in that: in step (2), the concentration of ammoniacal liquor is 35 ~ 75g/L; Ammoniacal liquor and FeCl 36H 2o/FeSO 47H 2o total mass ratio is 1:0.5 ~ 1:2.0.
4. C/Fe as claimed in claim 1 3o 4the preparation method of porous nano coral ball composite, is characterized in that: the concentration of the sucrose solution of step (3) is 50 ~ 70g/L; In sucrose solution, the quality of sucrose and small particle diameter Fe 3o 4nano particle, spherical nanometer C/Fe 3o 4the ratio of gross mass is 1:2.0 ~ 1:3.0.
5. C/Fe as claimed in claim 1 3o 4the preparation method of porous nano coral ball composite, is characterized in that: in step (3), and the consisting of of described nitration mixture: 2 ~ 5mL concentrated sulfuric acid, 0.2 ~ 0.5gNaNO 3, 0.5 ~ 1gKMnO 4.
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CN112657476A (en) * 2021-01-11 2021-04-16 西北师范大学 Preparation of PEI-PAN-Ppy core-shell structure nanofiber membrane and application of PEI-PAN-Ppy core-shell structure nanofiber membrane in adsorption of chromium ions

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Cited By (7)

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CN103825019A (en) * 2014-02-21 2014-05-28 浙江大学 Fe3O4/C composite material, its preparation method and its application in lithium ion battery
CN105155002A (en) * 2015-07-09 2015-12-16 长春理工大学 Nanometer cable with three functions of conduction, magnetism and absorption and preparation method for same
CN106587095A (en) * 2016-12-21 2017-04-26 西北师范大学 Ordered mesoporous MCM-41 molecular sieve/ferroferric oxide nanocomposite and preparation method thereof
CN109464981A (en) * 2018-09-30 2019-03-15 天津大学 Magnetic Nano material preparation method uses the magnetic Nano material for the method for Simulation moving bed stationary phase Separation of boron isotopes
CN109908866A (en) * 2019-03-28 2019-06-21 中国科学院兰州化学物理研究所 The method and its application of two-dimensional magnetic porous carbon composite are prepared by calcining
CN109908866B (en) * 2019-03-28 2021-12-31 中国科学院兰州化学物理研究所 Method for preparing two-dimensional magnetic porous carbon composite material through calcination and application thereof
CN112657476A (en) * 2021-01-11 2021-04-16 西北师范大学 Preparation of PEI-PAN-Ppy core-shell structure nanofiber membrane and application of PEI-PAN-Ppy core-shell structure nanofiber membrane in adsorption of chromium ions

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