CN104276607B - Prepare the method for wustite nano flake - Google Patents

Prepare the method for wustite nano flake Download PDF

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CN104276607B
CN104276607B CN201410494120.1A CN201410494120A CN104276607B CN 104276607 B CN104276607 B CN 104276607B CN 201410494120 A CN201410494120 A CN 201410494120A CN 104276607 B CN104276607 B CN 104276607B
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fused salt
divalent metal
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CN104276607A (en
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娄正松
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Jiangsu University of Technology
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Abstract

The invention discloses a kind of method preparing wustite nano flake, bivalent metallic compound as raw material, the ferric iron compound as raw material, the sodium-chlor as fused salt and the Repone K as fused salt are ground, mix, mixture is positioned in crucible, again crucible is put into tube furnace, be warming up to 800 DEG C ~ 880 DEG C roasting 4h ~ 6h, obtain nano ferrite through aftertreatment; The mol ratio of described raw material and described fused salt is 3: 11y, wherein 13≤y≤50, and obtained nano ferrite is wustite nano flake; Divalent metal in described raw material and ferric mol ratio are x: 3-x, wherein 0.01≤x≤1; Sodium-chlor in described fused salt and the mol ratio of Repone K are 10: 1.Method equipment of the present invention is simple, and the reaction times is short, and energy consumption is low, environmental friendliness, and cost is lower, and product type is enriched, and is suitable for suitability for industrialized production.

Description

Prepare the method for wustite nano flake
The application is application number is 201210499432.2, and the applying date is on November 29th, 2012, and invention and created name is the divisional application of the application for a patent for invention of " method that molten-salt growth method prepares nano ferrite ".
Technical field
The present invention relates to a kind of preparation method of wustite, be specifically related to a kind of method that molten-salt growth method prepares nano ferrite.
Background technology
Spinel type wustite has been widely used in mutual inductance device, magnetic recording material as a kind of soft magnetic material.At present, along with the development of technology, the practical ranges of spinel type wustite is also increasingly extensive, such as, as catalyzer, can be applied in the oxidation deoxygenation of synthetic ammonia, butylene.It is found that, after the size of material reaches nanometer range, there will be and body phase material different properties, such as, Japan Kobe university uses wustite nanometer ball as the carrier of medicine, and Hepatoma therapy, kidney succeed.This shows that the carrier that wustite can be used as cancer therapy drug has good prospect in medical.Therefore, the synthesis of novel Ferrite Nanocrystalline Materials and character research become study hotspot widely.
A few days ago, the existing research to the synthesis of spinel type wustite is mainly on nano magnetic microballoon both at home and abroad, and its preparation method mainly contains Physical and the large class of chemical method two.
Physical mainly adopt high energy mechanical grind make presoma react generate needed for nanocrystalline, presoma is generally two kinds of corresponding oxide compounds of metal, prepares corresponding wustite.The advantage of Physical is that technique is simple, and chemical constitution easily controls.Shortcoming is then consume energy comparatively greatly, and long reaction time, particularly easily introduces impurity, and dispersiveness is good not.
Chemical method mainly makes the uniform ion of reactant mix by chemical reaction, obtains the granular product of nano-scale at a certain temperature, as hydrothermal method or solvent-thermal method (as Chinese patent literature CN1645530A, CN102583567A etc.).The advantage of chemical method is that particle size is less, and pattern is homogeneous.Shortcoming is then that the crystallinity of product is bad, and needs organic solvent and tensio-active agent, so not only adds cost but also easily causes environmental pollution.
Summary of the invention
The object of the invention is to solve the problem, provide that a kind of equipment is simple, the reaction times is short, energy consumption is low, environmental friendliness, cost are lower, product type is enriched, be suitable for the method that the molten-salt growth method of suitability for industrialized production prepares nano ferrite.
The technical scheme realizing the object of the invention is: a kind of molten-salt growth method prepares the method for nano ferrite, it is ground the bivalent metallic compound as raw material, the ferric iron compound as raw material, the sodium-chlor as fused salt and the Repone K as fused salt, mix, mixture is positioned in crucible, again crucible is put into tube furnace, be warming up to 800 DEG C ~ 880 DEG C roasting 4h ~ 6h, obtain nano ferrite through aftertreatment.
The mol ratio of described raw material and described fused salt is 3: 11y, wherein 0.6≤y≤50; Divalent metal in described raw material and ferric mol ratio are x: 3-x, wherein 0.01≤x≤1; Sodium-chlor in described fused salt and the mol ratio of Repone K are 10: 1.
Described ferric iron compound is ferric oxide, ironic hydroxide, iron nitrate, ironic acetate, ironic oxalate or iron carbonate.
Described bivalent metallic compound is bivalent metal oxide, Divalent metal hydroxide, divalent metal nitrate, divalent metal acetate, divalent metal oxalate or bivalent metal carbonate.
Described divalent metal is one in magnesium, nickel, copper, cadmium, calcium, strontium, barium, zinc, manganese or two kinds.
Or described divalent metal is one in lead, cobalt, tin or two kinds, in preparation process, before intensification roasting, passes into rare gas element in tube furnace.
Aforesaid method can according to the different nano ferrites that obtain different-shape of raw material from the mol ratio of fused salt: as 0.6≤y < 13, obtained nano ferrite is wustite nanometer ball.When 13≤y≤50, obtained nano ferrite is wustite nano flake.
And aforesaid method can obtain the nano ferrite of different composition according to the quantity of divalent metal in raw material and the different of ferric mol ratio and divalent metal.Specific as follows:
(1) when only having a kind of divalent metal and divalent metal and ferric mol ratio are 1: 2, then obtain consisting of MFe 2o 4nano ferrite, wherein M represents divalent metal.
Generate oxide compound because oxyhydroxide, nitrate, acetate, oxalate, carbonate etc. at high temperature decompose, therefore above-mentioned chemical reaction is expressed as follows:
MO (s)+Fe 2O 3(s)+NaCl+KCl→MFe 2O 4(s)。
(2) when only having a kind of divalent metal and divalent metal and ferric mol ratio are x: 3-x (0.01≤x < 1), then obtain consisting of M xfe 3-xo 4nano ferrite, wherein M represents divalent metal.
Above-mentioned chemical reaction is expressed as follows:
xMO (s)+(3-x)/2Fe 2O 3(s)+NaCl+KCl→M xFe 3-xO 4(s)。
(3) when there being two kinds of divalent metals, mole total amount of divalent metal and ferric mol ratio are 1: 2, and when the mol ratio between two kinds of divalent metals is x: 1-x (0.01≤x < 1), can obtain M 1 xm 2 1-xfe 2o 4nano ferrite, wherein M 1, M 2represent different divalent metals.
Above-mentioned chemical reaction is expressed as follows:
xM 1O (s)+(1-x)M 2O (s)+Fe 2O 3(s)+NaCl+KCl→M 1 xM 2 1-xFe 2O 4(s)。
(4) when there being two kinds of divalent metals, mole total amount of divalent metal and ferric mol ratio are x: 3-x(0.01≤x < 1), and the mol ratio between two kinds of divalent metals is when being m: x-m (0.01≤m < x), can obtain M 1 mm 2 x-mfe 3-xo 4nano ferrite, wherein M 1, M 2represent different divalent metals.
Above-mentioned chemical reaction is expressed as follows:
mM 1O (s)+(x-m)M 2O (s)+(3-x)/2Fe 2O 3(s)+NaCl+KCl→M 1 mM 2 x-mFe 3-xO 4(s)。
The positively effect that the present invention has: (1) the inventive method adopts sodium-chlor and Repone K (mol ratio is 10: 1) as fused salt, by heating fused salt, raw material is reacted in the environment of melting sodium-chlor and Repone K and can obtain nano ferrite in several hours, have that equipment is simple, easy and simple to handle, the reaction times is short, energy consumption is low, advantages of environment protection.(2) method of the present invention is by controlling the mol ratio of fused salt and raw material, not only can obtain wustite nanometer (magnetic bead) ball, wustite nano flake can also be obtained, thus also have that product type is abundant, excellent performance, steady quality, controllability strong, be suitable for the advantages such as suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the MgFe that embodiment 1 obtains 2o 4the x-ray diffraction pattern of nanometer ball.
Fig. 2 is the MgFe that embodiment 1 obtains 2o 4the field emission scanning electron microscope figure of nanometer ball.
Fig. 3 is Ni prepared by embodiment 3 0.6fe 2.4o 4the scanning electron microscope (SEM) photograph of nanometer ball Flied emission.
Fig. 4 is Mn prepared by embodiment 4 0.4zn 0.6fe 2o 4the scanning electron microscope (SEM) photograph of nanometer ball.
Fig. 5 is ZnFe prepared by embodiment 5 2o 4the scanning electron microscope (SEM) photograph of nano flake.
Fig. 6 is Mg prepared by embodiment 8 0.5ni 0.5fe 2o 4the scanning electron microscope (SEM) photograph of nano flake.
Embodiment
(embodiment 1)
The present embodiment is MgFe 2o 4the preparation method of nanometer ball:
Put 1mmol magnesium oxide, 2mmol iron nitrate, 100mmol sodium-chlor, the grinding of 10mmol Repone K, Homogeneous phase mixing, is positioned over mixture in alumina crucible, then alumina crucible is put into tube furnace, by the ramp to 820 DEG C of 5 DEG C/min, and roasting 4h.
Naturally cool to envrionment temperature (0 ~ 40 DEG C, lower same), distilled water dipping desalination, suction filtration, washing, 70 DEG C of dryings, obtained MgFe 2o 4nanometer ball.
This MgFe 2o 4the x-ray diffraction pattern of nanometer ball is shown in Fig. 1, as shown in Figure 1: the X-ray diffraction peak position of this product is consistent with standard X-ray diffraction card (JCPDS36-0398), proves that the present embodiment products therefrom is the MgFe of pure phase 2o 4powder.
This MgFe 2o 4the field emission scanning electron microscope figure of nanometer ball is shown in Fig. 2, and as shown in Figure 2: this product has spherical morphology, diameter is greatly about 700nm ~ 900nm, MgFe 2o 4the productive rate of nanometer ball is approximately 90wt%.
Control divalent metal and ferric mol ratio are 1: 2, the mol ratio of raw material and fused salt is 3: 11y(0.6≤y < 13), replace above-mentioned Mg with Ni, Cu, Cd, Ca, Sr, Ba, Zn, Mn etc. respectively, adopt identical method can obtain NiFe respectively 2o 4, CuFe 2o 4, CdFe 2o 4, CaFe 2o 4, SrFe 2o 4, BaFe 2o 4, ZnFe 2o 4, MnFe 2o 4deng wustite nanometer ball.
(embodiment 2)
The present embodiment is PbFe 2o 4the preparation method of nanometer ball:
Put 2mmol lead carbonate, 4mmol iron nitrate, 100mmol sodium-chlor, the grinding of 10mmol Repone K; Homogeneous phase mixing; mixture is positioned in alumina crucible; again alumina crucible is put into tube furnace; pass into rare gas element; under protection of inert gas, by the ramp to 840 DEG C of 5 DEG C/min, roasting 4h.
Naturally cool to envrionment temperature, flood desalination with distilled water, suction filtration, washing, 60 DEG C of dryings, obtained particle diameter is the PbFe of 800nm ~ 1000nm 2o 4nanometer ball.
Control divalent metal and ferric mol ratio are 1: 2, and the mol ratio of raw material and fused salt is 3: 11y(0.6≤y < 13), Pb is replaced to Co or Sn, adopts identical method can obtain CoFe respectively 2o 4, SnFe 2o 4nanometer ball.
(embodiment 3)
The present embodiment is Ni 0.6fe 2.4o 4the preparation method of nanometer ball:
Set to 0 .6mmol nickelous nitrate, the iron nitrate of 2.4mmol, 80mmol sodium-chlor, the grinding of 8mmol Repone K, Homogeneous phase mixing, is positioned over mixture in alumina crucible, then alumina crucible is put into tube furnace, by the ramp to 860 DEG C of 5 DEG C/min, roasting 6h.
Naturally cool to envrionment temperature, distilled water dipping desalination, suction filtration, washing, 60 DEG C of dryings, obtained Ni 0.6fe 2.4o 4nanometer ball.
This Ni 0.6fe 2.4o 4the field emission scanning electron microscope figure of nanometer ball is shown in Fig. 3, and as shown in Figure 3: this product has spherical morphology, diameter is greatly about 600nm ~ 1100nm, Ni 0.6fe 2.4o 4the productive rate of nanometer ball is approximately 80wt%.
Control divalent metal and ferric mol ratio are x: 3-x(0.01≤x < 1), the mol ratio of raw material and fused salt is 3: 11y(0.6≤y < 13), replace above-mentioned Ni with Mg, Cu, Cd, Ca, Sr, Ba, Zn, Mn etc. respectively, adopt identical method can obtain Mg respectively xfe 3-xo 4, Cu xfe 3-xo 4, Cd xfe 3-xo 4, Ca xfe 3-xo 4, Sr xfe 3-xo 4, Ba xfe 3-xo 4, Zn xfe 3-xo 4, Mn xfe 3-xo 4deng wustite nanometer ball.
(embodiment 4)
The present embodiment is Mn 0.4zn 0.6fe 2o 4the preparation method of nanometer ball:
Set to 0 .6mmol zinc nitrate, 0.4mmol manganous oxalate, 2mmol iron nitrate, 90mmol sodium-chlor, the grinding of 9mmol Repone K, Homogeneous phase mixing, is positioned over mixture in alumina crucible, then alumina crucible is put into tube furnace, by the ramp to 820 DEG C of 5 DEG C/min, roasting 6h.
Naturally cool to envrionment temperature, distilled water dipping desalination, suction filtration, washing, 80 DEG C of dryings, obtained Mn 0.4zn 0.6fe 2o 4nanometer ball.
This Mn 0.4zn 0.6fe 2o 4the scanning electron microscope (SEM) photograph of nanometer ball is shown in Fig. 4, and as shown in Figure 4: this product has spherical morphology, diameter is greatly about 500nm ~ 800nm, Mn 0.4zn 0.6fe 2o 4the productive rate of nanometer ball is approximately 80wt%.
Mole total amount and the ferric mol ratio that control divalent metal equal 1: 2, the mol ratio of raw material and fused salt is 3: 11y(0.6≤y < 13), adopt any two kinds of above-mentioned Zn and Mn of replacement in Mg, Ni, Cu, Cd, Ca, Sr, Ba, Zn, Mn, adopt same procedure can obtain corresponding acid ferric complex salt nanometer ball.
(embodiment 5)
The present embodiment is ZnFe 2o 4the preparation method of nano flake:
Put 1mmol zinc nitrate, 2mmol iron nitrate, 150mmol sodium-chlor, the grinding of 15mmol Repone K, Homogeneous phase mixing, is positioned over mixture in alumina crucible, then alumina crucible is put into tube furnace, by the ramp to 820 DEG C of 5 DEG C/min, and roasting 6h.
Naturally cool to envrionment temperature, distilled water dipping desalination, suction filtration, washing, 60 DEG C of dryings, obtained ZnFe 2o 4nano flake.
This ZnFe 2o 4the scanning electron microscope (SEM) photograph of nano flake is shown in Fig. 5, as shown in Figure 5: this ZnFe 2o 4have sheet structure, the Thickness Ratio of nano flake is more homogeneous, and productive rate is approximately 85wt%.
Control divalent metal and ferric mol ratio are 1: 2, and the mol ratio of raw material and fused salt is 3: 11y(13≤y≤50), replace above-mentioned Zn with Mg, Ni, Cu, Cd, Ca, Sr, Ba, Mn etc. respectively, adopt identical method can obtain MgFe respectively 2o 4, NiFe 2o 4, CuFe 2o 4, CdFe 2o 4, CaFe 2o 4, SrFe 2o 4, BaFe 2o 4, MnFe 2o 4deng wustite nano flake.
(embodiment 6)
The present embodiment is CoFe 2o 4the preparation method of nano flake:
Put 1mmol Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, 2mmol iron nitrate, 0.2mol sodium-chlor, the grinding of 0.02mol Repone K; Homogeneous phase mixing; mixture is positioned in alumina crucible; again alumina crucible is put into tube furnace; pass into rare gas element; under protection of inert gas, by the ramp to 840 DEG C of 5 DEG C/min, roasting 4h.
Naturally cool to envrionment temperature, distilled water dipping desalination, suction filtration, washing, 50 DEG C of dryings, obtained CoFe 2o 4nano flake.
Control divalent metal and ferric mol ratio are 1: 2, and the mol ratio of raw material and fused salt is 3: 11y(13≤y≤50), Co is replaced to Pb or Sn, adopts identical method can obtain PbFe respectively 2o 4, SnFe 2o 4nano flake.
(embodiment 7)
The present embodiment is Mn 0.4fe 2.6o 4the preparation method of nano flake:
Set to 0 .4mmol manganous oxalate, 2.6mmol iron nitrate, 0.2mol sodium-chlor, the grinding of 0.02mol Repone K, Homogeneous phase mixing, is positioned over mixture in alumina crucible, then alumina crucible is put into tube furnace, by the ramp to 840 DEG C of 5 DEG C/min, roasting 6h.
Naturally cool to envrionment temperature, distilled water dipping desalination, suction filtration, washing, 60 DEG C of dryings, obtained Mn 0.4fe 2.6o 4nano flake.
Control divalent metal and ferric mol ratio are x: 3-x(0.01≤x < 1), the mol ratio of raw material and fused salt is 3: 11y(13≤y≤50), replace above-mentioned Mn with Mg, Ni, Cu, Cd, Ca, Sr, Ba, Zn etc. respectively, adopt identical method can obtain Mg respectively xfe 3-xo 4, Ni xfe 3-xo 4, Cu xfe 3-xo 4, Cd xfe 3-xo 4, Ca xfe 3-xo 4, Sr xfe 3-xo 4, Ba xfe 3-xo 4, Zn xfe 3-xo 4deng wustite nano flake.
(embodiment 8)
The present embodiment is Mg 0.5ni 0.5fe 2o 4the preparation method of nano flake:
Set to 0 .5mmol magnesium nitrate, 0.5mmol nickelous nitrate, 2mmol iron nitrate, 180mmol sodium-chlor, the grinding of 18mmol Repone K, Homogeneous phase mixing, is positioned over mixture in alumina crucible, then alumina crucible is put into tube furnace, by the ramp to 820 DEG C of 5 DEG C/min, roasting 6h.
Naturally cool to envrionment temperature, distilled water dipping desalination, suction filtration, washing, 70 DEG C of dryings, obtained Mg 0.5ni 0.5fe 2o 4nano flake.
This Mg 0.5ni 0.5fe 2o 4the scanning electron microscope (SEM) photograph of nano flake is shown in Fig. 6, as shown in Figure 6: this Mg 0.5ni 0.5fe 2o 4have sheet structure, the thickness of nano flake is homogeneous, and productive rate is approximately 80wt%.
Mole total amount and the ferric mol ratio that control divalent metal equal 1: 2, the mol ratio of raw material and fused salt is 3: 11y(13≤y≤50), adopt any two kinds of above-mentioned Mg and Ni of replacement in Mg, Ni, Cu, Cd, Ca, Sr, Ba, Zn, Mn, adopt same procedure can obtain corresponding acid ferric complex salt nano flake.

Claims (1)

1. prepare the method for wustite nano flake for one kind, it is characterized in that: the bivalent metallic compound as raw material, the ferric iron compound as raw material, the sodium-chlor as fused salt and the Repone K as fused salt are ground, mix, mixture is positioned in crucible, again crucible is put into tube furnace, be warming up to 800 DEG C ~ 880 DEG C roasting 4h ~ 6h, obtain nano ferrite through aftertreatment; The mol ratio of described raw material and described fused salt is 3: 11y, wherein 13≤y≤50, and obtained nano ferrite is wustite nano flake; Divalent metal in described raw material and ferric mol ratio are x: 3-x, wherein 0.01≤x≤1; Sodium-chlor in described fused salt and the mol ratio of Repone K are 10: 1;
Described ferric iron compound is ferric oxide, ironic hydroxide, iron nitrate, ironic acetate, ironic oxalate or iron carbonate;
Described bivalent metallic compound is bivalent metal oxide, Divalent metal hydroxide, divalent metal nitrate, divalent metal acetate, divalent metal oxalate or bivalent metal carbonate;
Described divalent metal is one in magnesium, nickel, copper, cadmium, calcium, strontium, barium, zinc, manganese or two kinds.
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