CN105161246B - Nickel-zinc ferrite/polyacrylic acid nano-composite material and preparation method thereof - Google Patents
Nickel-zinc ferrite/polyacrylic acid nano-composite material and preparation method thereof Download PDFInfo
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- CN105161246B CN105161246B CN201510519492.XA CN201510519492A CN105161246B CN 105161246 B CN105161246 B CN 105161246B CN 201510519492 A CN201510519492 A CN 201510519492A CN 105161246 B CN105161246 B CN 105161246B
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Abstract
The invention discloses a nickel-zinc ferrite/polyacrylic acid nano-composite material and a preparation method thereof. The nano-composite material is in a core-shell structure and comprises core nickel-zinc ferrite and shell polyacrylic acid; the shell polyacrylic acid coats the nickel-zinc ferrite; and the nano-composite material is represented by Ni0.1-1Zn0.1-1Fe1-3O2-6/PAA. The preparation method of the nano-composite material mainly comprises the following steps: (1) weighing zinc sulfate, ferrous sulfate and nickel sulfate to prepare a metal salt solution, adding the metal salt solution into an ammonium oxalate solution; (2) adjusting the pH of the mixed solution, and separating and drying the mixed solution to obtain a ferrite precursor; (3) burning the ferrite precursor to obtain the nickel-zinc ferrite; and (4) mixing and reacting the nickel-zinc ferrite and acrylic acid, and separating and drying the mixture to obtain the nickel-zinc ferrite/polyacrylic acid nano-composite material. The nickel-zinc ferrite/polyacrylic acid nano-composite material has the advantages of low specific saturated magnetic field intensity, relatively low coercive force and relatively high soft magnetic property; and the preparation method disclosed by the invention is simple, feasible and low in cost.
Description
Technical field
The invention belongs to field of nanocomposite materials, more particularly to a kind of nickel-zinc ferrite/polyacrylic acid nano composite wood
Material and preparation method thereof.
Background technology
Nano composite material is many by one kind of two or more physically or chemically different material composition
Phase solid material, it is in nano level particulate, crystal grain, film or fiber in one-dimensional square that wherein at least has one；And it is new
The solid phase material of generation has different physically or chemically from common large scale material.Nano composite material presses solid-phase component
Generally can be divided into：Inorganic nano composite material, Organic/Inorganic Composite Nanomaterials, organic/organic nanocomposite.Due to
The nanometer phase included in nano composite material, so there is substantial amounts of interface between matrix and reinforcement, reinforcement.Its knot
Particularity on structure so that nano composite material possesses some unique effects, mainly small-size effect and surface or interface
Effect, thus have the difference of highly significant with the micro materials on the traditional concept of same composition in performance, show many
Excellent performance and brand-new function, in many fields wide application prospect is shown.
Magnetic nanometer composite material is the class new function composite for developing in recent years, according to magnetic Nano composite wood
The composition of material, can be divided into inorganic magnetic nano composite material (multiple including metal system magnetic Nano by magnetic nanometer composite material
Condensation material, ferrite magnetic nano composite, magnetic Nano composite granules film etc.), high polymer magnetic nanometer composite material (bag
Include natural high polymer magnetic nanometer composite material, artificial synthesized high polymer magnetic nanometer composite material etc.) and magnetic fluid (iron oxygen
Body magnetic fluid, metal MHD, nitridation magnetic fluid etc.) three classes.
Soft magnetic ferrite is that current purposes is wide, and wide in variety, quantity is big, a kind of high Ferrite Material of the output value.It is mainly used
Make various inductance elements, such as wave filter magnetic core, magnetic core of transformer, radio magnetic core and tape recording and video recording head,
It is the critical material of magnetic recording element, Ni ferrite is that a kind of purposes is wide, yield is big, the electronics industry of low cost and mechanotronics
Basic material.At present, as electronic product develops to miniaturization, density height, the soft magnet oxygen of uniform small grains are prepared
Body is particularly important, but this material, under weaker magnetic field, easy magnetization also easily demagnetizes, such as zinc chrome ferrite and nickel-zinc ferrite
Deng, because the magnetic energy stored in ferrite unit volume is relatively low, relatively low (the generally only 1/3-1/ of pure iron of the conjunction intensity of magnetization of satisfying
5), thus limit it in the low frequency forceful electric power required compared with high magnetic energy density and the application in high-power field.Therefore, soft magnetic ferrite
The research of nano composite material becomes one of focus of domestic and international research.
The content of the invention
Goal of the invention：An object of the present disclosure is to provide a kind of nickel-zinc ferrite/polypropylene with high soft magnetic characteristic
Sour nano composite material；The second object of the present invention is to provide the preparation method of the nano composite material.
Technical scheme：Nickel-zinc ferrite of the present invention/sodium polyacrylate nano composite material is core shell structure, preferably
Spherical particle, the core shell structure includes the shell polyacrylic acid of kernel nickel-zinc ferrite and cladding nickel-zinc ferrite, the material
Use Ni0.1～1Zn0.1～1Fe1～3O2～6/ PAA is represented, preferably can be Ni0.5Zn0.5Fe2O4/PAA。
The present invention prepares the nickel-zinc ferrite/sodium polyacrylate nano composite material using following steps：
(1) according to Ni0.1～1Zn0.1～1Fe1～3O2～6Stoichiometric proportion 0.1～1：0.1～1：1～3 weighs respectively sulfuric acid
Nickel, zinc sulfate, ferrous sulfate preparing metal salting liquid, configuration concentration is the ammonium oxalate solution of 0.5～1.5mol/L, by the oxalic acid
After ammonium salt solution is heated to 30～50 DEG C, and metal salt solution is added thereto to, wherein, the body of ammonium oxalate solution and metal salt solution
Product is than being 2:1, then insulated and stirred mixed solution.Preferably, Ni0.1～1Zn0.1～1Fe1～3O2～6Stoichiometric proportion 0.5～1：
0.5～1：2～3.
(2) pH for adjusting mixed solution with the NaOH solution of 6～8mol/L is 9～12.
(3) by mixed solution centrifugation, after obtaining sediment, deionized water and washes of absolute alcohol precipitation is respectively adopted
Thing 2～3 times.Furtherly, the rotating speed 5000r/min of centrifugation, time interval 10min.
(4) sediment after cleaning is dried under vacuum, obtains ferrite presoma.Furtherly, the drying
It is that 12～24h is dried under 40～80 DEG C of vacuum conditions.
(5) the ferrite presoma is calcined under the conditions of 100～300 DEG C 9～11h, then is warmed up to 700～900 DEG C of bars
1～3h is calcined under part, nickel-zinc ferrite is obtained.Preferably, the ferrite presoma is calcined into 10 under the conditions of 200～300 DEG C
～11h, then 2～3h is calcined under the conditions of being warmed up to 800～900 DEG C.First step precalcining can make ferrite nucleation, and second step is forged
Burn, make ferrite nucleating growth, obtain having magnetic ferrite, the ferrite compactness that this calcining manners are obtained is good, product
It is of fine quality good.
(6) nickel-zinc ferrite for obtaining is disperseed in deionized water, addition acrylic acid is under 50～80 DEG C of water bath conditions
1～3h of heating, while initiator, dispersant and crosslinking agent are added, wherein, nickel-zinc ferrite, acrylic acid, initiator, dispersion
The mass ratio of agent and crosslinking agent is 0.1～1：10～40：0.01～0.05：0.1～0.5：3～8, after reaction terminates, centrifugation
Separation product obtains sediment, deionized water and washes of absolute alcohol sediment 2～3 times is respectively adopted, in 40～80 DEG C of vacuum
Under the conditions of be dried 12～24h obtain nickel-zinc ferrite/sodium polyacrylate nano composite material.Preferably, the nickel-zinc ferrite, propylene
The mass ratio of acid, initiator, dispersant and crosslinking agent is 0.4～0.6：25～35：0.02～0.04：0.2～0.4：4～6；
Meanwhile, initiator can be ammonium persulfate, and dispersant can be isopropanol, and crosslinking agent can be glutaraldehyde.
Beneficial effect：Compared with prior art, remarkable advantage of the invention is nickel zinc iron/sodium polyacrylate nano composite material
With obvious core shell structure, there is hysteresis under externally-applied magnetic field, be far smaller than ferritic ratio than saturation magnetic field intensity
Saturation magnetic field intensity, coercivity is less, is preferable soft magnetic materials with higher soft magnetic characteristic, can be used as various inductance units
Part, such as wave filter magnetic core, magnetic core of transformer, radio magnetic core, and tape recording and video recording head etc., are also magnetic recording element
Critical material.Meanwhile, the preparation method materials of the present invention are simple, and preparation technology is easy to operate, without the need for complicated synthesis device,
Preparation cost is relatively low.
Description of the drawings
Fig. 1 is NiZn ferrites presoma (a) and the XRD of NiZn ferrites (b) of 800 DEG C of calcining 2h of Jing；
Fig. 2 is Ni0.5Zn0.5Fe2O4(a) and Ni0.5Zn0.5Fe2O4The infrared spectrogram of/PAA (b)；
Fig. 3 is the Ni that 800 DEG C of calcining 2h are obtained0.5Zn0.5Fe2O4The hysteresis curve of powder；
Fig. 4 is Ni0.5Zn0.5Fe2O4The hysteresis curve of/PAA composites；
Fig. 5 is Ni0.5Zn0.5Fe2O4TEM figure；
Fig. 6 is Ni0.5Zn0.5Fe2O4The TEM figures of/PAA.
Specific embodiment
Technical scheme is described further below in conjunction with the accompanying drawings.
Nickel-zinc ferrite/sodium polyacrylate the nano composite material of the present invention is core shell structure, including kernel nickel-zinc ferrite
And the shell polyacrylic acid of cladding nickel-zinc ferrite, composite Ni0.1～1Zn0.1～1Fe1～3O2～6/ PAA is represented, excellent
Choosing, the composite can be Ni0.5Zn0.5Fe2O4/PAA。
The preparation method of the nickel-zinc ferrite/sodium polyacrylate nano composite material of the present invention, comprises the steps：
(1) according to Ni0.1～1Zn0.1～1Fe1～3O2～6Stoichiometric proportion 0.1～1：0.1～1：1～3 weighs respectively sulfuric acid
Nickel, zinc sulfate, ferrous sulfate preparing metal salting liquid, configuration concentration is the ammonium oxalate solution of 0.5～1.5mol/L, by the oxalic acid
After ammonium salt solution is heated to 30～50 DEG C, metal salt solution is added thereto to, wherein, the volume of ammonium oxalate solution and metal salt solution
Than for 2:1, then insulated and stirred mixed solution, it is preferable that Ni0.1～1Zn0.1～1Fe1～3O2～6Stoichiometric proportion 0.5～1：0.5～
1：2～3.
(2) pH for adjusting mixed solution with the NaOH solution of 6～8mol/L is 9～12；
(3) mixed solution centrifugation is obtained after sediment, deionized water and washes of absolute alcohol precipitation is respectively adopted
Thing 2～3 times, furtherly, the rotating speed of centrifugation is 5000r/min, and time interval is 10min, the rotating speed and time interval
Mixed solution is conducive to separate abundant；
(4) sediment after cleaning is dried into 12～24h under 40～80 DEG C of vacuum conditions, obtains ferrite presoma.
(5) ferrite presoma is calcined under the conditions of 100～300 DEG C 9～11h, then is warmed up to 700～900 DEG C of conditions
1～3h of lower calcining, obtains nickel-zinc ferrite.
(6) nickel-zinc ferrite for obtaining is disperseed in deionized water, addition acrylic acid is under 50～80 DEG C of water bath conditions
1～3h of heating, while add that agent ammonium persulfate, isopropyl alcohol dispersant, crosslinking agent glutaraldehyde are sent out, wherein, nickel-zinc ferrite, propylene
The mass ratio of acid, initiator, dispersant and crosslinking agent is 0.1～1：10～40：0.01～0.05：0.1～0.5：3～8, instead
After should terminating, centrifugation product obtains sediment, and deionized water and washes of absolute alcohol sediment 2～3 times is respectively adopted,
12～24h is dried under 40～80 DEG C of vacuum conditions and obtains nickel-zinc ferrite/sodium polyacrylate nano composite material, it is preferable that nickel zinc iron
The mass ratio of oxysome, acrylic acid, initiator, dispersant and crosslinking agent is 0.4～0.6:25～35:0.02～0.04:0.2～
0.4:4～6.
Embodiment 1
(1) according to Ni0.5Zn0.5Fe2O4Stoichiometric proportion 0.5:0.5:2 weigh respectively nickel sulfate, zinc sulfate, sulfuric acid Asia
Iron preparing metal salting liquid, configuration concentration is the ammonium oxalate solution of 1.0mol/L, after the ammonium oxalate solution is heated to into 40 DEG C, to
It adds metal salt solution, wherein, ammonium oxalate solution is 2 with the volume ratio of metal salt solution:1, then insulated and stirred mixing is molten
Liquid.
(2) pH for adjusting mixed solution with the NaOH solution of 7mol/L is 10；
(3) by mixed solution centrifugation, the rotating speed of centrifugation is 5000r/min, and time interval is 10min, is obtained
After sediment, deionized water and washes of absolute alcohol sediment 2 times is respectively adopted.
(4) sediment after cleaning is dried into 24h under 60 DEG C of vacuum conditions, obtains ferrite presoma.
(5) ferrite presoma is calcined under the conditions of 200 DEG C and calcined 2 hours under the conditions of 10 hours, then 800 DEG C, it is natural
Required nickel-zinc ferrite is obtained after cooling；
(6) weigh nickel-zinc ferrite 0.5g to be put in the beaker of 100ml, add the distilled water of 60ml, ultrasonication 2h
Make its fully dispersed, the acrylic monomers for then measuring 30ml adds the above-mentioned aqueous solution, and under 65 DEG C of water bath conditions 2h is heated,
While the mass ratio 0.5 of the addition according to ferrite, acrylic acid, initiator, dispersant and crosslinking agent：30：0.03：0.3：
5, initiator ammonium persulfate, isopropyl alcohol dispersant and crosslinking agent glutaraldehyde are added, it is stirred continuously；After question response terminates,
Product centrifugation is obtained after sediment, deionized water and absolute ethanol washing sediment 3 times, finally in 60 DEG C of vacuum bars
24h is dried under part, Ni is obtained0.5Zn0.5Fe2O4/ PAA nano composite materials.
The experimental result of embodiment 1 is represented：
Fig. 1 is NiZn ferrites presoma (a) and the ferritic XRDs of NiZn of 800 DEG C of calcining 2h of Jing, can by Fig. 1 (a)
Know, diffraction peaks broadening is more serious, this is because crystallite dimension is less and crystallization degree is relatively low.In figure (b), 2 θ values are 27.28 °,
39.08 °, 44.54 °, 53.08 °, 64.96 °, 66.91 °, 73.46 ° and 84.78 ° of characteristic diffraction peak corresponds to respectively Ni Zn ferrimagnet
The diffraction maximum of (111), (220), (311), (400), (422), (511), (440) and (620) crystal face of body, the width of diffraction maximum
Consistent with standard diagram JCPDS standards with the relative intensity at peak, powder is crystalline state, in spinel cubic crystalline structure.
Fig. 2 is Ni0.5Zn0.5Fe2O4(a) and Ni0.5Zn0.5Fe2O4The infrared spectrogram of/PAA (b).
In figure (a), due to there is adsorbed water molecule, so sample is in 3440cm-1And 1632cm-1Nearby occur H-O-H's
Characteristic peak, 577cm-1And 420cm-1There is Ni in place0.5Zn0.5Fe2O4Characteristic peak.
In figure (b), it can be seen that in 1710cm-1Neighbouring strong absworption peak demonstrates the presence of-COOH；Composite exists
1582cm-1There is a new peak, 1411cm in place-1The relative intensity at place peak increases.In 1600cm-1The peak for nearby occurring is R-
The asymmetric stretching vibration of COO-, in 1400cm-1The peak for nearby occurring is the symmetrical stretching vibration of R-COO-, and this shows PAA's
Chemical reaction is there occurs between a part of carboxyl and ferrite.
Fig. 3 is the Ni nanoparticle that 800 DEG C of calcining 2h are obtained0.5Zn0.5Fe2O4The hysteresis curve of powder, from figure 3, it can be seen that
Prepared ferrite powder generates the hysteresis curve of closure.As can be seen that when applied field strengths it is little with 1500Oe when, sample
The intensity of magnetization of product is significantly increased with the increase of applied field strengths, when electric field strength more than 1500Oe with additional
The increase of magnetic field intensity slowly increases, until it reaches saturation.Ni0.5Zn0.5Fe2O4Powder saturation magnetization is 68.14emu
g-1, coercivity is to be approximately zero, and superparamagnetism is presented.
Fig. 4 is Ni nanoparticle0.5Zn0.5Fe2O4The hysteresis curve of/PAA composites.As seen from Figure 4, composite material exhibits
Go out obvious ferromagnetism, the saturation magnetization of composite nanoparticle is 6.83emug-1, coercivity is to be approximately zero.It is compound
The saturation magnetization of material is substantially reduced.
Fig. 5 is Ni0.5Zn0.5Fe2O4TEM figure.From fig. 5, it can be seen that major part Ni0.5Zn0.5Fe2O4Nano-particle
, in 40nm or so, particle is well dispersed, and ferrite particle is substantially spherical in shape for particle diameter, and its particle diameter is also occurred in that than more uniform
A certain degree of reunion.
Fig. 6 is Ni0.5Zn0.5Fe2O4The TEM figures of/PAA nano composite materials.From fig. 6, it can be seen that composite particles microcosmic shape
State mostly is spherical particle, and particle kernel has obvious contrast difference with outside border, shows central spherical particle with outside border
Parcel and wrapped relation are presented, obvious morphology of core-shell structure is formed.Color than it is thin be the polypropylene to form shell
Acid, the saturate ferrite nano particles for being to be formed core.
Embodiment 2
Step is substantially the same manner as Example 1, and difference is：Nickel-zinc ferrite, acrylic acid, initiator, dispersant and
The mass ratio of crosslinking agent is 0.1：40：0.01：0.5：8.
Embodiment 3
Step is substantially the same manner as Example 1, and difference is：Nickel-zinc ferrite, acrylic acid, initiator, dispersant and
The mass ratio of crosslinking agent is 1：10：0.05：0.1：3.
The performance comparison table of nickel-zinc ferrite/sodium polyacrylate nano composite material prepared by embodiment 1-3 of table 1
As shown in Table 1, the nickel-zinc ferrite/sodium polyacrylate nano composite material of the gained of embodiment 1 saturation magnetization,
Soft magnetism and coercivity performance better than embodiment 2 and embodiment 3, this be with nickel-zinc ferrite nano-particle in polyacrylic acid
Dispersity, organic and inorganic between chemical bonding act on surface nature to ferrite particle and the change of microstructure
And polymer is relevant to factors such as the coating functions of inorganic nano-particle.Integument is blocked up when polyacrylic acid is excessive, produces screen
The effect of covering, conversely, do not reach the effect of cladding, organic and inorganic Interaction Force weakens, all can affect saturation magnetization and
Coercivity, so as to change ferritic magnetic property.
Embodiment 4
Step is substantially the same manner as Example 1, and difference is：In step (1), according to Ni0.1Zn0.1Fe3O6Stoichiometry
Than 0.1:0.1:3 weigh respectively zinc sulfate, ferrous sulfate, nickel sulfate preparing metal salting liquid, and configuration concentration is 0.5mol/L's
Ammonium oxalate solution；In step (2), the concentration of NaOH solution is 8mol/L, and it is 9 to adjust pH；In step (4), by cleaning after it is heavy
Starch is dried 24h under 40 DEG C of vacuum conditions；Ferrite presoma is calcined 11h by step in (5) under the conditions of 100 DEG C, then is risen
Temperature calcines 3h under the conditions of 700 DEG C；In step (6), the matter of nickel-zinc ferrite, acrylic acid, initiator, dispersant and crosslinking agent
Amount is than being 0.4：35：0.02：0.4：4,3h is heated under 50 DEG C of water bath conditions, 12 are dried under 80 DEG C of vacuum conditions.
Embodiment 5
Step is substantially the same manner as Example 1, and difference is：In step (1), according to NiZnFeO2Stoichiometric proportion 1:
1:1 weighs respectively nickel sulfate, zinc sulfate, ferrous sulfate preparing metal salting liquid, and configuration concentration is molten for the ammonium oxalate of 1.5mol/L
Liquid；In step (2), the concentration of NaOH solution is 6mol/L, and it is 12 to adjust pH；In step (4), by the sediment after cleaning 80
12h is dried under DEG C vacuum condition；Ferrite presoma is calcined into 9h under the conditions of 300 DEG C in step (5), then is warmed up to 900 DEG C
Under the conditions of calcine 1h；In step (6), the mass ratio of nickel-zinc ferrite, acrylic acid, initiator, dispersant and crosslinking agent is
0.6：25：0.04：0.2：6,1h is heated under 80 DEG C of water bath conditions, it is dried 24h under 40 DEG C of vacuum conditions.
Embodiment 6
Design 9 groups of parallel tests, Ni0.1～1Zn0.1～1Fe1～3O2～6Middle Ni, Zn, Fe stoichiometric proportion is respectively (0.5：
0.5：2)、(0.1：0.1：3)、(1：1：1)、(0.05：0.5：2)、(1.2：0.5：2)、(0.5：0.05：2)、(0.5：1.2：2)、
(0.5：0.5：0.5)、(0.5：0.5：3.2).Preparation method is same as Example 1.
The performance comparison table of the nickel-zinc ferrite/sodium polyacrylate nano composite material of the different stoichiometric proportions of table 2
As shown in Table 2, the saturation magnetization of embodiment 1-3 and coercivity performance are better than embodiment 4-9, wherein when
Ni0.1～1Zn0.1～1Fe1～3O2～6Stoichiometric proportion 0.1～1:0.1～1:When 1～3, the performance phase of the composite of gained
To preferable；Again with stoichiometric proportion as 0.5:0.5:It is optimal when 2.Because coercivity is relevant with grain size, gained in embodiment 1
Product diffraction maximum is most strong, and crystallization is most complete, and crystal formation is most perfect, and crystallite dimension is big, coercivity closer to 0, with higher soft
Magnetic property；The diffraction peak intensity and crystallite dimension of other components has more with respect to the former the weaker its surface that is likely due to
Dangling bonds cause the enhancing of surface magnetic anisotropy so that on surface ionic bonding effect symmetry it is poor, make product have compared with
High coercivity.
Claims (10)
1. a kind of nickel-zinc ferrite/sodium polyacrylate nano composite material, it is characterised in that：The nano composite material is nucleocapsid knot
Structure, including the shell polyacrylic acid of kernel nickel-zinc ferrite and cladding nickel-zinc ferrite, use Ni0.1～1Zn0.1～1Fe1～3O2～6/
PAA represents that the preparation method of the composite comprises the steps：
(1) nickel-zinc ferrite is prepared：Nickel sulfate, zinc sulfate, ferrous sulfate are configured to into metal salt solution, and it is molten to configure ammonium oxalate
Liquid, after ammonium oxalate solution is heated to into 30～50 DEG C, adds metal salt solution, insulated and stirred to adjust molten with NaOH solution to it
The pH of liquid is 9～12, and centrifugation obtains sediment, is cleaned with detergent after sediment, is dried under vacuum, obtains
Ferrite presoma, the ferrite presoma subsequently calcined under the conditions of 100～300 DEG C 9～11h, then it is warmed up to 700～
1～3h is calcined under the conditions of 900 DEG C, you can；Wherein, the stoichiometric proportion 0.1～1 of nickel sulfate, zinc sulfate, ferrous sulfate:0.1～
1:1～3, the concentration of ammonium oxalate solution is 0.5～1.5mol/L, and ammonium oxalate solution is 2 with the volume ratio of metal salt solution:1；
(2) nickel-zinc ferrite/sodium polyacrylate nano composite material is prepared：The nickel-zinc ferrite for obtaining is dispersed in into deionized water
In, add acrylic acid to carry out heating response, while initiator, dispersant and crosslinking agent are added, wherein, the Ni Zn ferrimagnet
The mass ratio of body, acrylic acid, initiator, dispersant and crosslinking agent is 0.1～1：10～40：0.01～0.05：0.1～0.5：
3～8, after reaction terminates, centrifugation product obtains sediment, and sediment is cleaned with detergent, is dried.
2. nickel-zinc ferrite according to claim 1/sodium polyacrylate nano composite material, it is characterised in that：The nanometer
Composite Ni0.5Zn0.5Fe2O4/ PAA is represented.
3. a kind of method of the nickel-zinc ferrite/sodium polyacrylate nano composite material prepared described in claim 1, it is characterised in that
Comprise the steps：
(1) with nickel sulfate, zinc sulfate, ferrous sulfate as raw material stoichiometrically 0.1～1:0.1～1:1～3 preparing metal salt
Solution, configuration concentration is the ammonium oxalate solution of 0.5～1.5mol/L, after the ammonium oxalate solution is heated to into 30～50 DEG C, and to
Metal salt solution is wherein added, wherein, the ammonium oxalate solution is 2 with the volume ratio of metal salt solution:1, then insulated and stirred
Mixed solution；
(2) pH for adjusting the mixed solution with NaOH solution is 9～12；
(3) by the mixed solution centrifugation, after obtaining sediment, with detergent sediment is cleaned；
(4) sediment after cleaning is dried under vacuum, obtains ferrite presoma；
(5) the ferrite presoma is calcined under the conditions of 100～300 DEG C 9～11h, then is warmed up under the conditions of 700～900 DEG C
1～3h of calcining, obtains nickel-zinc ferrite；
(6) nickel-zinc ferrite for obtaining is disperseed in deionized water, to add acrylic acid to carry out heating response, while add causing
Agent, dispersant and crosslinking agent, wherein, the quality of the nickel-zinc ferrite, acrylic acid, initiator, dispersant and crosslinking agent
Than for 0.1～1：10～40：0.01～0.05：0.1～0.5：3～8, after reaction terminates, centrifugation product obtains sediment,
Sediment is cleaned with detergent, nickel-zinc ferrite/sodium polyacrylate nano composite material is dried to obtain.
4. the method for preparing nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterised in that：
In step (1), the zinc sulfate, nickel sulfate, ferrous sulfate are raw material stoichiometrically 0.5～1：0.5～1：2～3 prepare
Metal salt solution.
5. the method for preparing nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterised in that：
In step (5), the ferrite presoma is calcined into 10～11h under the conditions of 200～300 DEG C, be warmed up to 800～900 DEG C of bars
2～3h is calcined under part, the nickel-zinc ferrite is obtained.
6. the method for preparing nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterised in that：
In step (6), the mass ratio of the nickel-zinc ferrite, acrylic acid, initiator, dispersant and crosslinking agent is 0.4～0.6：25
～35：0.02～0.04：0.2～0.4：4～6.
7. the method for preparing nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterised in that：
In step (3) and step (6), the described sediment that cleaned with detergent is that deionized water and absolute ethanol washing 2 is respectively adopted
～3 times.
8. the method for preparing nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterised in that：
In step (4) and step (6), the drying is that 12～24h is dried under 40～80 DEG C of vacuum conditions.
9. the method for preparing nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterised in that：
It is described to be heated to be heating water bath in step (6), wherein, heating-up temperature is 50～80 DEG C, and the heat time is 1～3h.
10. the method for preparing nickel-zinc ferrite/sodium polyacrylate nano composite material according to claim 3, it is characterised in that：
In step (6), the initiator is ammonium persulfate, and dispersant is isopropanol, and crosslinking agent is glutaraldehyde.
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| CN113461071A (en) * | 2021-06-10 | 2021-10-01 | 贵州理工学院 | Method for preparing nickel-zinc ferrite from waste nickel-hydrogen waste battery |
| CN113559857B (en) * | 2021-08-04 | 2023-12-29 | 吉林化工学院 | Magnetic visible light heterogeneous Fenton core-shell structure CuFe 2 O 4 Catalyst and application thereof |
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