CN115634630A - NiFe 2 O 4 Wave-absorbing and heat-storing integrated material coated with mineral microspheres and preparation method and application thereof - Google Patents
NiFe 2 O 4 Wave-absorbing and heat-storing integrated material coated with mineral microspheres and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a NiFe 2 O 4 A wave-absorbing and heat-storing integrated material coated with mineral microspheres and a preparation method and application thereof. The invention uses acid activation to separate the attapulgite into bundles and purify the attapulgite to obtain the modified attapulgite, and uses hydrothermal synthesis to coat flower-shaped TiO on the surface of the modified attapulgite 2 Obtaining the attapulgite-TiO 2 The attapulgite-TiO is constructed by spray drying and calcining 2 -carbon nanotube composite microspheres by coating with NiFe 2 O 4 Construction of Attapulgite-TiO 2 -carbon nanotube-NiFe 2 O 4 Composite microsphere prepared from attapulgite as matrixDielectric constant of composite material, carbon nanotube as dielectric loss material and NiFe 2 O 4 The magnetic particles are magnetic loss materials, the composite microspheres are constructed, so that the intrinsic impedance and the free space impedance of the materials are balanced as much as possible, the phase change materials are packaged in the rigid structures of the composite microspheres to prevent leakage, and the wave-absorbing and heat-storing integrated material is obtained.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to NiFe 2 O 4 A wave-absorbing and heat-storing integrated material coated with mineral microspheres and a preparation method and application thereof.
Background
Electromagnetic radiation pollution becomes another important pollution source which greatly influences the health of urban residents after being polluted by waste water, waste gas, noise and solid wastes, and great threat is generated to the health of human beings. With the development of wireless communications, highly integrated, high-speed, miniaturized wireless communication devices tend to suffer from undesirable electromagnetic interference effects and significant heat generation. Therefore, in modern wireless communication, autonomous cars, and portable devices, materials having both excellent thermal management properties and excellent electromagnetic interference shielding properties have received much attention. Phase change materials can store and release energy in the form of latent heat while maintaining a constant temperature, have been widely used in various fields such as thermal energy storage and thermal management of electronic devices due to their ultra-high volumetric energy density and narrow temperature distribution range during energy conversion and utilization, and are known as optimal temperature control materials for thermal protection and electronic cooling systems. However, the low thermal conductivity and leakage problems inherent in phase change materials have prevented their practical application in various fields.
Most of the composite phase change materials and microwave absorbing materials for electronic devices reported at present are concentrated on a single-purpose project, and the problems of complex preparation method, poor mechanical strength, low economic benefit and the like generally exist. In smart devices with small volume, light weight, and high energy density, it becomes very important to develop a protection system with dual functions of electromagnetic interference shielding and thermal management. However, designing a flexible, lightweight, and low volume integrated material with both efficient emi shielding and thermal management functions remains a significant challenge.
Disclosure of Invention
The present invention aims to provide a NiFe alloy with high strength and high strength, which is suitable for the above-mentioned defects of the prior art 2 O 4 A wave-absorbing and heat-storing integrated material coated with mineral microspheres and a preparation method and application thereof.
The invention relates to a NiFe 2 O 4 The preparation method of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres comprises the following steps:
s1, soaking and activating attapulgite by using acid liquor to obtain modified attapulgite;
s2, coating flower-shaped TiO by modified attapulgite 2 (ii) a Weighing modified attapulgite, placing the modified attapulgite in an isopropanol solution, slowly adding a diethylenetriamine solution, fully stirring and ultrasonically treating, adding an isopropyl titanate solution, slightly stirring by using a glass rod to obtain a mixed suspension, carrying out hydrothermal synthesis on the mixed suspension, collecting a black powder product after the reaction is finished, washing by using deionized water or absolute ethyl alcohol, and drying;
s3, modified attapulgite-TiO 2 Mixing and stirring the carbon nano tube slurry, sodium hexametaphosphate and water, and performing ultrasonic treatment to obtain attapulgite-TiO 2 -a carbon nanotube suspension;
s4, constructing attapulgite-TiO by the suspension through spray drying 2 -carbon nanotube composite microspheres;
s5, calcining to obtain attapulgite-TiO 2 -carbon nanotube composite microspheres;
s6, attapulgite-TiO 2 NiFe coated with-carbon nanotube composite microsphere 2 O 4 (ii) a Weighing NiCl 2 ·6H 2 O and FeCl 3 ·6H 2 Dissolving O in ethylene glycol solution, stirring and ultrasonic treating, adding CH 3 COONa and PEG2000, stirring and ultrasonic treating, adding attapulgite-TiO 2 Carbon nanotube composite microspheres, stirring and ultrasound to obtain a mixed suspension,carrying out hydro-thermal synthesis on the mixed suspension, collecting a black powder product after the reaction is finished, washing the black powder product with deionized water or absolute ethyl alcohol, and drying the black powder product;
s7, washing the composite microspheres with alkali; weighing coated NiFe 2 O 4 Placing the composite microspheres in alkali liquor, stirring to obtain a mixed suspension, carrying out hydro-thermal synthesis on the mixed suspension, collecting a black powder product after the reaction is finished, washing with deionized water or absolute ethyl alcohol, and drying;
s8, calcining the composite microspheres;
s9, carrying out vacuum impregnation on the composite microspheres and the phase-change material to obtain the NiFe with the performance of synchronously realizing heat management and microwave absorption 2 O 4 The wave-absorbing and heat-storing integrated material is coated with mineral microspheres.
Further, in the step S1, the process of immersing and activating the attapulgite acid solution mainly comprises: soaking in acid solution, performing solid-liquid separation, washing and drying; wherein the acid liquor is H + The inorganic strong acid aqueous solution with the concentration of 1-4 mol/L is soaked in the stirring, the stirring speed is 500-1000r/min, the soaking temperature is 60-90 ℃, and the soaking time is 30-120 min.
Further, in the step S2, the modified attapulgite, the isopropanol, the diethylenetriamine and the isopropyl titanate are calculated according to the following parts by weight:
modified attapulgite: 0.2 to 1 portion
Isopropyl alcohol: 30 to 80 portions of
Diethylenetriamine: 0.02 to 0.1 portion
Isopropyl titanate: 2-8 parts of a solvent;
in the step S2, the stirring speed is 500-1000r/min, and the stirring time is 30-60 min; the hydrothermal synthesis temperature is 180-200 ℃, and the hydrothermal synthesis time is 12-36 h.
Further, in step S3, the modified attapulgite-TiO 2 The carbon nano tube slurry, the sodium hexametaphosphate and the water are calculated according to the following parts by weight:
modified attapulgite-TiO 2 :0.5 to 2 portions of
Carbon nanotube slurry: 10 to 50 portions of
Sodium hexametaphosphate: 0.2 to 1 portion
Water: 40-100 parts;
the stirring speed is 600-1000r/min, and the stirring time is 30-60 min; the ultrasonic treatment time is 30-120 min;
the concentration of the carbon nanotube slurry was 10%.
Furthermore, in step S5, the calcining temperature is 300-400 ℃, the calcining time is 1-4 h, and the calcining atmosphere is inert gas.
Further, in step S6, the modified attapulgite-TiO 2 The carbon nano tube slurry, the sodium hexametaphosphate and the water are calculated according to the following parts by weight:
Attapulgite-TiO 2 -carbon nanotube composite microspheres: 0.05 to 0.5 portion
NiCl 2 ·6H 2 O:0.1 to 0.5 portion
FeCl 3 ·6H 2 O:0.2 to 1 portion
Ethylene glycol: 30 to 60 portions of
CH 3 COONa:0.4 to 1 portion
PEG2000: 0.2-0.6 part;
the stirring speed is 500-1000r/min, and the stirring time is 30-60 min; the hydrothermal synthesis temperature is 180-200 ℃, and the hydrothermal synthesis time is 8-24 h.
Further, in the step S7, the dosage relation of the composite microspheres and the alkali liquor is 1-3: 300-600 wt.%, wherein the alkali liquor is 0.5-2 mol/L NaOH solution; the stirring speed is 500-1000r/min, and the stirring time is 30-60 min; the hydrothermal synthesis temperature is 120-180 ℃, and the hydrothermal synthesis time is 8-24 h.
Further, in step S8, the calcining temperature is 300-400 ℃, the calcining time is 1-4 h, the heating rate is 5-10 ℃/min, and the calcining atmosphere is inert gas.
Further, in the spray drying process: the through needle of the spray dryer is set to be 3.0, the frequency of a fan is set to be 35.00Hz, the air inlet temperature is set to be 150-180 ℃, and the peristaltic speed is 1-5 RPM.
Further, in step S9, the usage relationship between the composite microspheres and the phase change material is as follows: 40-60 wt.%: 40-60 wt.%.
Preferably, in step S9, the vacuum impregnation is performed for 10 to 50min at room temperature and then for 10 to 50min at 40 to 90 ℃.
NiFe prepared by adopting preparation method 2 O 4 The wave-absorbing and heat-storing integrated material is coated with mineral microspheres.
NiFe as described above 2 O 4 The application of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres is used for electromagnetic interference shielding and heat energy adjustment of high-end electronic equipment.
The invention obtains the modified attapulgite by acid activation and purification of the attapulgite, and the surface of the modified attapulgite is coated with flower-shaped TiO by hydrothermal synthesis 2 Obtaining attapulgite-TiO 2 The attapulgite-TiO is constructed by spray drying and calcining 2 -carbon nanotube composite microspheres by coating with NiFe 2 O 4 Construction of Attapulgite-TiO 2 -carbon nanotube-NiFe 2 O 4 Composite microsphere, which takes attapulgite as a matrix material to adjust the dielectric constant of a composite material, carbon nano tubes as a dielectric loss material and NiFe 2 O 4 The magnetic particles are magnetic loss materials, the composite microspheres are constructed, so that the intrinsic impedance and the free space impedance of the materials are balanced as much as possible, the phase change materials are packaged in the rigid structures of the composite microspheres to prevent leakage, and the wave-absorbing and heat-storing integrated material is obtained.
The invention adjusts the complex dielectric constant of the composite material to a proper range by introducing the attapulgite, ensures the impedance matching characteristic balance of the material, and coats the surface of the attapulgite with the flower-shaped TiO 2 The constructed composite microspheres have a hierarchical porous structure, can provide a large number of adsorption sites for the phase-change material, and are beneficial to improving the loading capacity of the support material on the phase-change material. Meanwhile, the incident electromagnetic wave can be lost by multiple reflections in the sphere, and NiFe is combined 2 O 4 The strong magnetic loss capacity of the magnetic particles and the synergistic effect of multiple loss mechanisms enable the wave-absorbing and heat-storing integrated material to have excellent wave-absorbing and heat-storing performances.
The attapulgite-TiO constructed by the invention 2 -carbon nanotube-NiFe 2 O 4 The wave-absorbing and heat-storing integrated material is prepared by vacuum impregnation of the composite microspheres and loading of paraffin, and the loading capacity of the composite microspheres to paraffin is about 53.2%. Melting phase-change enthalpy and solidification phase-change enthalpy of the wave-absorbing and heat-storing integrated material respectively reach 112.4J/g and 108.2J/g, and the prepared heat-storing and wave-absorbing integrated material has excellent heat-storing capacity. The melting and solidification phase transition temperatures of the paraffin are 57.9 ℃ and 56.2 ℃, respectively, and the paraffin with the phase transition temperatures is suitable for thermal energy adjustment of electronic equipment.
The wave-absorbing and heat-storing integrated material constructed by the invention has the advantages that the effective wave-absorbing bandwidth can reach 4.96GHz when the thickness is only 1.55mm, and the maximum reflection loss value of 22.95dB is reached at 16.88GHz when the thickness is 1.4mm, so that the composite material has excellent microwave absorption performance. The material can simultaneously realize wave absorption and heat storage functions, and has important significance for synchronously realizing electromagnetic interference shielding and heat energy regulation of high-end electronic equipment.
Drawings
FIG. 1 is a scanning electron microscope photograph of the modified attapulgite prepared by the technical proposal of the embodiment 1;
FIG. 2 shows the attapulgite-TiO prepared by the technical scheme of the embodiment 2 2 Scanning electron microscope photographs of (a);
FIG. 3 shows attapulgite-TiO prepared by the technical scheme 7 of the embodiment 2 -carbon nanotube-NiFe 2 O 4 Scanning electron microscope photographs of the composite microspheres;
FIG. 4 is a diagram of the electromagnetic wave absorption characteristics of the wave absorbing and heat storing integrated material prepared in the technical solution of example 10;
FIG. 5 is a DSC curve of the heat-storage wave-absorbing integrated material prepared in the technical solution of example 10;
FIG. 6 is a thermogravimetric analysis curve of the heat-storage wave-absorbing integrated material prepared in example 10;
FIG. 7 is a graph of an infrared spectrum of a material prepared in examples 9 and 10;
FIG. 8 is a nitrogen desorption isotherm (a) and a BJH pore size distribution plot (b) of materials prepared in examples 1 and 9.
Detailed Description
The following are specific embodiments of the present invention and are further described with reference to the accompanying drawings, but the present invention is not limited to these embodiments.
Example 1:
this example prepared modified attapulgite.
Weighing 10g of attapulgite raw ore, placing the attapulgite raw ore into a beaker filled with 100ml of hydrochloric acid solution with the mass fraction of 4wt.%, placing the beaker into a water bath kettle with the constant temperature of 80 ℃, stirring, carrying out ultrasonic treatment and water bath pickling for 60min, washing the attapulgite raw ore with deionized water by a suction filtration method to be neutral, drying, grinding and sieving with a 180-mesh sieve to obtain the modified attapulgite.
Example 2:
this example prepared Attapulgite-TiO 2
Weighing 0.5g of prepared modified attapulgite, placing the weighed modified attapulgite in 40mL of isopropanol solution, slowly dripping 0.05mL of diethylenetriamine solution, fully stirring, adding 5mL of isopropyl titanate, slightly stirring by using a glass rod to obtain a mixed suspension, pouring the mixed suspension into a polytetrafluoroethylene liner, transferring the mixed suspension into a stainless steel reaction kettle, and placing the stainless steel reaction kettle in an oven at 200 ℃ for 24 hours for hydrothermal synthesis. And collecting a black powder product after the reaction is finished, washing the black powder product by using deionized water or absolute ethyl alcohol, and drying the black powder product in an oven at the temperature of 60 ℃.
Example 3:
this example constructed Attapulgite-TiO 2 -carbon nanotube composite microspheres
(1) Weighing 1g of attapulgite-TiO 2 Mixing 20g of 10% carbon nanotube slurry, 0.5g of sodium hexametaphosphate and 50ml of deionized water, stirring for 30min, and performing ultrasonic treatment for 60min to obtain attapulgite-TiO 2 -a suspension of carbon nanotubes.
(2) Mixing attapulgite-TiO 2 -spray drying the carbon nanotube suspension. The through needle of the spray dryer is set to be 3.0, the frequency of the fan is set to be 35.00Hz, the air inlet temperature is set to be 160 ℃, and the peristaltic speed is 2RPM. Collecting the dried material.
(3) Transferring the dried material collected by spray drying into a muffle furnace,calcining at 350 deg.C for 2h under argon atmosphere at a heating rate of 10 deg.C/min to obtain attapulgite-TiO 2 -carbon nanotube composite microspheres.
Example 4:
this example constructed Attapulgite-TiO 2 -carbon nanotube composite microspheres
(1) Weighing 1g of attapulgite-TiO 2 30g of carbon nano tube slurry with the concentration of 10 percent, 0.5g of sodium hexametaphosphate and 50ml of deionized water are mixed and stirred for 30min and subjected to ultrasonic treatment for 60min to obtain attapulgite-TiO 2 -a carbon nanotube suspension.
(2) Mixing attapulgite-TiO 2 -spray drying the carbon nanotube suspension. The through needle of the spray dryer is set to be 3.0, the frequency of a fan is set to be 35.00Hz, the air inlet temperature is set to be 160 ℃, and the peristaltic speed is 2RPM. And collecting the dried material.
(3) Transferring the dried material collected by spray drying into a muffle furnace, calcining at 350 deg.C for 2h in argon atmosphere at a heating rate of 10 deg.C/min to obtain attapulgite-TiO 2 -carbon nanotube composite microspheres.
Example 5:
this example constructed Attapulgite-TiO 2 -carbon nanotube-NiFe 2 O 4 Composite microspheres
(1) 0.118g of NiCl was weighed 2 ·6H 2 O and 0.27g FeCl 3 ·6H 2 Dissolving O in 50mL of ethylene glycol solution, stirring for 20min, performing ultrasonic treatment for 20min, and adding 0.328g of CH 3 COONa and 0.2g PEG2000, stirring for 20min and sonicating for 20min, adding 0.1g attapulgite-TiO prepared in example 4 2 And (3) stirring the carbon nano tube composite microspheres for 30min and carrying out ultrasonic treatment for 60min to obtain a mixed suspension, pouring the mixed suspension into a 100mL polytetrafluoroethylene lining, transferring the mixed suspension into a stainless steel reaction kettle, and keeping the stainless steel reaction kettle in a 200 ℃ oven for 12h for hydrothermal synthesis. And collecting a black powder product after the reaction is finished, washing the black powder product by using deionized water or absolute ethyl alcohol, and drying the black powder product.
Example 6:
this example constructed Attapulgite-TiO 2 -carbon nanotube-NiFe 2 O 4 Composite microspheres
(1) 0.354g of NiCl was weighed 2 ·6H 2 O and 0.81g FeCl 3 ·6H 2 Dissolving O in 50mL of ethylene glycol solution, stirring for 20min, performing ultrasonic treatment for 20min, and adding 0.984g of CH 3 COONa and 0.6g PEG2000, stirring for 20min and sonicating for 20min, adding 0.1g of the attapulgite-TiO prepared in example 4 2 And (3) stirring the carbon nano tube composite microspheres for 30min and carrying out ultrasonic treatment for 60min to obtain a mixed suspension, pouring the mixed suspension into a 100mL polytetrafluoroethylene lining, transferring the mixed suspension into a stainless steel reaction kettle, and keeping the stainless steel reaction kettle in a drying oven at the temperature of 200 ℃ for 12h for hydrothermal synthesis. And collecting a black powder product after the reaction is finished, washing the black powder product by using deionized water or absolute ethyl alcohol, and drying the black powder product.
Example 7:
this example constructed Attapulgite-TiO 2 -carbon nanotube-NiFe 2 O 4 Composite microspheres
(1) 0.236g NiCl was weighed 2 ·6H 2 O and 0.54g FeCl 3 ·6H 2 Dissolving O in 50mL of ethylene glycol solution, stirring for 20min, performing ultrasonic treatment for 20min, and adding 0.656g of CH 3 COONa and 0.4g PEG2000, stirred for 20min and sonicated for 20min, 0.1g attapulgite-TiO prepared in example 4 was added 2 And (3) stirring the carbon nano tube composite microspheres for 30min and carrying out ultrasonic treatment for 60min to obtain a mixed suspension, pouring the mixed suspension into a 100mL polytetrafluoroethylene lining, transferring the mixed suspension into a stainless steel reaction kettle, and keeping the stainless steel reaction kettle in a 200 ℃ oven for 12h for hydrothermal synthesis. And collecting a black powder product after the reaction is finished, washing the black powder product by using deionized water or absolute ethyl alcohol, and drying the black powder product.
Example 8:
this example alkaline washes attapulgite-TiO 2 -carbon nanotube-NiFe 2 O 4 And (3) compounding the microspheres.
Attapulgite-TiO prepared in example 7 was weighed 2 -carbon nanotube-NiFe 2 O 4 0.1g of composite microspheres are placed in 1mol/L NaOH solution and stirred for 30min to obtain mixed suspension, the mixed suspension is poured into a polytetrafluoroethylene liner, the polytetrafluoroethylene liner is transferred into a stainless steel reaction kettle, and the stainless steel reaction kettle is placed in a 150 ℃ oven and kept for 12h for hydrothermal synthesis. Collecting black powder product after the reaction is finished, and using deionized water or anhydrous ethyl alcoholWashed with alcohol and dried in an oven at 60 ℃.
Example 9:
this example calcines attapulgite-TiO 2 -carbon nanotube-NiFe 2 O 4 And (3) compounding the microspheres.
Transferring the dry material collected in the example 5 to a tubular furnace, calcining for 2h at 350 ℃, wherein the calcining atmosphere is argon, and the heating rate is 5 ℃/min to obtain the attapulgite-TiO 2 -carbon nanotube-NiFe 2 O 4 And (3) compounding the microspheres.
Example 10:
the wave-absorbing and heat-storing integrated material is prepared by the embodiment.
Weighing 2g of the Attapulgite-TiO prepared in example 6 2 -carbon nanotube-NiFe 2 O 4 Transferring the composite microspheres and 3g of paraffin (P) into a suction flask, vacuumizing for 30min at room temperature, vacuumizing for 30min under the condition of 90 ℃ water bath, and performing oven heat filtration for 24h at 60 ℃ to obtain the wave-absorbing and heat-storing integrated material.
Referring to the attached figure 1, it is a scanning electron microscope photograph of the modified attapulgite prepared by the technical scheme of the embodiment 1. It can be seen that the modified attapulgite aggregates after the acid activation treatment are reduced, the attapulgite is de-bundled to a certain degree, and the method is beneficial to coating more flower-shaped TiO on the surface of the attapulgite in the follow-up process 2 。
Referring to the attached figure 2, the attapulgite-TiO prepared by the technical proposal of the embodiment 2 is shown 2 Scanning electron microscope photograph of (1). As can be seen, the surface of the attapulgite is successfully coated with a large amount of flower-shaped TiO 2 The porous structure provides a large number of adsorption sites for the phase-change material, and is beneficial to improving the loading capacity of the support material to the phase-change material.
Referring to the attached figure 3, which is the attapulgite-TiO prepared by the technical scheme 7 of the embodiment 2 -carbon nanotube-NiFe 2 O 4 Scanning electron micrographs of the composite microspheres. It can be seen that the size of the constructed composite microspheres is about 9 μm, and the spherical structure is better. The surface of the composite microsphere is successfully coated with a large amount of NiFe 2 O 4 And (3) particles. NiFe 2 O 4 The magnetic particles areBetter magnetic loss material is beneficial to improving the microwave absorption performance of the composite microsphere.
Referring to the attached figure 4, the electromagnetic wave absorption characteristics of the wave-absorbing and heat-storing integrated material prepared by the technical scheme of the embodiment 10 are shown, the reflection loss value of a sample is calculated in a simulation mode according to the relative complex dielectric constant and magnetic conductivity under different given absorber thicknesses and by combining a transmission line theory, and a corresponding two-dimensional curve graph is drawn. The composite microsphere is in a range of 2-18GHz, when the thickness is only 1.55mm, the effective wave-absorbing bandwidth can reach 4.96GHz, and when the thickness is 1.4mm, the maximum reflection loss value at 16.88GHz is 22.95dB. The introduction of attapulgite can adjust the complex dielectric constant of the composite material to a proper range, ensure the impedance matching characteristic balance of the material, and coat flower-shaped TiO on the surface of the attapulgite 2 The constructed composite microsphere has a hierarchical porous structure, can cause incident electromagnetic waves to generate multiple reflection in the sphere to cause loss, and is combined with NiFe 2 O 4 The strong magnetic loss capacity of the magnetic particles and the synergistic effect of multiple loss mechanisms enable the wave-absorbing and heat-storing integrated material to have excellent wave-absorbing performance.
Referring to the attached figure 5, it is a DSC curve of the heat storage and wave absorption integrated material prepared by the technical scheme of the embodiment 10. The melting phase-change enthalpy and the solidification phase-change enthalpy of the composite material respectively reach 112.4J/g and 108.2J/g, and the prepared heat-storage wave-absorbing integrated material has excellent heat storage capacity. The melting and solidification phase transition temperatures of the paraffin are 57.9 ℃ and 56.2 ℃ respectively, the electronic equipment can generate heat to damage the equipment when running for a long time, and the paraffin with the phase transition temperature is suitable for heat energy adjustment of the electronic equipment.
Referring to the attached figure 6, which is a thermogravimetric analysis curve of the heat-storage wave-absorbing integrated material prepared in example 10, the loading amount of the composite microspheres to paraffin is about 53.2%, the porous structure and the large specific surface of the composite microspheres provide a large number of adsorption sites for paraffin, and paraffin is packaged in a rigid structure of the composite microspheres, so that the composite phase-change material has excellent heat energy storage capacity.
Referring to FIG. 7, which is an infrared spectrum of the materials prepared in examples 9 and 10, it can be seen from the infrared spectrum of paraffin wax that it is 2917cm -1 And 2847cm -1 Respectively belong to the asymmetric and symmetric stretching vibration peaks of C-H. In addition, 1466cm -1 Is caused by the bending vibration of C-H. Located at 725cm -1 Is due to CH 2 Is caused by the rolling vibration of (a). When the paraffin and the composite microspheres are compounded, no new absorption peak exists in the prepared composite phase change material in a paraffin-composite microsphere spectrum, which shows that no chemical action exists between the paraffin and the composite microspheres, and the compatibility is good.
Referring to FIG. 8, which is a graph showing the nitrogen desorption isotherms (a) and the BJH pore size distribution of the materials prepared in examples 1 and 9, it can be seen that the composite microspheres combine type I and type IV isotherms at P/P o In the range of 0.50 to 0.95, there is a weak hysteresis loop, which means that many micropores and mesopores coexist. Therefore, the composite microsphere is a typical hierarchical porous material and has various pore structure characteristics. The specific surface areas of the modified attapulgite and the composite microspheres are 248.6m respectively by analyzing and calculating the nitrogen adsorption and desorption curve 2 (ii)/g and 87.3m 2 The/g is that although the specific surface area of the modified attapulgite is large, the bundle-shaped encapsulated paraffin of the modified attapulgite is easy to leak, and the composite microspheres can encapsulate the paraffin in a rigid structure to prevent leakage. The average pore diameters of the modified attapulgite and the composite microsphere are respectively 9.3nm and 18.2 nm, and the larger pore diameter in a certain range is more beneficial to the paraffin adsorption of the support material.
The above is not relevant and is applicable to the prior art.
While certain specific embodiments of the present invention have been described in detail by way of illustration, it will be understood by those skilled in the art that the foregoing is illustrative only and is not limiting of the scope of the invention, as various modifications or additions may be made to the specific embodiments described and substituted in a similar manner by those skilled in the art without departing from the scope of the invention as defined in the appending claims. It should be understood by those skilled in the art that any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. NiFe 2 O 4 The preparation method of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres is characterized by comprising the following steps of: the method comprises the following steps:
s1, soaking and activating attapulgite by using acid liquor to obtain modified attapulgite;
s2, coating flower-shaped TiO by modified attapulgite 2 (ii) a Weighing modified attapulgite, placing the modified attapulgite in an isopropanol solution, slowly adding a diethylenetriamine solution, fully stirring and ultrasonically treating, adding an isopropyl titanate solution, slightly stirring by using a glass rod to obtain a mixed suspension, carrying out hydrothermal synthesis on the mixed suspension, collecting a black powder product after the reaction is finished, washing by using deionized water or absolute ethyl alcohol, and drying;
s3, modified attapulgite-TiO 2 Mixing and stirring the carbon nano tube slurry, sodium hexametaphosphate and water, and performing ultrasonic treatment to obtain attapulgite-TiO 2 -a carbon nanotube suspension;
s4, constructing attapulgite-TiO by the suspension through spray drying 2 -carbon nanotube composite microspheres;
s5, calcining to obtain attapulgite-TiO 2 -carbon nanotube composite microspheres;
s6, attapulgite-TiO 2 NiFe coated with-carbon nanotube composite microsphere 2 O 4 (ii) a Weighing NiCl 2 ·6H 2 O and FeCl 3 ·6H 2 Dissolving O in glycol solution, stirring and ultrasonic treating, adding CH 3 COONa and PEG2000, stirring and ultrasonic treating, adding attapulgite-TiO 2 -carbon nanotube composite microspheres, stirring and ultrasonically treating to obtain a mixed suspension, carrying out hydrothermal synthesis on the mixed suspension, collecting a black powder product after the reaction is finished, washing with deionized water or absolute ethyl alcohol, and drying;
s7, washing the composite microspheres with alkali; weighing coated NiFe 2 O 4 Placing the composite microspheres in alkali liquor, stirring to obtain mixed suspension, carrying out hydrothermal synthesis on the mixed suspension, collecting black powder product after the reaction is finished, and adding deionized water or anhydrous ethyl acetateWashing with alcohol and drying;
s8, calcining the composite microspheres;
s9, carrying out vacuum impregnation on the composite microspheres and the phase-change material to obtain the NiFe with the performance of synchronously realizing heat management and microwave absorption 2 O 4 The wave-absorbing and heat-storing integrated material is coated with mineral microspheres.
2. An NiFe of claim 1 2 O 4 The preparation method of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres is characterized by comprising the following steps of: in the step S1, the process of immersing and activating the attapulgite acid liquor mainly comprises the following steps: soaking in acid liquor, performing solid-liquid separation, washing and drying; wherein the acid solution is H + Soaking inorganic strong acid water solution with the concentration of 1-4 mol/L in stirring at the stirring speed of 500-1000r/min at the soaking temperature of 60-90 ℃ for 30-120 min.
3. An NiFe of claim 1 2 O 4 The preparation method of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres is characterized by comprising the following steps of: in the step S2, the modified attapulgite, the isopropanol, the diethylenetriamine and the isopropyl titanate are calculated according to the following parts by weight:
modified attapulgite: 0.2 to 1 portion
Isopropyl alcohol: 30 to 80 portions of
Diethylenetriamine: 0.02 to 0.1 portion
Isopropyl titanate: 2-8 parts of a solvent;
in the step S2, the stirring speed is 500-1000r/min, and the stirring time is 30-60 min; the hydrothermal synthesis temperature is 180-200 ℃, and the hydrothermal synthesis time is 12-36 h.
4. A NiFe according to claim 1 2 O 4 The preparation method of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres is characterized by comprising the following steps of: in step S3, the modified attapulgite-TiO 2 The carbon nano tube slurry, the sodium hexametaphosphate and the water are calculated according to the following parts by weight:
modified attapulgite-TiO 2 :0.5 to 2 portions of
Carbon nanotube slurry: 10 to 50 portions of
Sodium hexametaphosphate: 0.2 to 1 portion
Water: 40-100 parts;
the stirring speed is 600-1000r/min, and the stirring time is 30-60 min; the ultrasonic treatment time is 30-120 min;
the concentration of the carbon nanotube slurry was 10%.
5. An NiFe of claim 1 2 O 4 The preparation method of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres is characterized by comprising the following steps of: in the step S5, the calcining temperature is 300-400 ℃, the calcining time is 1-4 h, and the calcining atmosphere is inert gas.
6. A NiFe according to claim 1 2 O 4 The preparation method of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres is characterized by comprising the following steps of: in step S6, the modified attapulgite-TiO 2 The carbon nano tube slurry, the sodium hexametaphosphate and the water are calculated according to the following parts by weight:
Attapulgite-TiO 2 -carbon nanotube composite microspheres: 0.05 to 0.5 portion
NiCl 2 ·6H 2 O:0.1 to 0.5 portion
FeCl 3 ·6H 2 O:0.2 to 1 portion
Ethylene glycol: 30 to 60 portions of
CH 3 COONa:0.4 to 1 portion
PEG2000: 0.2-0.6 part;
the stirring speed is 500-1000r/min, and the stirring time is 30-60 min; the hydrothermal synthesis temperature is 180-200 ℃, and the hydrothermal synthesis time is 8-24 h.
7. A NiFe according to claim 1 2 O 4 The preparation method of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres is characterized by comprising the following steps of: in the step S7, the dosage relationship of the composite microspheres and the alkali liquor is 1-3: 300-600 wt.%, wherein the alkali liquor is 0.5-2 mol/L NaOH solution; the stirring speed is 500-1000r/min, and the stirring time is 30-60 min; the hydrothermal synthesis temperature is 120-180 ℃, and the hydrothermal synthesis time is 8-24 h.
8. An NiFe of claim 1 2 O 4 The preparation method of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres is characterized by comprising the following steps of: in step S8, the calcination temperature is 300-400 ℃, the calcination time is 1-4 h, the heating rate is 5-10 ℃/min, and the calcination atmosphere is inert gas.
9. NiFe prepared by the preparation method of any one of claims 1-8 2 O 4 The wave-absorbing and heat-storing integrated material is coated with mineral microspheres.
10. A NiFe as claimed in claim 9 2 O 4 The application of the wave-absorbing and heat-storing integrated material coated with the mineral microspheres is characterized in that: electromagnetic interference shielding and thermal energy regulation for high-end electronic devices.
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