CN114906877A - Preparation method of cobalt ferrite capable of being compounded with LDPE (Low-Density polyethylene) to prepare magnetic nano dielectric medium - Google Patents
Preparation method of cobalt ferrite capable of being compounded with LDPE (Low-Density polyethylene) to prepare magnetic nano dielectric medium Download PDFInfo
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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Abstract
A preparation method of cobalt ferrite capable of being compounded with LDPE to prepare magnetic nano dielectric belongs to the technical field of electrical insulation. The invention aims to solve the problem of the existing CoFe 2 O 4 The problem that the powder preparation process is difficult to have good compatibility with LDPE matrix is that CoSO is used 4 ·7H 2 O、FeCl 3 ·6H 2 Dissolving O and NaOH in deionized water respectively to obtain a solution A, B, C; mixing the solution A and the solution B, and dropwise adding the solution C under continuous stirring until the solution C becomes a suspension solution D; transferring the suspension solution D into a hydrothermal reaction kettle, and adding the suspension solution D to the surfaceReacting an active agent for 10-20h at 100-160 ℃ to obtain a reaction solution E; cooling to room temperature, centrifuging and collecting the lower-layer solid matter of the reaction solution E; sequentially washing by using distilled water and heptane to obtain the nano CoFe 2 O 4 Drying the granules in vacuum; and compounding the LDPE and the LDPE by a melt blending method. CoFe prepared in the invention 2 O 4 Can be well compatible with an LDPE matrix under the action of the coated surfactant, and is applied to the field of electrical insulation.
Description
Technical Field
The invention belongs to the technical field of electrical insulation, and particularly relates to a preparation method of a cobalt ferrite capable of being compounded with LDPE (low-density polyethylene) to prepare a magnetic nano dielectric medium.
Background
Low Density Polyethylene (LDPE) is one of the materials mainly used in industry, and has been widely used in the field of electrical insulation due to its excellent dielectric and mechanical properties. Space charge is an important influencing factor for LDPE insulated cables, damaging the LDPE matrix by distorting local electric fields and affecting high field conduction and breakdown phenomena. Space charge accumulation is generally considered to be a major factor in accelerating insulation degradation of high voltage direct current transmission polymers. Researches find that the addition of a small amount of polar groups can greatly reduce the formation of space charges in polyolefin compounds, thereby improving the performance of LDPE-based insulating materials. Currently, inorganic fillers commonly used in LDPE-based composite dielectrics used in insulated power cables are montmorillonite (MMT), TiO 2 、MgO、ZnO、SiO 2 、BaTiO 3 Nanotubes, graphene, and the like. But the research on the magnetic nano dielectric prepared by compounding the LDPE and the magnetic nano particles is less. Magnetic nanocomposite media have the small size effect characteristic of nanomagnetic particles themselves and the inherent properties of the original polymer. In general, magnetic nanocomposite media exhibit novel properties, such as good film formation and processability, in addition to electrical, magnetic and optical properties, and thus can potentially find applications in cell separation, medical diagnostics, high density information storage media, electromagnetic wave absorption materials, electromagnetic devices, and electromagnetic interference suppression. In addition, the conductivity of the material can be reduced due to the introduced magnetic nanoparticlesAnd polarization effects, which can affect the dielectric properties of the material. On the basis of the consideration, the dispersion of the magnetic nanoparticles in the LDPE can possibly reduce the formation of space charge in the LDPE and simultaneously bring magnetism to the LDPE-based composite dielectric, thereby inhibiting the influence of a magnetic field caused by a high-voltage direct-current electric field on the LDPE-based composite dielectric, and even possibly widening the application of the LDPE-based composite dielectric in the fields of electromagnetic wave absorption, electromagnetic devices, electromagnetic interference inhibition and the like.
Spinel type cobalt ferrite (CoFe) 2 O 4 ) Has high saturation magnetization, high magnetocrystalline anisotropy and good chemical stability and wear resistance, has wide application prospect in the field of magnetic recording media and magnetostrictive materials, and is attracted by people. The key to the synthesis of cobalt ferrite is the control of the particle size. At present, the synthesis method of ferrite has two physical and chemical methods. Physically, there are a low-temperature pulverization method, an ultrasonic pulverization method, a high-energy ball milling method, a shock wave pulverization method, a rapid steam cooling method, a thermal plasma method, and the like. The product obtained by physical synthesis has more impurities. Therefore, chemical methods are often adopted for synthesizing the ferrite at present. The chemical method includes a gel method, a hydrothermal method, a chemical coprecipitation method, a vapor deposition method, and the like. For example, Wujuan uses hydrothermal method to prepare composite medium of nanometer cobalt ferrite and body-centered cubic cobalt iron alloy. The sample was subjected to X-ray diffraction analysis and its morphology was observed. The results show that the obtained nanoparticles have a uniform particle size distribution and a cubic spherical shape. Mossbauer Spectroscopy (MS) shows that the synthesized product is composed of nano cobalt ferrite and body-centered cubic cobalt iron alloy. The magnetic hysteresis loop of the composite medium is measured by using VSM, which shows that the composite medium of the nano cobalt ferrite and the body-centered cubic cobalt iron alloy has higher saturation magnetization. The body-centered cubic cobalt-iron alloy is added into the cobalt ferrite to effectively improve the magnetic property of the cobalt ferrite. The preparation method of the nano cobalt ferrite particles by using a hydrothermal method is provided by Chengxue. By changing the reaction temperature and the cobalt content, the magnetic properties of the cobalt ferrite particles are changed. The XRD results show that the higher the temperature, the larger the cobalt ferrite grain size. SEM and TEM analysis results show that the nano cobalt ferrite is in a spherical structure. M D JOSEPH SEBASTIAN et al prepared cobalt ferrite (CoxFe) by thermal decomposition method 3 -xO 4 ) And are favorable toThe changes in the Mossbauer parameters, lattice parameters and crystallite size of the product caused by the Fe/Co changes were studied using X-ray diffraction and Mossbauer spectroscopy techniques. It was verified to be a nano cobalt ferrite particle with a defective structure and found to be optimal for Fe/Co 3:2 in the initial precursor oxide. Chinese patent' A spinel type ferrite CoFe 2 O 4 Hydrothermal preparation method of nanopowder (publication No. CN112408498A) CoFe was prepared by hydrothermal method using cobalt salt, iron salt and ethanolamine as raw materials 2 O 4 A material; chinese patent' A CoFe 2 O 4 /g-C 3 N 4 Magnetic nano material and its preparation method (publication No. CN106582772A) using cobalt salt, iron salt and sodium acetate as raw material and utilizing high-temp. calcination method to prepare CoFe 2 O 4 A material; CoFe 2 O 4 Method for producing nanoparticles (publication No. CN109264792A), CoFe was produced by high-temperature calcination method using cobalt salt, iron salt and oxalate as raw materials 2 O 4 Materials, etc.; but because of these methods in the preparation of CoFe 2 O 4 The problem of complex compatibility with LDPE is not involved, so that the LDPE is not coated with proper surfactant and is difficult to disperse uniformly in an LDPE matrix. At present, CoFe capable of being well compounded with LDPE to prepare magnetic nano dielectric medium 2 O 4 The research on the preparation and modification method of the low-density polyethylene (LDPE) has not been carried out yet, so that the application in the aspect needs a nano-CoFe which can be well compounded with the LDPE to prepare the magnetic nano-dielectric 2 O 4 The preparation method of (1).
Disclosure of Invention
The invention aims to solve the problem of the existing CoFe 2 O 4 The problem that the powder preparation process is difficult to have good compatibility with an LDPE matrix is solved, and the preparation method of the cobalt ferrite which can be compounded with the LDPE to prepare the magnetic nano dielectric medium is provided. The invention takes cobalt sulfate, ferric chloride and sodium hydroxide as raw materials and liquid water as reaction solution to prepare nano CoFe by a hydrothermal method 2 O 4 The particles are surface-modified by different surfactants so as to select proper surfactants to improve the compatibility of the particles with an LDPE matrix, and the method is favorable for the compatibility of the particles with the LDPE matrixFor its application in nano-dielectrics.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of cobalt ferrite capable of being compounded with LDPE to prepare magnetic nano dielectric medium comprises the following steps:
step one, CoSO 4 ·7H 2 O、FeCl 3 ·6H 2 Dissolving O and NaOH in deionized water respectively to obtain a solution A, B, C;
step two, mixing the solution A and the solution B, and dripping the solution C under continuous stirring until the solution C becomes a suspension to obtain a suspension solution D;
transferring the suspension solution D into a hydrothermal reaction kettle, adding a surfactant, and reacting at 100-160 ℃ for 10-20h to obtain a reaction solution E;
step four, cooling the reaction liquid E to room temperature, and centrifuging to collect solid substances at the lower layer of the reaction liquid E; washing the solid matter at the lower layer for 2-5 times by using distilled water and heptane in sequence to obtain the nano CoFe 2 O 4 Drying the granules in vacuum; the nano CoFe 2 O 4 The size of the particles is 8-20 nm.
Step five, LDPE and nano CoFe are mixed by a melt blending method by using a torque rheometer 2 O 4 The particles are compounded to obtain CoFe 2 O 4 a/LDPE composite material.
In the invention, the LDPE is a nonpolar high polymer and has poor compatibility with the nanoparticles, and the nanoparticles are very easy to agglomerate into large clusters in the compounding process, so that the nanoparticles in the prepared composite medium are not uniformly dispersed in a small size, and after the surface of the nanoparticles is coated with a surfactant added in the process of preparing the nanoparticles, the surfactant can simultaneously play a role in reducing the surface energy of the nanoparticles and increasing the compatibility of the nanoparticles with the LDPE, so that the nanoparticles can be uniformly dispersed without large-scale agglomeration in the blending process, and the LDPE is easier for actual industrial production.
Further, in the first step, CoSO in the solution A 4 FeCl in solution B 3 And the mass fraction of NaOH in solution CThe number is 1-20%.
Further, in the second step, the mass ratio of the solution A, B, C is 1: 2-2.5: 6 to 10.
Further, in the third step, the mass fraction of the surfactant is 0.1% -3%.
Further, in the third step, the surfactant is one or two of oleic acid diethanolamide, oleylamine, castor oil polyoxyethylene ether, sorbitan fatty acid ester, polyvinyl alcohol and oleic acid.
Further, in the fourth step, the centrifugal rotating speed is 5000r/min to 10000r/min, and the time is 5min to 20 min.
Further, in the fifth step, the temperature of the vacuum drying is room temperature, and the time is 5-20 min.
Further, in step five, the CoFe 2 O 4 CoFe in/LDPE composite material 2 O 4 The mass percentage of (B) is 1-5%.
Further, in the fifth step, the composite temperature of the torque rheometer is 100-150 ℃, and the rotating speed is set to be 20-200 r/min.
Compared with the prior art, the invention has the beneficial effects that:
firstly, CoFe prepared in the invention 2 O 4 Can be well compatible with LDPE matrix under the action of the coated surfactant, is applied to the field of electrical insulation, and has a dispersion particle size of 100-150 nm.
The method is simple, the size and the crystallinity of the generated particles are easy to control, the raw materials are easy to obtain, the operation is simple, the cost is low, and the method is suitable for large-scale production;
third, CoFe prepared by the invention 2 O 4 The particle size is uniform, and the particle size can be controlled according to the use requirement.
Fourthly, CoFe prepared by the invention 2 O 4 The size of the crystal is 8 nm-20 nm, and the crystal has good crystallinity and dispersibility.
Fifthly, using CoSO 4 ·7H 2 O、FeCl 3 ·6H 2 O and NaOH are used as raw materials, and water heating is utilizedThe method can obtain the nano CoFe with good compatibility with LDPE matrix 2 O 4 A particle;
sixthly, adding proper surfactant to simultaneously control CoFe in hydrothermal reaction 2 O 4 The double effects of the nano-particle size and the improvement of the compatibility of the nano-particle with the LDPE matrix expand the application of the nano-particle in the field of electrical insulation.
Drawings
FIG. 1 is CoFe prepared in example 1 2 O 4 Transmission electron microscopy of nanoparticles;
FIG. 2 is CoFe prepared in example 1 2 O 4 Nanoparticle XRD pattern;
FIG. 3 is CoFe prepared in example 1 2 O 4 SEM image of/LDPE composite dielectric;
FIG. 4 is CoFe prepared in comparative example 2 2 O 4 Transmission electron microscopy of nanoparticles.
Detailed Description
The technical solution of the present invention is further described below with reference to the embodiments and the drawings, but the present invention is not limited thereto, and modifications or equivalent substitutions may be made to the technical solution of the present invention without departing from the spirit of the technical solution of the present invention, and the technical solution of the present invention is covered by the protection scope of the present invention.
Example 1:
CoFe with good compatibility with LDPE matrix 2 O 4 The preparation method comprises the following steps:
firstly, CoSO is added 4 ·7H 2 O、FeCl 3 ·6H 2 Dissolving O and NaOH in deionized water respectively to obtain a solution CoSO 4 、FeCl 3 And a NaOH solution; the CoSO 4 CoSO in solution 4 、FeCl 3 FeCl in solution 3 And NaOH in the NaOH solution by mass percent of 5-20 percent;
secondly, the solution is CoSO 4 And FeCl 3 After the solutions were mixed, the NaOH solution was added dropwise with constant stirring until it became a suspension, giving Co (OH) 2 And Fe (OH) 3 Mixing the suspension solution; CoSO 4 Solutions of、FeCl 3 The mass ratio of the solution to the NaOH solution is 1: 2-2.5: 6 to 10
Thirdly, mixing Co (OH) 2 And Fe (OH) 3 Transferring the mixed suspension solution to a hydrothermal reaction kettle, adding a surfactant, and reacting at 100-160 ℃ for 10-20h to obtain CoFe 2 O 4 Suspending liquid; the mass fraction of the surfactant is 0.5-3%; the surfactant is one or two of oleic acid diethanolamide, oleylamine, castor oil polyoxyethylene ether, sorbitan fatty acid ester, polyvinyl alcohol and oleic acid; the more uniform the grain shape but the larger the size as the reaction time extends.
Fourthly, mixing CoFe 2 O 4 Cooling the suspension to room temperature, centrifuging for 5-20 min at the centrifugation speed of 5000-10000 r/min, pouring out the supernatant, discarding, and collecting the lower-layer solid matter; washing the collected lower-layer solid substance for 3-5 times by using distilled water and heptane in sequence to obtain the nano CoFe 2 O 4 Putting the particles into a vacuum oven to be dried for 8-20 h at room temperature in vacuum;
fifthly, Low Density Polyethylene (LDPE) and nano CoFe are mixed by a melt blending method by utilizing a torque rheometer 2 O 4 Compounding the particles at 110-130 ℃ to obtain CoFe with good compatibility 2 O 4 a/LDPE composite material. The CoFe 2 O 4 CoFe in/LDPE composite material 2 O 4 The mass percentage of (A) is 1% -5%. The rotating speed of the torque rheometer is set to be 100-200 r/min.
CoFe prepared as shown in FIG. 1 2 O 4 The nanoparticles are spheroidal with a size of substantially around 10 nm. As shown in FIG. 2, which is an XRD pattern, it can be seen that peaks (111), (220), (311), (400), (433), (511) and (440) are respectively corresponding to 17.51 °, 30.03 °, 35.57 °, 43.75 °, 53.54 ° 57.48 ° and 62.06 °, which is equivalent to CoFe 2 O 4 (JCPDS-22-1086) Standard cards were matched, confirming that the material produced was CoFe 2 O 4 . The half-peak width shows that the prepared material is about 8-12 nm. CoFe prepared in example 1 2 O 4 After the nano particles and LDPE are compounded according to 1wt percentThe SEM of the tablet fracture shows FIG. 3, from which FIG. 3 shows that CoFe 2 O 4 The particles are uniformly dispersed in the LDPE matrix at around 100 nm.
Comparative example 1:
the comparative example is different from example 1 in that: in the first step, the NaOH solution is replaced by NH with equal mass fraction 3 ·H 2 O; in the second step, the solution is CoSO 4 And FeCl 3 After the solution is mixed, NH is added dropwise under continuous stirring 3 ·H 2 O; as shown in FIG. 4, the resulting CoFe 2 O 4 The particle size is about 50nm and the morphology is less uniform. The other steps and parameters were the same as in example 1.
Claims (9)
1. A preparation method of cobalt ferrite capable of being compounded with LDPE to prepare magnetic nano dielectric medium is characterized by comprising the following steps: the method specifically comprises the following steps:
step one, CoSO 4 ·7H 2 O、FeCl 3 ·6H 2 Dissolving O and NaOH in deionized water respectively to obtain a solution A, B, C;
step two, mixing the solution A and the solution B, and dripping the solution C under continuous stirring until the solution C becomes a suspension to obtain a suspension solution D;
transferring the suspension solution D into a hydrothermal reaction kettle, adding a surfactant, and reacting at 100-160 ℃ for 10-20h to obtain a reaction solution E;
step four, cooling the reaction liquid E to room temperature, and centrifuging to collect solid substances at the lower layer of the reaction liquid E; washing the solid matter at the lower layer by using distilled water and heptane in sequence to obtain the nano CoFe 2 O 4 Drying the granules in vacuum;
step five, LDPE and nano CoFe are mixed by a melt blending method by using a torque rheometer 2 O 4 The particles are compounded to obtain CoFe 2 O 4 a/LDPE composite material.
2. The preparation method of the cobalt ferrite capable of being compounded with LDPE to prepare the magnetic nano dielectric according to claim 1, which is characterized in that: in the first step, theCoSO in solution A 4 FeCl in solution B 3 And the mass fraction of NaOH in the solution C is 1-20%.
3. The method for preparing the cobalt ferrite capable of being compounded with the LDPE for preparing the magnetic nano dielectric according to the claim 1 or 2, which is characterized in that: in the second step, the mass ratio of the solution A, B, C is 1: 2-2.5: 6 to 10.
4. The preparation method of the cobalt ferrite capable of being compounded with LDPE to prepare the magnetic nano dielectric according to claim 1, which is characterized in that: in the third step, the mass fraction of the surfactant is 0.1-3%.
5. The preparation method of the cobalt ferrite capable of being compounded with the LDPE to prepare the magnetic nano dielectric according to claim 1, characterized in that: in the third step, the surfactant is one or two of oleic acid diethanolamide, oleylamine, castor oil polyoxyethylene ether, sorbitan fatty acid ester, polyvinyl alcohol and oleic acid.
6. The preparation method of the cobalt ferrite capable of being compounded with LDPE to prepare the magnetic nano dielectric according to claim 1, which is characterized in that: in the fourth step, the centrifugal rotating speed is 5000r/min to 10000r/min, and the time is 5min to 20 min.
7. The preparation method of the cobalt ferrite capable of being compounded with the LDPE to prepare the magnetic nano dielectric according to claim 1, characterized in that: and fifthly, the temperature of the vacuum drying is room temperature, and the time is 5-20 min.
8. The preparation method of the cobalt ferrite capable of being compounded with the LDPE to prepare the magnetic nano dielectric according to claim 1, characterized in that: in step five, the CoFe 2 O 4 CoFe in/LDPE composite material 2 O 4 The mass percentage of (A) is 1% -5%.
9. The preparation method of the cobalt ferrite capable of being compounded with the LDPE to prepare the magnetic nano dielectric according to claim 1, characterized in that: in the fifth step, the composite temperature of the torque rheometer is 100-150 ℃, and the rotating speed is set to be 20-200 r/min.
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