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Green industrial preparation method of ferroferric oxide/reduced graphene oxide and wave-absorbing resin composite material prepared from ferroferric oxide/reduced graphene oxide

A technology of ferroferric oxide and composite materials, which is applied in the field of nano-electromagnetic functional materials, can solve the problems that the wave-absorbing particles cannot be environmentally friendly and the electromagnetic parameters in the thickness direction are not uniform, and achieve excellent impedance matching performance, safe production process, The effect of guaranteeing uniformity

Active Publication Date: 2022-05-27
ZHONGBEI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention solves the problem that the preparation of ferroferric oxide / graphene nanocomposite wave-absorbing particles cannot be environmentally friendly, and when using ferroferric oxide / reduced graphene oxide as a wave-absorbing agent and resin as a matrix to prepare a wave-absorbing composite material There will be a problem of uneven electromagnetic parameters in the thickness direction, and a green industrial preparation method of ferric oxide / reduced graphene oxide and its wave-absorbing resin composite material are provided

Method used

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  • Green industrial preparation method of ferroferric oxide/reduced graphene oxide and wave-absorbing resin composite material prepared from ferroferric oxide/reduced graphene oxide
  • Green industrial preparation method of ferroferric oxide/reduced graphene oxide and wave-absorbing resin composite material prepared from ferroferric oxide/reduced graphene oxide
  • Green industrial preparation method of ferroferric oxide/reduced graphene oxide and wave-absorbing resin composite material prepared from ferroferric oxide/reduced graphene oxide

Examples

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Effect test

Embodiment 1

[0044]A green industrial preparation method of Fe3O4 / reduced graphene oxide nano-wave absorbing particles: adding distilled water, and preparing 1400g of industrial graphene oxide slurry with a concentration of 1.0wt% into 21L of graphene oxide with a concentration of 0.67mg / mL Dispersion (mass of graphene oxide is 14 g). 326.48g FeCl 3 ·6H 2 O and 240.16g FeCl 2 ·4H 2 O was dissolved in water to prepare 7L of iron salt mixed solution with a concentration of 0.08g / L. The prepared iron salt mixed solution and graphene oxide dispersion were poured into the reactor, and nitrogen protection was introduced. Under the mechanical stirring of 200r / min, the NaOH aqueous solution of 0.2g / mL was added dropwise after being heated to 90°C, until The pH of the solution reached 10-11, and then the reaction was carried out at 90 °C for 2 h under the mechanical stirring of 200 r / min. After the first-stage reaction was completed, 21 g of ascorbic acid was added to the reaction kettle, kept...

Embodiment 2

[0046] A green industrial preparation method of ferric oxide / reduced graphene oxide nano-absorbing particles: adding distilled water, and preparing 1000 g of industrial graphene oxide slurry with a concentration of 1.0 wt % into 15 L of graphene oxide with a concentration of 0.67 mg / mL Dispersion (mass of graphene oxide is 10 g). 233g FeCl 3 ·6H 2 O and 172g FeCl 2 ·4H 2 O was dissolved in water to prepare 5L of iron salt mixed solution with a concentration of 0.08g / L. The prepared iron salt mixed solution and graphene oxide dispersion were poured into the reaction kettle, and nitrogen protection was introduced. Under the mechanical stirring of 200r / min, the ammonia water of mass fraction 25wt% was added dropwise after being heated to 90°C until the solution was The pH was 10-11, and then the reaction was carried out at 90 °C for 3 h under the mechanical stirring of 200 r / min. After the first-stage reaction was completed, 15 g of ascorbic acid was added to the reaction ke...

Embodiment 3

[0048] A specific preparation method of ferric oxide / reduced graphene oxide / epoxy resin wave-absorbing composite material: weigh 129.72g of bisphenol A epoxy resin E-51, add 103.26g of curing agent hexahydrophthalic anhydride (HHPA) , at 35 ° C, according to the particle filling amount of 30%, add the weighed ferric oxide / reduced graphene oxide nano-absorbing particles prepared in Example 1, after uniform dispersion, add 1.16g accelerator 2,4, 6-Tris(dimethylaminomethyl)phenol, after uniform dispersion, a blending system of particles and epoxy resin is obtained, which is divided into three equal parts.

[0049] Apply mold release agent to the mold with the inner size of 250×250×20mm, and put it in the oven to preheat. In the process of layered pouring, the first blend of nano-wave absorbing particles and epoxy resin was poured into the mold and leveled, heated at 100 °C for 1 hour to reach a gel state, and then the second The blend of nano-absorbing particles and epoxy resin ...

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Abstract

The invention provides a green industrial preparation method of ferroferric oxide / reduced graphene oxide and a wave-absorbing resin composite material prepared from the ferroferric oxide / reduced graphene oxide. The preparation method comprises the following steps: heating and stirring a graphene oxide dispersion liquid and a mixed solution of bivalent and trivalent iron salts in a reaction kettle, adjusting the pH value with an alkaline solution, carrying out a first-stage reaction, adding a reducing agent, carrying out a second-stage reaction, carrying out precipitation separation in a strong magnetic field after the reaction is completed, and drying the washed precipitate to obtain the graphene oxide / ferric iron salt composite material. The ferroferric oxide / reduced graphene oxide nano wave-absorbing particles are obtained. According to the method, toxic and harmful raw materials are not used, and good controllability and stability are achieved. In addition, the ferroferric oxide / reduced graphene oxide / epoxy resin wave-absorbing composite material is prepared by using a layered curing process. Dielectric loss and magnetic loss of electromagnetic waves are effectively combined, and the problem of sedimentation of functional particles with large specific gravity in the blending and curing process of the functional particles and resin is solved through a simple process with good controllability and stability.

Description

technical field [0001] The invention belongs to the technical field of nano-electromagnetic functional materials, in particular to a green industrial preparation method of ferric oxide / reduced graphene oxide and a wave-absorbing resin composite material thereof. Background technique [0002] The widespread use of electronic equipment has provided a powerful boost to economic construction and military development. However, the electromagnetic radiation and electromagnetic interference it produces not only affects the use of electronic equipment, but also endangers people's health. One of the key technologies to effectively control electromagnetic radiation pollution and reduce its harm is to develop high-performance electromagnetic wave absorbing materials. Among them, two-dimensional materials represented by graphene have unique microstructure, physicochemical properties and good dielectric loss capability. , has always been a research hotspot in the field of electromagneti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K3/22C08K3/04C08K9/04C08L63/02C08L63/00C01B32/184C01G49/08
CPCC08K3/22C08K3/042C08K9/04C01G49/08C01B32/184C01P2006/42C08L63/00Y02E60/10
Inventor 刘亚青韩冠宇樊益泽黄绍梁温凯赵贵哲
Owner ZHONGBEI UNIV