CN116285343B - Preparation method of high-performance glass fiber radiation damping material - Google Patents

Preparation method of high-performance glass fiber radiation damping material Download PDF

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CN116285343B
CN116285343B CN202310497089.6A CN202310497089A CN116285343B CN 116285343 B CN116285343 B CN 116285343B CN 202310497089 A CN202310497089 A CN 202310497089A CN 116285343 B CN116285343 B CN 116285343B
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glass fiber
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hydrochloric acid
damping material
radiation damping
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CN116285343A (en
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苏本璋
李道林
江源源
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Anhui Tongli New Materials Co ltd
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    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/0083—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive non-fibrous particles embedded in an electrically insulating supporting structure, e.g. powder, flakes, whiskers
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    • C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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Abstract

The application discloses a preparation method of a high-performance glass fiber radiation damping material, and relates to the technical field of electromagnetic shielding materials. The preparation method comprises the following steps: loading ferroferric oxide on graphene oxide to obtain a component I; and uniformly mixing the component I, the modified glass fiber and the base material to obtain the radiation damping material. The material prepared by the application has the advantages of good electromagnetic shielding effect and excellent mechanical property.

Description

Preparation method of high-performance glass fiber radiation damping material
Technical Field
The application relates to the technical field of electromagnetic shielding materials, in particular to a preparation method of a high-performance glass fiber radiation damping material.
Background
With the rapid development of information technology, electronic products and electronic communication bring convenience to life of people, and meanwhile, some troubles such as electromagnetic radiation, electromagnetic interference and the like are generated, so that the normal operation, information safety and human health of electronic equipment are seriously affected. In order to reduce the negative effects of electromagnetic waves, high-performance electromagnetic shielding materials are receiving attention. The electromagnetic shielding is generally realized by using an electrically conductive or magnetically conductive material as a shielding body and sealing the shielding body in a field to be protected, and by the action of the material surface on the reflection of electromagnetic waves or the absorption of electromagnetic waves by the material interior, the attenuation function of electromagnetic waves is realized, thereby realizing the effect of radiation damping.
The conductive polymer-based electromagnetic shielding material is applied to the field of electromagnetic shielding by utilizing the composite application of conductive polymers, magnetic particles and conductive fillers, and the conductive composite material prepared by single fillers is required to meet good shielding efficiency, and generally has the problems of difficult processing, reduced mechanical property and the like due to larger addition amount. In the prior art, the composite material is obtained by blending and compounding nano ferroferric oxide, graphene and base materials, and the magnetic loss of the ferroferric oxide is utilized to attenuate electromagnetic waves, so that the total shielding effectiveness of the composite material is improved. However, the magnetic particle ferroferric oxide has obvious agglomeration phenomenon, and the coating and loading effects of the material and the performances of the final material are affected.
Disclosure of Invention
The application aims to provide a preparation method of a high-performance glass fiber radiation damping material, which solves the following technical problems:
in the composite material prepared in the prior art, the magnetic particle ferroferric oxide has obvious agglomeration phenomenon, and the coating and loading effects of the material and the performances of the final material are affected.
The aim of the application can be achieved by the following technical scheme:
a preparation method of a high-performance glass fiber radiation damping material comprises the following steps:
s1: adding graphene oxide, polyethylene glycol 4000 and ethylene glycol into a reaction bottle, uniformly dispersing, and adding FeCl 3 ·6H 2 O, sodium acetate, heating to 180-200 ℃, preserving heat for 9-12h, washing and drying to obtain a component I;
s2: and uniformly mixing the component I, the modified glass fiber and the base material to obtain the radiation damping material.
As a further aspect of the application: graphene oxide in S1: polyethylene glycol: ethylene glycol: feCl 3 ·6H 2 O: the mass ratio of the sodium acetate is 1:10-50:200-500:4-8:20-40.
As a further aspect of the application: and in S2, a component I: modified glass fiber: the mass ratio of the base materials is 0.1-1:0.05-0.5:5, and the base materials are polyaniline.
As a further aspect of the application: the preparation method of the modified glass fiber comprises the following steps:
a1: after deoiling and washing the glass fiber, adding the glass fiber into nitric acid solution, heating to 55-65 ℃, and preserving heat for 10-30min to obtain pretreated glass fiber;
a2: mixing the pretreated glass fiber, ethyl acetate and gamma-aminopropyl triethoxysilane, and treating at normal temperature for 1-3h to obtain silane modified glass fiber;
a3: immersing silane modified glass fiber into SnCl 2 ·2H 2 Mixing with hydrochloric acid solution of O for 5-10min, and transferring to PdCl 2 Placing the mixture in hydrochloric acid for 2-5min, and placing in sodium hypophosphite solution for 10-30min to obtain activated glass fiber;
a4: placing the activated glass fiber into a plating solution, heating to 88 ℃, and preserving heat for 1-3 hours to obtain a metallized glass fiber;
a5: adding the metallized glass fiber into a methanol solution of stearic acid, heating to 30-40 ℃, and reacting for 12-18h at a constant temperature to obtain the modified glass fiber.
As a further aspect of the application: the specific steps of deoiling and washing the glass fiber are as follows: 10g of glass fibers, 30mL of acetone, 70mL of deionized water were washed with water.
As a further aspect of the application: glass fiber in A1: the solid-to-liquid ratio of the nitric acid solution is 1g:2-10mL, and the nitric acid solution is 60-70wt% nitric acid aqueous solution.
As a further aspect of the application: pretreatment of glass fibers in A2: ethyl acetate: the mass ratio of the gamma-aminopropyl triethoxysilane is 1:10-20:0.1-0.5.
As a further aspect of the application: the SnCl 2 ·2H 2 The mixed solution of the O and the hydrochloric acid is 20-30g/LSnCl 2 ·2H 2 Mixing O and 40-80g/L hydrochloric acid solution in equal volume to obtain; the PdCl 2 The hydrochloric acid mixed solution is 1-2g/L PdCl 2 Mixing with 2-4mL/L hydrochloric acid solution in equal volume to obtain the final product; the sodium hypophosphite solution is 1-3.5wt% sodium hypophosphite solution; silane modified glass fiber: snCl 2 ·2H 2 O hydrochloric acid mixed solution: pdCl 2 Hydrochloric acid mixed solution: the solid-to-liquid ratio of the sodium hypophosphite solution is 10:10-50:10-50:10-50.
As a further aspect of the application: the preparation method of the plating solution in A4 comprises the following steps: sequentially adding 30-40g of nickel sulfate and 5-10g of copper sulfate into a reaction bottle, adding water, mixing, adding 30-50g of nitrilotriacetic acid, stirring uniformly, continuously adding 25-30g of sodium hypophosphite, and finally adding hydrochloric acid to adjust the pH to 4.8 and fixing the volume to 1L.
As a further aspect of the application: metallized glass fiber in A5: the solid-to-liquid ratio of the stearic acid methanol solution is 10g:20-100mL, and the stearic acid methanol solution is 0.05-0.1mol/L stearic acid methanol solution.
The application has the beneficial effects that:
(1) Firstly, a large number of oxygen-containing functional groups such as hydroxyl and carboxyl exist on graphene oxide, the graphene oxide is mixed in glycol, the functional groups are ionized to present electronegativity, ferric trichloride hexahydrate is dissolved and ionized into positively charged iron ions and is attracted to the graphene oxide through electrostatic action, part of the iron ions are reduced into ferrous ions, the iron ions and the ferrous ions form ferroferric oxide crystals on the surface of the graphene oxide through coprecipitation dehydration reaction, meanwhile, the graphene oxide is reduced into graphene, glycol is used as a solvent and a reducing agent, and polyethylene glycol-4000 is used as a surfactant, so that the dispersibility and uniformity of the ferroferric oxide are improved. The ferroferric oxide is used as a main wave-absorbing material of the composite material, and absorbs electromagnetic waves through magnetic loss, so that the wave-absorbing performance of the composite material is promoted; the graphene is used as a matrix, has a high specific surface area, is favorable for loading more wave-absorbing nano particles, and improves the wave-absorbing performance of the material.
(2) According to the material disclosed by the application, modified glass fibers are added, micropores or tiny etching pits are formed on the surfaces of the glass fibers after the glass fibers are roughened by nitric acid, then a silane coupling agent is utilized to react through hydroxyl groups on the surfaces of the glass fibers to form a monomolecular layer on the surfaces of the fibers, the surfaces of the glass fibers have certain hydrophilic capacity, the catalytic activity requirement of chemical plating is met through reduction reaction, nickel and copper coated on the surfaces of the glass fibers are distributed at the interface of a polymer matrix and the glass fibers, meanwhile, the continuous distribution and networking construction of nickel and copper in the material are realized by utilizing the structural characteristics of large length-diameter ratio and easiness in lap joint of the glass fibers, and the composite material has a lower conductive percolation threshold due to the continuous distribution of nickel and copper plated glass fibers, so that the electromagnetic shielding performance of the material is further improved.
(3) The application grafts stearic acid on the metallized glass fiber, and the organic molecular chain grafts to the glass fiber, so that the glass fiber generates a flexible interface layer at the interface, the flexible interface layer is introduced into the composite material, the interface stress generated when the composite material is molded and is acted by external force is relaxed, and the composite material has higher mechanical property.
Detailed Description
The following description will clearly and fully describe the technical solutions of the embodiments of the present application, and it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application.
Example 1
The preparation method of the modified glass fiber comprises the following steps:
a1: washing 10g of glass fiber, 30mL of acetone and 70mL of deionized water, adding into 20mL of 60wt% nitric acid aqueous solution, heating to 55 ℃, and preserving heat for 10min to obtain pretreated glass fiber;
a2: 10g of pretreated glass fiber, 100g of ethyl acetate and 0.1g of gamma-aminopropyl triethoxysilane are mixed and treated for 1 hour at normal temperature to obtain silane modified glass fiber;
A3：SnCl 2 ·2H 2 the mixture of the O and the hydrochloric acid is 20g/L SnCl 2 ·2H 2 Mixing O and 40g/L hydrochloric acid solution in equal volume to obtain; pdCl 2 Hydrochloric acid mixed solution is 1g/L PdCl 2 Mixing with 2mL/L hydrochloric acid solution in equal volume to obtain;
a4: 10g of silane modified glass fiber was immersed in 10mL of SnCl 2 ·2H 2 In the mixed solution of O and hydrochloric acid for 5min, the mixture is transferred to 10mL of PdCl 2 Placing the mixture in hydrochloric acid for 2min and then in 10mL of 1wt% sodium hypophosphite solution for 10min to obtain activated glass fiber;
a5: sequentially adding 30g of nickel sulfate and 5g of copper sulfate into a reaction bottle, adding water, mixing, adding 30g of nitrilotriacetic acid, stirring uniformly, continuously adding 25g of sodium hypophosphite, finally adding hydrochloric acid to adjust the pH to 4.8, and fixing the volume to 1L to prepare a plating solution;
a6: placing the activated glass fiber into a plating solution, heating to 88 ℃, and preserving heat for 1h to obtain a metallized glass fiber;
a7: 10g of the metallized glass fiber is added into 20mL of 0.05mol/L stearic acid methanol solution, the temperature is raised to 30 ℃, and the reaction is carried out for 12 hours under the heat preservation, thus obtaining the modified glass fiber.
Example 2
The preparation method of the modified glass fiber comprises the following steps:
a1: washing 10g of glass fiber, 30mL of acetone and 70mL of deionized water, adding into 20mL of 60wt% nitric acid aqueous solution, heating to 55 ℃, and preserving heat for 10min to obtain pretreated glass fiber;
a2: 10g of pretreated glass fiber, 150g of ethyl acetate and 0.4g of gamma-aminopropyl triethoxysilane are mixed and treated for 2 hours at normal temperature to obtain silane modified glass fiber;
A3：SnCl 2 ·2H 2 the mixture of the O and the hydrochloric acid is 20g/L SnCl 2 ·2H 2 Mixing O and 40g/L hydrochloric acid solution in equal volume to obtain; the PdCl 2 Hydrochloric acid mixed solution is 1g/L PdCl 2 Mixing with 2mL/L hydrochloric acid solution in equal volume to obtain;
a4: 10g of silane modified glass fiber was immersed in 10mL of SnCl 2 ·2H 2 In the mixed solution of O and hydrochloric acid for 10min, transferring to 10mL of PdCl 2 Placing the mixture in hydrochloric acid for 5min and then in 10mL of 1wt% sodium hypophosphite solution for 20min to obtain activated glass fiber;
a5: sequentially adding 30g of nickel sulfate and 5g of copper sulfate into a reaction bottle, adding water, mixing, adding 30g of nitrilotriacetic acid, stirring uniformly, continuously adding 25g of sodium hypophosphite, finally adding hydrochloric acid to adjust the pH to 4.8, and fixing the volume to 1L to prepare a plating solution;
a6: placing the activated glass fiber into a plating solution, heating to 88 ℃, and preserving heat for 1-3 hours to obtain a metallized glass fiber;
a7: 10g of the metallized glass fiber is added into 20mL of 0.05mol/L stearic acid methanol solution, the temperature is raised to 30 ℃, and the reaction is carried out for 12 hours under the heat preservation, thus obtaining the modified glass fiber.
Example 3
The preparation method of the modified glass fiber comprises the following steps:
a1: washing 10g of glass fiber, 30mL of acetone and 70mL of deionized water, adding into 20mL of 60wt% nitric acid aqueous solution, heating to 55 ℃, and preserving heat for 10min to obtain pretreated glass fiber;
a2: mixing 10g of pretreated glass fiber, 200g of ethyl acetate and 0.5g of gamma-aminopropyl triethoxysilane, and treating at normal temperature for 1-3 hours to obtain silane modified glass fiber;
A3：SnCl 2 ·2H 2 the mixture of the O and the hydrochloric acid is 20g/L SnCl 2 ·2H 2 Mixing O and 40g/L hydrochloric acid solution in equal volume to obtain; the PdCl 2 Hydrochloric acid mixed solution is 1g/L PdCl 2 Mixing with 2mL/L hydrochloric acid solution in equal volume to obtain;
a4: 10g of silane modified glass fiber was immersed in 50mL of SnCl 2 ·2H 2 In the mixed solution of O and hydrochloric acid for 10min, the mixture is transferred to 50mL of PdCl 2 Placing the mixture in hydrochloric acid for 5min and then placing the mixture in 50mL of 3.5wt% sodium hypophosphite solution for 30min to obtain activated glass fiber;
a5: sequentially adding 30g of nickel sulfate and 5g of copper sulfate into a reaction bottle, adding water, mixing, adding 30g of nitrilotriacetic acid, stirring uniformly, continuously adding 25g of sodium hypophosphite, finally adding hydrochloric acid to adjust the pH to 4.8, and fixing the volume to 1L to prepare a plating solution;
a6: placing the activated glass fiber into a plating solution, heating to 88 ℃, and preserving heat for 3 hours to obtain a metallized glass fiber;
a7: 10g of the metallized glass fiber is added into 20mL of 0.05mol/L stearic acid methanol solution, the temperature is raised to 30 ℃, and the reaction is carried out for 12 hours under the heat preservation, thus obtaining the modified glass fiber.
Example 4
A preparation method of a high-performance glass fiber radiation damping material comprises the following steps:
s1: adding 10g of graphene oxide, 100g of polyethylene glycol 4000 and 2000g of ethylene glycol into a reaction bottle, uniformly dispersing, and adding 40g of FeCl 3 ·6H 2 O, 200g vinegarSodium carbonate, heating to 180 ℃, preserving heat for 9 hours, washing and drying to obtain a component I;
s3: uniformly mixing 2g of the first component, 0.5g of the modified glass fiber prepared in the embodiment 1 and 50g of polyaniline to obtain the radiation damping material.
Example 5
In comparison with example 4, only the modified glass fiber prepared in example 1 was replaced with the modified glass fiber prepared in example 2 in equal amounts, and the remaining components and steps were completely identical to those of example 4.
Example 6
In comparison with example 4, only the modified glass fiber prepared in example 1 was replaced with the modified glass fiber prepared in example 3 in equal amounts, and the remaining components and steps were completely identical to those of example 4.
Comparative example 1
The preparation method of the modified glass fiber comprises the following steps:
a1: washing 10g of glass fiber, 30mL of acetone and 70mL of deionized water, adding into 20mL of 60wt% nitric acid aqueous solution, heating to 55 ℃, and preserving heat for 10min to obtain pretreated glass fiber;
a2: 10g of pretreated glass fiber, 150g of ethyl acetate and 0.4g of gamma-aminopropyl triethoxysilane are mixed and treated for 2 hours at normal temperature to obtain silane modified glass fiber;
A3：SnCl 2 ·2H 2 the mixture of the O and the hydrochloric acid is 20g/L SnCl 2 ·2H 2 Mixing O and 40g/L hydrochloric acid solution in equal volume to obtain; the PdCl 2 Hydrochloric acid mixed solution is 1g/L PdCl 2 Mixing with 2mL/L hydrochloric acid solution in equal volume to obtain;
a4: 10g of silane modified glass fiber was immersed in 10mL of SnCl 2 ·2H 2 In the mixed solution of O and hydrochloric acid for 10min, transferring to 10mL of PdCl 2 Placing the mixture in hydrochloric acid for 5min and then in 10mL of 1wt% sodium hypophosphite solution for 20min to obtain activated glass fiber;
a5: sequentially adding 30g of nickel sulfate and 5g of copper sulfate into a reaction bottle, adding water, mixing, adding 30g of nitrilotriacetic acid, stirring uniformly, continuously adding 25g of sodium hypophosphite, finally adding hydrochloric acid to adjust the pH to 4.8, and fixing the volume to 1L to prepare a plating solution;
a6: and (3) placing the activated glass fiber into a plating solution, heating to 88 ℃, and preserving heat for 1-3 hours to obtain the modified glass fiber.
Comparative example 2
The preparation method of the modified glass fiber comprises the following steps:
A1：SnCl 2 ·2H 2 the mixture of the O and the hydrochloric acid is 20g/L SnCl 2 ·2H 2 Mixing O and 40g/L hydrochloric acid solution in equal volume to obtain; the PdCl 2 Hydrochloric acid mixed solution is 1g/L PdCl 2 Mixing with 2mL/L hydrochloric acid solution in equal volume to obtain;
a2: 10g of glass fibers were immersed in 10mL of SnCl 2 ·2H 2 In the mixed solution of O and hydrochloric acid for 10min, transferring to 10mL of PdCl 2 Placing the mixture in hydrochloric acid for 5min and then in 10mL of 1wt% sodium hypophosphite solution for 20min to obtain activated glass fiber;
a3: sequentially adding 30g of nickel sulfate and 5g of copper sulfate into a reaction bottle, adding water, mixing, adding 30g of nitrilotriacetic acid, stirring uniformly, continuously adding 25g of sodium hypophosphite, finally adding hydrochloric acid to adjust the pH to 4.8, and fixing the volume to 1L to prepare a plating solution;
a4: placing the activated glass fiber into a plating solution, heating to 88 ℃, and preserving heat for 1-3 hours to obtain a metallized glass fiber;
a5: 10g of the metallized glass fiber is added into 20mL of 0.05mol/L stearic acid methanol solution, the temperature is raised to 30 ℃, and the reaction is carried out for 12 hours under the heat preservation, thus obtaining the modified glass fiber.
Comparative example 3
The preparation method of the modified glass fiber comprises the following steps:
A1：SnCl 2 ·2H 2 the mixture of the O and the hydrochloric acid is 20g/L SnCl 2 ·2H 2 Mixing O and 40g/L hydrochloric acid solution in equal volume to obtain; the PdCl 2 Hydrochloric acid mixed solution is 1g/L PdCl 2 Mixing with 2mL/L hydrochloric acid solution in equal volume to obtain;
a2: 10g of glass fibers were immersed in 10mL of SnCl 2 ·2H 2 In the mixed solution of O and hydrochloric acid for 10min, transferring to 10mL of PdCl 2 The mixture of hydrochloric acid for 5min is placed in 10mL of 1wt% sodium hypophosphiteThe activated glass fiber is obtained after 20min in the solution;
a3: sequentially adding 30g of nickel sulfate and 5g of copper sulfate into a reaction bottle, adding water, mixing, adding 30g of nitrilotriacetic acid, stirring uniformly, continuously adding 25g of sodium hypophosphite, finally adding hydrochloric acid to adjust the pH to 4.8, and fixing the volume to 1L to prepare a plating solution;
a4: and (3) placing the activated glass fiber into a plating solution, heating to 88 ℃, and preserving heat for 1-3 hours to obtain the modified glass fiber.
Comparative example 4
A preparation method of a high-performance glass fiber radiation damping material comprises the following steps:
s1: 40g FeCl 3 ·6H 2 O, 200g of sodium acetate, heating to 180 ℃, preserving heat for 9 hours, washing and drying to obtain a component I;
s2: adding 10g of graphene oxide, 100g of polyethylene glycol 4000 and 2000g of ethylene glycol into a reaction bottle, uniformly dispersing, adding the first component, and uniformly mixing to obtain the second component;
s3: uniformly mixing 2g of the second component, 0.5g of the modified glass fiber prepared in the embodiment 1 and 50g of polyaniline to obtain the radiation damping material.
Comparative example 5
In comparison with example 4, the modified glass fiber prepared in example 1 was merely replaced with the modified glass fiber prepared in comparative example 1 in equal amounts, and the remaining components and steps were completely identical to those of example 4.
Comparative example 6
In comparison with example 4, the modified glass fiber prepared in example 1 was merely replaced with the modified glass fiber prepared in comparative example 2 in equal amounts, and the remaining components and steps were completely identical to those of example 4.
Comparative example 7
In comparison with example 4, the modified glass fiber prepared in example 1 was merely replaced with the modified glass fiber prepared in comparative example 3 in equal amounts, and the remaining components and steps were completely identical to those of example 4.
Comparative example 8
In comparison with example 4, only the modified glass fibers prepared in example 1 were replaced with glass fibers in equal amounts, and the remaining components and steps were completely identical to those of example 4.
Performance detection
(1) Electromagnetic parameters: the prepared materials of examples 4-6 and comparative examples 5-8 are used as samples to be tested, an HP8722ES type vector grid analyzer of Beijing aviation materials research institute is used for testing electromagnetic parameters of the samples to be tested by adopting a coaxial transmission line method, the samples to be tested and paraffin are mixed and melted, the filling amount of the samples to be tested accounts for 40% of the total mass, annular discs for testing are prepared in a die, the filling amount of sample powder is 40%, and the testing frequency range is 1-18GHz;
(2) Microwave absorption performance: from the electromagnetic parameter test, complex dielectric constants (epsilon=epsilon '-j epsilon') and complex magnetic permeability (mu=mu '-j mu') are obtained, and according to a relation formula between the reflection loss and the complex dielectric constants, the complex magnetic permeability, the electromagnetic wave frequency and the sample thickness, the microwave absorption performance of the material with different thicknesses is calculated, wherein the calculation result is shown in table 1:
table 1: examples 4 to 6 and comparative examples 5 to 8 were shown to have microwave absorption properties
As can be seen from Table 1, the radiation damping material prepared by the present application has excellent electromagnetic shielding function.
The foregoing describes one embodiment of the present application in detail, but the description is only a preferred embodiment of the present application and should not be construed as limiting the scope of the application. All equivalent changes and modifications within the scope of the present application are intended to be covered by the present application.

Claims (8)

1. The preparation method of the high-performance glass fiber radiation damping material is characterized by comprising the following steps of:
s1: adding graphene oxide, polyethylene glycol 4000 and ethylene glycol into a reaction bottle, uniformly dispersing, and adding FeCl 3 ·6H 2 O, sodium acetate, heating to 180-200 ℃, preserving heat for 9-12h, washing and drying to obtain a component I;
s2: uniformly mixing the component I, the modified glass fiber and the base material to obtain a radiation damping material;
the preparation method of the modified glass fiber comprises the following steps:
a1: after deoiling and washing the glass fiber, adding the glass fiber into nitric acid solution, heating to 55-65 ℃, and preserving heat for 10-30min to obtain pretreated glass fiber;
a2: mixing the pretreated glass fiber, ethyl acetate and gamma-aminopropyl triethoxysilane, and treating at normal temperature for 1-3h to obtain silane modified glass fiber;
a3: immersing silane modified glass fiber into SnCl 2 ·2H 2 Mixing with hydrochloric acid solution of O for 5-10min, and transferring to PdCl 2 Placing the mixture in hydrochloric acid for 2-5min, and placing in sodium hypophosphite solution for 10-30min to obtain activated glass fiber;
a4: placing the activated glass fiber into a plating solution, heating to 88 ℃, and preserving heat for 1-3 hours to obtain a metallized glass fiber;
a5: adding the metallized glass fiber into a methanol solution of stearic acid, heating to 30-40 ℃, and reacting for 12-18h at a constant temperature to obtain the modified glass fiber.
2. The method for preparing the high-performance glass fiber radiation damping material according to claim 1, wherein graphene oxide in S1: polyethylene glycol: ethylene glycol: feCl 3 ·6H 2 O: the mass ratio of the sodium acetate is 1:10-50:200-500:4-8:20-40.
3. The method for preparing a high performance glass fiber radiation damping material according to claim 1, wherein the component one of S2: modified glass fiber: the mass ratio of the base materials is 0.1-1:0.05-0.5:5, and the base materials are polyaniline.
4. The method for preparing the high-performance glass fiber radiation damping material according to claim 1, wherein the glass fiber in A1: the solid-to-liquid ratio of the nitric acid solution is 1g:2-10mL, and the nitric acid solution is 60-70wt% nitric acid aqueous solution.
5. The method for preparing a high performance glass fiber radiation damping material according to claim 1, wherein the glass fiber is pretreated in A2: ethyl acetate: the mass ratio of the gamma-aminopropyl triethoxysilane is 1:10-20:0.1-0.5.
6. The method for preparing the high-performance glass fiber radiation damping material according to claim 1, wherein the SnCl is prepared by the following steps 2 ·2H 2 The mixture of the O and the hydrochloric acid is 20-30g/L SnCl 2 ·2H 2 Mixing O and 40-80g/L hydrochloric acid solution in equal volume to obtain; the PdCl 2 The hydrochloric acid mixed solution is 1-2g/L PdCl 2 Mixing with 2-4mL/L hydrochloric acid solution in equal volume to obtain the final product; the sodium hypophosphite solution is 1-3.5wt% sodium hypophosphite solution; silane modified glass fiber: snCl 2 ·2H 2 O hydrochloric acid mixed solution: pdCl 2 Hydrochloric acid mixed solution: the solid-to-liquid ratio of the sodium hypophosphite solution is 10:10-50:10-50:10-50.
7. The method for preparing the high-performance glass fiber radiation damping material according to claim 1, wherein the preparation method of the plating solution in A4 is as follows: sequentially adding 30-40g of nickel sulfate and 5-10g of copper sulfate into a reaction bottle, adding water, mixing, adding 30-50g of nitrilotriacetic acid, stirring uniformly, continuously adding 25-30g of sodium hypophosphite, and finally adding hydrochloric acid to adjust the pH to 4.8 and fixing the volume to 1L.
8. The method for preparing a high performance glass fiber radiation damping material according to claim 1, wherein the metallized glass fiber in A5: the solid-to-liquid ratio of the stearic acid methanol solution is 10g:20-100mL, and the stearic acid methanol solution is 0.05-0.1mol/L stearic acid methanol solution.
CN202310497089.6A 2023-05-05 2023-05-05 Preparation method of high-performance glass fiber radiation damping material Active CN116285343B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104860303A (en) * 2015-04-27 2015-08-26 安徽大学 Preparation method of reduced graphene oxide/ferroferric oxide/CdSeTe@ZnS@SiO2 nanocomposite
CN107265888A (en) * 2017-07-13 2017-10-20 济南大学 A kind of Fe3O4 of high magnetic permeability is grapheme modified/glass fiber compound material and preparation method thereof
CN108546547A (en) * 2018-04-02 2018-09-18 西安交通大学 A kind of preparation method of multiple spectra composite wave-absorbing agent
CN109932449A (en) * 2019-04-03 2019-06-25 东北师范大学 A kind of preparation of magnetic porous graphene and its rapid detection method applied to triclosan at low triclosan concentrations in water
CN110835447A (en) * 2019-12-02 2020-02-25 西安交通大学 Ku waveband composite wave-absorbing material and preparation method thereof
KR20220029821A (en) * 2020-08-28 2022-03-10 주식회사 데브 Electromagnetic shielding material comprising malic acid grafted polypropylene, graphene oxide and glass fiber coated with graphene oxide and MAXene

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104860303A (en) * 2015-04-27 2015-08-26 安徽大学 Preparation method of reduced graphene oxide/ferroferric oxide/CdSeTe@ZnS@SiO2 nanocomposite
CN107265888A (en) * 2017-07-13 2017-10-20 济南大学 A kind of Fe3O4 of high magnetic permeability is grapheme modified/glass fiber compound material and preparation method thereof
CN108546547A (en) * 2018-04-02 2018-09-18 西安交通大学 A kind of preparation method of multiple spectra composite wave-absorbing agent
CN109932449A (en) * 2019-04-03 2019-06-25 东北师范大学 A kind of preparation of magnetic porous graphene and its rapid detection method applied to triclosan at low triclosan concentrations in water
CN110835447A (en) * 2019-12-02 2020-02-25 西安交通大学 Ku waveband composite wave-absorbing material and preparation method thereof
KR20220029821A (en) * 2020-08-28 2022-03-10 주식회사 데브 Electromagnetic shielding material comprising malic acid grafted polypropylene, graphene oxide and glass fiber coated with graphene oxide and MAXene

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