CN110294912A - A kind of preparation method of conductive polymer base composite electric magnetic shielding material - Google Patents
A kind of preparation method of conductive polymer base composite electric magnetic shielding material Download PDFInfo
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- CN110294912A CN110294912A CN201910581964.2A CN201910581964A CN110294912A CN 110294912 A CN110294912 A CN 110294912A CN 201910581964 A CN201910581964 A CN 201910581964A CN 110294912 A CN110294912 A CN 110294912A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
- C08L33/12—Homopolymers or copolymers of methyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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Abstract
The invention discloses a kind of preparation methods of conductive polymer base composite electric magnetic shielding material.First with nano-cellulose and the graphene oxide stable Pickering emulsion technology containing polymer altogether, and nano-cellulose/graphene oxide/polymer composites are obtained in conjunction with suction filtration technology, then nano-cellulose/redox graphene/polymer compound electromagnetic shielding material, as conductive polymer base composite electric magnetic shielding material are prepared using hydrazine hydrate reduction and two step heat pressing process technologies.Preparation process of the present invention is simple, and raw material is easy to get, and quality of materials obtained is light, thickness is small, has good electric conductivity, and meets domestic electromagnetic shielding material requirement in X-band, there is good application prospect in terms of domestic electromagnetic shielding material.
Description
Technical field
The invention belongs to functional form field of nanocomposite materials, in particular to a kind of to be based on nano-cellulose and graphite oxide
The Pickering emulsion technology of alkene jointly stabilizing is come the method for preparing highly conductive type polymer matrix composite electromagnetic shield materials.
Background technique
Current social, the same atmosphere pollution of electromagnetic radiation pollution, pollution of waterhead and noise pollution are referred to as human residential environment
" four big pollution ", drastically influence the health of the mankind, therefore solve the problems, such as electromagnetic radiation pollution, exploitation and prepare novel property
The excellent electromagnetic shielding material of energy is the task of top priority.Electromagnetic shielding material can be divided into Types Below: metal electromagnetic shielding material,
Polymer matrix electromagnetic shielding material and novel shielding material.Its density of material of metal electromagnetic shielding material is big, it is perishable plus
Work performance is poor, at high cost and electromagnet shield effect modulability is poor.So electromagnetic shielding material research in the past 20 years is more intended to
Polymer matrix electromagnetic shielding material.
Graphene has excellent mechanics, optically and electrically performance, is electrical-conductive nanometer in polymer matrix electromagnetic shielding material
The preferential selection of particle.But its precursor material graphene oxide contain a large amount of oxygen-containing functional group such as-OH ,-C (O) C- ,-
COOH ,-COO- etc. possess good hydrophilicity, difficult evenly dispersed in a polymer matrix to limit its application.Cause
This, the present invention develops a kind of simple process, low in cost, green non-pollution, graphene using Pickering emulsion technology
The preparation method of evenly dispersed highly conductive type composite electromagnetic shield materials in a polymer matrix has certain reality meaning
Justice.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of conductive polymer base composite electric magnetic shielding material.
Thinking of the present invention: contain the O/ of the organic solution of polymer using graphene oxide and nano-cellulose jointly stabilizing
W type Pickering emulsion technology, prepares based on redox graphene and receives in conjunction with suction filtration, reduction and heat pressing process technology
The polymer matrix composite of the three-dimensional net structure enhancing of rice cellulose.In a polymer matrix by reduction-oxidation graphite
The formation of three-dimensional net structure improves its dispersibility in the base, and then obtains having the polymer matrix of high conductivity compound
Electromagnetic shielding material.
Specific steps are as follows:
(1) aqueous dispersions that are blended of preparation of nano cellulose and graphene oxide, wherein the mass concentration of nano-cellulose be
0.01 ~ 0.1%, the mass concentration of graphene oxide is 0.1 ~ 1%.
(2) polymer solution that the blending aqueous dispersions and mass concentration prepared step (1) are 0.5 ~ 7% is according to volume
Than being mixed for 1 ~ 10:1, ultrasonic emulsification 0.5 ~ 30 minute, obtains nano-cellulose and oxygen under the ultrasonic wave of 100 ~ 1000W
The oil-in-water type Pickering lotion of graphite alkene jointly stabilizing obtains emulsion gel after standing 12 ~ 24 hours；Wherein it polymerize
Object solution is the solution of polymer dissolution in organic solvent.
(3) emulsion gel obtained in step (2) is filtered, and had used in polymer solution in step (2)
The mixed solution of solvent and ethyl alcohol washs 4 ~ 6 times, obtains nano-cellulose/graphene oxide/polymer cake.
(4) hydrazine hydrate solution that mass concentration is 1 ~ 20% is prepared.
(5) filter cake obtained in step (3) is immersed in the hydrazine hydrate solution of step (4) preparation, at 60 ~ 100 DEG C
0.5 ~ 3h is reacted, then filter cake is placed in hot pressing die in 60 ~ 100 DEG C of baking oven to the reaction was continued and is dried to leather hard
State.
(6) leather hard filter cake obtained in step (5) is put into flat-bed press and carries out hot pressing, obtain nanofiber
Element/redox graphene/polymer compound electromagnetic shielding material, as conductive polymer base composite electric magnetic shielding material.
The nano-cellulose is cellulosic material of at least one-dimensional scale in nanometer range, including is mentioned from raw material
Take the Cellulose nanocrystal and cellulose Nanowire with appearance structure of preparation, chinese raw materials be cotton, timber, bamboo or
Crudefiber crop.
The graphene oxide is monolithic layer structure, and lamellar spacing is 0.8 ~ 1.2nm.
The polymer is non-soluble polymer, specially polystyrene, polycarbonate, polyamide, polylactic acid, poly- first
Base methyl acrylate, polycaprolactone, poly lactide-glycolide acid or cellulose acetate.
The organic solvent is methylene chloride, 1,2- dichloroethanes, chloroform, n-hexane or hexamethylene.
Heat pressing process in the step (6) uses two-step method: hot pressing under conditions of 80 DEG C, pressure is 0.5MPa first
5 ~ 15min further removes the organic solvent in filter cake；Then 150 DEG C, pressure be 12MPa under conditions of hot pressing 15 ~
60min。
The purity of the chemical reagent and raw material is to analyze the pure and above purity.
The advantages of the method for the present invention:
(1) the method for the present invention is suitable for extracting the nano-cellulose of the different-shape of preparation from various raw material, utilizes various systems
The graphene oxide and various water-insoluble polymer of Preparation Method preparation, it is easy to promote large-scale.
(2) agents useful for same is all common agents in the method for the present invention, cheap, and preparation process is easy quickly.
(3) composite electromagnetic shield materials made from the method for the present invention, light weight, thickness is small, has good electric conductivity, and
And meet domestic electromagnetic shielding material requirement in X-band, there is good application prospect in terms of domestic electromagnetic shielding material.
Detailed description of the invention
Fig. 1 is the digital photograph of conductive polymer base composite electric magnetic shielding material prepared by the embodiment of the present invention 1.
Fig. 2 is the conductivity of conductive polymer base composite electric magnetic shielding material prepared by the embodiment of the present invention 1,2,3 and 4
Test chart.
Fig. 3 is the conductive polymer base composite electric magnetic shielding material of the preparation of the embodiment of the present invention 1,2,3 and 4 in X-band
The shield effectiveness curve of (8.2 ~ 12.4GHz).
Specific embodiment
The present invention is described further combined with specific embodiments below, but the present invention is not limited to following embodiment, with
Chemical reagent used in lower embodiment and raw material are that analysis is pure.
Embodiment 1:
Aqueous dispersions are blended as water phase, the poly- first of 2wt% with 0.3wt% graphene oxide using 0.03wt% is cellulose nano-fibrous
1, the 2- dichloroethane solution of base methyl acrylate mixes ultrasound 30min as oily phase, according to water oil volume ratio 3:1, makes its cream
It is melted into the stable oil-in-water type Pickering lotion of nano-cellulose/graphene oxide, and stands 24 hours and obtains emulsion gel.
Then emulsion gel is filtered, and is washed with the mixed solutions for many times of 1,2- dichloroethanes and ethyl alcohol, finally obtain nanometer
Cellulose/graphene oxide/polymethyl methacrylate filter cake.Then gained filter cake is immersed in the water that mass concentration is 3.0%
It closes after being reacted 1 hour at 80 DEG C in hydrazine solution, filter cake is replaced in hot pressing die and the reaction was continued in 80 DEG C of baking ovens
And it is dried to leather hard.Finally half dry state filter cake is put into flat-bed press and carries out two step hot pressing, first at 80 DEG C, pressure
Power is hot pressing 5min under conditions of 0.5MPa, further removes the organic solvent in filter cake；Then at 150 DEG C, pressure 12MPa
Under conditions of hot pressing 30min to get arrive nano-cellulose/redox graphene/polymethyl methacrylate compound electric magnetic cup
Cover material.
Embodiment 2:
Aqueous dispersions are blended as water phase, the poly- first of 2wt% with 0.3wt% graphene oxide using 0.03wt% is cellulose nano-fibrous
1, the 2- dichloroethane solution of base methyl acrylate mixes ultrasound 30min as oily phase, according to water oil volume ratio 4:1, makes its cream
It is melted into the stable oil-in-water type Pickering lotion of nano-cellulose/graphene oxide, and stands 24 hours and obtains emulsion gel.
Then emulsion gel is filtered, and is washed with the mixed solutions for many times of 1,2- dichloroethanes and ethyl alcohol, finally obtain nanometer
Cellulose/graphene oxide/polymethyl methacrylate filter cake.Then gained filter cake is immersed in the water that mass concentration is 3.0%
It closes after being reacted 1 hour at 80 DEG C in hydrazine solution, filter cake is replaced in hot pressing die and the reaction was continued in 80 DEG C of baking ovens
And it is dried to leather hard.Finally half dry state filter cake is put into flat-bed press and carries out two step hot pressing, first at 80 DEG C, pressure
Power is hot pressing 5min under conditions of 0.5MPa, further removes the organic solvent in filter cake；Then at 150 DEG C, pressure 12MPa
Under conditions of hot pressing 30min to get arrive nano-cellulose/redox graphene/polymethyl methacrylate compound electric magnetic cup
Cover material.
Embodiment 3:
Aqueous dispersions are blended as water phase, the poly- first of 5wt% with 0.3wt% graphene oxide using 0.03wt% is cellulose nano-fibrous
1, the 2- dichloroethane solution of base methyl acrylate mixes ultrasound 30min as oily phase, according to water oil volume ratio 3:1, makes its cream
It is melted into the stable oil-in-water type Pickering lotion of nano-cellulose/graphene oxide, and stands 24 hours and obtains emulsion gel.
Then emulsion gel is filtered, and is washed with the mixed solutions for many times of 1,2- dichloroethanes and ethyl alcohol, finally obtain nanometer
Cellulose/graphene oxide/polymethyl methacrylate filter cake.Then gained filter cake is immersed in the water that mass concentration is 3.0%
It closes after being reacted 1 hour at 80 DEG C in hydrazine solution, filter cake is replaced in hot pressing die and the reaction was continued in 80 DEG C of baking ovens
And it is dried to leather hard.Finally half dry state filter cake is put into flat-bed press and carries out two step hot pressing, first at 80 DEG C, pressure
Power is hot pressing 5min under conditions of 0.5MPa, further removes the organic solvent in filter cake；Then at 150 DEG C, pressure 12MPa
Under conditions of hot pressing 30min to get arrive nano-cellulose/redox graphene/polymethyl methacrylate compound electric magnetic cup
Cover material.
Embodiment 4:
Aqueous dispersions are blended as water phase, the poly- first of 5wt% with 0.3wt% graphene oxide using 0.03wt% is cellulose nano-fibrous
1, the 2- dichloroethane solution of base methyl acrylate mixes ultrasound 30min as oily phase, according to water oil volume ratio 4:1, makes its cream
It is melted into the stable oil-in-water type Pickering lotion of nano-cellulose/graphene oxide, and stands 24 hours and obtains emulsion gel.
Then emulsion gel is filtered, and is washed with the mixed solutions for many times of 1,2- dichloroethanes and ethyl alcohol, finally obtain nanometer
Cellulose/graphene oxide/polymethyl methacrylate filter cake.Then gained filter cake is immersed in the water that mass concentration is 3.0%
It closes after being reacted 1 hour at 80 DEG C in hydrazine solution, filter cake is replaced in hot pressing die and the reaction was continued in 80 DEG C of baking ovens
And it is dried to leather hard.Finally half dry state filter cake is put into flat-bed press and carries out two step hot pressing, first at 80 DEG C, pressure
Power is hot pressing 5min under conditions of 0.5MPa, further removes the organic solvent in filter cake；Then at 150 DEG C, pressure 12MPa
Under conditions of hot pressing 30min to get arrive nano-cellulose/redox graphene/polymethyl methacrylate compound electric magnetic cup
Cover material.
Only about 0.16mm(is shown in attached drawing 1 to conductive polymer base composite electric magnetic shielding material thickness obtained in embodiment 1),
And there is excellent electric conductivity.The conductivity of the resulting conductive polymer base composite electric magnetic shielding material of embodiment 2 is up to
Attached drawing 2 is seen to 88.13S/m().And its electromagnet shield effect in each frequency of X-band (8.2 ~ 12.4GHz) keeps stablizing,
Its average shield effectiveness is optimal, reaches 26.10dB(and sees attached drawing 3).
Claims (1)
1. a kind of preparation method of conductive polymer base composite electric magnetic shielding material, it is characterised in that specific steps are as follows:
(1) aqueous dispersions that are blended of preparation of nano cellulose and graphene oxide, wherein the mass concentration of nano-cellulose be
0.01 ~ 0.1%, the mass concentration of graphene oxide is 0.1 ~ 1%；
(2) polymer solution that the blending aqueous dispersions and mass concentration prepared step (1) are 0.5 ~ 7% is 1 according to volume ratio
~ 10:1 is mixed, ultrasonic emulsification 0.5 ~ 30 minute under the ultrasonic wave of 100 ~ 1000W, obtains nano-cellulose and oxidation stone
The oil-in-water type Pickering lotion of black alkene jointly stabilizing obtains emulsion gel after standing 12 ~ 24 hours；Wherein polymer is molten
Liquid is the solution of polymer dissolution in organic solvent；
(3) emulsion gel obtained in step (2) is filtered, and organic molten used in polymer solution in step (2)
The mixed solution of agent and ethyl alcohol washs 4 ~ 6 times, obtains nano-cellulose/graphene oxide/polymer cake；
(4) hydrazine hydrate solution that mass concentration is 1 ~ 20% is prepared；
(5) filter cake obtained in step (3) is immersed in the hydrazine hydrate solution of step (4) preparation, is reacted at 60 ~ 100 DEG C
Filter cake, is then placed in hot pressing die in 60 ~ 100 DEG C of baking oven that the reaction was continued and is dried to leather hard by 0.5 ~ 3h；
(6) leather hard filter cake obtained in step (5) is put into flat-bed press and carries out hot pressing, obtain nano-cellulose/
Redox graphene/polymer compound electromagnetic shielding material, as conductive polymer base composite electric magnetic shielding material；
The nano-cellulose is cellulosic material of at least one-dimensional scale in nanometer range, including extracts and make from raw material
The standby Cellulose nanocrystal and cellulose Nanowire with appearance structure, chinese raw materials are cotton, timber, bamboo or fiber crops
Class；
The graphene oxide is monolithic layer structure, and lamellar spacing is 0.8 ~ 1.2nm；
The polymer is non-soluble polymer, specially polystyrene, polycarbonate, polyamide, polylactic acid, poly- methyl-prop
E pioic acid methyl ester, polycaprolactone, poly lactide-glycolide acid or cellulose acetate；
The organic solvent is methylene chloride, 1,2- dichloroethanes, chloroform, n-hexane or hexamethylene；
Heat pressing process in the step (6) uses two-step method: first under conditions of 80 DEG C, pressure is 0.5MPa hot pressing 5 ~
15min further removes the organic solvent in filter cake；Then 150 DEG C, pressure be 12MPa under conditions of hot pressing 15 ~ 60min；
The purity of the chemical reagent and raw material is to analyze the pure and above purity.
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Cited By (4)
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| CN113136083A (en) * | 2021-04-21 | 2021-07-20 | 浙江优可丽新材料有限公司 | Composite electromagnetic shielding material for low-frequency wave band and preparation method thereof |
| CN113415800A (en) * | 2021-06-23 | 2021-09-21 | 桂林理工大学 | Carbon foam material and preparation method and application thereof |
| CN117865544A (en) * | 2023-12-21 | 2024-04-12 | 科顺民用建材有限公司 | RGO modified polymer emulsion and preparation method thereof, mortar composition, electromagnetic shielding waterproof mortar and preparation method thereof |
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Effective date of registration: 20230113 Address after: Room 103, Enterprise Zone, Innovation and Entrepreneurship Base, Guilin University of Technology, No. 12, Jiangan Road, Qixing District, Guilin City, Guangxi Zhuang Autonomous Region, 541010 Patentee after: Guilin Qi Hong Technology Co.,Ltd. Address before: 541004 the Guangxi Zhuang Autonomous Region Guilin City Seven Star District Building Road No. 12 Patentee before: GUILIN University OF TECHNOLOGY |