CN110256732A - A kind of ferroso-ferric oxide-graphene-cellulose conduction composite aerogel and preparation method thereof applied to electromagnetic shielding field - Google Patents
A kind of ferroso-ferric oxide-graphene-cellulose conduction composite aerogel and preparation method thereof applied to electromagnetic shielding field Download PDFInfo
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
Abstract
The invention discloses a kind of ferroso-ferric oxide-graphene-cellulose conduction composite aerogels and preparation method thereof applied to electromagnetic shielding field.The preparation method include: by cellulose dissolution in sodium hydroxide/urea aqueous solution, then casting film-forming obtains hydrogel after graphene oxide water solution being mixed with cellulose solution, after reducing agent in-situ reducing, hydrogel is successively impregnated in the aqueous solution and aqueous slkali of iron chloride and frerrous chloride to in-situ preparation ferroso-ferric oxide again, after deionized water is repeatedly rinsed, up to the ferroso-ferric oxide-graphene-cellulose conduction composite aerogel for being applied to electromagnetic shielding field after freeze-drying.The effectiveness of aeroge provided by the invention is fine.Preparation method provided by the invention has many advantages, such as that technical process is simple and convenient to operate and no pollution to the environment.Composite aerogel provided by the invention can be applied in the fields such as electromagnetic shielding material.
Description
Technical field
The invention belongs to be electromagnetically shielded field, and in particular to a kind of ferroso-ferric oxide-stone applied to electromagnetic shielding field
Black alkene-cellulose conduction composite aerogel and preparation method thereof.
With the development of Modern communication devices, electronic equipment and radio communication are made extensively in our daily life
With.Simultaneously.The harm of electromagnetic radiation is also on the rise, and can not only interfere the normal operation of electronic equipment, can also be to people
The health of class causes damages.Therefore, the harm that this electromagnetic radiation is eliminated using electromagnetic shielding material is urgent need
's.Currently, electromagnetic shielding is widely used in military project and civil field, such as wireless device, aircraft manufacturing, electronic equipment etc..
Therefore, our requirements and performance for electromagnetic shielding material now is also higher and higher.However, traditional electromagnetic shielding material base
It originally is to have based on metal and be unfavorable for processing, easily corrode, therefore the defects of shielding material density is high explores matter
Gently, stable and high electromagnetic shielding performance electromagnetic shielding material is problem in the urgent need to address.Simultaneously with white pollution and
Plastics recovery problem is increasingly severe, recoverable and biodegradable natural polymer more and more attention has been paid to.Fiber
Element has wide application prospects as a kind of the most abundant natural high polymer.Since it is cheap and biodegradable, can be used for
Packaging film and functional material are prepared, to solve problem of environmental pollution.In addition, adding well since cellulose aerogels material has
Work, can electromagnetic shielding material matrix and ferroso-ferric oxide and graphene play a role jointly, to improve the electricity of this material
Magnetic shield performance.The existing good magnetic property of this aerogel material and the advantages such as electric conductivity and light weight, then have
Excellent electromagnetic shielding performance also has the workability and mechanical property of high molecular material, can be widely used in electromagnetic shielding
Etc. multiple fields.
Summary of the invention
In order to overcome the shortcomings of the prior art, the object of the present invention is to provide a kind of applied to electromagnetic shielding field
Ferroso-ferric oxide-graphene-cellulose conduction composite aerogel and preparation method thereof.
The purpose of the present invention is realized at least through one of following technical solution.
A kind of ferroso-ferric oxide-graphene-cellulose conduction applied to electromagnetic shielding field provided by the invention is compound
The preparation method of aeroge, comprising: using cellulose as substrate, combined oxidation graphene, the oxidation of in-situ preparation four three again after reduction
The aerogel composite for being electromagnetically shielded field is prepared in iron;The technique for preparing composite aerogel has process letter
The advantages that single, easy to operate and no pollution to the environment.Composite conducting aeroge provided by the invention can be applied to be electromagnetically shielded
The fields such as material.
A kind of ferroso-ferric oxide-graphene-cellulose conduction applied to electromagnetic shielding field provided by the invention is compound
The preparation method of aeroge, includes the following steps:
(1) sodium hydroxide and urea are added to the water, are uniformly mixed and obtain sodium hydroxide/urea mixed aqueous solution,
Graphene oxide is dispersed in water, and obtains the aqueous solution of graphene oxide;
(2) mixed aqueous solution of step (1) sodium hydroxide/urea is subjected to precooling treatment, cellulose is then added,
It is uniformly mixing to obtain cellulose solution;The aqueous solution of step (1) described graphene oxide is added in cellulose solution, mixing is equal
It is even to obtain mixed liquor;By mixed liquor casting film-forming, coagulating bath processing is then carried out in dilution heat of sulfuric acid, solidification forming obtains water
Gel, repeatedly washing in deionized water after taking-up;
(3) hydrogel after step (2) washing is immersed in progress reduction treatment (in-situ reducing) in reducing agent solution,
Graphene-cellulose composite hydrogel is obtained, repeatedly washing in deionized water after taking-up;
(4) iron chloride and frerrous chloride are added to the water, are uniformly mixed and obtain iron chloride and the mixing of frerrous chloride is water-soluble
Graphene-cellulose composite hydrogel after step (3) washing is successively immersed in the mixed of the iron chloride and frerrous chloride by liquid
In Heshui solution and alkaline solution, ferroso-ferric oxide-graphene-cellulose composite hydrogel is obtained, deionized water is repeatedly washed,
Freeze-drying obtains the ferroso-ferric oxide-graphene-cellulose conduction composite aerogel for being applied to electromagnetic shielding field.
Further, the mass ratio of step (1) sodium hydroxide and urea is 6:14~8:10;The urea and water
Mass ratio is 10:82~14:80;The mass percent concentration of the aqueous solution of the graphene oxide is 0.2~2%.
Preferably, step (2) precooling temperature is -12~-20 DEG C, and pre-coo time is 1-2 hours;Preferably, step
(2) mixing time (mixing time of dissolution cellulose) stirred evenly is 5~10 minutes.
Further, the quality of step (2) described cellulose be sodium hydroxide/urea mixed aqueous solution quality 2~
8%;The mass ratio of step (1) graphene oxide and step (2) described cellulose is 2:98-8:92.
Further, the volume of the aqueous solution of step (2) described graphene oxide is the 10%- of cellulose solution volume
30%.
Further, the mass percent concentration of step (2) described dilution heat of sulfuric acid is 4%-6%, at the coagulating bath
The time of reason is 5-10 minutes.
Further, step (3) described reducing agent solution includes ascorbic aqueous solution, the ascorbic aqueous solution
Concentration be 30-50g/L;The temperature of the reduction treatment is 90-95 degrees Celsius, and the time of the reduction treatment is 1-2 hours.
Further, the molar ratio of step (4) iron chloride and frerrous chloride is 1.6:1.4-2.4:0.6;The chlorine
The mass volume ratio for changing iron and water is 5-10:1g/L.
Further, graphene-cellulose composite hydrogel after step (4) described washing is immersed in iron chloride and chlorination
The time of ferrous mixed aqueous solution is 30-60 minutes;Step (4) described alkaline solution includes sodium hydroxide solution, quality hundred
Point specific concentration is 5%-10%, and graphene-cellulose composite hydrogel after the washing is immersed in the time in aqueous slkali and is
5-10 minutes.
Preferably, the time of freeze-drying described in step (3) is 20-24 hours.
The present invention provides a kind of ferroso-ferric oxide-stone for being applied to electromagnetic shielding field as made from above-mentioned preparation method
Black alkene-cellulose conduction composite aerogel.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
(1) preparation method provided by the invention, used raw cellulose are most extensive volume natural polymers in nature
Sub- material, it is from a wealth of sources, it is cheap, belong to environment-friendly material;The preparation method have simple process, to equipment requirement not
Height is conducive to the advantages that being mass produced and is simple to operate.
(2) the cellulose base aeroge that the present invention is prepared, abscess is uniform, while graphene and ferroso-ferric oxide play
Synergistic effect, can improve the effectiveness of this aerogel material jointly.
Specific embodiment
Specific implementation of the invention is described further below in conjunction with example, but implementation and protection of the invention is not limited to
This.If being that those skilled in the art can refer to prior art reality it is noted that there is the process of not special detailed description below
It is existing or understanding.Reagents or instruments used without specified manufacturer, being considered as can be by the commercially available conventional products being commercially available.
Embodiment 1
The conductive compound airsetting of ferroso-ferric oxide-graphene applied to electromagnetic shielding field that embodiment 1 provides-cellulose
The preparation method of glue, includes the following steps:
(1) 20g sodium hydroxide is added to the water with urea, is uniformly mixed and obtains sodium hydroxide/urea mixed aqueous solution,
In the mixed aqueous solution of the sodium hydroxide/urea, the mass percent concentration of sodium hydroxide is 7wt%, the quality of urea
Percent concentration is 12wt%;0.08 gram of graphene oxide is dispersed in 20 milliliters of water, the aqueous solution of graphene oxide is obtained;
(2) mixed aqueous solution of step (1) sodium hydroxide/urea is subjected to precooling treatment, the temperature of precooling treatment
It is -12 degrees Celsius, the time of precooling treatment is 1 hour;3.92 grams of celluloses are added to 96 grams of sodium hydroxide/urea mixing
It in aqueous solution, stirs 5 minutes, is uniformly mixing to obtain cellulose solution, 100 millis are added in the aqueous solution of 20 milliliters of graphene oxides
It rises in cellulose solution, is uniformly mixed and obtains mixed liquor;By mixed liquor casting film-forming on a glass, then in dilution heat of sulfuric acid
Coagulating bath processing is carried out in (dilution heat of sulfuric acid concentration is 4wt%), the time of coagulating bath processing is 5 minutes, obtains hydrogel, uses
Deionized water washing;
(3) hydrogel after washing step (2) is immersed in 500 milliliters of reducing agent solutions, and (concentration is the vitamin of 30g/L
The aqueous solution of C) in carry out reduction treatment, the temperature of reduction treatment is 95 degrees Celsius, and the time of reduction treatment is 1 hour, is obtained
Graphene-cellulose composite hydrogel, is washed with deionized;
(4) 8mmol iron chloride and 4mmol frerrous chloride are added in 200 milliliters of water, are uniformly mixed and obtain iron chloride and chlorine
Change ferrous mixed aqueous solution;By step (3) washing after graphene-cellulose composite hydrogel be immersed in the iron chloride with
In the mixed aqueous solution of frerrous chloride, soaking time is 30 minutes;Then 100 milliliters of alkaline solution (concentration 5wt% are immersed in
Sodium hydroxide solution) in, soaking time be 5 minutes, obtain ferroso-ferric oxide-graphene-cellulose composite hydrogel, use
Deionized water is repeatedly washed, and freeze-drying obtains the ferroso-ferric oxide-graphene-cellulose for being applied to electromagnetic shielding field
Conductive composite aerogel, the time of freeze-drying are 1 hour.It counts by weight, step (1) graphene oxide and fiber
The ratio of element is 2:98.
(5) pass through above-mentioned steps, ferroso-ferric oxide-graphene-cellulose conduction composite aerogel of preparation is with a thickness of 2 millis
Rice, electromagnetic shielding performance 44dB.This light aerogel material only joined a small amount of graphene, and electromagnetic shielding performance is just
More than the application requirement (20dB) of electromagnetic shielding material.
Embodiment 2
The conductive compound airsetting of ferroso-ferric oxide-graphene applied to electromagnetic shielding field that embodiment 2 provides-cellulose
The preparation method of glue, includes the following steps:
(1) 20g sodium hydroxide is added to the water with urea, is uniformly mixed and obtains sodium hydroxide/urea mixed aqueous solution,
In the mixed aqueous solution of the sodium hydroxide/urea, the mass percent concentration of sodium hydroxide is 6wt%, the quality of urea
Percent concentration is 14wt%;0.16 gram of graphene oxide is dispersed in 20 milliliters of water, the aqueous solution of graphene oxide is obtained;
(2) mixed aqueous solution of step (1) sodium hydroxide/urea is subjected to precooling treatment, the temperature of precooling treatment
It is -18 degrees Celsius, the time of precooling treatment is 1.5 hours;It is mixed that 3.84 grams of celluloses are added to 96 grams of sodium hydroxide/urea
It in Heshui solution, stirs 5 minutes, is uniformly mixing to obtain cellulose solution, the aqueous solution of 10 milliliters of graphene oxides is added 100
In milliliter cellulose solution, it is uniformly mixed and obtains mixed liquor;It is then molten in dilute sulfuric acid by mixed liquor casting film-forming on a glass
Coagulating bath processing is carried out in liquid (dilution heat of sulfuric acid concentration is 4wt%), the time of coagulating bath processing is 7 minutes, obtains water-setting
Glue is washed with deionized;
(3) hydrogel after washing step (2) is immersed in 500 milliliters of reducing agent solutions, and (concentration is the vitamin of 40g/L
The aqueous solution of C) in carry out reduction treatment, the temperature of reduction treatment is 95 degrees Celsius, and the time of reduction treatment is 1.5 hours, is obtained
To graphene-cellulose composite hydrogel, it is washed with deionized;
(4) 8mmol iron chloride and 4mmol frerrous chloride are added in 200 milliliters of water, are uniformly mixed and obtain iron chloride and chlorine
Change ferrous mixed aqueous solution;By step (3) washing after graphene-cellulose composite hydrogel be immersed in the iron chloride with
In the mixed aqueous solution of frerrous chloride, soaking time is 1 hour;Then 100 milliliters of alkaline solution (concentration 5wt% are immersed in
Sodium hydroxide solution) in, soaking time be 5 minutes, obtain ferroso-ferric oxide-graphene-cellulose composite hydrogel, use
Deionized water is repeatedly washed, and freeze-drying obtains the ferroso-ferric oxide-graphene-cellulose for being applied to electromagnetic shielding field
Conductive composite aerogel, the time of freeze-drying are 22 hours.It counts by weight, step (1) graphene oxide and fine
The ratio of dimension element is 4:96.
(5) pass through above-mentioned steps, ferroso-ferric oxide-graphene-cellulose conduction composite aerogel of preparation is with a thickness of 2 millis
Rice, electromagnetic shielding performance 50dB.This light aerogel material only joined a small amount of graphene, and electromagnetic shielding performance is just
More than the application requirement (20dB) of electromagnetic shielding material.Meanwhile with the raising of graphene content, electromagnetic wave is caused in airsetting
Route of transmission in glue material increases, to obtain higher electromagnetic shielding performance.
Embodiment 3
The conductive compound airsetting of ferroso-ferric oxide-graphene applied to electromagnetic shielding field that embodiment 3 provides-cellulose
The preparation method of glue, includes the following steps:
(1) 20g sodium hydroxide is added to the water with urea, is uniformly mixed and obtains sodium hydroxide/urea mixed aqueous solution,
In the mixed aqueous solution of the sodium hydroxide/urea, the mass percent concentration of sodium hydroxide is 8wt%, the quality of urea
Percent concentration is 10wt%;0.24 gram of graphene oxide is dispersed in 20 milliliters of water, the aqueous solution of graphene oxide is obtained;
(2) mixed aqueous solution of step (1) sodium hydroxide/urea is subjected to precooling treatment, the temperature of precooling treatment
It is -20 degrees Celsius, the time of precooling treatment is 1 hour;3.76 grams of celluloses are added to 96 grams of sodium hydroxide/urea mixing
It in aqueous solution, stirs 5 minutes, is uniformly mixing to obtain cellulose solution, 100 millis are added in the aqueous solution of 30 milliliters of graphene oxides
It rises in cellulose solution, is uniformly mixed and obtains mixed liquor;By mixed liquor casting film-forming on a glass, then in dilution heat of sulfuric acid
Coagulating bath processing is carried out in (dilution heat of sulfuric acid concentration is 6wt%), the time of coagulating bath processing is 5 minutes, obtains hydrogel, uses
Deionized water washing;
(3) hydrogel after washing step (2) is immersed in 500 milliliters of reducing agent solutions, and (concentration is the vitamin of 50g/L
The aqueous solution of C) in carry out reduction treatment, the temperature of reduction treatment is 90 degrees Celsius, and the time of reduction treatment is 2 hours, is obtained
Graphene-cellulose composite hydrogel, is washed with deionized;
(4) 8mmol iron chloride and 4mmol frerrous chloride are added in 200 milliliters of water, are uniformly mixed and obtain iron chloride and chlorine
Change ferrous mixed aqueous solution;By step (3) washing after graphene-cellulose composite hydrogel be immersed in the iron chloride with
In the mixed aqueous solution of frerrous chloride, soaking time is 1 hour;Then 100 milliliters of alkaline solution (concentration 10wt% are immersed in
Sodium hydroxide solution), soaking time be 5 minutes, obtain ferroso-ferric oxide-graphene-cellulose composite hydrogel, spend from
Sub- water repeatedly washs, and freeze-drying obtains the ferroso-ferric oxide-graphene-cellulose applied to electromagnetic shielding field and leads
Electric composite aerogel, the time of freeze-drying are 24 hours.It counts by weight, step (1) graphene oxide and fiber
The ratio of element is 6:94.
(5) pass through above-mentioned steps, ferroso-ferric oxide-graphene-cellulose conduction composite aerogel of preparation is with a thickness of 2 millis
Rice, electromagnetic shielding performance 62dB.This light aerogel material only joined a small amount of graphene, and electromagnetic shielding performance is just
Considerably beyond the application requirement (20dB) of electromagnetic shielding material.Meanwhile with the raising of graphene content, causes electromagnetic wave and exist
Route of transmission in aerogel material increases, to obtain higher electromagnetic shielding performance.
Embodiment 4
The conductive compound airsetting of ferroso-ferric oxide-graphene applied to electromagnetic shielding field that embodiment 4 provides-cellulose
The preparation method of glue, includes the following steps:
(1) 20g sodium hydroxide is added to the water with urea, is uniformly mixed and obtains sodium hydroxide/urea mixed aqueous solution,
In the mixed aqueous solution of the sodium hydroxide/urea, the mass percent concentration of sodium hydroxide is 7wt%, the quality of urea
Percent concentration is 12wt%;0.32 gram of graphene oxide is dispersed in 20 milliliters of water, the aqueous solution of graphene oxide is obtained;
(2) mixed aqueous solution of step (1) sodium hydroxide/urea is subjected to precooling treatment, the temperature of precooling treatment
It is -12 degrees Celsius, the time of precooling treatment is 1 hour;3.68 grams of celluloses are added to 96 grams of sodium hydroxide/urea mixing
It in aqueous solution, stirs 5 minutes, is uniformly mixing to obtain cellulose solution, 100 millis are added in the aqueous solution of 20 milliliters of graphene oxides
It rises in cellulose solution, is uniformly mixed and obtains mixed liquor;By mixed liquor casting film-forming on a glass, then in dilution heat of sulfuric acid
Coagulating bath processing is carried out in (dilution heat of sulfuric acid concentration is 5wt%), the time of coagulating bath processing is 5 minutes, obtains hydrogel, uses
Deionized water washing;
(3) hydrogel after washing step (2) is immersed in 500 milliliters of reducing agent solutions, and (concentration is the vitamin of 30g/L
The aqueous solution of C) in carry out reduction treatment, the temperature of reduction treatment is 95 degrees Celsius, and the time of reduction treatment is 1 hour, is obtained
Graphene-cellulose composite hydrogel, is washed with deionized;
(4) 8mmol iron chloride and 4mmol frerrous chloride are added in 200 milliliters of water, are uniformly mixed and obtain iron chloride and chlorine
Change ferrous mixed aqueous solution;By step (3) washing after graphene-cellulose composite hydrogel be immersed in the iron chloride with
In the mixed aqueous solution of frerrous chloride, soaking time is 1 hour;Then 100 milliliters of alkaline solution (concentration 5wt% are immersed in
Sodium hydroxide solution) in, soaking time be 5 minutes, obtain ferroso-ferric oxide-graphene-cellulose composite hydrogel, use
Deionized water is repeatedly washed, and freeze-drying obtains the ferroso-ferric oxide-graphene-cellulose for being applied to electromagnetic shielding field
Conductive composite aerogel, the time of freeze-drying are 1 hour.It counts by weight, step (1) graphene oxide and fiber
The ratio of element is 8:92.
(5) pass through above-mentioned steps, ferroso-ferric oxide-graphene-cellulose conduction composite aerogel of preparation is with a thickness of 2 millis
Rice, electromagnetic shielding performance 74dB.This light aerogel material only joined a small amount of graphene, and electromagnetic shielding performance is just
More than the application requirement (20dB) of electromagnetic shielding material.Meanwhile with the raising of graphene content, electromagnetic wave is caused in airsetting
Route of transmission in glue material increases, to obtain higher electromagnetic shielding performance.
Above embodiments are only preferrred embodiment of the present invention, for explaining only the invention, are not intended to limit the present invention, this
Field technical staff should belong to guarantor of the invention without departing from change made under spirit of the invention, replacement, modification etc.
Protect range.
Claims (10)
1. a kind of ferroso-ferric oxide-graphene-cellulose conduction composite aerogel preparation side applied to electromagnetic shielding field
Method, which comprises the steps of:
(1) sodium hydroxide and urea are added to the water, are uniformly mixed and obtain sodium hydroxide/urea mixed aqueous solution, oxidation
Graphene dispersion in water, obtains the aqueous solution of graphene oxide;
(2) mixed aqueous solution of step (1) sodium hydroxide/urea is subjected to precooling treatment, cellulose is then added, stirred
Uniformly obtain cellulose solution;The aqueous solution of step (1) described graphene oxide is added in cellulose solution, is uniformly mixed
To mixed liquor;By mixed liquor casting film-forming, coagulating bath processing is then carried out in dilution heat of sulfuric acid, obtains hydrogel, wash;
(3) hydrogel after step (2) washing is immersed in reducing agent solution and carries out reduction treatment, obtain graphene-fiber
Plain composite hydrogel, washing;
(4) iron chloride and frerrous chloride are added to the water, are uniformly mixed and obtain the mixed aqueous solution of iron chloride and frerrous chloride, it will
Graphene-cellulose composite hydrogel after step (3) washing is successively immersed in the mixing water of the iron chloride and frerrous chloride
In solution and alkaline solution, ferroso-ferric oxide-graphene-cellulose composite hydrogel is obtained, is washed, freeze-drying obtains described
Ferroso-ferric oxide-graphene-cellulose conduction composite aerogel applied to electromagnetic shielding field.
2. preparation method according to claim 1, which is characterized in that the quality of step (1) sodium hydroxide and urea
Than for 6:14-8:10;The mass ratio of the urea and water is 10:82-14:80;The quality of the aqueous solution of the graphene oxide
Percent concentration is 0.2-2%.
3. preparation method according to claim 1, which is characterized in that step (2) precooling temperature is -20 DEG C ~ -12
DEG C, pre-coo time is 1-2 hours;The quality of step (2) described cellulose is sodium hydroxide/urea mixed aqueous solution quality
2~8%;The mass ratio of step (1) graphene oxide and step (2) described cellulose is 2:98-8:92.
4. preparation method according to claim 1, which is characterized in that the aqueous solution of step (2) described graphene oxide
Volume is the 10%-30% of cellulose solution volume.
5. preparation method according to claim 1, which is characterized in that the quality percentage of step (2) described dilution heat of sulfuric acid
Specific concentration is 4%-6%, and the time of the coagulating bath processing is 5-10 minutes.
6. preparation method according to claim 1, which is characterized in that step (3) described reducing agent solution includes vitamin C
Aqueous solution, the concentration of the ascorbic aqueous solution is 30-50g/L;The temperature of the reduction treatment is 90-95 degrees Celsius,
The time of the reduction treatment is 1-2 hours.
7. preparation method according to claim 1, which is characterized in that step (4) iron chloride and frerrous chloride rub
You are than being 1.6:1.4-2.4:0.6;The mass volume ratio of the iron chloride and water is 5-10:1g/L.
8. preparation method according to claim 1, which is characterized in that step (4) graphene-cellulose compound water congealing
The time that glue is immersed in the mixed aqueous solution of iron chloride and frerrous chloride is 30-60 minutes;Step (4) described alkaline solution includes
Sodium hydroxide solution, the mass percent concentration of the alkaline solution are 5%-10%, the graphene-cellulose composite hydrogel
The time being immersed in alkaline solution is 5-10 minutes.
9. preparation method according to claim 1, which is characterized in that the time of step (4) described freeze-drying is 20-24
Hour.
10. a kind of four oxidations for being applied to electromagnetic shielding field as made from the described in any item preparation methods of claim 1-9
Three-iron-graphene-cellulose conduction composite aerogel.
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CN110790974A (en) * | 2019-11-25 | 2020-02-14 | 华南理工大学 | Cellulose-graphene aerogel material applied to field of gas detection and preparation method thereof |
CN112497860A (en) * | 2020-05-07 | 2021-03-16 | 刘家浩 | Long-acting flame-retardant anti-piercing anti-radiation composite fabric |
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