AU2021107284A4 - A method of preparing efficient electromagnetic shielding aerogel from waste paper - Google Patents
A method of preparing efficient electromagnetic shielding aerogel from waste paper Download PDFInfo
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- 239000004964 aerogel Substances 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 14
- 239000010893 paper waste Substances 0.000 title claims abstract description 13
- 229920000767 polyaniline Polymers 0.000 claims abstract description 33
- 229920002678 cellulose Polymers 0.000 claims abstract description 29
- 239000001913 cellulose Substances 0.000 claims abstract description 29
- 239000002131 composite material Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 239000002699 waste material Substances 0.000 claims abstract description 5
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 18
- 229910021641 deionized water Inorganic materials 0.000 claims description 18
- 239000000178 monomer Substances 0.000 claims description 12
- 239000005457 ice water Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010907 mechanical stirring Methods 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 6
- 229960002218 sodium chlorite Drugs 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims 3
- 229920001131 Pulp (paper) Polymers 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004108 freeze drying Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005670 electromagnetic radiation Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000005595 deprotonation Effects 0.000 description 1
- 238000010537 deprotonation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2479/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2461/00 - C08J2477/00
- C08J2479/02—Polyamines
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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
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/02—Polyamines
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
The invention relates to a method for preparing polyaniline/cellulose aerogel composite
materials from renewable waste paper. Concretely, the ultra-light and conductive cellulose
aerogels modified by polyaniline were synthesized through a simple in-situ polymerization
and freeze-drying process. The obtained polyaniline/cellulose aerogels have the excellent
electromagnetic shielding performances. The invention develops a method for realizing the
high-value conversion and utilization of waste via a green and environment-friendly process.
Thus, the invention has important applied values in manufacturing sustainable and
high-performance electromagnetic shielding materials.
Description
Field of the Invention
The invention relates to a method of preparing polyaniline/cellulose aerogel composite
materials with high-efficiency electromagnetic shielding performances, which belongs to the
field of material fabrication.
Background of the Invention
With the rapid development of modern scientific information and electronic technology,
the various new electronic components, motor and metal products are widely applied in
various fields such as electronic industry, military and natural science. Meanwhile, the
electromagnetic radiation has become a new kind of environmental pollution. At present, the
electromagnetic shielding materials can effectively inhibit the electromagnetic radiation
pollution. However, the conventional electromagnetic shielding materials have high density,
poor flexibility and complicated preparation process.
Cellulose is a kind of natural and renewable material, which is widely used due to its
biocompatibility, richness and processability. Cellulose aerogels are often used as the
three-dimensional skeleton of composites, because of their large specific surface area, good
flexibility, high mechanical strength and abundant surface hydroxyl groups. Such structure
makes it possible to prepare aerogel with electromagnetic shielding properties, which is of
great significance for efficient electromagnetic shielding materials. Although the significant
efforts have been put into developing cellulose aerogel composites with high electromagnetic
shielding properties, the challenges still exist due to that the cellulose separation and assembly
process is energy/chemical intensive.
The conductive polymers have excellent electrochemical activity, light weight, flexibility
and other properties, and have attracted much attention in electromagnetic shielding materials.
Among them, the polyaniline has a controllable conductivity and good environmental stability
through a simple protonation/deprotonation process, which has attracted widespread attention.
Therefore, the applications of polyaniline in sensor, photoelectron, electrochromic devices and
fuel cells have been widely explored. In addition, the polyaniline has a mechanism for
shielding electromagnetic interference through absorption, which makes it particularly suitable
for military. However, the existence of conjugated system in the polyaniline improves the
stiffness of the material, which reduces the machining and mechanical properties of the
material.
Summary of the Invention
The invention provides a method of preparing polyaniline/cellulose aerogel composite
materials with high efficiency electromagnetic shielding performance, which is implemented
in the following steps:
(1) the waste paper was soaked in deionized water and mechanically stirred for 3 h at a
certain speed to form a homogeneous pulp. Subsequently, the pulp of was taken into a beaker
and mixed with the sodium chlorite. Afterwards, the pH of the solution was adjusted to 4.5 by
acetic acid, then solution was oxidized at 80 °C for 2 h under the mechanical stirring. After that,
the obtained solution was washed with the deionized water until pH = 6, and then washed with
anhydrous ethanol for three times;
(2) the appropriate amount of aniline monomer was added to HCl solution, followed by
stirring to disperse aniline monomer evenly. Then, the obtained pulp from step (1) was added
to the above solution and mechanically stirred. Subsequently, 0.125~1.5 g APS was added as
an oxidant (APS/aniline ratio was 1.25 w/w), and aniline was polymerized in an ice water bath.
After that, the products were centrifuged and washed, and dispersed in the deionized water;
(3) the solution obtained from step (2) was freeze-dried to obtain polyaniline/cellulose
aerogel.
Preferably, the waste pulp described in step (1) has a concentration of 10~15 mg/mL.
Preferably, the concentration of the HCl solution described in step (2) is 0.5~2 mol L- .
Preferably, the wet pulp described in step (3) has a mass of 1~3 g.
Preferably, the mass ratio of APS/aniline described in step (3) is 1.25 and the aniline mass fraction in wet pulp is 5~30%.
Preferably, the reaction time of aniline polymerization in ice water bath described in step (3) is 1-3 h.
The purpose of the invention is to provide a polyaniline/cellulose aerogel composite material, which is prepared according to the above preparation method of the invention.
Another purpose of the present invention is to provide applications of the polyaniline/cellulose aerogel composites in terms of electromagnetic shielding properties.
Beneficial effects of the present disclosure
The invention develops a method of preparing efficient electromagnetic shielding aerogels from waste paper, which has the following beneficial effects: (1) The invention uses waste paper as the renewable, low-cost raw material to alleviate the low formability and fragility of polyaniline and realize the high-value conversion and utilization of waste. (2) The invention uses the polyaniline as a conductive polymer to improve the electrical conductivity of the aerogels by in situ polymerization, which effectively improve the mechanical and electromagnetic shielding properties of the aerogels. (3) The polyaniline/cellulose aerogels are prepared by the freeze-drying method without any volatile organic solvent. The preparing process is green, environment-friendly and highly operable. (4) The polyaniline/cellulose aerogels have the low density and porous structure, which effectively improve the electromagnetic shielding performances.
Brief Description of the Drawings
Fig. 1 is the morphology of polyaniline/cellulose aerogel (CEL-PANI5) obtained from the
embodiment 1.
Fig. 2 is the SEM images of CEL-PANI30 obtained from the embodiment 4.
Fig. 3 is the diagrams of electromagnetic shielding effectiveness of CEL-PANIlO and
CEL-PANI30 respectively obtained from the embodiments 2 and 4.
Detailed Description of the Embodiments
The invention will be further described in detail in combination with the following
embodiments and attached figures.
Embodiment 1
The 5% polyaniline/cellulose aerogel (CEL-PANI5) was prepared by the following steps:
(1) the waste paper was soaked in deionized water and mechanically stirred for 3 h at a
certain speed to form a homogeneous pulp with the concentration of 10 mg/mL. Subsequently,
the pulp of 400 mL was taken into a beaker and mixed with the sodium chlorite of 2 g.
Afterwards, the pH of the solution was adjusted to 4.5 by acetic acid, then solution was
oxidized at 80 °C for 2 h under the mechanical stirring. After that, the obtained solution was
washed with the deionized water until pH = 6, and then washed with anhydrous ethanol for
three times;
(2) the appropriate amount of aniline monomer was added to 0.5 mol/L HCl solution,
followed by stirring to disperse aniline monomer evenly. Then, the obtained pulp (1 g) from
step (1) was added to the above solution and mechanically stirred. Subsequently, 0.125 g APS
was added as an oxidant (APS/aniline ratio was 1.25 w/w), and aniline was polymerized for 3
h in an ice water bath. After that, the products were centrifuged and washed, and dispersed in
the deionized water;
(3) the solution obtained from step (2) was freeze-dried to obtain polyaniline/cellulose
aerogel with the aniline of 5 wt.%, which was labeled as CEL-PANI5.
Embodiment 2
The 10% polyaniline/cellulose aerogel (CEL-PANI1) was prepared by the following
steps:
(1) the waste paper was soaked in deionized water and mechanically stirred for 3 h at a
certain speed to form a homogeneous pulp with the concentration of 15 mg/mL. Subsequently,
the pulp of 267 mL was taken into a beaker and mixed with the sodium chlorite of 2 g.
Afterwards, the pH of the solution was adjusted to 4.5 by acetic acid, then solution was
oxidized at 80 °C for 2 h under the mechanical stirring. After that, the obtained solution was
washed with the deionized water until pH = 6, and then washed with anhydrous ethanol for
three times;
(2) the appropriate amount of aniline monomer was added to 2 mol/L HCl solution,
followed by stirring to disperse aniline monomer evenly. Then, the obtained pulp (1 g) from
step (1) was added to the above solution and mechanically stirred. Subsequently, 0.25 g APS
was added as an oxidant (APS/aniline ratio was 1.25 w/w), and aniline was polymerized for 3
h in an ice water bath. After that, the products were centrifuged and washed, and dispersed in
the deionized water;
(3) the solution obtained from step (2) was freeze-dried to obtain polyaniline/cellulose
aerogel with the aniline of 10 wt.%, which was labeled as CEL-PANI10.
Embodiment 3
The 20% polyaniline/cellulose aerogel (CEL-PANI20) was prepared by the following
steps:
(1) the waste paper was soaked in deionized water and mechanically stirred for 3 h at a
certain speed to form a homogeneous pulp with the concentration of 10 mg/mL. Subsequently,
the pulp of 400 mL was taken into a beaker and mixed with the sodium chlorite of 2 g.
Afterwards, the pH of the solution was adjusted to 4.5 by acetic acid, then solution was oxidized at 80 °C for 2 h under the mechanical stirring. After that, the obtained solution was washed with the deionized water until pH = 6, and then washed with anhydrous ethanol for three times; (2) the appropriate amount of aniline monomer was added to 1 mol/L HCl solution, followed by stirring to disperse aniline monomer evenly. Then, the obtained pulp (3 g) from step (1) was added to the above solution and mechanically stirred. Subsequently, 1.5 g APS was added as an oxidant (APS/aniline ratio was 1.25 w/w), and aniline was polymerized for 1 h in an ice water bath. After that, the products were centrifuged and washed, and dispersed in the deionized water; (3) the solution obtained from step (2) was freeze-dried to obtain polyaniline/cellulose aerogel with the aniline of 20 wt.%, which was labeled as CEL-PANI20.
Embodiment 4
The 30% polyaniline/cellulose aerogel (CEL-PANI30) was prepared by the following steps: (1) the waste paper was soaked in deionized water and mechanically stirred for 3 h at a certain speed to form a homogeneous pulp with the concentration of 10 mg/mL. Subsequently, the pulp of 400 mL was taken into a beaker and mixed with the sodium chlorite of 2 g. Afterwards, the pH of the solution was adjusted to 4.5 by acetic acid, then solution was oxidized at 80 °C for 2 h under the mechanical stirring. After that, the obtained solution was washed with the deionized water until pH = 6, and then washed with anhydrous ethanol for three times; (2) the appropriate amount of aniline monomer was added to 1 mol/L HCl solution, followed by stirring to disperse aniline monomer evenly. Then, the obtained pulp (1 g) from step (1) was added to the above solution and mechanically stirred. Subsequently, 0.75 g APS was added as an oxidant (APS/aniline ratio was 1.25 w/w), and aniline was polymerized for 3 h in an ice water bath. After that, the products were centrifuged and washed, and dispersed in the deionized water; (3) the solution obtained from step (2) was freeze-dried to obtain polyaniline/cellulose aerogel with the aniline of 30 wt.%, which was labeled as CEL-PANI30.
Fig. 1 shows the morphology of polyaniline/cellulose aerogel (CEL-PANI5) obtained
from the embodiment 1. It can be found from Fig. 1 that CEL-PANI5 has fluffy
three-dimensional porous structure and low density of 0.05 g/cm 3. Fig. 2 shows the SEM
images of CEL-PANI30 obtained from the embodiment 4. As can be seen from Fig. 2, the fine
and acicular particles of polyaniline are deposited on the surface of fibers, which are
conducive to the electron migration and the improvement of electromagnetic shielding
performances. Fig. 3 shows the diagrams of electromagnetic shielding effectiveness of
CEL-PANIlO and CEL-PANI30 respectively obtained from the embodiments 2 and 4. It can
be found from Fig. 3 that the electromagnetic shielding efficiency of aerogels increases with
the increase in the content of polyaniline. The electromagnetic shielding efficiency of
CEL-PANI30 can reach up to 9.5 dB.
The invention uses the waste paper as raw material to prepare the polyaniline/cellulose
aerogel composite materials with high electromagnetic shielding efficiency, aiming at realizing
the high-value conversion and utilization of waste. In addition, the preparation process is
green and environment-friendly. Thus, the invention has important applied values in
manufacturing sustainable and high-performance electromagnetic shielding materials.
The above embodiments and related figures are merely used to describe the technical
scheme of the invention but not restrict the invention. The invention is described in detail by
referring to the preferred embodiments. The general technicians in related fields should
understand that the changes, modifications, additions, or replacements made within the
essential scope of the invention are also in the protective scope specified in the claims of the
invention.
Claims (8)
1. A method of preparing polyaniline/cellulose aerogel composite materials is characterized by adopting the following steps: (1) the waste paper was soaked in deionized water, and mechanically stirred for 3 h at a certain speed to form homogeneous pulp, appropriate amount of sodium chlorite and pulp were mixed at mass ratio of 0.5:1, then the resulting pulp was oxidized by mechanical stirring after pH was adjusted to 4.5 by acetic acid, after the reaction, the waste paper pulp was washed with deionized water until the pH reached to 6, and then washed with anhydrous ethanol for three times to remove the residual water; (2) add a certain amount of aniline monomer to HCl solution and stir to disperse aniline monomer and hydrochloric acid evenly, take an appropriate amount of wet pulp in step (1) and add it to the above solution, then ammonium persulfate (APS) was added as an oxidant to polymerize the aniline in an ice bath, after a period of reaction, the product was centrifuged and washed and then dispersed in the deionized water; (3) the solution in step (2) was freeze-dried to obtain polyaniline/cellulose aerogel.
2. According to the claim 1, its characteristic is that the concentration of waste pulp described in step (1) is 10~15 mg/mL.
3. According to the claim 1, the characteristic is that the concentration of the HCl solution described in step (2) is 0.5-2 mol/L.
4. According to the claim 1, the characteristic is that the mass of wet pulp described in step (2) is 1-3 g.
5. According to the claim 1, the characteristic is that the mass ratio of APS/aniline described in step (2) is 1.25, and the mass fraction of aniline in wet pulp is 5~30%.
6. According to the claim 1, the characteristic is that the reaction time of aniline polymerization in ice water bath described in step (2) is 1-3 h.
7. According to any item of claims 1~6, the polyaniline/cellulose aerogel composites can be obtained.
8. According to the claim 7, the polyaniline/cellulose aerogel composites can be applied in the electromagnetic shielding.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114725404A (en) * | 2022-04-22 | 2022-07-08 | 福州大学 | Biocompatible microbial fuel cell composite anode material and preparation method thereof |
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2021
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114725404A (en) * | 2022-04-22 | 2022-07-08 | 福州大学 | Biocompatible microbial fuel cell composite anode material and preparation method thereof |
| CN114725404B (en) * | 2022-04-22 | 2023-09-01 | 福州大学 | Biocompatible microbial fuel cell composite anode material and preparation method thereof |
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