CN108341949A - Covalent bond Polyaniline Grafted nanometer stick array is modified carbon-based composite wave-absorbing material and preparation method - Google Patents
Covalent bond Polyaniline Grafted nanometer stick array is modified carbon-based composite wave-absorbing material and preparation method Download PDFInfo
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- CN108341949A CN108341949A CN201810131004.1A CN201810131004A CN108341949A CN 108341949 A CN108341949 A CN 108341949A CN 201810131004 A CN201810131004 A CN 201810131004A CN 108341949 A CN108341949 A CN 108341949A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/0206—Polyalkylene(poly)amines
- C08G73/0213—Preparatory process
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
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- C08G73/0206—Polyalkylene(poly)amines
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention relates to one kind preparing a kind of covalent bond Polyaniline Grafted nanometer stick array modification carbon-based composite wave-absorbing material by two-step reaction, wherein：Carbon material and p-phenylenediamine, sodium nitrite pH value appropriate and at a temperature of, amidized carbon material is obtained by diazo reaction, then, amidized carbon material obtains uniform covalent bond Polyaniline Grafted nano-array by home position polymerization reaction with aniline monomer and is modified C-base composte material.The present invention provides material simultaneously have small density, high temperature resistant, high resistance loss (carbon fiber), high dielectric loss (polyaniline) function admirable absorbing material.Therefore, the invention has great scientific meaning, and there is huge actual application values in terms of microwave absorbing composite material production.
Description
Technical field
The invention belongs to composite materials and technical field of fine, are related to a kind of covalent bond Polyaniline Grafted nanometer rods battle array
The modified carbon-based composite wave-absorbing material of row and preparation method.
Background technology
The fast development of modern science and technology so that various electronics, the daily life that electrical equipment is social production and people
Work brings great convenience.In turn, the electromagnetic radiation that electronic equipment generates drastically influences our life again with interference problem,
And it is ubiquitous, cause the electromagnetic environment worsening of human living space to become the tool after water source, air and noise
There is larger harmfulness and is not easy the new pollution sources protected.The pollution for how reducing electromagnetic wave is current assistant officer problem to be solved.Closely
The preparation of Nian Lai, electromagnetic wave absorbent material become research hotspot.Ideal wave absorbing agent should be with " thickness is thin, absorption band is wide, matter
Amount is light, absorbability is strong " Comprehensive Characteristics.
Carbon fiber, graphite microchip, activated carbon etc. have density small, and superhigh temperature resistant under non-oxidizing atmosphere, fatigue durability is good, than
For hot and electric conductivity between nonmetallic between metal, coefficient of thermal expansion is small and has anisotropy, good corrosion resistance.With good
Electrical and thermal conductivity performance, the advantages that electromagnetic wave shielding is good.But as absorbing material for, since it has larger conductivity,
Kelvin effect can be caused, therefore limits its application in terms of microwave absorption.Up to the present, this kind of carbon material how is reduced
Conductivity and keep primary characteristic be still great challenge for researchers.
Polyaniline is a kind of conducting polymer composite after doped, and raw material is cheap and easy to get, and synthesis is simple, is had good
Environmental stability, excellent chemical property and chemical stability.As absorbing material its with excellent dielectric loss performance.
Therefore, researcher has carried out a large amount of report to it both at home and abroad at present.However, how simple, controllable preparation has centainly
The polyaniline composite material of pattern is still scientific research problem.
Up to the present, document report is had no：One, using covalent bond Polyaniline Grafted nanometer stick array modified carbon fiber,
Prepare composite material；Two, using covalent bond Polyaniline Grafted nanometer stick array modified graphite microplate, composite material is prepared；Three, on
It states two kinds of composite materials and carries out electricity, magnetic property research.Therefore, there is very big scientific research and actual production for the exploitation of above-mentioned material
Meaning.
Invention content
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes that a kind of covalent bond Polyaniline Grafted nanometer stick array changes
Property carbon-based composite wave-absorbing material and preparation method, and its absorbing property is studied.The result shows that covalent bond Polyaniline Grafted
It is a kind of ideal wave absorbing agent that nanometer stick array, which is modified carbon-based composite wave-absorbing material,.
Technical solution
A kind of covalent bond Polyaniline Grafted nanometer stick array modification carbon-based composite wave-absorbing material, it is characterised in that：Internal layer is
Carbon material its mass fraction is 50-70%, and it is 30-50%, two kinds of materials that outer layer, which is polyaniline nano-rod array its mass fraction,
The sum of component is 100%.
The carbon material is carbon fiber, graphite microchip or activated carbon.
A method of it preparing the covalent bond Polyaniline Grafted nanometer stick array and is modified carbon-based composite wave-absorbing material, it is special
Sign is that steps are as follows：
Step 1：Carbon material is pre-processed；
Step 2：In deionized water by pretreated carbon material and p-phenylenediamine ultrasonic disperse, then into mixed solution
The micro concentrated sulfuric acid is added and so that the amount of sulfuric acid in mixed liquor is 0.016mol/L and equimolar sodium nitrite, later at 50-80 DEG C
Under be stirred to react 2-6 hours, filter, washed 3 times with straight alcohol, obtain amidized carbon material；The carbon material with to benzene two
The mass ratio of amine is about 2：3；The molar ratio of the p-phenylenediamine and sodium nitrite is 1：1；
In deionized water by the dispersion of amidized carbon material, the aqueous solution of amidized carbon material is obtained；
Step 3：Perchloric acid is added into the aqueous solution of amidized carbon material so that a concentration of 1M of perchloric acid of system,
Then the system is cooled down to 0-10 DEG C, aniline monomer stirring 30-60min is added, at this point, a concentration of 0.01- of aniline monomer
0.015mol/L is added ammonium persulfate control system temperature and is reacted 18-24 hours at 3-5 DEG C later；Stop stirring, filter, uses
Deionized water is washed 3 times, is then washed 2 times with absolute ethyl alcohol, can be obtained covalent bond Polyaniline Grafted nano-array after dry
Modified C-base composte material；The molar ratio of the aniline monomer and ammonium persulfate is 5：3.
The pretreatment is using the immersion of alkaline solution, acid solution or organic solvent.
The pretreatment is to be handled using calcination.
Advantageous effect
A kind of covalent bond Polyaniline Grafted nanometer stick array proposed by the present invention is modified carbon-based composite wave-absorbing material and preparation
Method prepares a kind of covalent bond Polyaniline Grafted nanometer stick array modification carbon-based composite wave-absorbing material by two-step reaction, wherein：
Carbon material and p-phenylenediamine, sodium nitrite pH value appropriate and at a temperature of, amidized carbon material is obtained by diazo reaction,
Then, amidized carbon material obtains uniform covalent bond Polyaniline Grafted nanometer battle array with aniline monomer by home position polymerization reaction
The modified C-base composte material of row.
The present invention is surface-treated (grease and other impurities that eliminate surface) to carbon material first, while in its table
Some hydroxyls are modified in face, then p-phenylenediamine, sodium nitrite and pH value appropriate and at a temperature of, by diazo reaction to carbon
Material surface carries out ammoxidation, and the uniform covalent bond in its surface is made to be grafted some amino groups.Finally, in aniline monomer and mistake
In the presence of ammonium persulfate initiator, using home position polymerization reaction, in carbon material surface, by amino group prepared by oxidation polymerization
Polyaniline nano-rod, and then obtain the C-base composte material of covalent bond Polyaniline Grafted nanometer stick array modification.
When the C-base composte material surface that incident electromagnetic radiation is modified to two polyaniline nano-rod arrays, first, hang down
The straight polyaniline nano-rod for being grown in carbon material surface is not only able to fully demonstrate its characteristic in microwave absorption, and can make
Obtain the absorption that repeatedly refraction reflection promotion electromagnetic wave occurs for electromagnetic wave.Secondly as polyaniline nano-rod uniformly, closely disperses
In carbon material surface prevent from contacting between two carbon materials, therefore conductive network will not be formed.The current-carrying of carbon material
Son is considered as being limited in a smaller region, therefore inhibits Kelvin effect, utilizes the high electrical loss characteristic of carbon material
Further improve the microwave absorbing property of material.Finally, it prepares the present invention provides a kind of while having that density is small, resistance to height
Temperature, high resistance loss (carbon fiber), high dielectric loss (polyaniline) function admirable absorbing material.Therefore, the invention has weight
Big scientific meaning, there is huge actual application values in terms of microwave absorbing composite material production.
Description of the drawings
Fig. 1：Each material microscopic appearance prepared by the present invention
(a) carbon fiber, (b), (c) and (d) polyaniline nano-rod array modified carbon fiber
Fig. 2：The microwave absorbing property of PANI-NH-GNPs composite materials prepared by the present invention
Fig. 3：The thermal stability of PANI-NH-GNPs composite materials
Specific implementation mode
In conjunction with embodiment, attached drawing, the invention will be further described：
Preparation method is sketched：By taking covalent bond Polyaniline Grafted nanometer stick array modified carbon fiber composite wave-suction material as an example
1. the pretreatment of carbon fiber
10g chopped carbon fibers are washed 3 times with acetone, sodium hydroxide (1M) aqueous solution is added after dry, stirs 30-
Then 60min is washed with deionized until neutrality, finally impregnate 2 hours in concentrated nitric acid, be then washed with deionized
It is dried 3 hours in 100 DEG C of baking ovens for neutrality.
2. carbon fiber amination
The pretreated chopped carbon fibers of 0.1-0.5g are gone with 0.2-0.3g p-phenylenediamine ultrasonic disperse in 130-200mL
In ionized water, the micro concentrated sulfuric acid and 0.2-0.4g sodium nitrites are then added into mixed solution, is then stirred at 50-80 DEG C
Reaction 2-6 hours, filtering, is washed 3 times with straight alcohol, obtains amidized carbon fiber, and dispersion is spare in deionized water.
3. the preparation of polyaniline nano-rod array modified carbon fiber composite material
The dense perchloric acid of 40-42mL is added into the aqueous solution of the amidized carbon fiber of above-mentioned preparation, is diluted to 500mL,
The system is cooled to 10 DEG C hereinafter, addition 500-600 μ L aniline monomers, are vigorously stirred a period of time, quickly add in ice-water bath
Enter 0.5-1.5g ammonium persulfates, stirs lower reaction 24 hours.Stop stirring, filtering is washed with deionized 2 times, then uses nothing
Water-ethanol washs 2 times, can be obtained covalent bond Polyaniline Grafted nanometer stick array modified carbon fiber composite material after dry.
4. obtained covalent bond Polyaniline Grafted nanometer stick array modified carbon fiber composite material and paraffin are uniformly mixed,
Pressurization prepares loop sample (ΦOuter diameter:7.0mm, ΦInternal diameter:3.04mm) carry out microwave absorbing property test.
Embodiment 1：
The preparation of covalent bond Polyaniline Grafted nanometer stick array modified carbon fiber composite material
1. the pretreatment of carbon fiber
5g chopped carbon fibers are washed 3 times with 30mL acetone, 100mL sodium hydroxides (1M), which are added, after dry stirs 30min,
Then be washed with deionized until neutrality, finally impregnated 2 hours in 20mL concentrated nitric acids, be then washed with deionized for
Neutrality is dried 3 hours in 100 DEG C of baking ovens.
2. carbon fiber amination
By the pretreated chopped carbon fibers of 0.5g and 0.25g p-phenylenediamine ultrasonic disperse in 200mL deionized waters, so
The 200 μ L concentrated sulfuric acids and 0.23g sodium nitrites is added in backward mixed solution, is then stirred to react at 60 DEG C 4 hours, filters,
It is washed 3 times with straight alcohol, obtains amidized carbon fiber, be dispersed in spare in 200mL deionized waters.
3. the preparation of polyaniline nano-rod array modified carbon fiber composite material
The dense perchloric acid of 41mL is added into the aqueous solution of the amidized carbon fiber of above-mentioned preparation, is diluted to 500mL, the body
It ties up in ice-water bath and is cooled to 10 DEG C hereinafter, 500 μ L aniline monomers of addition, are vigorously stirred a period of time, rapidly join 0.9g mistakes
Ammonium sulfate, control system temperature stir lower reaction 24 hours at 5 DEG C or so.Stop stirring, filtering is washed with deionized 2
It is secondary, it is then washed 2 times with absolute ethyl alcohol, it is multiple that covalent bond Polyaniline Grafted nanometer stick array modified carbon fiber is can be obtained after dry
Condensation material
Embodiment 2：
The preparation of covalent bond Polyaniline Grafted nanometer stick array modified graphite microchip composite material
1. the pretreatment of graphite microchip
By 0.5g graphite in 850-900 DEG C of stove thermal shock 20 seconds, then cool down and be immersed in 50mL ethyl alcohol
Ultrasound stripping, until graphite is totally submerged in ethyl alcohol, preservation is for use.
2. carbon fiber amination
The graphite microchip solution of above-mentioned preparation is mixed with 0.5g p-phenylenediamine, then adds water to mixed liquor about 200mL.So
The 250 μ L concentrated sulfuric acids and 0.4g sodium nitrites is added in backward mixed solution, is then stirred to react at 60 DEG C 6 hours, filters, uses
Straight alcohol washs 3 times, obtains amidized graphite microchip, and dispersion is spare in deionized water.
3. the preparation of polyaniline nano-rod array modified carbon fiber composite material
The dense perchloric acid of 41mL is added into the amidized graphite microchip mixed liquor of above-mentioned preparation, is diluted to 500mL, the body
It ties up in ice-water bath and is cooled to 10 DEG C hereinafter, 600 μ L aniline monomers of addition, are vigorously stirred a period of time, rapidly join 0.9g mistakes
Ammonium sulfate, control system temperature stir lower reaction 10 hours, 0.5g ammonium persulfates, control system temperature are added again at 5 DEG C or so
Degree stirs lower reaction 14 hours at 5 DEG C or so.Stop stirring, filtering is washed with deionized 2 times, is then washed with absolute ethyl alcohol
It washs 2 times, can be obtained covalent bond Polyaniline Grafted nanometer stick array modified graphite microchip composite material after dry.
Embodiment 3：
The preparation of covalent bond Polyaniline Grafted nanometer stick array modified active carbon composite
1. the pretreatment of activated carbon
1g activated carbons are washed 3 times with 30mL acetone, is added in 20mL concentrated nitric acids and impregnates 2 hours after dry, then spend
Ion water washing is that neutrality is dried 3 hours in 100 DEG C of baking ovens
2. activated carbon amination
By the pretreated activated carbons of 0.3g and 0.5g p-phenylenediamine ultrasonic disperse in 150mL deionized waters, then to
The 180 μ L concentrated sulfuric acids and 0.4g sodium nitrites are added in mixed solution, is then stirred to react at 70 DEG C 5 hours, filters, with pure second
Alcohol washs 3 times, obtains amidized activated carbon, and dispersion is spare in deionized water.
3. the preparation of polyaniline nano-rod array modified active carbon composite
The dense perchloric acid of 42mL is added into the aqueous solution of the amidized activated carbon of above-mentioned preparation, is diluted to 500mL, the body
It ties up in ice-water bath and is cooled to 10 DEG C hereinafter, 300 μ L aniline monomers of addition, are vigorously stirred a period of time, rapidly join 0.9g mistakes
Ammonium sulfate, control system temperature stir lower reaction 10 hours, 300 μ L aniline monomers are added again, stirring one is small at 5 DEG C or so
0.5g ammonium persulfates are added in Shi Hou, and control system temperature stirs lower reaction 14 hours at 5 DEG C or so.Stop stirring, filter, uses
Deionized water is washed 2 times, is then washed 2 times with absolute ethyl alcohol, can be obtained covalent bond Polyaniline Grafted nanometer rods battle array after dry
Row modified active carbon composite.
Embodiment 4：
According to mass ratio it is 1 by the composite material of above-mentioned preparation and paraffin:2 are uniformly mixed, and are pressed in annular standard module
Standard component (the Φ that thickness is about the annular of 2mm is madeOuter diameter:7.0mm, ΦInternal diameter:3.04mm) use vector analysis instrument (Agilent
PNA N5224A) carry out 0.5-18GHz frequency ranges in electromagnetic parameter testing, then calculate material to electromagnetism according to formula
The reflection loss performance of wave.Test result is shown in Fig. 2.
Claims (5)
1. a kind of covalent bond Polyaniline Grafted nanometer stick array is modified carbon-based composite wave-absorbing material, it is characterised in that：Internal layer is carbon
Material its mass fraction is 50-70%, and it is 30-50%, two kinds of material groups that outer layer, which is polyaniline nano-rod array its mass fraction,
The sum of part is 100%.
2. covalent bond Polyaniline Grafted nanometer stick array is modified carbon-based composite wave-absorbing material, feature according to claim 1
It is：The carbon material is carbon fiber, graphite microchip or activated carbon.
3. a kind of preparing covalent bond Polyaniline Grafted nanometer stick array modification carbon-based composite wave-absorbing material described in claims 1 or 2
Method, it is characterised in that steps are as follows：
Step 1：Carbon material is pre-processed；
Step 2：In deionized water by pretreated carbon material and p-phenylenediamine ultrasonic disperse, it is then added into mixed solution
The micro concentrated sulfuric acid so that the amount of sulfuric acid in mixed liquor is 0.016mol/L and equimolar sodium nitrite, is stirred at 50-80 DEG C later
Reaction 2-6 hours is mixed, filtering is washed 3 times with straight alcohol, obtains amidized carbon material；The carbon material and p-phenylenediamine
Mass ratio is about 2：3；The molar ratio of the p-phenylenediamine and sodium nitrite is 1：1；
In deionized water by the dispersion of amidized carbon material, the aqueous solution of amidized carbon material is obtained；
Step 3：Perchloric acid is added into the aqueous solution of amidized carbon material so that a concentration of 1M of perchloric acid of system, then
The cooling system adds aniline monomer stirring 30-60min, at this point, a concentration of 0.01- of aniline monomer to 0-10 DEG C
0.015mol/L is added ammonium persulfate control system temperature and is reacted 18-24 hours at 3-5 DEG C later；Stop stirring, filter, uses
Deionized water is washed 3 times, is then washed 2 times with absolute ethyl alcohol, can be obtained covalent bond Polyaniline Grafted nano-array after dry
Modified C-base composte material；The molar ratio of the aniline monomer and ammonium persulfate is 5：3.
4. method according to claim 3, it is characterised in that：The pretreatment is using alkaline solution, acid solution or to have
Solvent is impregnated.
5. method according to claim 3, it is characterised in that：The pretreatment is to be handled using calcination.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112457629A (en) * | 2020-11-30 | 2021-03-09 | 吉林大学 | Carbon fiber surface grafted two-dimensional network structure reinforced polyether-ether-ketone composite material and preparation method thereof |
| CN112490016A (en) * | 2020-10-13 | 2021-03-12 | 江汉大学 | Nano composite material and preparation method and application thereof |
| CN115386337A (en) * | 2022-08-12 | 2022-11-25 | 许昌学院 | Chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112490016A (en) * | 2020-10-13 | 2021-03-12 | 江汉大学 | Nano composite material and preparation method and application thereof |
| CN112457629A (en) * | 2020-11-30 | 2021-03-09 | 吉林大学 | Carbon fiber surface grafted two-dimensional network structure reinforced polyether-ether-ketone composite material and preparation method thereof |
| CN115386337A (en) * | 2022-08-12 | 2022-11-25 | 许昌学院 | Chiral polyaniline/biomass-derived porous carbon composite wave-absorbing material and preparation method thereof |
| CN115386337B (en) * | 2022-08-12 | 2023-09-08 | 许昌学院 | Chiral polyaniline/biomass derived porous carbon composite wave-absorbing material and preparation method thereof |
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