CN109096752A - A kind of graphene conductive composite material and preparation method thereof - Google Patents
A kind of graphene conductive composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of graphene conductive composite materials and preparation method thereof, belong to graphene conductive Material Field.Vinyltriethoxysilane is added using graphene oxide as raw material in the present invention, and adhesion strength is glued at the interface improved between graphene oxide layer and conductive materials, facilitates the reduction of dielectric constant and dielectric loss, improves electrical efficiency；It is raw material through sodium periodate oxidation using bacteria cellulose, sodium hydrogensulfite sulfonation increases exchange site and the transport channel of ionic conduction, is improved electric conductivity, increases the conductivity of conducing composite material；Using polyvinyl alcohol as raw material, 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride is added, introduces quaternary ammonium group on polyvinyl alcohol side chain, add epoxychloropropane graft copolymerization, modified active agent is formed, so that the tensile strength and mechanical property of composite material get a promotion.The problem of present invention solves current graphene conductive material, and processing fluidity is poor in process of production, causes Compound Material Engineering that can decline.
Description
Technical field
The invention belongs to graphene conductive Material Fields, and in particular to a kind of graphene conductive composite material and its preparation side
Method.
Background technique
Graphite material has the advantages that machining accuracy height and surface effect are good, especially hard in precision, complexity, thin-walled, height
There is biggish advantage in the mold cavity processing of material.Graphite material compared with copper, have consumption less, the velocity of discharge it is fast, again
The superiority such as amount is light and thermal expansion coefficient is small, therefore gradually substitution copper electrode becomes the mainstream of electro-discharge machining material.Graphite is put
2-3 times faster than copper of electricity, material is unlikely to deform, with the obvious advantage in the processing of thin muscle electrode, the softening point of copper at 1000 DEG C or so,
It is easy to be deformed because heated, the sublimation temperature of graphite is 3650 DEG C or so, and in comparison, graphite material thermal expansion coefficient is only
There is the 1/30 of copper material.Graphene is with unusual electric conductivity, intensity beyond steel decades of times and fabulous translucency,
Its appearance is expected to cause a wheel revolution in modern electronic technology field.Due to the physical property that graphene is excellent, applied
In fields such as flexible electronic, sensor, medical treatment, radio-frequency antennas, high quality is prepared, while there is low cost, green high-efficient
Graphene series of products increasingly become the hot spot of research.In graphene, electronics can be migrated extremely efficiently, and traditional
Semiconductor and conductor, such as silicon and the copper graphene that is far from shows well.The electron energy of graphene will not be depleted, this makes
It is provided with extraordinary good characteristic.In order to obtain higher conductivity, high body to be usually added in a polymer matrix
The filler of integral, thus not only causing composite material, processing fluidity is deteriorated in process of production, and leads to composite material power
Performance decline, the production cost increases.In summary, it is therefore desirable to which a kind of better conductive material improves the prior art not
Foot.
Summary of the invention
The technical problems to be solved by the invention: it is directed to current graphene conductive material processing fluidity in process of production
Difference, the problem of causing Compound Material Engineering that can decline, provide a kind of graphene conductive composite material and preparation method thereof.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of graphene conductive composite material, including graphene substrate, nanometer additive, modified active agent；
The preparation method of the graphene substrate, includes the following steps:
(1) take graphene oxide 3 ~ 5:1 in mass ratio ~ 4:80 ~ 120 that vinyltriethoxysilane, absolute ethyl alcohol and stirring is added
Mixing adds the deionized water of graphene oxide quality 60 ~ 70%, adjusts pH to 3 ~ 4, and ultrasonic disperse is kept the temperature in 55 ~ 60 DEG C,
It filters, takes and filter slag through acetone washing, drying obtains dried object；
(2) it takes dried object 1 ~ 3:80 in mass ratio ~ 100 that ethyl alcohol is added, adds 4 ~ 6 times of dried object quality of methacryloxypropyl
Base propyl trimethoxy silicane is stirred, and obtains mixture, takes mixture 100 ~ 150:2 in mass ratio ~ 5 that Pt/C catalysis is added
Agent is passed through argon gas protection, is stirred, is cooled to room temperature to get graphene substrate.
Graphene substrate is stirred condition in the step (2) are as follows: is warming up to 45 ~ 50 DEG C and is stirred 3 ~ 5h.
The nanometer additive are as follows: take bacteria cellulose 1 ~ 3:8 in mass ratio ~ 10 that sodium periodate solution is added, be protected from light quiet
24 ~ 36h is set, is filtered, bacteria cellulose 2 ~ 5:8 in mass ratio ~ 15 after impregnating is taken out and is added in solution of sodium bisulfite, in 45 ~
50 DEG C are stirred, and filtering takes filter residue to wash through deionized water, dry, obtain nanometer additive.
The preparation method of the modified active agent, includes the following steps:
S1. it takes polyvinyl alcohol 2 ~ 5:6 in mass ratio ~ 8 that deionized water is added, is stirred 20 ~ 30min in 85 ~ 90 DEG C, adds
The potassium hydroxide of polyvinyl alcohol quality 5 ~ 10% is stirred 10 ~ 20min in 65 ~ 70 DEG C, obtains stirring mixture, take and be stirred
Object 4 ~ 9:2 in mass ratio ~ 4:30 ~ 40 is added 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride and is stirred, and must stir mixture a；
S2. it takes stirring mixture a to stir in 75 ~ 80 DEG C, 500r/min, the potassium hydroxide for being stirred amount of substance 40 ~ 50% is added
Solution is stirred, and adds the epoxychloropropane of stirring mixture a mass 50 ~ 60%, is adjusted pH to 10 ~ 11, is stirred,
PH to 6.8 ~ 7 is adjusted, stands, obtains modified active agent.
That mixture a is stirred in the step S1 is stirred condition are as follows: is stirred 2 ~ 5h in 65 ~ 70 DEG C.
A kind of preparation method of graphene conductive composite material, includes the following steps:
According to the mass fraction, take 10 ~ 30 parts of nanometer additives, 50 ~ 70 parts of graphene substrates, 8 ~ 15 parts of modified active agent, 90 ~
100 parts of deionized water mixing, ultrasonic disperse obtain ultrasonic disperse liquid, take aniline 1 ~ 4:7 in mass ratio ~ 9 that mixed in hydrochloric acid is added, obtain
Mixed liquor takes ultrasonic disperse liquid 2 ~ 5:1 in mass ratio ~ 3 that mixed liquor is added and is stirred, adds ultrasonic disperse liquid quality 3 ~ 7%
Ammonium persulfate, stand, dialysis takes dialyzate to be cast in Teflon mould, dry, removes to get graphene conductive
Composite material.
The addition mixed liquor is stirred condition are as follows: is stirred 2 ~ 5h in 75 ~ 80 DEG C.
The present invention is compared with other methods, and advantageous effects are:
(1) vinyltriethoxysilane is added using graphene oxide as raw material in the present invention, makes surface of graphene oxide containing useful
In the unsaturated double-bond of hydrosilylation, later with the Hyperbranched polysilane monomer methacryloxy containing activity double key
Propyl trimethoxy silicane, the existing si-h bond for hydrosilylation, and there are two unsaturated double bonds, are catalyzed in Pt/C
The graphene oxide and Hyperbranched polysilane monomer for being grafted vinylsiloxane under the action of agent carry out hydrosilylation,
It is smaller to the destruction of the lamellar structure of graphene oxide, while graphene oxide volume after modification is become larger, short texture, layer
Between active force reduce so that dispersion performance in the composite is improved, effectively inhibit the stacking again, poly- of its lamella
Collection, while silicon oxygen chain flexible is introduced in composite material network, while the introducing of longer soft segment can also make to be crosslinked
Chain link between point becomes larger, and then the effect of toughening is played to conducing composite material, so that mechanical property gets a promotion, obtains
Graphene substrate surface is rich in activity double key group, they can generate chemical bonding effect with conductive aniline, improves oxidation stone
Adhesion strength is glued at interface between black alkene lamella and conductive materials, these effects can effectively inhibit polymer chain movement and
The movement of polar group facilitates the reduction of dielectric constant and dielectric loss, improves electrical efficiency；
(2) present invention is raw material through sodium periodate oxidation using bacteria cellulose, then through sodium hydrogensulfite sulfonation, sulfonic group is introduced
On bacteria cellulose, the later period penetrates into aniline monomer in the network structure that dispersion is formed through in-situ polymerization, nanometer additive
On the amino of hydroxyl and aniline that has form hydrogen bond, can be evenly distributed in interface, while sulfonic introducing, increase
The exchange site of ionic conduction and transport channel increase the conductivity of conducing composite material so that electric conductivity is improved；
(3) using polyvinyl alcohol as raw material 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride is added, on polyvinyl alcohol side chain in the present invention
Quaternary ammonium group is introduced, epoxychloropropane graft copolymerization is added, forms modified active agent, the epoxy group of introducing, so that graphite
Compatibility between alkenyl material, nanometer additive and conductive materials is improved, and is provided for the graft copolymerization of conducing composite material
More active site plays respective advantage so that grafting rate improves, through being cross-linked to form fine and close knot after simultaneous processing
Structure, so that the tensile strength and mechanical property of composite material get a promotion.
Specific embodiment
Graphene substrate:
(1) take graphene oxide 3 ~ 5:1 in mass ratio ~ 4:80 ~ 120 that vinyltriethoxysilane, dehydrated alcohol, stirring is added
30 ~ 40min is mixed, the deionized water of graphene oxide quality 60 ~ 70% is added, adjusts pH to 3 ~ 4,1 ~ 3h of ultrasonic disperse, in
55 ~ 60 DEG C of 4 ~ 6h of heat preservation are filtered, and are taken and are filtered slag through acetone washing, drying obtains dried object；
(2) it takes dried object 1 ~ 3:80 in mass ratio ~ 100 that the ethyl alcohol that mass fraction is 80% is added, adds dried object quality 4 ~ 6
Methacryloxypropyl trimethoxy silane again, is stirred 30 ~ 40min, obtains mixture, take mixture in mass ratio
Pt/C catalyst is added in 100 ~ 150:2 ~ 5, is passed through argon gas protection, is warming up to 45 ~ 50 DEG C and is stirred 3 ~ 5h, be cooled to room temperature,
Up to graphene substrate.
Nanometer additive: taking bacteria cellulose 1 ~ 3:8 in mass ratio ~ 10 that concentration 0.04mol/L sodium periodate solution is added,
It is protected from light 24 ~ 36h of standing, is filtered, bacteria cellulose 2 ~ 5:8 in mass ratio ~ 15 after impregnating is taken out and the Asia that mass fraction is 5% is added
In sodium bisulfate, it is stirred 3 ~ 5h in 45 ~ 50 DEG C, filters, filter residue is taken to wash through deionized water, it is dry, it obtains nanometer and adds
Add agent.
Modified active agent:
S1. it takes polyvinyl alcohol 2 ~ 5:6 in mass ratio ~ 8 that deionized water is added, is stirred 20 ~ 30min in 85 ~ 90 DEG C, adds
The potassium hydroxide of polyvinyl alcohol quality 5 ~ 10% is stirred 10 ~ 20min in 65 ~ 70 DEG C, obtains stirring mixture, take and be stirred
3- chloro-2-hydroxypropyl-trimethyl ammonium chloride is added in object 4 ~ 9:2 in mass ratio ~ 4:30 ~ 40, is stirred 2 ~ 5h in 65 ~ 70 DEG C, obtains
Stir mixture a；
S2. stirring mixture a is taken to stir 20 ~ 30min in 75 ~ 80 DEG C, 500r/min, addition is stirred amount of substance 40 ~ 50%
Potassium hydroxide solution is stirred 30 ~ 50min, adds the epoxychloropropane of stirring mixture a mass 50 ~ 60%, adjusts pH
To 10 ~ 11, it is stirred 1 ~ 3h, adjusts pH to 6.8 ~ 7,1 ~ 3h is stood, obtains modified active agent.
A kind of preparation method of graphene conductive composite material, includes the following steps:
According to the mass fraction, take 10 ~ 30 parts of nanometer additives, 50 ~ 70 parts of graphene substrates, 8 ~ 15 parts of modified active agent, 90 ~
100 parts of deionized water mixing, 20 ~ 30min of ultrasonic disperse obtain ultrasonic disperse liquid, take aniline 1 ~ 4:7 in mass ratio ~ 9 that concentration is added
For the mixed in hydrochloric acid of 1.5mol/L, mixed liquor is obtained, takes ultrasonic disperse liquid 2 ~ 5:1 in mass ratio ~ 3 that mixed liquor is added, in 75 ~ 80 DEG C
It is stirred 2 ~ 5h, adds the ammonium persulfate of ultrasonic disperse liquid quality 3 ~ 7%, stand 18 ~ for 24 hours, dialysis takes dialyzate to be poured
It is dry in Teflon mould, it removes to get graphene conductive composite material.
Graphene substrate:
(1) it takes graphene oxide 3:1:80 in mass ratio that vinyltriethoxysilane, dehydrated alcohol is added, is stirred
30min adds the deionized water of graphene oxide quality 60%, adjusts pH to 3, ultrasonic disperse 1h, in 55 DEG C of heat preservation 4h, takes out
Filter takes and filters slag through acetone washing, and drying obtains dried object；
(2) it takes dried object 1:80 in mass ratio that the ethyl alcohol that mass fraction is 80% is added, adds 4 times of dried object quality of methyl
Acryloyloxypropyltrimethoxysilane is stirred 30min, obtains mixture, and mixture 100:2 in mass ratio is taken to be added
Pt/C catalyst is passed through argon gas protection, is warming up to 45 DEG C and is stirred 3h, be cooled to room temperature to get graphene substrate.
Nanometer additive: it takes bacteria cellulose 1:8 in mass ratio that concentration 0.04mol/L sodium periodate solution is added, is protected from light
Filtering for 24 hours is stood, bacteria cellulose 2:8 in mass ratio after impregnating is taken out and the solution of sodium bisulfite that mass fraction is 5% is added
In, it is stirred 3h in 45 DEG C, filters, filter residue is taken to wash through deionized water, it is dry, obtain nanometer additive.
Modified active agent:
S1. it takes polyvinyl alcohol 2:6 in mass ratio that deionized water is added, is stirred 20min in 85 DEG C, adds polyvinyl alcohol matter
The potassium hydroxide of amount 5%, is stirred 10min in 65 DEG C, obtains stirring mixture, and stirring mixture 4:2:30 in mass ratio is taken to add
Enter 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride, is stirred 2h in 65 DEG C, mixture a must be stirred；
S2. it takes stirring mixture a in 75 DEG C, 500r/min stirring 20min, the potassium hydroxide for being stirred amount of substance 40% is added
Solution is stirred 30min, adds the epoxychloropropane of stirring mixture a mass 50%, adjusts pH to 10, is stirred
1h adjusts pH to 6.8, stands 1h, obtains modified active agent.
A kind of preparation method of graphene conductive composite material, includes the following steps:
According to the mass fraction, take 10 parts of nanometer additives, 50 parts of graphene substrates, 8 parts of modified active agent, 90 parts of deionized waters mixed
It closing, ultrasonic disperse 20min obtains ultrasonic disperse liquid, and take aniline 1:7 in mass ratio that the mixed in hydrochloric acid that concentration is 1.5mol/L is added,
Mixed liquor is obtained, takes ultrasonic disperse liquid 2:1 in mass ratio that mixed liquor is added, is stirred 2h in 75 DEG C, adds ultrasonic disperse liquid
The ammonium persulfate of quality 3% stands 18h, and dialysis takes dialyzate to be cast in Teflon mould, dry, removes to get stone
Black alkene conducing composite material.
Graphene substrate:
(1) it takes graphene oxide 5:4:120 in mass ratio that vinyltriethoxysilane, dehydrated alcohol is added, is stirred
40min adds the deionized water of graphene oxide quality 70%, adjusts pH to 4, ultrasonic disperse 3h, in 60 DEG C of heat preservation 6h, takes out
Filter takes and filters slag through acetone washing, and drying obtains dried object；
(2) it takes dried object 3:100 in mass ratio that the ethyl alcohol that mass fraction is 80% is added, adds 6 times of dried object quality of methyl
Acryloyloxypropyltrimethoxysilane is stirred 40min, obtains mixture, and mixture 150:5 in mass ratio is taken to be added
Pt/C catalyst is passed through argon gas protection, is warming up to 50 DEG C and is stirred 5h, be cooled to room temperature to get graphene substrate.
Nanometer additive: it takes bacteria cellulose 3:10 in mass ratio that concentration 0.04mol/L sodium periodate solution is added, is protected from light
36h is stood, filtering takes out bacteria cellulose 5:15 in mass ratio after impregnating and the solution of sodium bisulfite that mass fraction is 5% is added
In, it is stirred 5h in 50 DEG C, filters, filter residue is taken to wash through deionized water, it is dry, obtain nanometer additive.
Modified active agent:
S1. it takes polyvinyl alcohol 5:8 in mass ratio that deionized water is added, is stirred 30min in 90 DEG C, adds polyvinyl alcohol matter
The potassium hydroxide of amount 10%, is stirred 20min in 70 DEG C, obtains stirring mixture, and stirring mixture 9:4:40 in mass ratio is taken to add
Enter 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride, is stirred 5h in 70 DEG C, mixture a must be stirred；
S2. it takes stirring mixture a in 80 DEG C, 500r/min stirring 30min, the potassium hydroxide for being stirred amount of substance 50% is added
Solution is stirred 50min, adds the epoxychloropropane of stirring mixture a mass 60%, adjusts pH to 11, is stirred
3h adjusts pH to 7, stands 3h, obtains modified active agent.
A kind of preparation method of graphene conductive composite material, includes the following steps:
According to the mass fraction, 30 parts of nanometer additives, 70 parts of graphene substrates, 15 parts of modified active agent, 100 parts of deionized waters are taken
Mixing, ultrasonic disperse 30min obtain ultrasonic disperse liquid, take aniline 4:9 in mass ratio that the salt acid-mixed that concentration is 1.5mol/L is added
It closes, obtains mixed liquor, take ultrasonic disperse liquid 5:3 in mass ratio that mixed liquor is added, be stirred 5h in 80 DEG C, add ultrasonic disperse
The ammonium persulfate of liquid quality 7% is stood for 24 hours, and dialysis takes dialyzate to be cast in Teflon mould, dry, removing to get
Graphene conductive composite material.
Graphene substrate:
(1) it takes graphene oxide 4:3:90 in mass ratio that vinyltriethoxysilane, dehydrated alcohol is added, is stirred
35min, adds the deionized water of graphene oxide quality 65%, adjusts pH to 3.5, ultrasonic disperse 2h, in 57 DEG C of heat preservation 5h,
It filters, takes and filter slag through acetone washing, drying obtains dried object；
(2) it takes dried object 2:90 in mass ratio that the ethyl alcohol that mass fraction is 80% is added, adds 5 times of dried object quality of methyl
Acryloyloxypropyltrimethoxysilane is stirred 35min, obtains mixture, and mixture 120:3 in mass ratio is taken to be added
Pt/C catalyst is passed through argon gas protection, is warming up to 47 DEG C and is stirred 4h, be cooled to room temperature to get graphene substrate.
Nanometer additive: it takes bacteria cellulose 2:9 in mass ratio that concentration 0.04mol/L sodium periodate solution is added, is protected from light
32h is stood, filtering takes out bacteria cellulose 3:11 in mass ratio after impregnating and the solution of sodium bisulfite that mass fraction is 5% is added
In, it is stirred 4h in 47 DEG C, filters, filter residue is taken to wash through deionized water, it is dry, obtain nanometer additive.
Modified active agent:
S1. it takes polyvinyl alcohol 3:7 in mass ratio that deionized water is added, is stirred 25min in 87 DEG C, adds polyvinyl alcohol matter
The potassium hydroxide of amount 6%, is stirred 15min in 67 DEG C, obtains stirring mixture, and stirring mixture 5:3:35 in mass ratio is taken to add
Enter 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride, is stirred 3h in 67 DEG C, mixture a must be stirred；
S2. it takes stirring mixture a in 78 DEG C, 500r/min stirring 25min, the potassium hydroxide for being stirred amount of substance 45% is added
Solution is stirred 35min, adds the epoxychloropropane of stirring mixture a mass 55%, adjusts pH to 10.5, is stirred
2h adjusts pH to 6.9, stands 2h, obtains modified active agent.
A kind of preparation method of graphene conductive composite material, includes the following steps:
According to the mass fraction, take 20 parts of nanometer additives, 60 parts of graphene substrates, 9 parts of modified active agent, 95 parts of deionized waters mixed
It closing, ultrasonic disperse 25min obtains ultrasonic disperse liquid, and take aniline 3:8 in mass ratio that the mixed in hydrochloric acid that concentration is 1.5mol/L is added,
Mixed liquor is obtained, takes ultrasonic disperse liquid 3:2 in mass ratio that mixed liquor is added, is stirred 3h in 77 DEG C, adds ultrasonic disperse liquid
The ammonium persulfate of quality 4% stands 21h, and dialysis takes dialyzate to be cast in Teflon mould, dry, removes to get stone
Black alkene conducing composite material.
Comparative example 1: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking graphene substrate.
Comparative example 2: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking nanometer additive.
Comparative example 3: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking modified active agent.
Comparative example 4: the graphene conductive composite material of company of Shenzhen production.
Above-mentioned graphene conductive composite material is detected, surface resistance test: using Keithley2700 to graphene
The surface resistance of conducing composite material is tested, and using intelligent compression Strength testing machine, is carried out to graphene conductive composite material
Compression strength, flexural strength detection obtain that the results are shown in Table 1 with the conductivity of conductivity apparatus measurement product.
Table 1:
| Detection project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 |
| Surface resistance (m Ω/sq) | 315 | 284 | 306 | 496 | 480 | 538 | 596 |
| Flexural strength (Mpa) | 6.1 | 8.54 | 7.03 | 4.23 | 3.5 | 3.68 | 3.18 |
| Compression strength (Mpa) | 23.22 | 55.56 | 37.96 | 22.32 | 20.03 | 21.21 | 13.05 |
| 10 × 103(S/m of conductivity) | 7.853 | 7.863 | 7.787 | 6.582 | 6.135 | 6.324 | 5.413 |
In summary, graphene conductive composite material effect of the invention is more preferable, is worth of widely use.
Claims (7)
1. a kind of graphene conductive composite material, which is characterized in that including graphene substrate, nanometer additive, modified active agent；
The preparation method of the graphene substrate, includes the following steps:
(1) take graphene oxide 3 ~ 5:1 in mass ratio ~ 4:80 ~ 120 that vinyltriethoxysilane, absolute ethyl alcohol and stirring is added
Mixing adds the deionized water of graphene oxide quality 60 ~ 70%, adjusts pH to 3 ~ 4, and ultrasonic disperse is kept the temperature in 55 ~ 60 DEG C,
It filters, takes and filter slag through acetone washing, drying obtains dried object；
(2) it takes dried object 1 ~ 3:80 in mass ratio ~ 100 that ethyl alcohol is added, adds 4 ~ 6 times of dried object quality of methacryloxypropyl
Base propyl trimethoxy silicane is stirred, and obtains mixture, takes mixture 100 ~ 150:2 in mass ratio ~ 5 that Pt/C catalysis is added
Agent is passed through argon gas protection, is stirred, is cooled to room temperature to get graphene substrate.
2. graphene conductive composite material according to claim 1, which is characterized in that graphene-based in the step (2)
Material is stirred condition are as follows: is warming up to 45 ~ 50 DEG C and is stirred 3 ~ 5h.
3. graphene conductive composite material according to claim 1, which is characterized in that the nanometer additive are as follows: take thin
Sodium periodate solution is added in fungin 1 ~ 3:8 in mass ratio ~ 10, is protected from light 24 ~ 36h of standing, filters, and it is fine to take out bacterium after impregnating
Tie up element 2 ~ 5:8 in mass ratio ~ 15 be added solution of sodium bisulfite in, be stirred in 45 ~ 50 DEG C, filtering, take filter residue gone from
Sub- water washing, it is dry, obtain nanometer additive.
4. graphene conductive composite material according to claim 1, which is characterized in that the preparation side of the modified active agent
Method includes the following steps:
S1. it takes polyvinyl alcohol 2 ~ 5:6 in mass ratio ~ 8 that deionized water is added, is stirred 20 ~ 30min in 85 ~ 90 DEG C, adds
The potassium hydroxide of polyvinyl alcohol quality 5 ~ 10% is stirred 10 ~ 20min in 65 ~ 70 DEG C, obtains stirring mixture, take and be stirred
Object 4 ~ 9:2 in mass ratio ~ 4:30 ~ 40 is added 3- chloro-2-hydroxypropyl-trimethyl ammonium chloride and is stirred, and must stir mixture a；
S2. it takes stirring mixture a to stir in 75 ~ 80 DEG C, 500r/min, the potassium hydroxide for being stirred amount of substance 40 ~ 50% is added
Solution is stirred, and adds the epoxychloropropane of stirring mixture a mass 50 ~ 60%, is adjusted pH to 10 ~ 11, is stirred,
PH to 6.8 ~ 7 is adjusted, stands, obtains modified active agent.
5. graphene conductive composite material according to claim 4, which is characterized in that stir mixture in the step S1
A's is stirred condition are as follows: is stirred 2 ~ 5h in 65 ~ 70 DEG C.
6. a kind of preparation method of the graphene conductive composite material as described in claim 1 ~ 5 any one, which is characterized in that
The preparation method includes the following steps:
According to the mass fraction, take 10 ~ 30 parts of nanometer additives, 50 ~ 70 parts of graphene substrates, 8 ~ 15 parts of modified active agent, 90 ~
100 parts of deionized water mixing, ultrasonic disperse obtain ultrasonic disperse liquid, take aniline 1 ~ 4:7 in mass ratio ~ 9 that mixed in hydrochloric acid is added, obtain
Mixed liquor takes ultrasonic disperse liquid 2 ~ 5:1 in mass ratio ~ 3 that mixed liquor is added and is stirred, adds ultrasonic disperse liquid quality 3 ~ 7%
Ammonium persulfate, stand, dialysis takes dialyzate to be cast in Teflon mould, dry, removes to get graphene conductive
Composite material.
7. the preparation method of graphene conductive composite material according to claim 6, which is characterized in that the addition mixing
Liquid is stirred condition are as follows: is stirred 2 ~ 5h in 75 ~ 80 DEG C.
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| CN111194105A (en) * | 2020-04-15 | 2020-05-22 | 广东康烯科技有限公司 | Platinum quantum dot doped graphene-based electric heating plate and electric heating device |
| CN112142862A (en) * | 2020-09-04 | 2020-12-29 | 广东轻工职业技术学院 | Method for preparing sulfonated cellulose |
| CN114775090A (en) * | 2022-05-17 | 2022-07-22 | 凯盛家纺股份有限公司 | Preparation method of graphene modified anti-static fabric |
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Application publication date: 20181228 |