CN106243378A - A kind of graphene conductive foam and preparation method thereof - Google Patents
A kind of graphene conductive foam and preparation method thereof Download PDFInfo
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- CN106243378A CN106243378A CN201610554640.6A CN201610554640A CN106243378A CN 106243378 A CN106243378 A CN 106243378A CN 201610554640 A CN201610554640 A CN 201610554640A CN 106243378 A CN106243378 A CN 106243378A
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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
- C08J9/36—After-treatment
- C08J9/40—Impregnation
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/06—Polyurethanes from polyesters
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Conductive Materials (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Electrostatic Charge, Transfer And Separation In Electrography (AREA)
Abstract
The present invention is a kind of graphene conductive foam and preparation method thereof, relate to composite functional material technical field, comprise the following raw materials by weight percent: foam base plate 5 20%, sodium nitrate 1 2%, concentrated sulphuric acid 80 90%, graphite 1 1.5%, potassium permanganate 6 10%, 30% hydrogen peroxide 5 7%, binding agent 1 5%, reducing agent 6 10%, 5% HCl solution 25 35%, furfuryl alcohol 15 35%, oxalic acid 1 10%.The graphene conductive foam that the present invention provides has the feature of low-density and high conductivity concurrently.
Description
Technical field
The invention belongs to composite functional material technical field, relate in particular to a kind of graphene conductive foam and preparation thereof
Method.
Background technology
Conductive foam is produced by polymer composite foaming technique, foaming uniform pore diameter, softness, high resilience,
Not desquamation.The even distribution of conductive foam can protect device pin, has corrosion resistance simultaneously, for antistatic, electromagnetic screen
Cover, air-sensitive or the field such as voltage sensitive sensor, sewage purification.The preparation method that conductive foam is conventional is filling conducting objects in polymer
Prepare through foam process after matter.Conductive foam can divide common conductive foam, nickel-clad copper conductive foam, gold-plated conductive foam, plating carbon
Conductive foam, tin plating conductive foam, conductive aluminum foil foam, copper-foil conducting electricity foam, all-directional conductive foam, SMT conductive foam, I/
O conductive foam liner etc..The foam density brought in prior art is relatively big, and the electric conductivity of carbon system packing material is the most not enough.Therefore,
It is badly in need of a kind of conductive foam having low-density and higher electric conductivity concurrently.
Summary of the invention
In view of this, the invention provides a kind of graphene conductive foam and preparation method thereof, to improve existing conduction bubble
Foam can not have low-density and the problem of high electric conductivity concurrently.
For reaching above-mentioned purpose, the technical solution used in the present invention is:
A kind of graphene conductive foam, comprises the following raw materials by weight percent: foam base plate 5-20%, sodium nitrate 1-2%, dense
Sulphuric acid 80-90%, graphite 1-1.5%, potassium permanganate 6-10%, 30% hydrogen peroxide 5-7%, binding agent 1-5%, reducing agent 6-10%, 5%
HCl solution 25-35%, furfuryl alcohol 15-35%, oxalic acid 1-10%.
Preferably, in the preferred embodiment, described foam base plate be polyurethane foam, polystyrene foam,
Any one in polyethylene, polyvinyl chloride foam or polypropylene foam.
Preferably, in the preferred embodiment, described foam base plate is polyurethane foam, described polyurethane foam
It is grouped into by the one-tenth of following mass fraction: PEPA 40-50 part, isocyanates 40-50 part, amine catalyst 0.5-0.75
Part, antioxidant 0.1-0.2 part, silicone oil 0.5-0.7 part, deionized water 4-6 part, polyurethane cross-linking agent 1-2 part.
It addition, present invention also offers the preparation method of a kind of graphene conductive foam, comprise the following steps:
(1) graphene oxide is prepared
A. described sodium nitrate is added mixing and stirring in described concentrated sulphuric acid, as reactant liquor, more described graphite is added institute
State in reactant liquor；
B. in described reactant liquor, add described potassium permanganate by several times, control temperature and be 20-30 DEG C, stir with 40-50r/min
30-40min；It is warming up to 35-40 DEG C, is incubated 65-95min；
C. described reactant liquor being added water while stirring, mixing speed is 60-80r/min, is warming up to 85-95 DEG C, is incubated 60-
90min；
D. add described 30% hydrogen peroxide, filter after stirring 5-8min；Filter with described 5% HCl solution and solution washing and produce
Thing is to sulfate radical-free in filtrate；
The most then with water, filtration product is disperseed, be centrifuged separating with 1000-2000r/min with centrifuge, it is thus achieved that oxidation stone
Ink alkene;Put in 60-70 DEG C of vacuum drying oven and be dried, standby；
(2) prepared by Graphene: is distributed in described furfuryl alcohol by dried graphene oxide, is warming up to 75-85 DEG C, ultrasonic disperse
1-1.5h, forming homogeneous concentration is 1-8mg/ml graphene oxide-furfuryl alcohol mixed liquor, adds described oxalic acid, and stirring is all
Even；
(3) described foam base plate is put into described graphene oxide-furfuryl alcohol mixed liquor dipping, with padding process by graphene oxide
It is coated in foam surface；
(4) after surface-coated having the foam of graphene oxide pull out immerse containing described reducing agent, described binding agent water-soluble
Liquid reacts, it is thus achieved that the conductive foam of surface-coated graphene conductive layer.
Preferably, in the preferred embodiment, the mass ratio with the graphite added that added water in step (1)-c is
300-400:1.
Preferably, in the preferred embodiment, the reducing agent described in step (4) is hydrazine, dimethylhydrazine, boron hydrogen
Change sodium, lithium aluminium hydride, hydroiodic acid or hydrobromic acid.
Preferably, in the preferred embodiment, described foam base plate surface and pore surfaces are coated with conductive layer,
Described conductive layer be thickness be the graphene oxide of 1-2nm.
Relative to prior art, beneficial effects of the present invention: the graphene conductive foam that the present invention prepares has lower
Density and more preferable electric conductivity.The conductive layer Graphene of foam surface does not falls off through water cyclic washing, dirty as environmental protection equipment
The material for core that dye thing filters can use with repetitive cycling through over cleaning after using.Graphene is plane bidimensional monoatomic layer carbon material
Material, is to have now been found that the hardest nano material, and under room temperature, the electron mobility of Graphene reaches 106cm2V-1s-1, resistance
Rate about 10-6 Ω cm, is also the material of resistivity minimum.The foam ratio prepared by Graphene of these performance guarantees of Graphene
Regular-type foam material has less density and higher electric conductivity.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme of the present invention is further described.
Embodiment 1:
Embodiments of the invention 1 provide a kind of graphene conductive foam, comprise the following raw materials by weight percent: foam-based
Body 5%, sodium nitrate 1%, concentrated sulphuric acid 80%, graphite 1%, potassium permanganate 6%, 30% hydrogen peroxide 5%, binding agent 1%, reducing agent 6%, 5%
HCl solution 25%, furfuryl alcohol 15%, oxalic acid 1%.
Foam base plate is polyurethane foam, and polyurethane foam is grouped into by the one-tenth of following mass fraction: PEPA 40
Part, isocyanates 40 parts, amine catalyst 0.5 part, antioxidant 0.1 part, silicone oil 0.5 part, deionized water 4 parts, urethane crosslinks
Agent 1 part.
It addition, the present embodiment additionally provides the preparation method of a kind of graphene conductive foam, comprise the following steps:
(1) graphene oxide is prepared
A. sodium nitrate is added mixing and stirring in concentrated sulphuric acid, as reactant liquor, then graphite is added in reactant liquor；
B. adding potassium permanganate in reactant liquor by several times, controlling temperature is 20 DEG C, stirs 30min with 40r/min；It is warming up to 35
DEG C, it is incubated 65min；
C., reactant liquor adds water while stirring, and mixing speed is 60r/min, is warming up to 85 DEG C, is incubated 60min；
D. add 30% hydrogen peroxide, filter after stirring 5min；With in 5% HCl solution and solution washing filtration product to filtrate
Sulfate radical-free；
The most then with water, filtration product is disperseed, be centrifuged separating with 1000r/min with centrifuge, it is thus achieved that graphene oxide;
Put in 60 DEG C of vacuum drying ovens and be dried, standby；
(2) prepared by Graphene: be distributed in furfuryl alcohol by dried graphene oxide, is warming up to 75 DEG C, ultrasonic disperse 1h, shape
The concentration becoming homogeneous is 1mg/ml graphene oxide-furfuryl alcohol mixed liquor, adds oxalic acid, stirs；
(3) foam base plate is put into graphene oxide-furfuryl alcohol mixed liquor dipping, with padding process, graphene oxide is coated in bubble
Foam surface；
(4) immerse in the aqueous solution containing reducing agent, binding agent after surface-coated having the foam of graphene oxide pull out and carry out
Reaction, it is thus achieved that the conductive foam of surface-coated graphene conductive layer.
The mass ratio of the graphite added water in step (1)-c and add is 300:1.
Reducing agent described in step (4) is hydrobromic acid.
Foam base plate surface and pore surfaces are coated with conductive layer, conductive layer be thickness be the graphene oxide of 1nm.
Embodiment 2:
Embodiments of the invention 2 provide a kind of graphene conductive foam, comprise the following raw materials by weight percent: foam-based
Body 20%, sodium nitrate 2%, concentrated sulphuric acid 90%, graphite 1.5%, potassium permanganate 10%, 30% hydrogen peroxide 7%, binding agent 5%, reducing agent 10%,
5% HCl solution 35%, furfuryl alcohol 35%, oxalic acid 10%.
Foam base plate is polyurethane foam, and polyurethane foam is grouped into by the one-tenth of following mass fraction: PEPA 50
Part, isocyanates 50 parts, amine catalyst 0.75 part, antioxidant 0.2 part, silicone oil 0.7 part, deionized water 6 parts, urethane crosslinks
Agent 2 parts.
It addition, the present embodiment additionally provides the preparation method of a kind of graphene conductive foam, comprise the following steps:
(1) graphene oxide is prepared
A. sodium nitrate is added mixing and stirring in concentrated sulphuric acid, as reactant liquor, then graphite is added in reactant liquor；
B. adding potassium permanganate in reactant liquor by several times, controlling temperature is 30 DEG C, stirs 40min with 50r/min；It is warming up to 40
DEG C, it is incubated 95min；
C., reactant liquor adds water while stirring, and mixing speed is 80r/min, is warming up to 95 DEG C, is incubated 90min；
D. add 30% hydrogen peroxide, filter after stirring 8min；With in 5% HCl solution and solution washing filtration product to filtrate
Sulfate radical-free；
The most then with water, filtration product is disperseed, be centrifuged separating with 2000r/min with centrifuge, it is thus achieved that graphene oxide;
Put in 70 DEG C of vacuum drying ovens and be dried, standby；
(2) prepared by Graphene: be distributed in furfuryl alcohol by dried graphene oxide, is warming up to 85 DEG C, ultrasonic disperse 1.5h,
Forming homogeneous concentration is 8mg/ml graphene oxide-furfuryl alcohol mixed liquor, adds oxalic acid, stirs；
(3) foam base plate is put into graphene oxide-furfuryl alcohol mixed liquor dipping, with padding process, graphene oxide is coated in bubble
Foam surface；
(4) immerse in the aqueous solution containing reducing agent, binding agent after surface-coated having the foam of graphene oxide pull out and carry out
Reaction, it is thus achieved that the conductive foam of surface-coated graphene conductive layer.
The mass ratio of the graphite added water in step (1)-c and add is 400:1.
Reducing agent described in step (4) is hydrazine.
Foam base plate surface and pore surfaces are coated with conductive layer, conductive layer be thickness be the graphene oxide of 2nm.
Embodiment 3:
Embodiments of the invention 3 provide a kind of graphene conductive foam, comprise the following raw materials by weight percent: foam-based
Body 12%, sodium nitrate 1.5%, concentrated sulphuric acid 85%, graphite 1.25%, potassium permanganate 8%, 30% hydrogen peroxide 6%, binding agent 3%, reducing agent
8%, 5% HCl solution 30%, furfuryl alcohol 25%, oxalic acid 5.5%.
Foam base plate is polyurethane foam, and polyurethane foam is grouped into by the one-tenth of following mass fraction: PEPA 45
Part, isocyanates 45 parts, amine catalyst 0.62 part, antioxidant 0.15 part, silicone oil 0.6 part, deionized water 5 parts, polyurethane are handed over
Connection agent 1.5 parts.
It addition, the present embodiment additionally provides the preparation method of a kind of graphene conductive foam, comprise the following steps:
(1) graphene oxide is prepared
A. sodium nitrate is added mixing and stirring in concentrated sulphuric acid, as reactant liquor, then graphite is added in reactant liquor；
B. adding potassium permanganate in reactant liquor by several times, controlling temperature is 25 DEG C, stirs 35min with 45r/min；It is warming up to 37
DEG C, it is incubated 80min；
C., reactant liquor adds water while stirring, and mixing speed is 70r/min, is warming up to 90 DEG C, is incubated 75min；
D. add 30% hydrogen peroxide, filter after stirring 6min；With in 5% HCl solution and solution washing filtration product to filtrate
Sulfate radical-free；
The most then with water, filtration product is disperseed, be centrifuged separating with 1500r/min with centrifuge, it is thus achieved that graphene oxide;
Put in 65 DEG C of vacuum drying ovens and be dried, standby；
(2) prepared by Graphene: be distributed in furfuryl alcohol by dried graphene oxide, is warming up to 80 DEG C, ultrasonic disperse 1.25h,
Forming homogeneous concentration is 4.5mg/ml graphene oxide-furfuryl alcohol mixed liquor, adds oxalic acid, stirs；
(3) foam base plate is put into graphene oxide-furfuryl alcohol mixed liquor dipping, with padding process, graphene oxide is coated in bubble
Foam surface；
(4) immerse in the aqueous solution containing reducing agent, binding agent after surface-coated having the foam of graphene oxide pull out and carry out
Reaction, it is thus achieved that the conductive foam of surface-coated graphene conductive layer.
The mass ratio of the graphite added water in step (1)-c and add is 350:1.
Reducing agent dimethylhydrazine described in step (4).
Foam base plate surface and pore surfaces are coated with conductive layer, conductive layer be thickness be the graphene oxide of 1.5nm.
The performance test of the graphene conductive foam that embodiment 1-3 prepares is as follows, and test result is as shown in table 1:
Table 1: graphene conductive foam performance test
| Embodiment | Density, mg/cm3 | Specific surface area m2/g | Electrical conductivity S/cm |
| Embodiment 1 | 5.28 | 485 | 9 |
| Embodiment 2 | 5.40 | 480 | 8 |
| Embodiment 3 | 4.43 | 500 | 10 |
As it can be seen from table 1 the graphite alkene foam electrical conductivity prepared by the present embodiment 1-3 is about 7-10S/cm, density is about
For 4.50-5.50 mg/cm3Between, than conventional conductive foam, there is higher electric conductivity and lower density.
Claims (7)
1. a graphene conductive foam, it is characterised in that comprise the following raw materials by weight percent: foam base plate 5-20%,
Sodium nitrate 1-2%, concentrated sulphuric acid 80-90%, graphite 1-1.5%, potassium permanganate 6-10%, 30% hydrogen peroxide 5-7%, binding agent 1-5%, also
Former dose of 6-10%, 5% HCl solution 25-35%, furfuryl alcohol 15-35%, oxalic acid 1-10%.
Graphene conductive foam the most according to claim 1, it is characterised in that: described foam base plate be polyurethane foam,
Any one in polystyrene foam, polyethylene, polyvinyl chloride foam or polypropylene foam.
Graphene conductive foam the most according to claim 1, it is characterised in that: described foam base plate is polyurethane foam,
Described polyurethane foam is grouped into by the one-tenth of following mass fraction: PEPA 40-50 part, isocyanates 40-50 part, amine are urged
Agent 0.5-0.75 part, antioxidant 0.1-0.2 part, silicone oil 0.5-0.7 part, deionized water 4-6 part, polyurethane cross-linking agent 1-2
Part.
4. the preparation method of the graphene conductive foam as described in any one of claim 1-3, it is characterised in that include with
Lower step:
(1) graphene oxide is prepared
A. described sodium nitrate is added mixing and stirring in described concentrated sulphuric acid, as reactant liquor, more described graphite is added institute
State in reactant liquor；
B. in described reactant liquor, add described potassium permanganate by several times, control temperature and be 20-30 DEG C, stir with 40-50r/min
30-40min；It is warming up to 35-40 DEG C, is incubated 65-95min；
C. described reactant liquor being added water while stirring, mixing speed is 60-80r/min, is warming up to 85-95 DEG C, is incubated 60-
90min；
D. add described 30% hydrogen peroxide, filter after stirring 5-8min；Filter with described 5% HCl solution and solution washing and produce
Thing is to sulfate radical-free in filtrate；
The most then with water, filtration product is disperseed, be centrifuged separating with 1000-2000r/min with centrifuge, it is thus achieved that oxidation stone
Ink alkene;Put in 60-70 DEG C of vacuum drying oven and be dried, standby；
(2) prepared by Graphene: is distributed in described furfuryl alcohol by described dried graphene oxide, is warming up to 75-85 DEG C, ultrasonic
Dispersion 1-1.5h, forming homogeneous concentration is 1-8mg/ml graphene oxide-furfuryl alcohol mixed liquor, adds described oxalic acid, stirring
Uniformly；
(3) described foam base plate is put into described graphene oxide-furfuryl alcohol mixed liquor dipping, with padding process by graphene oxide
It is coated in foam surface；
(4) after surface-coated having the foam of graphene oxide pull out immerse containing described reducing agent, described binding agent water-soluble
Liquid reacts, it is thus achieved that the conductive foam of surface-coated graphene conductive layer.
The preparation method of graphene conductive foam the most according to claim 4, it is characterised in that: added in step (1)-c
Water is 300-400:1 with the mass ratio of the graphite of addition.
The preparation method of graphene conductive foam the most according to claim 4, it is characterised in that: described in step (4)
Reducing agent is hydrazine, dimethylhydrazine, sodium borohydride, lithium aluminium hydride, hydroiodic acid or hydrobromic acid.
The preparation method of graphene conductive foam the most according to claim 4, it is characterised in that described foam base plate surface
And pore surfaces is coated with conductive layer, described conductive layer be thickness be the graphene oxide of 1-2nm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610554640.6A CN106243378A (en) | 2016-07-14 | 2016-07-14 | A kind of graphene conductive foam and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610554640.6A CN106243378A (en) | 2016-07-14 | 2016-07-14 | A kind of graphene conductive foam and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229304A (en) * | 2019-07-09 | 2019-09-13 | 兰州大学 | A kind of fire-retardant graphene polyurethane composite foam material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557022A (en) * | 2012-03-02 | 2012-07-11 | 杭州电子科技大学 | Preparation method of graphene conductive foam |
| CN103332686A (en) * | 2013-07-12 | 2013-10-02 | 中国科学院新疆理化技术研究所 | Preparation method of three-dimensional graphene-based foam material |
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2016
- 2016-07-14 CN CN201610554640.6A patent/CN106243378A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557022A (en) * | 2012-03-02 | 2012-07-11 | 杭州电子科技大学 | Preparation method of graphene conductive foam |
| CN103332686A (en) * | 2013-07-12 | 2013-10-02 | 中国科学院新疆理化技术研究所 | Preparation method of three-dimensional graphene-based foam material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229304A (en) * | 2019-07-09 | 2019-09-13 | 兰州大学 | A kind of fire-retardant graphene polyurethane composite foam material and preparation method thereof |
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