A kind of graphene conductive fabric and preparation method thereof
Technical field
This application involves function fabric technical fields, in particular to a kind of graphene conductive fabric and its preparation side
Method.
Background technique
Graphene industry development in recent years is rapid, and graphene obtains the attention of every profession and trade with its excellent performance, especially exists
Graphene is applied and industrialization aspect research is more and more extensive.Graphene is carbon atom with sp2The hexagon of hybridized orbit composition
Honeycomb two-dimension nano materials, just because of its special construction, graphene mechanics, electricity, optics and in terms of have
Immeasurable application prospect.
If graphene can be combined with textile industry, it can assign fabric new function by graphene, to mention
The added value of high textile product.By introducing graphene in textile material, can assign the excellent electric conductivity of textile substrate and
Far infrared heating function, but due to graphene itself and do not have the group that good combination is formed with textile material, this makes stone
Black alkene is poor with basal body binding force, and every physics fastness is not high, seriously affects product quality.
Summary of the invention
The application's is designed to provide a kind of graphene conductive fabric and preparation method thereof, can be improved graphene slurry
Adhesive force between fabric keeps the binding force between graphene slurry and fabric more preferable.
In a first aspect, the embodiment of the present application provides a kind of preparation method of graphene conductive fabric, include the following steps: by
Fabric is mixed with the aqueous slkali that mass concentration is 20g/L-40g/L, handles 20min- under conditions of temperature is 50 DEG C -75 DEG C
30min.Fabric after alkali process is subjected to supercritical carbon dioxide treatment and obtains pretreating fabrics.On the surface of pretreating fabrics
Attachment graphene slurry coating obtains graphene conductive fabric.
The mass concentration of aqueous slkali is 20g/L-40g/L in alkali process, and treatment temperature is 50 DEG C -75 DEG C, is had to fabric
Certain swelling action is stripped the epidermis of fabric fibre, generates peeling phenomenon, and the surface of fiber is etched away, fine
Dimension is internal to be exposed, but the main structure of fibrous inside will not be destroyed, and the mechanicalness of fabric will not be significantly destroyed
Energy.With the synergistic effect of supercritical carbon dioxide treatment, it can make fabric that there is good swelling effect, increase fabric surface
Roughness, and the degree being swollen can make the graphene sheet layer structure in graphene slurry coating enter inside and the swelling of fabric
Gap in, keep the electric conductivity of graphene conductive fabric more preferable, antistatic effect is stronger, and washing fastness is higher.
In a kind of possible embodiment, aqueous slkali includes NaOH solution or/and KOH solution, and the quality of aqueous slkali is dense
Degree is 20g/L-25g/L.
Alkali process is carried out to fabric under conditions of mass concentration is 20g/L-25g/L using strong base solution, it can be to knitting
Object plays swelling and etching effect, and can be more preferable with the synergistic effect of supercritical carbon dioxide treatment, to obtain swelling effect
Better fabric.
In a kind of possible embodiment, the condition of supercritical carbon dioxide treatment is: temperature is 32 DEG C -40 DEG C, pressure
Power is 73atm-80atm, and the processing time is 30s-5min.Optionally, the condition of supercritical carbon dioxide treatment is: temperature 33
DEG C -35 DEG C, pressure 75atm-77atm, the processing time is 2min-4min.
Temperature is lower than 32 DEG C and/or pressure is lower than 73atm, and carbon dioxide can not be in a supercritical state;Temperature is higher than 40
DEG C and/or pressure be higher than 80atm, supercritical carbon dioxide is smaller to the facilitation of the swelling effect of conductive fabric, and produces
The production cost of product increases.Using supercritical carbon dioxide treatment is carried out under above-mentioned condition, fabric can be swollen, this
It can be cooperated with alkali process under part, improve the swelling effect of fabric, the wash durability and conduction of graphene conductive fabric
More preferably, the synergy of alkali process and supercritical carbon dioxide treatment is more preferable for performance.And since fabric have passed through alkali process, make to surpass
The condition of critical carbon dioxide processing is more mild, is more easier to reach, can save the process cost.
In a kind of possible embodiment, after alkali process, before supercritical carbon dioxide treatment, further include to fabric into
The step of row calendering is handled.Optionally, the condition of calendering processing is: pressure 6MPa-10MPa, and temperature is 100 DEG C -140 DEG C,
Speed is 20m/min-30m/min.
After alkali process, fabric may generate certain curling, after first carrying out calendering processing to fabric, then carry out
Supercritical carbon dioxide treatment, fabric is more smooth when first supercritical processing, and the swelling of supercritical carbon dioxide treatment is more
Add uniformly.
In a kind of possible embodiment, the lamella size of graphene is 0.34nm-5nm, piece diameter in graphene slurry
It is 200nm-50 μm.Optionally, the lamella size of graphene is 3nm-5nm, and piece diameter is 5 μm -10 μm.
The lamella size and piece diameter size for controlling graphene, can enable graphene be embedded in the fabric of swelling, mention
High graphene is with fabric binding force and forms complete continuous conduction access, improves the electric conductivity and fastness to washing of fabric.
In a kind of possible embodiment, the dispersing agent in graphene slurry includes anion and nonionic.Optionally,
Dispersing agent includes di-2-ethylhexylphosphine oxide benzyl naphthalene bisgallic acid sodium salt, alkyl biphenyl ether sulfonate, naphthalene sulfonic acid condensate, di-2-ethylhexylphosphine oxide methyl naphthalene
One of sulfonate sodium and fat alcohol polyethylene ether silanes are a variety of.
The graphene dispersion in graphene slurry can be made more uniform, so as to graphene uniform be embedded in fabric
Portion or the surface for being attached to fabric, so that fabric plays the functional characteristic of graphene.
Optionally, fabric is cotton class, polyester kind fabric or polyesters and cellulosic fibre blended fabric.Optionally, it knits
Object is selected from one of all-cotton fabric, cotton ramie blended spinning fabric, polyester-cotton blend and polyester-viscose blended fabric.This fabric is after alkali process, no
The intensity of fabric can be made to decline excessive, make fabric that can have the function that swelling and etching under the conditions of alkali process.
In a kind of possible embodiment, adheres to after graphene slurry coating, further include to graphene conductive fabric
The step of carrying out hot pressing, washing and sizing.By being washed and being formed after hot pressing, extend the use of graphene conductive fabric
The performance time of time, the functional characteristic of graphene conductive fabric are longer, and after repeatedly washing, functional characteristic still will not
Decline disappears.
Second aspect, the embodiment of the present application provide a kind of graphene conductive fabric, by the system of above-mentioned graphene conductive fabric
Preparation Method is prepared.
Functional material distribution in the graphene slurry coating of obtained graphene conductive fabric is more uniform, can be to stone
Black alkene conductive fabric assigns good electric conductivity, and antistatic effect is more preferable, and wash durability is more preferably.
Detailed description of the invention
Technical solution in ord to more clearly illustrate embodiments of the present application, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only some embodiments of the application, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain the protection scope that other relevant attached drawings also belong to the application.
Fig. 1 is the SEM shape appearance figure for the graphene conductive fabric that the embodiment of the present application 1 provides;
Fig. 2 is the SEM shape appearance figure for the graphene conductive fabric that the embodiment of the present application 4 provides;
Fig. 3 is the SEM shape appearance figure for the sample 1 that the application experimental example 3 provides;
Fig. 4 is the SEM shape appearance figure for the sample 2 that the application experimental example 3 provides.
Specific embodiment
It, below will be in the embodiment of the present application to keep the purposes, technical schemes and advantages of the embodiment of the present application clearer
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Graphene conductive fabric of the embodiment of the present application and preparation method thereof is specifically described below.
The preparation method of graphene conductive fabric, includes the following steps:
S110, graphene slurry is prepared:
Graphene slurry, in parts by weight, including 5-15 parts of graphene (such as: 5 parts, 8 parts, 10 parts, 12 parts or 15
Part), 1-3 parts of dispersing agent (such as: 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts), 0.5-1.5 parts of wetting agent (such as: 0.5 part, 0.8
Part, 1 part, 1.2 parts or 1.5 parts), 0.1-3 parts of adhesive (such as: 0.1 part, 0.8 part, 1 part, 2 parts or 3 parts), 1-3 parts of coupling agent
(such as: 1 part, 1.5 parts, 2 parts, 2.5 parts or 3 parts), 1-2 parts of levelling agent (such as: 1 part, 1.2 parts, 1.5 parts, 1.8 parts or 2 parts),
0.1-2 parts of defoaming agent (such as: 0.1 part, 0.5 part, 1 part, 1.5 parts or 2 parts) and 70-90 parts of solvent (such as: 70 parts, 75 parts, 80
Part, 85 parts or 90 parts).
Wherein, in graphene slurry graphene lamella size 0.34nm-5nm, 200nm-50 μm of piece diameter;Optionally, stone
The lamella size 3nm-5nm of black alkene, 5 μm -10 μm of piece diameter.Such as: the lamella size of graphene be 0.34nm, 0.4nm, 0.8nm,
1nm, 2nm, 3nm, 4nm or 5nm, the piece diameter of graphene are 200nm, 500nm, 1 μm, 2 μm, 5 μm, 8 μm, 10 μm, 20 μm or 50 μ
m。
The graphene of above-mentioned lamella size and piece diameter can preferably be embedded in the fabric of swelling or be attached to fabric
Surface, improve graphene with fabric binding force and form complete continuous conduction access and make to assign fabric with electric conductivity
The antistatic effect of fabric is more preferable.
It should be understood that graphene is laminated structure, the lamella size of graphene refers to the thickness of graphene, graphene
Piece diameter refer to the plane width of every graphene.
Dispersing agent includes anion and nonionic.Optionally, dispersing agent includes di-2-ethylhexylphosphine oxide benzyl naphthalene bisgallic acid sodium salt, alkyl
One in biphenyl ether sulfonate, naphthalene sulfonic acid condensate, dispersing agent MF salt and fat alcohol polyethylene ether silanes
Kind is a variety of.This dispersing agent can make the dispersion of graphene slurry more uniform, and the case where not needing using organic solvent
Under can also obtain finely dispersed graphene slurry, so as to the subsequent surface that functional coating is attached to fabric, and make graphite
Alkene is embedded in fabric, assigns fabric with functional characteristic.
Wetting agent includes one or more of polyether modified silicane, octyl phenol polyoxyethylene ether and ionic wetting agent;
Adhesive includes one or more of polyester resin, PU resin, epoxy resin, PVA and alkyd resin;Coupling agent includes silane
One or more of class, phthalate and aluminate;Levelling agent includes modified organic silicon class, modified acrylic acid and fluorine carbon
One or more of compounds;Defoaming agent includes one of polyethers, organic silicon and Siloxane-Oxyalkylene Copolymers class
Or it is several.
In the embodiment of the present application, the solvent in graphene slurry is aqueous solvent, such as: ethyl alcohol, deionized water or ethyl alcohol
With the mixed solution of water.Good dispersion effect can be had by not needing addition organic solvent, so that subsequent imparting fabric is with function
It can characteristic.
S120, fabric is mixed with the aqueous slkali that mass concentration is 20g/L-40g/L, the item for being 50 DEG C -75 DEG C in temperature
20min-30min is handled under part.By fabric in the aqueous slkali that mass concentration is 20g/L-40g/L, temperature is 50 DEG C -75 DEG C into
Row alkali process can be such that fabric portions are swollen, and the epidermis of fabric fibre can be stripped, and generate peeling phenomenon, the surface of fiber
It is etched away, fibrous inside is exposed, but the main structure of fibrous inside will not be destroyed, and will not significantly destroy and knit
The mechanical performance of object.Optionally, fabric is immersed in aqueous slkali and carries out alkali process, the effect of portion swells is carried out more to fabric
It is good.
In the embodiment of the present application, aqueous slkali includes NaOH solution or/and KOH solution, and aqueous slkali can be NaOH solution, alkali
Solution can be KOH solution, and aqueous slkali can also be the mixed solution of NaOH solution and KOH solution.It is with aqueous slkali below
It is illustrated for NaOH solution.
The mode of alkali process includes: to mix fabric with the NaOH solution that mass concentration is 20g/L-25g/L, is in temperature
20min-30min is handled under conditions of 50 DEG C -75 DEG C.The concentration of NaOH solution is higher, can play preferable swelling, etching is made
With to cooperate the swelling for carrying out fabric with supercritical carbon dioxide treatment.Such as: the mass concentration of NaOH solution can be
20g/L, 25g/L, 30g/L or 40g/L, the temperature of alkali process can be 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C or 75 DEG C, alkali
The time of processing can be 20min, 22min, 25min, 28min or 30min.
Optionally, fabric is cotton class, polyesters or polyesters and cellulosic fibre blended fabric.This fabric is in alkali process
After, the intensity of fabric will not be made to decline excessive, make fabric that can have the function that swelling and etching under the conditions of alkali process.Into
One step, fabric is selected from one of all-cotton fabric, cotton ramie blended spinning fabric, polyester-cotton blend and polyester-viscose blended fabric.
Fabric after S130, cleaning alkali process.Optionally, the cleaning of fabric first is carried out using 40-60 DEG C of hot water, then made
The cleaning of fabric is carried out with cold water, the rear pH value for adjusting fabric to 6-8.
It is first cleaned using hot water, reuses cold water and cleaned, to remove the alkali of fabric surface, and pass through acid
Solution adjusts the pH of fabric, so as to subsequent carry out supercritical carbon dioxide treatment.
Optionally, the pH value that fabric is adjusted using acetic acid, avoids causing to damage to fabric.
S140, calendering processing is carried out to the fabric after cleaning, fabric can be made more smooth, make the filoplume of fabric towards together
The fiber in one direction, fabric is in compressive state, so as to subsequent carry out supercritical carbon dioxide treatment.
Optionally, calendering processing is carried out to the fabric after cleaning using calender, the condition of calendering is: pressure is
6MPa-10MPa, temperature are 100 DEG C -140 DEG C, speed 20m/min-30m/min.Such as: the condition of calendering is that pressure is
8MPa, temperature are 120 DEG C, speed 25m/min.
S150, supercritical carbon dioxide treatment is carried out to the fabric after calendering, passes through alkali process and supercritical carbon dioxide
The synergistic effect of processing can make fabric have good swelling effect, increase the roughness of fabric surface, make graphene slurry
Coating is able to enter in the inside of fabric and the gap of swelling, keeps the functional characteristic of graphene conductive fabric more preferable.
Wherein, the condition of supercritical carbon dioxide treatment is: temperature is 32 DEG C -40 DEG C, pressure 73atm-80atm, place
The reason time is 30s-5min;Optionally, the condition of supercritical carbon dioxide treatment is: temperature is 33 DEG C -35 DEG C, and pressure is
75atm-77atm, processing time are 2min-4min.
Such as: the temperature of supercritical carbon dioxide treatment are as follows: 32 DEG C, 33 DEG C, 34 DEG C, 35 DEG C, 36 DEG C, 38 DEG C or 40 DEG C,
Pressure be 73atm, 74atm, 75atm, 76atm, 77atm, 78atm, 79atm or 80atm, time 30s, 1min, 2min,
3min, 4min or 5min.
S160, on the surface of pretreating fabrics, attachment graphene slurry coating obtains graphene conductive fabric.Due to fabric
It has passed through the pretreating fabrics that above-mentioned processing is swollen, keep the graphene sheet layer structure in graphene slurry coating more preferable
Ground is embedded in swelling fabric, or is attached to the surface of swollen fiber.
Fabric after supercritical carbon dioxide treatment is immersed in graphene slurry and handles 30min-1h, fabric is taken out,
So that graphene slurry is attached to surface or the insertion fabric of fabric, obtains graphene conductive fabric, graphene conductive fabric
With excellent electric conductivity and washing fastness, there can be good antistatic property.
In one optionally embodiment, graphene slurry is scratched or is sprayed on the surface of fabric, starches graphene
Material is attached to surface or the insertion fabric of fabric, obtains graphene slurry coating.
In other embodiments, graphene slurry is attached to surface or the insertion fabric of fabric by way of padding
Inside obtains graphene slurry coating.Optionally, it carries out padding processing, condition by second dipping and rolling technique are as follows: pressure
0.5Mpa-2Mpa, speed 25m/min-35m/min, pick-up rate 70%-150%.Such as: pressure 1Mpa, speed 30m/
Min, pick-up rate 100%.
S170, to being attached to the step of fabric after graphene slurry coating carries out hot pressing, washing and sizing.To remove
Adhere to unstable graphene slurry, obtains functional characteristic more preferably graphene conductive fabric.
Optionally, hot pressing refers to that hot pressing is dried, and the pressure of hot pressing drying is 0.1MPa-2MPa, and the temperature of hot pressing drying is
80 DEG C -160 DEG C, hot pressing drying time be 30s-10min, such as: pressure 0.1MPa, 0.5MPa, 0.8MPa, 1MPa,
1.5MPa or 2MPa, temperature be 80 DEG C, 100 DEG C, 120 DEG C, 140 DEG C or 160 DEG C, time 30s, 1min, 2min, 4min,
6min, 8min or 10min.
In other embodiments, hot pressing can also be carried out by the way of baking, and the time baked is 30s-10min,
The temperature baked is 90 DEG C -180 DEG C;Such as: time 30s, 1min, 2min, 4min, 6min, 8min or 10min, temperature are
90 DEG C, 100 DEG C, 120 DEG C, 150 DEG C or 180 DEG C.
Optionally, the mode of washing is that band tension is washed, and removes the graphene slurry of the non-firm attachment of fabric surface, is promoted
The washing fastness of fabric.Wherein, the temperature of washing is 20 DEG C -80 DEG C, and speed when washing is 20m/min-50m/min.Such as:
Temperature is 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C or 80 DEG C, speed 20m/min, 30m/min, 40m/min or 50m/
min。
Optionally, softening agent can be added during sizing, keep fabric more soft, sense of touch is more preferable.Wherein, softening agent
For one or more, the concentration 2g-10g/ of softening agent in modified hydrophilic silicone oil class softening agent, quaternary ammonium salt and hydrophilic softener
L, processing bath obtain pH value 5-7.
Graphene conductive fabric is prepared by the preparation method of above-mentioned graphene conductive fabric, graphene can be made to starch
Material coating uniform is densely distributed in the surface of fabric and the inside of fabric, keeps the electric conductivity of graphene conductive fabric more preferable,
With excellent antistatic property, and water-fastness performance is more preferably.
Embodiment 1
The preparation method of function fabric, includes the following steps:
(1), graphene slurry is prepared:
By lamella size be 3nm-5nm, piece diameter is 5 μm -10 μm 10 parts of graphene, alkyl biphenyl ether sulfonic acid receive dispersing agent
2 parts, 1 part of polyether modified silicane wetting agent, 2 parts of waterborne polyurethane resin adhesive, 1 part of the silane coupling agent of model KH550,
1.5 parts of modified acroleic acid levelling agent, 0.5 part and 80 parts of deionized water of organic silicon defoamer is mixed to get graphene slurry.
(2), by all-cotton fabric (specification 50S/1JC*50S/1JC, grammes per square metre 130g/m2) immersion mass concentration be 25g/L
Sodium hydroxide solution in, be warming up in 70 DEG C of water, keep the temperature 25min, take out washing drying.
It (3), is 8MPa in pressure by calender by step (2) treated fabric, temperature is 120 DEG C, and speed is
Calendering processing is carried out under conditions of 25m/min.
(4), by calendering, treated that fabric is fixed in high-pressure bottle, is 34 DEG C, pressure 76atm in temperature, processing
Time carries out supercritical carbon dioxide treatment under conditions of being 3min.
(5), immersing step (4) treated fabric in graphene slurry obtained in step (1) in pressure is 1Mpa,
Speed is 30m/min, and pick-up rate carries out second dipping and rolling process under conditions of being 100%.
(6), the fabric obtained after step (5) processing is subjected to hot pressing, washing and sizing.
Embodiment 2
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the step of embodiment 1 is provided (3) and step (4) exchange obtain the present embodiment.
Embodiment 3
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the step of embodiment 1 is provided (3) removal obtains the present embodiment.
Embodiment 4
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the fabric that step (2) provides in the present embodiment is to wash 40D*40D DTY plain cloth entirely.
Embodiment 5
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the dispersing agent in the present embodiment in step (1) is the more succimides of polyisobutene.
Embodiment 6
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the dispersing agent in the present embodiment in step (1) is di-2-ethylhexylphosphine oxide benzyl naphthalene bisgallic acid sodium salt.
Embodiment 7
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: for the graphene sheet layer in the present embodiment in step (1) having a size of 0.34nm-3nm, piece diameter is 200nm-5 μ
m。
Embodiment 8
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: for the graphene sheet layer in the present embodiment in step (1) having a size of 3nm-5nm, piece diameter is 10 μm -50 μm.
Embodiment 9
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the graphene sheet layer in the present embodiment in step step (1) having a size of 5nm-10nm, piece diameter is 50 μm-
100μm。
Embodiment 10
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the temperature that sodium hydroxide solution is handled in step step (2) in the present embodiment is 50 DEG C.
Embodiment 11
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the temperature that sodium hydroxide solution is handled in step step (2) in the present embodiment is 75 DEG C.
Embodiment 12
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the concentration of the sodium hydroxide solution of step (2) is 20g/L in the present embodiment.
Embodiment 13
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the concentration of the sodium hydroxide solution of step (2) is 40g/L in the present embodiment.
Comparative example 1
The preparation method for the graphene conductive fabric that comparative example 1 provides and the preparation method that embodiment 1 provides are almost the same,
Its difference is: the step of sodium hydroxide solution is handled in the step of embodiment 1 is provided (2) removes.
Comparative example 2
The preparation method for the graphene conductive fabric that comparative example 2 provides and the preparation method that embodiment 1 provides are almost the same,
Its difference is: the step of embodiment 1 is provided (4) removal.
Comparative example 3
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the concentration of the sodium hydroxide solution of step (2) is 15g/L in this comparative example.
Comparative example 4
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the concentration of the sodium hydroxide solution of step (2) is 45g/L in this comparative example.
Comparative example 5
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the temperature of the sodium hydroxide solution processing of step (2) is 45 DEG C in this comparative example.
Comparative example 6
The preparation method basic one that the preparation method and embodiment 1 of graphene conductive fabric provided in this embodiment provide
Cause, difference is: the temperature of the sodium hydroxide solution processing of step (2) is 80 DEG C in this comparative example.
Experimental example 1
Fig. 1 is the SEM shape appearance figure for the graphene conductive fabric that embodiment 1 provides, and Fig. 2 is the graphene that embodiment 4 provides
The SEM shape appearance figure of conductive fabric.Please refer to Fig. 1 and Fig. 2, it can be seen that be embedded with graphene between the fiber and fiber of fabric
Lamellar structure, the surface of fiber is also attached with graphene sheet layer structure, and the coating of fiber surface more uniformly, it is fine and close, say
The graphite ene coatings for the graphene conductive fabric that bright embodiment 1 and embodiment 4 provide can uniformly, be densely supported on fabric
Surface, so that graphene conductive fabric plays its functional characteristic.
Experimental example 2
Detect the performance for the graphene conductive fabric that embodiment 1- embodiment 12 and comparative example 1 and comparative example 2 provide.Its
In, Testing index has: 1., wash before graphene conductive fabric sheet resistivity, 2., after washing graphene conductive fabric table
Face sheet resistance, 3., dry fastness, 4., fastness to wet rubbing, 5., washing fastness, wherein detection method 1. and 2. is referring to GB/
The detection method recorded in T22042-2008 " clothes antistatic performance surface resistivity test method ";4. 3. detection side
Method is referring to the detection method recorded in GB/T3920-2008 " textile color stability test colour fastness to rubbing " standard test;⑤
Detection method referring to GB/T8629-2001 " textile experiment use home washings and drying program " measure in the detection side that records
Method.Table 1 is obtained by above-mentioned detection,
The performance of 1 graphene conductive fabric of table
As it can be seen from table 1 embodiment 1 and comparative example 1 and the comparison of comparative example 2 as can be seen that fabric by alkali process and
After supercritical carbon dioxide treatment cooperation, the graphene conductive fabric finally obtained is in the case where washing times are more, water
Wash that fastness is still fine, and the sheet resistivity before washing and after washing is smaller, graphene sheet layer structure more enters swelling
Fabric and swelling gap in, after washing, the changing value of sheet resistance is smaller, and graphene-supported fastness is preferable, makes stone
The functional characteristic of black alkene conductive fabric can preferably be brought into play, and washing fastness is high.
In comparative example 1, after supercritical carbon dioxide treatment, wash 10 times, the washing of graphene conductive fabric
Fastness is 3 grades;It in comparative example 2, after alkali process, washes 10 times, the washing fastness of graphene conductive fabric is 3 grades;
In embodiment 1, after have passed through alkali process and supercritical carbon dioxide treatment collective effect, wash 25 times, graphene conductive is knitted
The washing fastness of object is 4 grades.The washing times of embodiment 1 are more than twice of the washing times of comparative example 1, also above comparative example 2
Twice of washing times, the washing times of embodiment 1 are more than the sum of comparative example 1 and the washing times of comparative example 2, and embodiment
The washing for the graphene conductive fabric that the washing fastness of the 1 graphene conductive fabric provided is also provided than comparative example 1 and comparative example 2
Fastness is big.Illustrate that alkali process and supercritical carbon dioxide treatment have synergistic effect well, can reach and significantly improve washing
The effect of fastness.And from the data of sheet resistivity it can also be seen that having good synergy therebetween.
Embodiment 1 is compared with comparative example 3 as can be seen that fabric is carried out swelling and fabric through too low through the alkali of excessive concentrations
The alkali of concentration carries out cleaning and compares, and illustrates, fabric is after the alkali process of excessive concentrations, and the swelling of fabric and etching effect are more
It is good, it enters more graphenes in the inside of fabric and the gap of swelling, enables the functional characteristic of graphene conductive fabric
Enough preferably to bring into play, washing fastness is high.Can only cleaning be played the role of to fabric by the alkali of low concentration, it can not be right
Fiber is swollen and is etched.
Embodiment 1 is as can be seen that the concentration of alkali process is higher compared with comparative example 4, and when being 45g/L, graphene conductive is knitted
The functional characteristic of object can not play well.The reason is that: since alkali concentration is excessively high, the viscosity of lye increases, to fabric
Swelling effect is bad, and graphene slurry can not combine well on the fabric.
For embodiment 1 as can be seen that the temperature of alkali process is too low compared with comparative example 5, fiber surface can not be molten well
Swollen and etching, graphene slurry can not be well bonded on fabric, and the functional characteristic of conductive fabric is bad, and washing fastness is not
It is high.
For embodiment 1 as can be seen that the temperature of alkali process is excessively high compared with comparative example 6, fiber surface etching can be more serious,
Fiber surface forms defect, and in the process of washing, fiber itself has the fracture of partial extent and falls, and seriously affects washing
Fastness keeps washing fastness lower.
Embodiment 1 and embodiment 2 compare it is found that first carry out calendering, carry out supercritical carbon dioxide treatment afterwards, make graphene
The functional characteristic of conductive fabric plays more preferable.
Embodiment 1 and embodiment 3 compare it is found that without calendering processing before supercritical carbon dioxide treatment, make graphite
The functional characteristic performance effect of alkene conductive fabric is bad, and washing fastness is not high.Illustrate, before supercritical carbon dioxide treatment not into
Row calendering processing, the swelling effect of fabric are bad.
From embodiment 1 and embodiment 4 as can be seen that the different types of fabric of selection, also can be used provided by the present application
Method is swollen fabric, more preferable to play the functional characteristic of graphene conductive fabric.But different fabric types warps
It crosses after identical processing, the effect of swelling has certain difference.
Embodiment 5 and embodiment 6 are as can be seen that use the dispersing agent for containing nonionic and anion as graphene slurry
Dispersing agent, keep the dispersion effect of graphene slurry good, graphene can preferably be embedded in the inside of the fabric after swelling and empty
In gap, play the functional characteristic of graphene conductive fabric more preferable.
If from embodiment 1, embodiment 7-9 can be seen that graphene sheet layer structure size and piece diameter it is excessive, graphene
Even if being supported on the surface of fabric, after washing, can also fall off, washing fastness is bad, the function of graphene conductive fabric
Energy characteristic can not be brought into play.
It can be seen that functional characteristic of the temperature to graphene conductive fabric of alkali process from embodiment 1, embodiment 10-11
Performance have it is certain influence, illustrate that the temperature of alkali process has a certain impact to the swelling effect tool of fabric, it is too high or too low
It will affect the swelling effect of fabric, and will affect the washing fastness of fabric.
From embodiment 10-11, comparative example 1-2 can be seen that alkali process temperature be 50 DEG C or 75 DEG C when, compared to independent
Alkali process or individual supercritical carbon dioxide treatment for, washing fastness is higher, and sheet resistance is smaller, illustrates at alkali
When the temperature of reason is 50 DEG C or 75 DEG C, alkali process and supercritical carbon dioxide treatment can still play preferable synergistic effect,
The performance of the graphene conductive fabric made is more preferably.
It can be seen that functional characteristic of the concentration to graphene conductive fabric of alkali process from embodiment 1, embodiment 12-13
Performance have it is certain influence, illustrate that the concentration of alkali process has a certain impact to the swelling effect tool of fabric, it is excessively high it is too low
It will affect the swelling effect of fabric, and will affect the washing fastness of fabric.
Experimental example 3
After fabric cleaning, immerses in the sodium hydroxide solution that mass concentration is 25g/L, be warming up in 70 DEG C of water, protect
Warm 30min takes out washing drying and obtains sample 1;After fabric cleaning, it is molten to immerse the sodium hydroxide that mass concentration is 15g/L
It in liquid, is warming up in 70 DEG C of water, keeps the temperature 30min, take out washing drying and obtain sample 2.SEM is carried out to sample 1 and sample 2 respectively
Electronic Speculum measurement, obtains SEM shape appearance figure such as Fig. 3 of sample 1, SEM shape appearance figure such as Fig. 4 of sample 2.Fig. 3 and Fig. 4 comparison can be seen
Out, after the aqueous slkali of low concentration handles fabric, swelling action can not be played;The aqueous slkali of high concentration to fabric into
After row processing, swelling action can be played, and the epidermis of fiber can be stripped, generate peeling phenomenon, the surface quilt of fiber
It etches away, fibrous inside is exposed, and is conducive to and the combination of graphene slurry.
Embodiments described above is some embodiments of the present application, instead of all the embodiments.The reality of the application
The detailed description for applying example is not intended to limit claimed scope of the present application, but is merely representative of the selected implementation of the application
Example.Based on the embodiment in the application, obtained by those of ordinary skill in the art without making creative efforts
Every other embodiment, shall fall in the protection scope of this application.