CN108793127A - A kind of production technology can be mass graphene non-woven fabrics - Google Patents
A kind of production technology can be mass graphene non-woven fabrics Download PDFInfo
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- CN108793127A CN108793127A CN201810584625.5A CN201810584625A CN108793127A CN 108793127 A CN108793127 A CN 108793127A CN 201810584625 A CN201810584625 A CN 201810584625A CN 108793127 A CN108793127 A CN 108793127A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
- D06C7/04—Carbonising or oxidising
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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Abstract
The invention discloses a kind of production technologies can be mass graphene non-woven fabrics, include the following steps, prepare graphene oxide；Graphene oxide is coated to fiber surface using ultrasonic wave dipping pressure rolling combination method, the non-woven weight after drying increases 20-30%；Fiber surface is coated with to the non-woven fabrics of graphene oxide, is placed in reducing solution, graphene oxide is reduced to graphene；Fiber surface is coated with graphene nonwoven be arranged into calcining furnace carried out under the conditions of protective gas calcination temperature be 1000-3000 DEG C, non-woven fabrics carbonization.A kind of production technology can be mass graphene non-woven fabrics according to the present invention, graphene oxide will be used to coat graphene oxide to non-woven fabrics fiber surface using ultrasonic wave dipping pressure rolling combination method, it is prepared using reduction calcining, it can be mass graphene non-woven fabrics, rational technology, prepared graphene non-woven fabrics can also include higher ultimate strength while with high conduction performance.
Description
Technical field
The present invention relates to graphene nonwoven production technical field, especially a kind of life can refer to production graphene non-woven fabrics
Production. art.
Background technology
With the fast development of economic globalization society, the foreground of global functional textile is also become better and better.New technology
New product is constantly updated, a piece of light of market prospects.In recent years, it was applied to fabric fibre about grapheme material both at home and abroad
Dimension, the report of function textile are commonplace.Nowadays functional non-woven fabric product is generally obtained there are three types of method, is respectively
With the direct woven fabric of functional fibrous raw material, common non-woven fabric and functional non-woven fabric structure composite and functional topical finishing is common
Non-woven fabrics.Wherein functional topical finishing is the method that current most convenient fast prepares functional non-woven fabric, but this method system
The functionality of standby functional non-woven fabric can weaken with the increase of access times even to be lost, and disposable type is only suitable for
Non-woven cloth products.
Graphene (Graphene) has excellent optics, electricity and mechanics etc. special as a kind of following revolutionary material
Property.The optically and electrically performance of graphene is because its internal carbon is with sp2 hybridized orbit bondings, and carbon atom has 4 valence electricity
Son, wherein 3 to electronics, each provides a non-bonding electrons in pz tracks, and the pz track closer from atom and plane at
The pi bond of underfill state is formed when vertical direction, pi-electron can move freely in crystal, have good electrical performance；And stone
Carbon atom ligancy is 3 in black alkene, wherein other than σ keys and other carbon atom chains are connected into the cellular layer structure of hexagonal ring,
The pz tracks perpendicular to layer plane of each carbon atom can form polyatomic big pi bond through holostrome, be similar to phenyl ring knot
Structure, thus there is excellent optical property.
Graphene oxide (Graphene oxide) is the oxide of graphene, and color is brown color, is powdered graphite
Product after chemical oxidation and stripping, because its single atomic layer structure, extensibility are especially good.By oxidation processes
Afterwards, the layer structure of graphite had not only been maintained, but also has introduced many groups on each layer of graphene sheet layer.Pass through these groups
It is set to exist with extremely stable state in water or polar solvent.
Research at this stage finds that graphene oxide has dual parent's property, is in from graphene platelet marginal portion to center portion
Reveal hydrophilic to hydrophobic property distribution.Therefore, graphene oxide can as interfacial agent generally there are on interface simultaneously
Reduce the energy between interface.Simultaneously as the presence of these groups so that graphene oxide layer is thicker compared with graphene sheet layer, about
1nm.These groups can be reacted with the group on non-woven viscose fabric surface so that graphene oxide can more firm and nonwoven
Cloth is combined together.
Graphene fiber artificially is better achieved in function in the plum etc. of engineering college in Beijing Institute of Clothing Tech's material science
Property textile field macroscopic view application, using certain density graphite oxide solution as spinning solution, calcium chloride solution is coagulating bath, lead to
It crosses wet spinning and prepares graphite oxide fiber, restored through hydroiodic acid and obtain graphene fiber.Using x-ray photoelectron spectroscopy and thoroughly
It penetrates electron microscope respectively to characterize the degree of oxidation and structure and morphology of graphene oxide spinning solution, finds graphene oxide
Degree of oxidation it is high, carbon-to-oxygen ratio is about 1：1, and show light lamellose fold pattern.Have studied different quality containing
Influence of the calcium chloride coagulation bath to graphene fiber tensile strength, the results showed that, it is made when calcium chloride mass fraction is 20%
The conductivity of graphene fiber is 180S/cm, and tensile strength 892MPa shows good electric conductivity and mechanical flexibility.
Textile garment institute of University Of Qingdao has studied functional graphene fiber element composite fibre in Rong Rong et al., test
Its mechanical property, anti-ultraviolet property, antistatic property and flame retardant property etc..Have studied how by graphene to nylon fibre into
Row modification prepares graphene functional textile.Finally, the application to functional graphene composite fibre and textile and develop into
Prospect is gone.
But the present production method of non-woven fabrics as pure graphene typically uses and solution is made in graphene uses
The method of Static Spinning prepares graphene non-woven fabrics.It is unsuitable for producing in batches using the method that the method for Static Spinning prepares graphene
Graphene non-woven fabrics.
Invention content
The object of the present invention is to provide a kind of production technologies can be mass graphene non-woven fabrics, using graphene coated
To fiber surface using calcining, graphene non-woven fabrics can be produced in batches.
In order to solve the above technical problems, the object of the present invention is achieved like this：
A kind of production technology can be mass graphene non-woven fabrics according to the present invention, includes the following steps：
(1), crystalline flake graphite is aoxidized, prepares graphene oxide；
(2), graphene oxide is coated to non-woven fabrics fiber surface using ultrasonic wave dipping pressure rolling combination method, and dried,
So that the non-woven weight after drying increases 20-30%；
(3), the fiber surface prepared by step (2) is coated with to the non-woven fabrics of graphene oxide, is placed in reducing solution
In, graphene oxide is reduced to by graphene by reduction reaction；
(4), the nonwoven that the fiber surface prepared by step (3) is coated with to graphene is arranged into calcining furnace and is protecting
It is calcined under gas condition, the temperature of calcining is 1000-3000 DEG C, and graphene non-woven fabrics is completed in non-woven fabrics carbonization
It prepares.
As a further illustration of the above scheme, the specific method of step (2) is：Using Hummers methods by crystalline flake graphite
Graphene oxide is made；It is molten that graphene oxide is prepared according to the ratio that 0.02g graphene oxides are put into the distilled water of 100ml
Liquid；And ultrasonic disperse is carried out to the graphene oxide solution of preparation using ultrasonic wave；By the nonwoven Jing Guo alkali process be arranged into through
It crosses in the graphene oxide solution of ultrasonic disperse and carries out ultrasonic wave dipping, pressure rolling and dry, until the weight of non-woven fabrics increases 20-
30%.
As a further illustration of the above scheme, the specific method of step (3) is：It selects hydrazine hydrate as reducing agent, presses
According to 3ml Hydrazine Hydrate Analyzing is pure plus distilled water is to the ratio of 100ml, be configured to a concentration of 3% hydrazine hydrate solution；By step
(2) nonwoven that the fiber obtained by is coated with graphene oxide is arranged into hydrazine hydrate solution, heating water bath under the conditions of 90 DEG C
Graphene oxide is restored to graphene by reaction；It is dried after net remaining hydrazine hydrate is washed with deionized water in non-woven fabrics again.
As a further illustration of the above scheme, the non-woven fabrics is viscose glue spunlace non-woven cloth.
As a further illustration of the above scheme, the preparation of the graphene oxide includes the following steps：
(1), graphite pre-oxidizes：Take 5g crystalline flake graphites, 2g potassium peroxydisulfates and the concentrated sulfuric acid of 4g phosphorus pentoxides and 20ml mixed
It closes, is warming up to 80 DEG C, fully reacts 5h, deionized water is added later to 200ml, stirs evenly, taken out after the solution layering such as standing
Supernatant is taken, the graphite after being pre-oxidized after adding deionized water to be filtered is 12 hours dry in 60 DEG C of vacuum drying ovens.
(2) graphite oxidation：It is placed in container in the obtained pre-oxidation graphite of step (1), under the conditions of 0 DEG C, is added
The concentrated sulfuric acid of 1g sodium nitrate and 40ml is uniformly mixed, and potassium permanganate is added according still further to the addition speed no more than 1g/4min, makes
With water-bath magnetic agitation 2h；The reaction was continued after being warming up to 45 DEG C again 30min, after drained with glass bar 100ml deionized waters be added
10min is reacted with the hydrogen peroxide of 8ml a concentration of 30%；The concentrated hydrochloric acid pickling of addition 6% three times, adds excessive deionized water,
It carries out centrifuging once under the conditions of 9000 turns of 15min, then taking precipitate centrifuges several times, directly under the conditions of 9000 turns of 30min
To neutrality, 400ml deionized waters are added in taking precipitate, and ultrasonic 30min continues centrifugation once under the conditions of 8000 turns of 15min, on
Clear liquid is graphite oxide solution, and drying obtains graphite oxide.
The beneficial effects of the invention are as follows：A kind of production work can be mass graphene non-woven fabrics according to the present invention
Skill, will using Hummers methods prepare graphene oxide using ultrasonic wave dipping pressure rolling combination method by graphene oxide coat to
Non-woven fabrics fiber surface is prepared using reduction calcining, can compared with conventional method of electrostatic spinning prepares pure graphene non-woven fabrics
Produce graphene non-woven fabrics in batches.Prepared graphene non-woven fabrics can also include higher while with high conduction performance
Ultimate strength.
Description of the drawings
Fig. 1 is the microgram of graphene non-woven fabrics according to the present invention.
Fig. 2 is the microgram of non-woven viscose fabric；
Fig. 3 is the photothermal conversion performance map of graphene/non-woven viscose fabric；
Volume resistivity when Fig. 4 is graphene/non-woven viscose fabric difference bending number.
Specific implementation mode
Present invention will be further explained below with reference to the attached drawings and specific examples.
Embodiment one
A kind of production technology can be mass graphene non-woven fabrics involved by the present embodiment, includes the following steps：
1, crystalline flake graphite is aoxidized, prepares graphene oxide.
2, graphene oxide is coated to non-woven fabrics fiber surface using ultrasonic wave dipping pressure rolling combination method, and dried, made
Non-woven weight after must drying increases by 20%；
3, fiber surface prepared by step (2) is coated with to the non-woven fabrics of graphene oxide, be placed in reducing solution,
Graphene oxide is reduced to graphene by reduction reaction；
4, nonwoven that fiber surface prepared by step (3) is coated with to graphene is arranged into calcining furnace and in protection gas
It is calcined under concrete conditions in the establishment of a specific crime, the temperature of calcining is 1000 DEG C, and the preparation of graphene non-woven fabrics is completed in non-woven fabrics carbonization.
Wherein be in step 1 crystalline flake graphite is made by graphene oxide using Hummers methods, including graphite pre-oxidation and
Graphite oxidation.
The method for preparing graphene oxide have mechanical stripping method, oxidation-reduction method, epitaxy method, silicon carbide epitaxy method,
The methods of He Mofa, chemical vapour deposition technique.Graphene is made by mechanical stripping method first, and this method is easy to operate, is made
Sample quality is high, but its poor controllability, and graphene size obtained is smaller and has very big uncertainty, while efficiency is low, cost
Height is not suitable for large-scale production.
Oxidation-reduction method (Hummers methods).Oxidation-reduction method becomes the most extensive and ripe side of research because of its yield height
Method, but gained quality of graphene is relatively low.Other methods are difficult to mass produce at this stage, and chemistry redox method is at this stage
Unique practical method.Its method is to handle graphite crystal using strong oxidizer, and piece interlayer Van der Waals is destroyed by supersound process
Power makes it be dispersed in water, forms graphene oxide.
Graphite pre-oxidation is that 5g crystalline flake graphites, 2g potassium peroxydisulfates and 4g phosphorus pentoxides is taken to be mixed with the concentrated sulfuric acid of 20ml,
80 DEG C are warming up to, 5h is fully reacted, deionized water is added later to 200ml, stirs evenly, is extracted after the solution layering such as standing
Clear liquid, the graphite after being pre-oxidized after adding deionized water to be filtered are 12 hours dry in 60 DEG C of vacuum drying ovens.
Graphite oxidation is will to be placed in dry container in obtained pre-oxidation graphite, and under the conditions of 0 DEG C, 1g nitre is added
The concentrated sulfuric acid of sour sodium and 40ml is uniformly mixed, and potassium permanganate is added according still further to the addition speed no more than 1g/4min, uses water
Bathe magnetic agitation 2h；The reaction was continued after being warming up to 45 DEG C again 30min, after drained with glass bar 100ml deionized waters and 8ml be added
A concentration of 30% hydrogen peroxide reacts 10min, and solution becomes yellow from brick-red at this time, obtains graphene oxide solution；It is added
6% concentrated hydrochloric acid pickling three times, adds excessive deionized water, carries out centrifuging once under the conditions of 9000 turns of 15min, takes precipitation
Then object centrifuges several times under the conditions of 9000 turns of 30min, until neutral, 400ml deionized waters, ultrasound is added in taking precipitate
30min continues centrifugation once under the conditions of 8000 turns of 15min, and supernatant is graphite oxide solution, and drying obtains graphite oxide.
In step 2, Hummers methods will be used made graphene oxide, according to 0.02g graphene oxides be put into
The ratio of the distilled water of 100ml prepares graphene oxide solution.And the graphene oxide solution of preparation is carried out using ultrasonic wave
Ultrasonic disperse is multilayer by graphite oxide made from hummers methods, thus the graphene oxide that obtain single layer need into
One step is processed.Main method is to be separated into single layer by using ultrasonic vibration instrument.By the nonwoven arrangement Jing Guo alkali process
Enter to carry out ultrasonic wave dipping, pressure rolling in the graphene oxide solution by ultrasonic disperse and dry, until the weight of non-woven fabrics increases
20-30%.The present invention obtained ultrasonic wave dipping refer to while being impregnated to non-woven fabrics, it is molten to graphene oxide
Liquid carries out ultrasonic wave dispersion, disperses graphene oxide that can be used can be easier to make for the inside of non-woven fabrics to its ultrasonic wave.
Zhang Xiansheng et al. according to University Of Qingdao has studied the performance of graphene viscose composite fiber in detail.Pass through its fibre
The microscopic pattern and internal structure of dimension are characterized；Further study the tensile strength performance of the fiber, flame retardant property and
Anti-ultraviolet property.The result shows that：Graphene viscose composite fiber has superior mechanical performance compared with common viscose fiber, and
Graphene is modified to viscose rayon, and the flame retardant property of fiber, anti-ultraviolet property is significantly improved, and graphene/viscose glue is multiple
Condensating fiber improves the added value of product of common viscose fiber, has broad application prospects.Non-woven fabrics selection is viscous in this step
The grammes per square metre of glue prick nonwoven cloth, viscose glue spunlace non-woven cloth is 100-120 grams every square metre.
And used alkali is sodium hydroxide in this step.Why to non-woven viscose fabric carry out alkali process, be because
For in non-woven viscose fabric production process, nonwoven surface has some slurries, surface size can lead to being starched for adhesive surface
Material is surrounded and can not be reacted with the surface group of graphene oxide, leads to the effect of non-woven viscose fabric oxide impregnation graphene solution
It is bad, graphene oxide can not be combined with viscose rayon, it is therefore desirable to slurry be needed to handle：Non-woven viscose fabric is put into bath
Than being 1：It is heated to 80 DEG C in 50 sodium hydroxide (NaOH) solution and boils 30min, drying is then washed with deionized.It obtains
Non-woven fabrics fabric not only eliminates slurry, can also remove some dust impurities on surface.
When coating graphene oxide to viscose rayon surface, it is possible to cannot be used by a ultrasonic wave dipping viscous
The weight of glue non-woven fabrics increases up to requirement, and the non-woven viscose fabric after being impregnated to ultrasonic wave is needed to dry and carry out ultrasonic wave leaching again
Stain or repeated ultrasonic wave dipping, until the rate of body weight gain of non-woven viscose fabric reaches requirement.
It by the graphene oxide for being coated on viscose rayon surface in non-woven fabrics was graphite originally that step 3, which is by reduction reaction,
Alkene.Specific method is to select hydrazine hydrate as reducing agent, according to the pure ratio for adding distilled water to 100ml of the Hydrazine Hydrate Analyzing of 3ml
Example, is configured to a concentration of 3% hydrazine hydrate solution；Fiber obtained by step (2) is coated with to the non-woven fabrics of graphene oxide
It is placed in hydrazine hydrate solution, graphene oxide is restored to graphene by heating in water bath for reaction under the conditions of 90 DEG C；Again by viscose glue without
Drying is washed with deionized water after net remaining hydrazine hydrate to get to graphene/non-woven viscose fabric after reduction in woven fabric.
The fracture contracting strength for being coated with the non-woven viscose fabric of the graphene after reduction has compared with non-woven viscose fabric and to become smaller
Trend, but the amount of reduction and little.Ultimate strength the reason of becoming smaller in Non-woven fabric ultrasonic wave impregnate and use water
When closing hydrazine reduction, viscose rayon can be made constantly to contact solution, certain destruction, and fiber occur using the structure of non-woven fabrics
Strength can also reduce.
To being coated with the non-woven viscose fabric of graphene in a stretched state, test resistance simultaneously calculates volume resistivity, it is known that
The electric conductivity of graphene/non-woven viscose fabric is 0.1-0.7 Ω * m, the viscose rayon in non-woven viscose fabric by measuring and calculation
Surface is complete by graphene coated, and volume resistivity is stablized 0.1 or so, graphene viscose rayon is coated it is more complete,
Pi-electron on fiber increases and mobile space becomes larger, and when coating number and reaching certain amount, graphene is by viscose rayon
Basic cladding is complete, and pi-electron only increases in fiber surface, and electric conductivity increases unobvious.
Fabric electric conductivity does not change substantially after multiple folded bent, in the present embodiment select 100,200,300,
400,500 times.Since graphene itself has preferable mechanical performance, while being combined by chemical group with viscose rayon, compared with
It is secured, is not easy because bending is fallen.So folded bent does not have much affect for electric conductivity.Illustrate graphene and viscose glue
In conjunction with more closely, there is preferable practical performance.
Light thermal property conversion of the graphene/non-woven viscose fabric than former non-woven viscose fabric has great promotion.In same intensity
Under Infrared irradiation, non-woven viscose fabric maximum temperature can only achieve 40 DEG C or so, and graphene/non-woven viscose fabric can reach
100 DEG C or more.When irradiating the graphene/non-woven viscose fabric through outer light source, measures and understand that its temperature can rise to 70- in 5s-10s
80 DEG C, and can be warming up to 100 DEG C or more after irradiating 60s.
Graphene/the non-woven viscose fabric is carried out doing ultraviolet performance and is tested, the UPF of the graphene/non-woven viscose fabric
Value has had reached 100+, and T (UVA) and T (UVB) is respectively less than 5%, by standard GB/T/T18830-2002《Textile is anti-
The evaluation of imparted energy》In " antiultraviolet product " measure and require regulation, as the UPF > 30 of sample, and T (UVA) AV < 5%
When, it can be described as " antiultraviolet product ".
The test structure of the above test event see the table below, test data is the average value repeatedly tested in table
In step 4, the nonwoven that prepared fiber surface is coated with to graphene is arranged into calcining furnace and with nitrogen
Gas calcines it as under the conditions of protective gas, and the temperature of calcining is 1000-3000 DEG C, and the time is 2 hours so that viscose glue
Non-woven fabrics is carbonized, and completes the preparation of graphene non-woven fabrics.Non-woven viscose fabric can be carbonized completely, form hollow graphene nonwoven
Cloth, weight per square meter are 20-30 grams.
Graphene non-woven fabrics after calcining, except ultimate strength becomes outside the pale of civilization, remaining changes less.Due to fiber surface
Complete by graphene coated, that is tested is determined by the property of graphene itself.Non-woven viscose fabric is in above-mentioned test event
In, the Hu ultimate strength that can influence.Such method has and can be mass compared with prepare pure graphene non-woven fabrics
Pure graphene non-woven fabrics.
Preferable spontaneous hot property and uvioresistant performance, impart the wider array of use scope of graphene non-woven fabrics, can
It is used in more extensive field.Since this kind of graphene non-woven fabrics is the viscose rayon surface in viscose glue spunlace non-woven cloth
It made by coated graphite alkene, may make it that there is structure similar with viscose glue spunlace non-woven cloth, can be used as filtering material use.
Raw material as used in the present invention is commercially available.Raw material sources see the table below.
Embodiment two
A kind of production technology can be mass graphene non-woven fabrics involved by the present embodiment, includes the following steps：
1, crystalline flake graphite is aoxidized, prepares graphene oxide.
2, graphene oxide is coated to non-woven fabrics fiber surface using ultrasonic wave dipping pressure rolling combination method, and dried, made
Non-woven weight after must drying increases by 30%；
3, fiber surface prepared by step (2) is coated with to the non-woven fabrics of graphene oxide, be placed in reducing solution,
Graphene oxide is reduced to graphene by reduction reaction；
4, nonwoven that fiber surface prepared by step (3) is coated with to graphene is arranged into calcining furnace and in protection gas
It is calcined under concrete conditions in the establishment of a specific crime, the temperature of calcining is 3000 DEG C, and the preparation of graphene non-woven fabrics is completed in non-woven fabrics carbonization.
In the present embodiment, difference lies in the reduction reaction in step 2 uses hydroiodic acid steam also with embodiment one
Original, the hydroiodic acid solution concentration for forming used hydroiodic acid steam are 40wt%-60wt%.Prepared by hydroiodic acid steam reduction
After fiber surface is coated with the non-woven fabrics of graphene oxide, after drying at room temperature.
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that those skilled in the art without
It needs creative work according to the present invention can conceive and makes many modifications and variations.Therefore, all technologies in the art
Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Technical solution, all should be in the protection domain being defined in the patent claims.
Claims (5)
1. a kind of production technology can be mass graphene non-woven fabrics, which is characterized in that include the following steps：
(1), crystalline flake graphite is aoxidized, prepares graphene oxide；
(2), graphene oxide is coated to non-woven fabrics fiber surface using ultrasonic wave dipping pressure rolling combination method, and dried so that
Non-woven weight after drying increases 20-30%；
(3), the fiber surface prepared by step (2) is coated with to the non-woven fabrics of graphene oxide, is placed in reducing solution, is led to
It crosses reduction reaction and graphene oxide is reduced to graphene；
(4), the nonwoven that the fiber surface prepared by step (3) is coated with to graphene is arranged into calcining furnace and in protective gas
Under the conditions of it is calcined, the temperature of calcining is 1000-3000 DEG C, and the preparation of graphene non-woven fabrics is completed in non-woven fabrics carbonization.
2. the production technology according to claim 1 that can be mass graphene non-woven fabrics, which is characterized in that step (2)
Specific method be：Crystalline flake graphite is made by graphene oxide using Hummers methods；According to 0.02g graphene oxides be put into
The ratio of the distilled water of 100ml prepares graphene oxide solution；And the graphene oxide solution of preparation is carried out using ultrasonic wave
Ultrasonic disperse；Nonwoven Jing Guo alkali process is arranged into progress ultrasonic wave leaching in the graphene oxide solution by ultrasonic disperse
Stain, pressure rolling are simultaneously dried, until the weight of non-woven fabrics increases 20-30%.
3. the production technology as described in claim 1 that can be mass graphene non-woven fabrics, which is characterized in that step (3)
Specific method is：It selects hydrazine hydrate as reducing agent, adds distilled water to the ratio of 100ml according to the Hydrazine Hydrate Analyzing of 3ml is pure, match
A concentration of 3% hydrazine hydrate solution is made；The nonwoven that fiber obtained by step (2) is coated with to graphene oxide is arranged into water
It closes in hydrazine solution, graphene oxide is restored to graphene by heating in water bath for reaction under the conditions of 90 DEG C；Again by non-woven fabrics spend from
Sub- water is dried after cleaning remaining hydrazine hydrate.
4. the production technology as described in claim 1 that can be mass graphene non-woven fabrics, which is characterized in that the nonwoven
Cloth is viscose glue spunlace non-woven cloth.
5. the production technology as described in claim 1 that can be mass graphene non-woven fabrics, which is characterized in that the oxidation
The preparation of graphene includes the following steps：
(1), graphite pre-oxidizes：It takes 5g crystalline flake graphites, 2g potassium peroxydisulfates and 4g phosphorus pentoxides to be mixed with the concentrated sulfuric acid of 20ml, rises
Temperature fully reacts 5h to 80 DEG C, and deionized water is added later to 200ml, stirs evenly, and supernatant is extracted after the solution layering such as standing
Liquid, the graphite after being pre-oxidized after adding deionized water to be filtered are 12 hours dry in 60 DEG C of vacuum drying ovens.
(2) graphite oxidation：It is placed in container in the obtained pre-oxidation graphite of step (1), under the conditions of 0 DEG C, 1g nitre is added
The concentrated sulfuric acid of sour sodium and 40ml is uniformly mixed, and potassium permanganate is added according still further to the addition speed no more than 1g/4min, uses water
Bathe magnetic agitation 2h；The reaction was continued after being warming up to 45 DEG C again 30min, after drained with glass bar 100ml deionized waters and 8ml be added
A concentration of 30% hydrogen peroxide reacts 10min；The concentrated hydrochloric acid pickling of addition 6% three times, adds excessive deionized water, 9000
Turning under the conditions of 15min centrifuge once, then taking precipitate centrifuges several times under the conditions of 9000 turns of 30min, until in
Property, taking precipitate addition 400ml deionized waters, ultrasonic 30min continues to centrifuge under the conditions of 8000 turns of 15min primary, supernatant
For graphite oxide solution, drying obtains graphite oxide.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN110184859A (en) * | 2019-05-16 | 2019-08-30 | 西安石油大学 | A kind of multi-layer graphene fibrous paper and preparation method thereof |
| CN111501333A (en) * | 2020-05-29 | 2020-08-07 | 诸暨先行机械科技有限公司 | Graphene sterilization cloth and preparation process thereof |
| CN112038114A (en) * | 2020-08-31 | 2020-12-04 | 贵州梅岭电源有限公司 | Preparation method of carbon fiber-based graphene/nano polyaniline composite material |
| CN112522844A (en) * | 2020-11-25 | 2021-03-19 | 佛山市精度纺织有限公司 | Novel cool quick-drying and ultraviolet-resistant knitted fabric and preparation method thereof |
| CN112609469A (en) * | 2020-12-17 | 2021-04-06 | 广东金发科技有限公司 | Graphene melt-blown non-woven fabric and preparation method thereof |
| CN112626709A (en) * | 2019-12-24 | 2021-04-09 | 中科量子(广州)新材料有限公司 | Fiber non-woven fabric and preparation method and application thereof |
| CN112921668A (en) * | 2021-01-07 | 2021-06-08 | 广东金发科技有限公司 | Graphene coated non-woven fabric and preparation method thereof |
| CN113152073A (en) * | 2021-04-25 | 2021-07-23 | 萬豐實業香港有限公司 | Graphene cloth and surface treatment process and application thereof |
| CN113201930A (en) * | 2021-05-18 | 2021-08-03 | 华侨大学 | Graphene non-woven fabric electromagnetic shielding composite material and preparation method thereof |
| CN113249961A (en) * | 2021-04-25 | 2021-08-13 | 北京邮电大学 | Flexible device structure based on conductive fiber network and preparation method and application thereof |
| CN114053034A (en) * | 2021-11-19 | 2022-02-18 | 青岛大学 | Expansion pressurization band-aid/application and preparation method |
| CN114575148A (en) * | 2022-04-29 | 2022-06-03 | 中北大学 | Simplified preparation method of graphene conductive fiber cloth and broadband electromagnetic wave absorption composite material thereof |
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|---|---|---|---|---|
| CN109722881A (en) * | 2018-12-14 | 2019-05-07 | 杭州纳尔森精细化工有限公司 | A kind of medical antistatic new textile |
| CN110184859A (en) * | 2019-05-16 | 2019-08-30 | 西安石油大学 | A kind of multi-layer graphene fibrous paper and preparation method thereof |
| CN110184859B (en) * | 2019-05-16 | 2021-08-27 | 西安石油大学 | Multilayer graphene fiber paper and preparation method thereof |
| CN112626709A (en) * | 2019-12-24 | 2021-04-09 | 中科量子(广州)新材料有限公司 | Fiber non-woven fabric and preparation method and application thereof |
| CN111501333A (en) * | 2020-05-29 | 2020-08-07 | 诸暨先行机械科技有限公司 | Graphene sterilization cloth and preparation process thereof |
| CN112038114A (en) * | 2020-08-31 | 2020-12-04 | 贵州梅岭电源有限公司 | Preparation method of carbon fiber-based graphene/nano polyaniline composite material |
| CN112522844A (en) * | 2020-11-25 | 2021-03-19 | 佛山市精度纺织有限公司 | Novel cool quick-drying and ultraviolet-resistant knitted fabric and preparation method thereof |
| CN112609469A (en) * | 2020-12-17 | 2021-04-06 | 广东金发科技有限公司 | Graphene melt-blown non-woven fabric and preparation method thereof |
| CN112609469B (en) * | 2020-12-17 | 2022-06-07 | 广东金发科技有限公司 | Graphene melt-blown non-woven fabric and preparation method thereof |
| CN112921668A (en) * | 2021-01-07 | 2021-06-08 | 广东金发科技有限公司 | Graphene coated non-woven fabric and preparation method thereof |
| CN113152073A (en) * | 2021-04-25 | 2021-07-23 | 萬豐實業香港有限公司 | Graphene cloth and surface treatment process and application thereof |
| CN113249961A (en) * | 2021-04-25 | 2021-08-13 | 北京邮电大学 | Flexible device structure based on conductive fiber network and preparation method and application thereof |
| CN113201930A (en) * | 2021-05-18 | 2021-08-03 | 华侨大学 | Graphene non-woven fabric electromagnetic shielding composite material and preparation method thereof |
| CN114053034A (en) * | 2021-11-19 | 2022-02-18 | 青岛大学 | Expansion pressurization band-aid/application and preparation method |
| CN114575148A (en) * | 2022-04-29 | 2022-06-03 | 中北大学 | Simplified preparation method of graphene conductive fiber cloth and broadband electromagnetic wave absorption composite material thereof |
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