CN108793127B - Production process capable of producing graphene non-woven fabrics in batches - Google Patents
Production process capable of producing graphene non-woven fabrics in batches Download PDFInfo
- Publication number
- CN108793127B CN108793127B CN201810584625.5A CN201810584625A CN108793127B CN 108793127 B CN108793127 B CN 108793127B CN 201810584625 A CN201810584625 A CN 201810584625A CN 108793127 B CN108793127 B CN 108793127B
- Authority
- CN
- China
- Prior art keywords
- woven fabric
- graphene
- graphene oxide
- graphite
- fiber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
-
- 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
-
- 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
Abstract
The invention discloses a production process capable of producing graphene non-woven fabrics in batches, which comprises the following steps of preparing graphene oxide; coating graphene oxide on the surface of the fiber by adopting an ultrasonic dipping and rolling combined method, and increasing the weight of the dried non-woven fabric by 20-30%; placing the non-woven fabric with the surface of the fiber coated with the graphene oxide into a reducing solution to reduce the graphene oxide into graphene; and placing the non-woven fabric with the surface of the fiber coated with the graphene into a calcining furnace, calcining at the temperature of 1000-3000 ℃ under the condition of protective gas, and carbonizing the non-woven fabric. The invention relates to a production process capable of producing graphene non-woven fabrics in batches, which is characterized in that graphene oxide is coated on the surface of non-woven fabric fibers by adopting an ultrasonic dipping and rolling combined method, and then the graphene oxide non-woven fabrics are prepared by reduction and calcination.
Description
Technical Field
The invention relates to the technical field of graphene non-woven fabric production, in particular to a production process for producing graphene non-woven fabric.
Background
With the rapid development of the economic global society, the prospect of the global functional textile is better and better. New products of the new technology are continuously updated, and the market prospect is bright. In recent years, reports about the application of graphene materials to novel textile fibers and functional textiles are frequent at home and abroad. At present, functional non-woven fabric products are generally obtained by three methods, namely direct spinning of functional fiber raw materials, compounding of common non-woven fabrics and functional non-woven fabric structures and functional after-finishing of common non-woven fabrics. The functional after-finishing is the most convenient and rapid method for preparing the functional non-woven fabric at present, but the functionality of the functional non-woven fabric prepared by the method is weakened or even lost along with the increase of the use times, and the method is only suitable for disposable non-woven fabric products.
Graphene (Graphene) as a future revolutionary material has excellent optical, electrical and mechanical properties. The optical and electrical properties of the graphene are that the carbon atoms in the graphene are bonded by sp2 hybridized orbitals, the carbon atoms have 4 valence electrons, 3 to three electrons each provide one unbonded electron to a pz orbit, and the pz orbit close to the atom forms a pi bond in an unfilled state when forming a vertical direction with a plane, and the pi electron can freely move in the crystal and has good electrical properties; and the coordination number of carbon atoms in graphene is 3, wherein besides a honeycomb-type layered structure in which sigma bonds are linked with other carbon atoms to form hexagonal rings, pz orbitals of each carbon atom perpendicular to the plane of the layer can form large pi bonds of multiple atoms throughout the entire layer, similar to a benzene ring structure, and thus have excellent optical properties.
Graphene oxide (Graphene oxide) is an oxide of Graphene, has a brown-yellow color, is a product of graphite powder after chemical oxidation and exfoliation, and has a particularly good extensibility due to its single atomic layer structure. After the oxidation treatment, the layered structure of the graphite is maintained, and a plurality of groups are introduced into graphene sheets of each layer. These groups allow the presence thereof in an extremely stable state in water or a polar solution.
The research at present finds that the graphene oxide has double-affinity and shows a property distribution from hydrophilic to hydrophobic from the edge part to the central part of the graphene sheet. Thus, graphene oxide may be present at the interface as a surfactant and reduce the energy between the interfaces. Also, the graphene oxide sheets are thicker than graphene sheets, about 1nm, due to the presence of these groups. The groups can react with the groups on the surface of the viscose non-woven fabric, so that the graphene oxide can be more firmly combined with the non-woven fabric.
The Beijing clothing college material science is used for Zhang Mei of engineering college and the like to better realize the macroscopic application of the graphene fiber in the field of functional textiles, the graphite oxide solution with certain concentration is used as spinning solution, the calcium chloride solution is used as coagulating bath, the graphite oxide fiber is prepared by wet spinning, and the graphene fiber is obtained by the reduction of hydroiodic acid. Respectively representing the oxidation degree and the structural morphology of the graphene oxide spinning solution by adopting an X-ray photoelectron spectrum and a transmission electron microscope, and finding that the oxidation degree of the graphene oxide is high, and the carbon-oxygen ratio of the graphene oxide is about 1: 1, and shows the wrinkle appearance of a light and thin sheet layer. The influence of calcium chloride coagulating baths with different mass fractions on the tensile strength of the graphene fiber is researched, and the result shows that when the mass fraction of calcium chloride is 20%, the conductivity of the prepared graphene fiber is 180S/cm, the tensile strength is 892MPa, and the graphene fiber shows good conductivity and mechanical flexibility.
Functional graphene cellulose composite fibers are researched by the Yangtze university of Qingdao, textile and clothing college, and the mechanical property, the ultraviolet resistance, the antistatic property, the flame retardant property and the like of the functional graphene cellulose composite fibers are tested. Researches how to modify the polyamide fiber with graphene to prepare the graphene functional textile. Finally, the application and development of the functional graphene composite fiber and the textile are expected.
However, the conventional production method of the non-woven fabric made of pure graphene generally uses a method of preparing graphene into a solution and using electrostatic spinning to prepare the graphene non-woven fabric. The method of preparing graphene using the electrostatic spinning method is not suitable for mass production of graphene non-woven fabrics.
Disclosure of Invention
The invention aims to provide a production process capable of producing graphene non-woven fabrics in batches, which is characterized in that graphene is coated on the surface of a fiber and then calcined, so that the graphene non-woven fabrics can be produced in batches.
In order to solve the technical problem, the invention aims to realize that:
the invention relates to a production process capable of producing graphene non-woven fabrics in batches, which comprises the following steps:
(1) oxidizing the flake graphite to prepare graphene oxide;
(2) coating graphene oxide on the surface of the non-woven fabric fiber by adopting an ultrasonic dipping and rolling combined method, and drying to increase the weight of the dried non-woven fabric by 20-30%;
(3) placing the non-woven fabric with the surface of the fiber coated with the graphene oxide prepared in the step (2) into a reducing solution, and reducing the graphene oxide into graphene through a reduction reaction;
(4) and (3) placing the non-woven fabric with the surface of the fiber coated with the graphene prepared in the step (3) into a calcining furnace and calcining the non-woven fabric under the condition of protective gas, wherein the calcining temperature is 1000-3000 ℃, and the non-woven fabric is carbonized to finish the preparation of the graphene non-woven fabric.
As a further explanation of the above scheme, the specific method of step (2) is: preparing the crystalline flake graphite into graphene oxide by using a Hummers method; preparing a graphene oxide solution according to the proportion of 0.02g of graphene oxide in 100ml of distilled water; carrying out ultrasonic dispersion on the prepared graphene oxide solution by adopting ultrasonic waves; and (3) placing the non-woven fabric subjected to alkali treatment into the graphene oxide solution subjected to ultrasonic dispersion for ultrasonic dipping, rolling and drying until the weight of the non-woven fabric is increased by 20-30%.
As a further explanation of the above scheme, the specific method of step (3) is: selecting hydrazine hydrate as a reducing agent, and preparing a hydrazine hydrate solution with the concentration of 3 percent according to the proportion that 3ml of hydrazine hydrate is analytically pure and distilled water is added to 100 ml; placing the non-woven fabric coated with graphene oxide by the fiber prepared in the step (2) into a hydrazine hydrate solution, and reducing graphene oxide to graphene by a water bath heating reaction at 90 ℃; and then washing the non-woven fabric with deionized water to remove the residual hydrazine hydrate and drying.
As a further explanation of the above scheme, the nonwoven fabric is a viscose spunlace nonwoven fabric.
As a further illustration of the above scheme, the preparation of the graphene oxide comprises the following steps:
(1) pre-oxidizing graphite: mixing 5g of crystalline flake graphite, 2g of potassium persulfate, 4g of phosphorus pentoxide and 20ml of concentrated sulfuric acid, heating to 80 ℃, fully reacting for 5 hours, adding deionized water to 200ml, uniformly stirring, standing, layering solutions, extracting supernatant, adding deionized water, performing suction filtration to obtain pre-oxidized graphite, and drying in a vacuum oven at 60 ℃ for 12 hours.
(2) And (3) graphite oxidation: putting the pre-oxidized graphite obtained in the step (1) into a container, adding 1g of sodium nitrate and 40ml of concentrated sulfuric acid at the temperature of 0 ℃, uniformly mixing, adding potassium permanganate at the adding speed of not more than 1g/4min, and magnetically stirring for 2 hours by using a water bath; heating to 45 deg.C, reacting for 30min, draining with glass rod, adding 100ml deionized water and 8ml 30% hydrogen peroxide, and reacting for 10 min; adding 6% concentrated hydrochloric acid for pickling for three times, adding excessive deionized water, centrifuging once under 9000-15 min, taking out precipitate, centrifuging for several times under 9000-30 min until the precipitate is neutral, adding 400ml deionized water into the precipitate, performing ultrasonic treatment for 30min, centrifuging once under 8000-15 min, collecting supernatant as graphite oxide solution, and oven drying to obtain graphite oxide.
The invention has the beneficial effects that: according to the production process capable of producing the graphene non-woven fabric in batches, the graphene oxide prepared by the Hummers method is coated on the surface of the non-woven fabric fiber by an ultrasonic dipping and rolling combined method, and is prepared by reduction and calcination. The prepared graphene non-woven fabric has high conductivity and high breaking strength.
Drawings
Fig. 1 is a microscopic view of a graphene nonwoven fabric according to the present invention.
FIG. 2 is a microscopic view of the adhesive nonwoven fabric;
fig. 3 is a graph of photothermal conversion performance of graphene/viscose nonwoven fabric;
fig. 4 is the volume specific resistance of the graphene/viscose non-woven fabric at different bending times.
Detailed Description
The invention is further described with reference to the following figures and specific examples.
Example one
The production process capable of producing the graphene non-woven fabric in batches comprises the following steps:
1. and oxidizing the flake graphite to prepare graphene oxide.
2. Coating graphene oxide on the surface of the non-woven fabric fiber by adopting an ultrasonic dipping and rolling combined method, and drying to increase the weight of the dried non-woven fabric by 20%;
3. placing the non-woven fabric with the surface of the fiber coated with the graphene oxide prepared in the step (2) into a reducing solution, and reducing the graphene oxide into graphene through a reduction reaction;
4. and (4) placing the non-woven fabric with the surface of the fiber coated with the graphene prepared in the step (3) into a calcining furnace, calcining the non-woven fabric in a protective gas condition, wherein the calcining temperature is 1000 ℃, and carbonizing the non-woven fabric to finish the preparation of the graphene non-woven fabric.
In the step 1, the scale graphite is prepared into graphene oxide by using a Hummers method, wherein the graphene oxide comprises graphite preoxidation and graphite oxidation.
The graphene oxide can be prepared by mechanical stripping, redox, epitaxial, silicon carbide, Hermer, and chemical vapor deposition. The graphene is firstly prepared by a mechanical stripping method, the method is simple to operate, the prepared sample is high in quality, but the controllability is poor, the prepared graphene is small in size and has great uncertainty, and meanwhile, the efficiency is low, the cost is high, and the method is not suitable for large-scale production.
Redox method (Hummers method). The redox method is the most widely studied and mature method due to its high yield, but the obtained graphene has low quality. Other methods are difficult to produce in large scale at the present stage, and the chemical oxidation-reduction method is the only practical method at the present stage. The method comprises the steps of treating graphite crystals by using a strong oxidant, and destroying van der Waals force between sheet layers through ultrasonic treatment to uniformly disperse the graphite crystals in water to form the graphene oxide.
The graphite preoxidation is to take 5g of crystalline flake graphite, 2g of potassium persulfate, 4g of phosphorus pentoxide and 20ml of concentrated sulfuric acid to mix, heat the mixture to 80 ℃, fully react for 5 hours, then add deionized water to 200ml, stir the mixture evenly, stand the mixture to layer the solution, extract supernatant, add deionized water to carry out suction filtration, and obtain preoxidized graphite which is dried for 12 hours in a vacuum oven at 60 ℃.
The graphite oxidation is to put the obtained pre-oxidized graphite into a dry container, add 1g of sodium nitrate and 40ml of concentrated sulfuric acid at 0 ℃, mix them evenly, add potassium permanganate at the adding speed of not more than 1g/4min, and stir for 2h by using water bath magnetic force; heating to 45 ℃, continuing to react for 30min, then draining by using a glass rod, adding 100ml of deionized water and 8ml of 30% hydrogen peroxide to react for 10min, and changing the solution from brick red to yellow to obtain a graphene oxide solution; adding 6% concentrated hydrochloric acid for pickling for three times, adding excessive deionized water, centrifuging once under 9000-15 min, taking out precipitate, centrifuging for several times under 9000-30 min until the precipitate is neutral, adding 400ml deionized water into the precipitate, performing ultrasonic treatment for 30min, centrifuging once under 8000-15 min, collecting supernatant as graphite oxide solution, and oven drying to obtain graphite oxide.
In step 2, graphene oxide prepared by the Hummers method is put into a graphene oxide solution in a proportion of 0.02g of graphene oxide to 100ml of distilled water. And ultrasonic dispersion is carried out on the prepared graphene oxide solution by adopting ultrasonic waves, and the graphene oxide prepared by the hummers method is multilayer, so that further processing is needed to obtain single-layer graphene oxide. The main method is to disperse it into a monolayer by using a sonicator. And (3) placing the non-woven fabric subjected to alkali treatment into the graphene oxide solution subjected to ultrasonic dispersion for ultrasonic dipping, rolling and drying until the weight of the non-woven fabric is increased by 20-30%. The ultrasonic impregnation in the present invention means that the graphene oxide solution is ultrasonically dispersed while the nonwoven fabric is impregnated, and the graphene oxide can be more easily dispersed into the nonwoven fabric by using the ultrasonic dispersion.
The performance of graphene viscose composite fibers is studied in detail according to Zhang constitutional et al of Qingdao university. Characterized by the microscopic morphology and internal structure of its fibers; the tensile strength performance, flame retardant performance and ultraviolet resistance of the fiber are further researched. The results show that: compared with common viscose fibers, the graphene viscose composite fibers have more excellent mechanical properties, the flame retardant property and the ultraviolet resistance of the fibers are remarkably improved after the viscose fibers are modified by graphene, the added value of the common viscose fibers is improved by the graphene/viscose composite fibers, and the graphene/viscose composite fibers have wide application prospects. In the step, the non-woven fabric is viscose spunlace non-woven fabric, and the gram weight of the viscose spunlace non-woven fabric is 100-120 g per square meter.
And the base used in this step is sodium hydroxide. So carry out alkali treatment to viscose non-woven fabrics, because in viscose non-woven fabrics production process, the non-woven fabrics surface has some thick liquids, and surface thick liquids can lead to being surrounded by thick liquids on viscose surface and can't react with the surface group of oxidation graphite alkene, lead to the effect of viscose non-woven fabrics flooding oxidation graphite alkene solution not good, can't combine together oxidation graphite alkene and viscose fiber, consequently need go the thick liquid and handle: putting the viscose non-woven fabric into a bath with the bath ratio of 1: heating 50 of sodium hydroxide (NaOH) solution to 80 ℃, boiling for 30min, washing with deionized water and drying. The obtained non-woven fabric can remove not only the sizing agent, but also some dust and impurities on the surface.
When wrapping up graphite oxide alkene to viscose fiber surface, probably can not use the weight increase of viscose non-woven fabrics to reach the requirement through once ultrasonic impregnation, need dry and carry out ultrasonic impregnation again to the viscose non-woven fabrics after the ultrasonic impregnation, or ultrasonic impregnation many times, until the rate of increase of weight of viscose non-woven fabrics reaches the requirement.
And 3, converting the graphene oxide coated on the surfaces of the viscose fibers in the non-woven fabric into graphene through a reduction reaction. Selecting hydrazine hydrate as a reducing agent, and preparing a hydrazine hydrate solution with the concentration of 3% according to the proportion that 3ml of hydrazine hydrate is analytically pure and distilled water is added to 100 ml; placing the non-woven fabric coated with graphene oxide by the fiber prepared in the step (2) into a hydrazine hydrate solution, and reducing graphene oxide to graphene by a water bath heating reaction at 90 ℃; and cleaning the viscose non-woven fabric with deionized water to remove residual hydrazine hydrate, and drying to obtain the reduced graphene/viscose non-woven fabric.
The breaking shrinkage strength of the viscose nonwoven fabric coated with the reduced graphene tends to be smaller than that of the viscose nonwoven fabric, but the reduction amount is not large. Among the reasons for the reduction of the breaking strength, when the nonwoven fabric is subjected to ultrasonic impregnation and reduction with hydrazine hydrate, the viscose fibers are continuously contacted with the solution, the structure of the nonwoven fabric is damaged to a certain extent, and the strength of the fibers is reduced.
The resistance is tested and the volume specific resistance is calculated under the stretching state of the viscose non-woven fabric coated with the graphene, the conductivity of the graphene/viscose non-woven fabric can be known, the conductivity is calculated to be 0.1-0.7 omega m through testing, the surface of viscose fiber in the viscose non-woven fabric is completely coated by the graphene, the volume specific resistance is stabilized to be about 0.1, the more completely the viscose fiber is coated by the graphene, pi electrons on the fiber are increased and the moving space is enlarged, when the coating times reach a certain number, the viscose fiber is basically and completely coated by the graphene, the pi electrons are only increased on the surface of the fiber, and the conductivity is not obviously increased.
The conductivity of the fabric is basically unchanged after being folded and bent for multiple times, and 100, 200, 300, 400 and 500 times are selected in the embodiment. Because graphite alkene itself has better mechanical properties, passes through chemical group with viscose fiber simultaneously and combines, and is comparatively firm, is difficult for dropping because of the bending. The folding bending does not have much influence on the electrical conductivity. The graphene and the viscose are combined more closely, and the practical performance is better.
The photo-thermal performance conversion of graphite alkene/viscose non-woven fabrics than former viscose non-woven fabrics has very big promotion. Under the irradiation of infrared light with the same intensity, the maximum temperature of the viscose non-woven fabric can only reach about 40 ℃, and the maximum temperature of the graphene/viscose non-woven fabric can reach more than 100 ℃. When the graphene/viscose non-woven fabric is irradiated by an external light source, the temperature can be raised to 70-80 ℃ within 5s-10s through measurement, and can be raised to more than 100 ℃ after being irradiated for 60 s.
The ultraviolet resistance performance of the graphene/viscose non-woven fabric is tested, the UPF value of the graphene/viscose non-woven fabric reaches 100+, and both T (UVA) and T (UVB) are less than 5%, according to the determination requirement of ultraviolet-proof products in national standard GB/T18830-2002 evaluation on ultraviolet-proof performance of textiles, when the UPF of a sample is more than 30 and the AV of T (UVA) is less than 5%, the sample is called as the ultraviolet-proof product.
The test structures of the above test items are shown in the following table, in which the test data are the average values of multiple tests
In step 4, the prepared non-woven fabric with the surface coated with the graphene is placed in a calcining furnace and is calcined under the condition that nitrogen is used as protective gas, the calcining temperature is 1000-3000 ℃, and the time is 2 hours, so that the viscose non-woven fabric is carbonized, and the preparation of the graphene non-woven fabric is completed. The viscose non-woven fabric can be completely carbonized to form a hollow graphene non-woven fabric, and the weight of the square meter is 20-30 g.
The calcined graphene non-woven fabric has little change except the change of breaking strength. Since the surface of the fiber is completely coated by graphene, all the tests are determined by the properties of graphene. The viscose nonwoven fabric can affect the breaking strength of the Chinese fiddle stick in the test items. Compared with the preparation of the pure graphene non-woven fabric, the method has the advantage of being capable of realizing batch production of the pure graphene non-woven fabric.
Better self-heating performance and ultraviolet resistance, wider application range of the graphene non-woven fabric, and wider application range in wider fields. Because this kind of graphite alkene non-woven fabrics is that viscose fiber surface cladding graphite alkene makes in viscose water thorn non-woven fabrics, can make it have with viscose water thorn non-woven fabrics similar structure, can regard as filtering material to use.
The starting materials used in the present invention are commercially available. The source of the raw materials is shown in the following table.
Example two
The production process capable of producing the graphene non-woven fabric in batches comprises the following steps:
1. and oxidizing the flake graphite to prepare graphene oxide.
2. Coating graphene oxide on the surface of the non-woven fabric fiber by adopting an ultrasonic dipping and rolling combined method, and drying to increase the weight of the dried non-woven fabric by 30%;
3. placing the non-woven fabric with the surface of the fiber coated with the graphene oxide prepared in the step (2) into a reducing solution, and reducing the graphene oxide into graphene through a reduction reaction;
4. and (4) placing the non-woven fabric with the surface of the fiber coated with the graphene prepared in the step (3) into a calcining furnace, calcining the non-woven fabric in a protective gas condition, wherein the calcining temperature is 3000 ℃, and carbonizing the non-woven fabric to finish the preparation of the graphene non-woven fabric.
In this example, the difference from the first example is that the reduction reaction in step 2 is carried out using hydriodic acid vapor, and the hydriodic acid solution concentration of the hydriodic acid vapor used is 40 to 60% by weight. And (3) drying the non-woven fabric with the surface coated with the graphene oxide on the fiber surface prepared by the hydriodic acid steam reduction at room temperature.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (2)
1. A production process capable of producing graphene non-woven fabrics in batches is characterized by comprising the following steps:
(1) oxidizing the flake graphite to prepare graphene oxide;
(2) coating graphene oxide on the surface of the non-woven fabric fiber by adopting an ultrasonic dipping and rolling combined method, and drying to increase the weight of the dried non-woven fabric by 20-30%;
(3) placing the non-woven fabric with the surface of the fiber coated with the graphene oxide prepared in the step (2) into a reducing solution, and reducing the graphene oxide into graphene through a reduction reaction;
(4) placing the non-woven fabric with the surface of the fiber coated with the graphene prepared in the step (3) into a calcining furnace and calcining the non-woven fabric under the condition of protective gas, wherein the calcining temperature is 1000-3000 ℃, and carbonizing the non-woven fabric to finish the preparation of the graphene non-woven fabric;
the specific method comprises the following steps: preparing the crystalline flake graphite into graphene oxide by using a Hummers method; preparing a graphene oxide solution according to the proportion of 0.02g of graphene oxide in 100ml of distilled water; carrying out ultrasonic dispersion on the prepared graphene oxide solution by adopting ultrasonic waves; placing the non-woven fabric subjected to alkali treatment into the graphene oxide solution subjected to ultrasonic dispersion for ultrasonic dipping, rolling and drying until the weight of the non-woven fabric is increased by 20-30%;
the non-woven fabric is viscose spunlace non-woven fabric; putting the viscose spunlace non-woven fabric into a bath with the bath ratio of 1: heating 50 parts of sodium hydroxide solution to 80 ℃, boiling for 30min, washing with deionized water and drying;
the specific method of the step (3) is as follows: selecting hydrazine hydrate as a reducing agent, and preparing a hydrazine hydrate solution with the concentration of 3 percent according to the proportion that 3ml of hydrazine hydrate is analytically pure and distilled water is added to 100 ml; placing the non-woven fabric coated with graphene oxide by the fiber prepared in the step (2) into a hydrazine hydrate solution, and reducing graphene oxide to graphene by a water bath heating reaction at 90 ℃; and then washing the non-woven fabric with deionized water to remove the residual hydrazine hydrate and drying.
2. The process for producing graphene non-woven fabric according to claim 1, wherein the graphene oxide is prepared by the following steps:
(1) pre-oxidizing graphite: mixing 5g of crystalline flake graphite, 2g of potassium persulfate, 4g of phosphorus pentoxide and 20ml of concentrated sulfuric acid, heating to 80 ℃, fully reacting for 5 hours, adding deionized water to 200ml, uniformly stirring, standing, layering solutions, extracting supernatant, adding deionized water, performing suction filtration to obtain pre-oxidized graphite, and drying in a vacuum oven at 60 ℃ for 12 hours;
(2) and graphite oxidation: putting the pre-oxidized graphite obtained in the step (1) into a container, adding 1g of sodium nitrate and 40ml of concentrated sulfuric acid at the temperature of 0 ℃, uniformly mixing, adding potassium permanganate at the adding speed of not more than 1g/4min, and magnetically stirring for 2 hours by using a water bath; heating to 45 deg.C, reacting for 30min, draining with glass rod, adding 100ml deionized water and 8ml 30% hydrogen peroxide, and reacting for 10 min; adding 6% concentrated hydrochloric acid for pickling for three times, adding excessive deionized water, centrifuging once under 9000-15 min, taking out precipitate, centrifuging for several times under 9000-30 min until the precipitate is neutral, adding 400ml deionized water into the precipitate, performing ultrasonic treatment for 30min, centrifuging once under 8000-15 min, collecting supernatant as graphite oxide solution, and oven drying to obtain graphite oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810584625.5A CN108793127B (en) | 2018-06-08 | 2018-06-08 | Production process capable of producing graphene non-woven fabrics in batches |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810584625.5A CN108793127B (en) | 2018-06-08 | 2018-06-08 | Production process capable of producing graphene non-woven fabrics in batches |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108793127A CN108793127A (en) | 2018-11-13 |
| CN108793127B true CN108793127B (en) | 2022-02-01 |
Family
ID=64088873
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810584625.5A Active CN108793127B (en) | 2018-06-08 | 2018-06-08 | Production process capable of producing graphene non-woven fabrics in batches |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108793127B (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110184859B (en) * | 2019-05-16 | 2021-08-27 | 西安石油大学 | Multilayer graphene fiber paper and preparation method thereof |
| CN112626709B (en) * | 2019-12-24 | 2022-11-01 | 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 |
| CN112038114B (en) * | 2020-08-31 | 2022-03-29 | 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 |
| 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 |
| CN112921668B (en) * | 2021-01-07 | 2023-01-24 | 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 |
| CN113249961B (en) * | 2021-04-25 | 2023-04-07 | 北京邮电大学 | Flexible device structure based on conductive fiber network and preparation method and application thereof |
| CN113201930B (en) * | 2021-05-18 | 2023-03-24 | 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 |
| CN114575148B (en) * | 2022-04-29 | 2022-09-20 | 中北大学 | Simplified preparation method of graphene conductive fiber cloth and broadband electromagnetic wave absorption composite material thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102785437A (en) * | 2012-07-19 | 2012-11-21 | 中国航空工业集团公司北京航空材料研究院 | Composite conductive film, its preparation method and its application |
| CN105256465A (en) * | 2015-11-19 | 2016-01-20 | 武汉市知富企业管理咨询有限公司 | Preparation method for nanometer non-woven fabric based on graphene oxide-silicon carbide modification |
| CN105829593A (en) * | 2013-12-27 | 2016-08-03 | 东丽株式会社 | Carbon fiber nonwoven fabric, production method for carbon fiber nonwoven fabric, and nonwoven fabric of carbon fiber precurser fibers |
| CN106671525A (en) * | 2016-12-27 | 2017-05-17 | 中国航空工业集团公司北京航空材料研究院 | Hybrid modified composite material with high-conductivity and high-toughness structure and preparation method of hybrid modified composite material |
| KR20170088813A (en) * | 2017-07-25 | 2017-08-02 | 주식회사 지에이치엘 | Functional molded product using graphene hybrid material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI588089B (en) * | 2015-10-20 | 2017-06-21 | Acelon Chem & Fiber Corp | Method of preparing of graphene-natural cellulose blended meltblown nonwoven fabric |
-
2018
- 2018-06-08 CN CN201810584625.5A patent/CN108793127B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102785437A (en) * | 2012-07-19 | 2012-11-21 | 中国航空工业集团公司北京航空材料研究院 | Composite conductive film, its preparation method and its application |
| CN105829593A (en) * | 2013-12-27 | 2016-08-03 | 东丽株式会社 | Carbon fiber nonwoven fabric, production method for carbon fiber nonwoven fabric, and nonwoven fabric of carbon fiber precurser fibers |
| CN105256465A (en) * | 2015-11-19 | 2016-01-20 | 武汉市知富企业管理咨询有限公司 | Preparation method for nanometer non-woven fabric based on graphene oxide-silicon carbide modification |
| CN106671525A (en) * | 2016-12-27 | 2017-05-17 | 中国航空工业集团公司北京航空材料研究院 | Hybrid modified composite material with high-conductivity and high-toughness structure and preparation method of hybrid modified composite material |
| KR20170088813A (en) * | 2017-07-25 | 2017-08-02 | 주식회사 지에이치엘 | Functional molded product using graphene hybrid material |
Non-Patent Citations (2)
| Title |
|---|
| "超细碳纤维毡的制备及其形貌研究";张玉军 等;《化学与黏合》;20091231;第31卷(第1期);第25-27页 * |
| "还原自组装石墨烯粘胶织物的制备";杨绍钦 等;《印染》;20161231(第23期);第23-26页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108793127A (en) | 2018-11-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108793127B (en) | Production process capable of producing graphene non-woven fabrics in batches | |
| CN106255238B (en) | A kind of graphene thermo electric material and its application | |
| Liu et al. | Fabricating conductive poly (ethylene terephthalate) nonwoven fabrics using an aqueous dispersion of reduced graphene oxide as a sheet dyestuff | |
| CN109183396A (en) | A method of graphene is promoted in dacron area load amount | |
| CN103588195A (en) | Preparation method of graphene | |
| CN106149359A (en) | A kind of fire-retardant uvioresistant curtain and preparation method thereof | |
| CN103625085B (en) | The preparation method of large-area graphene/polymer fiber three-dimensional network composite foam film | |
| CN104370285A (en) | Method for macroscopically preparing high-quality graphene by using bio-mineralized material | |
| CN107523988B (en) | W18O49Coated carbon fiber composite material and preparation method thereof | |
| CN105420689B (en) | A kind of aligned carbon nanotube-aluminum oxide hybridization fiber and preparation method thereof | |
| Hasan et al. | Functionalization of polypropylene nonwoven fabrics using cold plasma (O2) for developing graphene-based wearable sensors | |
| CN108486752B (en) | Preparation method of nano knitted woolen fabric with self-cleaning function | |
| CN105728005A (en) | Preparation method of carbon-doped indium oxide with complex serving as precursor | |
| CN103693681A (en) | Method for preparing super-long titanate micro/nanotubes | |
| CN106702732A (en) | Graphene-copper composite fiber and preparation method thereof | |
| CN110364371B (en) | Active porous carbon framework/graphene composite fiber and preparation method thereof | |
| CN115341390A (en) | Preparation method and application of titanium carbide MXene fiber nanocomposite | |
| CN108774881A (en) | A kind of RGO/Ag+Assemble the production technology of cellulose conductive yam | |
| CN105752970A (en) | Method for preparing carbon nanotube/graphene compound | |
| CN104071783A (en) | Method for preparing flexible papyraceous reduced graphene oxide film | |
| Chen et al. | Two-step thermal treatment of electrochemical graphene oxide films for high-performance electrical heating and electromagnetic interference shielding | |
| Ma et al. | Formation of C-doped SiO2 coatings on carbon fibers by the sol-dipping process | |
| CN107082416B (en) | A method of graphene is prepared based on ozone oxidation | |
| CN106637937B (en) | A kind of graphene-cobalt composite fibre and preparation method thereof | |
| CN107190361A (en) | A kind of tungsten selenide/graphene/carbon nano-fiber composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |