CN109098038A - A kind of electromagnetic shielding paper and preparation method thereof - Google Patents

A kind of electromagnetic shielding paper and preparation method thereof Download PDF

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Publication number
CN109098038A
CN109098038A CN201811019861.9A CN201811019861A CN109098038A CN 109098038 A CN109098038 A CN 109098038A CN 201811019861 A CN201811019861 A CN 201811019861A CN 109098038 A CN109098038 A CN 109098038A
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preparation
mxene
electromagnetic shielding
electromagnetically shielded
phase
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甘坚梅
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Foshan Bean Technology Co Ltd
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Foshan Bean Technology Co Ltd
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00Special paper not otherwise provided for, e.g. made by multi-step processes
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H15/00Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution
    • D21H15/02Pulp or paper, comprising fibres or web-forming material characterised by features other than their chemical constitution characterised by configuration
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21JFIBREBOARD; MANUFACTURE OF ARTICLES FROM CELLULOSIC FIBROUS SUSPENSIONS OR FROM PAPIER-MACHE
    • D21J5/00Manufacture of hollow articles by transferring sheets, produced from fibres suspensions or papier-mâché by suction on wire-net moulds, to couch-moulds
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073Shielding materials
    • H05K9/0081Electromagnetic shielding materials, e.g. EMI, RFI shielding

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Paper (AREA)

Abstract

The present invention relates to a kind of electromagnetic shielding paper and preparation method thereof, the electromagnetic shielding paper is made of the modified MXene in the surface of the lignocellulosic nanofiber of mass fraction 20%-60% and mass fraction 40%-80%, the modified MXene in the surface includes MXene carrier and load layer, load layer includes zinc oxide phase, carbon phase and titanium dioxide phase, the electromagnetic shielding paper mix in proportion by the modified MXene in lignocellulosic nanofiber and surface, filtered, roll-in, obtained after drying, and electromagnetic shielding paper obtained is with good mechanical performance and electromagnetic shielding performance.

Description

A kind of electromagnetic shielding paper and preparation method thereof
Technical field
The present invention relates to speciality paper fields more particularly to a kind of electromagnetic shielding paper and preparation method thereof.
Background technique
Electromagnetic radiation is called electronic smoke, is the phenomenon that energy is emitted to space with electromagnetic wave, electronics and information industry Fast development, be greatly promoted the universal of wireless telecom equipment and high-frequency electron device, also result in the electricity got worse Magnetic disturbance and electromagnetic pollution not only interfere the normal work of electronic component, and potential health danger can be also caused to human body Evil, electromagenetic wave radiation are listed in the fourth-largest pollution sources after water source, atmosphere, noise, long-term excessive electromagnetic radiation meeting pair Human body reproduction, nerve and immune system etc. damage.
Electromagnetic shielding paper can absorb the electromagnetic wave issued with reflective electron equipment to a certain extent, thus electromagnetism of decaying Radiation energy reduces transmitance, reaches shielding purpose.Existing electromagnetic shielding paper is mostly reached with adding traditional suction wave substance Absorb the effect with shielding electromagnetic wave, such as carbon-based material, the silicon carbide of dielectric loss type, the ferrite of magnetic loss type or ultra-fine Metal, patent CN101994275A disclose a kind of complex phase electromagnetic shielding paper, using the waste paper pulp fiber of non-deinking as matrix, dispersion There are carbon fiber and carbon black, but its electromagnet shield effect, mechanical strength and heat resistance are poor;Patent CN103114503A discloses one Kind nickel-coated carbon fibers shielding paper, not only technique is excessively complicated, and the coat of metal is also easy to crack;Patent CN107630386A discloses one Electromagnetic shielding paper of the kind containing carbon nanotube, carbon nanotube has excellent mechanics and Electromagnetism Characteristics, available to have both machine The electromagnetic shielding paper of tool performance and shield effectiveness, but carbon nanotube assembles reunion easily in the form of pencil or entanglement shape, and hardly It is molten, it is difficult to preferably to disperse in a solvent.
Summary of the invention
The present invention is intended to provide a kind of electromagnetic shielding paper and preparation method thereof, set forth above to solve the problems, such as.
A kind of electromagnetic shielding paper and preparation method thereof is provided in the embodiment of the present invention, the electromagnetic shielding paper is by quality point The lignocellulosic nanofiber of number 20%-60% and the modified MXene in the surface of mass fraction 40%-80% are constituted, the table The modified MXene in face includes MXene carrier and load layer, and load layer includes zinc oxide phase, carbon phase and titanium dioxide phase;The electromagnetic screen The preparation method for covering paper includes that the preparation of lignocellulosic nanofiber, the preparation of the modified MXene in surface, mixed slurry filter Molding;
Preferably, the electromagnetic shielding paper by mass fraction 40% lignocellulosic nanofiber and mass fraction 60% The modified MXene in surface is constituted;
Preferably, the pretreatment is that raw material wood powder uses petroleum ether, glacial acetic acid and sodium chlorite, sodium hydroxide molten respectively Liquid, hydrochloric acid solution processing;
Preferably, the broken homogenization is Ultrasonic Pulverization processing and high-pressure homogeneous processing;
Preferably, the MXene carrier is that titanium aluminum carbide etches to obtain through the concentrated hydrochloric acid solution dissolved with lithium fluoride;
It is further preferred that fluorination lithium concentration is 0.05g/ml;
Preferably, the zinc oxide is mutually by MXene carrier through zinc ion load, hydrazine hydrate reduction, carbon dioxide high temperature oxygen Change obtains;The carbon phase and titanium dioxide are mutually obtained by MXene carrier through carbon dioxide high-temperature oxydation;
It is further preferred that the process temperature of the carbon dioxide high-temperature oxydation is 850 DEG C, soaking time 60min, dioxy Change carbon flow 150ml/min.
The technical solution that the embodiment of the present invention provides can include the following benefits:
By providing bigger surface and interface to MXene surface microstructure Modification design, stacking and dimensional effect are reduced Caused by contact resistance, enhance electric conductivity, increase electromagnetic wave propagation path, promote its decaying, improve material impedance matching, Effective absorption band is widened, electromagnetic wave absorption performance is improved, a kind of electromagnetic shielding paper provided by the invention is received by lignocellulosic The mixed slurry of rice fiber and the modified MXene in surface filter molding and are made, and have both excellent toughness, tensile resistance and shielding effect Can, and prepare raw material and be easy to get, the machinability of preparation process is strong.
The additional aspect of the present invention and advantage will be set forth in part in the description, and will partially become from the following description Obviously, or practice through the invention is recognized.It should be understood that above general description and following detailed description are only Be it is exemplary and explanatory, the present invention can not be limited.
Specific embodiment
Example embodiments are described in detail here.Embodiment described in following exemplary embodiment Do not represent all embodiments consistented with the present invention.On the contrary, they be only with as being described in detail in the appended claims , the examples of the device and method that some aspects of the invention are consistent.
Electromagnetic shielding material can absorb the electromagnetic wave issued with reflective electron equipment to a certain extent, be developed A variety of electromagnetic shielding materials are to eliminate electromagnetic pollution, and traditional electromagnetic shielding material uses the metals such as copper, aluminium to manufacture more, high density It is limited in the application of the multiple fields such as movable equipment, wearable electronic product and physical protection, Qi Taru with large volume Nickel cobalt metallic fiber is overlying on to paraffin based composites, the carbonization silicon sponge, graphene-dimethyl silicone polymer of biological Carbon fibe Composite sponge, it is big that there are density, using the wide disadvantage of thickness, therefore, develops light, high tenacity and the strong electromagnetic screen of machinability Covering material and product will be with important research significance and practical application value.
MXene is a kind of two-dimentional new material with class graphene-structured, special metalloid characteristic and stratiform knot Structure makes it have potential application in electromagnetic shielding field, but its absorbing property is unsatisfactory, this is with material with the phase interaction of electromagnetic wave Related with mechanism and impedance matching capability, exploitation lightweight, broad absorption band be wide, high-absorbility MXene class material, need to its into Row microstructure design surface is modified to promote Absorbing Materials.
The embodiment of the present invention is related to a kind of electromagnetic shielding paper and preparation method thereof, and the electromagnetic shielding paper is by mass fraction The lignocellulosic nanofiber of 20%-60% and the modified MXene in the surface of mass fraction 40%-80% are constituted, the surface Modified MXene includes MXene carrier and load layer, and load layer includes zinc oxide phase, carbon phase and titanium dioxide phase;The electromagnetic shielding The preparation method of paper includes, the preparation of lignocellulosic nanofiber, the preparation of the modified MXene in surface, mixed slurry filter at Type;
Preferably, the electromagnetic shielding paper by mass fraction 40% lignocellulosic nanofiber and mass fraction 60% The modified MXene in surface is constituted;
Preferably, the pretreatment is that raw material wood powder uses petroleum ether, glacial acetic acid and sodium chlorite, sodium hydroxide molten respectively Liquid, hydrochloric acid solution processing;
Preferably, the broken homogenization is Ultrasonic Pulverization processing and high-pressure homogeneous processing;
Preferably, the MXene carrier is that titanium aluminum carbide etches to obtain through the concentrated hydrochloric acid solution dissolved with lithium fluoride;
It is further preferred that fluorination lithium concentration is 0.05g/ml;
Preferably, the zinc oxide is mutually by MXene carrier through zinc ion load, hydrazine hydrate reduction, carbon dioxide high temperature oxygen Change obtains;The carbon phase and titanium dioxide are mutually obtained by MXene carrier through carbon dioxide high-temperature oxydation;
As oxidant and oxidizing condition is controlled using carbon dioxide, part oxygen while keeping the lamellar structure of MXene carrier Change, in its Surface Creation carbon phase and titanium dioxide phase, improves conductivity and impedance matching, intrinsic defect increases dipole polarization;It carves Obtained MXene carrier surface is lost with electron rich group, is easily combined, is reduced in the form of electrostatic or complexing with zinc metal ion Radical position, enhancing is conductive, then is reduced to Metal Supported in MXene carrier surface, and zinc oxide is that a kind of direct band gap is wide Bandgap semiconductor has low dielectric constant, can form the heterogeneous of multiple class fish scales with titanium dioxide phase, carbon phase, MXene carrier Interface shows high dielectric loss, hinders the effective mobility of electronics in the structure, under the action of electromagnetic wave, material surface The a large amount of charges inspired are assembled at the hetero-junctions of interface, form space charge doping region, form scattering effect to electron transfer, Dielectric dipolar interaction and relevant relaxation effect are generated, dissipative electromagnetic wave, performance is better than single-phase MXene carrier or respectively Ingredient is simply mixed;
It is further preferred that the process temperature of the carbon dioxide high-temperature oxydation is 850 DEG C, soaking time 60min, dioxy Change carbon flow 150ml/min.
Enumerate embodiment further below with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this Invention is further described, and should not be understood as limiting the scope of the invention, those skilled in the art is according to this hair Some nonessential modifications and adaptations that bright above content is made all belong to the scope of protection of the present invention.Following examples are specific Technological parameter etc. is also only an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper In the range of select, and do not really want to be defined in hereafter exemplary specific value.
Embodiment 1
In the present embodiment, a kind of electromagnetic shielding paper, by the lignocellulosic nanofiber and quality point of mass fraction 20% The modified MXene in the surface of number 80% is constituted, and the modified MXene in the surface includes MXene carrier and load layer, and load layer includes oxygen Change zinc phase, carbon phase and titanium dioxide phase;The preparation method of the electromagnetic shielding paper includes, the preparation of lignocellulosic nanofiber, The preparation of the modified MXene in surface, mixed slurry filter molding, specifically includes the following steps:
(1) prepared by lignocellulosic nanofiber
A, it pre-processes
It weighing 60 mesh wood powder 5g, 60-90 DEG C of boiling range of petroleum ether 400ml is added, 80 DEG C of reflux 6h are filtered out, ethanol washing, Deionized water 300ml, glacial acetic acid 7ml, sodium chlorite 10g, 80 DEG C of temperature constant magnetic stirring 3h is added from volatile dry in room temperature, takes out Filter cake is filtered and be washed with distilled water, 3wt% sodium hydroxide solution 300ml, 80 DEG C of temperature constant magnetic stirring 2h are added in filter cake, filter And be washed with distilled water filter cake, in filter cake be added 1wt% hydrochloric acid solution 200ml, 80 DEG C of temperature constant magnetic stirring 2h, filter and with steaming Distilled water washs filter cake;
B, it is crushed homogenization
Filter cake is formulated as the suspension of 2wt%, and 600W Ultrasonic Pulverization 2h enters high pressure homogenizer and recycles homogeneous 3 times, homogeneous pressure Strong 1000bar obtains lignocellulosic nanofiber solution;
(2) the modified MXene preparation in surface
A, MAX phase is etched
Lithium fluoride 1g is added in through the cooling polytetrafluoroethylcontainer container of ice water, is slowly added to the hydrochloric acid of 20ml 10mol/L Solution stirs 30min, weighs the titanium aluminum carbide powder 1g of 500 mesh, controls temperature at 50 DEG C hereinafter, being slowly added to several times In above-mentioned solution, 35 DEG C of heat preservation 72h after addition, every 6h shake is primary, after reaction, repeated centrifugation, washing to washing Liquid is in neutrality, drying precipitated;
B, Zn is loaded
A step precipitating 2g obtained, ultrasonication in (2) are added in 100ml deionized water and handles 2min, ultrasonic power 270W, ultrasonic time: then 0.86g anhydrous zinc chloride, 0.36g cetyl trimethyl bromination is added in dwell time 1s:2s Ammonium, stirring and dissolving, ammonium hydroxide adjust pH value of solution to 10, stir 30min, obtain suspending liquid A, hexadecane is added in 50ml deionized water Base trimethylammonium bromide 0.18g, hydrazine hydrate 5g obtain solution B, solution B are slowly added into suspending liquid A, stir 2h, alternately It is repeatedly washed with dehydrated alcohol and distilled water, 50 DEG C of drying;
c、CO2High-temperature oxydation
Sample obtained by b step in (2) of 0.2g is weighed, under argon atmosphere, 600 DEG C is warming up to, keeps the temperature 45min, Temperature rises to 750 DEG C, keeps the temperature 15min, and atmosphere is switched to carbon dioxide gas, and gas flow 150ml/min keeps the temperature 60min, Atmosphere is switched to argon gas, after being cooled to room temperature certainly, obtains oxidation product;
(3) molding is filtered
It is received by lignocellulosic nanofiber with the mass ratio of the modified MXene in surface for 20:80 mixing lignocellulosic Rice fiber solution and the modified MXene in surface, stir 12h, filter, roll-in, and electromagnetic shielding paper is made in drying.
Embodiment 2
In the present embodiment, a kind of electromagnetic shielding paper, by the lignocellulosic nanofiber and quality of mass fraction 40% The modified MXene in the surface of score 60% is constituted, and the modified MXene in the surface includes MXene carrier and load layer, and load layer includes Zinc oxide phase, carbon phase and titanium dioxide phase;The preparation method of the electromagnetic shielding paper includes the system of lignocellulosic nanofiber Standby, the modified MXene in surface preparation, mixed slurry filter molding, specifically includes the following steps:
(1) prepared by lignocellulosic nanofiber
A, it pre-processes
It weighing 60 mesh wood powder 5g, 60-90 DEG C of boiling range of petroleum ether 400ml is added, 80 DEG C of reflux 6h are filtered out, ethanol washing, Deionized water 300ml, glacial acetic acid 7ml, sodium chlorite 10g, 80 DEG C of temperature constant magnetic stirring 3h is added from volatile dry in room temperature, takes out Filter cake is filtered and be washed with distilled water, 3wt% sodium hydroxide solution 300ml, 80 DEG C of temperature constant magnetic stirring 2h are added in filter cake, filter And be washed with distilled water filter cake, in filter cake be added 1wt% hydrochloric acid solution 200ml, 80 DEG C of temperature constant magnetic stirring 2h, filter and with steaming Distilled water washs filter cake;
B, it is crushed homogenization
Filter cake is formulated as the suspension of 2wt%, and 600W Ultrasonic Pulverization 2h enters high pressure homogenizer and recycles homogeneous 3 times, homogeneous pressure Strong 1000bar obtains lignocellulosic nanofiber solution;
(2) the modified MXene preparation in surface
A, MAX phase is etched
Lithium fluoride 1g is added in through the cooling polytetrafluoroethylcontainer container of ice water, is slowly added to the hydrochloric acid of 20ml 10mol/L Solution stirs 30min, weighs the titanium aluminum carbide powder 1g of 500 mesh, controls temperature at 50 DEG C hereinafter, being slowly added to several times In above-mentioned solution, 35 DEG C of heat preservation 72h after addition, every 6h shake is primary, after reaction, repeated centrifugation, washing to washing Liquid is in neutrality, drying precipitated;
B, Zn is loaded
The precipitating 2g of a step is added in 100ml deionized water, ultrasonication handles 2min, ultrasonic power 270W, ultrasound Time: then 0.86g anhydrous zinc chloride is added in dwell time 1s:2s, 0.36g cetyl trimethylammonium bromide stirs molten Solution, ammonium hydroxide adjust pH value of solution to 10, stir 30min, obtain suspending liquid A, cetyl trimethyl is added in 50ml deionized water Ammonium bromide 0.18g, hydrazine hydrate 5g, obtains solution B, and solution B is slowly added into suspending liquid A, stirs 2h, alternately anhydrous second Pure and mild distilled water is repeatedly washed, 50 DEG C of drying;
c、CO2High-temperature oxydation
Sample obtained by 0.2g b step is weighed, under argon atmosphere, 600 DEG C is warming up to, keeps the temperature 45min, temperature liter To 750 DEG C, 15min is kept the temperature, atmosphere is switched to carbon dioxide gas, and gas flow 150ml/min keeps the temperature 60min, and atmosphere is cut It is changed to argon gas, after being cooled to room temperature certainly, obtains oxidation product;
(3) molding is filtered
It is received by lignocellulosic nanofiber with the mass ratio of the modified MXene in surface for 40:60 mixing lignocellulosic Rice fiber solution and the modified MXene in surface, stir 12h, filter, roll-in, and electromagnetic shielding paper is made in drying.
Embodiment 3
In the present embodiment, a kind of electromagnetic shielding paper, by the lignocellulosic nanofiber and quality of mass fraction 60% The modified MXene in the surface of score 40% is constituted, and the modified MXene in the surface includes MXene carrier and load layer, and load layer includes Zinc oxide phase, carbon phase and titanium dioxide phase;The preparation method of the electromagnetic shielding paper includes the system of lignocellulosic nanofiber Standby, the modified MXene in surface preparation, mixed slurry filter molding, specifically includes the following steps:
(1) prepared by lignocellulosic nanofiber
A, it pre-processes
It weighing 60 mesh wood powder 5g, 60-90 DEG C of boiling range of petroleum ether 400ml is added, 80 DEG C of reflux 6h are filtered out, ethanol washing, Deionized water 300ml, glacial acetic acid 7ml, sodium chlorite 10g, 80 DEG C of temperature constant magnetic stirring 3h is added from volatile dry in room temperature, takes out Filter cake is filtered and be washed with distilled water, 3wt% sodium hydroxide solution 300ml, 80 DEG C of temperature constant magnetic stirring 2h are added in filter cake, filter And be washed with distilled water filter cake, in filter cake be added 1wt% hydrochloric acid solution 200ml, 80 DEG C of temperature constant magnetic stirring 2h, filter and with steaming Distilled water washs filter cake;
B, it is crushed homogenization
Filter cake is formulated as the suspension of 2wt%, and 600W Ultrasonic Pulverization 2h enters high pressure homogenizer and recycles homogeneous 3 times, homogeneous pressure Strong 1000bar obtains lignocellulosic nanofiber solution;
(2) the modified MXene preparation in surface
A, MAX phase is etched
Lithium fluoride 1g is added in through the cooling polytetrafluoroethylcontainer container of ice water, is slowly added to the hydrochloric acid of 20ml 10mol/L Solution stirs 30min, weighs the titanium aluminum carbide powder 1g of 500 mesh, controls temperature at 50 DEG C hereinafter, being slowly added to several times In above-mentioned solution, 35 DEG C of heat preservation 72h after addition, every 6h shake is primary, after reaction, repeated centrifugation, washing to washing Liquid is in neutrality, drying precipitated;
B, Zn is loaded
The precipitating 2g of a step is added in 100ml deionized water, ultrasonication handles 2min, ultrasonic power 270W, ultrasound Time: then 0.86g anhydrous zinc chloride is added in dwell time 1s:2s, 0.36g cetyl trimethylammonium bromide stirs molten Solution, ammonium hydroxide adjust pH value of solution to 10, stir 30min, obtain suspending liquid A, cetyl trimethyl is added in 50ml deionized water Ammonium bromide 0.18g, hydrazine hydrate 5g, obtains solution B, and solution B is slowly added into suspending liquid A, stirs 2h, alternately anhydrous second Pure and mild distilled water is repeatedly washed, 50 DEG C of drying;
c、CO2High-temperature oxydation
Sample obtained by 0.2g b step is weighed, under argon atmosphere, 600 DEG C is warming up to, keeps the temperature 45min, temperature liter To 750 DEG C, 15min is kept the temperature, atmosphere is switched to carbon dioxide gas, and gas flow 150ml/min keeps the temperature 60min, and atmosphere is cut It is changed to argon gas, after being cooled to room temperature certainly, obtains oxidation product;
(3) molding is filtered
It is received by lignocellulosic nanofiber with the mass ratio of the modified MXene in surface for 60:40 mixing lignocellulosic Rice fiber solution and the modified MXene in surface, stir 12h, filter, roll-in, and electromagnetic shielding paper is made in drying.
Comparative example 1
It with the mass ratio precipitated obtained by a step in (2) is 40:60 mixing wood fibre by lignocellulosic nanofiber It is precipitated obtained by a step in plain nanofiber solution and (2), stirs 12h, filtered, roll-in, drying.
Experiment test:
Using the test method of the Materials ' Shielding Effectiveness in SJ50524-1995 standard 100 × 103—1.5×109kHz Frequency range in test can be carried out to the electromagnetic wave shielding of electromagnetic shielding paper of embodiment preparation, using integrating physical measurement system Unite and electromagnetic shielding paper conductivity at room temperature tested, using omnipotent mechanics machine to the toughness of electromagnetic shielding paper and Tensile break stress is tested, sample size 1cm × 3cm, test result such as table 1.
1 embodiment test result of table
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (8)

1. a kind of preparation method for being electromagnetically shielded paper, which comprises the following steps:
(1) preparation of lignocellulosic nanofiber;
(2) preparation of the modified MXene in surface;
(3) mixed slurry of lignocellulosic nanofiber and the modified MXene in surface, which filter, forms.
2. a kind of preparation method for being electromagnetically shielded paper according to claim 1, which is characterized in that the lignocellulosic is received Rice fiber preparation include pretreatment and broken homogenization, it is described pretreatment be raw material wood powder use respectively petroleum ether, glacial acetic acid with Sodium chlorite, sodium hydroxide solution, hydrochloric acid solution processing;The broken homogenization is that pretreatment product carries out at Ultrasonic Pulverization Reason and high-pressure homogeneous processing.
3. a kind of preparation method for being electromagnetically shielded paper according to claim 1, which is characterized in that the surface is modified MXene includes MXene carrier and load layer, and load layer includes zinc oxide phase, carbon phase and titanium dioxide phase.
4. a kind of preparation method for being electromagnetically shielded paper according to claim 3, which is characterized in that the MXene carrier is Titanium aluminum carbide etches to obtain through the concentrated hydrochloric acid solution dissolved with lithium fluoride, and fluorination lithium concentration is 0.05g/ml.
5. a kind of preparation method for being electromagnetically shielded paper according to claim 3, which is characterized in that the zinc oxide mutually by MXene carrier is obtained through zinc ion load, hydrazine hydrate reduction, carbon dioxide high-temperature oxydation;The carbon phase and titanium dioxide mutually by MXene carrier is obtained through carbon dioxide high-temperature oxydation.
6. a kind of preparation method for being electromagnetically shielded paper according to claim 5, which is characterized in that the carbon dioxide high temperature The process temperature of oxidation is 850 DEG C, soaking time 60min, carbon dioxide flow 150ml/min.
7. a kind of preparation method for being electromagnetically shielded paper according to claim 1, which is characterized in that in the mixed slurry Insoluble matter group changes as the lignocellulosic nanofiber of mass fraction 20%-60% and the surface of mass fraction 40%-80% Property MXene.
8. -7 any preparation methods are obtained according to claim 1 is electromagnetically shielded paper.
CN201811019861.9A 2018-09-03 2018-09-03 A kind of electromagnetic shielding paper and preparation method thereof Withdrawn CN109098038A (en)

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Cited By (6)

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CN110117416A (en) * 2019-04-19 2019-08-13 陕西科技大学 A kind of Ti2C3/ p-aramid fiber nanofiber electromagnetic shielding composite material and preparation method thereof
CN111993725A (en) * 2020-09-02 2020-11-27 苏州大学 Method for improving electromagnetic shielding performance of MXene-based composite fabric material
CN113373728A (en) * 2020-03-31 2021-09-10 中科院广州化学有限公司 High-strength electromagnetic shielding and heat conducting ultrathin composite paper and preparation method and application thereof
WO2021237862A1 (en) * 2020-05-26 2021-12-02 苏州大学 Macroscopic high-conductivity mxene ribbon-like fibers with ordered stacking of nanosheets, and flexible capacitor
CN113881108A (en) * 2021-10-07 2022-01-04 华南理工大学 Pineapple leaf fiber-reinforced flexible electromagnetic shielding film and preparation method thereof
CN114507383A (en) * 2022-03-23 2022-05-17 陕西科技大学 Preparation method of esterified cellulose loaded MXene high-toughness film

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