CN105177745B - A kind of novel electromagnetic shielding nano-sized carbon conductive fiber material and preparation method thereof - Google Patents
A kind of novel electromagnetic shielding nano-sized carbon conductive fiber material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material and preparation method thereof, belong to technical field of nano material, described material includes：Graphite, carbon nano-fiber, conducting polymer, polymer adhesive, dispersant, alkali metal fluoride, metallic catalyst, conductive metal, surface conditioning agent；Described preparation method is：Graphite alkali metal fluoride pretreatment；It is separately added into surface conditioning agent after carbon nano-fiber mixing acid oxidase and conductive metal carries out heat treated；With dispersant, conducting polymer, polymer adhesive blending, ultrasonic disperse, ozonation treatment after pretreated graphite and carbon nano-fiber dissolving, grind, form the solution of homogenizing；It is blended with chemical blend thing, prepare nano-sized carbon conductive fiber material with method of electrostatic spinning again.The novel electromagnetic shielding nano-sized carbon conductive fiber material of present invention preparation has good capability of electromagnetic shielding, nontoxic, without any carcinogen, can be used for manufacturing exposure suit etc..
Description
Technical field
The invention belongs to technical field of nano material, a kind of specifically novel electromagnetic shielding nanometer carbon conductive fibers material
Material and preparation method thereof.
Background technology
People enjoy digital information technology bring convenient when, also subject " breaking of " invisible killer "
Residual "-Contamination of Electromagnetic Wave, pour in family, electromagnetism spoke with household electrical appliance, communication equipment, electronic product and electric equipment etc.
The covering penetrated has been deep into each corner of human lives, artificial electromagnetic energy with the speed increase in 10%-15%/year,
Electromagnetic pollution has become the fourth-largest polluter after waste water,waste gas and industrial residue.
Scientific research and it is demonstrated experimentally that these Radiation On Human bodies are harmful, if people is chronically exposed to stronger electromagnetism
Cell state exception and cell function can be led in the radiation of field abnormal, neurasthenia and nervous dysfunction, endocrine can be led to
Imbalance, serious even induces canceration, therefore it should avoid accepting radiation, particularly anemia of pregnant woman and infant as far as possible, more should subtract
Less and avoid receiving these radiation, so needing to manufacture radiation proof material to protect human body.Existing radiation proof material on the market
The main external electromagnetic that reflected by the screen layer of metallic fiber is radiated, to avoid these radiation to enter human body.However, it is this anti-
Radiation clothes can not stop all radiation from entering inside clothes, when radiation enters radioprotective by the gap such as neckline, cuff, bottom
When in clothes, this reflective screen layer can make these radiation multiple reflections and superposition that crosses, consequently, it is possible to allowing exposure suit
Interior radiant intensity becomes may make the radiation injury that human body is subject to bigger so that wearing exposure suit greatly, so existing radioprotective
The radiation-proof effect of clothes is poor, can not meet radioprotective demand at all.
Through overtesting, new material such as graphite and carbon nano-fiber, have proved that its conductive radiation protection ability is splendid, no
By external interference, reach the effect of radiation-proof anti-static, but in existing technology, directly by graphite dispersion to fabric fibre
In, the poor dispersion of graphite, easily assemble, so poor performance, in addition simple carbon nano-fiber spinning moulding effect is poor,
All have much room for improvement.
Accordingly, it would be desirable to by graphite and carbon nano-fiber are carried out certain process, then it is compounded in one with conducting polymer
Rise, and be manufactured into novel electromagnetic shielding textile fabric so as to have good capability of electromagnetic shielding, be used further to manufacture radioprotective
Clothes.
Content of the invention
Present invention solves the technical problem that being to provide a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material, have good
Capability of electromagnetic shielding, can be used for manufacture exposure suit.
The Second Problem that the present invention solves is to provide a kind of preparation of novel electromagnetic shielding nano-sized carbon conductive fiber material
Method.
For solving above-mentioned first technical problem, the technical solution adopted in the present invention is：A kind of novel electromagnetic shielding is received
Rice carbon conductive fibers material, component meter by weight includes following components：3～6 parts of graphite, 15～35 parts of carbon nano-fiber, conduction
60～98 parts of polymer, 0.2～0.8 part of polymer adhesive, 0.5～1.0 part of dispersant, alkali metal fluoride 0.02～0.1
Part, 0.1～0.2 part of metallic catalyst, 0.03～0.15 part of conductive metal, 0.5～1.0 part of surface conditioning agent；Described conduction
Polymer is poly- (indenofluorene-triphenylamine), described polymer adhesive be 1,3- double-(3,3,4,4- di carboxyl phenyloxy) benzene and
4,4- pair-(4- amino-benzene oxygen)-diphenyl presses 1:2～3 combine, and described dispersant is ethylene stearic bicine diester
Amine, described metallic catalyst is metallocene, and described surface conditioning agent is ITO or SnO2, described conductive metal include barium, silver,
The salt of at least one metallic element in cobalt, nickel, stannum, metal-oxide, metal chloride or metal nitride.
Further, a kind of described novel electromagnetic shielding nano-sized carbon conductive fiber material, also includes 0.01～0.03 part
Dispersible X-Ray and electron beam shielding material, described material is the change of at least one element in silicon, strontium, magnesium, europium and dysprosium
Compound, these materials can shield to radioactive radiation, strengthens its performance, widens the range of material of the present invention.
For solving above-mentioned second technical problem, the technical solution adopted in the present invention is：A kind of novel electromagnetic shielding is received
The preparation method of rice carbon conductive fibers material, comprises the following steps：
(1) Graphitic pretreatment, mixes alkali metal fluoride in Nano graphite powder, and adds metallic catalyst, mixes,
Heat at 500～700 DEG C under inert gas shielding, control heat time heating time at 8～20 minutes, described noble gases are from an oxidation
One or more mixed gas selecting in carbon, methane, acetylene, ethylene and propane, alkali metal fluoride is fixed on a nanometer stone
On toner surface；
(2) carbon nano-fiber pretreatment, Nano carbon fibers Wesy concentrated sulphuric acid and potassium permanganate are carried out mixing acid oxidase, through super
After sound or high shear are stirred vigorously, obtain carboxylated carbon nano-fiber, add surface conditioning agent, heat at 200～300 DEG C
Process 5～8 minutes, add conductive metal, nitrogen and argon mixed gas protected under heat 20 at 300～500 DEG C～
30 minutes, conductive metal is dispersed in carbon nano-fiber；
(3) carbon nano-fiber of the graphite of step (1) pretreatment and step (2) pretreatment is placed in container, with 240～
300 parts of polar solvent dissolvings, add dispersant, conducting polymer, polymer adhesive, are blended with forced mixer, then
Carry out ultrasonic disperse with ultrasound wave separating apparatus again, supersonic frequency is 20KHz, the time is 0.5～1.0 hour, then be placed in ozone sending out
Carry out ozonation treatment in generating apparatus, ozonation treatment can promote the hydrophiling on the surface of raw fibre, polished, formed
The solution of homogenizing；
(4) solution that step (3) obtains is carried out chemical blend with chemical blend thing, described chemical blend thing is polyoxy second
Alkene, the mass fraction of described chemical blend thing accounts for the 20～35% of original solution, prepares a nanometer carbonaceous conductive fibre with method of electrostatic spinning
Dimension material, a diameter of 1.0～1.2mm of conical pipe sharp-crested used by described electrostatic spinning, conical pipe is from the horizontal by 6～8 °
Angle, is beneficial to conical pipe sharp-crested droplet formation, adds the electric field intensity of 1.2kV/cm at solution two ends.
Further, in such scheme, described concentrated sulphuric acid consumption is 420～480 parts, and potassium permanganate consumption is 10～50
Part, described concentrated sulphuric acid concentration is 95～98%, and with potassium permanganate and use can improve treatment effeciency to concentrated sulphuric acid.
Further, in such scheme, described polar solvent is selected from isopropanol (IPA), Ketohexamethylene, ethyl acetate, N-
Any one in methyl pyrrolidone (NMP), butyl acetate or methyl iso-butyl ketone (MIBK).
Further, in such scheme, described alkali metal fluoride is LiF or CsF.
The invention has the beneficial effects as follows：First, its good dispersion of graphite after being processed using the inventive method, it is difficult to gather
Collection；Second, the carbon nano-fiber after being processed using the inventive method not only has improved electric conductivity, can easily gather with conduction
Compound is combined with each other, and also has the physical property of reinforcement relatively, and has improved tensile strength and tear resistance；3rd, this
Inventing the nano-sized carbon conductive fiber material made has a good capability of electromagnetic shielding, nontoxic, do not contain any carcinogen, to human body and
Environment is safe from harm, and is highly suitable for manufacturing exposure suit etc..
Specific embodiment
Embodiment 1：A kind of novel electromagnetic shielding nano-sized carbon conductive fiber material, component meter by weight includes following components：
3 parts of graphite, 15 parts of carbon nano-fiber, 60 parts of poly- (indenofluorene-triphenylamine), 1,3- be double-(3,3,4,4- di carboxyl phenyloxy) benzene
- (4- amino-benzene oxygen)-diphenyl double with 4,4- presses 1:0.2 part of the polymer adhesive that 2 combine, 1,2- ethylenebis are hard
0.5 part of acyl amine, 0.02 part of alkali metal fluoride, 0.1 part of metallocene, barium and silver are led as the metal-oxide composition of any ratio
0.03 part of electric type metal, the Dispersible X-Ray of compound composition of 0.5 part of ITO, silicon and strontium and 0.01 part of electron beam shielding material,
These materials can shield to radioactive radiation, strengthens its performance, widens the range of material of the present invention.
A kind of preparation method of novel electromagnetic shielding nano-sized carbon conductive fiber material, comprises the following steps：
(1) Graphitic pretreatment, mixes alkali metal fluoride LiF in Nano graphite powder, and adds metallic catalyst, mixes
Even, heat at 500 DEG C under inert gas shielding, control heat time heating time at 8 minutes, described noble gases are carbon monoxides, will
Alkali metal fluoride is fixed on Nano graphite powder surface；
(2) carbon nano-fiber pretreatment, by 420 parts of concentration of Nano carbon fibers Wesy be 95% concentrated sulphuric acid and 10 parts of permanganic acid
Potassium carries out mixing acid oxidase, and with potassium permanganate and use can improve treatment effeciency to concentrated sulphuric acid, is stirred vigorously through ultrasonic or high shear
Afterwards, obtain carboxylated carbon nano-fiber, add surface conditioning agent, in 200 DEG C of heat treated 5 minutes, add conductivity type gold
Belong to, nitrogen and argon mixed gas protected under heat 20 minutes at 300 DEG C, conductive metal is dispersed in nano-sized carbon
In fiber；
(3) carbon nano-fiber of the graphite of step (1) pretreatment and step (2) pretreatment is placed in container, with 240 parts
Polar solvent isopropanol (IPA) dissolves, and adds dispersant, conducting polymer, polymer adhesive, with forced mixer altogether
Mixed, then carry out ultrasonic disperse with ultrasound wave separating apparatus again, supersonic frequency is 20KHz, the time is 0.5 hour, then is placed in ozone
Carry out ozonation treatment, ozonation treatment can promote the hydrophiling on the surface of raw fibre, polished, shape in generating meanss
Become the solution of homogenizing；
(4) solution that step (3) obtains is carried out chemical blend with chemical blend thing, described chemical blend thing is polyoxy second
Alkene, the mass fraction of described chemical blend thing accounts for the 2% of original solution, prepares a nanometer carbon conductive fibers material with method of electrostatic spinning
Material, a diameter of 1.0mm of conical pipe sharp-crested used by described electrostatic spinning, conical pipe, from the horizontal by 6 ° of angles, is beneficial to taper
Tip mouth droplet formation, adds the electric field intensity of 1.2kV/cm at solution two ends.
Embodiment 2：A kind of novel electromagnetic shielding nano-sized carbon conductive fiber material, component meter by weight includes following components：
4.5 parts of graphite, 25 parts of carbon nano-fiber, 79 parts of poly- (indenofluorene-triphenylamine), 1,3- be double-and (3,3,4,4- di carboxyl phenyloxy)
Benzene and 4,4- pair-(4- amino-benzene oxygen)-diphenyl press 1:0.5 part of the polymer adhesive that 2.5 combine, 1,2- ethylidene
0.75 part of bis-stearamides, 0.06 part of alkali metal fluoride, 0.15 part of metallocene, silver and cobalt press the metal chloride group of any ratio
0.09 part of the conductive metal of one-tenth, SnO2The Dispersible X-Ray of compound composition of 0.75 part, magnesium and europium and electron beam shielding material
0.02 part of material, these materials can shield to radioactive radiation, strengthens its performance, widens the use model of material of the present invention
Enclose.
A kind of preparation method of novel electromagnetic shielding nano-sized carbon conductive fiber material, comprises the following steps：
(1) Graphitic pretreatment, mixes alkali metal fluoride LiF in Nano graphite powder, and adds metallic catalyst, mixes
Even, heat at 600 DEG C under inert gas shielding, control heat time heating time at 14 minutes, described noble gases are methane and propane
Mixed gas, alkali metal fluoride is fixed on Nano graphite powder surface；
(2) carbon nano-fiber pretreatment, by 450 parts of concentration of Nano carbon fibers Wesy be 96% concentrated sulphuric acid and 30 parts of permanganic acid
Potassium carries out mixing acid oxidase, and with potassium permanganate and use can improve treatment effeciency to concentrated sulphuric acid, is stirred vigorously through ultrasonic or high shear
Afterwards, obtain carboxylated carbon nano-fiber, add surface conditioning agent, in 250 DEG C of heat treated 6.5 minutes, add conductivity type
Metal, nitrogen and argon mixed gas protected under heat 25 minutes at 400 DEG C, conductive metal is dispersed in nanometer
In carbon fiber；
(3) carbon nano-fiber of the graphite of step (1) pretreatment and step (2) pretreatment is placed in container, with 270 parts
Polar solvent ethyl acetate dissolves, and adds dispersant, conducting polymer, polymer adhesive, is blended with forced mixer, so
Carry out ultrasonic disperse with ultrasound wave separating apparatus more afterwards, supersonic frequency is 20KHz, the time is 0.75 hour, then be placed in ozone occurring
Carry out ozonation treatment in device, ozonation treatment can promote the hydrophiling on the surface of raw fibre, polished, formed all
The solution of matter；
(4) solution that step (3) obtains is carried out chemical blend with chemical blend thing, described chemical blend thing is polyoxy second
Alkene, the mass fraction of described chemical blend thing accounts for the 27.5% of original solution, prepares nanometer carbon conductive fibers with method of electrostatic spinning
Material, a diameter of 1.1mm of conical pipe sharp-crested used by described electrostatic spinning, conical pipe, from the horizontal by 7 ° of angles, is beneficial to cone
Shape tip mouth droplet formation, adds the electric field intensity of 1.2kV/cm at solution two ends.
Embodiment 3：A kind of novel electromagnetic shielding nano-sized carbon conductive fiber material, component meter by weight includes following components：
6 parts of graphite, 35 parts of carbon nano-fiber, 98 parts of poly- (indenofluorene-triphenylamine), 1,3- be double-(3,3,4,4- di carboxyl phenyloxy) benzene
- (4- amino-benzene oxygen)-diphenyl double with 4,4- presses 1:0.8 part of the polymer adhesive that 3 combine, 1,2- ethylenebis are hard
1.0 parts of acyl amine, 0.1 part of alkali metal fluoride, 0.2 part of metallocene, nickel and stannum are led as the metal nitride composition of any ratio
0.15 part of electric type metal, SnO2The Dispersible X-Ray of compound composition of 1.0 parts, europium and dysprosium and electron beam shielding material 0.03
Part, these materials can shield to radioactive radiation, strengthens its performance, widens the range of material of the present invention.
A kind of preparation method of novel electromagnetic shielding nano-sized carbon conductive fiber material, comprises the following steps：
(1) Graphitic pretreatment, mixes alkali metal fluoride CsF in Nano graphite powder, and adds metallic catalyst, mixes
Even, heat at 700 DEG C under inert gas shielding, control heat time heating time at 20 minutes, described noble gases are from acetylene and second
The mixed gas of alkene, alkali metal fluoride is fixed on Nano graphite powder surface；
(2) carbon nano-fiber pretreatment, by 480 parts of concentration of Nano carbon fibers Wesy be 98% concentrated sulphuric acid and 50 parts of permanganic acid
Potassium carries out mixing acid oxidase, and with potassium permanganate and use can improve treatment effeciency to concentrated sulphuric acid, is stirred vigorously through ultrasonic or high shear
Afterwards, obtain carboxylated carbon nano-fiber, add surface conditioning agent, in 300 DEG C of heat treated 8 minutes, add conductivity type gold
Belong to, nitrogen and argon mixed gas protected under heat 30 minutes at 500 DEG C, conductive metal is dispersed in nano-sized carbon
In fiber；
(3) carbon nano-fiber of the graphite of step (1) pretreatment and step (2) pretreatment is placed in container, with 300 parts
Polar solvent N-Methyl pyrrolidone (NMP) dissolves, and adds dispersant, conducting polymer, polymer adhesive, mixed with strength
Clutch is blended, and then carries out ultrasonic disperse with ultrasound wave separating apparatus again, and supersonic frequency is 20KHz, and the time is 1.0 hours, then puts
Carry out ozonation treatment in ozone generating-device, ozonation treatment can promote the hydrophiling on the surface of raw fibre, through grinding
After mill, form the solution of homogenizing；
(4) solution that step (3) obtains is carried out chemical blend with chemical blend thing, described chemical blend thing is polyoxy second
Alkene, the mass fraction of described chemical blend thing accounts for the 35% of original solution, prepares a nanometer carbon conductive fibers material with method of electrostatic spinning
Material, a diameter of 1.2mm of conical pipe sharp-crested used by described electrostatic spinning, conical pipe, from the horizontal by 8 ° of angles, is beneficial to taper
Tip mouth droplet formation, adds the electric field intensity of 1.2kV/cm at solution two ends.
Finally it should be noted that：Above example only in order to technical scheme to be described, is not intended to limit；Although
With reference to the foregoing embodiments the present invention is described in detail, it will be understood by those within the art that：It still may be used
To modify to the technical scheme described in previous embodiment, or equivalent is carried out to wherein some technical characteristics；And
These modifications or replacement, do not make the essence of appropriate technical solution depart from spirit and the model of embodiment of the present invention technical scheme
Enclose.
Claims (4)
1. a kind of preparation method of electromagnetic shielding nano-sized carbon conductive fiber material it is characterised in that：Described electromagnetic shielding nano-sized carbon
Conductive fiber material：Component meter by weight includes following components：3～6 parts of graphite, 15～35 parts of carbon nano-fiber, conducting polymer
60～98 parts of thing, 0.2～0.8 part of polymer adhesive, 0.5～1.0 part of dispersant, 0.02～0.1 part of alkali metal fluoride, gold
0.1～0.2 part of metal catalyst, 0.03～0.15 part of conductive metal, 0.5～1.0 part of surface conditioning agent；Described conducting polymer
For poly- (indenofluorene-triphenylamine), described polymer adhesive is 1,3- pair-(3,3,4,4- di carboxyl phenyloxy) benzene and 4,4-
Double-(4- amino-benzene oxygen)-diphenyl presses 1:2～3 combine, and described dispersant is ethylene bis-stearamides, institute
Stating metallic catalyst is metallocene, and described surface conditioning agent is ITO or SnO2, described conductive metal include barium, silver, cobalt, nickel,
The salt of at least one metallic element in stannum, metal-oxide, metal chloride or metal nitride；
Described electromagnetic shielding nano-sized carbon conductive fiber material comprises the following steps：
(1) Graphitic pretreatment, mixes alkali metal fluoride in Nano graphite powder, and adds metallic catalyst, mixes, in inertia
Heat at 500～700 DEG C under gas shield, described noble gases are choosings from carbon monoxide, methane, acetylene, ethylene and propane
One or more mixed gas selected, alkali metal fluoride is fixed on Nano graphite powder surface；
(2) carbon nano-fiber pretreatment, Nano carbon fibers Wesy concentrated sulphuric acid and potassium permanganate are carried out mixing acid oxidase, through ultrasonic or
After high shear is stirred vigorously, obtain carboxylated carbon nano-fiber, add surface conditioning agent, in 200～300 DEG C of heat treated
5～8 minutes, add conductive metal, nitrogen and argon mixed gas protected under heat 20～30 points at 300～500 DEG C
Clock, conductive metal is dispersed in carbon nano-fiber；
(3) carbon nano-fiber of the graphite of step (1) pretreatment and step (2) pretreatment is placed in container, uses polar solvent
Dissolving, adds dispersant, conducting polymer, polymer adhesive, blending, ultrasonic disperse, then is placed in ozone generating-device
Carry out ozonation treatment, grind, form the solution of homogenizing；
(4) solution that step (3) obtains is blended with chemical blend thing, described chemical blend thing is polyoxyethylene, then uses electrostatic
Spin processes prepare nano-sized carbon conductive fiber material.
2. a kind of preparation method of novel electromagnetic shielding nano-sized carbon conductive fiber material as claimed in claim 1, its feature exists
In：Described concentrated sulphuric acid consumption be 420～480 parts, potassium permanganate consumption be 10～50 parts, described concentrated sulphuric acid concentration be 95～
98%.
3. a kind of preparation method of novel electromagnetic shielding nano-sized carbon conductive fiber material as claimed in claim 2, its feature exists
In：Described polar solvent be selected from isopropanol (IPA), Ketohexamethylene, ethyl acetate, N-Methyl pyrrolidone (NMP), butyl acetate or
Any one in methyl iso-butyl ketone (MIBK).
4. a kind of preparation method of novel electromagnetic shielding nano-sized carbon conductive fiber material as claimed in claim 2, its feature exists
In：Described alkali metal fluoride is LiF or CsF.
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|---|---|---|---|---|
| FR2933426B1 (en) * | 2008-07-03 | 2010-07-30 | Arkema France | PROCESS FOR PRODUCING COMPOSITE CONDUCTIVE FIBERS, FIBERS OBTAINED BY THE PROCESS AND USE OF SUCH FIBERS |
| DE102009017262A1 (en) * | 2009-04-11 | 2010-10-14 | Karlsruher Institut für Technologie | Cathode material for fluoride-based conversion electrodes, process for its preparation and its use |
| CN104099683B (en) * | 2013-04-12 | 2016-05-25 | 中国石油化工股份有限公司 | A kind of polymer/conductive filler/metal composite fiber and preparation method thereof |
| CN104790067B (en) * | 2015-04-17 | 2017-10-03 | 东华大学 | Conductivity high molecule nanometer/graphene composite fibre and its preparation method and application |
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2015
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