CN105177745A - Novel electromagnetic shielding nanocarbon conductive fibrous material and preparation method thereof - Google Patents
Novel electromagnetic shielding nanocarbon conductive fibrous material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a novel electromagnetic shielding nanocarbon conductive fibrous material and a preparation method thereof, and belongs to the field of a nano-material technology. The material comprises the following components: graphite, a nanometer carbon fiber, a conductive polymer, a polymer adhesive, a dispersant, alkali metal fluoride, a metal catalyst, a conductive metal and a surface conditioning agent. The preparation method comprises the following steps: the graphite is subjected to pretreatment with alkali metal fluoride; the nanometer carbon fiber is oxidized by an acid mixture, the surface conditioning agent and the conductive metal are added separately, and a heating treatment is carried out; after the pretreated graphite and the pretreated nanometer carbon fiber are dissolved, the dispersant, the conductive polymer and the polymer adhesive are added for blending, and ultrasonic dispersion, ozonization treatment and grinding are carried out to form a homogeneous solution; a chemical blend is blended with the obtained solution, and the nanocarbon conductive fibrous material is prepared by a electrostatic spinning method. The novel electromagnetic shielding nanocarbon conductive fibrous material prepared by the invention has good electromagnetic shielding performance, and does not have toxicity and any carcinogenic substances; the novel electromagnetic shielding nanocarbon conductive fibrous material can be used for manufacturing radiation-proof clothes and the like.
Description
Technical field
The invention belongs to technical field of nano material, specifically a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material and preparation method thereof.
Background technology
People enjoy digital information technology bring convenient when, also at " wrecking "-Contamination of Electromagnetic Wave that subject " invisible killer ", along with household electrical appliance, communication equipment, electronic product and electric equipment etc. pour in family, the covering of electromagnetic radiation has been deep into each corner of human lives, artificial electromagnetic energy is with the speed increase in 10%-15%/year, and electromagnetic pollution has become the fourth-largest pollution sources after waste water,waste gas and industrial residue.
Scientific research and experiment prove; these Radiation On Human bodies are harmful; if people is chronically exposed in stronger electromagnetic field radiation can cause cell state exception and cell function extremely; can cause neurasthenia and nerve dysfunction, endocrinopathy, serious even brings out canceration, therefore; should avoid accepting radiation as far as possible; particularly pregnant woman and infant, more should reduce and avoid receiving these radiation, so need to manufacture radiation proof material to protect human body.Existing radiation proof material on the market carrys out reflect ambient electromagnetic radiation mainly through the screen layer of metal fibre, enters human body to avoid these radiation.But, this exposure suit can not stop all radiation to enter clothes inside, when radiation is entered in exposure suit by gaps such as neckline, cuff, the bottoms, this reflective screen layer can make these radiation multiple reflections and the superposition that crosses, thus the radiation intensity in exposure suit may be allowed to become large, make to wear the radiation injury that exposure suit may make human body be subject to larger, so the radiation-proof effect of existing exposure suit is poor, radiation proof demand can not be met at all.
Novel material is as graphite and carbon nano-fiber, prove that its conduction radiation protection ability is splendid through overtesting, not by external interference, reach the effect of radiation-proof anti-static, but in existing technology, directly by graphite dispersion in fabric fibre, the dispersiveness of graphite is bad, easily assembles, so poor performance, carbon nano-fiber spinning moulding weak effect simple in addition, all haves much room for improvement.
Therefore, need by graphite and carbon nano-fiber are carried out certain process, then be combined with each other with conducting polymer, and manufacture novel electromagnetic shielding textile fabric, make it have good capability of electromagnetic shielding, be used further to manufacture exposure suit.
Summary of the invention
The technical problem that the present invention solves is to provide a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material, has good capability of electromagnetic shielding, can be used for manufacturing exposure suit.
The Second Problem that the present invention solves is to provide a kind of preparation method of novel electromagnetic shielding nano-sized carbon conductive fiber material.
For solving above-mentioned first technical problem, the technical solution adopted in the present invention is: a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material, and component meter comprises following component by weight: 3 ~ 6 parts, graphite, carbon nano-fiber 15 ~ 35 parts, conducting polymer 60 ~ 98 parts, polymer adhesive 0.2 ~ 0.8 part, dispersant 0.5 ~ 1.0 part, alkali metal fluoride 0.02 ~ 0.1 part, metallic catalyst 0.1 ~ 0.2 part, conductive metal 0.03 ~ 0.15 part, surface conditioning agent 0.5 ~ 1.0 part; Described conducting polymer is poly-(indenofluorene-triphenylamine), described polymer adhesive is 1,3-two-(3,3,4,4-di carboxyl phenyloxy) benzene and 4,4-pair-(4-amino-benzene oxygen)-diphenyl combines by 1:2 ~ 3, and described dispersant is 1,2-ethylenebisstearamide, described metallic catalyst is metallocene, and described surface conditioning agent is ITO or SnO
2, described conductive metal comprises the salt of at least one metallic element in barium, silver, cobalt, nickel, tin, metal oxide, metal chloride or metal nitride.
Further, described a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material, also comprise Dispersible X-Ray and the electron beam shielding material of 0.01 ~ 0.03 part, described material is the compound of at least one element be selected from silicon, strontium, magnesium, europium and dysprosium, these materials can shield radioactive radiation, strengthen its performance, widen the scope of application 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 preparation method of novel electromagnetic shielding nano-sized carbon conductive fiber material, comprises the following steps:
(1) Graphitic pretreatment, alkali metal fluoride is mixed in Nano graphite powder, and add metallic catalyst, mixing, 500 ~ 700 DEG C of heating under inert gas shielding, control heat time heating time at 8 ~ 20 minutes, described inert gas is one or more mists selected from carbon monoxide, methane, acetylene, ethene and propane, alkali metal fluoride is fixed on Nano graphite powder on the surface;
(2) carbon nano-fiber preliminary treatment, the Nano carbon fibers Wesy concentrated sulfuric acid and potassium permanganate are carried out mixed acid oxidation, after ultrasonic or high shear vigorous stirring, obtain carboxylated carbon nano-fiber, add surface conditioning agent, 200 ~ 300 DEG C of heat treated 5 ~ 8 minutes, add conductive metal, nitrogen and argon gas mixed gas protected under 300 ~ 500 DEG C of heating 20 ~ 30 minutes, conductive metal is dispersed in carbon nano-fiber;
(3) step (1) pretreated graphite and step (2) pretreated carbon nano-fiber are placed in container, dissolve with 240 ~ 300 parts of polar solvents, add dispersant, conducting polymer, polymer adhesive again, blended with forced mixer, and then carry out ultrasonic disperse with ultrasonic wave separating apparatus, supersonic frequency is 20KHz, time is 0.5 ~ 1.0 hour, be placed in ozone generating-device again and carry out ozonation treatment, ozonation treatment can promote the hydrophiling on the surface of raw fiber, after grinding, form the solution of homogeneous;
(4) solution step (3) obtained and chemical blend thing carry out chemical blend, described chemical blend thing is polyoxyethylene, the mass fraction of described chemical blend thing accounts for 20 ~ 35% of original solution, nano-sized carbon conductive fiber material is prepared with method of electrostatic spinning, described electrostatic spinning conical pipe sharp-crested diameter used is 1.0 ~ 1.2mm, conical pipe, from the horizontal by 6 ~ 8 ° of angles, is beneficial to conical pipe sharp-crested drop and is formed, add the electric-field intensity of 1.2kV/cm at solution two ends.
Further, in such scheme, described concentrated sulfuric acid consumption is 420 ~ 480 parts, and potassium permanganate consumption is 10 ~ 50 parts, and described concentrated sulfuric acid concentration is 95 ~ 98%, and the concentrated sulfuric acid and potassium permanganate are also with improving treatment effeciency.
Further, in such scheme, described polar solvent be selected from isopropyl alcohol (IPA), cyclohexanone, ethyl acetate, 1-METHYLPYRROLIDONE (NMP), butyl acetate or methyl iso-butyl ketone (MIBK) any one.
Further, in such scheme, described alkali metal fluoride is LiF or CsF.
The invention has the beneficial effects as follows: the first, adopt its good dispersion of graphite after the inventive method process, not easily assemble; The second, adopt the carbon nano-fiber after the inventive method process not only to have the electric conductivity of improvement, can easily be combined with each other with conducting polymer, also have the physical property of relative reinforcement, and there is TENSILE STRENGTH and the tear resistance of improvement; 3rd, the nano-sized carbon conductive fiber material that the present invention makes has good capability of electromagnetic shielding, nontoxic, not containing any carcinogenic substance, be safe from harm to human body and environment, is highly suitable for manufacturing exposure suit etc.
Detailed description of the invention
Embodiment 1: a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material, component meter comprises following component by weight: 3 parts, graphite, carbon nano-fiber 15 parts, poly-(indenofluorene-triphenylamine) 60 parts, 1, 3-two-(3, 3, 4, 4-di carboxyl phenyloxy) benzene and 4, the polymer adhesive 0.2 part that 4-pair-(4-amino-benzene oxygen)-diphenyl combines by 1:2, 1, 2-ethylenebisstearamide 0.5 part, alkali metal fluoride 0.02 part, metallocene 0.1 part, the conductive metal 0.03 part that barium and silver form by the metal oxide of any ratio, ITO0.5 part, the Dispersible X-Ray of the compound composition of silicon and strontium and electron beam shielding material 0.01 part, these materials can shield radioactive radiation, strengthen its performance, widen the scope of application of material of the present invention.
A preparation method for novel electromagnetic shielding nano-sized carbon conductive fiber material, comprises the following steps:
(1) Graphitic pretreatment, alkali metal fluoride LiF is mixed in Nano graphite powder, and add metallic catalyst, mixing, 500 DEG C of heating under inert gas shielding, control heat time heating time at 8 minutes, described inert gas is carbon monoxide, alkali metal fluoride is fixed on Nano graphite powder on the surface;
(2) carbon nano-fiber preliminary treatment, by Nano carbon fibers Wesy 420 parts of concentration be 95% the concentrated sulfuric acid and 10 parts of potassium permanganate carry out mixed acid oxidation, the concentrated sulfuric acid and potassium permanganate are also with improving treatment effeciency, after ultrasonic or high shear vigorous stirring, obtain carboxylated carbon nano-fiber, add surface conditioning agent, 200 DEG C of heat treated 5 minutes, add conductive metal, nitrogen and argon gas mixed gas protected under 300 DEG C of heating 20 minutes, conductive metal is dispersed in carbon nano-fiber;
(3) step (1) pretreated graphite and step (2) pretreated carbon nano-fiber are placed in container, dissolve with 240 parts of polar solvent isopropyl alcohols (IPA), add dispersant, conducting polymer, polymer adhesive again, blended with forced mixer, and then carry out ultrasonic disperse with ultrasonic wave separating apparatus, supersonic frequency is 20KHz, time is 0.5 hour, be placed in ozone generating-device again and carry out ozonation treatment, ozonation treatment can promote the hydrophiling on the surface of raw fiber, after grinding, form the solution of homogeneous;
(4) solution step (3) obtained and chemical blend thing carry out chemical blend, described chemical blend thing is polyoxyethylene, the mass fraction of described chemical blend thing accounts for 2% of original solution, nano-sized carbon conductive fiber material is prepared with method of electrostatic spinning, described electrostatic spinning conical pipe sharp-crested diameter used is 1.0mm, conical pipe, from the horizontal by 6 ° of angles, is beneficial to conical pipe sharp-crested drop and is formed, add 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 comprises following component by weight: 4.5 parts, graphite, carbon nano-fiber 25 parts, poly-(indenofluorene-triphenylamine) 79 parts, 1,3-two-(3,3,4,4-di carboxyl phenyloxy) benzene and 4, conductive metal 0.09 part, SnO that the polymer adhesive 0.5 part that 4-pair-(4-amino-benzene oxygen)-diphenyl combines by 1:2.5,1,2-ethylenebisstearamide 0.75 part, alkali metal fluoride 0.06 part, metallocene 0.15 part, silver and cobalt form by the metal chloride of any ratio
20.75 part, the Dispersible X-Ray of the compound composition of magnesium and europium and electron beam shielding material 0.02 part, these materials can shield radioactive radiation, strengthen its performance, widen the scope of application of material of the present invention.
A preparation method for novel electromagnetic shielding nano-sized carbon conductive fiber material, comprises the following steps:
(1) Graphitic pretreatment, alkali metal fluoride LiF is mixed in Nano graphite powder, and add metallic catalyst, mixing, 600 DEG C of heating under inert gas shielding, control heat time heating time at 14 minutes, described inert gas is the mist of methane and propane, alkali metal fluoride is fixed on Nano graphite powder on the surface;
(2) carbon nano-fiber preliminary treatment, by Nano carbon fibers Wesy 450 parts of concentration be 96% the concentrated sulfuric acid and 30 parts of potassium permanganate carry out mixed acid oxidation, the concentrated sulfuric acid and potassium permanganate are also with improving treatment effeciency, after ultrasonic or high shear vigorous stirring, obtain carboxylated carbon nano-fiber, add surface conditioning agent, 250 DEG C of heat treated 6.5 minutes, add conductive metal, nitrogen and argon gas mixed gas protected under 400 DEG C of heating 25 minutes, conductive metal is dispersed in carbon nano-fiber;
(3) step (1) pretreated graphite and step (2) pretreated carbon nano-fiber are placed in container, with 270 parts of polar solvent acetic acid ethyl dissolutions, add dispersant, conducting polymer, polymer adhesive again, blended with forced mixer, and then carry out ultrasonic disperse with ultrasonic wave separating apparatus, supersonic frequency is 20KHz, time is 0.75 hour, be placed in ozone generating-device again and carry out ozonation treatment, ozonation treatment can promote the hydrophiling on the surface of raw fiber, after grinding, form the solution of homogeneous;
(4) solution step (3) obtained and chemical blend thing carry out chemical blend, described chemical blend thing is polyoxyethylene, the mass fraction of described chemical blend thing accounts for 27.5% of original solution, nano-sized carbon conductive fiber material is prepared with method of electrostatic spinning, described electrostatic spinning conical pipe sharp-crested diameter used is 1.1mm, conical pipe, from the horizontal by 7 ° of angles, is beneficial to conical pipe sharp-crested drop and is formed, add 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 comprises following component by weight: 6 parts, graphite, carbon nano-fiber 35 parts, poly-(indenofluorene-triphenylamine) 98 parts, 1,3-two-(3,3,4,4-di carboxyl phenyloxy) benzene and 4,4-is two-polymer adhesive 0.8 part, 1,2-ethylenebisstearamide 1.0 parts, alkali metal fluoride 0.1 part, metallocene 0.2 part, nickel and tin that (4-amino-benzene oxygen)-diphenyl combines by the 1:3 conductive metal 0.15 part, the SnO that form by the metal nitride of any ratio
21.0 parts, the Dispersible X-Ray of the compound composition of europium and dysprosium and electron beam shielding material 0.03 part, these materials can shield radioactive radiation, strengthen its performance, widen the scope of application of material of the present invention.
A preparation method for novel electromagnetic shielding nano-sized carbon conductive fiber material, comprises the following steps:
(1) Graphitic pretreatment, alkali metal fluoride CsF is mixed in Nano graphite powder, and add metallic catalyst, mixing, 700 DEG C of heating under inert gas shielding, control heat time heating time at 20 minutes, described inert gas is the mist from acetylene and ethene, alkali metal fluoride is fixed on Nano graphite powder on the surface;
(2) carbon nano-fiber preliminary treatment, by Nano carbon fibers Wesy 480 parts of concentration be 98% the concentrated sulfuric acid and 50 parts of potassium permanganate carry out mixed acid oxidation, the concentrated sulfuric acid and potassium permanganate are also with improving treatment effeciency, after ultrasonic or high shear vigorous stirring, obtain carboxylated carbon nano-fiber, add surface conditioning agent, 300 DEG C of heat treated 8 minutes, add conductive metal, nitrogen and argon gas mixed gas protected under 500 DEG C of heating 30 minutes, conductive metal is dispersed in carbon nano-fiber;
(3) step (1) pretreated graphite and step (2) pretreated carbon nano-fiber are placed in container, dissolve with 300 parts of polar solvent 1-METHYLPYRROLIDONEs (NMP), add dispersant, conducting polymer, polymer adhesive again, blended with forced mixer, and then carry out ultrasonic disperse with ultrasonic wave separating apparatus, supersonic frequency is 20KHz, time is 1.0 hours, be placed in ozone generating-device again and carry out ozonation treatment, ozonation treatment can promote the hydrophiling on the surface of raw fiber, after grinding, form the solution of homogeneous;
(4) solution step (3) obtained and chemical blend thing carry out chemical blend, described chemical blend thing is polyoxyethylene, the mass fraction of described chemical blend thing accounts for 35% of original solution, nano-sized carbon conductive fiber material is prepared with method of electrostatic spinning, described electrostatic spinning conical pipe sharp-crested diameter used is 1.2mm, conical pipe, from the horizontal by 8 ° of angles, is beneficial to conical pipe sharp-crested drop and is formed, add the electric-field intensity of 1.2kV/cm at solution two ends.
Last it is noted that above embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in previous embodiment, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of embodiment of the present invention technical scheme.
Claims (6)
1. a novel electromagnetic shielding nano-sized carbon conductive fiber material, is characterized in that: component meter comprises following component by weight: 3 ~ 6 parts, graphite, carbon nano-fiber 15 ~ 35 parts, conducting polymer 60 ~ 98 parts, polymer adhesive 0.2 ~ 0.8 part, dispersant 0.5 ~ 1.0 part, alkali metal fluoride 0.02 ~ 0.1 part, metallic catalyst 0.1 ~ 0.2 part, conductive metal 0.03 ~ 0.15 part, surface conditioning agent 0.5 ~ 1.0 part; Described conducting polymer is poly-(indenofluorene-triphenylamine), described polymer adhesive is 1,3-two-(3,3,4,4-di carboxyl phenyloxy) benzene and 4,4-pair-(4-amino-benzene oxygen)-diphenyl combines by 1:2 ~ 3, and described dispersant is 1,2-ethylenebisstearamide, described metallic catalyst is metallocene, and described surface conditioning agent is ITO or SnO
2, described conductive metal comprises the salt of at least one metallic element in barium, silver, cobalt, nickel, tin, metal oxide, metal chloride or metal nitride.
2. a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material as claimed in claim 1, it is characterized in that: the Dispersible X-Ray and the electron beam shielding material that also comprise 0.01 ~ 0.03 part, described material is the compound of at least one element be selected from silicon, strontium, magnesium, europium and dysprosium.
3. the preparation method of a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material as claimed in claim 1, is characterized in that: comprise the following steps:
(1) Graphitic pretreatment, alkali metal fluoride is mixed in Nano graphite powder, and add metallic catalyst, mixing, 500 ~ 700 DEG C of heating under inert gas shielding, described inert gas is one or more mists selected from carbon monoxide, methane, acetylene, ethene and propane, alkali metal fluoride is fixed on Nano graphite powder on the surface;
(2) carbon nano-fiber preliminary treatment, the Nano carbon fibers Wesy concentrated sulfuric acid and potassium permanganate are carried out mixed acid oxidation, after ultrasonic or high shear vigorous stirring, obtain carboxylated carbon nano-fiber, add surface conditioning agent, 200 ~ 300 DEG C of heat treated 5 ~ 8 minutes, add conductive metal, nitrogen and argon gas mixed gas protected under 300 ~ 500 DEG C of heating 20 ~ 30 minutes, conductive metal is dispersed in carbon nano-fiber;
(3) step (1) pretreated graphite and step (2) pretreated carbon nano-fiber are placed in container, dissolve with polar solvent, add dispersant, conducting polymer, polymer adhesive again, blended, ultrasonic disperse, be placed in ozone generating-device again and carry out ozonation treatment, grinding, form the solution of homogeneous;
(4) solution step (3) obtained and chemical blend thing blended, described chemical blend thing is polyoxyethylene, then prepares nano-sized carbon conductive fiber material with method of electrostatic spinning.
4. the preparation method of a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material as claimed in claim 3, it is characterized in that: described concentrated sulfuric acid consumption is 420 ~ 480 parts, potassium permanganate consumption is 10 ~ 50 parts, and described concentrated sulfuric acid concentration is 95 ~ 98%.
5. the preparation method of a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material as claimed in claim 3, is characterized in that: described polar solvent be selected from isopropyl alcohol (IPA), cyclohexanone, ethyl acetate, 1-METHYLPYRROLIDONE (NMP), butyl acetate or methyl iso-butyl ketone (MIBK) any one.
6. its preparation method of a kind of novel electromagnetic shielding nano-sized carbon conductive fiber material as claimed in claim 3, is characterized in that: described alkali metal fluoride is LiF or CsF.
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