CN106835712A - A kind of preparation method of ferrite/polyaniline Electromagnetically shielding fabrics - Google Patents
A kind of preparation method of ferrite/polyaniline Electromagnetically shielding fabrics Download PDFInfo
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- CN106835712A CN106835712A CN201710114082.6A CN201710114082A CN106835712A CN 106835712 A CN106835712 A CN 106835712A CN 201710114082 A CN201710114082 A CN 201710114082A CN 106835712 A CN106835712 A CN 106835712A
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- CN
- China
- Prior art keywords
- ferrite
- polyaniline
- preparation
- fabric
- electromagnetically shielding
- 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.)
- Pending
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- 239000004744 fabric Substances 0.000 title claims abstract description 114
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 66
- 229910000859 α-Fe Inorganic materials 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 29
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 14
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 14
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000005642 Oleic acid Substances 0.000 claims abstract description 14
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 14
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 14
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 23
- 239000003795 chemical substances by application Substances 0.000 claims description 23
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical class CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 11
- 239000003513 alkali Substances 0.000 claims description 10
- 239000003822 epoxy resin Substances 0.000 claims description 9
- 239000000178 monomer Substances 0.000 claims description 9
- 229920000647 polyepoxide Polymers 0.000 claims description 9
- 238000000151 deposition Methods 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 238000007711 solidification Methods 0.000 claims description 7
- 230000008023 solidification Effects 0.000 claims description 7
- 239000003085 diluting agent Substances 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 4
- 239000007848 Bronsted acid Substances 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 150000001298 alcohols Chemical class 0.000 claims description 2
- 150000001412 amines Chemical group 0.000 claims description 2
- 150000008064 anhydrides Chemical class 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 claims description 2
- 239000005077 polysulfide Substances 0.000 claims description 2
- 229920001021 polysulfide Polymers 0.000 claims description 2
- 150000008117 polysulfides Polymers 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- 229920003002 synthetic resin Polymers 0.000 claims description 2
- 239000000057 synthetic resin Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 7
- 239000002184 metal Substances 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 5
- 150000002739 metals Chemical class 0.000 abstract description 3
- 238000006116 polymerization reaction Methods 0.000 abstract description 3
- 239000011358 absorbing material Substances 0.000 abstract description 2
- 239000002322 conducting polymer Substances 0.000 abstract description 2
- 229920001940 conductive polymer Polymers 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 230000007812 deficiency Effects 0.000 abstract description 2
- 239000007791 liquid phase Substances 0.000 abstract 1
- 229910003264 NiFe2O4 Inorganic materials 0.000 description 12
- NQNBVCBUOCNRFZ-UHFFFAOYSA-N nickel ferrite Chemical compound [Ni]=O.O=[Fe]O[Fe]=O NQNBVCBUOCNRFZ-UHFFFAOYSA-N 0.000 description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- 238000000576 coating method Methods 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000001291 vacuum drying Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 8
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 7
- 239000002585 base Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- 239000004952 Polyamide Substances 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000013019 agitation Methods 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 description 5
- 239000012065 filter cake Substances 0.000 description 5
- 239000012530 fluid Substances 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- 239000004642 Polyimide Substances 0.000 description 4
- 230000005670 electromagnetic radiation Effects 0.000 description 4
- 229920002647 polyamide Polymers 0.000 description 4
- 229920001721 polyimide Polymers 0.000 description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910000570 Cupronickel Inorganic materials 0.000 description 1
- 229920000914 Metallic fiber Polymers 0.000 description 1
- -1 PTT compound Chemical class 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- YOCUPQPZWBBYIX-UHFFFAOYSA-N copper nickel Chemical compound [Ni].[Cu] YOCUPQPZWBBYIX-UHFFFAOYSA-N 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000007903 penetration ability Effects 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/61—Polyamines polyimines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
-
- 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
- D06M11/32—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—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 oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
-
- 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/55—Epoxy resins
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The present invention relates to a kind of preparation method of ferrite/polyaniline Electromagnetically shielding fabrics, including:Polyaniline is deposited in fabric face first by the way of liquid phase in-situ polymerization, the ferrite that oleic acid is modified is combined with polyaniline/fabric by resinous coat method then.It is main absorbing material that the present invention uses magnetic Jie type ferrite and electric Jie's type polyaniline, and prepared ferrite/polyaniline compound fabric mainly absorbs spatial electromagnetic ripple by two kinds of forms of magnetic loss and electrical loss, reduces secondary pollution of the electromagnetic wave to environment;The method prepare loomage shield effectiveness is high, good stability, water-fastness, while breaching the deficiency of conventional metals type shielding fabric, also compensate for the single conducting polymer type shielding fabric shielding defect that wave band is narrow, shield effectiveness is low.
Description
Technical field
The invention belongs to be electromagnetically shielded field, the preparation side of more particularly to a kind of ferrite/polyaniline Electromagnetically shielding fabrics
Method.
Background technology
With the extensive use of radiotechnics, electromagnetic radiation has turned into after noise pollution, air pollution, water pollution
The fourth-largest public hazards.Electromagnetic radiation can not only disturb the normal operation of various electronic equipments, and to the healthy with very of people
Big harm, is called " invisible killer ".Additionally, coming out one after another with New Type Radar Detection Techniques and precision guided weapon, generation
The possibility that the military defense system and aircraft of various countries of boundary are detected by enemy, track and attacked is increasing, military target
The penetration ability of survival ability and armament systems receives serious threat.Therefore, electromagnetic shielding material is reducing electromagnetic radiation
Pollute, protect health and prevent the application in information leakage from causing increasing concern, in civil and military neck
Domain is respectively provided with wide application prospect.
Electromagnetically shielding fabrics are the important ways for protecting human body from hazards of electromagnetic radiation.The electromagnetism for occurring in the market
Loomage is mainly by techniques such as conductive metallic fiber blending, fabric face metal-plated, metal coating and vulcanization copper coatings
It is obtained.For example:Application number 200410024079.8 is by using conventional plating techniques in fabric face continuous electroplating metallic nickel, copper
And silver, so as to be prepared for the Electromagnetically shielding fabrics that a kind of shield effectiveness is good, electric conductivity is high;The disclosure of application number 201310014809.5
A kind of preparation method of silver-bearing copper nickel composite metal fabric, its technique is to carry out that plasma is silver-plated successively in fabric face, change
Copper facing and electronickelling are learned, so as to prepare a kind of high-performance electromagnetic shield fabric, its electromagnet shield effect is reached on 75dB.With
Electromagnetically shielding fabrics shield effectiveness prepared by top method is high, good conductivity, but it is complicated to there is preparation technology, expensive, metal
It is perishable, it is oxidizable, crock fastness and washing fastness difference the problems such as;In addition, it is mainly by the reflection of fabric face metal level
Loss reaches shield effectiveness high, can not effectively reduce the electromagnetic wave quantity of local space, causes secondary pollution.
In recent years, electrically conductive polyaniline (Polyaniline, PANI) is because its is convieniently synthesized, good stability, electrical conductivity are easily adjusted
The advantages of, show wide application prospect in electromagnetic shielding and field of microwave absorption.Application number 201510222706.7 is first
Amino is introduced on fabric base by plasma etching activation, aniline monomer is then grafted to fabric face, then lead to
Cross situ aggregation method and a kind of Electromagnetically shielding fabrics be obtained, its can effective electromagnetic wave absorption radiation, in below 10MHz low-frequency ranges
Shield effectiveness reach 18dB;But loomage prepared by the method is present, and shielding mechanism is single, frequency range is narrow for shielding, shield effectiveness
Low problem.Application number 201410245742.0 discloses a kind of preparation method for inhaling wave mode Electromagnetically shielding fabrics, and its technique is
First in PTT fabric face in-situ polymerization PANI, then carry out activating-being sensitized operation, and then trigger chemical nickel plating, it is prepared
Ni/PANI/PTT compound fabrics have widened shielding frequency band range based on absorption loss shielding mechanism, reduce secondary pollution;But
Compound fabric water-wash resistance prepared by the method is poor, and crock fastness is low, and in addition with precious metal palladium as active centre, price is held high
It is expensive, and reclaim difficult.
The content of the invention
The technical problems to be solved by the invention are to overcome existing loomage preparation technology complicated, involve great expense and shield
The main problem based on reflection loss of mechanism, there is provided a kind of preparation method of ferrite/polyaniline Electromagnetically shielding fabrics, the party
Method is simple, mild condition, and compared with conventional metals coating process low cost, and the Electromagnetically shielding fabrics for preparing are main with absorption
Based on loss, bandwidth is shielded, shield effectiveness is good.
A kind of preparation method of ferrite/polyaniline Electromagnetically shielding fabrics of the invention, including:
(1) fabric is carried out into alkali process, is subsequently dipped in the acid solution containing aniline monomer, fabric face is fully adsorbed
Aniline monomer, is subsequently adding the acid ammonium persulfate solution with the acid solution same volume containing aniline monomer, be stirred at room temperature into
Row in-situ chemical polymerisation, reaction is cleaned after terminating, dried, and obtaining final product surface deposition has the fabric of polyaniline;
(2) ferrite is carried out into oleic acid to be modified, then modified ferrite is placed in epoxy resin, add diluent
And curing agent, ultrasonic disperse obtains resin finishing agent, and above-mentioned surface is deposited with resin finishing agent then the fabric of polyaniline
Top finish is carried out, final curing, drying obtain final product ferrite/polyaniline Electromagnetically shielding fabrics;Wherein, the group of resin finishing agent
Turn into:Modified ferrite 1.2-8.4g, epoxy resin 10-12g, diluent 1-2.4g, curing agent 1-2.4g.
Alkali process in the step (1) are processed using NaOH, and specific process parameter is:Naoh concentration
10-15g/L, bath raio 1:25-50,40-80 DEG C of its alkali purification temp, alkali process time 10-30min;Alkali process terminate after in 60-80
Dried in DEG C baking oven.
Concentration of aniline 0.25-0.5mol/L, proton acid concentration in the acid solution containing aniline monomer in the step (1)
0.5-1mol/L。
Ammonium persulfate concentrations 0.25-0.5mol/L, proton acid concentration in acid ammonium persulfate solution in the step (1)
0.5-1mol/L。
The Bronsted acid is hydrochloric acid, nitric acid, sulfuric acid or DBSA.
The time of fabric acid solution of the immersion containing aniline monomer in the step (1) is 30-60min;In-situ chemical
Polymerization reaction time is 2-6 hours.
Ferrite in the step (2) is ferrite, strontium ferrite, barium ferrite or Conjugate ferrite.
Oleic acid in the step (2) is modified specially:1-6g ferrites are placed in 60-360ml aqueous isopropanols, ultrasound
10-30min, is subsequently adding 2-12ml oleic acid, and 2-4h, 60-90 DEG C of drying temperature, drying are stirred under 50-60 DEG C of water bath condition
Time 3-5h.
Diluent in the step (2) is alcohols, ketone or aromatic hydrocarbons;Curing agent is amine, anhydrides, synthetic resin
Class or polysulfide rubber class.
Ultrasonic disperse 1-2h in the step (2);20-40 DEG C of solidification temperature, hardening time 12-48h.
The present invention deposits polyaniline (technological process is as shown in Figure 1) using situ aggregation method in fabric face first, is obtained
Polyaniline/fabric with satisfactory electrical conductivity;Then ferrite and resin are improved by oleic acid modified (mechanism is as shown in Figure 2)
Between compatibility;Modified ferrite and polyaniline/fabric are combined using resinous coat technique finally and obtain ferrite/polyaniline
Loomage.Gained compound fabric breaches the deficiency of conventional metals type shielding fabric, also compensate for single conducting polymer species
Loomage shielding wave band is narrow, the low defect of shield effectiveness, and good stability, water-fastness.
Beneficial effect
It is main absorbing material that the present invention uses magnetic Jie type ferrite and electric Jie's type polyaniline, and preparation is with absorption loss
It is the loomage of main shielding mechanism, it mainly absorbs spatial electromagnetic ripple by two kinds of forms of magnetic loss and electrical loss, reduces
Secondary pollution of the electromagnetic wave to environment;In addition, electrically conductive polyaniline raw material be easy to get, convieniently synthesized, good conductivity, environmental stability
Height, and ferrite magnetic conductance is high, absorptivity is high, ferrite/polyaniline compound fabric has higher as a kind of shielding material
Shield effectiveness and screening frequencies scope wider;And preparation process is simple, reduces using the cost of noble metal, with good
Application prospect.
Brief description of the drawings
Fig. 1 is process chart of the invention;
Fig. 2 is the modified ferrite schematic diagram of oleic acid in the present invention.
Specific embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content for having read instruction of the present invention, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
In the embodiment of the present invention, polyimides (Polyimide, the PI) fabric for using is purchased from Jiangsu god's new material share difficult to understand
Co., Ltd, nanometer Ni ferrite (NiFe used2O4) it is purchased from Nanjing Ai Purui nano materials Co., Ltd.All reagents are equal
It is that analysis is pure, in use without further purifying.
Embodiment 1
It is base material to use polyimides fabric (PI), prepares NiFe2O4/ PANI/PI Electromagnetically shielding fabrics, specific steps are such as
Under:
(1) fabric pretreatment
A. 10 × 10cm PI fabrics are taken;
B. polyimides fabric is placed in 10g/L sodium hydroxide solutions, bath raio 1:50, processed under 60 DEG C of water bath conditions
20min, fully washs after taking-up PI fabrics and with deionized water, is dried in 60 DEG C of baking ovens;
(2) polyaniline deposition
A. the PI fabrics of above-mentioned pretreatment are immersed into aniline containing 0.5mol/L and 1mol/L HNO3In solution, it is stored at room temperature
30min;
B. same volume ammonium persulfate containing 0.5mol/L and 1mol/L HNO are added3Solution, is stirred at room temperature, and reacts 4h, takes
It is colourless to go out fabric and cleaned with deionized water to cleaning fluid, and room temperature is dried, and obtains PANI/PI fabrics;
(3) ferrite is modified
A. 2g Ni ferrites (NiFe is taken2O4) be placed in 120ml isopropanols, ultrasonic disperse 20min, 4ml oleic acid is added,
Mechanical agitation 2h under 60 DEG C of water bath conditions;
B. suction filtration, filter cake is cleaned three times using isopropanol, is subsequently placed in 90 DEG C of vacuum drying ovens and is dried 3h;
(4) resinous coat
A. the above-mentioned modified ferrites of 1.2g are taken to insert in 10g E51 epoxy resin, and adds 1g absolute ethyl alcohols and 1g 650
Polyamide, ultrasonic disperse 2h is obtained containing 10% modified ferritic coating finishing agent;
B. above-mentioned finishing agent is carried out into top finish to PANI/PI fabrics, is placed in 40 DEG C of vacuum drying oven solidification 24h, obtained
NiFe2O4/ PANI/PI composite shielding fabrics.
Embodiment 2
It is base material to use PI fabrics, prepares NiFe2O4/ PANI/PI Electromagnetically shielding fabrics, comprise the following steps that:
(1) fabric pretreatment
A. 10cm × 10cm PI fabrics are taken;
B. PI fabrics are placed in 10g/L sodium hydroxide solutions, bath raio 1:50,20min is processed under 60 DEG C of water bath conditions, take
Go out after PI fabrics and fully washed with deionized water, dried in 60 DEG C of baking ovens;
(2) polyaniline deposition
A. the PI fabrics of above-mentioned pretreatment are immersed into aniline containing 0.5mol/L and 1mol/L HNO3In solution, it is stored at room temperature
30min;
B. same volume ammonium persulfate containing 0.5mol/L and 1mol/L HNO are added3Solution, is stirred at room temperature, and reacts 4h, takes
It is colourless to go out fabric and cleaned with deionized water to cleaning fluid, and room temperature is dried, and obtains PANI/PI fabrics;
(3) ferrite is modified
A. 3g Ni ferrites (NiFe is taken2O4) be placed in 180ml isopropanols, ultrasonic disperse 20min, 6ml oleic acid is added,
Mechanical agitation 2h under 60 DEG C of water bath conditions;
B. suction filtration, filter cake is cleaned three times using isopropanol, is subsequently placed in 90 DEG C of vacuum drying ovens and is dried 3h;
(4) resinous coat
A. the above-mentioned modified ferrites of 2.4g are taken to insert in 10g E51 epoxy resin, and adds 1g absolute ethyl alcohols and 1g 650
Polyamide, ultrasonic disperse 2h is obtained containing 20% modified ferritic coating finishing agent;
B. above-mentioned finishing agent is carried out into top finish to PANI/PI fabrics, is placed in 40 DEG C of vacuum drying oven solidification 24h, obtained
NiFe2O4/ PANI/PI composite shielding fabrics.
Embodiment 3
It is base material to use PI fabrics, prepares NiFe2O4/ PANI/PI Electromagnetically shielding fabrics, comprise the following steps that:(1) fabric
In advance
Treatment
A. 10cm × 10cm PI fabrics are taken;
B. PI fabrics are placed in 10g/L sodium hydroxide solutions, bath raio 1:50,20min is processed under 60 DEG C of water bath conditions, take
Go out after PI fabrics and fully washed with deionized water, dried in 60 DEG C of baking ovens;
(2) polyaniline deposition
A. the PI fabrics of above-mentioned pretreatment are immersed into aniline containing 0.5mol/L and 1mol/L HNO3In solution, it is stored at room temperature
30min;
B. same volume ammonium persulfate containing 0.5mol/L and 1mol/L HNO are added3Solution, is stirred at room temperature, and reacts 4h, takes
It is colourless to go out fabric and cleaned with deionized water to cleaning fluid, and room temperature is dried, and obtains PANI/PI fabrics;
(3) ferrite is modified
A. 4g Ni ferrites (NiFe is taken2O4) be placed in 240ml isopropanols, ultrasonic disperse 20min, 8ml oleic acid is added,
Mechanical agitation 2h under 60 DEG C of water bath conditions;
B. suction filtration, filter cake is cleaned three times using isopropanol, is subsequently placed in 90 DEG C of vacuum drying ovens and is dried 3h;
(4) resinous coat
A. the above-mentioned modified ferrites of 3.6g are taken to insert in 10g E51 epoxy resin, and adds 1g absolute ethyl alcohols and 1g 650
Polyamide, ultrasonic disperse 2h is obtained containing 30% modified ferritic coating finishing agent;
B. above-mentioned finishing agent is carried out into top finish to PANI/PI fabrics, is placed in 40 DEG C of vacuum drying oven solidification 24h, obtained
NiFe2O4/ PANI/PI composite shielding fabrics.
Embodiment 4
It is base material to use PI fabrics, prepares NiFe2O4/ PANI/PI Electromagnetically shielding fabrics, comprise the following steps that:(1) fabric
Pretreatment
A. 10cm × 10cm PI fabrics are taken;
B. PI fabrics are placed in 10g/L sodium hydroxide solutions, bath raio 1:50,20min is processed under 60 DEG C of water bath conditions, take
Go out after PI fabrics and fully washed with deionized water, dried in 60 DEG C of baking ovens;
(2) polyaniline deposition
A. the PI fabrics of above-mentioned pretreatment are immersed into aniline containing 0.5mol/L and 1mol/L HNO3In solution, it is stored at room temperature
30min;
B. same volume ammonium persulfate containing 0.5mol/L and 1mol/L HNO are added3Solution, is stirred at room temperature, and reacts 4h, takes
It is colourless to go out fabric and cleaned with deionized water to cleaning fluid, and room temperature is dried, and obtains PANI/PI fabrics;
(3) ferrite is modified
A. 5g Ni ferrites (NiFe is taken2O4) be placed in 300ml isopropanols, ultrasonic disperse 20min, 10ml oleic acid is added,
Mechanical agitation 2h under 60 DEG C of water bath conditions;
B. suction filtration, filter cake is cleaned three times using isopropanol, is subsequently placed in 90 DEG C of vacuum drying ovens and is dried 3h;
(4) resinous coat
A. the above-mentioned modified ferrites of 4.8g are taken to insert in 10g E51 epoxy resin, and adds 1g absolute ethyl alcohols and 1g 650
Polyamide, ultrasonic disperse 2h is obtained containing 40% modified ferritic coating finishing agent;
B. above-mentioned finishing agent is carried out into top finish to PANI/PI fabrics, is placed in 40 DEG C of vacuum drying oven solidification 24h, obtained
NiFe2O4/ PANI/PI composite shielding fabrics.
Embodiment 5
It is base material to use PI fabrics, prepares NiFe2O4/ PANI/PI Electromagnetically shielding fabrics, comprise the following steps that:(1) fabric
Pretreatment
A. 10 × 10cm PI fabrics are taken;
B. PI fabrics are placed in 10g/L sodium hydroxide solutions, bath raio 1:50,20min is processed under 60 DEG C of water bath conditions, take
Go out after PI fabrics and fully washed with deionized water, dried in 60 DEG C of baking ovens;
(2) polyaniline deposition
A. the PI fabrics of above-mentioned pretreatment are immersed into aniline containing 0.5mol/L and 1mol/L HNO3In solution, it is stored at room temperature
30min;
B. same volume ammonium persulfate containing 0.5mol/L and 1mol/L HNO are added3Solution, is stirred at room temperature, and reacts 4h, takes
It is colourless to go out fabric and cleaned with deionized water to cleaning fluid, and room temperature is dried, and obtains PANI/PI fabrics;
(3) ferrite is modified
A. 6g Ni ferrites (NiFe is taken2O4) be placed in 360ml isopropanols, ultrasonic disperse 20min, 12ml oleic acid is added,
Mechanical agitation 2h under 60 DEG C of water bath conditions;
B. suction filtration, filter cake is cleaned three times using isopropanol, is subsequently placed in 90 DEG C of vacuum drying ovens and is dried 3h;
(4) resinous coat
A. the above-mentioned modified ferrites of 6g are taken to insert in 10g E51 epoxy resin, and adds 1g absolute ethyl alcohols and 1g 650 poly-
Amide resin, ultrasonic disperse 2h is obtained containing 50% modified ferritic coating finishing agent;
B. above-mentioned finishing agent is carried out into top finish to PANI/PI fabrics, is placed in 40 DEG C of vacuum drying oven solidification 24h, obtained
NiFe2O4/ PANI/PI composite shielding fabrics.
According to GB/T25471《The shield effectiveness measuring method of electromagnetic screen coating》And SJ204524《Materials ' Shielding Effectiveness
Measuring method》PANI/PI compound fabrics prepared in testing example 1-5 and NiFe2O4The screen of/PANI/PI loomages
Efficiency is covered, as a result as shown in table 1:
The fabric electromagnet shield effect of table 1
As shown in Table 1, after being arranged through the method, fabric has preferable shield effectiveness.It is prepared in embodiment 1-5
NiFe2O4/ PANI/PI loomages reach more than 6.24dB at 50MHz to electromagnetic shielding effectiveness, and with electromagnetic wave
The raising of frequency, shield effectiveness increased;In addition, with NiFe in coating finishing agent2O4The raising of content, shield effectiveness increases
Plus, and increase at low frequency 50MHz the most obvious.
Claims (10)
1. the preparation method of a kind of ferrite/polyaniline Electromagnetically shielding fabrics, including:
(1) fabric is carried out into alkali process, is subsequently dipped in the acid solution containing aniline monomer, be subsequently adding the acidity of same volume
Ammonium persulfate solution, being stirred at room temperature carries out in-situ chemical polymerisation, and reaction is cleaned after terminating, dried, and obtaining final product surface deposition has
The fabric of polyaniline;
(2) ferrite is carried out into oleic acid to be modified, then modified ferrite is placed in epoxy resin, added diluent and consolidate
Agent, ultrasonic disperse obtains resin finishing agent, and then depositing the fabric for having polyaniline to above-mentioned surface with resin finishing agent is carried out
Top finish, final curing, drying obtain final product ferrite/polyaniline Electromagnetically shielding fabrics;Wherein, the composition of resin finishing agent is:
Modified ferrite 1.2-8.4g, epoxy resin 10-12g, diluent 1-2.4g, curing agent 1-2.4g.
2. the preparation method of a kind of ferrite/polyaniline Electromagnetically shielding fabrics according to claim 1, it is characterised in that:
Alkali process in the step (1) are processed using NaOH, and specific process parameter is:Naoh concentration 10-15g/
L, bath raio 1:25-50,40-80 DEG C of its alkali purification temp, alkali process time 10-30min;Alkali process terminate after in 60-80 DEG C of baking oven
Middle drying.
3. the preparation method of a kind of ferrite/polyaniline Electromagnetically shielding fabrics according to claim 1, it is characterised in that:
Concentration of aniline 0.25-0.5mol/L, proton acid concentration 0.5- in the acid solution containing aniline monomer in the step (1)
1mol/L。
4. the preparation method of a kind of ferrite/polyaniline Electromagnetically shielding fabrics according to claim 1, it is characterised in that:
Ammonium persulfate concentrations 0.25-0.5mol/L, proton acid concentration 0.5- in acid ammonium persulfate solution in the step (1)
1mol/L。
5. a kind of preparation method of ferrite/polyaniline Electromagnetically shielding fabrics according to claim 3 or 4, its feature exists
In:The Bronsted acid is hydrochloric acid, nitric acid, sulfuric acid or DBSA.
6. the preparation method of a kind of ferrite/polyaniline Electromagnetically shielding fabrics according to claim 1, it is characterised in that:
The time of fabric acid solution of the immersion containing aniline monomer in the step (1) is 30-60min;In-situ chemical polymerisation
Time is 2-6 hours.
7. the preparation method of a kind of ferrite/polyaniline Electromagnetically shielding fabrics according to claim 1, it is characterised in that:
Ferrite in the step (2) is ferrite, strontium ferrite, barium ferrite or Conjugate ferrite.
8. the preparation method of a kind of ferrite/polyaniline Electromagnetically shielding fabrics according to claim 1, it is characterised in that:
Oleic acid in the step (2) is modified specially:1-6g ferrites are placed in 60-360ml aqueous isopropanols, ultrasonic 10-
30min, is subsequently adding 2-12ml oleic acid, and 2-4h, 60-90 DEG C of drying temperature, drying time are stirred under 50-60 DEG C of water bath condition
3-5h。
9. the preparation method of a kind of ferrite/polyaniline Electromagnetically shielding fabrics according to claim 1, it is characterised in that:
Diluent in the step (2) is alcohols, ketone or aromatic hydrocarbons;Curing agent is amine, anhydrides, synthetic resin or polysulfide
Rubber-like.
10. the preparation method of a kind of ferrite/polyaniline Electromagnetically shielding fabrics according to claim 1, it is characterised in that:
Ultrasonic disperse 1-2h in the step (2);20-40 DEG C of solidification temperature, hardening time 12-48h.
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CN110359294A (en) * | 2019-07-18 | 2019-10-22 | 上海工程技术大学 | A method of improving copper cobalt nickel ferrite compound binding strength on cotton fabric |
CN110846881A (en) * | 2019-11-26 | 2020-02-28 | 东华大学 | Co3O4Preparation method of/PANI/MXene/PI electromagnetic shielding fabric |
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