CN111270513A - Preparation method of ferroferric oxide/copper sulfide composite electromagnetic shielding fabric - Google Patents

Preparation method of ferroferric oxide/copper sulfide composite electromagnetic shielding fabric Download PDF

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CN111270513A
CN111270513A CN202010331095.0A CN202010331095A CN111270513A CN 111270513 A CN111270513 A CN 111270513A CN 202010331095 A CN202010331095 A CN 202010331095A CN 111270513 A CN111270513 A CN 111270513A
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fabric
ferroferric oxide
polyacrylonitrile
electromagnetic shielding
copper sulfide
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CN111270513B (en
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潘玮
王艳芝
刘忠柱
王坤
李英华
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Zhongyuan University of Technology
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    • 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
    • D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
    • D06M11/53—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 sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
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    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0043—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers
    • D06N3/0052—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by their foraminous structure; Characteristics of the foamed layer or of cellular layers obtained by leaching out of a compound, e.g. water soluble salts, fibres or fillers; obtained by freezing or sublimation; obtained by eliminating drops of sublimable fluid
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    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/0056—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the compounding ingredients of the macro-molecular coating
    • D06N3/0063—Inorganic compounding ingredients, e.g. metals, carbon fibres, Na2CO3, metal layers; Post-treatment with inorganic compounds
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    • D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
    • D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
    • D06N3/04—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06N3/042—Acrylic polymers
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    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
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    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
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    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
    • D06M2101/28—Acrylonitrile; Methacrylonitrile
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    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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  • Electromagnetism (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)

Abstract

The invention relates to the field of electromagnetic shielding materials, in particular to a preparation method of a ferroferric oxide/copper sulfide composite electromagnetic shielding fabric. The invention firstly uses nano ferroferric oxide/polyacrylonitrile blended solution to coat the acrylic fiber blended fabric, uses water as a coagulating bath, and solvent molecules and non-solvent molecules are subjected to double diffusion in the coagulating bath to be coagulated to form a nano ferroferric oxide/polyacrylonitrile coating, and on the basis, copper sulfide is deposited by adopting a chemical reaction method to prepare the composite electromagnetic shielding fabric. The polyethylene glycol 200 in the coating liquid plays a role of a pore-forming agent in the coating forming process, so that the coating has a continuously distributed reticular pore structure, and the copper sulfide is deposited on the surface of the flexible film and grows in the flexible film, so that the formed copper sulfide can cover the surface of the flexible substrate film and penetrates through the interior of the film, the effective load of the copper sulfide is really completed, and the composite material has excellent electromagnetic shielding performance.

Description

Preparation method of ferroferric oxide/copper sulfide composite electromagnetic shielding fabric
Technical Field
The invention relates to the field of electromagnetic shielding materials, in particular to a preparation method of a ferroferric oxide/copper sulfide composite electromagnetic shielding fabric.
Background
With the development of modern science and technology and the progress of industrial civilization, the application of various electronic instruments and equipment is increased day by day, more and more electromagnetic radiation is generated, the electromagnetic interference caused by the electromagnetic radiation is serious day by day, and the electromagnetic interference becomes a main obstacle whether a plurality of equipment can play a role or not; meanwhile, electromagnetic pollution has permeated into the aspects of production and life, and the health of people is seriously influenced. Therefore, how to effectively prevent and eliminate electromagnetic interference has become an important issue in the scientific and technological field.
The conventional electromagnetic shielding fabric can be classified into a metal-plated fabric, a surface-coated fabric, a metal foil-attached fabric, a conductive fiber blended fabric, and the like. The gold-plated coated fabric has the problems of poor binding force between metal and the fabric, easy shedding, easy scraping and loss of shielding performance of a plating layer, serious pollution in the preparation process and the like, and is not widely applied in the electromagnetic shielding field at present, while the metal fiber blended fabric also has the problems of easy winding, easy breakage of metal fiber, low production efficiency, high production cost and the like in the weaving process, and the shielding performance of the product produced by the method is relatively poor. Therefore, the exploration of the efficient electromagnetic shielding material, especially the flexible electromagnetic shielding fabric, has very important significance for preventing electromagnetic interference caused by electromagnetic waves, improving the safety reliability and personal safety of electronic products, ammunition, fuzes, precise electronic weapon equipment and the like.
The novel electromagnetic shielding fabric material is developed towards the wave-absorbing fabric material, and the shielding fabric material is required to have the characteristics of thinness, lightness, width and strength. The metal sulfide has special performance in the aspects of optics, photoelectrochemistry, catalysis, environmental protection and the like. They have good chemical and thermal stability and are good photoelectric materials. The method for producing the flexible polymer composite conductive material by utilizing the characteristics of the metal sulfide is mostly a polymer surface chemical reaction method which is mainly used for generating adsorption on the surface of the fiber through chemical treatment, namely, by dipping reaction liquid, and then covering the surface of the high polymer material with the metal sulfide through chemical reaction. The method has the advantages of simple process, low cost, less damage to the strength, softness, smoothness and the like of the fabric, but the fabric prepared by the method has poor electromagnetic shielding performance. The nano ferroferric oxide has excellent superparamagnetic property and good surface stability, so that the nano ferroferric oxide has wide prospects in the fields of electromagnetic shielding, immunomagnetic beads, controlled drug release and the like.
A great deal of research shows that a single electromagnetic shielding material is difficult to meet the use requirements, so that two or more materials are required to be used in a composite manner. Patent CN201010620154.2 discloses a fabric coating finishing agent with electromagnetic shielding function and a preparation method thereof, the patent adopts an in-situ chemical method to prepare a nano ferroferric oxide/polypyrrole composite material on the surface of a fabric, and provides an inorganic-organic composite coating finishing agent.
Disclosure of Invention
The invention provides a preparation method of a ferroferric oxide/copper sulfide composite electromagnetic shielding fabric, aiming at improving the electromagnetic shielding performance of a coated fabric, and the method is simple and easy to implement.
The technical scheme of the invention is realized as follows:
a preparation method of ferroferric oxide/copper sulfide composite electromagnetic shielding fabric comprises the following steps:
(1) putting polyacrylonitrile powder into a mixed solvent, and stirring for 2-3h at 60-80 ℃ to completely dissolve polyacrylonitrile to obtain a polyacrylonitrile solution;
(2) adding nano ferroferric oxide and a silane coupling agent into the polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic treatment for 60-120min to obtain a ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain a coating solution;
(3) uniformly coating the coating solution obtained in the step (2) on the acrylic fiber blended fabric, then immersing the acrylic fiber blended fabric with the coating solution in deionized water at the temperature of 20-40 ℃, and staying in the deionized water for 0.5-2 hours to obtain the acrylic fiber blended fabric taking nano ferroferric oxide and polyacrylonitrile as a coating;
(4) and (3) immersing the acrylic fiber blended fabric taking the nano ferroferric oxide and polyacrylonitrile as the coating obtained in the step (3) into a copper sulfate pentahydrate aqueous solution, soaking for 5-30 minutes at 10-40 ℃, adding a sodium thiosulfate aqueous solution, heating to 75-95 ℃, reacting for 0.5-4 hours, taking out the fabric, rinsing with water, and drying to obtain the electromagnetic shielding fabric.
The mixed solvent in the step (1) is polyethylene glycol 200 and dimethyl sulfoxide according to the mass ratio of (3-15): (85-97), and the mass of the polyacrylonitrile powder is 5-10% of that of the mixed solvent.
The mass ratio of the nano ferroferric oxide to the silane coupling agent to the polyacrylonitrile solution in the step (2) is (1-5): (0.1-0.5): (90-120).
The silane coupling agent is any one of KH-570, KH-550 or KH-560, and the size of the nano ferroferric oxide is 20-100 nm.
The acrylic fiber blended fabric in the step (3) is a nitrile-polyester blended fabric, a nitrile-viscose blended fabric or a nitrile-cotton blended fabric, wherein the acrylic fiber accounts for 40-60 wt%, and other fibers account for 40-60 wt%.
In the step (4), the mass concentration of the copper sulfate pentahydrate aqueous solution is 2-8% by weight, and the mass concentration of the sodium thiosulfate aqueous solution is 2-8% by weight.
The invention has the beneficial effects that:
(1) the invention firstly uses nano ferroferric oxide/polyacrylonitrile blended solution to coat the acrylic fiber blended fabric, uses water as a coagulating bath, and solvent molecules and non-solvent molecules are subjected to double diffusion in the coagulating bath to be coagulated to form a nano ferroferric oxide/polyacrylonitrile coating, and on the basis, copper sulfide is deposited by adopting a chemical reaction method to prepare the composite electromagnetic shielding fabric. The polyethylene glycol 200 in the coating liquid plays a role of a pore-forming agent in the coating forming process, so that the coating has a continuously distributed reticular pore structure shown in figure 2b, copper sulfide is deposited on the surface of the flexible film and grows in the flexible film, the formed copper sulfide can cover the surface of the flexible substrate film shown in figure 2c and penetrates into the flexible substrate film, the effective load of the copper sulfide is really completed, and the composite material has excellent electromagnetic shielding performance.
(2) The nano ferroferric oxide and copper sulfide particles are fillers of different types, and are mutually dispersed in gaps in a matrix, so that the filling factor of the fillers can be increased, more conductive path networks are formed as shown in figure 2b, the resistance is reduced, and the composite material with better electromagnetic shielding performance is obtained.
(3) The preparation method has the advantages of easily controlled conditions, simple operation, low raw material cost and low energy consumption, and is suitable for large-scale industrial production. Because polyacrylonitrile in the coating liquid is used as the same substance as acrylon in the matrix fabric, compared with other products, the electromagnetic shielding composite material prepared by the invention has the advantages that the adhesive force between the conductive layer and the matrix is obviously improved, the conductive layer is more compact, and the abrasion resistance and the solvent resistance are outstanding; the product has good electromagnetic shielding property and flexibility, and the surface resistance of the product is sensitive to the change of environment such as pressure, elasticity and the like, so the product can be widely applied to the fields of sensors, static prevention, electromagnetic shielding and the like.
Drawings
Fig. 1 shows a process for preparing an electromagnetic shielding fabric according to the present invention.
FIG. 2 is a comparison scanning electron microscope image of the original fabric, the coated fabric and the fabric after chemical deposition in example 1 of the present application, wherein a is the original fabric, b is the coated fabric and c is the fabric after chemical deposition.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to the embodiment is shown in the schematic diagram of the preparation process in fig. 1, and the preparation steps are as follows:
(1) 15 g of polyacrylonitrile powder is put into a mixed solvent composed of 170 g of dimethyl sulfoxide and 30 g of polyethylene glycol 200, and stirred for 2.5 hours at 70 ℃ to completely dissolve polyacrylonitrile, so that a polyacrylonitrile solution is obtained.
(2) Adding 2.5 g of nano ferroferric oxide and 0.3 g of silane coupling agent KH-550 into 95 g of polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic dispersion for 120min to obtain nano ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain the coating solution.
(3) And (3) uniformly coating the coating solution obtained in the step (2) on acrylic and polyester (acrylic fiber 50% and polyester 50%) blended fabric, immersing the acrylic blended fabric with the coating solution in deionized water at 20 ℃, staying in the deionized water for 1 hour to obtain the acrylic blended fabric taking nano ferroferric oxide and polyacrylonitrile as a coating, wherein polyethylene glycol 200 in the coating solution plays a role of a pore-making agent in the coating forming process, so that the coating has a continuously distributed reticular pore structure shown in figure 2 b.
(4) And (3) taking 10 g of the nitrile-polyester blended fabric which is obtained in the step (3) and takes the nano ferroferric oxide and the polyacrylonitrile as coatings, immersing the fabric into 50 g of a 5% copper sulfate pentahydrate aqueous solution, after immersing the fabric for 30 minutes at 30 ℃, adding 50 g of a 5% sodium thiosulfate aqueous solution, heating the fabric to 95 ℃ for reaction for 0.5 hour, taking out the blended film, rinsing the blended film with water, and drying the rinsed film to obtain the acrylic fiber blended electromagnetic shielding fabric, wherein copper sulfide is deposited on the surface of the flexible film and grows in the flexible film, so that the formed copper sulfide can cover the surface of the flexible substrate film as shown in figure 2c and penetrates into the interior of the flexible substrate film, the effective load of the copper sulfide is really completed, and the composite material has excellent electromagnetic shielding performance. The ferroferric oxide/copper sulfide composite electromagnetic shielding fabric prepared by the embodiment has the shielding effectiveness of 45dB within the range of 80MHz-6 GHz.
Example 2
The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to the embodiment is as shown in fig. 1, and comprises the following steps:
(1) 20 g of polyacrylonitrile powder is put into a mixed solvent composed of 185 g of dimethyl sulfoxide and 15 g of polyethylene glycol 200, and stirred for 3 hours at 72 ℃ to completely dissolve polyacrylonitrile, so that a polyacrylonitrile solution is obtained.
(2) And (2) adding 5 g of nano ferroferric oxide and 0.5 g of silane coupling agent KH-550 into 110 g of polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic dispersion for 90min to obtain nano ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain the coating solution.
(3) And (3) uniformly coating the coating solution obtained in the step (2) on acrylic cotton (acrylic fiber 40% and cotton 60%) blended fabric, immersing the acrylic fiber blended fabric with the coating solution in deionized water at 25 ℃, and staying in the deionized water for 1 hour to obtain the acrylic fiber blended fabric taking nano ferroferric oxide and polyacrylonitrile as coatings.
(4) And (3) taking 10 g of the acrylic and polyester blended fabric which is obtained in the step (3) and takes the nano ferroferric oxide and the polyacrylonitrile as coatings, immersing the fabric into 50 g of copper sulfate pentahydrate aqueous solution with the concentration of 3 percent, adding 50 g of sodium thiosulfate aqueous solution with the concentration of 3 percent after immersing the fabric for 30 minutes at 25 ℃, heating the fabric to 80 ℃, reacting for 1.5 hours, taking out the blended membrane, rinsing the blended membrane with water, and drying the blended membrane to obtain the acrylic fiber blended electromagnetic shielding fabric. The obtained ferroferric oxide/copper sulfide composite electromagnetic shielding fabric has the shielding effectiveness of 35dB within the range of 80MHz-6 GHz.
Example 3
The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to the embodiment is as shown in fig. 1, and comprises the following steps:
(1) 10 g of polyacrylonitrile powder is put into a mixed solvent composed of 194 g of dimethyl sulfoxide and 6g of polyethylene glycol 200, and stirred for 3 hours at 60 ℃ to completely dissolve polyacrylonitrile, so that a polyacrylonitrile solution is obtained.
(2) Adding 3 g of nano ferroferric oxide and 0.4 g of silane coupling agent KH-570 into 90 g of polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic dispersion for 60min to obtain nano ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain the coating solution.
(3) And (3) uniformly coating the coating solution obtained in the step (2) on acrylic and polyester (acrylic fiber 40% and polyester 60%) blended fabric, immersing the acrylic blended fabric with the coating solution in deionized water at 40 ℃, and staying in the deionized water for 0.5 hour to obtain the acrylic blended fabric taking nano ferroferric oxide and polyacrylonitrile as coatings.
(4) And (3) taking 10 g of the acrylic polyester blended fabric which is obtained in the step (3) and takes the nano ferroferric oxide and the polyacrylonitrile as coatings, immersing the fabric into 50 g of a copper sulfate pentahydrate aqueous solution with the mass concentration of 2%, after immersing the fabric for 30 minutes at 10 ℃, adding 50 g of a sodium thiosulfate aqueous solution with the mass concentration of 2%, heating the fabric to 95 ℃, reacting for 0.5 hour, taking out the fabric, rinsing the fabric with water, and drying the fabric to obtain the acrylic fiber blended electromagnetic shielding fabric. The obtained ferroferric oxide/copper sulfide composite electromagnetic shielding fabric has the shielding effectiveness of 26dB within the range of 80MHz-6 GHz.
Example 4
The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to the embodiment is as shown in fig. 1, and comprises the following steps:
(1) 20 g of polyacrylonitrile powder is put into a mixed solvent composed of 194 g of dimethyl sulfoxide and 6g of polyethylene glycol 200, and stirred for 1 hour at 80 ℃ to completely dissolve polyacrylonitrile, so that a polyacrylonitrile solution is obtained.
(2) Adding 2.2 g of nano ferroferric oxide and 0.15 g of silane coupling agent KH-560 into 120 g of polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic dispersion for 90min to obtain nano ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain the coating solution.
(3) And (3) uniformly coating the coating solution obtained in the step (2) on acrylic and polyester (acrylic fiber 40% and polyester 60%) blended fabric, immersing the acrylic blended fabric with the coating solution in deionized water at 10 ℃, and staying in the deionized water for 2 hours to obtain the acrylic blended fabric taking nano ferroferric oxide and polyacrylonitrile as coatings.
(4) And (3) taking 10 g of the acrylic and polyester blended fabric which is obtained in the step (3) and takes the nano ferroferric oxide and the polyacrylonitrile as coatings, immersing the fabric into 50 g of a 5% copper sulfate pentahydrate aqueous solution, after immersing the fabric for 30 minutes at 30 ℃, adding 50 g of a 5% sodium thiosulfate aqueous solution, heating the fabric to 85 ℃, reacting for 2 hours, taking out the blended film, rinsing the blended film with water, and drying the blended film to obtain the acrylic fiber blended electromagnetic shielding fabric. The obtained ferroferric oxide/copper sulfide composite electromagnetic shielding fabric has the shielding effectiveness of 38dB within the range of 80MHz-6 GHz.
Example 5
The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to the embodiment is as shown in fig. 1, and comprises the following steps:
(1) 18 g of polyacrylonitrile powder is put into a mixed solvent composed of 180 g of dimethyl sulfoxide and 20 g of polyethylene glycol 200, and stirred for 3 hours at 75 ℃ to completely dissolve polyacrylonitrile, so that a polyacrylonitrile solution is obtained.
(2) Adding 1.8 g of nano ferroferric oxide and 0.3 g of silane coupling agent KH-570 into 100 g of polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic dispersion for 100min to obtain nano ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain the coating solution.
(3) And (3) uniformly coating the coating solution obtained in the step (2) on acrylic cotton (acrylic fiber 50% and cotton 50%) blended fabric, immersing the acrylic fiber blended fabric with the coating solution in deionized water at 25 ℃, and staying in the deionized water for 1 hour to obtain the acrylic fiber blended fabric taking nano ferroferric oxide and polyacrylonitrile as coatings.
(4) And (3) taking 10 g of the acrylic and polyester blended fabric which is obtained in the step (3) and takes the nano ferroferric oxide and the polyacrylonitrile as coatings, immersing the fabric into 50 g of copper sulfate pentahydrate aqueous solution with the concentration of 8 percent, adding 50 g of sodium thiosulfate aqueous solution with the concentration of 8 percent after immersing the fabric for 30 minutes at the temperature of 30 ℃, heating the fabric to 90 ℃ for reaction for 1 hour, taking out the blended film, rinsing the blended film with water, and drying the blended film to obtain the acrylic fiber blended electromagnetic shielding fabric. The obtained ferroferric oxide/copper sulfide composite electromagnetic shielding fabric has the shielding effectiveness of 33dB in the range of 80MHz-6 GHz.
Example 6
The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to the embodiment is as shown in fig. 1, and comprises the following steps:
(1) 14 g of polyacrylonitrile powder is put into a mixed solvent composed of 190 g of dimethyl sulfoxide and 10 g of polyethylene glycol 200, and stirred for 2.5 hours at 74 ℃ to completely dissolve polyacrylonitrile, so that a polyacrylonitrile solution is obtained.
(2) And (2) adding 1.8 g of nano ferroferric oxide and 0.09 g of silane coupling agent KH-550 into 98 g of polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic dispersion for 110min to obtain nano ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain the coating solution.
(3) And (3) uniformly coating the coating solution obtained in the step (2) on acrylic cotton (acrylic fiber 60% and cotton 40%) blended fabric, immersing the acrylic fiber blended fabric with the coating solution in deionized water at 30 ℃, and staying in the deionized water for 0.8 hour to obtain the acrylic fiber blended fabric taking nano ferroferric oxide and polyacrylonitrile as coatings.
(4) And (3) taking 10 g of the acrylic and polyester blended fabric which is obtained in the step (3) and takes the nano ferroferric oxide and the polyacrylonitrile as coatings, immersing the fabric into 50 g of a 4% copper sulfate pentahydrate aqueous solution at 25 ℃ for 30 minutes, adding 50 g of a 4% sodium thiosulfate aqueous solution, heating to 82 ℃ for reaction for 1.5 hours, taking out the blended film, rinsing with water, and drying to obtain the acrylic fiber blended electromagnetic shielding fabric. The obtained ferroferric oxide/copper sulfide composite electromagnetic shielding fabric has the shielding effectiveness of 42dB within the range of 80MHz-6 GHz.
Example 7
The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to the embodiment is as shown in fig. 1, and comprises the following steps:
(1) 12 g of polyacrylonitrile powder is put into a mixed solvent composed of 182 g of dimethyl sulfoxide and 18 g of polyethylene glycol 200, and stirred for 2.5 hours at 76 ℃ to completely dissolve polyacrylonitrile, so that a polyacrylonitrile solution is obtained.
(2) Adding 3.7 g of nano ferroferric oxide and 0.33 g of silane coupling agent KH-550 into 105 g of polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic dispersion for 105min to obtain nano ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain the coating solution.
(3) And (3) uniformly coating the coating solution obtained in the step (2) on acrylic viscose (60% of acrylic fibers and 40% of viscose fibers) blended fabric, immersing the acrylic blended fabric with the coating solution in deionized water at 30 ℃, and staying in the deionized water for 0.8 hour to obtain the acrylic blended fabric taking nano ferroferric oxide and polyacrylonitrile as coatings.
(4) And (3) taking 10 g of the acrylic and polyester blended fabric which is obtained in the step (3) and takes the nano ferroferric oxide and the polyacrylonitrile as coatings, immersing the fabric into 50 g of 6% blue copperas aqueous solution at 25 ℃ for 30 minutes, adding 50 g of 6% sodium thiosulfate aqueous solution, heating to 88 ℃ for reaction for 1.5 hours, taking out the blended membrane, rinsing with water, and drying to obtain the acrylic fiber blended electromagnetic shielding fabric. The obtained ferroferric oxide/copper sulfide composite electromagnetic shielding fabric has the shielding effectiveness of 38dB within the range of 80MHz-6 GHz.
Example 8
The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to the embodiment is as shown in fig. 1, and comprises the following steps:
(1) 13 g of polyacrylonitrile powder is put into a mixed solvent composed of 175 g of dimethyl sulfoxide and 25 g of polyethylene glycol 200, and stirred for 2.5 hours at 76 ℃ to completely dissolve polyacrylonitrile, so that a polyacrylonitrile solution is obtained.
(2) Adding 4.8 g of nano ferroferric oxide and 0.45 g of silane coupling agent KH-550 into 100 g of polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic dispersion for 120min to obtain nano ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain the coating solution.
(3) And (3) uniformly coating the coating solution obtained in the step (2) on acrylic viscose (50% of acrylic fibers and 50% of viscose fibers) blended fabric, immersing the acrylic blended fabric with the coating solution in deionized water at 25 ℃, and staying in the deionized water for 1 hour to obtain the acrylic blended fabric taking nano ferroferric oxide and polyacrylonitrile as coatings.
(4) And (3) taking 10 g of the acrylic and polyester blended fabric which is obtained in the step (3) and takes the nano ferroferric oxide and the polyacrylonitrile as coatings, immersing the fabric into 50 g of 6% blue copperas aqueous solution at 25 ℃ for 30 minutes, adding 50 g of 6% sodium thiosulfate aqueous solution, heating to 88 ℃ for reaction for 1.5 hours, taking out the blended membrane, rinsing with water, and drying to obtain the acrylic fiber blended electromagnetic shielding fabric. The obtained ferroferric oxide/copper sulfide composite electromagnetic shielding fabric has the shielding effectiveness of 50dB within the range of 80MHz-6 GHz.
Example 9
The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to the embodiment is as shown in fig. 1, and comprises the following steps:
(1) 10 g of polyacrylonitrile powder is put into a mixed solvent composed of 194 g of dimethyl sulfoxide and 6g of polyethylene glycol 200, and stirred for 3 hours at 80 ℃ to completely dissolve polyacrylonitrile, so that a polyacrylonitrile solution is obtained.
(2) And (2) adding 5 g of nano ferroferric oxide and 0.1 g of silane coupling agent KH-550 into 120 g of polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic dispersion for 120min to obtain nano ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain the coating solution.
(3) And (3) uniformly coating the coating solution obtained in the step (2) on a nitrile viscose (acrylic fiber 40% and viscose fiber 60%) blended fabric, immersing the acrylic fiber blended fabric with the coating solution in deionized water at 40 ℃, and staying in the deionized water for 2 hours to obtain the acrylic fiber blended fabric taking nano ferroferric oxide and polyacrylonitrile as coatings.
(4) And (3) taking 10 g of the acrylic and polyester blended fabric which is obtained in the step (3) and takes the nano ferroferric oxide and the polyacrylonitrile as coatings, immersing the fabric into 50 g of copper sulfate pentahydrate aqueous solution with the concentration of 8 percent, adding 50 g of sodium thiosulfate aqueous solution with the concentration of 8 percent after immersing the fabric for 30 minutes at the temperature of 40 ℃, heating the fabric to 88 ℃ for reaction for 1.5 hours, taking out the blended membrane, rinsing the blended membrane with water, and drying the blended membrane to obtain the acrylic fiber blended electromagnetic shielding fabric. The obtained ferroferric oxide/copper sulfide composite electromagnetic shielding fabric has the shielding effectiveness of 50dB within the range of 80MHz-6 GHz.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (6)

1. A preparation method of a ferroferric oxide/copper sulfide composite electromagnetic shielding fabric is characterized by comprising the following steps:
(1) putting polyacrylonitrile powder into a mixed solvent, and stirring for 2-3h at 60-80 ℃ to completely dissolve polyacrylonitrile to obtain a polyacrylonitrile solution;
(2) adding nano ferroferric oxide and a silane coupling agent into the polyacrylonitrile solution obtained in the step (1), stirring and mixing, performing ultrasonic treatment for 60-120min to obtain a ferroferric oxide/polyacrylonitrile blended solution, and standing and defoaming to obtain a coating solution;
(3) uniformly coating the coating solution obtained in the step (2) on the acrylic fiber blended fabric, then immersing the acrylic fiber blended fabric with the coating solution in deionized water at the temperature of 20-40 ℃, and staying in the deionized water for 0.5-2 hours to obtain the acrylic fiber blended fabric taking nano ferroferric oxide and polyacrylonitrile as a coating;
(4) and (3) immersing the acrylic fiber blended fabric taking the nano ferroferric oxide and polyacrylonitrile as the coating obtained in the step (3) into a copper sulfate pentahydrate aqueous solution, soaking for 5-30 minutes at 10-40 ℃, adding a sodium thiosulfate aqueous solution, heating to 75-95 ℃, reacting for 0.5-4 hours, taking out the fabric, rinsing with water, and drying to obtain the electromagnetic shielding fabric.
2. The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to claim 1, characterized by comprising the following steps: the mixed solvent in the step (1) is polyethylene glycol 200 and dimethyl sulfoxide according to the mass ratio of (3-15): (85-97), and the mass of the polyacrylonitrile powder is 5-10% of that of the mixed solvent.
3. The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to claim 1, characterized by comprising the following steps: the mass ratio of the nano ferroferric oxide to the silane coupling agent to the polyacrylonitrile solution in the step (2) is (1-5): (0.1-0.5): (90-120).
4. The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to claim 3, characterized by comprising the following steps: the silane coupling agent is any one of KH-570, KH-550 or KH-560, and the size of the nano ferroferric oxide is 20-100 nm.
5. The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to claim 1, characterized by comprising the following steps: the acrylic fiber blended fabric in the step (3) is a nitrile-polyester blended fabric, a nitrile-viscose blended fabric or a nitrile-cotton blended fabric, wherein the acrylic fiber accounts for 40-60 wt%, and other fibers account for 40-60 wt%.
6. The preparation method of the ferroferric oxide/copper sulfide composite electromagnetic shielding fabric according to claim 1, characterized by comprising the following steps: in the step (4), the mass concentration of the copper sulfate pentahydrate aqueous solution is 2-8% by weight, and the mass concentration of the sodium thiosulfate aqueous solution is 2-8% by weight.
CN202010331095.0A 2019-06-20 2020-04-24 Preparation method of ferroferric oxide/copper sulfide composite electromagnetic shielding fabric Expired - Fee Related CN111270513B (en)

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