CN116219741A - Preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber - Google Patents

Preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber Download PDF

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CN116219741A
CN116219741A CN202310277797.9A CN202310277797A CN116219741A CN 116219741 A CN116219741 A CN 116219741A CN 202310277797 A CN202310277797 A CN 202310277797A CN 116219741 A CN116219741 A CN 116219741A
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silver
meta
aramid fiber
pmia
amine
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曲荣君
王家飞
张盈
孙昌梅
王颖
耿胜男
任冰洁
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Ludong University
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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
    • D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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    • D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
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    • 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
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    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/0084—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising a single continuous metallic layer on an electrically insulating supporting structure, e.g. metal foil, film, plating coating, electro-deposition, vapour-deposition
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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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    • D06M2101/36—Aromatic polyamides

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Abstract

The invention discloses a preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber, which comprises the following steps: adding ultra-pure water into hyperbranched polyamide-amine, dissolving, then dripping a cross-linking agent, magnetically stirring in a constant-temperature water bath, and performing cross-linking reaction to obtain hyperbranched polyamide-amine solution; extracting the aramid fiber with absolute ethyl alcohol, washing, drying, immersing in hyperbranched polyamide-amine solution, drying to obtain cross-linked hyperbranched polyamide-amine modified meta-aramid fiber, immersing in silver ammonia solution, starting ultrasonic treatment, carrying out silver ion ultrasonic adsorption, maintaining ultrasonic treatment after adsorption, dropwise adding glucose solution dropwise for ultrasonic reduction, standing, filtering, washing with ultrapure water, and vacuum drying to obtain the product. According to the invention, hyperbranched polyamide-amine is utilized to modify meta-aramid fiber, active sites capable of being combined with metal particles are added, silver plating meta-aramid fiber with excellent conductivity and electromagnetic shielding performance is obtained by chemical silver deposition, the plating layer is firmly bonded with fiber, and the mechanical property is kept good.

Description

Preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber
Technical Field
The invention relates to silver-plated fibers, in particular to a preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fibers.
Background
The meta-aramid is fully called as poly m-phenylene isophthalamide, commonly called as "aramid 1313", and is called PMIA for short, the structure is formed by directly connecting at least 85% of amide bonds with two benzene rings, and a strong hydrogen bond three-dimensional network structure is displayed in molecules and among molecules, so that the meta-aramid has excellent heat resistance, heat stability, dimensional stability, self-extinguishing flame retardance, electrical insulation, chemical stability, radiation resistance, outstanding mechanical properties and the like, and has great application value in the fields of aerospace, rail transit, high-temperature filtration, electrical insulation, construction, marine fire protection, sports automobiles, protection and the like.
However, in various flammable and explosive working environments, clothing made of flame-retardant meta-aramid fiber is easy to cause static electricity on the surface of the clothing due to high insulativity, and electric spark is generated, so that explosion accidents are caused. Meanwhile, the non-anti-electric/magnetic meta-aramid protective clothing causes workers engaged in electronic instruments to suffer from health damage due to electromagnetic wave radiation. Therefore, the multifunctional protective clothing with single function cannot meet the complex requirements, and has flame retardance, static resistance and electromagnetic shielding.
Conductive aramid is a high performance material that eliminates static electricity by electron conduction and corona discharge, generally referred to as having a resistivity of less than 10 at 20 ℃ and 65% relative humidity standard 8 Omega cm material with resistivity up to 10-10 -3 Omega cmThe conductive aramid fiber can shield electromagnetic waves.
Because of the excellent conductivity of metals, the surface of PMIA is metallized, so that the PMIA has the functions of eliminating static electricity, conducting electricity, shielding electromagnetic waves and the like. The surface metallization of PMIA is realized, which not only shows the metal characteristic, but also keeps the flexibility of PMIA, and has the advantages of lighter weight, low cost, flexibility and the like than metal. The prior aramid fiber surface metallization method mainly comprises chemical plating, sputtering plating, vacuum deposition, surface coating, blending spinning method and the like. Among them, the electroless plating method of surface metallization is one of the effective methods of depositing metal on meta-aramid fiber because of the advantages of moderate cost, uniform coating formation on various substrates, simple and convenient equipment, etc. However, the prior reported conductive material prepared by chemical plating has the defects of larger mechanical damage of aramid fiber, weak plating layer and the like.
Disclosure of Invention
Aiming at the problems of large mechanical damage and infirm plating of the existing aramid fiber metal plating fiber, the invention provides a preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver plating meta-aramid fiber, which comprises the following steps: (1) Adding ultra-pure water into hyperbranched polyamide-amine, heating and stirring to completely dissolve and disperse the ultra-pure water, dripping a cross-linking agent, magnetically stirring in a constant-temperature water bath, performing cross-linking reaction to obtain a cross-linked hyperbranched polyamide-amine solution, and preserving heat for later use; (2) Extracting the aramid fiber with absolute ethyl alcohol, washing, drying, immersing the aramid fiber into the cross-linked hyperbranched polyamide-amine solution obtained in the step (1), taking out and drying to obtain the cross-linked hyperbranched polyamide-amine modified meta-aramid fiber; (3) Immersing the cross-linked hyperbranched polyamide-amine modified meta-aramid fiber obtained in the step (2) into silver ammonia solution, starting ultrasonic, performing silver ion ultrasonic adsorption, after the adsorption is completed, maintaining ultrasonic, dropwise adding glucose solution dropwise for ultrasonic reduction, standing, filtering, washing the filtrate with ultrapure water, and vacuum drying to obtain the cross-linked dendrimer silver-plated meta-aramid fiber.
The aramid fibers adopted by the invention can be aramid fiber filaments and staple fibers, or aramid non-woven fabrics or aramid woven fabrics.
The invention adopts the following technological parameters to optimize the method, or obtain the cross-linked dendrimer silver-plated meta-aramid fiber with excellent performance.
In the step (1), the number average molecular weight of the hyperbranched polyamide-amine is 500-1000, the concentration is 0.5-40g/L, and the hyperbranched polyamide-amine is an irregular highly branched ball-like novel three-dimensional macromolecule containing a large number of holes and terminal primary amino functional groups, and has unique physical and chemical characteristics. At present, hyperbranched polyamide-amine which is simple and quick to synthesize, low in cost and capable of being produced in a large scale has good application in the aspects of paint curing agents, medicine carriers, sewage treatment, catalysts, molecular recognition, self-assembly, surfactants, conductive materials and the like, therefore, meta-aramid fiber/fabric is selected as a base material, and hyperbranched polyamide-amine with highly branched and multifunctional surface functional groups is adopted as a surface modifier, so that a large number of active sites can be introduced on the surface of the fiber/fabric, and meanwhile, the mechanical and flexibility properties are improved, and the conductive and electromagnetic shielding meta-aramid fiber/fabric can be prepared by chemical silver plating as a secondary reaction platform, so that the defects of high mechanical property damage of the fiber/fabric, high cost of a modifying agent, poor adhesion between a plating layer and the fiber/fabric and the like caused by an electroless plating method can be effectively solved.
The cross-linking agent is one of monoepoxy compounds, dicycloxy compounds, diglycidyl esters or polyepoxy compounds. Specifically, the monoepoxy compound is epichlorohydrin, epibromohydrin or epoxypropionic acid; the bisepoxy compound is diglycidyl ether, ethylene glycol diglycidyl ether, diethylene glycol diglycidyl ether, 1, 4-butanediol diglycidyl ether, poly (propylene glycol diglycidyl ether), bisphenol a diglycidyl ether, resorcinol diglycidyl ether or poly (dimethylsiloxane) diglycidyl ether; the diglycidyl ester is diglycidyl phthalate, diglycidyl adipate or diglycidyl aniline; the polyepoxy compound is glycerol triglycidyl ether or pentaerythritol triglycidyl ether. The molar ratio of the cross-linking agent to the hyperbranched polyamide-amine is (0.1-12) 1; the crosslinking reaction time is 0.5-12h; the water bath temperature is 10-100 ℃, and the magnetic stirring speed is 120-2400rpm.
In the step (2), the soaking time is 0.5-6h. In the step (3), the ultrasonic frequency is 40KHz, the power is 120-360W, the ultrasonic adsorption time is 0.1-3h, and the ultrasonic reduction time is 0.5-4h; the vacuum drying temperature is 30-90 ℃ and the time is 6-24h.
The invention can adopt the existing silver ammonia solution, but as a better choice, the invention provides a preparation method of silver ammonia solution: dropwise adding ammonia water into the silver nitrate aqueous solution to make the solution become clear and transparent, regulating the pH value of the solution to 10-13 by potassium hydroxide, continuously adding the ammonia water dropwise to make the mixed solution become clear and transparent again, and finally adding polyvinylpyrrolidone K30 to obtain the silver ammonia solution. Wherein, the concentration of the silver nitrate aqueous solution is 5-40g/L, the concentration of potassium hydroxide is 3-9g/L, and the concentration of polyvinylpyrrolidone is 1-10g/L.
The composition of glucose solution matched with the silver ammonia solution is as follows: 10-50 g/L of anhydrous glucose, 20-60 mL/L of absolute ethyl alcohol and 60-90 mg/L of polyethylene glycol 2000; the dropping speed of the glucose liquid is 0.5-3 drops/second.
According to the invention, the meta-aramid fiber is modified by using the cross-linked hyperbranched polyamide-amine through a surface physical coating modification method, so that the active sites capable of being combined with metal particles are remarkably increased, the mechanical properties are improved, and the modification reagent is low in cost; according to the invention, silver plating meta-aramid fiber with excellent conductivity and electromagnetic shielding performance is obtained by chemical silver deposition, the plating layer is firmly bonded with the fiber, the mechanical property is kept good, and the experimental steps are simple and easy to implement.
Drawings
FIG. 1 shows the clean PMIA raw fiber of example 2, the modified fiber PMIA/HP of example 2 5 EGDE 3 PMIA/Ag fiber in comparative example 1, silver-plated fiber PMIA/HP in example 2 5 EGDE 3 Scanning electron microscope image of/Ag.
FIG. 2 shows the clean PMIA raw fiber of example 2, the modified fiber PMIA/HP of example 2 5 EGDE 3 PMIA/Ag fiber in comparative example 1, silver-plated fiber PMIA/HP in example 2 5 EGDE 3 Atomic force microscopy of Ag.
FIG. 3 is a clean PMIA fiber of example 13Modified fiber PMIA/HP 5 DGDE 2 PMIA/HP for silver-plated fiber 5 DGDE 2 XRD patterns of/Ag, and PMIA/Ag in comparative example 1.
FIG. 4 shows the clean PMIA raw fiber of example 13, the modified fiber PMIA/HP of example 13 5 DGDE 2 PMIA/Ag fiber in comparative example 1, silver-plated fiber PMIA/HP in example 13 5 DGDE 2 Analysis chart of mechanical properties of Ag.
FIG. 5 shows the cleaned PMIA fibers and modifier HP of example 14 5 ECH 2 Modified fiber PMIA/HP 5 ECH 2 PMIA/HP for silver-plated fiber 5 ECH 2 Graph of thermal weight loss of Ag.
Fig. 6 is a surface resistivity analysis chart of the conductive fibers prepared in examples 1 to 7, examples 2 and 8 to 12 and comparative example 1 (examples 1, 2, 3, 4, 5, 6, 7 are shown in the order of from left to right in fig. 6A; and examples 8, 9, 2, 10, 11, 12, and rectangular shadows are shown in the order of from left to right in fig. 6B as comparative example 1).
FIG. 7 is a PMIA/HP of example 11 5 EGDE 5 Graph of firmness analysis of silver layer on Ag fiber surface.
FIG. 8 shows PMIA raw fabric and modified fabric PMIA/HP cleaned in example 16 5 DGDE 3 PMIA/Ag fabric in comparative example 2, silver plated fabric PMIA/HP of example 16 5 DGDE 3 Scanning electron microscope image of/Ag.
FIG. 9 is a schematic representation of a silver plated fabric PMIA/HP of example 16 5 DGDE 3 Square resistance value of Ag.
FIG. 10 is a schematic representation of a silver plated fabric PMIA/HP of example 16 5 DGDE 3 Electromagnetic shielding effectiveness value of Ag.
Detailed Description
The invention is described below in connection with examples which are given solely for the purpose of illustration and are not intended to limit the scope of the invention.
The hyperbranched polyamide-amine adopted in the embodiment of the invention is provided by WiHai Chen Source molecular New Material Co., ltd, and the model is CYD-D014.
Example 1
A preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber comprises the following steps:
1. preparation of crosslinked hyperbranched polyamide-amine modifier
50mL of ultra-pure water (1 g/L) was added to 0.05g of hyperbranched polyamide-amine (HPAMAM), heated at 60℃and stirred to be sufficiently dissolved and uniformly dispersed; then dripping 0.029mL Ethylene Glycol Diglycidyl Ether (EGDE) into the obtained HPAMAM water solution, wherein the mol ratio of EGDE to HPAMAM is 3:1, and carrying out crosslinking reaction for 1h under the constant temperature water bath of 80 ℃ and the magnetic stirring with the speed of 360rpm, thus obtaining the crosslinking modification reaction liquid HP 1 EGDE 3 。
2. Pretreatment of meta-aramid fiber
Meta-aramid fiber (PMIA) was placed in a Soxhlet extractor, extracted with absolute ethanol for 18h, followed by vacuum drying at 60℃for 8h.
3. Preparation of cross-linked hyperbranched polyamide-amine modified meta-aramid fiber
Immersing 0.5g of PMIA fibers pretreated in step 2 in HP of step 1 1 EGDE 3 In the mixed solution, carrying out fiber surface modification reaction for 2h at room temperature, and then carrying out vacuum drying for 8h at 60 ℃ to obtain the modified meta-aramid fiber PMIA/HP 1 EGDE 3 。
4. Preparation of cross-linked hyperbranched polyamide-amine silver-plated conductive meta-aramid fiber
Dropwise adding ammonia water into 50mL of 15g/L silver nitrate aqueous solution until the solution is clear and transparent, then adjusting the pH value of the solution to 12.0 by using 8g/L KOH aqueous solution, continuously dripping ammonia water to make the solution clear and transparent again, adding 0.35g polyvinylpyrrolidone K30 (PVP) into the transparent solution, and fully stirring to completely dissolve the solution to obtain silver-ammonia solution;
adding 0.0042g of polyethylene glycol 2000 (PEG) and 2mL of absolute ethyl alcohol into 1.2g of absolute glucose, primarily stirring, and adding ultrapure water into the mixture to 50mL of absolute ethyl alcohol to prepare a glucose reduction solution;
will be 025g of PMIA/HP prepared in step 3 1 EGDE 3 Immersing in silver ammonia solution, and carrying out ultrasonic adsorption for 0.5h at 35 ℃, wherein the ultrasonic frequency is 40KHz, and the power is 240W; then dripping glucose reducing solution into the reaction kettle at a speed of 1 drop/second, and carrying out ultrasonic reduction at 30 ℃ for 0.5h, wherein the frequency is 40KHz, and the power is 240W; standing for a period of time to enable silver particles to be fully deposited on the fibers; filtering the fiber, and washing the fiber with ultrapure water for 3 times until the washing liquid is not turbid; finally, the silver-plated fiber is put into a vacuum drying oven for drying at 60 ℃ for 8 hours to prepare PMIA/HP 1 EGDE 3 Ag conductive fibers.
Example 2
The only difference from example 1 is that: in step 1, the HPAMAM concentration is 5g/L, and the obtained silver-plated conductive meta-aramid fiber is PMIA/HP 5 EGDE 3 /Ag。
Example 3
The only difference from example 1 is that: in step 1, the HPAMAM concentration is 10g/L, and the obtained silver-plated conductive meta-aramid fiber is PMIA/HP 10 EGDE 3 /Ag。
Example 4
The only difference from example 1 is that: in step 1, the HPAMAM concentration is 15g/L, and the obtained silver-plated conductive meta-aramid fiber is PMIA/HP 15 EGDE 3 /Ag。
Example 5
The only difference from example 1 is that: in step 1, the HPAMAM concentration is 20g/L, and the obtained silver-plated conductive meta-aramid fiber is PMIA/HP 20 EGDE 3 /Ag。
Example 6
The only difference from example 1 is that: in step 1, the HPAMAM concentration is 25g/L, and the obtained silver-plated conductive meta-aramid fiber is PMIA/HP 25 EGDE 3 /Ag。
Example 7
The only difference from example 1 is that: in step 1, the HPAMAM concentration is 30g/L, and the obtained silver-plated conductive meta-aramid fiber is PMIA/HP 30 EGDE 3 /Ag。
Example 8
A preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber comprises the following steps:
1. preparation of crosslinked hyperbranched polyamide-amine modifier
50mL of ultra-pure water (5 g/L) was added to 0.25g of HPAMAM, heated at 65℃and stirred to be sufficiently dissolved and dispersed uniformly; then, 0.049mL EGDE,EGDE and HPAMM are added dropwise into the obtained HPAMM water solution in a molar ratio of 1:1, and crosslinking reaction is carried out for 1h under the constant-temperature water bath at 65 ℃ and the magnetic stirring at the speed of 400rpm, thus obtaining crosslinking modified reaction liquid HP 5 EGDE 1 。
2. Pretreatment of meta-aramid fiber
PMIA was placed in a Soxhlet extractor, extracted with absolute ethanol for 12h, and then dried in vacuo at 60℃for 8h.
3. Preparation of cross-linked hyperbranched polyamide-amine modified meta-aramid fiber
Immersing 0.5g of PMIA fibers pretreated in step 2 in HP of step 1 5 EGDE 1 In the mixed solution, carrying out fiber surface modification reaction for 1h at room temperature, and then carrying out vacuum drying at 60 ℃ for 10h to obtain the modified meta-aramid fiber PMIA/HP 5 EGDE 1 。
4. Preparation of cross-linked hyperbranched polyamide-amine silver-plated conductive meta-aramid fiber
Dropwise adding ammonia water into 50mL of 15g/L silver nitrate aqueous solution until the solution is clear and transparent, then adjusting the pH value of the solution to 12.0 by using 8g/L KOH aqueous solution, continuously dripping ammonia water to make the solution clear and transparent again, adding 0.5g PVP into the transparent solution, and fully stirring to completely dissolve the solution to obtain silver-ammonia solution;
adding 0.0045g of PEG and 2mL of absolute ethyl alcohol into 2.5g of absolute glucose, primarily stirring, and adding ultrapure water into the mixture to 50mL of absolute ethyl alcohol to prepare a glucose reduction solution;
0.25g of PMIA/HP prepared in step 3 was reacted with 5 EGDE 1 Immersing in silver ammonia solution, and carrying out ultrasonic adsorption for 0.5h at 25 ℃, wherein the ultrasonic frequency is 40KHz, and the power is 120W; then dripping glucose reducing solution into the mixture at a speed of 2 drops/second, and carrying out ultrasonic reduction at 25 ℃ for 2 hours at a frequency of 40KHz and a power of 120W; standing for a period of time to make silver particlesFully depositing the seeds on the fibers; filtering the fiber, and washing the fiber with ultrapure water for 3 times until the washing liquid is not turbid; finally, the silver-plated fiber is put into a vacuum drying oven for drying at 60 ℃ for 8 hours to prepare PMIA/HP 5 EGDE 1 Ag conductive fibers.
Example 9
The only difference from example 8 is that: in the step 1, the molar ratio of EGDE to HPAMAM is 2:1, and the obtained silver-plated conductive meta-aramid fiber is PMIA/HP 5 EGDE 2 /Ag。
Example 10
The only difference from example 8 is that: in the step 1, the molar ratio of EGDE to HPAMAM is 4:1, and the obtained silver-plated conductive meta-aramid fiber is PMIA/HP 5 EGDE 4 /Ag。
Example 11
The only difference from example 8 is that: in the step 1, the molar ratio of EGDE to HPAMAM is 5:1, and the obtained silver-plated conductive meta-aramid fiber is PMIA/HP 5 EGDE 5 /Ag。
Example 12
The only difference from example 8 is that: in the step 1, the molar ratio of EGDE to HPAMAM is 6:1, and the obtained silver-plated conductive meta-aramid fiber is PMIA/HP 5 EGDE 6 /Ag。
Example 13
A preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber comprises the following steps:
1. preparation of crosslinked hyperbranched polyamide-amine modifier
50mL of ultrapure water (5 g/L) is added into 0.25g of HPAMAM, and the mixture is heated and stirred at the temperature of 40-80 ℃ to be fully dissolved and uniformly dispersed; then dripping 0.125mL of Diethylene Glycol Diglycidyl Ether (DGDE) into the obtained HPAMAM water solution, wherein the mol ratio of DGDE to HPAMAM is 2:1, and carrying out crosslinking reaction for 5h under the constant-temperature water bath at 80 ℃ and magnetic stirring at the speed of 360rpm to obtain crosslinking modified reaction liquid HP 5 DGDE 2 。
2. Pretreatment of meta-aramid fiber
PMIA was placed in a Soxhlet extractor, extracted with absolute ethanol for 15h, and then dried in vacuo at 60℃for 8h.
3. Preparation of cross-linked hyperbranched polyamide-amine modified meta-aramid fiber
0.5g of the PMIA fabric pretreated in step 2 was immersed in the HP in step 1 5 DGDE 2 In the mixed solution, carrying out fabric surface modification reaction for 0.5h at room temperature, and then carrying out vacuum drying for 8h at 60 ℃ to obtain the modified meta-aramid fiber PMIA/HP 5 DGDE 2 。
4. Preparation of cross-linked hyperbranched polyamide-amine silver-plated conductive meta-aramid fiber
Dropwise adding ammonia water into 50mL 12g/L silver nitrate aqueous solution until the solution is clear and transparent, then adjusting the pH value of the solution to 11.0 by using 6g/L KOH aqueous solution, continuously dripping ammonia water to make the solution clear and transparent again, adding 0.15g PVP into the transparent solution, and fully stirring to make the solution completely dissolved to obtain silver-ammonia solution;
adding 0.0035g of PEG and 1mL of absolute ethyl alcohol into 1.0g of absolute glucose, primarily stirring, and adding ultrapure water into the mixture to 50mL of absolute ethyl alcohol to prepare a glucose reduction solution;
0.25g of PMIA/HP prepared in step 3 was reacted with 5 DGDE 2 Immersing in silver ammonia solution, and performing ultrasonic adsorption for 0.5h at 30 ℃, wherein the ultrasonic frequency is 40KHz, and the power is 252W; then dripping glucose reducing solution into the reaction kettle at the speed of 2 drops/second, and carrying out ultrasonic reduction at the temperature of 30 ℃ for 2 hours, wherein the frequency is 40KHz, and the power is 252W; standing for a period of time to enable silver particles to be fully deposited on the fibers; filtering the fiber, and washing the fiber with ultrapure water for 3 times until the washing liquid is not turbid; finally, the silver-plated fiber is put into a vacuum drying oven for drying at 60 ℃ for 8 hours to prepare PMIA/HP 5 DGDE 2 Ag conductive fibers.
Example 14
A preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber comprises the following steps:
1. preparation of crosslinked hyperbranched polyamide-amine modifier
50mL of ultra-pure water (5 g/L) was added to 0.25g of HPAMAM, heated at 70℃and stirred to be sufficiently dissolved and dispersed uniformly; then, 0.052mL of epoxy chloride was added dropwise to the obtained HPAMAM aqueous solutionPropane (ECH), wherein the molar ratio of ECH to HPAMAM is 2:1, and carrying out crosslinking reaction for 4h under the constant-temperature water bath at 70 ℃ and the magnetic stirring at the speed of 300rpm to obtain crosslinking modification reaction liquid HP 5 ECH 2 。
2. Pretreatment of meta-aramid fiber
PMIA was placed in a Soxhlet extractor, extracted with absolute ethanol for 12h, and then dried in vacuo at 60℃for 8h.
3. Preparation of cross-linked hyperbranched polyamide-amine modified meta-aramid fiber
Immersing 0.5g of PMIA fibers pretreated in step 2 in HP of step 1 5 ECH 2 In the mixed solution, fiber surface modification reaction is carried out for 3h at room temperature, and after the reaction is finished, the mixture is taken out to lead HP 5 ECH 2 Curing at the surface of the fiber, followed by 1g/L Na 2 CO 3 Washing the fiber surface with water solution, and vacuum drying at 60deg.C for 8 hr to obtain modified meta-aramid fiber PMIA/HP 5 ECH 2 。
4. Preparation of cross-linked hyperbranched polyamide-amine silver-plated conductive and electromagnetic shielding meta-aramid fiber
Dropwise adding ammonia water into 50mL of 10g/L silver nitrate aqueous solution until the solution is clear and transparent, then adjusting the pH value of the solution to 10.0 by using 4g/L KOH aqueous solution, continuously dripping ammonia water to make the solution clear and transparent again, adding 0.5g PVP into the transparent solution, and fully stirring to completely dissolve the solution to obtain silver-ammonia solution;
adding 0.0030g of PEG and 3mL of absolute ethyl alcohol into 2.5g of absolute glucose, primarily stirring, and adding ultrapure water into the mixture to 50mL of absolute ethyl alcohol to prepare a glucose reduction solution;
0.25g of PMIA/HP prepared in step 3 was reacted with 5 ECH 2 Immersing in silver ammonia solution, and carrying out ultrasonic adsorption for 2 hours at 30 ℃, wherein the ultrasonic frequency is 40KHz, and the power is 180W; then dripping glucose reducing solution into the mixture at a speed of 1 drop/second, and carrying out ultrasonic reduction at 30 ℃ for 2 hours, wherein the frequency is 40KHz, and the power is 180W; standing for a period of time to enable silver particles to be fully deposited on the fibers; filtering the fiber, and washing the fiber with ultrapure water for 3 times until the washing liquid is not turbid; finally, the silver-plated fiber is put into a vacuum drying oven for drying at 60 DEG CDrying for 8 hr to obtain PMIA/HP 5 ECH 2 Ag conductive fibers.
Example 15
A preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber comprises the following steps:
1. preparation of crosslinked hyperbranched polyamide-amine modifier
100mL of ultrapure water (5 g/L) was added to 0.5g of HPAMAM, heated at 60℃and stirred to be sufficiently dissolved and dispersed uniformly; then, 0.293mL EGDE,EGDE and HPAMM are added dropwise into the obtained HPAMM water solution in a molar ratio of 3:1, and crosslinking reaction is carried out for 2h under the constant-temperature water bath at 60 ℃ and the magnetic stirring at the speed of 240rpm, thus obtaining crosslinking modified reaction liquid HP 5 EGDE 3 。
2. Pretreatment of meta-aramid fabric
PMIA was placed in a Soxhlet extractor, extracted with absolute ethanol for 12h, and then dried in vacuo at 60℃for 8h.
3. Preparation of cross-linked hyperbranched polyamide-amine modified meta-aramid fabric
1.0g of the PMIA fabric pretreated in step 2 was immersed in the HP in step 1 5 EGDE 3 In the mixed solution, carrying out fabric surface modification reaction for 1h at room temperature, and then carrying out vacuum drying for 8h at 60 ℃ to obtain the modified meta-aramid fabric PMIA/HP 5 EGDE 3 。
4. Preparation of cross-linked hyperbranched polyamide-amine silver-plated conductive and electromagnetic shielding meta-aramid fabric
Dropwise adding ammonia water into 100mL of 20g/L silver nitrate aqueous solution until the solution is clear and transparent, then regulating the pH value of the solution to 11.0 by using 6g/L KOH aqueous solution, continuously dripping ammonia water to make the solution clear and transparent again, adding 0.3g PVP into the transparent solution, and fully stirring to completely dissolve the solution to obtain silver-ammonia solution;
adding 0.0065g PEG and 2mL absolute ethyl alcohol into 1.5g absolute glucose, primarily stirring, and then adding ultrapure water into the mixture to 100mL to prepare glucose reduction solution;
0.5g of PMIA/HP prepared in step 3 was reacted with 5 EGDE 3 Immersing in silver-ammonia solution, ultrasonic adsorbing at 30 deg.C1h, the ultrasonic frequency is 40KHz, and the power is 120W; then dripping glucose reducing solution into the mixture at a speed of 2 drops/second, and carrying out ultrasonic reduction at 30 ℃ for 1h, wherein the frequency is 40KHz, and the power is 120W; standing for a period of time to enable silver particles to be fully deposited on the fabric; filtering the fabric, and washing the fabric with ultrapure water for 3 times until the washing liquid is not turbid; finally, the silver-plated fabric is put into a vacuum drying oven for drying at 60 ℃ for 8 hours to prepare PMIA/HP 5 EGDE 3 Ag conductive and electromagnetic shielding fabrics.
Example 16
A preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber comprises the following steps:
1. preparation of crosslinked hyperbranched polyamide-amine modifier
100mL of ultrapure water (5 g/L) was added to 0.5g of HPAMAM, heated at 50℃and stirred to be sufficiently dissolved and dispersed uniformly; then, 0.374mL DGDE,DGDE and HPAMM are added dropwise into the obtained HPAMM water solution in a molar ratio of 3:1, and crosslinking reaction is carried out for 4 hours under the constant-temperature water bath of 50 ℃ and the magnetic stirring at the speed of 480rpm, thus obtaining crosslinking modified reaction liquid HP 5 DGDE 3 。
2. Pretreatment of meta-aramid fabric
PMIA was placed in a Soxhlet extractor, extracted with absolute ethanol for 12h, and then dried in vacuo at 60℃for 8h.
3. Preparation of cross-linked hyperbranched polyamide-amine modified meta-aramid fabric
1.0g of the PMIA fabric pretreated in step 2 was immersed in the HP in step 1 5 DGDE 3 In the mixed solution, carrying out fabric surface modification reaction for 2h at room temperature, and then carrying out vacuum drying for 8h at 60 ℃ to obtain the modified meta-aramid fabric PMIA/HP 5 DGDE 3 。
4. Preparation of cross-linked hyperbranched polyamide-amine silver-plated conductive and electromagnetic shielding meta-aramid fabric
Dropwise adding ammonia water into 100mL of 15g/L silver nitrate aqueous solution until the solution is clear and transparent, then regulating the pH value of the solution to 11.0 by using 5g/L KOH aqueous solution, continuously dripping ammonia water to make the solution clear and transparent again, adding 0.5g PVP into the transparent solution, and fully stirring to completely dissolve the solution to obtain silver-ammonia solution;
adding 0.0060g PEG and 1mL absolute ethyl alcohol into 3.0g absolute glucose, primarily stirring, and then adding ultrapure water into the mixture to 100mL to prepare glucose reduction solution;
0.5g of PMIA/HP prepared in step 3 was reacted with 5 DGDE 3 Immersing in silver ammonia solution, and performing ultrasonic adsorption for 0.5h at 30 ℃, wherein the ultrasonic frequency is 40KHz, and the power is 252W; then dripping glucose reducing solution into the reaction kettle at a speed of 1 drop/second, and carrying out ultrasonic reduction at 30 ℃ for 2 hours, wherein the frequency is 40KHz, and the power is 252W; standing for a period of time to enable silver particles to be fully deposited on the fabric; filtering the fabric, and washing the fabric with ultrapure water for 3 times until the washing liquid is not turbid; finally, the silver-plated fabric is put into a vacuum drying oven for drying at 60 ℃ for 8 hours to prepare PMIA/HP 5 DGDE 3 Ag conductive and electromagnetic shielding fabrics.
Example 17
A preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber comprises the following steps:
1. preparation of crosslinked hyperbranched polyamide-amine modifier
100mL of ultrapure water (5 g/L) was added to 0.5g of HPAMAM, heated at 70℃and stirred to be sufficiently dissolved and dispersed uniformly; then dripping 0.156mL ECH with the molar ratio of ECH to HPAMAM of 3:1 into the obtained HPAMAM aqueous solution, and carrying out crosslinking reaction for 2h under the constant-temperature water bath of 70 ℃ and the magnetic stirring with the speed of 240rpm to obtain crosslinking modified reaction liquid HP 5 ECH 3 。
2. Pretreatment of meta-aramid fabric
PMIA was placed in a Soxhlet extractor, extracted with absolute ethanol for 12h, and then dried in vacuo at 60℃for 8h.
3. Preparation of cross-linked hyperbranched polyamide-amine modified meta-aramid fabric
1.0g of the PMIA fabric pretreated in step 2 was immersed in the HP in step 1 5 ECH 3 In the mixed solution, carrying out fabric surface modification reaction for 1.5h at room temperature, and then carrying out vacuum drying for 8h at 60 ℃ to obtain the modified meta-aramid fabric PMIA/HP 5 ECH 3 。
4. Preparation of cross-linked hyperbranched polyamide-amine silver-plated conductive meta-aramid fabric
Dropwise adding ammonia water into 100mL of 12g/L silver nitrate aqueous solution until the solution is clear and transparent, then regulating the pH value of the solution to 10.0 by using 5g/L KOH aqueous solution, continuously dripping ammonia water to make the solution clear and transparent again, adding 0.25g PVP into the transparent solution, and fully stirring to completely dissolve the solution to obtain silver-ammonia solution;
adding 0.0075g of PEG and 2mL of absolute ethyl alcohol into 3.0g of absolute glucose, primarily stirring, and adding ultrapure water into the mixture to 100mL of absolute ethyl alcohol to prepare a glucose reduction solution;
0.5g of PMIA/HP prepared in step 3 was reacted with 5 ECH 3 Immersing in silver ammonia solution, and performing ultrasonic adsorption for 0.5h at 30 ℃, wherein the ultrasonic frequency is 40KHz, and the power is 252W; then dripping glucose reducing solution into the reaction kettle at a speed of 1 drop/second, and carrying out ultrasonic reduction at 30 ℃ for 1h, wherein the frequency is 40KHz, and the power is 252W; standing for a period of time to enable silver particles to be fully deposited on the fabric; filtering the fabric, and washing the fabric with ultrapure water for 3 times until the washing liquid is not turbid; finally, the silver-plated fabric is put into a vacuum drying oven for drying at 60 ℃ for 8 hours to prepare PMIA/HP 5 ECH 3 Ag conductive and electromagnetic shielding fabrics.
Comparative example 1
The difference from example 1 is only that the meta-aramid fabric washed in step 2 was directly subjected to electroless silver plating without performing steps 1 and 3 to prepare PMIA/Ag fiber.
Comparative example 2
The difference from example 15 is only that the meta-aramid fabric washed in step 2 was directly subjected to electroless silver plating without performing steps 1 and 3 to prepare a PMIA/Ag fabric.
Test 1
The clean PMIA raw fiber, modified fiber PMIA/HP in example 2 was observed by using a scanning electron microscope 5 EGDE 3 PMIA/Ag in comparative example 1, silver-plated fiber PMIA/HP of example 2 5 EGDE 3 The surface morphology of Ag is shown in FIG. 1. As can be seen from FIG. 1, the PMIA surface is clean, but some axial direction existsIs modified to have surface grooves HP 5 EGDE 3 The coating becomes flat, and the silver layer is even and compact on the surface of the modified fiber after further chemical silver plating, but the silver layer on the surface of the direct silver plating fiber is not discontinuous.
Test 2
The clean PMIA raw fiber and modified fiber PMIA/HP of example 2 were analyzed by atomic force microscope 5 EGDE 3 PMIA/Ag in comparative example 1, silver-plated fiber PMIA/HP of example 2 5 EGDE 3 Surface roughness of Ag, the results are shown in fig. 2. As can be seen from fig. 2, the roughness of the modified and modified fabric is slightly reduced due to the smooth and flat surface, the roughness is significantly increased due to the thick silver layer coated on the surface of the fabric after electroless plating, and the surface pits of the fiber which is not modified and directly plated with silver are filled with a small amount of silver particles, so that the roughness is reduced.
Test 3
PMIA/HP of the clean PMIA fibers and modified fibers in example 13 5 DGDE 2 PMIA/HP for silver-plated fiber 5 DGDE 2 XRD analysis was performed on/Ag, and PMIA/Ag in comparative example 1, and the results are shown in FIG. 3. As can be seen from FIG. 3, PMIA has a significant diffraction peak between 15 and 30 degrees, indicating that meta-aramid fiber is partially crystallized by HP 5 DGDE 2 After modification, the crystallinity of the fiber is improved, characteristic diffraction peaks of silver respectively appear at 38.08 degrees, 44.26 degrees, 64.46 degrees, 77.42 degrees and 81.58 degrees after silver plating, the characteristic diffraction peaks respectively correspond to (111), (200), (220), (311) and (222) crystal faces (JCPSDSNo. 04-0783) of silver, and the characteristic diffraction peaks of the fiber are reserved to a certain extent, but PMIA characteristic diffraction peaks of the fiber directly plated with silver are basically covered by PMIA.
Test 4
PMIA/HP of the clean PMIA fibers and modified fibers in example 13 5 DGDE 2 PMIA/Ag fiber in comparative example 1, silver-plated fiber PMIA/HP in example 13 5 DGDE 2 The mechanical properties of Ag are analyzed and the results are shown in FIG. 4. As can be seen from FIG. 4, PMIA/HP 5 DGDE 2 Modified fiber、PMIA/HP 5 DGDE 2 The tensile strength of the silver-plated PMIA fiber is improved compared with that of the original PMIA, but the mechanical property of PMIA/Ag is reduced, which shows that the modifier can protect the PMIA fiber from being corroded by silver plating liquid.
Test 5
Characterization of the cleaned PMIA fibers, modifier HP in example 14 5 ECH 2 Modified fiber PMIA/HP 5 ECH 2 PMIA/HP for silver-plated fiber 5 ECH 2 Thermal stability of Ag, the results are shown in FIG. 5. It can be seen in fig. 5 that both the modified as well as the silver-plated fibers maintain good thermal stability of the original fibers.
Test 6
The surface resistivity of the conductive fibers prepared in examples 1 to 7, examples 2 and 8 to 12 and comparative example 1 were measured, and the results are shown in fig. 6. As can be seen from FIG. 6A, when the HPAMAM concentration is 5g/L, the resistivity is the smallest, and the conductivity is the best, which is 1.03X10 -4 Omega cm; as can be seen from FIG. 6B, the resistivity is minimized at 1.03X10 when the molar ratio of EGDE to HPAMM is 3:1 -4 Omega cm; whereas the meta-aramid fiber directly plated with silver has poor conductivity, the resistivity is 7.81×10 -4 Ω·cm。
Test 7
Testing PMIA/HP with example 11 5 EGDE 5 The firmness of the silver layer on the surface of the Ag fiber is shown in FIG. 7. As can be seen from fig. 7, the silver layer was firmly bonded to the fibers for the first 50 minutes of ultrasound, and the resistivity was only 2.98 times that before ultrasound even at 60 minutes.
Test 8
The clean PMIA raw fabric, modified fabric PMIA/HP in example 16 was observed using a scanning electron microscope 5 DGDE 3 PMIA/Ag fabric in comparative example 2, silver plated fabric PMIA/HP of example 16 5 DGDE 3 The surface morphology of Ag is shown in FIG. 8. As can be seen from FIG. 8, the PMIA fabric surface was smooth and clean, and after modification, the surface was HP-treated 5 DGDE 3 Covering, and after further chemical silver plating, the silver layer is uniformly and compactly arranged on the surface of the modified fabric, and the silver on the surface of the directly silver-plated fabric is not modifiedThe layer is loosely discontinuous.
Test 9
Examination of silver-plated fabrics PMIA/HP in example 16 using a four-probe tester 5 DGDE 3 The Ag conductivity is shown in FIG. 9. As can be seen from FIG. 9, PMIA/HP 5 DGDE 3 The sheet resistance of the/Ag fabric is as low as 10.14mΩ/sq.
Test 10
Investigation of silver-plated fabrics PMIA/HP in example 16 Using a vector network analyzer 5 DGDE 3 The results of the electromagnetic shielding performance/Ag are shown in FIG. 10. As can be seen from FIG. 10, PMIA/HP 5 DGDE 3 The electromagnetic shielding effectiveness of the/Ag fabric is up to about 105dB.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims (6)

1. The preparation method of the conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber is characterized by comprising the following steps of:
(1) Adding ultra-pure water into hyperbranched polyamide-amine, heating and stirring to completely dissolve and disperse the ultra-pure water, dripping a cross-linking agent, magnetically stirring in a constant-temperature water bath, performing cross-linking reaction to obtain a cross-linked hyperbranched polyamide-amine solution, and preserving heat for later use;
(2) Extracting the aramid fiber with absolute ethyl alcohol, washing, drying, immersing the aramid fiber into the cross-linked hyperbranched polyamide-amine solution obtained in the step (1), taking out and drying to obtain the cross-linked hyperbranched polyamide-amine modified meta-aramid fiber;
(3) Immersing the cross-linked hyperbranched polyamide-amine modified meta-aramid fiber obtained in the step (2) into silver ammonia solution, starting ultrasonic, performing silver ion ultrasonic adsorption, after the adsorption is completed, maintaining ultrasonic, dropwise adding glucose solution dropwise for ultrasonic reduction, standing, filtering, washing the filtrate with ultrapure water, and vacuum drying to obtain the cross-linked dendrimer silver-plated meta-aramid fiber.
2. The method of claim 1, wherein the aramid is one of an aramid fiber, an aramid nonwoven, or an aramid woven.
3. The process according to claim 1 or 2, characterized in that in step (1), the hyperbranched polyamide-amine has a number average molecular weight ranging from 500 to 1000 and a concentration ranging from 0.5 to 40g/L; the cross-linking agent is one of monoepoxy compound, dicycloxy compound, diglycidyl ester or polyepoxy compound, and the molar ratio of the cross-linking agent to hyperbranched polyamide-amine is (0.1-12) 1; the crosslinking reaction time is 0.5-12h; the water bath temperature is 10-100 ℃, and the magnetic stirring speed is 120-2400rpm.
4. A method according to claim 3, wherein the monoepoxy compound is epichlorohydrin, epibromohydrin or epoxypropionic acid; the bisoxy compound is diglycidyl ether, ethylene glycol diglycidyl ether, diethylene glycol diglycidyl ether, 1, 4-butanediol diglycidyl ether, poly (propylene glycol diglycidyl ether), bisphenol a diglycidyl ether, resorcinol diglycidyl ether or poly (dimethylsiloxane) diglycidyl ether; the diglycidyl esters are diglycidyl phthalate, diglycidyl adipate or diglycidyl aniline; the polyepoxy compound is glycerol triglycidyl ether or pentaerythritol triglycidyl ether.
5. The method according to claim 1 or 2, wherein in step (2), the soaking time is 0.5 to 6 hours.
6. The method according to claim 1 or 2, wherein in step (3), the ultrasonic frequency is 40KHz, the power is 120-360W, the ultrasonic adsorption time is 0.1-3h, and the ultrasonic reduction time is 0.5-4h; the vacuum drying temperature is 30-90 ℃ and the time is 6-24h.
CN202310277797.9A 2023-03-21 2023-03-21 Preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber Pending CN116219741A (en)

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Publication number Priority date Publication date Assignee Title
CN104532553A (en) * 2014-12-19 2015-04-22 东华大学 Method for chemical silver-plating of aramid conductive fibers
CN105780493A (en) * 2016-04-19 2016-07-20 东华大学 Making method of cotton fabric having conductive and electromagnetic shielding properties
US20210222358A1 (en) * 2018-05-04 2021-07-22 Soochow University Surface-modified aramid fiber and preparation method therefor
US20210310184A1 (en) * 2018-12-18 2021-10-07 Nantong Textile & Silk Industrial Technology Research Institute Flame-retardant ultraviolet-resistant aramid fiber
CN113512876A (en) * 2021-04-29 2021-10-19 鲁东大学 Preparation method of crosslinked dendrimer-para-aramid silver-plated conductive fiber
CN114225709A (en) * 2021-12-14 2022-03-25 浙江工业大学 Preparation method of super-amphiphilic oil-water separation membrane for fixing in-situ grown silver nanoparticles
CN115323789A (en) * 2022-08-26 2022-11-11 鲁东大学 Preparation method of chemically bonded dendrimer silver-plated conductive para-aramid fiber

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104532553A (en) * 2014-12-19 2015-04-22 东华大学 Method for chemical silver-plating of aramid conductive fibers
CN105780493A (en) * 2016-04-19 2016-07-20 东华大学 Making method of cotton fabric having conductive and electromagnetic shielding properties
US20210222358A1 (en) * 2018-05-04 2021-07-22 Soochow University Surface-modified aramid fiber and preparation method therefor
US20210310184A1 (en) * 2018-12-18 2021-10-07 Nantong Textile & Silk Industrial Technology Research Institute Flame-retardant ultraviolet-resistant aramid fiber
CN113512876A (en) * 2021-04-29 2021-10-19 鲁东大学 Preparation method of crosslinked dendrimer-para-aramid silver-plated conductive fiber
CN114225709A (en) * 2021-12-14 2022-03-25 浙江工业大学 Preparation method of super-amphiphilic oil-water separation membrane for fixing in-situ grown silver nanoparticles
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