CN113652860A - Sock with electromagnetic shielding function for pilot and preparation method thereof - Google Patents

Sock with electromagnetic shielding function for pilot and preparation method thereof Download PDF

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Publication number
CN113652860A
CN113652860A CN202110998407.8A CN202110998407A CN113652860A CN 113652860 A CN113652860 A CN 113652860A CN 202110998407 A CN202110998407 A CN 202110998407A CN 113652860 A CN113652860 A CN 113652860A
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Prior art keywords
soaking
fiber
solution
minutes
nylon fiber
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CN113652860B (en
Inventor
邱婧
吴国栋
卜庆革
王卫红
邢军
侯登才
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Qingdao Hengtong X Silver Specialty Textile Co ltd
Pla 93114
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Qingdao Hengtong X Silver Specialty Textile Co ltd
Pla 93114
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    • 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
    • D06M11/83—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
    • A—HUMAN NECESSITIES
    • A41—WEARING APPAREL
    • A41B—SHIRTS; UNDERWEAR; BABY LINEN; HANDKERCHIEFS
    • A41B11/00—Hosiery; Panti-hose
    • A—HUMAN NECESSITIES
    • A41—WEARING APPAREL
    • A41B—SHIRTS; UNDERWEAR; BABY LINEN; HANDKERCHIEFS
    • A41B17/00—Selection of special materials for underwear
    • 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
    • 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
    • D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
    • 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • 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
    • D06M13/11—Compounds containing epoxy groups or precursors 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
    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322—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 nitrogen
    • D06M13/325—Amines
    • D06M13/328—Amines the amino group being bound to an acyclic or cycloaliphatic carbon atom
    • 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
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides 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
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • 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
    • D06M2101/34—Polyamides

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Chemical Or Physical Treatment Of Fibers (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

The invention discloses a sock with an electromagnetic shielding function for pilots and a preparation method thereof. The socks prepared by the invention have good flexibility, high strength, good conductivity and electromagnetic shielding performance, especially have excellent shielding value for electromagnetic radiation with radio frequency of 10MHZ to 40GHz, and can be applied to electronic countermeasure environment to protect the feet of pilots.

Description

Sock with electromagnetic shielding function for pilot and preparation method thereof
Technical Field
The invention relates to the field of military materials, in particular to a sock with an electromagnetic shielding function for pilots and a preparation method thereof.
Background
When electronic equipment or equipment is used for electronic countermeasure, electromagnetic radiation sources in the environment are dense, electromagnetic spectrum is complex, almost all frequency spectrums from long wave, short wave, microwave, millimeter wave, infrared to ultraviolet are covered, influence on human bodies is diversified, for example, time Lanchun and the like disclose that electromagnetic radiation can influence the kidney function of officers and soldiers in electronic countermeasure troops and the number and the composition of peripheral blood cells. See release military preventive medicine journal, Vol.34, No. 5, 2016, 10 months. The married couple and the like reviewed the damage mechanism of electromagnetic radiation in their "research progress of electromagnetic radiation on damage to living bodies". The health impact of electromagnetic radiation is becoming increasingly appreciated, requiring the necessary protection of certain personnel.
The air force carries out certain electromagnetic protection in the electronic combat, but lacks special protection measures for body parts such as feet. Currently, socks for pilots are common socks and are not specially treated, and the socks mainly focus on the performances of comfort, deodorization and the like and have no protective performance.
The information in this background is only for the purpose of illustrating the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art that is known to a person skilled in the art.
Disclosure of Invention
In order to solve at least part of technical problems in the prior art, the invention provides a sock with an electromagnetic shielding function for a pilot and a preparation method thereof, wherein the sock has an excellent electromagnetic shielding effect, is durable and can be used in an electronic combat environment. Specifically, the present invention includes the following.
In a first aspect of the present invention, there is provided a method for preparing socks for pilots with electromagnetic shielding function, which includes a step of preparing functionalized nylon fibers, specifically including:
(1) soaking nylon fiber raw material in silver salt solution at 35-45 deg.C for 30-60 min, drying at 40-50 deg.C, soaking in alkali liquor at 50-65 deg.C for 30-50 min, and drying;
(2) soaking the nylon fiber obtained in the step (1) into a crosslinking solution containing cysteamine or salt thereof, and soaking at 45-55 ℃;
(3) soaking the nylon fiber obtained in the step (2) in a mixed aqueous solution of sodium citrate and tetrachloropalladate (II) acid; and
(4) soaking the nylon fiber obtained in the step (3) into a copper salt-containing reaction solution for reaction for 10-30 minutes, soaking and washing the obtained fiber with deionized water for 15-40 minutes, and drying.
According to the preparation method of the first aspect of the present invention, preferably, the copper salt-containing reaction solution is an aqueous solution containing copper sulfate, sodium tartrate, disodium ethylenediaminetetraacetate, sodium hydroxide, sodium carbonate, formaldehyde, ethanol, bipyridine, potassium ferrocyanide, and nickel chloride.
According to the production method of the first aspect of the present invention, preferably, the silver salt is a silver salt of fulvic acid or a silver nitrate salt.
According to the preparation method of the first aspect of the present invention, preferably, the temperature of the mixed aqueous solution is 45 to 60 ℃ for 50 to 100 minutes.
The preparation method according to the first aspect of the present invention, preferably, further comprises a step of washing the nylon fiber with an emulsifier-containing alkali solution before the step (1).
According to the production method of the first aspect of the present invention, preferably, the silver salt solution contains cetyltrimethylammonium bromide and sodium dodecylbenzenesulfonate.
According to the production method of the first aspect of the present invention, preferably, the silver salt solution further contains epichlorohydrin.
According to the preparation method of the first aspect of the present invention, preferably, the nylon fabric has a surface resistance of 0.05 ohm/cm or less and a shielding effectiveness of 10MHZ to 40 GHZ.
In a second aspect of the present invention, there is provided a sock for pilots with electromagnetic shielding function, which is prepared by the preparation method of the first aspect.
The functional fiber obtained by the invention can keep the characteristics of the original fiber such as flexibility, bending resistance, strength and the like, has good conductivity and electromagnetic shielding performance, particularly has a high shielding value for electromagnetic radiation with the radio frequency of 10MHZ to 40GHz, has important significance for aerospace lightweight, and can be applied to various electronic countermeasure environments.
In addition, the functionalized nylon fiber does not need a chemical coarsening process during preparation, avoids using toxic and harmful substances, does not damage the structure of the original fiber, and keeps higher strength.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that the upper and lower limits of the range, and each intervening value therebetween, is specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control. Unless otherwise indicated, "%" is percent by weight.
The sock is special for pilots, and is particularly suitable for protecting feet in environments with complex electromagnetic radiation generated by electronic fight. The sock has excellent electromagnetic shielding effect, the shielding effectiveness is 10 MHZ-40 GHZ, and the DB value is 65 DB-70 DB. In addition, after long-term use, the shielding effect of the protective socks is basically not attenuated, and the socks are durable.
The sock body comprises a nylon fabric layer with an electromagnetic shielding function. The nylon fabric layer is knitted or woven from a special nylon fiber material (sometimes referred to herein simply as "functionalized nylon fiber"). The functional nylon fiber has metal particles on the surface of the raw material, more importantly, in the interior of the raw material, and the nylon fiber has excellent electromagnetic shielding function through metallization treatment.
In the invention, the functionalized nylon fiber is prepared by a special preparation process, and comprises metal inside the fiber and metal outside the fiber, wherein the metal and the metal are preferably different metals, and preferably two metals respectively having shielding effects on different frequency bands. The preparation of the nylon fiber of the present invention is explained below.
The preparation method of the functionalized nylon fiber comprises the following steps: soaking the pretreated nylon fiber in a mixed aqueous solution of sodium citrate and tetrachloropalladium (II) acid, further soaking the nylon fiber in a copper salt-containing reaction solution for reaction for 10 to 30 minutes, soaking and washing the obtained fiber in deionized water for 15 to 40 minutes, and drying the fiber to obtain the nylon fiber. The metal is strongly bonded to the fiber surface by the above treatment, particularly the treatment of the mixed aqueous solution.
In the present invention, the mixed aqueous solution contains sodium citrate and tetrachloropalladate (II) acid (H)2PdCl4) Wherein the concentration of sodium citrate is generally 0.1-0.5M/L, preferably 0.2-0.3M/L. The concentration of tetrachloropalladium (II) acid is generally 0.01 to 0.10M/L, preferably 0.03 to 0.07M/L. The impregnation temperature is generally50-70 deg.C, preferably 55-60 deg.C. The soaking time is 40-120 minutes. By this step, metal palladium particles can be formed on the surface of the fiber, and the metal palladium particles serve as active centers to further reduce other metals to the surface of the fiber. The surface metallized fiber obtained by the method has stronger metal bonding force. The reason for this may be that active metal palladium particles are formed on the surface of the fiber, then other metals are more easily reduced, and the reduced metal crystal nuclei themselves become catalytic layers of metal ions, so that the reduction reaction of the plating metal continues on the surfaces of the new crystal nuclei, thereby improving the hardness, metal coverage uniformity and corrosion resistance of the functionalized fiber.
In the present invention, the reaction solution containing a copper salt contains a copper salt, a reducing agent, a complexing agent, and preferably an aqueous solution further containing a stabilizer, a pH adjuster, and an accelerator. In order to improve the performance of the reaction solution, other components may be further included. In some preferred embodiments of the present invention, some surfactant is also added to the electroless copper plating solution, for example, to reduce the surface tension of the copper salt-containing reaction solution and improve the quality of the plated layer. The copper metal layer is formed on the surface of the fiber through the treatment of the copper salt-containing reaction solution, so that the obtained fabric can further form a mesh-shaped shielding layer of copper metal for high-frequency radiation protection.
In the present invention, as the copper salt, examples thereof include, but are not limited to, copper sulfate, copper chloride, basic copper carbonate, copper tartrate and copper acetate, for example, and one or more of them may be used in the present invention. As the reducing agent, examples thereof include, but are not limited to, formaldehyde, sodium hypophosphite, and dimethylaminoborane, one or more of which may be used in the present invention. As the complexing agent, examples thereof include, but are not limited to, for example, sodium tartrate, sodium citrate, sodium gluconate, triethanolamine, tetrahydroxypropylethylenediamine, glycerin, glycolic acid, and EDTA, one or more of which may be used in the present invention. As the stabilizer, an effect for stabilizing the plating solution and improving the quality of the plating layer, and examples thereof include, but are not limited to, for example, methanol, thiourea, alkyl mercaptan and dihydroxybenzene, one or more of which may be used in the present invention. Examples thereof include, but are not limited to, sodium hydroxide or sodium carbonate, for example, as a conditioning agent. As the accelerator, it is used for improving the plating rate and the quality of the plating layer, and examples thereof include, but are not limited to, ammonium salts, nitrates, and polyoxyethylene amino ethers, for example. One or more of which may be used in the present invention.
In certain embodiments, the copper salt-containing reaction solution of the present invention comprises an aqueous solution of copper sulfate, sodium tartrate, disodium ethylenediaminetetraacetate, sodium hydroxide, sodium carbonate, formaldehyde, ethanol, bipyridine, potassium ferrocyanide, and nickel chloride. Preferably, the weight ratio of copper sulfate: and (3) the mass g of sodium tartrate: the mass g of the ethylene diamine tetraacetic acid disodium salt is as follows: sodium hydroxide mass g: sodium carbonate mass g: formaldehyde volume mL: ethanol volume mL: the mass mg of bipyridine is: the mass mg of ferrous potassium thiocyanate: the mass g of nickel chloride is as follows: ratio of volume of water L10: 25: 25: 10: 3: 20: 15: 15: 15: 1: 1, preparing a mixed solution.
In the invention, the nylon fiber needs to be pretreated before being soaked in the mixed aqueous solution, thereby further improving the performance of the nylon fiber. Preferably, the pretreatment comprises the steps of immersing the nylon fiber raw material into a silver salt solution, immersing at 35-45 ℃ for 30-60 minutes, and drying at 40-50 ℃; then immersing in alkali liquor to treat at 50-65 deg.C for 30-50 min, and drying. The pretreatment can make silver ions permeate into the fiber, and avoid the adverse effects caused by the silver ions bonded on the surface of the fiber, such as easy oxidation or loose silver ion bonding. Meanwhile, the electromagnetic shielding effect is further enhanced, and particularly the electromagnetic shielding effect on different frequency bands is enhanced.
In the present invention, the silver salt solution contains an aqueous solution of silver salt, cetyltrimethylammonium bromide, and sodium dodecylbenzenesulfonate. The silver salt is generally contained in an amount of 5 to 7 parts by weight, cetyltrimethylammonium bromide is generally used in an amount of 4 to 9 parts by weight, and sodium dodecylbenzenesulfonate is generally used in an amount of 4 to 10 parts by weight, based on 1000 parts by weight of water. The silver salt solution may further comprise other ingredients such as a gel, typically in an amount of 2 to 4 parts by weight. The preparation of the silver salt solution comprises mixing the components, stirring at 30-35 ℃ and 250-350 r/min for 0.5-1.5 h, and then performing microwave treatment for 10-20 min. Preferably, the silver salt solution further comprises epichlorohydrin to enhance the access of silver ions to the interior of the fiber, generally in an amount of 6.58% or less, such as 5%, 4%, etc. If the content is too high, the silver salt solution tends to be turbid, which is disadvantageous in the progress of the reaction.
In the invention, the alkali liquor is an aqueous solution containing cyclodextrin and sodium hydroxide or potassium hydroxide. Preferably, the cyclodextrin is β -cyclodextrin. The amount of cyclodextrin in the alkali solution is generally 100-150 parts by weight, and the amount of sodium hydroxide or potassium hydroxide is generally 20-60 parts by weight, based on 1000 parts by weight of water. The binding force of silver ions is further improved after alkali liquor treatment.
In the invention, preferably, a subsequent pretreatment step is further carried out, which comprises soaking the nylon fiber treated by the silver salt solution into a crosslinking solution at 45-55 ℃, so as to further improve the bonding force of metal on the surface of the fiber. It should be noted that the crosslinking solution is used to enhance the bonding between the metal and the fibers, not between the fibers. Wherein the crosslinking solution preferably comprises cysteamine or a salt thereof having two active groups, namely amino groups and mercapto groups, wherein the amino groups can be combined on the surface of the nylon fiber, the mercapto groups can be combined with metal ions, particularly palladium ions, and sodium citrate can reduce the palladium ions to the surface of the nylon fiber to form metal palladium particles.
Example 1
1.5 g of NaOH and 5g of emulsifier are dissolved by 1L of water to prepare washing liquid, the nylon fiber is soaked for 30 minutes at the temperature of 40 ℃, and then the washing liquid is used for washing.
2. Soaking the fiber obtained in the step (1) in a silver salt solution at the temperature of 30 ℃ for 30 minutes, wherein the weight ratio of the fiber to the silver salt solution is 1:5, and then drying the fiber at the temperature of 45 ℃; then soaking in alkali liquor at 55 deg.C for 30 min at a fiber/alkali liquor weight ratio of 1:3, and drying at 50 deg.C. Wherein the silver salt solution comprises 5% of silver nitrate salt, 6% of hexadecyl trimethyl ammonium bromide, 7% of sodium dodecyl benzene sulfonate and 2% of gel.
3. And (3) soaking the nylon fiber obtained in the step (2) into 0.1M/L cysteamine hydrochloride solution, wherein the soaking temperature is 50 ℃, and the soaking time is 40 minutes.
4. Soaking the fiber obtained in the step (3) into sodium citrate and H2PdCl4The activated nylon fiber with Pd particles loaded on the surface is obtained in the mixed aqueous solution, wherein the concentration of sodium citrate is 0.25M/L, H2PdCl4The concentration of the active ingredients is 0.04M/L, the soaking temperature is 50 ℃, and the soaking time is 80 minutes.
5. And (3) adjusting the temperature of the copper-containing reaction solution to 30 ℃, immersing the fiber obtained in the step (4) into the copper-containing reaction solution for reaction for 20 minutes, then soaking and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the functionalized nylon fiber 1. The electromagnetic shielding property of the functionalized nylon fiber 1 is excellent after long-term use.
Example 2
1.5 g of NaOH and 5g of emulsifier are dissolved by 1L of water to prepare washing liquid, the nylon fiber is soaked for 30 minutes at the temperature of 40 ℃, and then the washing liquid is used for washing.
2. Soaking the fiber obtained in the step (1) in a silver salt solution at the temperature of 30 ℃ for 30 minutes, wherein the weight ratio of the fiber to the silver salt solution is 1:5, and then drying the fiber at the temperature of 45 ℃; then soaking in alkali liquor at 55 deg.C for 30 min at a fiber/alkali liquor weight ratio of 1:4, and drying at 50 deg.C. Wherein the silver salt solution comprises 5% of fulvic acid silver salt, 6% of hexadecyl trimethyl ammonium bromide, 7% of sodium dodecyl benzene sulfonate and 5% of epoxy chloropropane.
3. And (3) soaking the nylon fiber obtained in the step (2) into 0.2M/L cysteamine hydrochloride solution, wherein the soaking temperature is 55 ℃, and the soaking time is 30 minutes.
4. Soaking the fiber obtained in the step (3) into sodium citrate and H2PdCl4The activated nylon fiber with Pd particles loaded on the surface is obtained in the mixed aqueous solution, wherein the concentration of sodium citrate is 0.3M/L, H2PdCl4The concentration of (A) is 0.05M/L, the soaking temperature is 50 ℃, and the soaking time is 80 minutes.
5. And (3) adjusting the temperature of the copper-containing reaction solution to 30 ℃, immersing the fiber obtained in the step (4) into the copper-containing reaction solution for reaction for 20 minutes, then soaking and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the functionalized nylon fiber 2. The electromagnetic shielding property of the functionalized nylon fiber 2 is excellent after long-term use.
Example 3
1.5 g of NaOH and 5g of emulsifier are dissolved by 1L of water to prepare washing liquid, the nylon fiber is soaked for 30 minutes at the temperature of 40 ℃, and then the washing liquid is used for washing.
2. Soaking the fiber obtained in the step (1) in a silver salt solution at the temperature of 30 ℃ for 30 minutes, wherein the weight ratio of the fiber to the silver salt solution is 1:5, and then drying the fiber at the temperature of 45 ℃; then soaking in alkali liquor at 55 deg.C for 30 min at a fiber/alkali liquor weight ratio of 1:4, and drying at 50 deg.C. Wherein the silver salt solution comprises 5% of fulvic acid silver salt, 6% of hexadecyl trimethyl ammonium bromide, 7% of sodium dodecyl benzene sulfonate, 5% of epichlorohydrin and 2% of gel.
3. And (3) soaking the nylon fibers obtained in the step (2) into 0.1M/L cysteamine solution at the temperature of 50 ℃ for 40 minutes.
4. Soaking the fiber obtained in the step (3) into sodium citrate and H2PdCl4The activated nylon fiber with Pd particles loaded on the surface is obtained in the mixed aqueous solution, wherein the concentration of sodium citrate is 0.25M/L, H2PdCl4The concentration of the active ingredients is 0.04M/L, the soaking temperature is 50 ℃, and the soaking time is 80 minutes.
5. And (3) adjusting the temperature of the copper-containing reaction solution to 30 ℃, immersing the fiber obtained in the step (4) into the copper-containing reaction solution for reaction for 20 minutes, then soaking and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the functionalized nylon fiber 3. The electromagnetic shielding property of the functionalized nylon fiber 3 is excellent after long-term use.
Comparative example 1
1.5 g of NaOH and 5g of emulsifier are dissolved by 1L of water to prepare washing liquid, the nylon fiber is soaked for 30 minutes at the temperature of 40 ℃, and then the washing liquid is used for washing.
2. Soaking the fiber obtained in the step (1) in a silver salt solution at the temperature of 30 ℃ for 30 minutes, wherein the weight ratio of the fiber to the silver salt solution is 1:5, and then drying the fiber at the temperature of 45 ℃; then soaking in alkali liquor at 55 deg.C for 30 min at a fiber/alkali liquor weight ratio of 1:4, and drying at 50 deg.C. Wherein the silver salt solution comprises 5% of fulvic acid silver salt, 6% of hexadecyl trimethyl ammonium bromide, 7% of sodium dodecyl benzene sulfonate and 5% of epoxy chloropropane.
3. And (3) soaking the nylon fiber obtained in the step (2) into the coarsening solution at the soaking temperature of 55 ℃ for 30 minutes. Wherein the roughening solution is prepared by dissolving 40g of potassium permanganate, 40g of sodium hydroxide, 5g of emulsifier in 1000ml of water.
4. Soaking the fiber obtained in the step (3) into sodium citrate and H2PdCl4The activated nylon fiber with Pd particles loaded on the surface is obtained in the mixed aqueous solution, wherein the concentration of sodium citrate is 0.3M/L, H2PdCl4The concentration of (A) is 0.05M/L, the soaking temperature is 50 ℃, and the soaking time is 80 minutes.
5. And (3) adjusting the temperature of the copper-containing reaction solution to 30 ℃, immersing the fiber obtained in the step (4) into the copper-containing reaction solution for reaction for 20 minutes, then soaking and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the nylon fiber 1 for comparison. The electromagnetic shielding property of the comparative nylon fiber 1 is good after long-term use.
Comparative example 2
1.5 g of NaOH and 5g of emulsifier are dissolved by 1L of water to prepare washing liquid, the nylon fiber is soaked for 30 minutes at the temperature of 40 ℃, and then the washing liquid is used for washing.
2. Soaking the fiber obtained in the step (1) in a silver salt solution at the temperature of 30 ℃ for 30 minutes, wherein the weight ratio of the fiber to the silver salt solution is 1:5, and then drying the fiber at the temperature of 45 ℃; then soaking in alkali liquor at 55 deg.C for 30 min at a fiber/alkali liquor weight ratio of 1:4, and drying at 50 deg.C. Wherein the silver salt solution comprises 5% of fulvic acid silver salt, 6% of hexadecyl trimethyl ammonium bromide, 7% of sodium dodecyl benzene sulfonate and 5% of epoxy chloropropane.
3. And (3) soaking the nylon fiber obtained in the step (2) into 0.2M/L cysteamine hydrochloride solution, wherein the soaking temperature is 55 ℃, and the soaking time is 30 minutes.
4. And (3) soaking the fiber obtained in the step (3) into a copper-containing reaction solution, adjusting the temperature to 30 ℃, reacting for 20 minutes, soaking and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the comparative nylon fiber 2. The electromagnetic shielding property of the comparative nylon fiber 2 was poor after long-term use.
Comparative example 3
1.5 g of NaOH and 5g of emulsifier are dissolved by 1L of water to prepare washing liquid, the nylon fiber is soaked for 30 minutes at the temperature of 40 ℃, and then the washing liquid is used for washing.
2. Soaking the nylon fiber obtained in the step (1) into 0.1M/L cysteamine solution, wherein the soaking temperature is 50 ℃, and the soaking time is 40 minutes.
3. Soaking the fiber obtained in the step (2) into sodium citrate and H2PdCl4The activated nylon fiber with Pd particles loaded on the surface is obtained in the mixed aqueous solution, wherein the concentration of sodium citrate is 0.25M/L, H2PdCl4The concentration of the active ingredients is 0.04M/L, the soaking temperature is 50 ℃, and the soaking time is 80 minutes.
4. And (4) immersing the fiber obtained in the step (3) into a silver salt solution, and reacting for 10 minutes at 90 ℃ under the condition of compressed air stirring to obtain the nylon fiber 3. Wherein the silver salt solution is prepared as follows: dissolving 5g of silver nitrate, 20g of ammonium citrate, 25g of formaldehyde, 30 g of methanol and 15 g of malonic acid by using 1L of deionized water, and then adjusting the pH of the solution to 5.0-5.5 by using sodium hydroxide.
5. And (3) adjusting the temperature of the copper-containing reaction solution to 30 ℃, immersing the fiber obtained in the step (4) into the copper-containing reaction solution for reaction for 20 minutes, then soaking and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the comparative nylon fiber 3. The electromagnetic shielding property of the comparative nylon fiber 3 was poor after long-term use.
The properties of the nylon fibers of the examples and comparative examples were measured, and the results are shown in Table 1. It can be seen that the functional nylon fibers prepared in the embodiments 1 to 3 of the present invention are superior to those of the comparative examples 1 to 3 in strength, conductivity and strength, which indicates that the preparation method provided by the present invention is simple and convenient to operate, and the prepared functional fibers not only have good conductivity, but also have good flexibility, strength and electromagnetic shielding effect.
TABLE 1
Figure BDA0003234605780000101
Figure BDA0003234605780000111
While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. Many modifications and variations may be made to the exemplary embodiments of the present description without departing from the scope or spirit of the present invention. The scope of the claims is to be accorded the broadest interpretation so as to encompass all modifications and equivalent structures and functions.

Claims (9)

1. A preparation method of socks with electromagnetic shielding function for pilots is characterized by comprising the step of preparing functional nylon fibers, and comprises the following steps:
(1) soaking nylon fiber raw material in silver salt solution at 35-45 deg.C for 30-60 min, drying at 40-50 deg.C, soaking in alkali liquor at 50-65 deg.C for 30-50 min, and drying;
(2) soaking the nylon fiber obtained in the step (1) into a crosslinking solution containing cysteamine or salt thereof, and soaking at 45-55 ℃;
(3) soaking the nylon fiber obtained in the step (2) in a mixed aqueous solution of sodium citrate and tetrachloropalladate (II) acid; and
(4) soaking the nylon fiber obtained in the step (3) into a copper salt-containing reaction solution for reaction for 10-30 minutes, soaking and washing the obtained fiber with deionized water for 15-40 minutes, and drying.
2. The method according to claim 1, wherein the copper salt-containing reaction solution is an aqueous solution containing copper sulfate, sodium tartrate, disodium ethylenediaminetetraacetate, sodium hydroxide, sodium carbonate, formaldehyde, ethanol, bipyridine, potassium ferrocyanide, and nickel chloride.
3. The method of claim 1, wherein the silver salt is a silver salt of fulvic acid or a silver nitrate salt.
4. The method according to claim 1, wherein the temperature of the mixed aqueous solution is 45 to 60 ℃ for 50 to 100 minutes.
5. The method of claim 1, wherein step (1) is preceded by a step of washing the nylon fiber with an emulsifier-containing lye.
6. The method of claim 1, wherein the silver salt solution comprises cetyltrimethylammonium bromide and sodium dodecylbenzenesulfonate.
7. The method according to claim 6, characterized in that the silver salt solution further comprises epichlorohydrin.
8. The method as claimed in claim 1, wherein the nylon fabric has a surface resistance of 0.05 ohm/cm or less and a shielding effectiveness of 10MHZ to 40 GHZ.
9. A sock for pilots with electromagnetic shielding function, characterized by being prepared by the preparation method according to any one of claims 1 to 8.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1280223A (en) * 1999-07-07 2001-01-17 刘绍芝 Fabric for shielding electromagnetic wave and its producing method
CN106702356A (en) * 2017-01-12 2017-05-24 卜庆革 Conductive polyimide fibers and product and preparation method thereof
CN108221368A (en) * 2017-12-15 2018-06-29 华南理工大学 A kind of conductive fabric and preparation method thereof
CN109440461A (en) * 2018-11-08 2019-03-08 珠海鑫康源新材料科技有限公司 Novel antibacterial radiation protection silver seeps solid fabric lining and preparation method thereof
CN112980034A (en) * 2021-02-26 2021-06-18 清华大学深圳国际研究生院 Electromagnetic shielding film and preparation method thereof
CN113235295A (en) * 2021-04-30 2021-08-10 青岛天银纺织科技有限公司 Mixed metal nuclear radiation resistant material and preparation method and garment thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1280223A (en) * 1999-07-07 2001-01-17 刘绍芝 Fabric for shielding electromagnetic wave and its producing method
CN106702356A (en) * 2017-01-12 2017-05-24 卜庆革 Conductive polyimide fibers and product and preparation method thereof
CN108221368A (en) * 2017-12-15 2018-06-29 华南理工大学 A kind of conductive fabric and preparation method thereof
CN109440461A (en) * 2018-11-08 2019-03-08 珠海鑫康源新材料科技有限公司 Novel antibacterial radiation protection silver seeps solid fabric lining and preparation method thereof
CN112980034A (en) * 2021-02-26 2021-06-18 清华大学深圳国际研究生院 Electromagnetic shielding film and preparation method thereof
CN113235295A (en) * 2021-04-30 2021-08-10 青岛天银纺织科技有限公司 Mixed metal nuclear radiation resistant material and preparation method and garment thereof

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