CN113652860B - Pilot sock with electromagnetic shielding function and preparation method thereof - Google Patents

Pilot sock with electromagnetic shielding function and preparation method thereof Download PDF

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Publication number
CN113652860B
CN113652860B CN202110998407.8A CN202110998407A CN113652860B CN 113652860 B CN113652860 B CN 113652860B CN 202110998407 A CN202110998407 A CN 202110998407A CN 113652860 B CN113652860 B CN 113652860B
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minutes
immersing
parts
weight
fiber
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CN113652860A (en
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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)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
  • Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)

Abstract

The invention discloses a pilot sock with an electromagnetic shielding function and a preparation method thereof. The sock prepared by the invention has good flexibility, high strength, good conductivity and electromagnetic shielding performance, particularly has excellent shielding value for electromagnetic radiation of radio frequency ranging from 10MHz to 40GHz, and can be applied to electronic countermeasure environment for protecting the feet of pilots.

Description

Pilot sock with electromagnetic shielding function and preparation method thereof
Technical Field
The invention relates to the field of military materials, in particular to a pilot sock with an electromagnetic shielding function and a preparation method thereof.
Background
When electronic equipment or equipment is utilized 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 Shi Lanchun and the like disclose that electromagnetic radiation can influence renal functions and peripheral blood cell numbers and compositions of officers and soldiers of electronic countermeasure armies. See, J.Release army preventive medicine, vol.34, 5 th, month 10 in 2016. Zhou Qingluan et al reviewed the mechanism of damage by electromagnetic radiation in its progress of "research of damage to organisms by electromagnetic radiation". Electromagnetic radiation is increasingly gaining importance for health and requires the necessary protection of specific personnel.
Air force performs certain electromagnetic protection during electronic combat operations, but lacks special protection measures for body parts such as feet. Currently, the socks for pilots are general socks, which are not specially treated, and are mainly focused on comfort, deodorization and other performances, and have no protective performance.
The information in the background section is only for the purpose of illustrating the general background of the invention and is not to be construed as an admission or any form of suggestion that such information forms the prior art that is well known to those of ordinary skill in the art.
Disclosure of Invention
In order to solve at least part of the technical problems in the prior art, the invention provides the pilot sock with the electromagnetic shielding function and the preparation method thereof, wherein the sock has an excellent electromagnetic shielding effect, is durable and can be used for an electronic fight against environment. Specifically, the present invention includes the following.
In a first aspect of the present invention, a method for preparing a pilot sock with electromagnetic shielding function is provided, comprising the steps of preparing functionalized nylon fibers, specifically comprising:
(1) Immersing nylon fiber raw material in silver salt solution, immersing at 35-45 ℃ for 30-60 minutes, drying at 40-50 ℃, immersing in alkali liquor, treating at 50-65 ℃ for 30-50 minutes, and then drying;
(2) Soaking the nylon fiber obtained in the step (1) into a cross-linking 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 tetrachloropalladiumacid (II); and
(4) Immersing the nylon fiber obtained in the step (3) into copper salt-containing reaction liquid for reaction for 10-30 minutes, immersing and washing the obtained fiber with deionized water for 15-40 minutes, and drying.
According to the production 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 ethylenediamine tetraacetate, sodium hydroxide, sodium carbonate, formaldehyde, ethanol, bipyridine, potassium ferrocyanide, and nickel chloride.
According to the preparation method of the first aspect of the present invention, preferably, the silver salt is a silver fulvate salt 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 at the time of soaking is 45-60 ℃ for 50-100 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 alkali solution containing an emulsifier 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 invention, preferably, the surface resistance of the nylon fabric is below 0.05 ohm per cm, and the shielding effectiveness is between 10MHz and 40 GHz.
In a second aspect of the invention, there is provided a pilot sock having electromagnetic shielding function, prepared by the preparation method of the first aspect.
The functional fiber obtained by the invention can keep the flexibility, bending resistance, strength and other characteristics of the fibril, has good conductivity and electromagnetic shielding performance, has higher shielding value for electromagnetic radiation of 10MHz to 40GHz of radio frequency, has great significance for aerospace lightweight, and can be applied to various electronic countermeasure environments.
In addition, the functionalized nylon fiber does not need chemical roughening process during preparation, so that the use of some toxic and harmful substances is avoided, the structure of the fibril is not damaged, and the prepared functionalized fiber keeps higher strength.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions 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. In addition, for numerical ranges in the present invention, it is understood that the upper and lower limits of the ranges and each intermediate value therebetween are specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, 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 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 an environment where complex electromagnetic radiation is generated by electronics against combat. The sock has excellent electromagnetic shielding effect, the shielding efficiency 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 protective socks are durable.
The sock body of the invention comprises a nylon fabric layer with 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 fibers"). The functional nylon fiber not only has metal particles on the surface of the raw material, but also has excellent electromagnetic shielding function through metallization treatment.
In the invention, the functional nylon fiber is prepared by a special preparation process and comprises metal in the fiber and metal outside, wherein the metal is preferably different metals, and the metal is preferably two metals with shielding effects on different frequency bands respectively. The preparation of the nylon fiber of the present invention is described below.
The preparation method of the functionalized nylon fiber comprises the following steps: and (3) soaking the pretreated nylon fiber in a mixed aqueous solution of sodium citrate and tetrachloropalladiumII acid, further soaking in a copper salt-containing reaction solution for reaction for 10-30 minutes, soaking and washing the obtained fiber in deionized water for 15-40 minutes, and drying to obtain the nylon fiber. The metal is firmly 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, palladium (II) tetrachloride acid (H 2 PdCl 4 ) Wherein the concentration of sodium citrate is generally 0.1-0.5M/L, preferably 0.2-0.3M/L. The concentration of the palladium (II) tetrachloride acid is generally 0.01 to 0.10M/L, preferably 0.03 to 0.07M/L. The impregnation temperature is generally 50-70℃and preferably 55-60 ℃. The soaking time is 40-120 minutes. By this step, metallic palladium particles can be formed on the surface of the fiber, and the metallic 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 binding force. The reason for this may be that active metal palladium particles are formed on the surface of the fiber, and then other metals are more easily reduced, and the reduced metal nuclei themselves become catalytic layers of metal ions, so that the reduction reaction of the plating metal continues on the new nuclei surfaces, thereby improving the hardness, metal coverage uniformity and corrosion resistance of the functionalized fiber.
In the present invention, the copper salt-containing reaction liquid contains a copper salt, a reducing agent, and a complexing agent, and preferably further contains an aqueous solution of a stabilizer, a pH adjustor, and an accelerator. Other components may be further contained in order to improve the performance of the reaction solution. For example, to reduce the surface tension of the copper salt-containing reaction solution and improve the coating quality, in preferred embodiments of the invention, some surfactant is also added to the electroless copper plating solution. The copper metal layer is formed on the surface of the fiber by the treatment of the copper salt-containing reaction liquid, and the obtained fabric can further form a reticular shielding layer of copper metal for high-frequency radiation protection.
In the present invention, as copper salts, 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 thereof may be used in the present invention. Examples of reducing agents include, but are not limited to, formaldehyde, sodium hypophosphite, and dimethylaminoborane, one or more of which may be used in the present invention. Examples of complexing agents include, but are not limited to, sodium tartrate, sodium citrate, sodium gluconate, triethanolamine, tetrahydroxypropyl ethylenediamine, glycerol, glycolic acid, and EDTA, for example, one or more of which may be used in the present invention. As the stabilizer, for stabilizing the plating solution and improving the quality of the plating layer, examples thereof include, but are not limited to, for example, methanol, thiourea, alkyl thiols and dihydroxybenzene, and one or more thereof may be used in the present invention. Examples of the regulator include, but are not limited to, sodium hydroxide or sodium carbonate, for example. As the accelerator, which is used to improve plating speed and plating quality, 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 with 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 ethylenediamine tetraacetate, sodium hydroxide, sodium carbonate, formaldehyde, ethanol, bipyridine, potassium ferrothiocyanide, and nickel chloride. Preferably, the weight of copper sulfate g: sodium tartrate mass g: disodium edetate mass g: sodium hydroxide mass g: sodium carbonate mass g: formaldehyde volume mL: ethanol volume mL: bipyridine mass mg: potassium ferrothiocyanide mass mg: nickel chloride mass g: the ratio of the volume L of water is 10:25:25:10:3:20:15:15:15:1: 1.
In the invention, pretreatment is needed before the nylon fiber is soaked in the mixed aqueous solution, so that the performance of the nylon fiber is further improved. Preferably, the pretreatment comprises immersing the nylon fiber raw material in silver salt solution, immersing at 35-45 ℃ for 30-60 minutes, and drying at 40-50 ℃; then immersing in alkali liquor for 30-50 minutes at 50-65 ℃ and then drying. By this pretreatment, silver ions can be infiltrated into the fiber, and adverse effects caused by bonding of silver ions to the fiber surface, such as easy oxidation or weak bonding of silver ions and falling off, can be avoided. And simultaneously, the electromagnetic shielding effect is further enhanced, and particularly, the electromagnetic shielding effect on electromagnetic waves in 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 used 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 silver salt solution is prepared by mixing the components, stirring at 30-35deg.C and 250-350 r/min for 0.5-1.5 hr, and microwave treating for 10-20 min. Preferably, the silver salt solution further comprises epichlorohydrin to enhance the entry of silver ions into the fiber, typically in an amount of less than 6.58%, such as 5%, 4%, etc. If the content is too high, the silver salt solution tends to be turbid, which is detrimental to the progress of the reaction.
In the present invention, the lye is an aqueous solution comprising cyclodextrin and sodium hydroxide or potassium hydroxide. Preferably, the cyclodextrin is beta-cyclodextrin. The cyclodextrin is generally used in an amount of 100 to 150 parts by weight, and the sodium hydroxide or potassium hydroxide is generally used in an amount of 20 to 60 parts by weight, based on 1000 parts by weight of water. After alkali liquor treatment, the binding force of silver ions is further improved.
In the present invention, preferably, a subsequent pretreatment step is further performed, which includes immersing the nylon fiber treated with the silver salt solution in a crosslinking solution at 45-55 ℃ to further enhance the binding force of the metal on the fiber surface. 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 cross-linking solution preferably comprises cysteamine or a salt thereof, which has two active groups of amino groups and mercapto groups, wherein the amino groups are capable of binding to the surface of the nylon fiber and the mercapto groups are capable of binding to metal ions, particularly palladium ions, and sodium citrate is capable of reducing the palladium ions to the surface of the nylon fiber to form metallic palladium particles.
Example 1
1.5 g of NaOH and 5g of emulsifier are dissolved in 1L of water to prepare a washing liquid, and nylon fibers are soaked for 30 minutes at 40 ℃ and then washed by water.
2. Immersing the fibers in the step (1) into silver salt solution at the immersion temperature of 30 ℃ for 30 minutes, wherein the weight ratio of the fibers to the silver salt solution is 1:5, and then drying the fibers at 45 ℃; then immersing in alkali liquor at 55 ℃ for 30 minutes, wherein the weight ratio of the fiber to the alkali liquor is 1:3, and then drying at 50 ℃. Wherein the silver salt solution comprises 5% silver nitrate, 6% cetyltrimethylammonium bromide, 7% sodium dodecyl benzene sulfonate and 2% gel.
3. And (3) soaking the nylon fiber in the step (2) into 0.1M/L cysteamine hydrochloride solution at a temperature of 50 ℃ for 40 minutes.
4. Immersing the fiber of the step (3) into sodium citrate and H 2 PdCl 4 Activated nylon fiber with Pd particles supported on the surface is obtained, wherein the concentration of sodium citrate is 0.25M/L, H 2 PdCl 4 The concentration of (2) was 0.04M/L, the soaking temperature was 50℃and the soaking time was 80 minutes.
5. And (3) regulating the temperature of the copper-containing reaction liquid to 30 ℃, immersing the fiber obtained in the step (4) into the copper-containing reaction liquid for reaction for 20 minutes, immersing and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the functionalized nylon fiber 1. The functionalized nylon fiber 1 has excellent electromagnetic shielding properties after long-term use.
Example 2
1.5 g of NaOH and 5g of emulsifier are dissolved in 1L of water to prepare a washing liquid, and nylon fibers are soaked for 30 minutes at 40 ℃ and then washed by water.
2. Immersing the fibers in the step (1) into silver salt solution at the immersion temperature of 30 ℃ for 30 minutes, wherein the weight ratio of the fibers to the silver salt solution is 1:5, and then drying the fibers at 45 ℃; then immersing in alkali liquor at 55 ℃ for 30 minutes, wherein the weight ratio of the fiber to the alkali liquor is 1:4, and then drying at 50 ℃. Wherein the silver salt solution comprises 5% of silver fulvate, 6% of cetyltrimethylammonium bromide, 7% of sodium dodecyl benzene sulfonate and 5% of epichlorohydrin.
3. And (3) soaking the nylon fiber in the step (2) into 0.2M/L cysteamine hydrochloride solution at a temperature of 55 ℃ for 30 minutes.
4. Immersing the fiber of the step (3) into sodium citrate and H 2 PdCl 4 Activated nylon fiber with Pd particles loaded on the surface is obtained, wherein the concentration of sodium citrate is 0.3M/L, H 2 PdCl 4 The concentration of (C) is 0.05M/L, the soaking temperature is 50 ℃, and the soaking time is 80 minutes.
5. And (3) regulating the temperature of the copper-containing reaction liquid to 30 ℃, immersing the fiber obtained in the step (4) into the copper-containing reaction liquid for reaction for 20 minutes, immersing and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the functionalized nylon fiber 2. The functionalized nylon fiber 2 has excellent electromagnetic shielding properties after long-term use.
Example 3
1.5 g of NaOH and 5g of emulsifier are dissolved in 1L of water to prepare a washing liquid, and nylon fibers are soaked for 30 minutes at 40 ℃ and then washed by water.
2. Immersing the fibers in the step (1) into silver salt solution at the immersion temperature of 30 ℃ for 30 minutes, wherein the weight ratio of the fibers to the silver salt solution is 1:5, and then drying the fibers at 45 ℃; then immersing in alkali liquor at 55 ℃ for 30 minutes, wherein the weight ratio of the fiber to the alkali liquor is 1:4, and then drying at 50 ℃. Wherein the silver salt solution comprises 5% of silver fulvate, 6% of cetyltrimethylammonium bromide, 7% of sodium dodecyl benzene sulfonate, 5% of epichlorohydrin and 2% of gel.
3. And (3) soaking the nylon fiber obtained in the step (2) into 0.1M/L cysteamine solution at a soaking temperature of 50 ℃ for 40 minutes.
4. Immersing the fiber of the step (3) into sodium citrate and H 2 PdCl 4 Activated nylon fiber with Pd particles supported on the surface is obtained, wherein the concentration of sodium citrate is 0.25M/L, H 2 PdCl 4 The concentration of (2) was 0.04M/L, the soaking temperature was 50℃and the soaking time was 80 minutes.
5. And (3) regulating the temperature of the copper-containing reaction liquid to 30 ℃, immersing the fiber obtained in the step (4) into the copper-containing reaction liquid for reaction for 20 minutes, immersing and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the functionalized nylon fiber 3. The functionalized nylon fiber 3 has excellent electromagnetic shielding properties after long-term use.
Comparative example 1
1.5 g of NaOH and 5g of emulsifier are dissolved in 1L of water to prepare a washing liquid, and nylon fibers are soaked for 30 minutes at 40 ℃ and then washed by water.
2. Immersing the fibers in the step (1) into silver salt solution at the immersion temperature of 30 ℃ for 30 minutes, wherein the weight ratio of the fibers to the silver salt solution is 1:5, and then drying the fibers at 45 ℃; then immersing in alkali liquor at 55 ℃ for 30 minutes, wherein the weight ratio of the fiber to the alkali liquor is 1:4, and then drying at 50 ℃. Wherein the silver salt solution comprises 5% of silver fulvate, 6% of cetyltrimethylammonium bromide, 7% of sodium dodecyl benzene sulfonate and 5% of epichlorohydrin.
3. And (3) soaking the nylon fiber obtained in the step (2) into a roughening solution at a 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. Immersing the fiber of the step (3) into sodium citrate and H 2 PdCl 4 Activated nylon fiber with Pd particles loaded on the surface is obtained, wherein the concentration of sodium citrate is 0.3M/L, H 2 PdCl 4 The concentration of (C) is 0.05M/L, the soaking temperature is 50 ℃, and the soaking time is 80 minutes.
5. And (3) regulating the temperature of the copper-containing reaction liquid to 30 ℃, immersing the fiber obtained in the step (4) into the copper-containing reaction liquid for reaction for 20 minutes, immersing and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the nylon fiber 1 for comparison. The comparative nylon fiber 1 has a good electromagnetic shielding effect after long-term use.
Comparative example 2
1.5 g of NaOH and 5g of emulsifier are dissolved in 1L of water to prepare a washing liquid, and nylon fibers are soaked for 30 minutes at 40 ℃ and then washed by water.
2. Immersing the fibers in the step (1) into silver salt solution at the immersion temperature of 30 ℃ for 30 minutes, wherein the weight ratio of the fibers to the silver salt solution is 1:5, and then drying the fibers at 45 ℃; then immersing in alkali liquor at 55 ℃ for 30 minutes, wherein the weight ratio of the fiber to the alkali liquor is 1:4, and then drying at 50 ℃. Wherein the silver salt solution comprises 5% of silver fulvate, 6% of cetyltrimethylammonium bromide, 7% of sodium dodecyl benzene sulfonate and 5% of epichlorohydrin.
3. And (3) soaking the nylon fiber in the step (2) into 0.2M/L cysteamine hydrochloride solution at a temperature of 55 ℃ for 30 minutes.
4. And (3) immersing the fiber obtained in the step (3) into a copper-containing reaction solution, adjusting the temperature to 30 ℃, reacting for 20 minutes, immersing and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the nylon fiber 2 for comparison. The comparative nylon fiber 2 had poor electromagnetic shielding properties after long-term use.
Comparative example 3
1.5 g of NaOH and 5g of emulsifier are dissolved in 1L of water to prepare a washing liquid, and nylon fibers are soaked for 30 minutes at 40 ℃ and then washed by water.
2. And (3) soaking the nylon fiber obtained in the step (1) into 0.1M/L cysteamine solution at a soaking temperature of 50 ℃ for 40 minutes.
3. Immersing the fiber in the step (2) into sodium citrate and H 2 PdCl 4 Activated nylon fiber with Pd particles supported on the surface is obtained, wherein the concentration of sodium citrate is 0.25M/L, H 2 PdCl 4 The concentration of (2) is 0.04M/L, the soaking temperature is 50 ℃, and the soaking time is 80 minutesAnd (3) a clock.
4. Immersing the fiber in the step (3) into silver salt solution, and reacting for 10 minutes at 90 ℃ under the condition of compressed air stirring to obtain 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 methanol and 15 malonic acid with 1L of deionized water, and then regulating the pH of the solution to be between 5.0 and 5.5 with sodium hydroxide.
5. And (3) adjusting the temperature of the copper-containing reaction liquid to 30 ℃, immersing the fiber obtained in the step (4) into the copper-containing reaction liquid for reaction for 20 minutes, immersing and washing the obtained fiber with deionized water for 25 minutes, and drying to obtain the nylon fiber 3 for comparison. The comparative nylon fiber 3 had poor electromagnetic shielding properties after long-term use.
The nylon fiber properties of examples and comparative examples were tested and the results are shown in table 1. It can be seen that the functionalized nylon fibers prepared by adopting the embodiments 1-3 of the invention are superior to the comparative examples 1-3 in strength, conductivity and strength, which indicates that the preparation method provided by the invention is simple and convenient to operate, and the prepared functionalized fibers have good conductivity, flexibility, strength and electromagnetic shielding effect.
TABLE 1
While the 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. Various modifications or changes may be made to the exemplary embodiments of the present disclosure without departing from the scope or spirit of the 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 (6)

1. The preparation method of the pilot sock with the electromagnetic shielding function is characterized by comprising the steps of preparing functionalized nylon fibers, and the preparation method comprises the following steps of:
(1) Immersing a nylon fiber raw material in a silver salt solution, immersing at 35-45 ℃ for 30-60 minutes, drying at 40-50 ℃, immersing in alkali liquor, treating at 50-65 ℃ for 30-50 minutes, and then drying, wherein the silver salt solution comprises at least one silver salt selected from the group consisting of silver fulvate and silver nitrate, cetyltrimethylammonium bromide, sodium dodecyl benzene sulfonate, epichlorohydrin and gel, the silver salt content is 5-7 parts by weight, the cetyltrimethylammonium bromide dosage is 4-9 parts by weight, the sodium dodecyl benzene sulfonate dosage is 4-10 parts by weight, and the gel dosage is 2-4 parts by weight based on 1000 parts by weight of water; the alkali liquor is an aqueous solution containing cyclodextrin and sodium hydroxide or potassium hydroxide, the dosage of the cyclodextrin in the alkali liquor is 100-150 parts by weight, and the dosage of the sodium hydroxide or the potassium hydroxide is 20-60 parts by weight based on 1000 parts by weight of water;
(2) Soaking the nylon fiber obtained in the step (1) into a cross-linking 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 tetrachloropalladiumacid (II); and
(4) Immersing the nylon fiber obtained in the step (3) into copper salt-containing reaction liquid for reaction for 10-30 minutes, immersing 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 ethylenediamine tetraacetate, sodium hydroxide, sodium carbonate, formaldehyde, ethanol, bipyridine, potassium ferrothiocyanide, and nickel chloride.
3. The method according to claim 1, wherein the temperature of the mixed aqueous solution is 45-60 ℃ for 50-100 minutes.
4. The method of claim 1, further comprising the step of washing the nylon fibers with an emulsifier-containing lye prior to step (1).
5. The preparation method of claim 1, wherein the nylon fiber has a surface resistance of less than 0.05 ohm per cm and a shielding effectiveness of 10mhz to 40 ghz.
6. A pilot sock with electromagnetic shielding function, characterized in that it is produced by the method according to any one of claims 1-5.
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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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