CN1357664A - Fiber with electromagnetic shielding function and its prepn - Google Patents
Fiber with electromagnetic shielding function and its prepn Download PDFInfo
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- CN1357664A CN1357664A CN 00127706 CN00127706A CN1357664A CN 1357664 A CN1357664 A CN 1357664A CN 00127706 CN00127706 CN 00127706 CN 00127706 A CN00127706 A CN 00127706A CN 1357664 A CN1357664 A CN 1357664A
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- fiber
- acid
- electromagnetic shielding
- sulfur
- shielding function
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- 239000000835 fiber Substances 0.000 title claims abstract description 102
- 125000004093 cyano group Chemical group *C#N 0.000 claims abstract description 12
- 239000010949 copper Substances 0.000 claims description 28
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 24
- 229910052717 sulfur Inorganic materials 0.000 claims description 23
- 239000011593 sulfur Substances 0.000 claims description 23
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 22
- 239000003638 chemical reducing agent Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 18
- 150000003839 salts Chemical class 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000002253 acid Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 11
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 10
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 235000011054 acetic acid Nutrition 0.000 claims description 8
- 229910052802 copper Inorganic materials 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical group [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 5
- 229920001021 polysulfide Polymers 0.000 claims description 5
- 239000005077 polysulfide Substances 0.000 claims description 5
- 150000008117 polysulfides Polymers 0.000 claims description 5
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 5
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 3
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- GRWZHXKQBITJKP-UHFFFAOYSA-N dithionous acid Chemical compound OS(=O)S(O)=O GRWZHXKQBITJKP-UHFFFAOYSA-N 0.000 claims description 3
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 3
- 229910000403 monosodium phosphate Inorganic materials 0.000 claims description 3
- 235000019799 monosodium phosphate Nutrition 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 claims description 3
- HYHCSLBZRBJJCH-UHFFFAOYSA-N sodium polysulfide Chemical compound [Na+].S HYHCSLBZRBJJCH-UHFFFAOYSA-N 0.000 claims description 3
- 159000000000 sodium salts Chemical class 0.000 claims description 3
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 3
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 239000005639 Lauric acid Substances 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000004327 boric acid Substances 0.000 claims description 2
- 235000010338 boric acid Nutrition 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 235000011007 phosphoric acid Nutrition 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 229920000098 polyolefin Polymers 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 150000008043 acidic salts Chemical class 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 16
- 239000000463 material Substances 0.000 description 9
- 239000002585 base Substances 0.000 description 8
- 239000004744 fabric Substances 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 229910000365 copper sulfate Inorganic materials 0.000 description 5
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 238000004043 dyeing Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000004061 bleaching Methods 0.000 description 2
- 229910052947 chalcocite Inorganic materials 0.000 description 2
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 239000005749 Copper compound Substances 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 235000011229 Prunus domestica subsp. syriaca Nutrition 0.000 description 1
- 240000005462 Prunus umbellata var. umbellata Species 0.000 description 1
- 235000005138 Spondias dulcis Nutrition 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000013043 chemical agent Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 150000001880 copper compounds Chemical class 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- 238000009990 desizing Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000010409 ironing Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- -1 sulfur ion Chemical class 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229920006027 ternary co-polymer Polymers 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Landscapes
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The present invention discloses fiber with electromagnetic shielding function and its preparation. The fiber features that it contains filming Cu9S5 crystal layer in 10-17 wt% and cyano group containing fiber in 83-90 wt%. The fiber has conducting layer of stable Cu9S5 crystal with the features of being dense, homogeneous in thickness, durable and chemical corrosion resistant. The fiber can be widely used in aeronautic equipment, astronautic equipment, radar station, satellite, TV station, power plant, etc. and in various fields needing electromagnetic shielding.
Description
The invention relates to the technical field of fiber fabrics, in particular to a fiber fabric with an electromagnetic shielding function and a preparation method thereof.
The existing method for preparing conductive fibre or antistatic fabric or electromagnetic shielding fabric and film by using cyano-containing fibre as base material and using copper sulfide to chelate is not limited, no matter the finished fibre adopts intermittent immersion treatment method, adopts boiling-dyeing method to make fibre undergo the process of two-bath treatment of copper compound and sulfur-containing compound or adopts polyacrylonitrile wet tow fibre and makes it pass through a conductive reaction bath containing copper ion and sulfur ion to make the interior of fibre embed copper sulfide, then makes densification so as to obtain the invented conductive component with sulfurA copper CuS or Cu2S or self-name Cu9S5The conductivity of copper blue (CuS) is higher than that of copper chalcocite (Cu)2S) is higher than 1 magnitude, but CuS is unstable in crystallization and can easily react with oxygen in air in humid air to generate copper sulfate which is easily dissolved in water, namely ；Cu2S is more stable than CuS, but Cu2When S is heated in air, or encounters a strong oxidant, the following reactions occur:
thus chalcocite (Cu)2S) is not resistant to high temperature (steaming, ironing), is not resistant to chemical agents (such as bleaching treatment before printing and dyeing), is made from durable conductive fibers using homopolyacrylonitrile fibers as a base material according to the Kansu Kaisha, and is made from Nihon Sanno Dyling CO. LTD; the defects of the conductive fibers are poor in durability and weather resistance, specific resistance of the conductive fibers is increased by 4-5 orders of magnitude after the conductive fibers are stored or used for half a year to one year under high-temperature humid weather (such as the yellow plum season), and in order to solve the problems of poor durability, weather resistance and chemical reagent resistance of the conductive fibers, the conductive fibers collected at home and abroad are analyzed by an electronic energy spectrum analysis (ESCA) method, an X-ray diffraction method and a precise element analysis method in sequence, the species of fragments falling off after losing conductivity are collected and analyzed, and all the fragments falling off after the conductivity of all the conductive fibers is lost are all Cu9S5Although dissociated in Cu9S5The conductivity of 6-10% of CuS between crystals is higher than that of Cu9S5However, under humid and higher air temperature conditions, it is easily oxidized by oxygen in the air to form CuSO which is easily soluble in water4Making Cu9S5The conductive layer has many holes or has a crystallized layer and fibersThe gaps create favorable conditions for the peeling of the conductive crystalline layer, and in order to solve the problems of the non-durability and the non-chemical resistance of the conductive fibers, the conductive crystalline layer is required to be combined with the fibers by a firm valence-matching bond through the orchite crystalline layer which is not oxidized, insoluble in water, acid and alkali and high in chemical stability, and the crystalline layer needs to be as thick and thin as possible, uniform and smooth in surface.
The invention aims to provide a fiber with electromagnetic shielding function and a preparation method thereof, the fiber has the electromagnetic wave shielding function, and the conductive fibers have durability and chemical resistance.
The technical scheme of the invention is realized as follows: a fiber having an electromagnetic shielding function, characterized in that: the fiber neutralization surface contains 10-17 wt% of film-forming pentasulfide nonacopper (molecular formula is Cu)9S5) Crystalline layers and 83-90% cyano-containing fibers.
A preparation method of fiber with electromagnetic shielding function is characterized in that: firstly, treating the fiber by adopting 10-60 wt% of acid or acid salt, wherein the bath ratio is 1: 5-1: 25, the temperature is 50-80 ℃, the soaking time is 20-60 minutes, and then taking out and drying the fiber; then, processing by adopting 10-50% of metal salt and 15-55% of sulfur-containing reducing agent in percentage by weight, adding the sulfur-containing reducing agent for 2-5 times at 45-75 ℃, adjusting the bath ratio of the sulfur-containing reducing agent to be 1: 10-1: 40, adjusting the pH value to be 1.5-4.5 by using sulfuric acid or acetic acid, heating to 85-100 ℃ after the aqueous solution containing the metal salt and the sulfur-containing reducing agent is clear, preserving heat for 20-60 minutes, and cooling, cleaning and drying; then the fiber is put into 10 percent ammonium polysulfide solution with the bath ratio of 1: 10-1: 25, heated to 65-80 ℃, sealed and insulated for 30-60 minutes, and then cooled, cleaned and dried.
Compared with the prior art, the invention has the following advantages:
1. the copper-containing salt content of the pretreated conductive fiber can be increased by adopting acid or acid salt for pretreatment;
2. the main treatment is carried out by adopting metal salt and reducing agent containing sulfur, and stable Cu can be generated9S5A conductive crystalline layer;
3. the conductive crystallization layer can become 100 percent of Cu by adopting the post-treatment of the sulfur-containing compound9S5Stabilize the crystal, and make the crystal layer more compact, the thickness more uniform, have durability and chemical resistance more.
A comparison of the relevant data is shown in tables 1 and 2.
Table 1 shows several conductive fibers used in a standing, washing 100 times and printing and dyeing process according to T/C*The specific resistance after the treatment changed.
The treatment conditions of the T/C fabric printing and dyeing process are as follows: desizing (8% NaOH in water solution impregnated and then steaming at 100 ℃ for 60 minutes); scouring bleaching (5g/L H)2O2And 3g/lnaoh.100 ℃ for 60 minutes); mercerizing (280g/L NaOH, 60 seconds, hot water washing and cold water washing).
TABLE 2 comparison of the performance of woven dust-removing filter bags made of polyester fabrics with 5% of the yarns and threads of the present invention embedded therein with those imported from Japan
The invention can be widely used for products such as electromagnetic wave shielding covers, shielding walls, protective clothing, protective vests, hats and the like in places such as aviation, aerospace, radar stations, satellites, radio stations, television stations, power plants, transformer substations, high-voltage wires, cables, computers, televisions, microwave ovens, mobile phones, BP machines and the like; it can also be used for coloring equipment of aluminum boxes, materials of robots, semiconductor materials for heating and high-efficiency antibacterial deodorant fabric products. 3-5% of the fiber or yarn of the invention is blended or interwoven with any other fiber yarn to prepare various antistatic, dedusting,The fog-eliminating product may be used widely in steel plant, power plant, cement product plant, pharmaceutical plant, grain processing plant and other fields to reduce dust content to below 50mg/M3And the packaging materials of safe antistatic working clothes and semiconductor devices in inflammable and explosive occasions such as oil fields, oil depots, oil tankers, petroleum processing plants, coal mines and the like; if the antistatic fabric product is made into gauze with pores of 0.5-0.8 mm, the fog on airports and expressways can be removed, and the fog can be prevented from entering the airports and expresswaysWithin the range.
The present invention will be further described with reference to the following examples.
The invention relates to a fiber with electromagnetic shielding function, which is characterized in that: the fiber neutralization surface contains 10-17 wt% of film-forming pentasulfide nonacopper (molecular formula is Cu)9S5) A crystalline layer and 83-90% cyano-containing fibers; in specific embodiments, the cyano-containing fiber includes homopolyacrylonitrile fiber, modified polyacrylonitrile fiber, polyester fiber, polyamide fiber, and polyolefin fiber, and these cyano-containing fibers are conventionally called base materials, which are basic fiber materials that have not been subjected to special treatment.
A preparation method of fiber with electromagnetic shielding function is characterized in that: firstly, treating the fiber by adopting 10-60 wt% of acid or acid salt, wherein the acid or acid salt comprises formic acid, acetic acid, propionic acid, butyric acid, lauric acid, oxalic acid, boric acid, phosphoric acid and sodium dihydrogen phosphate, the bath ratio of the acid or acid salt to water is 1: 5-1: 25, the temperatureis 50-80 ℃, the soaking time is 20-60 minutes, and then taking out and drying; then, metal salt with the weight percentage of 10-50% and reducing agent containing sulfur with the weight percentage of 15-55% are adopted for processing, the metal salt comprises metal ions of copper, silver and gold of 1B group elements, the reducing agent containing sulfur of iron, cobalt, nickel, palladium, iridium and platinum of 8B group elements is added for 2-5 times at the temperature of 45-75 ℃, the bath ratio of the reducing agent containing sulfur is 1: 10-1: 40, the PH value is adjusted to be 1.5-4.5 by sulfuric acid or acetic acid, after the aqueous solution containing the metal salt and the reducing agent containing sulfur is clear, the temperature is increased to 85-100 ℃, the temperature is kept for 20-60 minutes, and then cooling, cleaning and drying are carried out, and the reducing agent containing sulfur is sodium bisulfite, sulfurous acid, dithionous acid and sodium salt thereof, sodium thiosulfate, hydrogen sulfide, rongalite and compounds thereof; putting the fiber into a solution containing 2-35% of sulfur compounds with the bath ratio of 1: 10-1: 25, heating to 40-80 ℃, sealing, preserving the temperature for 20-90 minutes, cooling, cleaning and drying to obtain the fiber, wherein the sulfur-containing reducing agent is sodium bisulfite, sulfurous acid, dithionous acid and sodium salt thereof, sodium thiosulfate, hydrogen sulfide, rongalite and the compounds of the sulfur-containing reducing agent are sodium bisulfite, rongalite, sodium polysulfide, ammonium polysulfide and ammonium sulfide, and the weight percentages are based on the weight of the base fiber.
The pretreatment of the invention is to reduce certain crystallinity of polyacrylonitrile fiber or other modified fibers with cyano groups as a base material, increase the surface area to expose more cyano groups on the surface or in pores of the fiber, so that the fiber can adsorb more divalent Cu ions in a copper salt solution, even if the fiber achieves the purposes of swelling and etching to a certain degree and little strength reduction; the main treatment of the invention is to add a sulfur-containing reducing agent at 45-75 ℃ to ensure that Cu adsorbed on the surface and in pores of the fiber2+The ions are reduced to Cu+Ions and a large amount of S is generated in the reaction bath2-Ion, Cu+The ions can generate strong coordinate bonds with-CN groups in the fiber and on the surface layer and simultaneously react with S in the reaction bath2-Ion bonding to form Cu2S, when Cu2When the ratio of S to CuS reaches 4: 1, when Cu is added9S5Stable Cu is generated under the condition of crystallization kinetics requirement9S5A conductive crystalline layer; the conductive fiber crystallization layer treated by the method is subjected to precise element analysis, and about 1 percent of free CuS crystals still exist, so that the conductive fiber crystallization layer is necessarily subjected to sulfide-containing solutionTreatment, e.g. where the CuS crystals are either sparingly soluble in the ammonium polysulfide solution, or the solution is capable of taking place Reaction, which makes the cyano group on the fiber to bond with Cu with strong coordinate bond9S5Combined on the surface of the fiber withA layer of 100% Cu with uniform thickness, compact structure and high chemical stability is formed in a certain depth9S5The stable conductive crystalline layer of (1).
Examples are given below, the percentages in the examples being by weight, based on the weight of the fibers, unless otherwise indicated.
Example 1
Ternary copolymer acrylonitrile fiber is used as a base material, the fiber is soaked for one hour by adopting 80 percent sodium dihydrogen phosphate at the temperature of 30 ℃, and then the fiber is taken out and dried; putting the spin-dried fiber into CuSO with the bath ratio of 1: 254.H2Adding H into solution with O concentration of 0.03M/L2SO4Acidifying until the pH value of the solution is about 3, heating to 70 deg.C, maintaining the temperature for 30 min, stirring at constant temperature, and adding Na for 4 times2S2O3Solid, to make Na in solution2S2O3The concentration reaches 0.038M/L, then the temperature is raised to 95 ℃ at the temperature rise rate of 1-4 ℃ per minute, the temperature is kept for 1 hour, and the mixture is cooled, cleaned, decolored and dried; then the spun-dried fiber is put into 10 percent ammonium polysulfide solution with the bath ratio of 1: 20, heated to 75 ℃, sealed and kept for 45 minutes, cooled, cleaned and spun-dried to obtain the fiber with the specific resistance of 2.5 multiplied by 10-2Omega-cm electromagnetic wave shielding fiber.
Example 2
Taking polyacrylonitrile fiber as a base material, adopting 30% industrial acetic acid for pretreatment, carrying out bath ratio of 1: 10, the treatment temperature of 70-75 ℃, soaking for 30 minutes, then putting the polyacrylonitrile fiber into a cylinder at normal temperature, circulating for 5 minutes, heating to 75 ℃, keeping the temperature for 30 minutes, taking the polyacrylonitrile fiber out of the cylinder, entering main treatment, putting the pretreated polyacrylonitrile fiber into a solution containing 25% of copper sulfate and 28% of sodium hydrosulfite, carrying out bath ratio of 1: 12, adjusting the pH value to 3.5 by using acetic acid, carrying out the main treatment by the specific steps of putting the polyacrylonitrile fiber into the cylinder at normal temperature, gradually heating to 50 ℃, adding 1/3% of copper sulfate and sodium hydrosulfite, heating to 60 ℃, adding 1/3% of copper sulfate and sodium hydrosulfite, continuing to heat to 70 ℃, adding another 1/3 of copper sulfate and sodium hydrosulfite, heating at the rate of 1 ℃ per minute after keeping the temperature for 20 minutes, heating to 85 deg.CKeeping the temperature for 30 minutes and taking out the cylinder; adding 15% sodium polysulfide into the mixture after post-treatment, heating the mixture to 80 ℃ with a bath ratio of 1: 10, preserving the heat for 30 minutes, and cleaning and drying the mixture to obtain the product with a specific resistance of 2.3 multiplied by 10-2Omega-cm electromagnetic wave shielding fiber.
Example 3
Using wool acrylic fiber as a base material, adopting 10% oxalic acid for pretreatment, the treatment temperature is 50-55 ℃, the soaking time is 30 minutes, the bath ratio is 1: 25, then putting the fiber into a cylinder at normal temperature, circulating for 5 minutes, heating to 70 ℃, keeping the temperature for 40 minutes, taking the fiber out of the cylinder, putting the fiber into a main treatment, putting the pretreated fiber into 0.15M/L silver nitrate and 0.1 ml/L99% concentrated sulfuric acid, adjusting the pH value to 4, and putting the fiber into NaHSO2-CH2O-2H2O1.5g/L, bath ratio of 1: 40, the main treatment concrete steps are, the above ingredients room temperature into the cylinder, with every 2 minutes heating rate of 1 degree, heating to boiling point, heat preservation for 60 minutes, cooling, washing to the surface floating color to remove the whole post treatment, the post treatment and example 1 in the same post treatment.
Claims (7)
1. A fiber having an electromagnetic shielding function, characterized in that: the fiber neutralization surface contains 10-17 wt% of film-forming pentasulfide nonacopper (molecular formula is Cu)9S5) Crystalline layers and 83-90% cyano-containing fibers.
2. A fiber having an electromagnetic shielding function according to claim 1, wherein: the cyano-containing fiber comprises homopolymerized polyacrylonitrile fiber, modified polyacrylonitrile fiber, polyester fiber, polyamide fiber and polyolefin fiber.
3. A method for preparing a fiber having an electromagnetic shielding function according to claim 1, wherein: firstly, treating the fiber by adopting 10-60 wt% of acid or acid salt, wherein the bath ratio is 1: 5-1: 25, the temperature is 50-80 ℃, the soaking time is 20-60 minutes, and then taking out and drying the fiber; then, processing by adopting 10-50% of metal salt and 15-55% of sulfur-containing reducing agent in percentage by weight, adding the sulfur-containing reducing agent for 2-5 times at 45-75 ℃, adjusting the bath ratio of the sulfur-containing reducing agent to be 1: 10-1: 40, adjusting the pH value to be 1.5-4.5 by using sulfuric acid or acetic acid, heating to 85-100 ℃ after the aqueous solution containing the metal salt and the sulfur-containing reducing agent is clear, preserving heat for 20-60 minutes, and cooling, cleaning and drying; then putting the fiber into a solution of 2-35% sulfur-containing compound with a bath ratio of 1: 10-1: 25, heating to 40-80 ℃, preserving heat for 20-90 minutes under sealing, cooling, cleaning and drying.
4. The method for preparing fiber with electromagnetic shielding function according to claim 4, wherein the method comprises the following steps: the acid or acidic salt includes formic acid, acetic acid, propionic acid, butyric acid, lauric acid, oxalic acid, boric acid, phosphoric acid, acetic acid, sodium dihydrogen phosphate.
5. The method for preparing fiber with electromagnetic shielding function according to claim 4, wherein the method comprises the following steps: the metal salt comprises metal ions of copper, silver and gold of 1B group elements, and iron, cobalt, nickel, palladium, iridium and platinum of 8B group elements.
6. The method for preparing fiber with electromagnetic shielding function according to claim 4, wherein the method comprises the following steps: the sulfur-containing reducing agent is sodium bisulfite, sulfurous acid, dithionous acid and its sodium salt, sodium thiosulfate, hydrogen sulfide, rongalite and their compounds.
7. The method for preparing fiber with electromagnetic shielding function according to claim 4, wherein the method comprises the following steps: the sulfur-containing compound is sodium bisulfite, rongalite, sodium polysulfide, ammonium polysulfide, or ammonium sulfide.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103510379A (en) * | 2012-06-14 | 2014-01-15 | （株）宇宙染色 | Method for applying conductivity to nylon fiber |
| CN104141220A (en) * | 2014-08-05 | 2014-11-12 | 卜庆革 | Method for preparing metalized silver aramid fiber fabric, metalized silver aramid fiber fabric prepared through method and garment formed by metalized silver aramid fiber fabric |
| CN104404756A (en) * | 2014-11-13 | 2015-03-11 | 南通大学 | Iron nickel conductive sound-insulation electromagnetic shielding fabric preparation method |
| CN107956108A (en) * | 2017-11-09 | 2018-04-24 | 常熟市翔鹰特纤有限公司 | A kind of acrylic fibers electrically conductive filament and its preparation method for being complexed doping method |
| CN108625157A (en) * | 2018-05-29 | 2018-10-09 | 合肥爱家防辐射科技有限公司 | A kind of production method of water-fastness type Electromagnetically shielding fabrics |
| CN113699785A (en) * | 2021-08-31 | 2021-11-26 | 河南景源新材料有限公司 | Conductive material and preparation method and application method thereof |
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2000
- 2000-12-05 CN CN 00127706 patent/CN1357664A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103510379A (en) * | 2012-06-14 | 2014-01-15 | （株）宇宙染色 | Method for applying conductivity to nylon fiber |
| CN104141220A (en) * | 2014-08-05 | 2014-11-12 | 卜庆革 | Method for preparing metalized silver aramid fiber fabric, metalized silver aramid fiber fabric prepared through method and garment formed by metalized silver aramid fiber fabric |
| CN104404756A (en) * | 2014-11-13 | 2015-03-11 | 南通大学 | Iron nickel conductive sound-insulation electromagnetic shielding fabric preparation method |
| CN107956108A (en) * | 2017-11-09 | 2018-04-24 | 常熟市翔鹰特纤有限公司 | A kind of acrylic fibers electrically conductive filament and its preparation method for being complexed doping method |
| CN108625157A (en) * | 2018-05-29 | 2018-10-09 | 合肥爱家防辐射科技有限公司 | A kind of production method of water-fastness type Electromagnetically shielding fabrics |
| CN113699785A (en) * | 2021-08-31 | 2021-11-26 | 河南景源新材料有限公司 | Conductive material and preparation method and application method thereof |
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