CN104452272A - Preparation method of silver-plated aromatic polysulphonamide fiber - Google Patents
Preparation method of silver-plated aromatic polysulphonamide fiber Download PDFInfo
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Abstract
The invention relates to a preparation method of a silver-plated aromatic polysulphonamide fiber. The preparation method of the silver-plated aromatic polysulphonamide fiber specifically comprises the following steps: (a) washing and deoiling; (b) carrying out pretreatment on the surface of the fiber by using a pretreatment reagent to improve roughness and wettability of the surface of the fiber; (c) activating; (d) reducing; (e) chemically plating silver; and (f) coating the surface of the fiber with a film and protecting the fiber. The silver-plated aromatic polysulphonamide fiber prepared by the method has the characteristics of excellent conductivity, heat resistance, flame retardance, light weight, high strength and the like; the anti-ageing performance of a silver-plating layer is good; the silver-plated fiber can be used for preparing antistatic and electromagnetic shielding fabrics, shielding layers of special cables and conductor materials. Therefore, the silver-plated fiber can be widely used in special departments such as aviation, spaceflight, war industry and communication; the individual protection requirements of workers occupied in radar, medical treatment and television transmit can be met.
Description
Technical field
The invention provides a kind of preparation method of silver-plated aromatic polysulfonamides fibre.
Background technology
Along with the develop rapidly of scientific and technological level, increasing electric/electronic device has spread to the every field of human lives, the electromagnetic interference simultaneously caused by electromagnetic wave and electromagnetic compatibility problem also day by day serious.These not only can cause interference to electronic instrument and damage, and pollute the environment, and harm humans is healthy; Electromagnetic-wave leakage also can cause the valuable informations such as politics, economy, national defence, science and technology to divulge a secret in addition, jeopardizes the safety of national information safety and military secrecy.The product corresponding birth of various electromagnetic shielding.Conductive fiber had both maintained lightweight, the pliability of general fibre because of it, had again certain conduction and capability of electromagnetic shielding, therefore had good application in many departments of national economy.
Patent CN 101215779 A teaches a kind of preparation method of high-performance conductive fiber, and it is chemical plating layer of metal silver on terylene, nylon and polypropylene fibre.Patent CN 1089309 A of E. I. Du Pont de Nemours and Co is one deck silver metal at aromatic polyamide fibre surface electroless.Patent CN101705614 B teaches a kind of method of chemical plating nickeline composite deposite on aromatic polyamide fibre.Patent CN 102421277 A of Shenzhen Longpont Co., Ltd. is a kind of shielding material that used the method for airless spraying metal to obtain on aromatic polyamide fibre paper.Patent CN 103221577 A of Xi Sikang Advanced Materials Corp. is coated with tin, nickel, copper, silver, gold and alloy thereof on full-aromatic polyester liquid crystal polymer fibre.
Organic high molecular polymer aromatic polysulfonamides applies engineering plastics more widely, has resistance to chemical attack, high temperature resistant, the premium properties such as noninflammability and electric insulation.Especially be made into textile fabric, due to its lightweight, the distinguishing feature such as high temperature resistant and fire-retardant, can be used to make some special spe-cial-purpose uniforms; Also excellent high-temperature-resistant filtering material can be made, or the insulating paper of motor.
Report the earliest about aromatic polysulfonamides fibre manufacture method comes from the former Soviet Union's " chemical fibre " magazine, patent CN 1176256 C " manufacture method of aromatic polysulfonamides fibre " then sees about the report of aromatic polysulfonamides fibre manufacture in China, and industrialization is produced.The chemical structural formula of aromatic polysulfonamides fibre is as follows:
；
Wherein m=0 ~ 1, n=1 ~ 0, m+n=1.
At aromatic polysulfonamides fibre coating surface conducting metal, fiber surface is metallized, the function eliminating electrostatic, conduction, transmission of electric signals can be made it have, and have than metal wire light weight, pliable and tough feature.But aromatic polysulfonamides fibre smooth surface, lacks active group, and surface energy is low, reactivity is low, causes chemical plating metal to be difficult to directly in fiber surface deposition, and fiber and coat of metal adhesion poor, the coat of metal easily comes off, thus affects electric conductivity and the durability of fiber.
Summary of the invention
The object of the invention is the preparation method providing a kind of silver-plated aromatic polysulfonamides fibre.The method by first carrying out cleaning oil removal treatment to matrix fiber (polysulfonamides fibre), removes the finish of fiber in process and surface smut; After oil removing, preliminary treatment is carried out to fiber surface, increase roughness and the wettability of fiber surface, to improve the binding strength between subsequent plating layer and base material; Activation is the material that fiber surface after the pre-treatment adsorbs one deck and is easily reduced, can carry out reduction treatment when reduction step; Fiber is formed on surface and the anchor node of substrate strong bonded and catalytic site after reduction; And then in fiber surface chemical plating silver, finally apply organic protection layer, prevent the coat of metal to be oxidized, finally obtain a kind of silver-plated aromatic polysulfonamides conductive fiber.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for silver-plated aromatic polysulfonamides fibre, is characterized in that the concrete steps of the method are:
A. washing and oil removing, removes fiber surface dirt, finish and impurity;
B. preliminary treatment, the roughness on increased fiber surface and wettability, improve the binding strength of fibrous matrix and subsequent plating layer;
C. activate, use precious metal salt solution to soak fiber, form the thin catalytic active layer of one deck at fiber surface;
D. reduce, use reducing solution to soak fiber, form noble metal granule layer at fiber surface, as the anchor point between fiber and subsequent plating layer, can also have the function of catalysis simultaneously;
E. chemical silvering, concrete steps are:
E-1 silver plating solution is made up of silver salt solution and reductant solution, and the composition of wherein said silver salt solution and the concentration of each composition are:
AgNO
38～16 g/L
Ammoniacal liquor 50 ~ 80 ml/L
Ethylenediamine 15 ~ 40 ml/L
KOH 3～8 g/L；
The composition of described reductant solution and the concentration of each composition are:
Glucose 4 ~ 12 g/L
Potassium sodium tartrate 2 ~ 5 g/L
Ethanol 30 ~ 70 ml/L
Stabilizing agent (sodium thiosulfate) 70 ~ 280 μ g/L.
Silver salt solution and reductant solution are pressed the volume ratio mixing of 1:1 by e-2, are immersed in reactant liquor by steps d gained fiber, at 25 ~ 35 DEG C, take out, use deionized water rinsed clean after stirring reaction 45 ~ 75 min, obtain the conductive fiber that surface uniform plating has silver;
F. coating protective, prevents the oxidation of the coat of metal.
Above-mentioned aromatic polysulfonamides fibre chemical structural formula is:
；
Wherein m=0 ~ 1, n=1 ~ 0, m+n=1.
The washing of above-mentioned step a and oil removal process are: aromatic polysulfonamides fibre is put into acetone, take out, use deionized water rinsed clean after Ultrasonic Cleaning 45 ~ 75 min.
The preprocessing process of above-mentioned step b is: the fiber after oil removing is put into pretreatment fluid, at 25 ~ 30 DEG C, takes out, use deionized water rinsed clean after dipping 15 ~ 45 min; Described pretreatment fluid is the acetone soln of liquor natrii hypochloritis, sodium dichloro cyanurate solution or sym-closene, and concentration is 2.5 ~ 20 g/L.
The activation process of above-mentioned step c is: pretreated fiber is put into the precious metal salt solution that concentration is 0.2 ~ 9 g/L, at 50 ~ 90 DEG C, takes out, with the slow rinsing of deionized water after dipping 45 ~ 60 min.
Above-mentioned precious metal salt solution is silver nitrate, palladium bichloride, chlorauride, osmium chloride or rhodium chloride solution.
The reduction process of above-mentioned steps d is: the fiber after activation is put into reducing solution, and at 25 ~ 35 DEG C, dipping 20 ~ 40 min carry out reduction treatment, rear taking-up, use deionized water rinsed clean; The sodium borohydride of described reducing solution to be concentration be 1 ~ 10 g/L, dimethylamine borane or hydrazine hydrate solution.
The painting membrane process of above-mentioned step f is: fiber plated surface being covered with silver immerses in the stearyl mercaptan solutions of 0.25 ~ 0.5 g/L, takes out after dipping 20 ~ 24 h, and in 60 ~ 80 DEG C of oven dry.
This patent, by carrying out surface preparation to aromatic polysulfonamides fibre, increases roughness and the wettability of fiber surface, to improve the adhesion of fiber and subsequent metal coating; Adopt the method for activation and reduction to combine in fiber surface formation and fiber afterwards and be firmly anchored point and catalytic site; And introduce ammoniacal liquor and ethylenediamine as complexing agent, potassium sodium tartrate and glucose as dual reducting agents in chemical silvering process subsequently, thus the silver-plated aromatic polysulfonamides fibre that obtained electric conductivity is good.
The silver-plated aromatic polysulfonamides conductive fiber obtained by the present invention has excellent electric conductivity, and show after tested, the resistance value of filament tow is 0.1 ~ 0.5 Ω/cm, and remains the characteristic of original fiber, soft, has fire-retardant self-extinguishment.And the conductive fiber to be obtained by the present invention has good ageing resistace, is contrasted by hydrogen sulfide accelerate corrosion test, after conservation treatment, the ageing resistace of silver plated fiber is far superior to without conservation treatment.
The inherent characteristics such as this technique is passed through at aromatic polysulfonamides fibre surface metallization electrically conductive layer, thus makes it have antistatic and conducting function, remains the high-strength light of fiber, heat-proof combustion-resistant simultaneously, soft.Therefore the specials such as Aeronautics and Astronautics, navigation, military project, medical treatment can be widely used in, as antistatic and the Electromagnetically shielding fabrics of individual protection, and the screen layer of microwave coaxial cable and conductor etc.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram sheet of aromatic polysulfonamides fibre.
Fig. 2 is the scanning electron microscope diagram sheet of aromatic polysulfonamides fibre after preliminary treatment.
Fig. 3 is the scanning electron microscope diagram sheet by the silver-plated rear aromatic polysulfonamides fibre of method described in embodiment 1.
Detailed description of the invention
embodiment 1:
The first step: oil removing, puts into acetone soln by aromatic polyamide fibre, takes out, use deionized water rinsed clean after Ultrasonic Cleaning 60 min.
Second step: preliminary treatment, immerses fiber in the acetone soln of 2.5 g/L sym-closenes, takes out after soaking 45 min at 25 DEG C, use deionized water rinsed clean.
3rd step: activation, the liquor argenti nitratis ophthalmicus pretreated fiber being put into 9 g/L carries out activation processing, and temperature is 90 DEG C, takes out slow rinsing after 60 min.
4th step: reduction, the sodium borohydride solution that 1 g/L put into by the fiber after activation is carried out reduction treatment, and temperature is 25 DEG C, takes out after 30 min, uses deionized water rinsed clean.
5th step: chemical silvering, the fiber after reduction is put into silver salt solution, and in chemical plating liquid, silver salt solution consists of: AgNO
310 g/L, ammoniacal liquor 50ml/L, KOH 6 g/L, ethylenediamine 30ml/L; Pour reductant solution into afterwards and stir, reductant solution consists of: glucose 8 g/L, sodium potassium tartrate tetrahydrate 2.5 g/L, ethanol 40 ml/L, sodium thiosulfate 70 μ g/L.Silver salt solution and reductant solution volume ratio are 1:1, and the temperature of chemical plating fluid is 30 DEG C, plating time 60 min.
6th step: be coated with diaphragm, the fiber after chemical silvering immersed in the stearyl mercaptan solutions of 0.3 g/L, take out after flooding 20 h, in 80 DEG C of oven dry.
The scanning electron microscope diagram sheet of aromatic polysulfonamides fibre is shown in accompanying drawing 1.2, accompanying drawing is the scanning electron microscope diagram sheet of aromatic polysulfonamides fibre after preliminary treatment, as can be seen from the figure, after pretreatment, there is many grooves in fiber surface, surface area, the roughness of fiber are improved, and contribute to the binding strength of increased fiber matrix and subsequent plating layer.
Accompanying drawing 3 is seen by the silver-plated rear aromatic polysulfonamides scanning electron microscope diagram sheet of method described in embodiment 1.Can find out, the coating surface of the aromatic polysulfonamides fibre silver layer of the smooth densification of one deck.
embodiment 2:
The first step: oil removing, puts into acetone soln by aromatic polysulfonamides fibre, takes out, use deionized water rinsed clean after Ultrasonic Cleaning 60 min.
Second step: preliminary treatment, immerses fiber in the sodium dichloro cyanurate solution of 5 g/L, takes out after soaking 30 min at 25 DEG C, use deionized water rinsed clean.
3rd step: activation, the liquor argenti nitratis ophthalmicus pretreated fiber being put into 10 g/L carries out activation processing, and temperature is take out slow rinsing after 90 DEG C of 60 min.
4th step: reduction, the dimethylamine borane solution that 3 g/L put into by the fiber after activation is carried out reduction treatment, and temperature is 25 DEG C, takes out after 30 min, uses deionized water rinsed clean.
5th step: chemical silvering, the fiber after reduction is put into silver salt solution, and in chemical plating liquid, silver salt solution consists of: AgNO
310 g/L, ammoniacal liquor 50ml/L, KOH 6 g/L, ethylenediamine 30ml/L; Pour reductant solution into afterwards and stir, reductant solution consists of: glucose 8 g/L, sodium potassium tartrate tetrahydrate 2.5 g/L, ethanol 40 ml/L, sodium thiosulfate 140 μ g/L.Silver salt solution and reductant solution volume ratio are 1:1, and the temperature of chemical plating fluid is 30 DEG C, plating time 60 min.
embodiment 3:
The first step: oil removing, puts into acetone soln by aromatic polysulfonamides fibre, takes out, use deionized water rinsed clean after Ultrasonic Cleaning 60 min.
Second step: preliminary treatment, immerses fiber in the sodium hypochlorite solution of 20 g/L, takes out after soaking 60 min at 25 DEG C, use deionized water rinsed clean.
3rd step: the acidic aqueous solution (palladium bichloride of 0.33 g/L and the concentrated hydrochloric acid of 4mL/L, the latter promotes the former dissolving) pretreated fiber being put into palladium bichloride carries out activation processing, and temperature is 50 DEG C, takes out slow rinsing after 45 min.
4th step: reduction, the hydrazine hydrate solution that 8 g/L put into by the fiber after activation is carried out reduction treatment, and temperature is 25 DEG C, takes out after 20 min, uses deionized water rinsed clean.
5th step: chemical silvering, the fiber after reduction is put into silver salt solution, and in chemical plating liquid, silver salt solution consists of: AgNO
310 g/L, ammoniacal liquor 50ml/L, KOH 6 g/L, ethylenediamine 30ml/L; Pour reductant solution into afterwards and stir, reductant solution consists of: glucose 8 g/L, sodium potassium tartrate tetrahydrate 2.5 g/L, ethanol 40 ml/L, sodium thiosulfate 280 μ g/L.Silver salt solution and reductant solution volume ratio are 1:1, and the temperature of chemical plating fluid is 30 DEG C, plating time 60 min.
Claims (8)
1. a preparation method for silver-plated aromatic polysulfonamides fibre, is characterized in that the concrete steps of the method are:
A. washing and oil removing, removes fiber surface dirt, finish and impurity;
B. preliminary treatment, the roughness on increased fiber surface and wettability, improve the binding strength of fibrous matrix and subsequent plating layer;
C. activate, use precious metal salt solution to soak fiber, form the thin catalytic active layer of one deck at fiber surface;
D. reduce, use reducing solution to soak fiber, form noble metal granule layer at fiber surface, as the anchor point between fiber and subsequent plating layer, can also have the function of catalysis simultaneously;
E. chemical silvering, concrete steps are:
E-1 silver plating solution is made up of silver salt solution and reductant solution, and the composition of wherein said silver salt solution and the concentration of each composition are:
AgNO
38～16 g/L
Ammoniacal liquor 50 ~ 80 ml/L
Ethylenediamine 15 ~ 40 ml/L
KOH 3～8 g/L；
The composition of described reductant solution and the concentration of each composition are:
Glucose 4 ~ 12 g/L
Potassium sodium tartrate 2 ~ 5 g/L
Ethanol 30 ~ 70 ml/L
Stabilizing agent (sodium thiosulfate) 70 ~ 280 μ g/L;
Silver salt solution and reductant solution are pressed the volume ratio mixing of 1:1 by e-2, are immersed in reactant liquor by steps d gained fiber, at 25 ~ 35 DEG C, take out, use deionized water rinsed clean after stirring reaction 45 ~ 75 min, obtain the conductive fiber that surface uniform plating has silver;
F. coating protective, prevents the oxidation of the coat of metal.
2. the preparation method of silver-plated aromatic polysulfonamides fibre according to claim 1, is characterized in that described aromatic polysulfonamides fibre chemical structural formula is:
；
Wherein m=0 ~ 1, n=1 ~ 0, m+n=1.
3. the preparation method of silver-plated aromatic polysulfonamides fibre according to claim 1 and 2, it is characterized in that washing and the oil removal process of described step a are: aromatic polysulfonamides fibre is put into acetone, take out after Ultrasonic Cleaning 45 ~ 75 min, use deionized water rinsed clean.
4. the preparation method of silver-plated aromatic polysulfonamides fibre according to claim 1 and 2, it is characterized in that the preprocessing process of described step b is: the fiber after oil removing is put into pretreatment fluid, at 25 ~ 30 DEG C, take out after dipping 15 ~ 45 min, use deionized water rinsed clean; Described pretreatment fluid is the acetone soln of liquor natrii hypochloritis, sodium dichloro cyanurate solution or sym-closene, and concentration is 2.5 ~ 20 g/L.
5. the preparation method of silver-plated aromatic polysulfonamides fibre according to claim 1 and 2, it is characterized in that the activation process of described step c is: pretreated fiber is put into the precious metal salt solution that concentration is 0.2 ~ 9 g/L, at 50 ~ 90 DEG C, take out, with the slow rinsing of deionized water after dipping 45 ~ 60 min.
6. the preparation method of silver-plated aromatic polysulfonamides fibre according to claim 5, is characterized in that described precious metal salt solution is silver nitrate, palladium bichloride, chlorauride, osmium chloride or rhodium chloride solution.
7. the preparation method of silver-plated aromatic polysulfonamides fibre according to claim 1 and 2, it is characterized in that the reduction process of described steps d is: the fiber after activation is put into reducing solution, at 25 ~ 35 DEG C, dipping 20 ~ 40 min carry out reduction treatment, rear taking-up, uses deionized water rinsed clean; The sodium borohydride of described reducing solution to be concentration be 1 ~ 10 g/L, dimethylamine borane or hydrazine hydrate solution.
8. the preparation method of silver-plated aromatic polysulfonamides fibre according to claim 1 and 2, it is characterized in that the painting membrane process of step f is: fiber plated surface being covered with silver immerses in the stearyl mercaptan solutions of 0.25 ~ 0.5 g/L, take out after dipping 20 ~ 24 h, and in 60 ~ 80 DEG C of oven dry.
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| CN105239248A (en) * | 2015-09-06 | 2016-01-13 | 南昌市婧麒服饰有限公司 | Anti-bacterial radiation protection fabric and manufacturing method thereof |
| CN105256291A (en) * | 2015-06-10 | 2016-01-20 | 上海大学 | Method for preparing aramid fiber nickel/copper plating double-plating-layer composite conductive fibers |
| CN105625028A (en) * | 2016-04-01 | 2016-06-01 | 吴江市林旺纺织厂 | Radiation-proof textile fiber and preparation method thereof |
| CN107326657A (en) * | 2017-08-03 | 2017-11-07 | 陈志豪 | A kind of preparation method of silver-plated conductive aramid fiber |
| CN108085968A (en) * | 2017-12-05 | 2018-05-29 | 武汉纺织大学 | A kind of preparation method of metallic coated fabric |
| CN110184808A (en) * | 2019-06-12 | 2019-08-30 | 苏州福洹纺织科技有限公司 | A kind of fire-retardant, anti-oxidant, electromagnetic wave shielding PIPD fabric preparation method |
| CN110761082A (en) * | 2019-11-08 | 2020-02-07 | 上海工程技术大学 | Polysulfonamide composite fabric and preparation method and application thereof |
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| CN111691030A (en) * | 2019-03-12 | 2020-09-22 | 财团法人纺织产业综合研究所 | Method for manufacturing conductive yarn |
| CN112796102A (en) * | 2020-12-30 | 2021-05-14 | 山东汇高智慧纺织科技集团有限公司 | Vacuum sputtering fiber silver plating, product and application thereof |
| CN112853409A (en) * | 2020-12-29 | 2021-05-28 | 哈尔滨工业大学（深圳） | Silver-containing plating solution and preparation method of foam metal material |
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| CN113737520A (en) * | 2021-09-07 | 2021-12-03 | 青岛天银纺织科技有限公司 | Electromagnetic radiation prevention underwear for air force pilots and preparation method thereof |
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| CN105133301A (en) * | 2015-06-10 | 2015-12-09 | 上海大学 | Preparation method of nickel plated aromatic polyarmide fiber |
| CN105256291A (en) * | 2015-06-10 | 2016-01-20 | 上海大学 | Method for preparing aramid fiber nickel/copper plating double-plating-layer composite conductive fibers |
| CN105239248A (en) * | 2015-09-06 | 2016-01-13 | 南昌市婧麒服饰有限公司 | Anti-bacterial radiation protection fabric and manufacturing method thereof |
| CN105625028A (en) * | 2016-04-01 | 2016-06-01 | 吴江市林旺纺织厂 | Radiation-proof textile fiber and preparation method thereof |
| CN107326657A (en) * | 2017-08-03 | 2017-11-07 | 陈志豪 | A kind of preparation method of silver-plated conductive aramid fiber |
| CN108085968B (en) * | 2017-12-05 | 2020-10-16 | 武汉纺织大学 | Preparation method of metal coated fabric |
| CN108085968A (en) * | 2017-12-05 | 2018-05-29 | 武汉纺织大学 | A kind of preparation method of metallic coated fabric |
| CN111691030B (en) * | 2019-03-12 | 2022-03-08 | 财团法人纺织产业综合研究所 | Method for manufacturing conductive yarn |
| CN111691030A (en) * | 2019-03-12 | 2020-09-22 | 财团法人纺织产业综合研究所 | Method for manufacturing conductive yarn |
| CN110184808A (en) * | 2019-06-12 | 2019-08-30 | 苏州福洹纺织科技有限公司 | A kind of fire-retardant, anti-oxidant, electromagnetic wave shielding PIPD fabric preparation method |
| CN110761082A (en) * | 2019-11-08 | 2020-02-07 | 上海工程技术大学 | Polysulfonamide composite fabric and preparation method and application thereof |
| CN110983764A (en) * | 2019-12-20 | 2020-04-10 | 上海大学 | Conductive aromatic polyamide fiber with composite metal coating structure |
| CN110983764B (en) * | 2019-12-20 | 2022-04-05 | 上海大学 | Conductive aromatic polyamide fiber with composite metal coating structure |
| CN112853409A (en) * | 2020-12-29 | 2021-05-28 | 哈尔滨工业大学（深圳） | Silver-containing plating solution and preparation method of foam metal material |
| CN112853409B (en) * | 2020-12-29 | 2022-07-22 | 哈尔滨工业大学（深圳） | Silver-containing plating solution and preparation method of foam metal material |
| CN112796102A (en) * | 2020-12-30 | 2021-05-14 | 山东汇高智慧纺织科技集团有限公司 | Vacuum sputtering fiber silver plating, product and application thereof |
| CN113512877A (en) * | 2021-07-30 | 2021-10-19 | 铜陵蔚屹新材料有限公司 | Continuous production process for silver metal firmly attached aromatic special fiber filament |
| CN113512877B (en) * | 2021-07-30 | 2022-05-03 | 铜陵蔚屹新材料有限公司 | Continuous production process for silver metal firmly attached aromatic special fiber filament |
| CN113737520A (en) * | 2021-09-07 | 2021-12-03 | 青岛天银纺织科技有限公司 | Electromagnetic radiation prevention underwear for air force pilots and preparation method thereof |
| CN113737520B (en) * | 2021-09-07 | 2023-10-31 | 青岛天银纺织科技有限公司 | Electromagnetic radiation preventing underwear for air force pilot and preparation method thereof |
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Application publication date: 20150325 |