CN104532553A - Method for chemical silver-plating of aramid conductive fibers - Google Patents
Method for chemical silver-plating of aramid conductive fibers Download PDFInfo
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- CN104532553A CN104532553A CN201410817976.8A CN201410817976A CN104532553A CN 104532553 A CN104532553 A CN 104532553A CN 201410817976 A CN201410817976 A CN 201410817976A CN 104532553 A CN104532553 A CN 104532553A
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Abstract
The invention relates to a method for chemical silver-plating of aramid conductive fibers. The method comprises the following steps: (1) preparing an acidic potassium permanganate solution, soaking aramid fibers, performing supersonic treatment at 20-50 DEG C for 20-40 minutes, then taking out the fibers, washing and drying; (2) dropwise adding a crosslinking agent into a chitosan solution under a low-temperature condition, stirring, soaking the aramid fibers, heating to room temperature, padding and baking; (3) preparing a palladium chloride solution, soaking the aramid fibers, and drying; and (4) preparing a silver-plating solution, soaking the aramid fibers, performing chemical silver-plating, and drying. The aramid conductive fibers prepared by the method provided by the invention are small in strength loss and high in conductivity (the fiber resistance is less than or equal to 0.4 ohm/cm), the reaction condition is mild, and the treatment method is simple, convenient and feasible.
Description
Technical field
The invention belongs to the silver-plated field of fiber, particularly a kind of method of aramid fiber conductive fiber chemical silvering.
Background technology
Aramid fiber is a kind of high performance high molecular synthetic material, has high-strength, Gao Mo, high temperature resistant, fire-retardant, the excellent properties such as chemical stability.Thus military project, protection field, industrial field etc. are widely used in.The macromolecular structure of Fanglun 1414's (abbreviation p-aramid fiber) is the high polymer that amido link is connected in a kind of approximate rigidity straight chain of the contraposition formation of phenyl ring, and chemical formula is as follows:
At aramid fiber surface plating conductive metal layer, fiber surface is metallized, the function eliminating electrostatic, conduction, electromagnetic shielding can be made it have, and have than metal wire light weight, soft feature, also may be used for the blending product of fiber.But because fiber surface is smooth, lack active group, the features such as reactivity is low, cause 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." preparation of silver-plated conduction aramid fiber and the performance study thereof " of the people such as beam Jingjing, in silver plating process, employ a kind of metalating reagent (NaH-DMSO), this reagent is inflammable and explosive, can not meet the needs of large-scale industrial production.The patent 201310685423.7 " a kind of aramid fiber Conductive Silver-Coated PET Fibers and preparation method thereof " of the people such as Zhu Yan flame invention uses traditional alligatoring, sensitization, activates the method for then chemical silvering, employ 10-30g stannous chloride and 0.1-1g palladium bichloride, stannous chloride has certain harm to environment, palladium belongs to noble metal, expensive.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of aramid fiber conductive fiber chemical silvering, the aramid fiber conductive fiber loss of strength that the method prepares is little, conductance high (fabric resistor≤0.4 Ω/cm), and reaction condition is gentle, and processing method is simple and easy to do.
The method of a kind of aramid fiber conductive fiber chemical silvering of the present invention, comprising:
(1) prepare acid permanganate soln, immerse aramid fiber, ultrasonic process 20-40 minute at 20-50 DEG C, then take out fiber and clean oven dry;
(2) under cryogenic conditions, instilled in chitosan solution by crosslinking agent and stir, then immerse aramid fiber, rise to room temperature, pad, bake, wherein, the mass ratio of crosslinking agent and shitosan is 1:4-1:5;
(3) prepare palladium chloride solution, immerse aramid fiber, dry;
(4) prepare silver plating liquid, immerse aramid fiber, carry out chemical silvering, dry.
In acid permanganate soln in described step (1), potassium permanganate consumption is 3-10g/L; Wherein, acid is one or more in sulfuric acid, nitric acid, phosphoric acid; The mass fraction of acid is 5%-20%.
Low temperature in described step (2) is 0-10 DEG C.
Crosslinking agent in described step (2) is formaldehyde, glutaraldehyde, hexandial or citric acid.
The concentration of the chitosan solution in described step (2) is 5-15g/L; The shitosan acetate dissolution of mass fraction 1%-4%.
The pick-up rate of padding in described step (2) is 60%-100%.
Baking temperature in described step (2) is 120-160 DEG C.
The concentration of the palladium chloride solution in described step (3) is 30-100mg/L.
Silver plating liquid in described step (4) consists of: silver ammino solution: 10-30g/L AgNO
3, drip ammoniacal liquor to clarification; Reducing solution: glucose 20-80g/L, tartaric acid 0.05-5g/L, ethanol 100-300mL/L, ethylenediamine 10-30mL/L, silver ammino solution and reducing solution are that 1:2 ~ 1:5 is mixed with chemical plating liquid with volume ratio.
Chemical silvering temperature in described step (4) is 40 ~ 60 DEG C, and the chemical silvering time is 30-60 minute.
The present invention first carries out roughening treatment to aramid fiber, increase contact surface area, then the Catalytic Layer formed by the functional group's chelating palladium bichloride on shitosan is applied at fiber surface, stannous chloride is replaced with biological material shitosan, decrease process and the pollution of sensitization activation, and greatly reduce the consumption of precious metal palladium, obtained conduction aramid fiber binding force of cladding material is strong, change the metal level fastness that is harsh, that cause by simple physical absorption of preparation condition in the past bad, the problems such as poor durability.By the aramid fiber conductive fiber that the method is obtained, surface deposition one deck even compact argent, and there is the functions such as antistatic, conduction, electromagnetic shielding.
beneficial effect
Because aramid fiber surface is smooth, lack active group, and excessive surface etch seriously can reduce fiber strength, therefore the present invention first carries out gentle roughening treatment to aramid fiber, then the Catalytic Layer formed by the functional group's chelating palladium bichloride on shitosan is applied at fiber surface, the adhesion between fiber and Catalytic Layer is increased by crosslinking agent, this palladium bichloride Catalytic Layer will cause chemical plating in chemical silvering process, obtained conduction aramid fiber binding force of cladding material is strong, change the metal level fastness in the past caused by simple physical absorption bad, the problems such as poor durability, the aramid fiber silver plated fiber electrical conductivity prepared by the present invention is high (fabric resistor≤0.4 Ω/cm), coating fastness excellent (supersound washing 30 minutes, conductivity variations≤5%).
Accompanying drawing explanation
Fig. 1 is (A) silver-plated front aramid fiber (sterogram) of embodiment 1; (B) silver-plated rear aramid fiber (sterogram);
Fig. 2 is (A) silver-plated front aramid fiber (SEM figure) of embodiment 1; (B) silver-plated rear aramid fiber (SEM figure);
Fig. 3 is process chart of the present invention.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) prepare acid permanganate soln, containing potassium permanganate 3g, sulfuric acid 100g in often liter of solution, immerse aramid fiber, under 20 DEG C of conditions, ultrasonic process 40 minutes, then takes out fiber, cleans, and dries.
(2) shitosan is dissolved with the acetum that mass fraction is 1%, chitosan solution concentration 5g/L, control temperature is at 0 DEG C, the speed of dripping with 10s/ drips 15ml formalin, and stir process 20 minutes, then immerses aramid fiber, rise to room temperature, pad, pick-up rate is 60%, and then 120 DEG C bake.
(3) prepare the palladium chloride solution of 50mg/L, immerse textile impregnation at 40 DEG C 60 minutes, 50 DEG C of oven dry.
(4) first silver ammino solution is prepared: 10g/L AgNO
3, drip ammoniacal liquor to clarification; Prepare reducing solution again: glucose 20g/L, tartaric acid 0.05g/L, ethanol 100mL/L, ethylenediamine 10mL/L.
Be that 1:2 mixes by silver ammino solution and reducing solution with volume ratio, be mixed with chemical plating liquid.Immerse fiber, carry out chemical silvering at 40 DEG C, plating 60 minutes.
(5) chemical silvering aramid fiber is dried under 100 DEG C of conditions.
The aramid fiber resistance prepared through this embodiment is 0.32 Ω/cm, supersound washing 30 minutes, resistance variations 4.2%.
Embodiment 2
(1) prepare acid permanganate soln, containing potassium permanganate 8g, nitric acid 100g in often liter of solution, immerse aramid fiber, under 30 DEG C of conditions, ultrasonic process 30 minutes, then takes out fiber, cleans, and dries.
(2) shitosan is dissolved with the acetum that mass fraction is 2%, chitosan solution concentration 10g/L, control temperature is at 5 DEG C, the speed of dripping with 10s/ drips 10ml glutaraldehyde solution, and stir process 20 minutes, then immerses aramid fiber, rise to room temperature, pad, pick-up rate is 80%, and then 140 DEG C bake.
(3) prepare the palladium chloride solution of 80mg/L, immerse textile impregnation at 40 DEG C 60 minutes, 50 DEG C of oven dry.
(4) first silver ammino solution is prepared: 20g/L AgNO
3, drip ammoniacal liquor to clarification; Prepare reducing solution again: glucose 60g/L, tartaric acid 3g/L, ethanol 150mL/L, ethylenediamine 20mL/L.
Be that 1:4 mixes by silver ammino solution and reducing solution with volume ratio, be mixed with chemical plating liquid.Immerse fiber, carry out chemical silvering at 50 DEG C, plating 50 minutes.
(5) chemical silvering aramid fiber is dried under 110 DEG C of conditions.
The aramid fiber resistance prepared through this embodiment is 0.28 Ω/cm, supersound washing 30 minutes, resistance variations 4.5%.
Embodiment 3
(1) prepare acid permanganate soln, containing potassium permanganate 10g, phosphatase 11 50g in often liter of solution, immerse aramid fiber, under 50 DEG C of conditions, ultrasonic process 20 minutes, then takes out fiber, cleans, and dries.
(2) shitosan is dissolved with the acetum that mass concentration is 3%, chitosan solution concentration 15g/L, control temperature is at 10 DEG C, the speed of dripping with 10s/ drips 5ml hexandial solution, and stir process 20 minutes, then immerses aramid fiber, rise to room temperature, pad, pick-up rate is 100%, and then 160 DEG C bake.
(3) prepare the palladium chloride solution of 100mg/L, immerse textile impregnation at 40 DEG C 60 minutes, 50 DEG C of oven dry.
(4) first silver ammino solution is prepared: 30g/L AgNO
3, drip ammoniacal liquor to clarification; Prepare reducing solution again: glucose 80g/L, tartaric acid 5g/L, ethanol 200mL/L, ethylenediamine 30mL/L.
Be that 1:5 mixes by silver ammino solution and reducing solution with volume ratio, be mixed with chemical plating liquid.Immerse fiber, carry out chemical silvering at 60 DEG C, plating 30 minutes.
(5) chemical silvering aramid fiber is dried under 100 DEG C of conditions.
The aramid fiber resistance prepared through this embodiment is 0.30 Ω/cm, supersound washing 30 minutes, resistance variations 5%.
Claims (10)
1. a method for aramid fiber conductive fiber chemical silvering, comprising:
(1) prepare acid permanganate soln, immerse aramid fiber, ultrasonic process 20-40 minute at 20-50 DEG C, then take out fiber and clean oven dry;
(2), under cryogenic conditions, crosslinking agent instilled in chitosan solution and stirs, then immerse aramid fiber, rise to room temperature, pad, bake; Wherein, the mass ratio of crosslinking agent and shitosan is 1:4-1:5;
(3) prepare palladium chloride solution, immerse aramid fiber, dry;
(4) prepare silver plating liquid, immerse aramid fiber, carry out chemical silvering, dry.
2. the method for a kind of aramid fiber conductive fiber chemical silvering according to claim 1, is characterized in that: in the acid permanganate soln in described step (1), potassium permanganate consumption is 3-10g/L; Wherein, acid is one or more in sulfuric acid, nitric acid, phosphoric acid; The mass fraction of acid is 5%-20%.
3. the method for a kind of aramid fiber conductive fiber chemical silvering according to claim 1, is characterized in that: the low temperature in described step (2) is 0-10 DEG C.
4. the method for a kind of aramid fiber conductive fiber chemical silvering according to claim 1, is characterized in that: the crosslinking agent in described step (2) is formaldehyde, glutaraldehyde, hexandial or citric acid.
5. the method for a kind of aramid fiber conductive fiber chemical silvering according to claim 1, is characterized in that: the concentration of the chitosan solution in described step (2) is 5-15g/L; The shitosan acetate dissolution of mass fraction 1%-4%.
6. the method for a kind of aramid fiber conductive fiber chemical silvering according to claim 1, is characterized in that: the pick-up rate of padding in described step (2) is 60%-100%.
7. the method for a kind of aramid fiber conductive fiber chemical silvering according to claim 1, is characterized in that: the baking temperature in described step (2) is 120-160 DEG C.
8. the method for a kind of aramid fiber conductive fiber chemical silvering according to claim 1, is characterized in that: the concentration of the palladium chloride solution in described step (3) is 30-100mg/L.
9. the method for a kind of aramid fiber conductive fiber chemical silvering according to claim 1, is characterized in that: the silver plating liquid in described step (4) consists of: silver ammino solution: 10-30g/L AgNO
3, drip ammoniacal liquor to clarification; Reducing solution: glucose 20-80g/L, tartaric acid 0.05-5g/L, ethanol 100-300mL/L, ethylenediamine 10-30mL/L, silver ammino solution and reducing solution are that 1:2 ~ 1:5 is mixed with chemical plating liquid with volume ratio.
10. the method for a kind of aramid fiber conductive fiber chemical silvering according to claim 1, it is characterized in that: the chemical silvering temperature in described step (4) is 40 ~ 60 DEG C, the chemical silvering time is 30-60 minute.
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Cited By (13)
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| CN106637930A (en) * | 2016-10-06 | 2017-05-10 | 常州市鼎升环保科技有限公司 | Anti-static conductive fiber material preparation method |
| CN106758150A (en) * | 2017-01-23 | 2017-05-31 | 西安工程大学 | A kind of method for improving kevlar fabric wetness guiding perspiration discharging performance |
| CN107164951A (en) * | 2017-07-03 | 2017-09-15 | 赣州西维尔金属材料科技有限公司 | A kind of preparation method of silver-plated conductive aramid fiber |
| CN107326657A (en) * | 2017-08-03 | 2017-11-07 | 陈志豪 | A kind of preparation method of silver-plated conductive aramid fiber |
| CN107354752A (en) * | 2017-06-21 | 2017-11-17 | 北京化工大学 | Cover silver-colored conductive fibers of F 12 and preparation method thereof in a kind of surface |
| CN107904927A (en) * | 2017-11-29 | 2018-04-13 | 广州天诺贸易有限公司 | The preparation method of nano Ag antibacterial fiber |
| CN110735326A (en) * | 2019-11-04 | 2020-01-31 | 济南雨墨科贸有限公司 | silver mask cloth and preparation method thereof |
| CN111118881A (en) * | 2020-01-17 | 2020-05-08 | 超美斯新材料股份有限公司 | Nano-zinc oxide modified aramid fiber and preparation method thereof |
| CN111254701A (en) * | 2020-03-12 | 2020-06-09 | 鲁东大学 | Aramid nanofiber composite material, preparation method thereof and application of aramid nanofiber composite material in adsorption of Hg ions in solution |
| CN111266136A (en) * | 2020-03-12 | 2020-06-12 | 鲁东大学 | Aramid nanofiber composite material, preparation method thereof and application thereof in photocatalytic degradation of rhodamine b |
| CN114195477A (en) * | 2021-11-29 | 2022-03-18 | 辽宁科大中驰镁建材科技有限公司 | Sulfur-oxygen-magnesium-based electromagnetic shielding material and preparation method thereof |
| WO2023082090A1 (en) * | 2021-11-10 | 2023-05-19 | 青岛科技大学 | Dendritic silver-plated aramid electrically conductive filler and preparation method therefor and application thereof, and polymer/dendritic silver-plated aramid composite material |
| CN116219741A (en) * | 2023-03-21 | 2023-06-06 | 鲁东大学 | Preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106637930A (en) * | 2016-10-06 | 2017-05-10 | 常州市鼎升环保科技有限公司 | Anti-static conductive fiber material preparation method |
| CN106758150A (en) * | 2017-01-23 | 2017-05-31 | 西安工程大学 | A kind of method for improving kevlar fabric wetness guiding perspiration discharging performance |
| CN107354752A (en) * | 2017-06-21 | 2017-11-17 | 北京化工大学 | Cover silver-colored conductive fibers of F 12 and preparation method thereof in a kind of surface |
| CN107354752B (en) * | 2017-06-21 | 2020-04-17 | 北京化工大学 | Surface-coated silver F-12 conductive fiber and preparation method thereof |
| CN107164951A (en) * | 2017-07-03 | 2017-09-15 | 赣州西维尔金属材料科技有限公司 | A kind of preparation method of silver-plated conductive aramid fiber |
| CN107326657A (en) * | 2017-08-03 | 2017-11-07 | 陈志豪 | A kind of preparation method of silver-plated conductive aramid fiber |
| CN107904927A (en) * | 2017-11-29 | 2018-04-13 | 广州天诺贸易有限公司 | The preparation method of nano Ag antibacterial fiber |
| CN110735326B (en) * | 2019-11-04 | 2022-06-07 | 济南雨墨科贸有限公司 | Silver mask cloth and preparation method thereof |
| CN110735326A (en) * | 2019-11-04 | 2020-01-31 | 济南雨墨科贸有限公司 | silver mask cloth and preparation method thereof |
| CN111118881A (en) * | 2020-01-17 | 2020-05-08 | 超美斯新材料股份有限公司 | Nano-zinc oxide modified aramid fiber and preparation method thereof |
| CN111118881B (en) * | 2020-01-17 | 2022-04-05 | 超美斯新材料股份有限公司 | Nano-zinc oxide modified aramid fiber and preparation method thereof |
| CN111266136A (en) * | 2020-03-12 | 2020-06-12 | 鲁东大学 | Aramid nanofiber composite material, preparation method thereof and application thereof in photocatalytic degradation of rhodamine b |
| CN111254701A (en) * | 2020-03-12 | 2020-06-09 | 鲁东大学 | Aramid nanofiber composite material, preparation method thereof and application of aramid nanofiber composite material in adsorption of Hg ions in solution |
| CN111266136B (en) * | 2020-03-12 | 2022-08-12 | 鲁东大学 | Aramid nanofiber composite material, preparation method thereof and application thereof in photocatalytic degradation of rhodamine b |
| WO2023082090A1 (en) * | 2021-11-10 | 2023-05-19 | 青岛科技大学 | Dendritic silver-plated aramid electrically conductive filler and preparation method therefor and application thereof, and polymer/dendritic silver-plated aramid composite material |
| CN114195477A (en) * | 2021-11-29 | 2022-03-18 | 辽宁科大中驰镁建材科技有限公司 | Sulfur-oxygen-magnesium-based electromagnetic shielding material and preparation method thereof |
| CN116219741A (en) * | 2023-03-21 | 2023-06-06 | 鲁东大学 | Preparation method of conductive and electromagnetic shielding crosslinked dendrimer silver-plated meta-aramid fiber |
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