CN103668944A - Silvered aramid conductive fiber and preparation method thereof - Google Patents
Silvered aramid conductive fiber and preparation method thereof Download PDFInfo
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- CN103668944A CN103668944A CN201310685423.7A CN201310685423A CN103668944A CN 103668944 A CN103668944 A CN 103668944A CN 201310685423 A CN201310685423 A CN 201310685423A CN 103668944 A CN103668944 A CN 103668944A
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Abstract
The invention provides a silvered aramid conductive fiber and a preparation method thereof. The preparation method is conducted according to the steps as follows: a. coarsening: coarsening the aramid fiber through putting the fiber into a mixed solution of sodium hydroxide, absolute ethanol and the balance of water, and neutralizing the fiber by rinsing; b. hydrolyzing: hydrolyzing the coarsened aramid fiber by putting the fiber into an acid solution; c. activation of palladium salt: activating the hydrolyzed aramid fiber subjected to activation of palladium salt in step b by putting the fiber into a mixed solution of hydrochloric acid, palladium chloride, stannous chloride and the balance of water; d. reducing: reducing the palladium salt activated aramid fiber in step c by putting the fiber into a mixed solution of hydrochloric acid, sodium hypophosphite and the balance of water; e. chemical silvering: chemical silvering the reduced aramid fiber in step d by putting the fiber into a chemical silvering solution of silver nitrate, sodium hydroxide, aqua ammonia, a complex agent, a reducing agent and the balance of water; f. drying: drying the chemical silvered aramid fiber in step e in the conventional manner to obtain the silvered aramid conductive fiber.
Description
Technical field
The invention belongs to conductive fiber field, relate to a kind of aramid fiber Conductive Silver-Coated PET Fibers and preparation method thereof.
Background technology
Due to aramid fiber, have the features such as density is little, intensity is high, Heat stability is good, the conductive fiber that uses aramid fiber to prepare for base material, when having given aramid fiber satisfactory electrical conductivity, has inherited the premium properties of aramid fiber matrix.Other polyester base material silver plated fiber, is mainly used in visit to the parents of schoolchildren or young workers medical treatment and sports goods aspect, and this series products is met fire or high heat is melting, drippage or burning, easily to user, causes secondary to burn, and is difficult to meet the requirement of high strength, high-temperature resistant performance.The conductive fiber that uses aramid fiber to prepare, also can be aerospace equipment electromagnetic shielding material is provided.
But aramid fiber is a kind of rigid macromolecule with high-crystallinity, high-orientation, in aramid fiber molecule, there is a large amount of aromatic rings, make that aramid fiber surface inertia is large, chemism is low, be difficult to realize metal and adhere to.Preparation and the performance study > > thereof of the silver-plated conduction aramid fiber of < < that the people such as beam Jingjing, Zou Xinguo carry out; need to use a kind of special metal reagent (NaH-DMSO); complex process; and coating uniformity, adhesive force is not good enough; still in the laboratory research stage, cannot meet large-scale production needs.And the people's such as Duan Yonghua patent of invention 201210425097.1 < < aramid fiber surface metallization treating method > >, what use is copper nickel metal layer, coating fragility is large, fiber stiffness is high, adhesion and poor electric conductivity.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art, and one of object is to provide that a kind of density is little, intensity is high, good conductivity (specific insulation :≤10
-5Ω cm) aramid fiber Conductive Silver-Coated PET Fibers; Two of object is to provide simple, safe and reliable, easy to operate, the economic environmental protection of a kind of technique, is easy to the dimension preparation method of the aramid fiber Conductive Silver-Coated PET Fibers of large-scale production.
One of object of the present invention can be achieved by the following technical measures:
This aramid fiber Conductive Silver-Coated PET Fibers be take aramid fiber as base material, is connected with outward by electroless plating method and carries out coated silver layer.
One of object of the present invention also can be achieved by the following technical measures:
Described base material is meta-aramid fibers (1313) or para-aramid fiber (1414); Described base material is fibre section width 0.36mm-1.12mm, fibre section thickness 0.038mm-0.076mm.
Two of object of the present invention can be achieved by the following technical measures:
The preparation method of a kind of aramid fiber Conductive Silver-Coated PET Fibers that one of object is described carries out as follows:
------------chemical silvering---cleans---oven dry---aramid fiber silver plated fiber product to the activation of palladium salt in reduction in aramid fiber hydrolysis in aramid fiber alligatoring.
A. alligatoring: aramid fiber is inserted by the mixed liquor of the absolute ethyl alcohol of the NaOH that contains 10-200g in every liter of mixed liquor, 10-50g and Yu Weishui, is alligatoring 30-120min under 60-100 ℃ of condition at this mixeding liquid temperature, then water cleans to neutral;
B. hydrolysis: a step is inserted in the acid solution that volumetric concentration is 50-200ml/L through the aramid fiber of roughening treatment, is 40-80 ℃ of Water Under solution 10-100min in this acid solution temperature, then water cleans to neutral;
C. palladium salt activation: the hydrochloric acid that b step is contained to 5-30ml in the aramid fiber of palladium salt activation processing is inserted by every liter of mixed liquor, the palladium bichloride of 0.1-1g are, in the mixed liquor of the stannous chloride of 10-30g and Yu Weishui, be palladium salt activation 10-30min under 40-80 ℃ of condition at this mixeding liquid temperature;
D. reduction: in the hydrochloric acid that c step is contained to 10-100ml in the aramid fiber of palladium salt activation processing is inserted by every liter of mixed liquor, the inferior sodium phosphate of 1-6g and the mixed liquor of Yu Weishui, at this mixeding liquid temperature, be under room temperature condition, to reduce 1-5min, then water cleans to neutral;
E. chemical silvering: the silver nitrate that the aramid fiber that d step is processed through reduction contains 1-5g in inserting by every liter of chemical plating liquid, the NaOH of 0.02-0.5g, the complexing agent of the ammoniacal liquor of 1.5-10ml, 0.1g-5g are, in the chemical plating liquid of the reductant of 3-20g and Yu Weishui, at this mixed chemical silver plating liquid liquid temp, be chemical silvering 30-120min under 30-60 ℃ of condition, then water cleans to neutral;
F. dry: the conventional oven dry of aramid fiber by e step after chemical silvering, obtains product.
Two of object of the present invention also can be achieved by the following technical measures:
Acid solution described in b step is a kind of in hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, glacial acetic acid solution or two or more mixed solution mixing with arbitrary proportion arbitrarily above; Complexing agent described in e step is Monosodium Edetate, disodium ethylene diamine tetraacetate, sodium versenate or tetrasodium ethylenediamine tetraacetate; Reductant described in e step is a kind of in glucose, sodium tartrate, sodium potassium tartrate tetrahydrate, inferior sodium phosphate or two or more mixture mixing with arbitrary proportion arbitrarily.
Above-mentioned aramid fiber Conductive Silver-Coated PET Fibers, its performance meets: specific insulation :≤10
-5the features such as Ω cm.
Above-mentioned cleaning process, can suitably increase wash number according to base material difference, until cleaning fluid shows as neutrality.
Above-mentioned drying course, bake out temperature 60-120 ℃, can carry out hot blast drying online, puts into hothouse and concentrate oven dry after also can rolling off the production line.
The present invention compares tool with conventional method and has the following advantages:
(3) the aramid fiber Conductive Silver-Coated PET Fibers that adopts the present invention to prepare, has that density is little, intensity is high, good conductivity (specific insulation :≤10
-5Ω cm) feature such as.Simple, safe and reliable, easy to operate, the economic environmental protection of the inventive method technique, is easy to large-scale production.
The specific embodiment:
Following examples are optimization formulas prepared by aramid fiber silver plated fiber; these formula indefiniteness embodiments; just, for illustrating the present invention, those skilled in the art can be protection scope of the present invention according to thinking of the present invention and the formula that the proportioning of selecting materials filters out completely.
Embodiment 1:
Described base material is meta-aramid fibers (1313) or para-aramid fiber (1414).
Described base material is fibre section width 0.36mm, fibre section thickness 0.076mm.
This preparation method carries out as follows:
A. alligatoring: the meta-aramid fibers (1313) of fibre section width 0.36mm, fibre section thickness 0.076mm is inserted by the mixed liquor of the absolute ethyl alcohol of the NaOH that contains 10g in every liter of mixed liquor, 50g and Yu Weishui, at this mixeding liquid temperature, be alligatoring 120min under 60 ℃ of conditions, then water cleans to neutral;
B. hydrolysis: a step is inserted in the hydrochloric acid solution that volumetric concentration is 50ml/L through the aramid fiber of roughening treatment, is 80 ℃ of Water Under solution 10min in this acid solution temperature, then water cleans to neutral;
C. palladium salt activation: the hydrochloric acid that b step is contained to 30ml in the meta-aramid fibers (1313) of palladium salt activation processing is inserted by every liter of mixed liquor, the palladium bichloride of 0.1g are, in the mixed liquor of the stannous chloride of 30g and Yu Weishui, be palladium salt activation 30min under 40 ℃ of conditions at this mixeding liquid temperature;
D. reduction: in hydrochloric acid, the inferior sodium phosphate of 6g and the mixed liquor of Yu Weishui that c step is contained to 10ml in the meta-aramid fibers (1313) of palladium salt activation processing is inserted by every liter of mixed liquor, at this mixeding liquid temperature, be under room temperature condition, to reduce 1min, then water cleans to neutral;
E. chemical silvering: the silver nitrate that the meta-aramid fibers (1313) that d step is processed through reduction contains 5g in inserting by every liter of chemical plating liquid, the NaOH of 0.02g are, in the glucose of Monosodium Edetate 20g and the chemical plating liquid of Yu Weishui of the ammoniacal liquor of 10ml, 0.1g, at this chemical silvering liquid temp, be chemical silvering 120min under 30 ℃ of conditions, then water cleans to neutral;
F. dry: the meta-aramid fibers by e step after chemical silvering (1313) is conventional dries, and obtains product (specific insulation :≤10
-5Ω cm).
Embodiment 2:
This preparation method carries out as follows:
A. alligatoring: the meta-aramid fibers (1313) of fibre section width 1.12mm, fibre section thickness 0.038mmmm is inserted by the mixed liquor of the absolute ethyl alcohol of the NaOH that contains 200g in every liter of mixed liquor, 10g and Yu Weishui, at this mixeding liquid temperature, be alligatoring 30min under 100 ℃ of conditions, then water cleans to neutral;
B. hydrolysis: a step is inserted in the hydrochloric acid solution that volumetric concentration is 200ml/L through the aramid fiber of roughening treatment, is 40 ℃ of Water Under solution 100min in this acid solution temperature, then water cleans to neutral;
C. palladium salt activation: the hydrochloric acid that b step is contained to 5ml in the meta-aramid fibers (1313) of palladium salt activation processing is inserted by every liter of mixed liquor, the palladium bichloride of 1g are, in the mixed liquor of the stannous chloride of 10g and Yu Weishui, be palladium salt activation 10min under 80 ℃ of conditions at this mixeding liquid temperature;
D. reduction: in hydrochloric acid, the inferior sodium phosphate of 1g and the mixed liquor of Yu Weishui that c step is contained to 100ml in the meta-aramid fibers (1313) of palladium salt activation processing is inserted by every liter of mixed liquor, at this mixeding liquid temperature, be under room temperature condition, to reduce 5min, then water cleans to neutral;
E. chemical silvering: the silver nitrate that the meta-aramid fibers (1313) that d step is processed through reduction contains 1g in inserting by every liter of chemical plating liquid, the NaOH of 0.5g, the Monosodium Edetate of the ammoniacal liquor of 1.5ml, 5g are, in the chemical plating liquid of the glucose of 3g and Yu Weishui, at this chemical silvering liquid temp, be chemical silvering 30min under 60 ℃ of conditions, then water cleans to neutral;
F. dry: the meta-aramid fibers by e step after chemical silvering (1313) is conventional dries, and obtains product (specific insulation :≤10
-5Ω cm).
Embodiment 3:
This preparation method carries out as follows:
A. alligatoring: the meta-aramid fibers (1313) of fibre section width 0.8mm, fibre section thickness 0.055 is inserted by the mixed liquor of the absolute ethyl alcohol of the NaOH that contains 100g in every liter of mixed liquor, 35g and Yu Weishui, at this mixeding liquid temperature, be alligatoring 8min under 80 conditions, then water cleans to neutral;
B. hydrolysis: a step is inserted in the hydrochloric acid solution that volumetric concentration is 120ml/L through the aramid fiber of roughening treatment, is 60 ℃ of Water Under solution 60min in this acid solution temperature, then water cleans to neutral;
C. palladium salt activation: the hydrochloric acid that b step is contained to 15ml in the meta-aramid fibers (1313) of palladium salt activation processing is inserted by every liter of mixed liquor, the palladium bichloride of 0.5g are, in the mixed liquor of the stannous chloride of 20g and Yu Weishui, be palladium salt activation 20min under 60 ℃ of conditions at this mixeding liquid temperature;
D. reduction: in hydrochloric acid, the inferior sodium phosphate of 4g and the mixed liquor of Yu Weishui that c step is contained to 50ml in the meta-aramid fibers (1313) of palladium salt activation processing is inserted by every liter of mixed liquor, at this mixeding liquid temperature, be under room temperature condition, to reduce 3min, then water cleans to neutral;
E. chemical silvering: the silver nitrate that the meta-aramid fibers (1313) that d step is processed through reduction contains 3g in inserting by every liter of chemical plating liquid, the NaOH of 0.04g, the Monosodium Edetate of the ammoniacal liquor of 6ml, 2.5g are, in the chemical plating liquid of the glucose of 10g and Yu Weishui, at this chemical silvering liquid temp, be chemical silvering 80min under 45 ℃ of conditions, then water cleans to neutral;
F. dry: the meta-aramid fibers by e step after chemical silvering (1313) is conventional dries, and obtains product (specific insulation :≤10
-5Ω cm).
Embodiment 4:
Different is to replace meta-aramid fibers (1313) with para-aramid fiber (1414), and other is respectively with embodiment 1-3.
Embodiment 5:
Different is with salpeter solution, to replace hydrochloric acid solution in b step, and other is respectively with embodiment 1-4.
Embodiment 6:
Different is with sulfuric acid solution, to replace hydrochloric acid solution in b step, and other is respectively with embodiment 1-4.
Embodiment 7:
Different is with phosphoric acid solution, to replace hydrochloric acid solution in b step, and other is respectively with embodiment 1-4.
Embodiment 8:
Different is with glacial acetic acid solution, to replace hydrochloric acid solution in b step, and other is respectively with embodiment 1-4.
Embodiment 9:
Different is mixed solution replacement hydrochloric acid solution that in b step, two or more mixes with arbitrary proportion arbitrarily with hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, glacial acetic acid solution, and other is respectively with embodiment 1-4.
Embodiment 10:
Different is with disodium ethylene diamine tetraacetate, to replace disodium ethylene diamine tetraacetate in e step, and other is respectively with embodiment 1-9.
Embodiment 11:
Different is with sodium versenate, to replace disodium ethylene diamine tetraacetate in e step, and other is respectively with embodiment 1-9.
Embodiment 12:
Different is with tetrasodium ethylenediamine tetraacetate, to replace disodium ethylene diamine tetraacetate in e step, and other is respectively with embodiment 1-9.
Embodiment 13:
Different is with sodium tartrate, to replace glucose in e step, and other is respectively with embodiment 1-12.
Embodiment 14:
Different is with sodium potassium tartrate tetrahydrate, to replace glucose in e step, and other is respectively with embodiment 1-12.
Embodiment 15:
Different is by inferior sodium phosphate, to replace glucose in e step, and other is respectively with embodiment 1-12.
Embodiment 16:
Different is mixture replacement glucose that in e step, two or more mixes with arbitrary proportion arbitrarily by glucose, sodium tartrate, sodium potassium tartrate tetrahydrate, inferior sodium phosphate, and other is respectively with embodiment 1-12.
Claims (7)
1. an aramid fiber Conductive Silver-Coated PET Fibers, is characterized in that it take aramid fiber as base material, is connected with outward by electroless plating method and carries out coated silver layer.
2. a kind of aramid fiber Conductive Silver-Coated PET Fibers according to claim 1, is characterized in that described base material is meta-aramid fibers or para-aramid fiber.
3. a kind of aramid fiber Conductive Silver-Coated PET Fibers according to claim 1 and 2, is characterized in that described base material is fibre section width 0.36mm-1.12mm, fibre section thickness 0.038mm-0.076mm.
4. the preparation method of a kind of aramid fiber Conductive Silver-Coated PET Fibers claimed in claim 1, is characterized in that this preparation method carries out as follows:
A. alligatoring: aramid fiber is inserted by the mixed liquor of the absolute ethyl alcohol of the NaOH that contains 10-200g in every liter of mixed liquor, 10-50g and Yu Weishui, is alligatoring 30-120min under 60-100 ℃ of condition at this mixeding liquid temperature, then water cleans to neutral;
B. hydrolysis: a step is inserted in the acid solution that volumetric concentration is 50-200ml/L through the aramid fiber of roughening treatment, is 40-80 ℃ of Water Under solution 10-100min in this acid solution temperature, then water cleans to neutral;
C. palladium salt activation: the hydrochloric acid that b step is contained to 5-30ml in the aramid fiber of palladium salt activation processing is inserted by every liter of mixed liquor, the palladium bichloride of 0.1-1g are, in the mixed liquor of the stannous chloride of 10-30g and Yu Weishui, be palladium salt activation 10-30min under 40-80 ℃ of condition at this mixeding liquid temperature;
D. reduction: in the hydrochloric acid that c step is contained to 10-100ml in the aramid fiber of palladium salt activation processing is inserted by every liter of mixed liquor, the inferior sodium phosphate of 1-6g and the mixed liquor of Yu Weishui, at this mixeding liquid temperature, be under room temperature condition, to reduce 1-5min, then water cleans to neutral;
E. chemical silvering: the silver nitrate that the aramid fiber that d step is processed through reduction contains 1-5g in inserting by every liter of chemical plating liquid, the NaOH of 0.02-0.5g, the complexing agent of the ammoniacal liquor of 1.5-10ml, 0.1g-5g are, in the chemical plating liquid of the reductant of 3-20g and Yu Weishui, at this chemical silvering liquid temp, be chemical silvering 30-120min under 30-60 ℃ of condition, then water cleans to neutral;
F. dry: the conventional oven dry of aramid fiber by e step after chemical silvering, obtains product.
5. the preparation method of a kind of aramid fiber Conductive Silver-Coated PET Fibers according to claim 4, is characterized in that the acid solution described in b step is one or more mixed liquors in hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, glacial acetic acid solution.
6. the preparation method of a kind of aramid fiber Conductive Silver-Coated PET Fibers according to claim 4, is characterized in that the complexing agent described in e step is Monosodium Edetate, disodium ethylene diamine tetraacetate, sodium versenate or tetrasodium ethylenediamine tetraacetate.
7. the preparation method of a kind of aramid fiber Conductive Silver-Coated PET Fibers according to claim 4, is characterized in that the reductant described in e step is one or more mixtures in glucose, sodium tartrate, sodium potassium tartrate tetrahydrate, inferior sodium phosphate.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104179004A (en) * | 2014-08-21 | 2014-12-03 | 大连工业大学 | Silver-plated conductive polyester fiber and preparation method thereof |
| CN104532553A (en) * | 2014-12-19 | 2015-04-22 | 东华大学 | Method for chemical silver-plating of aramid conductive fibers |
| CN104805685A (en) * | 2015-05-15 | 2015-07-29 | 张利荣 | Novel fiber or textile cold piling chemical silvering method |
| CN105350295A (en) * | 2014-08-19 | 2016-02-24 | 苏州钟纺纺织科技有限公司 | Preparation method of polyamide conductive fibers |
| CN105369601A (en) * | 2014-08-19 | 2016-03-02 | 苏州钟纺纺织科技有限公司 | Natural silk electric conduction fiber preparation method |
| 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 |
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| CN105369601A (en) * | 2014-08-19 | 2016-03-02 | 苏州钟纺纺织科技有限公司 | Natural silk electric conduction fiber preparation method |
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| 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 |
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| 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 |
| 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 |
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