CN103668944B - A kind of aramid fiber Conductive Silver-Coated PET Fibers and preparation method thereof - Google Patents
A kind of aramid fiber Conductive Silver-Coated PET Fibers and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of preparation method of aramid fiber Conductive Silver-Coated PET Fibers, this preparation method carries out as follows: a. alligatoring: inserted by aramid fiber in the mixed liquor of NaOH, absolute ethyl alcohol and Yu Weishui and carry out alligatoring, then extremely neutral with water cleaning; B. be hydrolyzed: a step is inserted in acid solution through the aramid fiber of roughening treatment and is hydrolyzed; C. palladium salt activation: b step is inserted in the mixed liquor of hydrochloric acid, palladium bichloride, stannous chloride and Yu Weishui through the aramid fiber of palladium salt activation processing and carries out the activation of palladium salt; D. reduce: step c is inserted in the mixed liquor of hydrochloric acid, inferior sodium phosphate and Yu Weishui through the aramid fiber of palladium salt activation processing and reduces; E. chemical silvering: Step d is inserted in the chemical plating liquid of silver nitrate, NaOH, ammoniacal liquor, complexing agent, reductant and Yu Weishui through the aramid fiber of reduction treatment and carries out chemical silvering; F. dry: the aramid fiber routine of step e after chemical silvering is dried, obtains product.
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
Have the features such as density is little, intensity is high, Heat stability is good due to aramid fiber, the conductive fiber using aramid fiber to prepare for base material, while imparting aramid fiber satisfactory electrical conductivity, inherits 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 meets fiery or high heat and melting, drippage or burning, easily causes secondary to burn to user, is difficult to the requirement meeting high strength, high-temperature resistant performance.The conductive fiber using aramid fiber to prepare, also can be aerospace equipment and provides electromagnetic shielding material.
But aramid fiber is a kind of rigid macromolecule with high-crystallinity, high-orientation, there is a large amount of aromatic rings in aramid fiber molecule, such that aramid fiber surface inertia is large, chemism is low, be difficult to realize metal attachment." preparation of silver-plated conduction aramid fiber and performance study thereof " that the people such as beam Jingjing, Zou Xinguo carry out; need use a kind of special metal reagent (NaH-DMSO), complex process, and coating uniformity, adhesive force are not good enough; still be in the laboratory research stage, large-scale production needs cannot be met.And the patent of invention 201210425097.1 " a kind of Aramid fiber surface metallization treatment method " of the people such as Duan Yonghua, use copper nickel metal layer, coating fragility is large, and 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.
An object of the present invention realizes by following technical measures:
This aramid fiber Conductive Silver-Coated PET Fibers take aramid fiber as base material, is connected with outward and carries out coated silver layer by electroless plating method.
An object of the present invention also realizes by 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 realizes by 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:
------palladium salt activates, and------chemical silvering---cleans---oven dry---aramid fiber silver plated fiber product in reduction in aramid fiber hydrolysis in aramid fiber alligatoring.
A. alligatoring: aramid fiber is inserted by containing in the mixed liquor of the NaOH of 10-200g, the absolute ethyl alcohol of 10-50g and Yu Weishui in often liter of mixed liquor, alligatoring 30-120min under this mixeding liquid temperature is 60-100 DEG C of condition, then extremely neutral with water cleaning;
B. be hydrolyzed: it is in the acid solution of 50-200ml/L that a step is inserted volumetric concentration through the aramid fiber of roughening treatment, is 40-80 DEG C of Water Under solution 10-100min in this acid solution temperature, then with water cleaning to neutral;
C. palladium salt activation: b step is inserted in the mixed liquor by the hydrochloric acid containing 5-30ml in often liter of mixed liquor, the palladium bichloride of 0.1-1g, the stannous chloride of 10-30g and Yu Weishui through the aramid fiber of palladium salt activation processing, palladium salt activation 10-30min under this mixeding liquid temperature is 40-80 DEG C of condition;
D. reduce: step c is inserted by containing in the mixed liquor of the hydrochloric acid of 10-100ml, the inferior sodium phosphate of 1-6g and Yu Weishui in often liter of mixed liquor through the aramid fiber of palladium salt activation processing, under this mixeding liquid temperature is room temperature condition, reduce 1-5min, then with water cleaning to neutral;
E. chemical silvering: in the chemical plating liquid that Step d is inserted by the ammoniacal liquor of the NaOH of the silver nitrate containing 1-5g in often liter of chemical plating liquid, 0.02-0.5g, 1.5-10ml, the complexing agent of 0.1g-5g, the reductant of 3-20g and Yu Weishui through the aramid fiber of reduction treatment, chemical silvering 30-120min under this mixed chemical silver plating liquid liquid temp is 30-60 DEG C of condition, then extremely neutral with water cleaning;
F. dry: the aramid fiber routine of step e after chemical silvering is dried, obtains product.
Two of object of the present invention also realizes by following technical measures:
Acid solution above described in b step is hydrochloric acid, a kind of in nitric acid, sulfuric acid, phosphoric acid, glacial acetic acid solution or two or more mixed solution mixed with arbitrary proportion arbitrarily; Complexing agent described in step e is Monosodium Edetate, disodium ethylene diamine tetraacetate, sodium versenate or tetrasodium ethylenediamine tetraacetate; Reductant described in step e is glucose, a kind of in sodium tartrate, sodium potassium tartrate tetrahydrate, inferior sodium phosphate or two or more mixture mixed 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, suitably can increase wash number according to base material difference, until cleaning fluid shows as neutrality.
Above-mentioned drying course, bake out temperature 60-120 DEG C, 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's tool compared with conventional method has the following advantages:
there is a large amount of aromatic rings in aramid fiber molecule, make that aramid fiber chemical inertness is large, surface-activity is low.The present invention, by acid solution process, makes aramid fiber be hydrolyzed, at fiber surface introducing-NH
2,-COOH isoreactivity group, increase surface activity of aramid fiber, for chemical silvering provides condition.
the chemical plating fluid that the present invention uses, composition is simple, product is more single, be easy to control and detect, different size and material base material coordinate corresponding reaction solution concentration, silver ion rate of release and silver layer deposition velocity keep relative equilibrium, and coating procedure plating solution remains clear state, and silver layer is even, light is fine and close.
(3) adopt the aramid fiber Conductive Silver-Coated PET Fibers prepared of the present invention, have that density is little, intensity is high, good conductivity (specific insulation :≤10
-5Ω cm) etc. feature.Simple, safe and reliable, easy to operate, the economic environmental protection of the inventive method technique, is easy to large-scale production.
Detailed description of the invention:
Following examples are optimization formulas prepared by aramid fiber silver plated fiber; these non-limiting implementation of filling a prescription; just for illustrating the present invention, the formula that those skilled in the art can filter out according to thinking of the present invention and proportioning of selecting materials completely is protection scope of the present invention.
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 containing in the mixed liquor of the NaOH of 10g, the absolute ethyl alcohol of 50g and Yu Weishui in often liter of mixed liquor, alligatoring 120min under this mixeding liquid temperature is 60 DEG C of conditions, then extremely neutral with water cleaning;
B. be hydrolyzed: it is in the hydrochloric acid solution of 50ml/L that a step is inserted volumetric concentration through the aramid fiber of roughening treatment, is 80 DEG C of Water Under solution 10min in this acid solution temperature, then with water cleaning to neutral;
C. palladium salt activation: b step is inserted in the mixed liquor by the hydrochloric acid containing 30ml in often liter of mixed liquor, the palladium bichloride of 0.1g, the stannous chloride of 30g and Yu Weishui through the meta-aramid fibers (1313) of palladium salt activation processing, palladium salt activation 30min under this mixeding liquid temperature is 40 DEG C of conditions;
D. reduce: step c is inserted by containing in the mixed liquor of the hydrochloric acid of 10ml, the inferior sodium phosphate of 6g and Yu Weishui in often liter of mixed liquor through the meta-aramid fibers (1313) of palladium salt activation processing, under this mixeding liquid temperature is room temperature condition, reduce 1min, then with water cleaning to neutral;
E. chemical silvering: Step d is inserted by the NaOH of the silver nitrate containing 5g in often liter of chemical plating liquid, 0.02g, the ammoniacal liquor of 10ml, the glucose of Monosodium Edetate 20g of 0.1g and the chemical plating liquid of Yu Weishui through the meta-aramid fibers (1313) of reduction treatment, chemical silvering 120min under this chemical silvering liquid temp is 30 DEG C of conditions, then extremely neutral with water cleaning;
F. dry: the meta-aramid fibers of step e after chemical silvering (1313) routine is dried, 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 containing in the mixed liquor of the NaOH of 200g, the absolute ethyl alcohol of 10g and Yu Weishui in often liter of mixed liquor, alligatoring 30min under this mixeding liquid temperature is 100 DEG C of conditions, then extremely neutral with water cleaning;
B. be hydrolyzed: it is in the hydrochloric acid solution of 200ml/L that a step is inserted volumetric concentration through the aramid fiber of roughening treatment, is 40 DEG C of Water Under solution 100min in this acid solution temperature, then with water cleaning to neutral;
C. palladium salt activation: b step is inserted in the mixed liquor by the hydrochloric acid containing 5ml in often liter of mixed liquor, the palladium bichloride of 1g, the stannous chloride of 10g and Yu Weishui through the meta-aramid fibers (1313) of palladium salt activation processing, palladium salt activation 10min under this mixeding liquid temperature is 80 DEG C of conditions;
D. reduce: step c is inserted by containing in the mixed liquor of the hydrochloric acid of 100ml, the inferior sodium phosphate of 1g and Yu Weishui in often liter of mixed liquor through the meta-aramid fibers (1313) of palladium salt activation processing, under this mixeding liquid temperature is room temperature condition, reduce 5min, then with water cleaning to neutral;
E. chemical silvering: in the chemical plating liquid that Step d is inserted by the ammoniacal liquor of the NaOH of the silver nitrate containing 1g in often liter of chemical plating liquid, 0.5g, 1.5ml, the Monosodium Edetate of 5g, the glucose of 3g and Yu Weishui through the meta-aramid fibers (1313) of reduction treatment, chemical silvering 30min under this chemical silvering liquid temp is 60 DEG C of conditions, then extremely neutral with water cleaning;
F. dry: the meta-aramid fibers of step e after chemical silvering (1313) routine is dried, 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 containing in the mixed liquor of the NaOH of 100g, the absolute ethyl alcohol of 35g and Yu Weishui in often liter of mixed liquor, alligatoring 8min under this mixeding liquid temperature is 80 conditions, then extremely neutral with water cleaning;
B. be hydrolyzed: it is in the hydrochloric acid solution of 120ml/L that a step is inserted volumetric concentration through the aramid fiber of roughening treatment, is 60 DEG C of Water Under solution 60min in this acid solution temperature, then with water cleaning to neutral;
C. palladium salt activation: b step is inserted in the mixed liquor by the hydrochloric acid containing 15ml in often liter of mixed liquor, the palladium bichloride of 0.5g, the stannous chloride of 20g and Yu Weishui through the meta-aramid fibers (1313) of palladium salt activation processing, palladium salt activation 20min under this mixeding liquid temperature is 60 DEG C of conditions;
D. reduce: step c is inserted by containing in the mixed liquor of the hydrochloric acid of 50ml, the inferior sodium phosphate of 4g and Yu Weishui in often liter of mixed liquor through the meta-aramid fibers (1313) of palladium salt activation processing, under this mixeding liquid temperature is room temperature condition, reduce 3min, then with water cleaning to neutral;
E. chemical silvering: in the chemical plating liquid that Step d is inserted by the ammoniacal liquor of the NaOH of the silver nitrate containing 3g in often liter of chemical plating liquid, 0.04g, 6ml, the Monosodium Edetate of 2.5g, the glucose of 10g and Yu Weishui through the meta-aramid fibers (1313) of reduction treatment, chemical silvering 80min under this chemical silvering liquid temp is 45 DEG C of conditions, then extremely neutral with water cleaning;
F. dry: the meta-aramid fibers of step e after chemical silvering (1313) routine is dried, obtains product (specific insulation :≤10
-5Ω cm).
Embodiment 4:
Replace meta-aramid fibers (1313) unlike with para-aramid fiber (1414), other is respectively with embodiment 1-3.
Embodiment 5:
Replace hydrochloric acid solution unlike in b step with salpeter solution, other is respectively with embodiment 1-4.
Embodiment 6:
Replace hydrochloric acid solution unlike in b step with sulfuric acid solution, other is respectively with embodiment 1-4.
Embodiment 7:
Replace hydrochloric acid solution unlike in b step with phosphoric acid solution, other is respectively with embodiment 1-4.
Embodiment 8:
Replace hydrochloric acid solution unlike in b step with glacial acetic acid solution, other is respectively with embodiment 1-4.
Embodiment 9:
Replace hydrochloric acid solution unlike in b step with hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, any mixed solution that two or more mixes with arbitrary proportion of glacial acetic acid solution, other is respectively with embodiment 1-4.
Embodiment 10:
Replace disodium ethylene diamine tetraacetate unlike in step e with disodium ethylene diamine tetraacetate, other is respectively with embodiment 1-9.
Embodiment 11:
Replace disodium ethylene diamine tetraacetate unlike in step e with sodium versenate, other is respectively with embodiment 1-9.
Embodiment 12:
Replace disodium ethylene diamine tetraacetate unlike in step e with tetrasodium ethylenediamine tetraacetate, other is respectively with embodiment 1-9.
Embodiment 13:
Replace glucose unlike in step e with sodium tartrate, other is respectively with embodiment 1-12.
Embodiment 14:
Replace glucose unlike in step e with sodium potassium tartrate tetrahydrate, other is respectively with embodiment 1-12.
Embodiment 15:
Replace glucose unlike in step e by inferior sodium phosphate, other is respectively with embodiment 1-12.
Embodiment 16:
Replace glucose unlike in step e with glucose, sodium tartrate, sodium potassium tartrate tetrahydrate, any mixture that two or more mixes with arbitrary proportion of inferior sodium phosphate, other is respectively with embodiment 1-12.
Claims (2)
1. an aramid fiber Conductive Silver-Coated PET Fibers, it is characterized in that it take aramid fiber as base material, be connected with outward and carry out coated silver layer by electroless plating method, described base material is meta-aramid fibers or para-aramid fiber, and described base material is fibre section width 0.36mm-1.12mm, fibre section thickness 0.038mm-0.076mm.
2. the preparation method of a kind of aramid fiber Conductive Silver-Coated PET Fibers according to claim 1, is characterized in that this preparation method carries out as follows:
A. alligatoring: aramid fiber is inserted by containing in the mixed liquor of the NaOH of 10-200g, the absolute ethyl alcohol of 10-50g and Yu Weishui in often liter of mixed liquor, alligatoring 30-120min under this mixeding liquid temperature is 60-100 DEG C of condition, then extremely neutral with water cleaning;
B. be hydrolyzed: it is in the acid solution of 50-200ml/L that a step is inserted volumetric concentration through the aramid fiber of roughening treatment, is 40-80 DEG C of Water Under solution 10-100min in this acid solution temperature, then with water cleaning to neutral; Described acid solution is one or more mixed liquors in hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, glacial acetic acid solution;
C. palladium salt activation: b step is inserted in the mixed liquor by the hydrochloric acid containing 5-30ml in often liter of mixed liquor, the palladium bichloride of 0.1-1g, the stannous chloride of 10-30g and Yu Weishui through the aramid fiber of palladium salt activation processing, palladium salt activation 10-30min under this mixeding liquid temperature is 40-80 DEG C of condition;
D. reduce: step c is inserted by containing in the mixed liquor of the hydrochloric acid of 10-100ml, the inferior sodium phosphate of 1-6g and Yu Weishui in often liter of mixed liquor through the aramid fiber of palladium salt activation processing, under this mixeding liquid temperature is room temperature condition, reduce 1-5min, then with water cleaning to neutral;
E. chemical silvering: in the chemical plating liquid that Step d is inserted by the ammoniacal liquor of the NaOH of the silver nitrate containing 1-5g in often liter of chemical plating liquid, 0.02-0.5g, 1.5-10ml, the complexing agent of 0.1g-5g, the reductant of 3-20g and Yu Weishui through the aramid fiber of reduction treatment, chemical silvering 30-120min under this chemical silvering liquid temp is 30-60 DEG C of condition, then extremely neutral with water cleaning; Described complexing agent is Monosodium Edetate, disodium ethylene diamine tetraacetate, sodium versenate or tetrasodium ethylenediamine tetraacetate; Described reductant is one or more mixtures in glucose, sodium tartrate, sodium potassium tartrate tetrahydrate, inferior sodium phosphate;
F. dry: the aramid fiber routine of step e after chemical silvering is dried, obtains product.
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