CN109881189A - The preparation method for the aromatic polyamide staple fiber that metallizes and stand-by provision processed - Google Patents

The preparation method for the aromatic polyamide staple fiber that metallizes and stand-by provision processed Download PDF

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CN109881189A
CN109881189A CN201910281041.5A CN201910281041A CN109881189A CN 109881189 A CN109881189 A CN 109881189A CN 201910281041 A CN201910281041 A CN 201910281041A CN 109881189 A CN109881189 A CN 109881189A
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storage tank
plating
control valve
liquid
cylinder
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CN109881189B (en
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白瑞成
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Suzhou Nektes Textile New Materials Co Ltd
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Suzhou Nektes Textile New Materials Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
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    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

Abstract

The invention discloses a kind of preparation method of aromatic polyamide staple fiber that metallizes and stand-by provisions processed, the device is equipped with Porous Base in the plating cylinder of plating cylinder group and porous pressing plate constrains the fiber of tiling, fibre metal is carried out in conjunction with the mode that liquid circulation in storage tank acts on fiber in plating cylinder, it specifically includes tiling fiber, decontamination, pretreatment, reduction, the step of chemical plating and dehydration and drying, using device and method of the present invention by the way of the fixed liquid circulation of fiber, it is possible to prevente effectively from being intertwine with each other between aramid fiber short fibre, and different types of metallization aramid fiber short fibre can be prepared in batches.

Description

The preparation method for the aromatic polyamide staple fiber that metallizes and stand-by provision processed
Technical field
The present invention relates to a kind of preparation method of staple fiber and stand-by provision processed more particularly to a kind of fragrant adoptions of metallization The preparation method of amide staple fiber and stand-by provision processed belong to organic fiber metal lining technical field.
Background technique
Aromatic polyamide fibre abbreviation aramid fiber, English are Aramid fiber, are developed earliest by DuPont Corporation, are A kind of typical and most widely used high performance fibre material, has high-strength, Gao Mo, high temperature resistant, ingrain fireproofing and acid-fast alkali-proof Equal excellent properties, are widely used in the high science and technology field such as aerospace.Aramid fiber mainly has p-aramid fiber (poly- paraphenylene terephthalamide P-phenylenediamine, PPTA, Fanglun l414) and meta-aramid (poly, PMIA, aramid fiber 1313) two types Type, wherein PPTA have superelevation it is strong and modulus, be mainly used in Lightweight high-strength composite material reinforcing material and it is shellproof, The protective materials such as explosion-proof, anti-cutting;PMIA takes adaptive with good, is mainly used for high-performance individual protection field.Two class aramid fibers Molecular structure it is as follows:
Aramid fiber surface is metallized, so that obtaining one kind has both aramid fiber lightweight, high-strength, flexible and metal material Excellent electricity, magnetic property are always a hot research problem in the novel conductive fibrous material of one.Aramid fiber surface gold Categoryization, commonly used chemical plating process realize that comprehensive existing disclosed patented technology is also primarily present following ask at present Topic: (1) using the strong corrosives reagent such as the concentrated sulfuric acid and metalating reagent (NaH-DMSO), although can effectively realize to aramid fiber fibre The surface etch of dimension, but it is easy to cause the excessive loss of fibrous mechanical property;(2) complex technical process, some are also continuing to use chlorine Change the traditional handicraft of stannous and palladium chloride activation sensitization;(3) fiber is easy to intertwine with each other during plating, it is difficult to realize that batch is made It is standby.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation methods of aromatic polyamide staple fiber that metallizes And stand-by provision processed, in conjunction with herein described device and using herein described simple process and to the small no palladium of fibre damage Depositing process is learned, can effectively avoid the entanglement between fiber, and is able to achieve efficient, batch the production preparation metallization short fibre of aramid fiber Dimension.
The technical scheme is that
The invention discloses a kind of metallization aromatic polyamide staple fiber stand-by provision, which includes passing through pipeline The plating cylinder group and liquid storage groove group of tandem connection circulation, and plate the pipeline between cylinder group and liquid storage groove group and be equipped at least one A circulating pump, wherein
Plating cylinder group includes the plating cylinder of several tandems connection, and the bottom of each plating cylinder is positioned puts equipped with a tiling The Porous Base set, and the movable positioning in top for plating cylinder is equipped with the porous pressing plate that a tiling is placed, and plates Porous Base in cylinder The accommodating area for the fiber that tiles is formed between porous pressing plate;
Liquid storage groove group includes that several of parallel connection independently pass in and out the storage tank of liquid, which includes extremely A few decontamination liquid storage tank, at least one cleaning solution storage tank, at least one pretreatment fluid storage tank, at least one reducing solution storage tank and At least one metal plating liquid storage tank, wherein decontamination liquid storage tank is provided with decontamination liquid, and cleaning solution storage tank is provided with cleaning solution, pretreatment Liquid storage tank is provided with pretreatment fluid, and reducing solution storage tank is provided with reducing solution, and metal plating liquid storage tank is provided with metal plating liquid.
The further technical solution of the device is:
The bottom of the plating cylinder offers plating cylinder inlet, and the plating cylinder inlet passes through the hole and appearance on Porous Base Set area's connection;Offer plating cylinder liquid outlet at the top of the plating cylinder, and the plating cylinder liquid outlet by hole on porous pressing plate with Accommodating area connection;Positioning is equipped with stiff spring on the lower surface of the porous pressing plate, and the other end of the stiff spring is located by connecting In on the upper surface of Porous Base.
The plating cylinder liquid outlet of previous plating cylinder and the plating cylinder inlet of next plating cylinder are connected by pipeline in several described plating cylinders It is logical.
Positioning is equipped with a control valve respectively at the inlet and liquid outlet of each storage tank;And the pretreatment fluid Positioning is equipped with heating and heat-insulating device respectively on storage tank and metal plating liquid storage tank.
The invention also discloses it is a kind of using above-mentioned apparatus carry out metallization aromatic polyamide staple fiber preparation method, The preparation method includes the following steps:
S1: fleece-laying:, should using porous pressing plate by the short fine uniformly laying of aramid fiber after on the Porous Base in plating cylinder The short fibre of aramid fiber constrains in accommodating area, phenyl-diformyl between wherein the short fibre of aramid fiber is poly(p-phenylene terephthalamide) staple fiber and is poly- One of m-phenylene diamine (MPD) staple fiber;It is this that the short fine tiling of aramid fiber is placed on to the mode that subsequent processing is carried out on Porous Base, energy It is enough effectively to avoid intertwineing with each other between staple fiber, and it is suitable for large batch of industrial treatment.
S2: decontamination cleaning: opening the control valve of decontamination liquid storage tank while opening circulating pump, makes decontamination liquid full of plating cylinder And circulate carry out continue decontamination 20-40min after close decontamination liquid storage tank control valve, wherein gone in decontamination liquid storage tank Soiling solution is preferably acetone, can also using other can remove fiber surface dirt, finish and impurity, do not damage fiber surface, The organic solvent of water can be dissolved in.The control valve for opening cleaning solution storage tank makes cleaning solution full of plating cylinder using circulating pump and follows Circulation is dynamic continue the control valve that cleaning solution storage tank is closed after cleaning 5-15min, and wherein the preferred deionized water of cleaning solution, is used In the removal remaining decontamination liquid of fiber surface.
S3: pretreatment and cleaning: pretreatment fluid is heated to by the heating and heat-insulating device opened on pretreatment fluid storage tank in advance After set temperature, the control valve of pretreatment fluid storage tank is opened, makes pretreatment fluid full of plating cylinder using circulating pump and circulates Carry out continue pretreatment 1-2h after close pretreatment fluid storage tank control valve.Wherein pretreatment fluid is by silver nitrate, deionized water It is formed with polar solvent, silver nitrate content 10-50g/L, the volume content of polar solvent is 30-50vol.%, and surplus is to go Ionized water, and polar solvent be N-Methyl pyrrolidone, dimethyl acetamide, dimethyl sulfoxide and dimethylformamide at least One kind, temperature when which is pre-processed are 50-100 DEG C, i.e., the set temperature that pretreatment fluid is heated to is 50- 100℃.The essence of the preprocessing process is to be swollen fiber by organic solvent, then by the surface layer of silver ion implantation fiber It is interior, silver ion is completed in the fixation of fiber sheath.The control valve for opening cleaning solution storage tank, is full of cleaning solution using circulating pump Plating cylinder and circulating continue the control valve that cleaning solution storage tank is closed after cleaning 5-15min, and wherein cleaning solution is preferably gone Ionized water, for removing the remaining pretreatment fluid of fiber surface.
S4: reduction and cleaning: opening the control valve of reducing solution storage tank, makes reducing solution full of plating cylinder using circulating pump and follows The dynamic control valve for carrying out continued reduction and handling closing reducing solution storage tank after 30-90min of circulation;Wherein reducing solution is to silver ion The aqueous solution of compound with reduction, and having the compound of reduction to silver ion is glucose, potassium tartrate At least one of sodium, formaldehyde and boron hydride, wherein boron hydride can be at least one in potassium borohydride, sodium borohydride Kind;The concentration of the reducing solution is 5-40g/L, and the temperature in step S4 when reducing solution progress reduction treatment is room temperature.The reduction The essence of step is that using to anion there is the compound of reduction to be reduced into the anion in-situ for injecting fiber sheath Argent grain makes fiber surface form original in-situ silver layer.The control valve for opening cleaning solution storage tank, makes cleaning solution using circulating pump Continue cleaning after 5-15min the control valve for closing cleaning solution storage tank full of plating cylinder and circulating, wherein cleaning solution is excellent Deionized water is selected, for removing the remaining reducing solution of fiber surface.
S5: chemical plating and cleaning: metal plating liquid is heated to by the heating and heat-insulating device on preparatory opening metal plating solution storage tank After set temperature (set temperature is different according to different metal plating liquids, generally 20-60 DEG C), opening metal plating solution storage tank Control valve makes metal plating liquid be full of plating cylinder and circulate and carries out closing metal after continuing plating 30-60min using circulating pump The control valve of plating solution storage tank;Wherein metal plating liquid be to metallic silver have catalytic activity metal plating liquid, can be used silver plating liquid, Copper plating bath, nickel-plating liquid etc., can also use the composite plating bath of above-mentioned plating solution, and the metal layer that can specifically plate as needed is selected Select, the metal plating liquid be formed by the coat of metal be silver layer, layers of copper, nickel layer or in which at least two composite deposite.It opens clear The control valve of washing lotion storage tank carries out cleaning solution after continuing cleaning 5-15min full of plating cylinder and circulating using circulating pump The control valve of cleaning solution storage tank is closed, wherein the preferred deionized water of cleaning solution, for removing the remaining metal-plated of fiber surface Liquid.
S6: dehydration and drying: it will carry out centrifugal dehydration and dry to obtain metallization aromatic polyamide after the short fine taking-up of aramid fiber Staple fiber.
The method have the benefit that: herein described device and preparation method are used, (1) eliminates traditional fibre Dimension roughening and activation-sensitization technical process, and avoid the use of stannous chloride and palladium chloride;(2) it is uniform, fine that coating can be obtained Dimension mechanical property damages metallization aramid fiber short fibre small, that coating binding strength is high;(3) it is possible to prevente effectively from aramid fiber short fibre it Between intertwine with each other, and may be implemented it is different types of metallization aramid fiber short fibre batch preparation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of stand-by provision processed of the present invention;
Fig. 2 is that the specific embodiment of the invention 3 prepares resulting silver-plated aramid fiber 1313 staple fiber finished figure;
Wherein:
100- plates cylinder group;101- plates cylinder;102- Porous Base;The porous pressing plate of 103-;The accommodating area 104-;105- plates cylinder feed liquor Mouthful;106- plates cylinder liquid outlet;
200- liquid storage groove group;201- decontamination liquid storage tank;202- cleaning solution storage tank;203- pretreatment fluid storage tank;204- is also Stoste storage tank;205- metal plating liquid storage tank;206- control valve;
300- circulating pump.
Specific embodiment
In order to better understand the technical means of the present invention, it and can be implemented in accordance with the contents of the specification, below In conjunction with the accompanying drawings and embodiments, specific embodiments of the present invention will be described in further detail, and following embodiment is for illustrating this Invention, but be not intended to limit the scope of the invention.
1 pair of metallization aromatic polyamide staple fiber stand-by provision described herein carries out detailed with reference to the accompanying drawing Thin description.Device described herein includes the plating cylinder group 100 and liquid storage groove group 200 recycled by the connection of pipeline tandem, Pipeline between the plating cylinder group and liquid storage groove group is equipped at least one circulating pump 300.
Plating cylinder group 100 includes the plating cylinder 101 that several are connected to by pipeline tandem, and the bottom of each plating cylinder 101 is opened Top equipped with a plating cylinder inlet 105, and each plating cylinder 101 offers a plating cylinder liquid outlet 106.The quantity for plating cylinder can be with The amount of the short fibre handled according to every batch of is configured, at least provided with a plating cylinder, when being provided at least two platings The plating cylinder inlet 105 of the plating cylinder liquid outlet 106 of previous plating cylinder and next plating cylinder forms multiple plating cylinders by pipeline connection when cylinder Concatenated form.Since the amount of the short fibre handled is not very big, only one plating of setting in this specific embodiment Cylinder.The bottom of each plating cylinder 101, which positions, in plating cylinder group 100 is equipped with the Porous Base 102 that a tiling is placed, the porous bottom Plate be set to plating cylinder in bottom be located at plating cylinder inlet above at, size and shape be able to make the side edge of Porous Base against On the plating inside wall of cylinder, convenient for the fiber being chopped that tiles on it.It is equally distributed that several are offered on the Porous Base 102 Through-hole plates cylinder inlet and is connected to by the through-hole with accommodating area, mainly makes the liquid flowed into from plating cylinder inlet slowly and equal The even short fibre by the bottom-up infiltration tiling of the through-hole thereon.The positioning method of Porous Base can be used in plating cylinder inner circumferential side Boss is set on wall, Porous Base is held on the mode on boss, claw can also be set on plating cylinder inner circumferential side wall, more Setting card slot in claw position is corresponded on the bottom plate of hole, positions Porous Base using the cooperation of claw and card slot, these positioning methods are This field conventional techniques repeat no more in the application.Plate the movable positioning in top of each plating cylinder 101 in cylinder group 100 Porous pressing plate 103 equipped with a tile mode, the porous pressing plate are set to plating cylinder inner top and are located at the lower section of plating cylinder liquid outlet, Its size and shape is also that the side edge of porous pressing plate be able to be made to be resisted against on the plating inside wall of cylinder.It is equally opened up on porous pressing plate 103 There are several equally distributed through-holes, plating cylinder liquid outlet is connected to by the through-hole with accommodating area, mainly makes to flow out from accommodating area Liquid slowly and uniformly by the through-hole is bottom-up collect after from plating cylinder liquid outlet outflow.The following table of porous pressing plate 103 Positioning is equipped with stiff spring on face, and the other end of the stiff spring is located by connecting on the upper surface of Porous Base, the traction bullet The main function of spring is the restoring force downward using spring, and porous pressing plate is made to have downward pulling force.Plate Porous Base in cylinder 101 The accommodating area 104 for the fiber that tiles is formed between porous pressing plate.When in use, porous pressing plate is pulled open, by what is be chopped Fiber is laid on Porous Base, then decontrols porous pressing plate, and using the restoring force that stiff spring is downward, porous pressing plate is pressed in On tiled short fibre, make short fibre is regular to be constrained in the accommodating area plated in cylinder, is not susceptible to the feelings of short fine chaotic winding Condition.
Liquid storage groove group 200 include parallel connection several independently pass in and out the storage tank of liquid, the feed liquor of each storage tank Positioning is equipped with a control valve 206 respectively at mouth and liquid outlet, which is mainly the corresponding storage tank liquid of control Outflow and inflow can also work as use using the electric control valve for having model on the market using conventional machinery valve When electric control valve, all control valves connect and are controlled by it with the numer centre component that can control the valve opening and closing. Several above-mentioned storage tanks include at least one decontamination liquid storage tank 201, at least one cleaning solution storage tank 202, at least one pre- place Liquid storage tank 203, at least one reducing solution storage tank 204 and at least one metal plating liquid storage tank 205 are managed, wherein decontamination liquid storage tank is built-in There is decontamination liquid, cleaning solution storage tank is provided with cleaning solution, and pretreatment fluid storage tank is provided with pretreatment fluid, and reducing solution storage tank is provided with also Stoste, metal plating liquid storage tank are provided with metal plating liquid, furthermore to enable the liquid in storage tank preferably to play a role, above-mentioned pre- Positioning is equipped with heating and heat-insulating device respectively on treatment fluid storage tank 203 and metal plating liquid storage tank 205, to in corresponding storage tank Liquid is heated and is kept the temperature, which can be the conventional setting collet outside storage tank and in collet Nei Tongre The mode of fluid, is also possible to winding heating wire etc. outside storage tank, which is this field conventional techniques, in the application It repeats no more.
The main function of circulating pump 300 is and will to plate cylinder in the plating cylinder of the liquid pump in each storage tank to plating cylinder group Interior liquid is pumped back in each storage tank.It the setting position of circulating pump can be in the liquid outlet of liquid storage groove group and the feed liquor of plating cylinder group On pipeline between mouthful, it can also be arranged on the pipeline between the liquid outlet of plating cylinder group and the inlet of liquid storage groove group, or Circulating pump is equipped at above-mentioned two.The setting quantity of the circulating pump can be transported according to the length, the pumpability of pump, liquid of pipeline The amount of sending etc. is selected.
It mainly include following steps when carrying out the preparation of metallization aromatic polyamide staple fiber using herein described device It is rapid:
S1: fleece-laying:, should using porous pressing plate by the short fine uniformly laying of aramid fiber after on the Porous Base in plating cylinder The short fibre of aramid fiber constrains in accommodating area, phenyl-diformyl between wherein the short fibre of aramid fiber is poly(p-phenylene terephthalamide) staple fiber and is poly- One of m-phenylene diamine (MPD) staple fiber;It is this that the short fine tiling of aramid fiber is placed on to the mode that subsequent processing is carried out on Porous Base, energy It is enough effectively to avoid intertwineing with each other between staple fiber, and it is suitable for large batch of industrial treatment.
S2: decontamination cleaning: opening the control valve of decontamination liquid storage tank while opening circulating pump, makes decontamination liquid full of plating cylinder And circulate carry out continue decontamination 20-40min after close decontamination liquid storage tank control valve, wherein gone in decontamination liquid storage tank Soiling solution is preferably acetone, can also using other can remove fiber surface dirt, finish and impurity, do not damage fiber surface, The organic solvent of water can be dissolved in.The control valve for opening cleaning solution storage tank makes cleaning solution full of plating cylinder using circulating pump and follows Circulation is dynamic continue the control valve that cleaning solution storage tank is closed after cleaning 5-15min, and wherein the preferred deionized water of cleaning solution, is used In the removal remaining decontamination liquid of fiber surface.
S3: pretreatment and cleaning: pretreatment fluid is heated to by the heating and heat-insulating device opened on pretreatment fluid storage tank in advance After set temperature, the control valve of pretreatment fluid storage tank is opened, makes pretreatment fluid full of plating cylinder using circulating pump and circulates Carry out continue pretreatment 1-2h after close pretreatment fluid storage tank control valve.Wherein pretreatment fluid is by silver nitrate, deionized water It is formed with polar solvent, silver nitrate content 10-50g/L, the volume content of polar solvent is 30-50vol.%, and surplus is to go Ionized water, and polar solvent be N-Methyl pyrrolidone, dimethyl acetamide, dimethyl sulfoxide and dimethylformamide at least One kind, temperature when which is pre-processed are 50-100 DEG C, i.e., the set temperature that pretreatment fluid is heated to is 50- 100℃.The essence of the preprocessing process is to be swollen fiber by organic solvent, then by the surface layer of silver ion implantation fiber It is interior, silver ion is completed in the fixation of fiber sheath.The control valve for opening cleaning solution storage tank, is full of cleaning solution using circulating pump Plating cylinder and circulating continue the control valve that cleaning solution storage tank is closed after cleaning 5-15min, and wherein cleaning solution is preferably gone Ionized water, for removing the remaining pretreatment fluid of fiber surface.
S4: reduction and cleaning: opening the control valve of reducing solution storage tank, makes reducing solution full of plating cylinder using circulating pump and follows The dynamic control valve for carrying out continued reduction and handling closing reducing solution storage tank after 30-90min of circulation;Wherein reducing solution is to silver ion The aqueous solution of compound with reduction, and having the compound of reduction to silver ion is glucose, potassium tartrate At least one of sodium, formaldehyde and boron hydride, wherein boron hydride can be at least one in potassium borohydride, sodium borohydride Kind;The concentration of the reducing solution is 5-40g/L, and the temperature in step S4 when reducing solution progress reduction treatment is room temperature.The reduction The essence of step is that using to anion there is the compound of reduction to be reduced into the anion in-situ for injecting fiber sheath Argent grain makes fiber surface form original in-situ silver layer.The control valve for opening cleaning solution storage tank, makes cleaning solution using circulating pump Continue cleaning after 5-15min the control valve for closing cleaning solution storage tank full of plating cylinder and circulating, wherein cleaning solution is excellent Deionized water is selected, for removing the remaining reducing solution of fiber surface.
S5: chemical plating and cleaning: metal plating liquid is heated to by the heating and heat-insulating device on preparatory opening metal plating solution storage tank After set temperature (set temperature is different according to different metal plating liquids, generally 20-60 DEG C), opening metal plating solution storage tank Control valve makes metal plating liquid be full of plating cylinder and circulate and carries out closing metal after continuing plating 30-60min using circulating pump The control valve of plating solution storage tank;Wherein metal plating liquid be to metallic silver have catalytic activity metal plating liquid, can be used silver plating liquid, Copper plating bath, nickel-plating liquid etc., can also use the composite plating bath of above-mentioned plating solution, and the metal layer that can specifically plate as needed is selected Select, the metal plating liquid be formed by the coat of metal be silver layer, layers of copper, nickel layer or in which at least two composite deposite.It opens clear The control valve of washing lotion storage tank carries out cleaning solution after continuing cleaning 5-15min full of plating cylinder and circulating using circulating pump The control valve of cleaning solution storage tank is closed, wherein the preferred deionized water of cleaning solution, for removing the remaining metal-plated of fiber surface Liquid.
S6: dehydration and drying: it will carry out centrifugal dehydration and dry to obtain metallization aromatic polyamide after the short fine taking-up of aramid fiber Staple fiber.
Illustrate herein described preparation method with specific preparation embodiment below to prepare metallization aromatic series polyamides Amine staple fiber.
Specific embodiment 1
S1: fleece-laying: the short fine uniformly laying of 500g aramid fiber 1313 is weighed after on the Porous Base in plating cylinder, using more Hole pressing plate constrains in the aramid fiber short fibre in accommodating area;
S2: decontamination cleaning: the control valve of decontamination liquid storage tank is opened while opening circulating pump, is made in decontamination liquid storage tank Acetone continue full of plating cylinder and circulating the control valve that decontamination liquid storage tank is closed after decontamination 30min;It is then turned on clear The control valve of washing lotion storage tank makes deionized water therein be full of plating cylinder and circulate and carries out continuing cleaning using circulating pump The control valve of cleaning solution storage tank is closed after 10min;
S3: pretreatment and cleaning: pretreatment fluid is heated to by the heating and heat-insulating device opened on pretreatment fluid storage tank in advance After 90 DEG C, the control valve of pretreatment fluid storage tank is opened, makes pretreatment fluid full of plating cylinder using circulating pump and circulates progress The control valve of pretreatment fluid storage tank is persistently closed after pretreatment 1.5h;It is then turned on the control valve of cleaning solution storage tank, is utilized Circulating pump makes deionized water continue full of plating cylinder and circulating the control valve for closing cleaning solution storage tank after cleaning 10min Door;Wherein pretreatment fluid is made of the deionized water of 30g/L silver nitrate, the dimethyl sulfoxide of 40vol.% and surplus;
S4: reduction and cleaning: opening the control valve of reducing solution storage tank, makes reducing solution full of plating cylinder using circulating pump and follows The dynamic control valve for carrying out continued reduction and handling closing reducing solution storage tank after 60min of circulation;Open the control valve of cleaning solution storage tank Door makes deionized water be full of plating cylinder and circulate and continue closing cleaning solution storage tank after cleaning 10min using circulating pump Control valve;Wherein reducing solution is the sodium borohydride aqueous solution of 15g/L, and the use temperature of reducing solution is room temperature;
S5: chemical plating and cleaning: metal plating liquid is heated to by the heating and heat-insulating device on preparatory opening metal plating solution storage tank After 45 DEG C, the control valve of opening metal plating solution storage tank makes metal plating liquid full of plating cylinder using circulating pump and circulates progress The control valve of metal plating liquid storage tank is closed after lasting plating 40min;It is then turned on the control valve of cleaning solution storage tank, using following Ring pump makes deionized water continue full of plating cylinder and circulating the control valve for closing cleaning solution storage tank after cleaning 10min. Wherein metal plating liquid is nickel-plating liquid, is hydrated by 33g/L two citric acid monohydrate trisodiums, 20g/L six hydration nickel sulfate, 15g/L mono- Sodium hypophosphite and 3g/L dimethylamino borine composition, and adjusting pH with ammonium hydroxide is 10;
S6: dehydration and drying: it will carry out centrifugal dehydration and dry to obtain nickel plating aramid fiber 1313 staple fiber after the short fine taking-up of aramid fiber.
Specific embodiment 2
S1: fleece-laying: the short fine uniformly laying of 500g Fanglun l414 is weighed after on the Porous Base in plating cylinder, using more Hole pressing plate constrains in the aramid fiber short fibre in accommodating area;
S2: decontamination cleaning: the control valve of decontamination liquid storage tank is opened while opening circulating pump, is made in decontamination liquid storage tank Acetone continue full of plating cylinder and circulating the control valve that decontamination liquid storage tank is closed after decontamination 30min;It is then turned on clear The control valve of washing lotion storage tank makes deionized water therein be full of plating cylinder and circulate and carries out continuing cleaning using circulating pump The control valve of cleaning solution storage tank is closed after 10min;
S3: pretreatment and cleaning: pretreatment fluid is heated to by the heating and heat-insulating device opened on pretreatment fluid storage tank in advance After 95 DEG C, the control valve of pretreatment fluid storage tank is opened, makes pretreatment fluid full of plating cylinder using circulating pump and circulates progress The control valve of pretreatment fluid storage tank is persistently closed after pretreatment 1.5h;It is then turned on the control valve of cleaning solution storage tank, is utilized Circulating pump makes deionized water continue full of plating cylinder and circulating the control valve for closing cleaning solution storage tank after cleaning 10min Door;Wherein pretreatment fluid is made of the deionized water of 40g/L silver nitrate, the N-Methyl pyrrolidone of 50vol.% and surplus;
S4: reduction and cleaning: opening the control valve of reducing solution storage tank, makes reducing solution full of plating cylinder using circulating pump and follows The dynamic control valve for carrying out continued reduction and handling closing reducing solution storage tank after 60min of circulation;Open the control valve of cleaning solution storage tank Door makes deionized water be full of plating cylinder and circulate and continue closing cleaning solution storage tank after cleaning 10min using circulating pump Control valve;Wherein reducing solution is the formalin of 30wt.%, and the use temperature of reducing solution is room temperature;
S5: chemical plating and cleaning: metal plating liquid is heated to by the heating and heat-insulating device on preparatory opening metal plating solution storage tank After 55 DEG C, the control valve of opening metal plating solution storage tank makes metal plating liquid full of plating cylinder using circulating pump and circulates progress The control valve of metal plating liquid storage tank is closed after lasting plating 50min;It is then turned on the control valve of cleaning solution storage tank, using following Ring pump makes deionized water continue full of plating cylinder and circulating the control valve for closing cleaning solution storage tank after cleaning 10min. Wherein metal plating liquid is copper plating bath, by 20g/L disodium ethylene diamine tetraacetate, 5g/L cupric sulfate pentahydrate, 35ml/L triethanolamine It is formed with 5g/L dimethylamino borine, and adjusting pH with sodium hydroxide is 8.5;
S6: dehydration and drying: it will carry out centrifugal dehydration and dry to obtain copper facing Fanglun l414 staple fiber after the short fine taking-up of aramid fiber.
Specific embodiment 3
S1: fleece-laying: the short fine uniformly laying of 500g aramid fiber 1313 is weighed after on the Porous Base in plating cylinder, using more Hole pressing plate constrains in the aramid fiber short fibre in accommodating area;
S2: decontamination cleaning: the control valve of decontamination liquid storage tank is opened while opening circulating pump, is made in decontamination liquid storage tank Acetone continue full of plating cylinder and circulating the control valve that decontamination liquid storage tank is closed after decontamination 30min;It is then turned on clear The control valve of washing lotion storage tank makes deionized water therein be full of plating cylinder and circulate and carries out continuing cleaning using circulating pump The control valve of cleaning solution storage tank is closed after 10min;
S3: pretreatment and cleaning: pretreatment fluid is heated to by the heating and heat-insulating device opened on pretreatment fluid storage tank in advance After 90 DEG C, the control valve of pretreatment fluid storage tank is opened, makes pretreatment fluid full of plating cylinder using circulating pump and circulates progress The control valve of pretreatment fluid storage tank is persistently closed after pretreatment 1.5h;It is then turned on the control valve of cleaning solution storage tank, is utilized Circulating pump makes deionized water continue full of plating cylinder and circulating the control valve for closing cleaning solution storage tank after cleaning 10min Door;Wherein pretreatment fluid is made of the deionized water of 30g/L silver nitrate, the dimethyl acetamide of 40vol.% and surplus;
S4: reduction and cleaning: opening the control valve of reducing solution storage tank, makes reducing solution full of plating cylinder using circulating pump and follows The dynamic control valve for carrying out continued reduction and handling closing reducing solution storage tank after 60min of circulation;Open the control valve of cleaning solution storage tank Door makes deionized water be full of plating cylinder and circulate and continue closing cleaning solution storage tank after cleaning 10min using circulating pump Control valve;Wherein reducing solution is the mixed aqueous solution being made of the glucose of 6g/L and the sodium potassium tartrate tetrahydrate of 2g/L, and is restored The use temperature of liquid is room temperature;
S5: chemical plating and cleaning: the control valve of opening metal plating solution storage tank makes metal plating liquid full of plating using circulating pump Cylinder and circulating carries out continuing at room temperature the control valve that metal plating liquid storage tank is closed after plating 60min;It is then turned on clear The control valve of washing lotion storage tank carries out deionized water after continuing cleaning 10min full of plating cylinder and circulating using circulating pump Close the control valve of cleaning solution storage tank.Wherein metal plating liquid is made of plating solution main salt solution and reducing solution two parts, plating solution master The composition of salting liquid are as follows: 10g/L silver nitrate, 60ml/L ammonium hydroxide, 20ml/L ethylenediamine and 6g/L potassium hydroxide;The composition of reducing solution Are as follows: 8g/L glucose, 2.5g/L sodium potassium tartrate tetrahydrate and 40ml/L ethyl alcohol need to mix plating solution main salt solution and reducing solution before use Uniformly;
S6: dehydration and drying: it will carry out centrifugal dehydration and dry to obtain silver-plated aramid fiber 1313 staple fiber after the short fine taking-up of aramid fiber.
The above-mentioned properties for preparing resulting plating metal aramid fiber short fibre are tested, test result is referring in table 1 It is described, in which: (1) that the strength of fiber is measured according to " GB/T14337-2008 man-made staple fibres Erichsen test method " Single wire fracture strength;(2) resistance is the DC resistance (Ω/cm) of the unit length measured with multimeter;(3) coating combines Performance is characterized with the DC resistance change before and after ultrasonic treatment (40Hz, 150W, 60min).
The performance of metallization aramid fiber obtained by table 1 (substrate is 220dtex aramid fiber 1313 and 1414)
The above is only a preferred embodiment of the present invention, it is not intended to restrict the invention, it is noted that for this skill For the those of ordinary skill in art field, without departing from the technical principles of the invention, can also make it is several improvement and Modification, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (10)

1. a kind of metallization aromatic polyamide staple fiber stand-by provision, which is characterized in that including being connected by pipeline tandem The plating cylinder group (100) and liquid storage groove group (200) of logical circulation, and plate the pipeline between cylinder group and liquid storage groove group and be equipped at least One circulating pump (300), wherein
Plating cylinder group includes the plating cylinder (101) of several tandems connection, and the bottom of each plating cylinder, which positions, is equipped with a tiling The Porous Base (102) of placement, and the movable positioning in top for plating cylinder is equipped with the porous pressing plate (103) that a tiling is placed, plating The accommodating area (104) for the fiber that tiles is formed in cylinder between Porous Base and porous pressing plate;
Liquid storage groove group includes that several of parallel connection independently pass in and out the storage tank of liquid, which includes at least one A decontamination liquid storage tank (201), at least one cleaning solution storage tank (202), at least one pretreatment fluid storage tank (203), at least one Reducing solution storage tank (204) and at least one metal plating liquid storage tank (205), wherein decontamination liquid storage tank is provided with decontamination liquid, cleaning solution Storage tank is provided with cleaning solution, and pretreatment fluid storage tank is provided with pretreatment fluid, and reducing solution storage tank is provided with reducing solution, metal plating liquid storage Slot is provided with metal plating liquid.
2. the apparatus according to claim 1, which is characterized in that the bottom of plating cylinder (101) offers plating cylinder inlet (105), and the plating cylinder inlet is connected to by the hole on Porous Base (102) with accommodating area;The top of plating cylinder (101) Plating cylinder liquid outlet (106) is offered, and the plating cylinder liquid outlet is connected to by the hole on porous pressing plate (103) with accommodating area;Institute It states positioning on the lower surface of porous pressing plate (103) and is equipped with stiff spring, the other end of the stiff spring is located by connecting in porous bottom On the upper surface of plate.
3. the apparatus according to claim 1, it is characterised in that: the plating cylinder of previous plating cylinder in several described platings cylinder (101) The plating cylinder inlet of liquid outlet and next plating cylinder passes through pipeline connection.
4. the apparatus according to claim 1, which is characterized in that distinguish at the inlet and liquid outlet of each storage tank Positioning is equipped with a control valve (206);And it is fixed respectively on the pretreatment fluid storage tank (203) and metal plating liquid storage tank (205) Position is equipped with heating and heat-insulating device.
5. a kind of preparation method that metallization aromatic polyamide staple fiber is carried out using device described in Claims 1-4 4, It is characterized in that, includes the following steps:
S1: fleece-laying: by the short fine uniformly laying of aramid fiber after on the Porous Base in plating cylinder, using porous pressing plate by the aramid fiber Short fibre constrains in accommodating area;
S2: decontamination cleaning: the control valve of decontamination liquid storage tank is opened while opening circulating pump, makes decontamination liquid full of plating cylinder and follows Circulation is dynamic continue the control valve that decontamination liquid storage tank is closed after decontamination 20-40min;Open the control valve of cleaning solution storage tank Door makes cleaning solution be full of plating cylinder and circulate and continue closing cleaning solution storage tank after cleaning 5-15min using circulating pump Control valve;
S3: pretreatment and cleaning: pretreatment fluid is heated to setting by the heating and heat-insulating device opened on pretreatment fluid storage tank in advance After temperature, the control valve of pretreatment fluid storage tank is opened, makes pretreatment fluid full of plating cylinder using circulating pump and circulates progress The control valve of pretreatment fluid storage tank is persistently closed after pretreatment 1-2h;The control valve for opening cleaning solution storage tank, utilizes circulation Pump makes cleaning solution continue full of plating cylinder and circulating the control valve for closing cleaning solution storage tank after cleaning 5-15min;
S4: reduction and cleaning: opening the control valve of reducing solution storage tank, makes reducing solution full of plating cylinder and recycle stream using circulating pump The dynamic control valve for carrying out continued reduction and handling closing reducing solution storage tank after 30-90min;Open the control valve of cleaning solution storage tank Door makes cleaning solution be full of plating cylinder and circulate and continue closing cleaning solution storage tank after cleaning 5-15min using circulating pump Control valve;
S5: chemical plating and cleaning: metal plating liquid is heated to setting by the heating and heat-insulating device on preparatory opening metal plating solution storage tank After temperature, the control valve of opening metal plating solution storage tank makes metal plating liquid full of plating cylinder using circulating pump and circulates progress The control valve of metal plating liquid storage tank is closed after lasting plating 30-60min;The control valve for opening cleaning solution storage tank, using following Ring pump makes cleaning solution continue full of plating cylinder and circulating the control valve for closing cleaning solution storage tank after cleaning 5-15min;
S6: dehydration and drying: it will carry out centrifugal dehydration and dry to obtain the metallization short fibre of aromatic polyamide after the short fine taking-up of aramid fiber Dimension.
6. preparation method according to claim 5, which is characterized in that aramid fiber described in step S1 is short fine for poly- terephthaldehyde One of acyl p-phenylenediamine staple fiber and poly staple fiber;It is gone in decontamination liquid storage tank in step S2 Soiling solution is acetone;Cleaning solution of the step S2 into S5 in cleaning solution storage tank is deionized water.
7. preparation method according to claim 5, which is characterized in that the pre- place in step S3 in pretreatment fluid storage tank Reason liquid is made of silver nitrate, deionized water and polar solvent, and wherein silver nitrate content is 10-50g/L, and the volume of polar solvent contains Amount is 30-50vol.%, and surplus is deionized water, and polar solvent is N-Methyl pyrrolidone, dimethyl acetamide, diformazan Asia At least one of sulfone and dimethylformamide;And temperature when pretreatment fluid is pre-processed in step S3 is 50-100 DEG C.
8. preparation method according to claim 5, which is characterized in that the reducing solution in step S4 in reducing solution storage tank To have the aqueous solution of the compound of reduction to silver ion, the concentration of the reducing solution is 5-40g/L, and is restored in step S4 Temperature when liquid carries out reduction treatment is room temperature.
9. preparation method according to claim 8, which is characterized in that the compound to silver ion with reduction For at least one of glucose, sodium potassium tartrate tetrahydrate, formaldehyde and boron hydride.
10. preparation method according to claim 5, which is characterized in that the metal-plated in step S5 in metal plating liquid storage tank Liquid is the metal plating liquid for having catalytic activity to metallic silver, and it is silver layer, layers of copper, nickel layer which, which is formed by the coat of metal, Or in which at least two composite deposite.
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CN112026272A (en) * 2020-08-17 2020-12-04 浙江工业大学 Novel wave-absorbing material with honeycomb structure and preparation method thereof

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CN106498715A (en) * 2016-10-12 2017-03-15 上海大学 A kind of aromatic polyamide conductive fibers preparation method of the coat of metal
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
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JP2006002213A (en) * 2004-06-17 2006-01-05 Nagoya Plating Co Ltd Electroless silver plating for aramid fiber material
CN104651812A (en) * 2013-11-13 2015-05-27 矢崎总业株式会社 Plating Device
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CN106498715A (en) * 2016-10-12 2017-03-15 上海大学 A kind of aromatic polyamide conductive fibers preparation method of the coat of metal
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CN112026272A (en) * 2020-08-17 2020-12-04 浙江工业大学 Novel wave-absorbing material with honeycomb structure and preparation method thereof

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