CN105133301A - Preparation method of nickel plated aromatic polyarmide fiber - Google Patents
Preparation method of nickel plated aromatic polyarmide fiber Download PDFInfo
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- CN105133301A CN105133301A CN201510568766.4A CN201510568766A CN105133301A CN 105133301 A CN105133301 A CN 105133301A CN 201510568766 A CN201510568766 A CN 201510568766A CN 105133301 A CN105133301 A CN 105133301A
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Abstract
The invention relates to a preparation method of nickel plated aromatic polyarmide fiber. The method concretely comprises the following steps of (a) performing washing and deoiling; (b) using preprocessing reagents for performing preprocessing on the surface of the fiber so that the fiber realizes dissolution and expansion; absorbing a layer of metal ions with catalytic activity after the reduction on the surface; increasing the fiber surface area and improving the wetting performance; (c) performing reduction; (d) performing chemical nickel plating. The nickel plated aromatic polyarmide fiber prepared by the invention has the characteristics of excellent conduction performance, heat resistance, flame resistance, light weight, high intensity and the like; in addition, a nickel plating layer has good wear-resistant performance and anti-corrosion performance. The nickel plated fiber can be used for preparing anti-static and electromagnetic shielding fabrics and shielding layers and conductor materials of special cables. Thereby the nickel plated fiber can be widely applied to special departments such as aviation, space flight, war industry, communication, and can also meet the individual protection requirements of work personnel engaged in radar, medical care, television relay broadcasting and the like.
Description
Technical field
The invention provides a kind of preparation method of nickel plating aromatic polyamide fibre.This technique by chemical plating method at aromatic polyamide fibre surface metallization electrically conductive layer, thus give resistant fiber electrostatic and conducting function, remain the high-strength light of fiber, heat-proof combustion-resistant, the inherent characteristic such as soft is a kind of advanced composite material (ACM) simultaneously.The specials such as Aeronautics and Astronautics, navigation, military project, medical treatment can be widely used in, as electromagnetic shielding material and the lightweight conductive material of individual protection.
Background technology
Aromatic polyamide fibre is called for short aramid fiber, English is Aramidfiber, is developed at first by du pont company, is a kind of novel high-tech synthetic fiber, there is superhigh intensity, high-modulus and high temperature resistant, acid-fast alkali-proof, the premium properties such as lightweight, its intensity is 5 ~ 6 times of steel wire, and modulus is 2 ~ 3 times of steel wire or glass fibre, and toughness is 2 times of steel wire, and weight is only about 1/5 of steel wire, at the temperature of 560 degree, do not decompose, non-fusible.It has good insulating properties and ageing resistace, has very long life cycle.Aramid fiber and composite thereof have been widely used in Aero-Space and military use, as the housing of the aircrafts such as Boeing 757,767, bulletproof jacket, bullet-proof vest, the helmet, space flight compression garments, high strength parachute, missile case material, extraordinary cable, storepipe, space shuttle energy storage tank and other high-pressure bottles etc.The discovery of aramid fiber, is considered to material circle very important historical progress, is therefore called as " fiber of dream ".
But aramid fiber is the same with other macromolecular material, its good electrical insulating property and dielectric properties, limit the application of aramid fiber in some fields.At present, the method for giving aramid fiber electric conductivity mainly contains the methods such as magnetron sputtering, co-blended spinning, chemical plating.Patent CN103668944A teaches a kind of preparation method of aramid fiber Conductive Silver-Coated PET Fibers, but adopt method of roughening to destroy the epidermal structure of fiber in its preparation process, damage the mechanical property of fiber, and the adhesion of the coating deposited and fiber is poor, easily come off, and the stability of coating is very poor, oxidizable, electric conductivity can prolongation in time and declining.
Current state inner conductive fiber is mainly with terylene, and nylon, cotton fiber etc. are substrate.Be that the conductive fiber of substrate rarely has report with aramid fiber, and there is a lot of defect, the adhesion of coating and fibrous matrix is very poor, not yet has the industrialization product of excellent performance to emerge.External Jin You du pont company grasps the core technology of producing this series products.
This patent adopts chemical plating method to prepare nickel plating conduction aramid fiber, and nickel plating conduction aramid fiber as shown in Figure 1.With domestic existing about conduct electricity aramid fiber report compared with, the method that this patent adopts is not only simple to operate in technique, economical, and the adhesion of the coating and the fibrous matrix that obtain is by force, and the stable in properties of coating, ABRASION RESISTANCE, corrosion resistance are good.Prepared nickel plating conduction aramid fiber electric conductivity is excellent, has broad application prospects in electromagnetic shielding field.
Summary of the invention
One of the object of the invention is to provide a kind of nickel plating aromatic polyamide fibre.
Two of the object of the invention is to provide a kind of preparation method of nickel plating aromatic polyamide fibre.
The present invention passes through first to carry out cleaning oil removal treatment to matrix fiber (aromatic polyamide fibre), the finish that removing fiber adsorbs in process and surface smut; After oil removing, preliminary treatment is carried out to fiber surface, make fiber swelling, increased fiber surface area and wettability, and after the reduction of adsorption one deck, there is the metal ion of catalytic activity, improve the binding strength of fibrous matrix and subsequent plating layer; Flooded by the solution that reductant put into by pretreated fiber, make the metal ion being adsorbed on fiber surface be reduced into metallic particles, this metal particle layer as the anchor point between fiber and subsequent plating layer, can also have the function of catalysis simultaneously; Then at the chemical nickel plating on surface of fiber, a kind of nickel plating aromatic polyamide conductive fibers is finally obtained.
The preparation method of a kind of nickel plating aromatic polyamide fibre of the present invention, is characterized in that having following process and step:
A. washing and oil removing: aromatic polyamide fibre is put into acetone, takes out after Ultrasonic Cleaning 40 ~ 80min, use deionized water rinsed clean;
B. preliminary treatment, puts into pretreatment fluid by the fiber after oil removing, and in pretreatment fluid, the concentration of salt is 5 ~ 50g/L treatment temperature is at 30 ~ 100 DEG C, takes out, use deionized water rinsed clean after dipping 1 ~ 4h;
C. reduce: pretreated fiber is put into 5 ~ 25g/L borane reducing agent sodium hydride aqueous solution or the potassium borohydride aqueous solution floods, at 20 ~ 50 DEG C, take out after dipping 20 ~ 60min;
D. chemical nickel plating:
Nickel-plating liquid with following material and water formulated, in reactant liquor, the content of each material is:
Nickelous sulfate 15 ~ 40g/L
Inferior sodium phosphate (reductant) 10 ~ 20g/L
Dimethylamino borine (reductant) 3 ~ 10g/L
Natrium citricum (complexing agent) 20 ~ 30g/L
Ammoniacal liquor (PH conditioning agent) 5 ~ 15ml/L
Aramid fiber after reduction is immersed in nickel-plating liquid, at 40 ~ 80 DEG C, takes out after reaction 0.5 ~ 1h, use deionized water rinsed clean, be placed in the dry 30min of drying box, obtain the aromatic polyamide fibre that surface uniform plating has nickel, namely conduct electricity aramid fiber.
Accompanying drawing explanation
Fig. 1 is the SEM figure of nickel plating aromatic polyamide fibre of the present invention.
Detailed description of the invention
after now embodiments of the invention being described in.
embodiment 1
detailed process and the step of the present embodiment are as described below:
(1) oil removing: Fanglun 1414 (PPTA) is put into acetone soln, takes out after Ultrasonic Cleaning 60min, use deionized water rinsed clean.
(2) preliminary treatment: immersed in the aqueous solution containing the methyl-sulfoxide of 5g/L cobaltous sulfate by fiber, wherein the volumetric concentration of methyl-sulfoxide is take out after soaking 1h at 30%, 50 DEG C.
(3) reduce: pretreated fiber is put into 15g/L sodium borohydride solution and carries out reduction treatment, temperature is 20 DEG C, takes out after 60min.
(4) chemical nickel plating: the fiber after reduction is put into nickel plating solution, and chemical nickel-plating liquid consists of: nickelous sulfate 40g/L, inferior sodium phosphate 10g/L, dimethylamino borine 10g/L, natrium citricum 30g/L, ammoniacal liquor 15ml/L, bath temperature is 40 DEG C, plating time 0.5h.
embodiment 2
detailed process and the step of the present embodiment are as described below:
(1) oil removing: Fanglun 1414 (PPTA) is put into acetone soln, takes out after Ultrasonic Cleaning 40min, use deionized water rinsed clean.
(2) preliminary treatment: immerse fiber containing in the methyl-sulfoxide of 30g/L cobalt nitrate and the aqueous solution of 1-METHYLPYRROLIDONE, wherein methyl-sulfoxide volumetric concentration is 20%, and the volumetric concentration of 1-METHYLPYRROLIDONE is take out after soaking 4h at 10%, 100 DEG C.
(3) reduce: pretreated fiber is put into 5g/L solution of potassium borohydride and carries out reduction treatment, temperature is 50 DEG C, takes out after 30min.
(4) chemical nickel plating: the fiber after reduction is put into nickel plating solution, and chemical nickel-plating liquid consists of: nickelous sulfate 15g/L, inferior sodium phosphate 20g/L, dimethylamino borine 3g/L, natrium citricum 20g/L, ammoniacal liquor 5ml/L, bath temperature is 60 DEG C, plating time 1h.
embodiment 3
detailed process and the step of the present embodiment are as described below:
(1) oil removing: Fanglun 1414 (PPTA) is put into acetone soln, takes out after Ultrasonic Cleaning 80min, use deionized water rinsed clean.
(2) preliminary treatment: immerse fiber containing in the dimethyl formamide of 50g/L cobalt chloride and the aqueous solution of dimethylacetylamide, wherein the volumetric concentration of dimethyl formamide is 15%, and the volumetric concentration of dimethylacetylamide is take out after soaking 2h at 15%, 30 DEG C.
(3) reduce: pretreated fiber is put into 25g/L sodium borohydride solution and carries out reduction treatment, temperature is 35 DEG C, takes out after 20min.
(4) chemical nickel plating: the fiber after reduction is put into nickel plating solution, and chemical nickel-plating liquid consists of: nickelous sulfate 25g/L, inferior sodium phosphate 15g/L, dimethylamino borine 6g/L, natrium citricum 25g/L, ammoniacal liquor 10ml/L, bath temperature is 80 DEG C, plating time 1h.
embodiment 4
detailed process and the step of the present embodiment are as described below:
(1) oil removing: Fanglun 1414 (PPTA) is put into acetone soln, takes out after Ultrasonic Cleaning 60min, use deionized water rinsed clean.
(2) preliminary treatment: fiber is immersed in the aqueous solution of the dimethyl formamide, 1-METHYLPYRROLIDONE and the methyl-sulfoxide three mixture that contain 30g/L silver nitrate, wherein the volumetric concentration of dimethyl formamide is 10%, the volumetric concentration of 1-METHYLPYRROLIDONE is 10%, the volumetric concentration of methyl-sulfoxide is take out after soaking 2h at 10%, 50 DEG C.
(3) reduce: pretreated fiber is put into 25g/L sodium borohydride solution and carries out reduction treatment, temperature is 35 DEG C, takes out after 20min.
(4) chemical nickel plating: the fiber after reduction is put into nickel plating solution, and chemical nickel-plating liquid consists of: nickelous sulfate 25g/L, inferior sodium phosphate 15g/L, dimethylamino borine 8g/L, natrium citricum 25g/L, ammoniacal liquor 10ml/L, bath temperature is 80 DEG C, plating time 1h.
embodiment 5
detailed process and the step of the present embodiment are as described below:
(1) oil removing: Fanglun 1313 (PMIA) is put into acetone soln, takes out after Ultrasonic Cleaning 30min, use deionized water rinsed clean.
(2) preliminary treatment: fiber after oil removing is immersed containing in the 1-METHYLPYRROLIDONE of 20g/L silver acetate and the aqueous solution of methyl-sulfoxide mixture, wherein the volumetric concentration of 1-METHYLPYRROLIDONE is 15%, the volumetric concentration of methyl-sulfoxide is take out after soaking 1h at 15%, 50 DEG C.
(3) reduce: pretreated fiber is put into 10g/L solution of potassium borohydride and carries out reduction treatment, temperature is 30 DEG C, takes out after 20min.
(4) chemical nickel plating: the fiber after reduction is put into nickel plating solution, and chemical nickel-plating liquid consists of: nickelous sulfate 25g/L, inferior sodium phosphate 15g/L, dimethylamino borine 8g/L, natrium citricum 25g/L, ammoniacal liquor 10ml/L, bath temperature is 80 DEG C, plating time 1h.
Claims (5)
1. a preparation method for nickel plating aromatic polyamide fibre, is characterized in that having following process and step:
A. washing and oil removing: aromatic polyamide fibre is put into acetone, takes out after Ultrasonic Cleaning 40 ~ 80min, use deionized water rinsed clean;
B. preliminary treatment, makes fiber swelling, increased fiber surface area and wettability, and after the reduction of adsorption one deck, has the metal ion of catalytic activity, to improve the binding strength of fibrous matrix and subsequent plating layer;
C. reduce: pretreated fiber is put into 5 ~ 25g/L borane reducing agent sodium hydride aqueous solution or the potassium borohydride aqueous solution floods, at 20 ~ 50 DEG C, take out after dipping 20 ~ 60min;
D. chemical nickel plating:
Nickel-plating liquid with following material and water formulated, in reactant liquor, the content of each material is:
Nickelous sulfate 15 ~ 40g/L
Inferior sodium phosphate (reductant) 10 ~ 20g/L
Dimethylamino borine (reductant) 3 ~ 10g/L
Natrium citricum (complexing agent) 20 ~ 30g/L
Ammoniacal liquor (PH conditioning agent) 5 ~ 15ml/L
Aramid fiber after reduction is immersed in nickel-plating liquid, at 40 ~ 80 DEG C, takes out after reaction 0.5 ~ 1h, use deionized water rinsed clean, be placed in the dry 30min of drying box, obtain the aromatic polyamide fibre that surface uniform plating has nickel, namely conduct electricity aramid fiber.
2. the preparation method of a kind of nickel plating aromatic polyamide fibre according to claim 1, is characterized in that described aromatic polyamide fibre is Fanglun 1414 (PPTA) and poly-mphenylen terephthalamide's fiber (PMIA).
3. the preparation method of a kind of nickel plating aromatic polyamide fibre according to claim 1, it is characterized in that step b preprocessing process is: the fiber after oil removing is put into pretreatment fluid, wherein in pretreatment fluid, the concentration of salt is 5 ~ 50g/L, at 30 ~ 100 DEG C, take out after dipping 1 ~ 4h, use deionized water rinsed clean.
4. pretreatment fluid according to claim 3, is characterized in that the composition of salt in pretreatment fluid is the cobalt salts such as cobaltous fluoride, cobalt chloride, cobaltous bromide, cobaltous sulfate, cobalt nitrate, and the silver salt such as silver nitrate, silver acetate.
5. pretreatment fluid according to claim 3, is characterized in that the composition of solvent in pretreatment fluid is the aqueous solution of one or more mixtures such as 1-METHYLPYRROLIDONE, dimethylacetylamide, methyl-sulfoxide and dimethyl formamide.
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| CN201510568766.4A CN105133301B (en) | 2015-06-10 | 2015-09-09 | A kind of preparation method of nickel plating aromatic polyamide fibre |
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| CN2015103133885 | 2015-06-10 | ||
| CN201510313388.5A CN104894539A (en) | 2015-06-10 | 2015-06-10 | Preparation method for nickel plating aromatic polyamide fibers |
| CN201510357550.3A CN104894846A (en) | 2015-06-26 | 2015-06-26 | Preparation method of nickel-plated aromatic polyamide fiber |
| CN2015103575503 | 2015-06-26 | ||
| CN201510568766.4A CN105133301B (en) | 2015-06-10 | 2015-09-09 | A kind of preparation method of nickel plating aromatic polyamide fibre |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106758136A (en) * | 2016-12-29 | 2017-05-31 | 四川大学 | The aromatic polymer fiber of composite performance high containing benzimidazole and preparation method thereof |
| CN111270519A (en) * | 2020-03-26 | 2020-06-12 | 苏州耐科泰斯纺织新材料有限公司 | Antibacterial flame-retardant fiber and preparation method thereof |
| CN112458751A (en) * | 2020-09-15 | 2021-03-09 | 鲁东大学 | Nano-silver para-aramid fiber, and preparation method and application thereof |
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| CN102899890A (en) * | 2012-10-31 | 2013-01-30 | 昆明理工大学 | Aramid fiber surface metallization treatment method |
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| CN104894846A (en) * | 2015-06-26 | 2015-09-09 | 上海大学 | Preparation method of nickel-plated aromatic polyamide fiber |
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| CN1089309A (en) * | 1992-12-08 | 1994-07-13 | 纳幕尔杜邦公司 | The aromatic poly of electroless coating surface and manufacture the method on this surface |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106758136A (en) * | 2016-12-29 | 2017-05-31 | 四川大学 | The aromatic polymer fiber of composite performance high containing benzimidazole and preparation method thereof |
| CN106758136B (en) * | 2016-12-29 | 2019-04-05 | 四川大学 | Aromatic polymer fiber and preparation method thereof of the high composite performance containing benzimidazole |
| CN111270519A (en) * | 2020-03-26 | 2020-06-12 | 苏州耐科泰斯纺织新材料有限公司 | Antibacterial flame-retardant fiber and preparation method thereof |
| CN112458751A (en) * | 2020-09-15 | 2021-03-09 | 鲁东大学 | Nano-silver para-aramid fiber, and preparation method and application thereof |
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