CN101775670B - Method for preparing polyimide/silver composite electrical conductivity fibers - Google Patents
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Abstract
The invention relates to a method for preparing polyimide/silver composite electrical conductivity fibers, which comprises the following steps: firstly preparing polyamic acid fibers from polyamic acid solution; then drawing polyamic acid fibers at constant speed to carry out iron exchange in soluble silver salt solution to make silver irons diffuse and immerse the surface of the polyamic acid fibers and combined with amic acid radical to obtain a silver salt compound of polyamic acid; and finally by heating, making the silver irons reduced and accumulate on the surface and making polyamic acid fibers cyclized into polyimide fibers to obtain the conductive polyimide/silver composite electrical conductivity fibers. The method of the invention has the advantages of integrated molding, simple process, low cost, no toxicity and no pollution, capacity of being used for large-scale industrial production, high adhesive strength of the silver salt on the surface layer of the fibers, metallic luster, excellent electrical conductivity and the like.
Description
Technical field
The present invention relates to a kind of preparation method of polyimide/silver composite conducting fiber, particularly by prepare the method for polyimide/silver composite conducting fiber at the direct Ag ion exchange original position of polyamic acid fiber self-metallization.
Background technology
Conductive fiber is meant that generally (20 ℃, 65%RH) electrical conductivity is 10 under the standard state
-8The fiber that S/cm is above because conductive fiber has conduction, antistatic, electric heating, reflection and multiple functions such as absorption electromagnetic wave, sensing, is widely used in electric power conveying, the anti-static clothing of power industry; The electric heating bandage of medical industry, anti-electromagnetic radiation Work Clothes; The electro-magnetic shielding cover of Aero-Space precise electronic industry, " stealthy " material; Aspects such as the conductivity sensor of sensing industry, optical pickocff.The conductive fiber kind is more, can comprehensively be divided into metal fibre, carbon fiber, non-conductive polymer conductive compositions cladded type fiber, non-conductive polymer conductive compositions composite fibre, conducting polymer cladded type fiber, conducting polymer composite fibre and structural conductive polymer fiber etc. by conductive compositions and the distribution in fiber thereof.Wherein metallic cover type organic fiber is the very important conductive fiber of a class, and this fiber not only has functions such as favorable conductive, electric heating, reflection and absorption electromagnetic wave, but also with the peculiar ventilative and softness characteristics of organic fiber fabric.Present this fiber is mainly based on nickel plating (copper) fiber, the shortcoming of existence be harden, not folding, not washable, human body skin is stimulated irritated.Compare with copper nickel, modern medicine circle thinks that silver has very effective broad spectrum antibacterial, do not find as yet at present that human body produces irritated any report to fine silver, and silver-plated conductive fiber goes out to have better conduction, heat conduction, lead wet, shielding property, more have the function of antibacterial and deodouring concurrently, have wear-resisting, washable, good characteristics such as anti-folding, Japan, Korea S, U.S.'s copper facing silver conductive fabric, pure silver-plated conductive fabric, silver-plated polyster fibre is widely adopted PDP-TV, LCD-TV, in military electronic product and the high-end electronic product, silver plated fiber and fabric have the trend of replacement nickel plating (copper) fiber and fabric.In addition, the matrix of metal current cladded type organic fiber mainly concentrates on the traditional fibre such as terylene, polyamide fibre and acrylic fibers, less for the research of high-performance fiber surface metalation both at home and abroad, the research of especially relevant surperficial patina polyimides composite conducting fiber yet there are no report.
The method of organic fiber surface metalation is divided into physical method (vacuum plating) and physico-chemical process (chemical plating of ion plating, no electrolysis and electrochemical deposition) according to preparation condition.Vacuum plating and ion plating need carry out under high vacuum state, need large-scale equipment, and big to fibre damage, are difficult to realize industrialization, so general is adopted when the fiber of processing specific use.The fabric of present argentiferous, its production technology generally adopts chemical silvering technology, publication number is that the patent of CN 101446037A has been carried out detailed explanation to the method for chemical plating metal, this method equipment needed thereby is simple, less to fibre damage, and can handle continuously fiber, the fiber excellent conductivity that obtains, but this procedure complexity, production efficiency is low, cost is high, seriously polluted.
Summary of the invention
The objective of the invention is to solve the deficiencies in the prior art, and provide a kind of integrated molding to prepare the technology of polyimide/silver high performance composite conductive fibre, its product surface is even, glossy, resistivity is low, the adhesive strength height, and technology is simple, with low cost, be expected to be used for industrialized mass.
1, a kind of method for preparing the polyimide/silver composite conducting fiber is characterized in that, may further comprise the steps:
A: adopting solid content is the polyamic acid solution of 3%-30%, uses wet spinning technology and prepares the polyamic acid fiber;
B: the polyamic acid fiber for preparing in the steps A is at the uniform velocity exchanged 1 second to 2 hours by the soluble silver salt effects of ion under the effect of godet roller, remove the silver salt of surface attachment again by water washing, and then at the uniform velocity remove the water of fiber surface by hanging down warm stove, the temperature of low warm stove is set at 50 ℃-200 ℃, obtains the surface and is the fiber of polyamic acid silver salt;
C: the surface that step B is obtained is that the fiber of polyamic acid silver salt at the uniform velocity carries out the reduction of silver and the imidizate of fiber by the elevated temperature heat stove under the effect of godet roller, the temperature of elevated temperature heat stove is 200 ℃-600 ℃, and keep 5min-8h, promptly obtain the polyimide/silver composite conducting fiber.
D: the preparation process of polyimide/silver composite conducting fiber, belong to integrated forming technique, through wet spinning, direct ion exchange, cleaning, oven dry and heating patina, can directly obtain the polyimide/silver composite conducting fiber by polyamic acid solution.
Wherein, polyamic acid solution in the steps A, be to make by any diamines and any dianhydride homogeneous polycondensation, as pyromellitic acid anhydride (PMDA)/4,4 '-diaminodiphenyl ether (ODA), 3,3 ', 4,4 '-two methyl phenyl ethers anisole tetracarboxylic dianhydrides (ODPA)/4,4 '-diaminodiphenyl ether (ODA), 3,3 ', 4,4 '-benzophenone tetracarboxylic dianhydride (BTDA)/4,4 '-diaminodiphenyl ether (ODA), 3,3 ', 4,4 '-bibenzene tetracarboxylic dianhydride (BPDA)/p-phenylenediamine (PPD) homopolymerization polyamic acid solutions such as (pPDA), perhaps make,, perhaps make by any several diamines and any several dianhydride mixed polycondensation as PMDA-ODA/pPDA copolyamide acid solution by any several diamines and any several dianhydride copolycondensation, as PMDA/ODA and BPDA/pPDA homopolymerization respectively earlier, the polyamic acid solution of preparation admixed together etc. again.
Polyamic acid fiber in the steps A adopts the wet spinning technology preparation, is about to polyamic acid solution and sprays thread by spinneret orifice, directly enters the chemical fibre spinning process that coagulating bath forms fiber.Coagulating bath can be a water, wherein one or more of methyl alcohol, ethanol, ethylene glycol, acetone, toluene N, dinethylformamide (DMF), N, N-dimethylacetylamide (DMAc), N-Methyl pyrrolidone, dimethyl sulfoxide (DMSO) (DMSO) etc.
Silver soluble salting liquid described in the step B is the aqueous solution of silver acetate, silver nitrate, silver carbonate, silver fluoride, silver benzoate, silver triflate, silver sulfate, boric acid silver, silver ammino solution, silver perchlorate or silver tetrafluoroborate.Consider factors such as price and silver salt concentration, be preferably silver ammino solution, the aqueous solution of silver nitrate or silver fluoride.
The concentration of the silver soluble salting liquid described in the step B is greater than 0.01mmol/l, for the Cmax of silver salt solution without limits, mainly be because there is inversely prroportional relationship in the concentration of fiber soak time and silver salt solution, the longest soak time of control got final product with interior at 2 hours.
After step C, can obtain the polyimide/silver composite conducting fiber.The metallization flow chart as shown in Figure 1.
Numeral 1 expression contains the spinning bucket of polyamic acid solution among the figure, in 2 expression spinneretss and the immersion coagulation bath 3, the aqueous solution that 4 expressions contain silver ion carries out ion-exchange, 5 expression waters clean, 6 expressions are with hot stove heating, drying and carry out the thermal reduction of silver ion and the imidizate of polyamic acid fiber, and 7 expressions are reeled and received silk.
Compared with prior art, the present invention has following excellent results:
1, the conductive fiber employing polyimide fiber of the present invention's preparation is a matrix, this fiber not only has the characteristic of high-strength and high-modulus, but also having superior performances such as high temperature resistant, resistance to chemical attack, radiation hardness, anti-combustion, the composite conducting fiber that finally makes is expected to be widely used in the very harsh research in fields such as atomic energy industry, space environment, the needs of recovering, Aero-Space, national defense construction, novel building, rapid, ocean development, sports apparatus, new forms of energy, environment industry and safety device.
2 methods that prepare the polyimide/silver composite conducting fiber provided by the invention, technology is simple, by integral process, can directly change the polyamic acid fiber into the polyimide/silver composite conducting fiber.
3 methods that prepare the polyimide/silver composite conducting fiber provided by the invention, not that argent is applied or is dipped on the surface of polyimide fiber, but make silver ion reduction and accumulate to the top layer and the shallow top layer of polyimide fiber by the method for heating, therefore have higher adhesive strength.
The polyimide/silver composite conducting fiber of 4 the inventive method preparations, surperficial silver-colored grain size and being evenly distributed, fiber has good metal gloss.
The medicine of using among 5 the present invention is all quite cheap, and consumption is few, and nontoxic, can not pollute environment, and the medicine of useful mistake can recycle.
6 processes of the invention process are simple, are easy to procedure, and industrial prospect is good.
The argent of this invention and the polyimide fiber adhesion is strong, pollution-free, cost is low, can produce continuously.Product can be used for industries such as electronics, military project, communication, medical treatment and extraordinary weaving, as electronic shield product, military shielding tent, extraordinary weaving anti-biotic material and civilian health textile.
Description of drawings
Fig. 1: the flow chart of the integrated preparation polyimide/silver of the inventive method composite conducting fiber.
Fig. 2: surface scan Electronic Speculum (SEM) photo of polyamic acid fiber.Wherein a and b are respectively multiplication factor 1000 and 5000.
Fig. 3: polyimide fiber surface scan Electronic Speculum (SEM) photo.Wherein a and b are respectively multiplication factor 1000 and 5000.
Surface scan Electronic Speculum (SEM) photo of the polyimide/silver composite fibre that Fig. 4: embodiment 1 makes.Wherein a and b are respectively multiplication factor 5000 and 30000.
Method of the present invention has prepared the polyimide/silver composite conducting fiber, Fig. 4 is the surface scan electromicroscopic photograph that adopts the polyimide/silver composite conducting fiber that this method prepares, compare with polyimide fiber monofilament surface stereoscan photograph (Fig. 3) with pure polyamic acid fibre single thread surface scan electromicroscopic photograph (Fig. 2), the polyimide fiber surface has generated the continuous silver layer of one deck, and silver layer distributes very evenly.
The specific embodiment
Method of the present invention focuses on integrated molding and prepares the polyimide/silver composite conducting fiber.Table 1 has provided polyimide/silver composite conducting fiber electrical property.As can be seen from Table 1, the polyimide/silver composite conducting fiber has higher electric conductivity.
Below in conjunction with drawings and Examples the present invention is further described.
A: adopting solid content is the polyamic acid solution of 15%PMDA/ODA, uses wet spinning technology and prepares the polyamic acid fiber;
B: with the polyamic acid fiber for preparing in the steps A at the uniform velocity is the silver ammino solution intermediate ion exchange 5min of 0.01mol/l by concentration under the effect that godet roller rotates, remove the silver salt of surface attachment again by water washing, and then at the uniform velocity remove the water of fiber surface by hanging down warm stove, the temperature of low warm stove is set at 100 ℃, be 10min heat time heating time, obtains the surface and be the fiber of polyamic acid silver;
C: the surface that step B is obtained is that the fiber of polyamic acid silver salt at the uniform velocity carries out the reduction of silver and the imidizate of fiber by the elevated temperature heat stove under the effect of godet roller, the temperature of elevated temperature heat stove is 220 ℃, and keep 2h, promptly obtain the polyimide/silver composite conducting fiber.
Embodiment 2
A: adopting solid content is the 20%PMDA/ODA polyamic acid solution, uses wet spinning technology and prepares the polyamic acid fiber;
B: with the polyamic acid fiber for preparing in the steps A at the uniform velocity is the liquor argenti nitratis ophthalmicus intermediate ion exchange 10min of 0.001mol/l by concentration under the effect that godet roller rotates, remove the silver salt of surface attachment again by water washing, and then at the uniform velocity remove the water of fiber surface by hanging down warm stove, the temperature of low warm stove is set at 180 ℃, be 5min heat time heating time, obtains the surface and be the fiber of polyamic acid silver;
C: the surface that step B is obtained is that the fiber of polyamic acid silver salt at the uniform velocity carries out the reduction of silver and the imidizate of fiber by the elevated temperature heat stove under the effect of godet roller, the temperature of elevated temperature heat stove is 350 ℃, and keep 1h, promptly obtain the polyimide/silver composite conducting fiber.
Embodiment 3
A: adopting solid content is the 25%PMDA/ODA polyamic acid solution, uses wet spinning technology and prepares the polyamic acid fiber;
B: with the polyamic acid fiber for preparing in the steps A at the uniform velocity is the liquor argenti nitratis ophthalmicus intermediate ion exchange 20min of 0.0001mol/l by concentration under the effect that godet roller rotates, remove the silver salt of surface attachment again by water washing, and then at the uniform velocity remove the water of fiber surface by hanging down warm stove, the temperature of low warm stove is set at 200 ℃, be 3min heat time heating time, obtains the surface and be the fiber of polyamic acid silver;
C: the surface that step B is obtained is that the fiber of polyamic acid silver salt at the uniform velocity carries out the reduction of silver and the imidizate of fiber by the elevated temperature heat stove under the effect of godet roller, the temperature of elevated temperature heat stove is 400 ℃, and keep 1h, promptly obtain the polyimide/silver composite conducting fiber.
Embodiment 4
A: adopting solid content is the polyamic acid solution of 10%PMDA-ODA/pPDA, uses wet spinning technology and prepares the polyamic acid fiber;
B: with the polyamic acid fiber for preparing in the steps A at the uniform velocity is the liquor argenti nitratis ophthalmicus intermediate ion exchange 1h of 0.1mol/l by concentration under the effect that godet roller rotates, remove the silver salt of surface attachment again by water washing, and then at the uniform velocity remove the water of fiber surface by hanging down warm stove, the temperature of low warm stove is set at 50 ℃, be 30min heat time heating time, obtains the surface and be the fiber of polyamic acid silver;
C: the surface that step B is obtained is that the fiber of polyamic acid silver salt at the uniform velocity carries out the reduction of silver and the imidizate of fiber by the elevated temperature heat stove under the effect of godet roller, the temperature of elevated temperature heat stove is 300 ℃, and keep 1.5h, promptly obtain the polyimide/silver composite conducting fiber.
Embodiment 5
A: adopting solid content is the polyamic acid solution of 5%PMDA/ODA and BPDA/pPDA blend, uses wet spinning technology and prepares the polyamic acid fiber;
B: with the polyamic acid fiber for preparing in the steps A at the uniform velocity is the silver fluoride effects of ion exchange 1.5h of 2mol/l by concentration under the effect that godet roller rotates, remove the silver salt of surface attachment again by water washing, and then at the uniform velocity remove the water of fiber surface by hanging down warm stove, the temperature of low warm stove is set at 150 ℃, be 20min heat time heating time, obtains the surface and be the fiber of polyamic acid silver;
C: the surface that step B is obtained is that the fiber of polyamic acid silver salt at the uniform velocity carries out the reduction of silver and the imidizate of fiber by the elevated temperature heat stove under the effect of godet roller, the temperature of elevated temperature heat stove is 350 ℃, and keep 1h, promptly obtain the polyimide/silver composite conducting fiber.
The performance of the polyimide/silver composite fibre that table 1 the inventive method is prepared
| Embodiment | The former monofilament of PAA | The |
1 | 2 | 3 | 4 | 5 |
| Electrical conductivity/s .cm -1 | NC | NC | 3.3 ×10 3 | 2.6 ×10 3 | 7.4 ×10 2 | 1.7 ×10 1 | 8.5 ×10 1 |
Annotate: the NC representative is non-conductive
It should be noted that at last: above embodiment only in order to the explanation the present invention and and unrestricted technical scheme described in the invention; Therefore, although this specification has been described in detail the present invention with reference to the above embodiments,, those of ordinary skill in the art should be appreciated that still and can make amendment or be equal to replacement the present invention; And all do not break away from the technical scheme and the improvement thereof of the spirit and scope of invention, and it all should be encompassed in the middle of the claim scope of the present invention.
Claims (4)
1. a method for preparing the polyimide/silver composite conducting fiber is characterized in that, may further comprise the steps:
A: adopting solid content is the polyamic acid solution of 3%-30%, uses wet spinning technology and prepares the polyamic acid fiber;
B: the polyamic acid fiber for preparing in the steps A is at the uniform velocity exchanged 1 second to 2 hours by the soluble silver salt effects of ion under the effect of godet roller, remove the silver salt of surface attachment again by water washing, and then at the uniform velocity remove the water of fiber surface by hanging down warm stove, the temperature of low warm stove is set at 50 ℃-200 ℃, obtains the surface and is the fiber of polyamic acid silver salt;
C: the surface that step B is obtained is that the fiber of polyamic acid silver salt at the uniform velocity carries out the reduction of silver and the imidizate of fiber by the elevated temperature heat stove under the effect of godet roller, the temperature of elevated temperature heat stove is 200 ℃-600 ℃, and keep 5min-8h, promptly obtain the polyimide/silver composite conducting fiber.
2. method according to claim 1 is characterized in that, the polyamic acid fiber in the steps A adopts the wet spinning technology preparation, is about to polyamic acid solution and sprays thread by spinneret orifice, directly enters the chemical fibre spinning process that coagulating bath forms fiber.
3. method according to claim 1, it is characterized in that the silver soluble salting liquid described in the step B is the aqueous solution of silver acetate, silver nitrate, silver carbonate, silver fluoride, silver benzoate, silver triflate, silver sulfate, boric acid silver, silver ammino solution, silver perchlorate or silver tetrafluoroborate.
4. method according to claim 1 is characterized in that, the concentration of the silver soluble salting liquid described in the step B is greater than 0.01mmol/l.
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| CN102168317B (en) * | 2011-03-11 | 2012-07-25 | 北京化工大学 | Method for preparing polyimide fibers |
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| CN110761071B (en) * | 2019-10-31 | 2023-05-30 | 南通先研新材料有限公司 | Nano silver wire fiber and preparation method thereof |
| CN111925550B (en) * | 2020-07-08 | 2023-02-10 | 中国航发北京航空材料研究院 | Preparation method of surface conductive thermosetting polyimide composite film |
| CN115012210B (en) * | 2022-07-06 | 2023-08-04 | 恒天嘉华非织造有限公司 | Tear-resistant antibacterial non-woven fabric and preparation method thereof |
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