CN105064009A - Preparation method of chemical conductive fibers - Google Patents
Preparation method of chemical conductive fibers Download PDFInfo
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- CN105064009A CN105064009A CN201510556483.8A CN201510556483A CN105064009A CN 105064009 A CN105064009 A CN 105064009A CN 201510556483 A CN201510556483 A CN 201510556483A CN 105064009 A CN105064009 A CN 105064009A
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- polyacrylonitrile
- yttrium nitrate
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- fiber
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Abstract
The invention discloses a preparation method of chemical conductive fibers. The preparation method comprises the following steps: preparing 100mL of polyacrylonitrile DMF (dimethylformamide) solution with mass fraction of 20-50%, dropping 3g of yttrium nitrate in the polyacrylonitrile DMF solution, and stirring, filtering and defoaming, thus preparing a polyacrylonitrile/yttrium nitrate mixed spinning solution; filtering and metering the polyacrylonitrile/yttrium nitrate mixed spinning solution, extruding the polyacrylonitrile/yttrium nitrate mixed spinning solution through spinneret orifices, enabling the polyacrylonitrile/yttrium nitrate mixed spinning solution to enter a coagulating bath and carrying out washing, drying and heat setting and winding procedures, thus preparing polyacrylonitrile/yttrium nitrate fibers; adding 1g of polyacrylonitrile/yttrium nitrate fibers to 100mL of plating solution to react at 50 DEG C for 30-60 minutes, fully washing the reactants with water and then drying and weighing the reactants, thus obtaining the products. The chemical conductive fibers have the advantages of stable structure, high silver ion deposition speed, good conductivity, and the like.
Description
Technical field
The present invention relates to a kind of preparation method of conductive material, particularly relate to a kind of preparation method of chemical conductive fiber.
Background technology
Polyacrylonitrile fibre, since realizing suitability for industrialized production, has received doting on of people with its excellent intensity, fluffy outward appearance and bright-coloured color and luster.But acrylic fiber hydrophily is poor, very easily produces electrostatic.
By carrying out chemical silvering process to acrylic fiber, the electric conductivity of acrylic fibers can be improved.Traditional chemical silvering process mainly improves silver-plated speed by improving the concentration of silver ion or the concentration of reductant in silver-plated temperature, increase plating solution.But silver-plated temperature is higher, the concentration of silver ion or the concentration of reductant larger, plating solution more easily decomposes, and causes silver-plated efficiency lower, affects the electric conductivity of finished product.
Summary of the invention
The present invention is directed to the defect of current techniques, disclose the preparation method of a kind of chemical silvering polyacrylonitrile/yttrium nitrate conductive fiber.
The present invention solves the problems of the technologies described above by the following technical solutions: a kind of preparation method of chemical silvering polyacrylonitrile/yttrium nitrate conductive fiber, and described preparation method comprises the following steps:
(1) polyacrylonitrile powder taking 20 ~ 50g is added in DMF, obtained mass fraction be 20% ~ 50% polyacrylonitrile solution add 3g yttrium nitrate to described polyacrylonitrile solution, after abundant stirring 30 ~ 90min, through filtration under diminished pressure, vacuum defoamation, obtained polyacrylonitrile/yttrium nitrate blend spinning liquid;
(2) on routine little formula wet process equipment, described polyacrylonitrile/yttrium nitrate blend spinning liquid is filtered, after metering, extruded by spinneret orifice, enter the coagulating bath be made up of DMF solvent and water, then through washing, dry heat sizing and rolling step, obtained polyacrylonitrile/yttrium nitrate fiber;
(3) silver ammino solution taking 30mL is added in the reducing solution of 70mL, and liquid is crossed in preparation; Add described 1g polyacrylonitrile/yttrium nitrate fiber to described in cross in liquid, at 50 DEG C react 30 ~ 60min, after fully washing with water, dry and weigh, obtaining product.
The present invention, by preparation polyacrylonitrile/yttrium nitrate blend spinning liquid, carries out solution-polymerized SBR, obtained polyacrylonitrile/yttrium nitrate fiber, then through Electroless Silver Plating, utilizes Rare Earth Y
3+can with NH
3form coordination thing, the main salt argent ion concentration of silver ammino solution is increased, promotes the transition of silver ion, assist silver-plated process, thus preparative chemistry silver-plated polyacrylonitrile/yttrium nitrate conductive fiber.
The invention has the advantages that: chemical silvering polyacrylonitrile/yttrium nitrate conductive fiber disclosed by the invention have Stability Analysis of Structures, silver ion deposition velocity fast, conduct electricity very well.
Accompanying drawing explanation
Fig. 1 be the present invention with the consumption of yttrium nitrate for variable, the chemical silvering deposition velocity curve map of test.
Fig. 2 be the present invention with the consumption of polyacrylonitrile for variable, the powerful curve map of the conductive fiber of test.
Detailed description of the invention
Below in conjunction with instantiation, the present invention is described in detail; should understand; embodiment is only for illustration of the present invention, instead of for limiting the present invention, any amendment, equivalent replacement etc. made on basis of the present invention is all in protection scope of the present invention.
Embodiment 1
The experiment that the consumption of different yttrium nitrate affects chemical silvering deposition velocity:
The polyacrylonitrile powder taking 40g is added in DMF, obtained mass fraction is the polyacrylonitrile solution of 40%, instill the yttrium nitrate of 1g, 2g, 3g, 4g, 5g respectively to described polyacrylonitrile solution, after abundant stirring 60min, through filtration under diminished pressure, vacuum defoamation, obtained polyacrylonitrile/yttrium nitrate blend spinning liquid.By after described polyacrylonitrile/yttrium nitrate blend spinning liquid filtration, metering on routine little formula wet process equipment, extruded by spinneret orifice, enter the coagulating bath be made up of DMF solvent and water, then through washing, dry heat sizing and rolling step, obtained polyacrylonitrile/yttrium nitrate fiber.The silver ammino solution taking 30mL is added in the reducing solution of 70mL, and liquid is crossed in preparation; Adding 1g polyacrylonitrile/yttrium nitrate fiber to crossing in liquid, at 50 DEG C, reacting 60min, after fully washing with water, dry and weigh, obtaining product.
The mensuration of sedimentation rate: after silver-plated a period of time, determine sedimentation rate, uses the quality of the silver-plated front and back of electronic balance weighing sample chemical, and by under time calculate sedimentation rate:
In formula, V is sedimentation rate (um/h), m
1and m
2be respectively the quality (g) of silver-plated forward and backward sample, p is the density (10.5g/cm of silver coating
3), A is the surface area (cm of sample
2), t is silver-plated time (h).
Shown in Fig. 1 curve, along with the increase of yttrium nitrate initial content, the deposition velocity of silver ion increases gradually, and when the consumption of yttrium nitrate is 4g, the deposition velocity of silver ion reaches maximum, and maximum deposition speed is 14.2um/h; The consumption of further increase yttrium nitrate, the deposition velocity of anion declines to some extent.This is because, when the consumption of yttrium nitrate is between 1 ~ 4g, along with the continuous increase of yttrium nitrate concentration in the plating solution, there is more Y
3+can with NH
3form coordination thing, consume a part of NH in silver ammino solution
3, main salt concentration of metal ions free in plating solution is increased, thus adds the some potential difference at interface, facilitate the transition of silver particles to catalytic surface, improve sedimentation rate; After the concentration of yttrium nitrate is greater than 4g, along with the increase of yttrium nitrate concentration, because excessive rare-earth yttrium is adsorbed on the surface of fiber, the outside of coated with silver particle, the autocatalysis of silver is restricted, and deposition velocity declines to some extent.
Embodiment 2
The consumption of different polyacrylonitrile is to the experiment of conductive fiber strong influence:
The polyacrylonitrile powder taking 10g, 20g, 30g, 40g, 50g is respectively added in DMF, obtained mass fraction is the polyacrylonitrile solution of 40%, instill the yttrium nitrate of 3g respectively to described polyacrylonitrile solution, after abundant stirring 60min, through filtration under diminished pressure, vacuum defoamation, obtained polyacrylonitrile/yttrium nitrate blend spinning liquid.By after described polyacrylonitrile/yttrium nitrate blend spinning liquid filtration, metering on routine little formula wet process equipment, extruded by spinneret orifice, enter the coagulating bath be made up of DMF solvent and water, then through washing, dry heat sizing and rolling step, obtained polyacrylonitrile/yttrium nitrate fiber.The silver ammino solution taking 30mL is added in the reducing solution of 70mL, and liquid is crossed in preparation; Adding 1g polyacrylonitrile/yttrium nitrate fiber to crossing in liquid, at 50 DEG C, reacting 60min, after fully washing with water, dry and weigh, obtaining product.
Broken filament brute force measures: at setting folder apart from d=20mm, retest frequency n=250 time, carry out constant speed tension test under draw speed v=30mm/min condition.
Shown in Fig. 2 curve, along with the increase of polyacrylonitrile initial content, the broken filament intensity of conductive fiber increases gradually, when polyacrylonitrile initial content is more than 40g, because concentration of dope is too high, macromolecular entanglements and crystallization, often make uniform dissolution become very difficult.Even and if dissolve, the mobility of solution and spinnability are also very poor, cannot realize spinning smoothly.
The foregoing is only the preferred embodiment of the invention; not in order to limit the invention; the any amendment done within all spirit in the invention and principle, equivalently to replace and improvement etc., within the protection domain that all should be included in the invention.
Claims (1)
1. a preparation method for chemical conductive fiber, is characterized in that: described preparation method comprises the following steps:
(1) polyacrylonitrile powder taking 20 ~ 50g is added in DMF, obtained mass fraction is the polyacrylonitrile solution of 20% ~ 50%, add the yttrium nitrate of 3g to described polyacrylonitrile solution, after abundant stirring 30 ~ 90min, through filtration under diminished pressure, vacuum defoamation, obtained polyacrylonitrile/yttrium nitrate blend spinning liquid;
(2) on routine little formula wet process equipment, described polyacrylonitrile/yttrium nitrate blend spinning liquid is filtered, after metering, extruded by spinneret orifice, enter the coagulating bath be made up of DMF solvent and water, then through washing, dry heat sizing and rolling step, obtained polyacrylonitrile/yttrium nitrate fiber;
(3) silver ammino solution taking 30mL is added in the reducing solution of 70mL, and preparation 100mL crosses liquid; Add described 1g polyacrylonitrile/yttrium nitrate fiber to described in cross in liquid, at 50 DEG C react 30 ~ 60min, after fully washing with water, dry and weigh, obtaining product.
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| CN201510556483.8A CN105064009A (en) | 2015-09-02 | 2015-09-02 | Preparation method of chemical conductive fibers |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244459B (en) * | 2008-03-25 | 2010-06-16 | 合肥工业大学 | Chemical plating silver copper powder, chemical plating liquid and chemical plating method |
| CN102051803B (en) * | 2009-11-10 | 2012-01-04 | 山东天诺光电材料有限公司 | Method for manufacturing silver-plated conductive fiber |
| CN102321879A (en) * | 2011-06-16 | 2012-01-18 | 东华大学 | Method for improving appearance and conductive performance of conductive microspheres |
-
2015
- 2015-09-02 CN CN201510556483.8A patent/CN105064009A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101244459B (en) * | 2008-03-25 | 2010-06-16 | 合肥工业大学 | Chemical plating silver copper powder, chemical plating liquid and chemical plating method |
| CN102051803B (en) * | 2009-11-10 | 2012-01-04 | 山东天诺光电材料有限公司 | Method for manufacturing silver-plated conductive fiber |
| CN102321879A (en) * | 2011-06-16 | 2012-01-18 | 东华大学 | Method for improving appearance and conductive performance of conductive microspheres |
Non-Patent Citations (3)
| Title |
|---|
| HAO YOU ETAL: "Low pressure high flux thin film nanofibrous composite membranes prepared by electrospraying technique combined with solution treatment", 《JOURNAL OF MEMBRANE SCIENCE》 * |
| YONGZHI WANG ETAL: ".Preparation of silver nanoparticles dispersed in polyacrylonitrile nanofiber film spun by electrospinning", 《MATERIALS LETTERS》 * |
| 于丽娜等: "聚丙烯腈纳米纤维载银复合膜绿色制备及其催化性质", 《高分子学报》 * |
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Application publication date: 20151118 |
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