CN102505493A - Preparation method for silver plating textile through nitrogen containing conductive polymers - Google Patents
Preparation method for silver plating textile through nitrogen containing conductive polymers Download PDFInfo
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Abstract
The invention relates to a preparation method for a silver plating textile through nitrogen containing conductive polymers; the preparation method comprises the following steps of: (1) immersing a textile in a detergent aqueous solution for washing; (2) putting the textile obtained in the step (1) in a roughening solution for roughening to obtain the roughened textile; (3) putting the roughened textile in a protonic acid solution of nitrogen containing polymer monomers, oscillating, adsorbing, and taking out and air-drying the textile; (4) immersing the textile obtained in the step (3) in an oxidant solution, then padding to obtain the textile covered by nitrogen containing polymers; (5) putting the textile covered by the nitrogen containing polymers in an aqueous solution containing stannous chloride and hydrochloric acid, and taking out and rinsing the textiles clean after oscillating; and (6) immersing the textile obtained in the step (5) in a silver plating reaction liquid, and taking out and rinsing the textiles clean after ultrasonic reaction, thereby obtaining the silver plating textile. The preparation method provided by the invention is simple, safe and environment-friendly and is low in cost; and the silver plating textile obtained by the preparation method has excellent electric conduction and electromagnetic shielding performances and has stable properties and wide application prospect.
Description
Technical field
The invention belongs to the preparation field of silver coating fabric, particularly a kind of preparation method via nitrogenous conducting polymer silver coating fabric.
Background technology
Progress along with the epoch; Single metal or structural conductive macromolecular material can not satisfy the requirement that people improve electromagnetic radiation protection day by day, exploitation possess more wide frequency ranges and Geng Gao shield effectiveness capability of electromagnetic shielding and other additional properties (as antibiotic, antistatic, prevent ultraviolet etc.) multifunction finishing agent become the focus that people competitively pay close attention to.
In textile field, metal is combined to be applied to structural conductive macromolecular in the fabric, on the one hand the static behaviour of fabric is improved greatly, can improve metallized fabric feeling and comfort level greatly on the other hand.Report that at present people such as Emmanuel Gasana study Nomex, discover that on the Nomex surface directly copper facing can not get desirable effect; So taked first chemical deposition polypyrrole, carry out the mode of electroless copper again, obtain to have good electrical conductivity (Emmanuel Gasana; Philippe Westbroek; Jean Hakuzimana, et al, Electroconductive textile structures through electroless deposition of polypyrrole and copper at polyaramide surfaces [J] .Surface and Coatings Technology; 2006,201 (6): 3547-3551.).People such as Nowoo Park study the metallization of dacron; Terylene has four steps in processing: clean and alkali decrement-PANI coating-palladium activation-copper facing (Park N; Kim W, Kim J.Copper Metallization of Poly (ethylene terephthalate) Fabrics via Intermediate Polyaniline Layers [J] .Fibers and Polymers, 2009; 10 (3): 310-314.); Through discovering, be that the method for intermediate layer makes fabric obtain lower resistance with the polyaniline, improved shield effectiveness.At present, being in the starting stage for the applied chemistry electroplating method in the research of structural conductive macromolecular layer plated metal abroad, is the existing minority report of research of matrix with the fabric.Though the domestic existing relevant report that metal is combined to be applied to field of textiles with conducting polymer; But application mode still adopts simple face coat; Be metal dust with the structural conductive macromolecular material in be coated on again after mixing fabric face (Wang Jun, Zhu Guohui, Mao Weimin. polyaniline proterties and content thereof are to the influence [J] of nickel powder/polyaniline coating shielding properties. functional material; 2008,39 (5): 737-739.).Domestic with the intermediate layer of structural conductive macromolecular as non-conductive matrix; Use (Zhang Peng to some extent in electron trade at its surface deposition metal; He Darong, Zhao Fayun. plastics (ABS) directly electroplating on surface technical studies [J]. material protection, 2001; 34 (6): 30-33.), but rarely have report in the application of the textile surface that is all non-conductive matrix.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method via nitrogenous conducting polymer silver coating fabric, and this method is simple, safety and environmental protection, and cost is low, and is low to the equipment requirements performance; Resulting silver coating fabric has excellent conduction and capability of electromagnetic shielding, has a extensive future.
A kind of preparation method via nitrogenous conducting polymer silver coating fabric of the present invention comprises:
(1) fabric is immersed in the water-detergent solution of 10～40g/L, 30 ℃～60 ℃ down dipping to take out rinsing after 10～40 minutes clean, to remove fabric face dirt, impurity and finish;
(2) fabric of step (1) gained is put into the coarsening solution alligatoring, 70 ℃～100 ℃ down concussion take out after 30～80 minutes, be cooled to room temperature, uses glacial acetic acid to regulate pH value and is 6.5-7.5, rinsing is clean then, dries, and gets the fabric after the alligatoring;
(3) fabric after the above-mentioned alligatoring is put into the Bronsted acid solution of nitrogen containing polymer monomer, under 70 ℃～100 ℃, concussion absorption was taken out after 50～120 minutes, dried;
(4) the textile impregnation 5～15S in the oxidation liquid of being made up of ammonium persulfate and Bronsted acid that step (3) is obtained is then in 0.5～2.5Kg/cm
2Pressure under pad, and under 0 ℃ environment, continue reaction, obtain being covered with the fabric of nitrogen containing polymer;
(5) the above-mentioned fabric that is covered with nitrogen containing polymer is put into contained stannous chloride (SnCl
2) and the aqueous solution of hydrochloric acid (HCl) in, under 20～50 ℃, shake that to take out rinsing after 5～30 minutes clean;
The pH value of (6) regulating silver plating reaction liquid is 10～11, and the fabric that step (5) obtains is immersed in the said silver plating reaction liquid, and 30～35 ℃ of following ultrasonic reactions take out rinsing after 20～60 minutes clean, promptly gets.
Fabric described in the step (1) is woven dacron, POLYAMIDE FABRIC, wash a kind of in the bright and beautiful cloth.
Coarsening solution described in the step (2) is the NaOH of 10～40g/L.
Adjusting pH value described in the step (2) is 3%～12% acetic acid adjusting for the use mass fraction.
Nitrogen containing polymer described in the step (3) is polyaniline or polypyrrole.
Bronsted acid described in step (3) and (4) is a kind of in hydrochloric acid, nitric acid, the DBSA.
The nitrogen containing polymer monomer concentration is 0.5～1.5mol/L in the Bronsted acid solution of the nitrogen containing polymer monomer described in the step (3), and the concentration of Bronsted acid is 0.5～1.5mol/L in the Bronsted acid solution of nitrogen containing polymer monomer.
Ammonium persulfate concentration is 0.2～0.8mol/L in the oxidation liquid described in the step (4), and the concentration of Bronsted acid is 0.2～0.8mol/L in the oxidation liquid.
Contain stannous chloride (SnCl described in the step (5)
2) and the aqueous solution of hydrochloric acid (HCl) in, the concentration of stannous chloride is 5～30g/L, the concentration of hydrochloric acid is 20ml/L～120ml/L.
AgN0 in the silver-colored reactant liquor described in the step (6)
3Concentration be 8～15g/L, the concentration of ammoniacal liquor is 50～130ml/L, the concentration of NaOH is 5～12g/L, glucose or concentration of sucrose are 2～4g/L.
A kind of preparation method via nitrogenous conducting polymer silver coating fabric of the present invention, summarize as follows:
The first step: washing and oil removing, remove fabric face dirt, impurity and finish;
Second step: alligatoring, the degree of roughness and the surface wettability of increase fabric face;
The 3rd step: adsorb, adsorb the monomer of nitrogenous conducting polymer at fabric face;
The 4th step: in-situ polymerization, nitrogenous conductive high polymer monomer in-situ polymerization are that nitrogen containing polymer is overlying on fabric face;
The 5th step: sensitization, the material that absorption one deck is reduced easily on fabric face;
The 6th step: the ultrasonic wave assistant chemical is silver-plated;
Mechanism: the present invention removes finish and the surperficial dirt of fabric in process through base fabric (terylene, polyamide fibre, wash brocade) is cleaned oil removal treatment earlier; After the oil removing, again fabric face is carried out roughened, to improve the close attachment fastness of nitrogen containing polymer and base material; Then the fabric after the alligatoring is adsorbed the nitrogen containing polymer monomer, and carry out in-situ oxidizing-polymerizing; The effect of sensitization is to be covered with the material that absorption one deck is reduced easily on the fabric face of nitrogen containing polymer; Adopt electroless plating method in the fabric face plate silver then, obtain high performance via the silver-plated fabric of nitrogenous conducting polymer.
The inventive method is through carrying out surface coarsening and etching to fabric; Increase the degree of roughness and the surface area of fabric face; Improve the adhesion of fabric and nitrogen containing polymer; Method through in-situ oxidizing-polymerizing is covered with the nitrogen containing polymer thin layer at fabric face again, and is silver-plated via the nitrogen containing polymer thin-layer chemical, improves adhesion and other performances of coating and substrate fabric.
The high-performance silver coating fabric of the present invention preparation, electric conductivity is good, and capability of electromagnetic shielding is excellent, high strength and have the softness of fabric; This fabric salt water resistance burn into is washable good with crocking resistance, the excellent bonding performance of coating and fabric; Surface side's resistance of fabric is 8～28m Ω/sq, and in the scope of 0.1MHz～18GHz, electromagnetic shielding effectiveness is greater than 60dB, i.e. electromagnetic wave radiation proof rate is greater than 99.9%; Can be widely used in the electromagnetic shielding of special sectors such as electromagnetic wave exposure suit and military affairs, national defence.
Beneficial effect
(1) preparation method of the present invention is simple, avoids the use of traditional activator palladium bichloride, has reduced pollution, safety and environmental protection, and cost is low, and is low to the equipment requirements performance;
(2) the resulting silver coating fabric of the present invention has excellent conduction and capability of electromagnetic shielding, and stable in properties satisfies the needs of developing high-grade electromagnetic screen textile, has a extensive future.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Present embodiment adopts POLYAMIDE FABRIC
(1) oil removing is put into the 20g/L water-detergent solution with fabric and soaked, and temperature is 45 ℃, takes out after 20 minutes, and is clean with the running water rinsing.
(2) alligatoring is immersed fabric in the 15g/L NaOH solution, and 90 ℃, take out after 50 minutes, be cooled to room temperature, the use mass fraction is 5% acetic acid neutralization, regulating the pH value is 6.5-7.5, clean with the running water rinsing.
(3) absorption is put into the aqueous solution that 0.5mol/L nitrogen containing polymer monomer-aniline and 0.5mol/L hydrochloric acid are formed with the fabric after the alligatoring, and temperature is 90 ℃, and concussion absorption 70 minutes is dried after taking out naturally.
(4) in-situ polymerization immerses 5S in 0.2mol/L ammonium persulfate and the 0.2mol/L aqueous solution of hydrochloric acid with the fabric after the absorption, is 1.5Kg/cm at pressure
2Padding machine on pad, and under 0 ℃ environment, continue reaction, obtain being covered with the fabric of nitrogen containing polymer.
(5) sensitization, the aqueous solution of the nylon fabric that is covered with polyaniline being put into 10g/L stannous chloride and 40ml/L hydrochloric acid composition carries out the sensitization processing, and temperature is 30 ℃, takes out rinsing 2～3 times after 10 minutes.
(6) chemical silvering under action of ultrasonic waves, is put into the silver plating bath plating with the fabric after the sensitization.Consisting of of chemical plating liquid: silver nitrate: 13g/L; Ammoniacal liquor: 100ml/L; NaOH:9g/L; Glucose: 2.7g/L; 30 ℃ of temperature, 50 minutes time.
Test shows, the resistance of the surface side of fabric is 8～12m Ω/sq, and electromagnet shield effect reaches more than the 60dB, and the electric conductivity and the capability of electromagnetic shielding of fabric are good, and have kept the original characteristic of fabric, and be soft, and rub resistance and washing fastness are good.
Embodiment 2
Present embodiment adopts washs bright and beautiful cloth
(1) oil removing is put into the 25g/L water-detergent solution with fabric and soaked, and temperature is 50 ℃, takes out after 15 minutes, and is clean with the running water rinsing.
(2) alligatoring is immersed fabric in the 20g/L NaOH solution, and 95 ℃, take out after 60 minutes, be cooled to room temperature, the use mass fraction is 8% acetic acid neutralization, regulating the pH value is 6.5-7.5, clean with the running water rinsing.
(3) absorption is put into the aqueous solution that 1.0mol/L nitrogen containing polymer monomer-aniline and 1.0mol/L DBSA are formed with the fabric after the alligatoring, and temperature is 95 ℃, and concussion absorption 60 minutes is dried after taking out naturally.
(4) in-situ polymerization with 8S in the aqueous solution of immersion 0.5mol/L ammonium persulfate of the fabric after the absorption and 0.5mol/L DBSA, is 1.0Kg/cm at pressure
2Padding machine on pad, and under 0 ℃ environment, continue reaction, obtain being covered with the fabric of nitrogen containing polymer.
(5) sensitization is put into the nylon fabric of washing that is covered with polyaniline the aqueous solution that 15g/L stannous chloride and 60ml/L hydrochloric acid forms and is carried out sensitization and handle, and temperature is 35 ℃, takes out rinsing 2～3 times after 10 minutes.
(6) chemical silvering under action of ultrasonic waves, is put into the silver plating bath plating with the fabric after the sensitization.Consisting of of chemical plating liquid: silver nitrate: 12g/L; Ammoniacal liquor: 80ml/L; NaOH:8g/L; Glucose: 2.6g/L; 30 ℃ of temperature, 40 minutes time.
Test shows, the resistance of the surface side of fabric is 9～14m Ω/sq, and electromagnet shield effect reaches more than the 60dB, and the electric conductivity and the capability of electromagnetic shielding of fabric are good, and have kept the original characteristic of fabric, and be soft, and rub resistance and washing fastness are good.
Embodiment 3
Present embodiment adopts woven dacron
(1) oil removing is put into the 30g/L water-detergent solution with fabric and soaked, and temperature is 50 ℃, takes out after 20 minutes, and is clean with the running water rinsing.
(2) alligatoring is immersed fabric in the 30g/LNaOH solution, and 85 ℃, take out after 70 minutes, be cooled to room temperature, using mass fraction is that regulating the pH value is 6.5-7.5, clean with the running water rinsing in 10% the acetic acid.
(3) absorption is put into the aqueous solution that 0.7mol/L nitrogen containing polymer monomer-pyrroles and 0.7mol/L DBSA are formed with the fabric after the alligatoring, and temperature is 85 ℃, and concussion absorption 65 minutes is dried after taking out naturally.
(4) in-situ polymerization with 10S in the aqueous solution of immersion 0.35mol/L ammonium persulfate of the fabric after the absorption and 0.35mol/L DBSA, is 1.5Kg/cm at pressure
2Padding machine on pad, and under 0 ℃ environment, continue reaction, obtain being covered with the fabric of nitrogen containing polymer.
(5) sensitization, the aqueous solution of the dacron that is covered with polypyrrole being put into 12g/L stannous chloride and 48ml/L hydrochloric acid composition carries out the sensitization processing, and temperature is 25 ℃, takes out rinsing 2～3 times after 15 minutes.
(6) chemical silvering under action of ultrasonic waves, is put into the silver plating bath plating with the fabric after the sensitization.Consisting of of chemical plating liquid: silver nitrate: 10g/L; Ammoniacal liquor: 70ml/L; NaOH:7g/L; Glucose: 2.4g/L; 30 ℃ of temperature, 35 minutes time.
Test shows, the resistance of the surface side of fabric is 14～20m Ω/sq, and electromagnet shield effect reaches more than the 60dB, and the electric conductivity and the capability of electromagnetic shielding of fabric are good, and have kept the original characteristic of fabric, and be soft, and rub resistance and washing fastness are good.
Embodiment 4
Present embodiment adopts woven dacron
(1) oil removing is put into the 15g/L water-detergent solution with fabric and soaked, and temperature is 40 ℃, takes out after 30 minutes, and is clean with the running water rinsing.
(2) alligatoring is immersed fabric in the 15g/L NaOH solution, and 80 ℃, take out after 70 minutes, be cooled to room temperature, the use mass fraction is 5% acetic acid neutralization, regulating the pH value is 6.5-7.5, clean with the running water rinsing.
(3) absorption is put into the aqueous solution that 1.0mol/L nitrogen containing polymer monomer-aniline and 1.0mol/L hydrochloric acid are formed with the fabric after the alligatoring, and temperature is 95 ℃, and concussion absorption 60 minutes is dried after taking out naturally.
(4) in-situ polymerization immerses 10S in 0.5mol/L ammonium persulfate and the 0.5mol/L aqueous solution of hydrochloric acid with the fabric after the absorption, is 2.0Kg/cm at pressure
2Padding machine on pad, and under 0 ℃ environment, continue reaction, obtain being covered with the fabric of nitrogen containing polymer.
(5) sensitization, the aqueous solution of the dacron that is covered with polyaniline being put into 15g/L stannous chloride and 60ml/L hydrochloric acid composition carries out the sensitization processing, and temperature is 30 ℃, takes out rinsing 2～3 times after 15 minutes.
(6) chemical silvering is put into the silver plating bath plating with the fabric after the sensitization.Consisting of of chemical plating liquid: silver nitrate: 8g/L; Ammoniacal liquor: 60ml/L; NaOH:6g/L; Glucose: 2.2g/L; 30 ℃ of temperature, 30 minutes time.
Test shows, the resistance of the surface side of fabric is 22～28m Ω/sq, and electromagnet shield effect reaches more than the 60dB, and the electric conductivity and the capability of electromagnetic shielding of fabric are good, and have kept the original characteristic of fabric, and be soft, and rub resistance and washing fastness are good.
Claims (10)
1. preparation method via nitrogenous conducting polymer silver coating fabric comprises:
(1) fabric is immersed in the water-detergent solution of 10～40g/L, the taking-up rinsing is clean after flooding 10～40 minutes under 30 ℃～60 ℃;
(2) fabric of step (1) gained is put into the coarsening solution alligatoring, 70 ℃～100 ℃ down concussion take out after 30～80 minutes, be cooled to room temperature, uses glacial acetic acid to regulate pH value and is 6.5-7.5, rinsing is clean then, dries, and gets the fabric after the alligatoring;
(3) fabric after the above-mentioned alligatoring is put into the Bronsted acid solution of nitrogen containing polymer monomer, under 70 ℃～100 ℃, concussion absorption was taken out after 50～120 minutes, dried;
(4) the textile impregnation 5～15S in the oxidation liquid of being made up of ammonium persulfate and Bronsted acid that step (3) is obtained is then in 0.5～2.5Kg/cm
2Pressure under pad, and under 0 ℃ environment, continue reaction, obtain being covered with the fabric of nitrogen containing polymer;
(5) the above-mentioned fabric that is covered with nitrogen containing polymer is put into contained stannous chloride and aqueous solution of hydrochloric acid, under 20～50 ℃, shake that to take out rinsing after 5～30 minutes clean;
The pH value of (6) regulating silver plating reaction liquid is 10～11, and the fabric that step (5) is obtained is immersed in the said silver plating reaction liquid, and 30～35 ℃ of following ultrasonic reactions take out rinsing after 20～60 minutes clean, promptly gets.
2. a kind of preparation method via nitrogenous conducting polymer silver coating fabric according to claim 1 is characterized in that: the fabric described in the step (1) is woven dacron, POLYAMIDE FABRIC, wash a kind of in the bright and beautiful cloth.
3. a kind of preparation method via nitrogenous conducting polymer silver coating fabric according to claim 1 is characterized in that: the coarsening solution described in the step (2) is the NaOH of 10～40g/L.
4. a kind of preparation method via nitrogenous conducting polymer silver coating fabric according to claim 1 is characterized in that: the adjusting pH value described in the step (2) is 3%～12% acetic acid adjusting for the use mass fraction.
5. a kind of preparation method via nitrogenous conducting polymer silver coating fabric according to claim 1 is characterized in that: the nitrogen containing polymer monomer described in the step (3) is aniline or pyrroles, and nitrogen containing polymer is polyaniline or polypyrrole.
6. a kind of preparation method via nitrogenous conducting polymer silver coating fabric according to claim 1 is characterized in that: the Bronsted acid described in step (3) and (4) is a kind of in hydrochloric acid, nitric acid, the DBSA.
7. a kind of preparation method according to claim 1 via nitrogenous conducting polymer silver coating fabric; It is characterized in that: the nitrogen containing polymer monomer concentration is 0.5～1.5mol/L in the Bronsted acid solution of the nitrogen containing polymer monomer described in the step (3), and the concentration of Bronsted acid is 0.5～1.5mol/L in the Bronsted acid solution of nitrogen containing polymer monomer.
8. a kind of preparation method according to claim 1 via nitrogenous conducting polymer silver coating fabric; It is characterized in that: ammonium persulfate concentration 0.2～0.8mol/L in the oxidation liquid described in the step (4), the concentration of Bronsted acid is 0.2～0.8mol/L in the oxidation liquid.
9. a kind of preparation method according to claim 1 via nitrogenous conducting polymer silver coating fabric; It is characterized in that: containing in stannous chloride and the aqueous solution of hydrochloric acid described in the step (5); The concentration of stannous chloride is 5～30g/L, and the concentration of hydrochloric acid is 20ml/L～120ml/L.
10. a kind of preparation method via nitrogenous conducting polymer silver coating fabric according to claim 1 is characterized in that: AgNO in the silver-colored reactant liquor described in the step (6)
3Concentration be 8～15g/L, the concentration of ammoniacal liquor is 50～130ml/L, the concentration of NaOH is 5～12g/L, glucose or concentration of sucrose are 2～4g/L.
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| CN105780493A (en) * | 2016-04-19 | 2016-07-20 | 东华大学 | Making method of cotton fabric having conductive and electromagnetic shielding properties |
| CN106183250A (en) * | 2016-07-08 | 2016-12-07 | 东华大学 | A kind of radioprotective sunshade fabric and preparation method thereof |
| CN110093777A (en) * | 2019-05-23 | 2019-08-06 | 余晨 | A kind of industrialized process for preparing of conductive fiber |
| CN110184808A (en) * | 2019-06-12 | 2019-08-30 | 苏州福洹纺织科技有限公司 | A kind of fire-retardant, anti-oxidant, electromagnetic wave shielding PIPD fabric preparation method |
| CN115613014A (en) * | 2022-10-17 | 2023-01-17 | 河北省纺织科学研究所 | Method for chemically plating silver on aramid fabric |
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Application publication date: 20120620 |