CN104695212A - Preparation method of electromagnetic shielding fabric - Google Patents
Preparation method of electromagnetic shielding fabric Download PDFInfo
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- CN104695212A CN104695212A CN201510123696.1A CN201510123696A CN104695212A CN 104695212 A CN104695212 A CN 104695212A CN 201510123696 A CN201510123696 A CN 201510123696A CN 104695212 A CN104695212 A CN 104695212A
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Abstract
The invention discloses a preparation method of an electromagnetic shielding fabric. The preparation method comprises the following specific operation steps: roughening; sensitizing; activating; performing chemical plating; cleaning; drying. The preparation method is easy and feasible, no pollution is caused in the preparation process, the preparation cost is low, and the prepared electromagnetic shielding fabric has the advantages of light weight, durability, wide shielding frequency, good comprehensive performance and the like.
Description
Technical field
The invention belongs to the preparation field of textiles, be specifically related to a kind of preparation method of Electromagnetically shielding fabrics.
Background technology
Along with the fast development of society, atmosphere pollution, water pollutions and noise pollution bring increasing harm, cause the extensive attention of people.People improve the environment outside our body by decreasing pollution gas purging, the means such as sewage disposal system and reduction noise decibel of improving, build harmonious living space.But, along with the fast development of electronic technology, create a kind of invisible pollution-electromagnetic interference newly.Electromagnetic radiation not only can disturb the operation of electric equipment and the transmitting-receiving of wireless signal, goes back grievous injury and health, is the pollution of a kind of " cannot see, can't smell, can not touch ".
The metal of conduction can produce reflection to electromagnetic wave, absorbs and negative function, thus plays the effect reducing electromagenetic wave radiation.Metallized fabrics is one of important kind of electromagnetic shielding fabric, and the approach realizing metallization of fabric at present mainly contains metal fibre blending, chemical plating and top finish.Wherein, chemical plating simply, easily realizes because of its technique, and its fabric not only has the performance such as conduction, magnetic conduction, electrical shielding of metal, and ventilative, soft, drapability is good, be widely used in the preparation of electromagnetic shielding fabric.
The electromagnetic shielding efficiency of metal fibre BLENDED FABRIC is low in the market, thickness is large, range of application is narrow.The electroless copper technology that chemical plating Electromagnetically shielding fabrics wherein uses is all using formaldehyde as reductant, and formaldehyde volatility and toxicity are comparatively strong, and solution is unstable, and maintenance difficulties is large.The production technology that the inferior sodium phosphate of the nontoxic pollution-free of present use makees reductant is extensively studied, but its electroless copper activating process difficulty, coating loosens, metal is combined the problem such as loosely and limits its industrialized enforcement with fabric, find to have higher complexing power and the catalytic metal support being easy to film forming is the problem that the art worker needs solution badly.
Summary of the invention
Technical problem to be solved by this invention is, for the shortcoming that above prior art exists, a kind of preparation method of Electromagnetically shielding fabrics is proposed, this preparation method is simple, pollution-free in preparation process, preparation cost is cheap, the advantages such as the Electromagnetically shielding fabrics light durable prepared, screening frequencies are wide, good combination property.
The technical scheme that the present invention solves above technical problem is:
A preparation method for Electromagnetically shielding fabrics, preparation method's concrete operation step is as follows: alligatoring → sensitization → activation → chemical plating → cleaning → oven dry
(1) alligatoring
(1) fabric being immersed in mass fraction is in the sodium hydroxide solution of 10%, bath raio 1:40,70-80 DEG C, process fabric under 30-40min condition, then use distilled water rinsed clean;
(2) fabric of above-mentioned rinsed clean is carried out plasma treatment;
Wherein, plasma processing condition is air-treatment 20min at ambient pressure, and distance between plates is 4-6mm, and power is 60W;
(2) sensitization
Get nickelous sulfate and citric acid, dissolve mixing respectively with a small amount of distilled water, then add water to concentration and be respectively 20g/L and 5g/L, bath raio is 20:1-30:1, takes out after sensitization 10-20min, prepares activation by distilled water rinsing post-drying
(3) activate
(1) dissolve palladium bichloride with concentrated hydrochloric acid, dilution, is made into the palladium chloride solution that concentration is 2g/L (in palladium);
(2) get the dendritic Polymer Solution of polyamidoamine to be dropwise added in palladium chloride solution, regulate PH in alkalescence with NaOH in whipping process, then constant volume is mixed with the activating solution that palladium ion concentration is 0.1g/L;
(3) carry out activation to fabric to arrange: two leachings two are pricked, pick-up rate is 40%, 100 DEG C dries 3-5min;
(4) the fabric thing through padding process is immersed 30-40min in the borohydride solution of 3-5g/L;
(5) by above-mentioned through padding the fabric washed with de-ionized water processed, dry;
(4) chemical plating
(1) carry out copper plating treatment by fabric good for activation processing immersion chemical plating fluid, wherein solution formula is, main salt 6-10g/L, secondary salt 1-3 g/L, reductant 30-40 g/L, solution buffer 25-30 g/L, main complexant 15-20 g/L, side reaction inhibitor 5-10 mL/L, adjustment pH is 8-10, temperature 50-60 DEG C, electroless plating time is 20-40min; bath raio is 1:50-1:100, then washes fabric, dries in the vacuum drying chamber of 30-40 DEG C;
Wherein, main salt be copper sulphate, secondary salt is nickelous sulfate, and reductant is inferior sodium phosphate, and solution buffer is boric acid, and main complexant is trisodium citrate, and side reaction inhibitor is ethanol;
(2) put in alkaline electroless plating nickel solution by the fabric that above-mentioned copper plating treatment is good, carry out plating nickel on surface process, reaction condition is: pH is 8.5-9.5, and temperature is 40-50 DEG C, and bath raio is 1:50-1:100;
Wherein, becoming of chemical nickel-plating solution: main salt nickelous sulfate, concentration is 20-25 g/L, reductant sodium hypophosphite, and concentration is 30-45 g/L, and complexing agent is natrium citricum, and concentration is 15-25 g/L, and buffer is ammonium chloride, and concentration is 10-20 g/L;
(5) clean
By the fabric washed with de-ionized water 5-8 time that above-mentioned steps (four) is handled well;
(6) dry
The fabric cleaned up is put into vacuum drying chamber and dries 4-5h, bake out temperature is 45-60 DEG C.
The further technical scheme of the present invention is:
In the preparation method of aforementioned electromagnetic loomage, dendritic high molecular preparation method is as follows for polyamidoamine:
(1) ethylenediamine and methyl alcohol are joined in the there-necked flask with magnetic agitation, reflux condensing tube and thermometer, under 25 DEG C of stirring conditions, start to drip methyl acrylate, reaction 24h, at 22 DEG C, carry out decompression distillation under the pressure of 133Pa, removing solvent methanol and excessive methyl acrylate, obtain the dendritic macromolecule of half PAMAM type;
Wherein, the mol ratio of ethylenediamine, methyl alcohol, methyl acrylate is 6:3:1;
(2) the dendritic macromolecule of half PAMAM type and methyl alcohol are joined in the there-necked flask with magnetic agitation, reflux condensing tube and thermometer, under 25 DEG C of stirring conditions, start to drip ethylenediamine, reaction 24h, at 72 DEG C, decompression distillation under the pressure of 133Pa, removing solvent methanol and excessive ethylenediamine, obtain the dendritic macromolecule of polyamidoamine;
Wherein, the mol ratio of the dendritic macromolecule of half PAMAM type, methyl alcohol, ethylenediamine is 1.5:10:12.
The invention has the beneficial effects as follows:
(1) Electromagnetically shielding fabrics that prepared by the present invention has the advantages such as cost is low, pollution-free, light durable, screening frequencies are wide, good combination property.
(2) adopt the NaOH of low concentration and plasma technology to carry out alligatoring to fabric in the present invention, fabric fibre can be made roughening, under pollution, do not affect the mechanical performance of fabric.
(3) Electromagnetically shielding fabrics prepared in the present invention has copper facing and nickel plating two kinds of metals simultaneously, has anti-electromagnetism effective, and solves the problem of metallic catalyst and fabric binding ability difference in conventional preparation techniques preferably.
(4) the dendritic macromolecule of the polyamidoamine prepared in the present invention, containing more amino, imino group in this high polymer, dendritic for polyamidoamine macromolecule and palladium are carried out Absorptive complex wave, pre-treatment is carried out to fabric, due to high complexing and the easy film forming of amine dendrimer, precious metal palladium is fixedly secured to be treated on plated fabric, causes the electroless copper reaction of fabric face, eliminates the activation process of very complicated in tradition preparation.
(5) method that the present invention carrys out preparative chemistry plating conductive fabric using dendrimer as palladium activated carrier has easy to operate, environmental protection, advantage energy-conservation, with low cost, easily realize industrialization to produce, and the conductive fabric coating of preparation is evenly glossy, has good conductive capability and taking.
(6) coating prepared of the present invention and fabric fibre have good adhesion, difficult drop-off, and fabric rub resistance.Water-wash resistance is good, and service life is longer, and its original drapability, gas permeability all tensile strength are only subject to minimal effect.
(7) dendrimer prepared in the present invention, has powerful complexing power and easily molten, easy filming performance significantly improves active mass, simplify the operation step, realizes effective control of activation process, is conducive to large-scale production.
(8) concentration of palladium ion solution has been reduced to 0.1 g/L by the present invention in fabric pretreatment, and in the preparation of traditional chemical copper facing fabric, palladium ion concentration lower than the standard of 1 g/L, can not have been saved cost, improve efficiency greatly.
Detailed description of the invention
embodiment 1
The present embodiment provides a kind of preparation method of Electromagnetically shielding fabrics, and preparation method's concrete operation step is as follows: alligatoring → sensitization → activation → chemical plating → cleaning → oven dry;
(1) alligatoring
(1) fabric being immersed in mass fraction is in the sodium hydroxide solution of 10%, bath raio 1:40,70 DEG C, process fabric under 30min condition, then use distilled water rinsed clean;
(2) fabric of above-mentioned rinsed clean is carried out plasma treatment;
Wherein, plasma processing condition is air-treatment 20min at ambient pressure, and distance between plates is 4mm, and power is 60W;
(2) sensitization
Get nickelous sulfate and citric acid, dissolve mixing respectively with a small amount of distilled water, then add water to concentration and be respectively 20g/L and 5g/L, bath raio is 20:1, takes out after sensitization 10min, prepares activation by distilled water rinsing post-drying;
(3) activate
(1) dissolve palladium bichloride with concentrated hydrochloric acid, dilution, is made into the palladium chloride solution that concentration is 2g/L (in palladium);
(2) get the dendritic Polymer Solution of polyamidoamine to be dropwise added in palladium chloride solution, regulate PH in alkalescence with NaOH in whipping process, then constant volume is mixed with the activating solution that palladium ion concentration is 0.1g/L;
(3) carry out activation to fabric to arrange: two leachings two are pricked, pick-up rate is 40%, 100 DEG C dries 3min;
(4) the fabric thing through padding process is immersed 30min in the borohydride solution of 3g/L;
(5) by above-mentioned through padding the fabric washed with de-ionized water processed, dry;
(4) chemical plating
(1) carry out copper plating treatment by fabric good for activation processing immersion chemical plating fluid, wherein solution formula is, main salt 6g/L, secondary salt 1g/L, reductant 30 g/L, solution buffer 25g/L, main complexant 15g/L, side reaction inhibitor 5mL/L, regulates pH to be 8, temperature 50 C, electroless plating time is 20min; bath raio is 1:50, then washes fabric, dries in the vacuum drying chamber of 30 DEG C;
Wherein, main salt is copper sulphate, and secondary salt is nickelous sulfate, and reductant is inferior sodium phosphate, and solution buffer is boric acid, and main complexant is trisodium citrate, and side reaction inhibitor is ethanol;
(3) put in alkaline electroless plating nickel solution by the fabric that above-mentioned copper plating treatment is good, carry out plating nickel on surface process, reaction condition is: pH is 8.5, and temperature is 40 DEG C, and bath raio is 1:50;
Wherein, becoming of chemical nickel-plating solution: main salt nickelous sulfate, concentration is 20g/L, reductant sodium hypophosphite, and concentration is 30 g/L, and complexing agent is natrium citricum, and concentration is 15g/L, and buffer is ammonium chloride, and concentration is 10 g/L;
(5) clean
The fabric washed with de-ionized water that above-mentioned steps (four) is handled well 5 times;
(6) dry
The fabric cleaned up is put into vacuum drying chamber and dries 4h, bake out temperature is 45 DEG C.
embodiment 2
The present embodiment provides a kind of preparation method of Electromagnetically shielding fabrics, and preparation method's concrete operation step is as follows: alligatoring → sensitization → activation → chemical plating → cleaning → oven dry;
(1) alligatoring
(1) fabric being immersed in mass fraction is in the sodium hydroxide solution of 10%, bath raio 1:40,80 DEG C, process fabric under 40min condition, then use distilled water rinsed clean;
(2) fabric of above-mentioned rinsed clean is carried out plasma treatment;
Wherein, plasma processing condition is air-treatment 20min at ambient pressure, and distance between plates is 6mm, and power is 60W;
(2) sensitization
Get nickelous sulfate and citric acid, dissolve mixing respectively with a small amount of distilled water, then add water to concentration and be respectively 20g/L and 5g/L, bath raio is 30:1, takes out after sensitization 20min, prepares activation by distilled water rinsing post-drying;
(3) activate
(1) dissolve palladium bichloride with concentrated hydrochloric acid, dilution, is made into the palladium chloride solution that concentration is 2g/L (in palladium);
(2) get the dendritic Polymer Solution of polyamidoamine to be dropwise added in palladium chloride solution, regulate PH in alkalescence with NaOH in whipping process, then constant volume is mixed with the activating solution that palladium ion concentration is 0.1g/L;
(3) carry out activation to fabric to arrange: two leachings two are pricked, pick-up rate is 40%, 100 DEG C dries 5min;
(4) the fabric thing through padding process is immersed 40min in the borohydride solution of 5g/L;
(5) by above-mentioned through padding the fabric washed with de-ionized water processed, dry;
(4) chemical plating
(1) carry out copper plating treatment by fabric good for activation processing immersion chemical plating fluid, wherein solution formula is, main salt 10g/L, secondary salt 3g/L, reductant 40 g/L, solution buffer 30 g/L, main complexant 20 g/L, side reaction inhibitor 10 mL/L, regulates pH to be 10, temperature 60 C, electroless plating time is 40min; bath raio is 1:100, then washes fabric, dries in the vacuum drying chamber of 40 DEG C;
Wherein, main salt is copper sulphate, and secondary salt is nickelous sulfate, and reductant is inferior sodium phosphate, and solution buffer is boric acid, and main complexant is trisodium citrate, and side reaction inhibitor is ethanol;
(3) put in alkaline electroless plating nickel solution by the fabric that above-mentioned copper plating treatment is good, carry out plating nickel on surface process, reaction condition is: pH is 8.5-9.5, and temperature is 40-50 DEG C, and bath raio is 1:50-1:100;
Wherein, becoming of chemical nickel-plating solution: main salt nickelous sulfate, concentration is 25 g/L, reductant sodium hypophosphite, and concentration is 45 g/L, and complexing agent is natrium citricum, and concentration is 25 g/L, and buffer is ammonium chloride, and concentration is 20 g/L;
(5) clean
The fabric washed with de-ionized water that above-mentioned steps (four) is handled well 8 times;
(6) dry
The fabric cleaned up is put into vacuum drying chamber and dries 5h, bake out temperature is 60 DEG C.
embodiment 3
The present embodiment provides a kind of preparation method of Electromagnetically shielding fabrics, and preparation method's concrete operation step is as follows: alligatoring → sensitization → activation → chemical plating → cleaning → oven dry;
(1) alligatoring
(1) fabric being immersed in mass fraction is in the sodium hydroxide solution of 10%, bath raio 1:40,75 DEG C, process fabric under 35min condition, then use distilled water rinsed clean;
(2) fabric of above-mentioned rinsed clean is carried out plasma treatment;
Wherein, plasma processing condition is air-treatment 20min at ambient pressure, and distance between plates is 5mm, and power is 60W;
(2) sensitization
Get nickelous sulfate and citric acid, dissolve mixing respectively with a small amount of distilled water, then add water to concentration and be respectively 20g/L and 5g/L, bath raio is 25:1, takes out after sensitization 15min, prepares activation by distilled water rinsing post-drying;
(3) activate
(1) dissolve palladium bichloride with concentrated hydrochloric acid, dilution, is made into the palladium chloride solution that concentration is 2g/L (in palladium);
(2) get the dendritic Polymer Solution of polyamidoamine to be dropwise added in palladium chloride solution, regulate PH in alkalescence with NaOH in whipping process, then constant volume is mixed with the activating solution that palladium ion concentration is 0.1g/L;
(3) carry out activation to fabric to arrange: two leachings two are pricked, pick-up rate is 40%, 100 DEG C dries 4min;
(4) the fabric thing through padding process is immersed 35min in the borohydride solution of 4g/L;
(5) by above-mentioned through padding the fabric washed with de-ionized water processed, dry;
(4) chemical plating
(1) carry out copper plating treatment by fabric good for activation processing immersion chemical plating fluid, wherein solution formula is, main salt 8g/L, secondary salt 2g/L, reductant 35g/L, solution buffer 28g/L, main complexant 17 g/L, side reaction inhibitor 8mL/L, regulates pH to be 9, temperature 55 DEG C, electroless plating time is 30min; bath raio is 1:75, then washes fabric, dries in the vacuum drying chamber of 35 DEG C;
Wherein, main salt is copper sulphate, and secondary salt is nickelous sulfate, and reductant is inferior sodium phosphate, and solution buffer is boric acid, and main complexant is trisodium citrate, and side reaction inhibitor is ethanol;
(3) put in alkaline electroless plating nickel solution by the fabric that above-mentioned copper plating treatment is good, carry out plating nickel on surface process, reaction condition is: pH is 9, and temperature is 45 DEG C, and bath raio is 1:75;
Wherein, becoming of chemical nickel-plating solution: main salt nickelous sulfate, concentration is 22g/L, reductant sodium hypophosphite, and concentration is 40 g/L, and complexing agent is natrium citricum, and concentration is 20g/L, and buffer is ammonium chloride, and concentration is 15g/L;
(5) clean
The fabric washed with de-ionized water that above-mentioned steps (four) is handled well 7 times;
(6) dry
The fabric cleaned up is put into vacuum drying chamber and dries 4h, bake out temperature is 50 DEG C.
embodiment 4
In above-described embodiment 1-3, the dendritic high molecular preparation method of polyamidoamine is as follows:
(1) ethylenediamine and methyl alcohol are joined in the there-necked flask with magnetic agitation, reflux condensing tube and thermometer, under 25 DEG C of stirring conditions, start to drip methyl acrylate, reaction 24h, at 22 DEG C, carry out decompression distillation under the pressure of 133Pa, removing solvent methanol and excessive methyl acrylate, obtain the dendritic macromolecule of half PAMAM type;
Wherein, the mol ratio of ethylenediamine, methyl alcohol, methyl acrylate is 6:3:1;
(2) the dendritic macromolecule of half PAMAM type and methyl alcohol are joined in the there-necked flask with magnetic agitation, reflux condensing tube and thermometer, under 25 DEG C of stirring conditions, start to drip ethylenediamine, reaction 24h, at 72 DEG C, decompression distillation under the pressure of 133Pa, removing solvent methanol and excessive ethylenediamine, obtain the dendritic macromolecule of polyamidoamine;
Wherein, the mol ratio of the dendritic macromolecule of half PAMAM type, methyl alcohol, ethylenediamine is 1.5:10:12.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of application claims.
Claims (2)
1. a preparation method for Electromagnetically shielding fabrics, is characterized in that, described preparation method's concrete operation step is as follows: alligatoring → sensitization → activation → chemical plating → cleaning → oven dry;
(1) alligatoring
(1) fabric being immersed in mass fraction is in the sodium hydroxide solution of 10%, bath raio 1:40,70-80 DEG C, process fabric under 30-40min condition, then use distilled water rinsed clean;
(2) fabric of above-mentioned rinsed clean is carried out plasma treatment;
Wherein, described plasma processing condition is air-treatment 20min at ambient pressure, and distance between plates is 4-6mm, and power is 60W;
(2) sensitization
Get nickelous sulfate and citric acid, dissolve mixing respectively with a small amount of distilled water, then add water to concentration and be respectively 20g/L and 5g/L, bath raio is 20:1-30:1, takes out after sensitization 10-20min, prepares activation by distilled water rinsing post-drying;
(3) activate
(1) dissolve palladium bichloride with concentrated hydrochloric acid, dilution, is made into the palladium chloride solution that concentration is 2g/L (in palladium);
(2) get the dendritic Polymer Solution of polyamidoamine to be dropwise added in palladium chloride solution, regulate PH in alkalescence with NaOH in whipping process, then constant volume is mixed with the activating solution that palladium ion concentration is 0.1g/L;
(3) carry out activation to fabric to arrange: two leachings two are pricked, pick-up rate is 40%, 100 DEG C dries 3-5min;
(4) the fabric thing through padding process is immersed 30-40min in the borohydride solution of 3-5g/L;
(5) by above-mentioned through padding the fabric washed with de-ionized water processed, dry;
(4) chemical plating
(1) carry out copper plating treatment by fabric good for activation processing immersion chemical plating fluid, wherein solution formula is, main salt 6-10g/L, secondary salt 1-3 g/L, reductant 30-40 g/L, solution buffer 25-30 g/L, main complexant 15-20 g/L, side reaction inhibitor 5-10 mL/L, adjustment pH is 8-10, temperature 50-60 DEG C, electroless plating time is 20-40min; bath raio is 1:50-1:100, then washes fabric, dries in the vacuum drying chamber of 30-40 DEG C;
Wherein, described main salt is copper sulphate, and secondary salt is nickelous sulfate, and described reductant is inferior sodium phosphate, and described solution buffer is boric acid, and described main complexant is trisodium citrate, and described side reaction inhibitor is ethanol;
(2) put in alkaline electroless plating nickel solution by the fabric that above-mentioned copper plating treatment is good, carry out plating nickel on surface process, reaction condition is: pH is 8.5-9.5, and temperature is 40-50 DEG C, and bath raio is 1:50-1:100;
Wherein, becoming of described chemical nickel-plating solution: main salt nickelous sulfate, concentration is 20-25 g/L, reductant sodium hypophosphite, and concentration is 30-45 g/L, and complexing agent is natrium citricum, and concentration is 15-25 g/L, and buffer is ammonium chloride, and concentration is 10-20 g/L;
(5) clean
By the fabric washed with de-ionized water 5-8 time that above-mentioned steps (four) is handled well;
(6) dry
The fabric cleaned up is put into vacuum drying chamber and dries 4-5h, bake out temperature is 45-60 DEG C.
2. the preparation method of the Electromagnetically shielding fabrics according to claim, is characterized in that, dendritic high molecular preparation method is as follows for described polyamidoamine:
(1) ethylenediamine and methyl alcohol are joined in the there-necked flask with magnetic agitation, reflux condensing tube and thermometer, under 25 DEG C of stirring conditions, start to drip methyl acrylate, reaction 24h, at 22 DEG C, carry out decompression distillation under the pressure of 133Pa, removing solvent methanol and excessive methyl acrylate, obtain the dendritic macromolecule of half PAMAM type;
Wherein, the mol ratio of described ethylenediamine, methyl alcohol, methyl acrylate is 6:3:1;
(2) the dendritic macromolecule of half PAMAM type and methyl alcohol are joined in the there-necked flask with magnetic agitation, reflux condensing tube and thermometer, under 25 DEG C of stirring conditions, start to drip ethylenediamine, reaction 24h, at 72 DEG C, decompression distillation under the pressure of 133Pa, removing solvent methanol and excessive ethylenediamine, obtain the dendritic macromolecule of polyamidoamine;
Wherein, the mol ratio of the dendritic macromolecule of described half PAMAM type, methyl alcohol, ethylenediamine is 1.5:10:12.
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