CN103485171B - Non-target spray activation method for fabric chemical plating - Google Patents
Non-target spray activation method for fabric chemical plating Download PDFInfo
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- CN103485171B CN103485171B CN201310430997.XA CN201310430997A CN103485171B CN 103485171 B CN103485171 B CN 103485171B CN 201310430997 A CN201310430997 A CN 201310430997A CN 103485171 B CN103485171 B CN 103485171B
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Abstract
The invention discloses a non-target spray activation method for fabric chemical plating, and belongs to the non-metallic material chemical plating technology. According to the invention, a nickel sulfate acid solution is atomized into liquid drops firstly through an atomization method, and deposited on the surface of the fabric, a sodium borohydride alkaline solution is atomized into liquid drops and reacts with nickel sulfate deposited on the fabric so as to produce nickel particles with catalytic activity, and then the chemical plating is performed. The activation method has the advantages that the activation method is simple, the raw materials are low in cost, the cross contamination of the solutions can be avoided, and the method can be applied to large-scale continuous production. Compared with the metal conductive fabric prepared through other activation methods, the metal conductive fabric prepared through the activation method disclosed by the invention has the advantages that the adhesive force between the metal layer of the fabric and the fabric substrate is strong, and the prominent abrasive resistance and washing fastness are achieved. The chemical plating metal fabric prepared through the preparation method has excellent electrical conductivity, electromagnetic shielding performance and flexibility, can be widely used for sensors, antistatic, antibacterial and radiation-proof clothes and special fields, such as military and national defense.
Description
Technical field
The present invention relates to a kind of textile chemistry plating without palladium atomizing activating method, belong to chemical plating of non-metal material technology.
Background technology
Metallized fabrics, as electromagnet compatible material, has the electric conductivity of metal concurrently, the softness of electromagnetic wave shielding and textiles, ventilating performance, be one of emerging and broad-spectrum shielding material, can national defence be widely used in, space flight, aviation, electronics, electric power, communication, field and the departments such as medical treatment.
Because fabric face does not have catalytic activity, making it form one deck active centre so carry out preliminary treatment to fabric before chemical plating, is the key of chemically plating for metallized fabrics.Traditional fabric activation method adopts SnCl2-PdCl2 sensitization-activation method, and the method processing step is complicated, and PdCl2 is expensive and poisonous, causes severe contamination to human body and environment.Textile journal, 2006,27(1): 34-37, article name (being applied to the new activation method [J] of textile chemistry plating), this article discloses the sodium borohydride reduction nickelous sulfate utilizing cotton to adsorb, the elemental nickel restored is adsorbed onto on cotton, thus forms active centre, the method easily causes the cross pollution between solution.Textile journal, 2012, 11:77-80, article name (preparation of nano nickel colloid and the application [J] in textile chemistry plating activation thereof), this article discloses with PVP is stabilizing agent, the nickel particle adopting sodium borohydride reduction nickelous sulfate to prepare in acid condition is catalyst, catalysis inferior sodium phosphate liquid-phase reduction nickelous sulfate, prepare nano nickel colloid, then this colloid is used for the activation procedure of electroless copper, when nano nickel colloid prepared by the method is applied to the chemical fibre class textiless such as polyester, binding strength difference and the problem such as coating is discontinuous between fabric and elemental nickel.
Summary of the invention
For above-mentioned existing problems, the object of the present invention is to provide and a kind ofly adopt the method without palladium atomizing activating: first the nickel sulfate solution of acidity is atomized into hanging drop and is deposited on fabric face, and then alkaline sodium borohydride solution is atomized into hanging drop is deposited on fabric face, and to react the nickel particle restoring and there is catalytic activity with nickelous sulfate, and then carry out chemical plating.For achieving the above object, technical solution of the present invention is:
Textile chemistry plating without a palladium atomizing activating method, described activation method carries out according to the following steps:
The preparation of a activating solution:
At ambient temperature, the hydrochloric acid of to be the nickelous sulfate of 0.02 ~ 0.1g/mL and concentration by concentration be 0.01 ~ 0.05mol/L is made into acid nickel sulfate solution, for subsequent use.
The NaOH of to be the sodium borohydride of 0.005 ~ 0.01g/mL and concentration by concentration be 0.01 ~ 0.05g/mL is made into alkaline sodium borohydride solution, for subsequent use.
The acid nickel sulfate solution loading of preparing through a step is placed with in the first reactor of atomizer by b, being loaded by alkaline sodium borohydride solution is placed with in the 3rd reactor of atomizer, first reactor, the 3rd reactor are inserted in cooling bath respectively, are placed in the second reactor by the fabric cleaned up.
First connect the atomizer in the first reactor and the air-flow bottle opening connection first reactor, making the acid nickel sulfate solution of the first reactor be atomized into hanging drop is equipped with in the second reactor of fabric with air-flow through pipeline importing, to fabric atomization 10 ~ 40min, close the atomizer in the first reactor and the air-flow bottle being connected the first reactor, connect the atomizer in the 3rd reactor and the air-flow bottle opening connection the 3rd reactor, making the alkaline sodium borohydride solution in the 3rd reactor be atomized into hanging drop imports in the second reaction vessel with air-flow through pipeline, atomizer and the air-flow bottle being connected the 3rd reactor in the 3rd reactor is closed to after fabric atomization 10 ~ 40min, take out the fabric in the second reactor, by washed with de-ionized water, fabric after cleaning is put into 60 DEG C of dry 30min of thermostatic drying chamber.
Owing to have employed above technical scheme, a kind of textile chemistry plating of the present invention without palladium atomizing activating method, what adopt is first the nickel sulfate solution of acidity is atomized into hanging drop to be deposited in fabric face and fabric pore, and then the sodium borohydride solution of alkalescence is atomized into hanging drop and reacts with the nickelous sulfate be deposited in fabric face and fabric pore, generate the nickel particle with catalytic activity, between the nickel particle obtained and fabric, there is stronger adhesion.Because fabric has good water imbibition, when acid nickel sulfate solution and alkaline sodium borohydride solution are sprayed onto fabric face with the form of drop, can permeate towards periphery when drop is absorbed by fabric face, thus the uniform pickup of drop at fabric face can be realized when being atomized a small amount of solution, save the consumption of solution, and nickelous sulfate and sodium borohydride cost ratio SnCl2, PdCl2 is low, thus has saved cost of material.Traditional activation method is first sensitization in SnCl2 solution, activate in PdCl2 solution again, the solution of previous step sensitization is easy to take in activated solution like this, seriously cause the pollution of activated solution, the present invention adopts the method for acid nickel sulfate solution and alkaline sodium borohydride solution being carried out to spray atomization, not only reduce the pollution of heavy metal, it also avoid the cross pollution between solution.The present invention be atomized restore have interaction force between nickel particle and fabric, so the absorption affinity between the metal level prepared in follow-up chemical plating and fabric is strong, obviously can improve the ABRASION RESISTANCE of metallized fabrics, washing resistance.Activation method of the present invention is simple, is suitable for large-scale continuous production.The chemical plating metal fabric prepared by activation method of the present invention has good electric conductivity, electromagnetic wave shielding, pliability, can be widely used in sensor, antistatic, antibacterial, reflects and absorbs ultraviolet and infrared ray, exposure suit and military affairs, the special dimensions such as national defence.
accompanying drawing illustrates:
Accompanying drawing is atomizing activating reaction principle schematic diagram of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, the invention will be further described, sees accompanying drawing.
Textile chemistry plating without a palladium atomizing activating method, described activation method carries out according to the following steps:
The preliminary treatment of a fabric:
Fabric is processed 60min in the sodium hydroxide solution of 20g/L under the condition of 90 DEG C, then cleans up, dry for standby.
The preparation of b activating solution:
At ambient temperature, the hydrochloric acid of to be the nickelous sulfate of 0.02 ~ 0.1g/mL and concentration by concentration be 0.01 ~ 0.05mol/L is made into acid nickel sulfate solution, for subsequent use.
The NaOH of to be the sodium borohydride of 0.005 ~ 0.01g/mL and concentration by concentration be 0.01 ~ 0.05g/mL is made into alkaline sodium borohydride solution, for subsequent use.
The acid nickel sulfate solution loading of preparing through a step is placed with in the first reactor 1 of atomizer by c, being loaded by alkaline sodium borohydride solution is placed with in the 3rd reactor 3 of atomizer, first reactor 1, the 3rd reactor 3 are inserted in cooling bath respectively, the fabric 5 cleaned up is placed in the second reactor the 2, four reactor 4 for collecting the remaining liquid of reaction.First connect the atomizer in the first reactor 1 and the air-flow bottle opening connection first reactor 1, gas in air-flow bottle can adopt nitrogen or air, making the acid nickel sulfate solution in the first reactor 1 be atomized into hanging drop is equipped with in the second reactor 2 of fabric 5 with air-flow through pipeline importing, 10 ~ 40min is atomized to fabric 5, close the atomizer in the first reactor 1 and the air-flow bottle being connected the first reactor 1, connect the atomizer in the 3rd reactor 3 and the air-flow bottle opening connection the 3rd reactor 3, making the alkaline sodium borohydride solution in the 3rd reactor 3 be atomized into hanging drop imports in the second reaction vessel 2 with air-flow through pipeline, atomizer and the air-flow bottle being connected the 3rd reactor 3 in the 3rd reactor 3 is closed after 10 ~ 40min is atomized to fabric 5, first the acid solution of nickelous sulfate is atomized into drop, and be deposited on fabric face, again the alkaline solution of sodium borohydride be atomized into drop and react with the nickelous sulfate be deposited on fabric, generate the nickel particle with catalytic activity, take out the fabric 5 in the second reactor 2, by washed with de-ionized water, fabric 5 after cleaning is put into 60 DEG C of dry 30min of thermostatic drying chamber.Then chemical nickel plating is carried out, copper facing, silver-plated.Fabric can horizontally suspend in the second reactor 2, obtain the fabric with upper surface activation, obtained in chemical plating solution have the metallized fabric of one side, and fabric also vertically can be placed in the second reactor 2, obtain the fabric of two sides activation, the fabric of obtained double-sided metallization in chemical plating solution.
Specific embodiment
Embodiment one
As stated above, fabric is placed in the sodium hydroxide solution of 20g/L, under the condition of 90 DEG C, processes 60min, then clean up, dry for standby;
At ambient temperature, prepare acid nickel sulfate solution, for subsequent use; Wherein the concentration of nickelous sulfate is 0.02g/mL, and concentration of hydrochloric acid is 0.01mol/L.Prepare alkaline sodium borohydride solution, wherein the concentration of sodium borohydride is 0.005g/mL, and the concentration of NaOH is 0.01g/mL.
Being loaded by the acid nickel sulfate solution prepared is placed with in the first reactor 1 of atomizer, being loaded by alkaline sodium borohydride solution is placed with in the 3rd reactor 3 of atomizer, first reactor 1, the 3rd reactor 3 are inserted in cooling bath respectively, are placed at by the fabric 5 cleaned up in the second reactor 2;
First connect the atomizer in the first reactor 1 and the air-flow bottle opening connection first reactor 1, making the acid nickel sulfate solution of the first reactor 1 be atomized into hanging drop horizontally suspends in the second reactor 2 of fabric 5 with air-flow through pipeline importing, 10min is atomized to fabric 5, close the atomizer in the first reactor 1 and the air-flow bottle being connected the first reactor 1, connect the atomizer in the 3rd reactor 3 and the air-flow bottle opening connection the 3rd reactor 3, making the alkaline sodium borohydride solution in the 3rd reactor 3 be atomized into hanging drop imports in the second reaction vessel 2 with air-flow through pipeline, atomizer and the air-flow bottle being connected the 3rd reactor 3 in the 3rd reactor 3 is closed after 10min is atomized to fabric 5, take out the fabric 5 in the second reactor 2, by washed with de-ionized water, take out after fabric 5 after cleaning is put into 60 DEG C of dry 30min of thermostatic drying chamber and carry out chemical nickel plating.Wherein, chemical plating fluid consists of: nickelous sulfate 35g/L, malic acid 30g/L, succinic acid 28g/L, inferior sodium phosphate 30g/L, and pH value is 7, reacts 30min under the condition that temperature is 65 DEG C, then takes out cleaning-drying.
Embodiment two
As stated above, fabric is placed in the sodium hydroxide solution of 20g/L, under the condition of 90 DEG C, processes 60min, then clean up, dry for standby;
At ambient temperature, prepare acid nickel sulfate solution, for subsequent use; Wherein the concentration of nickelous sulfate is 0.1g/mL, and concentration of hydrochloric acid is 0.05mol/L.Prepare alkaline sodium borohydride solution, wherein the concentration of sodium borohydride is 0.01g/mL, and the concentration of NaOH is 0.05g/mL.
Being loaded by the acid nickel sulfate solution prepared is placed with in the first reactor 1 of atomizer, being loaded by alkaline sodium borohydride solution is placed with in the 3rd reactor 3 of atomizer, first reactor 1, the 3rd reactor 3 are inserted in cooling bath respectively, are horizontally suspended by the fabric 5 cleaned up in the second reactor 2;
First connect the atomizer in the first reactor 1 and the air-flow bottle opening connection first reactor 1, making the acid nickel sulfate solution of the first reactor 1 be atomized into hanging drop horizontally suspends in the second reactor 2 of fabric 5 with air-flow through pipeline importing, 40min is atomized to fabric 5, close the atomizer in the first reactor 1 and the air-flow bottle being connected the first reactor 1, connect the atomizer in the 3rd reactor 3 and the air-flow bottle opening connection the 3rd reactor 3, making the alkaline sodium borohydride solution in the 3rd reactor 3 be atomized into hanging drop imports in the second reaction vessel 2 with air-flow through pipeline, atomizer and the air-flow bottle being connected the 3rd reactor 3 in the 3rd reactor 3 is closed after 40min is atomized to fabric 5, take out the fabric 5 in the second reactor 2, by washed with de-ionized water, take out after fabric 5 after cleaning is put into 60 DEG C of dry 30min of thermostatic drying chamber and carry out electroless copper.Wherein, chemical plating fluid consists of: copper sulphate 10g/L, sodium potassium tartrate tetrahydrate 50g/L, NaOH 10g/L, formaldehyde 10g/L, and pH value is 12, reacts 30min under the condition that temperature is 25 DEG C, then takes out cleaning-drying.
Embodiment three
As stated above, fabric is placed in the sodium hydroxide solution of 20g/L, under the condition of 90 DEG C, processes 60min, then clean up, dry for standby;
At ambient temperature, prepare acid nickel sulfate solution, for subsequent use; Wherein the concentration of nickelous sulfate is 0.05g/mL, and concentration of hydrochloric acid is 0.03mol/L.Prepare alkaline sodium borohydride solution, wherein the concentration of sodium borohydride is 0.008g/mL, and the concentration of NaOH is 0.04g/mL.
Being loaded by the acid nickel sulfate solution prepared is placed with in the first reactor 1 of atomizer, being loaded by alkaline sodium borohydride solution is placed with in the 3rd reactor 3 of atomizer, first reactor 1, the 3rd reactor 3 are inserted in cooling bath respectively, are hung vertically in by the fabric 5 cleaned up in the second reactor 2;
First connect the atomizer in the first reactor 1 and the air-flow bottle opening connection first reactor 1, making the acid nickel sulfate solution of the first reactor 1 be atomized into hanging drop has in the second reactor 2 of fabric 5 with air-flow through pipeline importing vertical hanging, 30min is atomized to fabric 5, close the atomizer in the first reactor 1 and the air-flow bottle being connected the first reactor 1, connect the atomizer in the 3rd reactor 3 and the air-flow bottle opening connection the 3rd reactor 3, making the alkaline sodium borohydride solution in the 3rd reactor 3 be atomized into hanging drop imports in the second reaction vessel 2 with air-flow through pipeline, atomizer and the air-flow bottle being connected the 3rd reactor 3 in the 3rd reactor 3 is closed after 30min is atomized to fabric 5, take out the fabric 5 in the second reactor 2, by washed with de-ionized water, take out after fabric 5 after cleaning is put into 60 DEG C of dry 30min of thermostatic drying chamber and carry out chemical silvering.Wherein, chemical plating fluid consists of: silver nitrate 12g/L, glucose 2.8g/L, ammoniacal liquor 100mL/L, and NaOH 8g/L reacts 50min under the condition that temperature is 30 DEG C, then takes out cleaning-drying.
Claims (1)
1. textile chemistry plating without a palladium atomizing activating method, it is characterized in that: describedly to carry out according to the following steps without palladium atomizing activating method:
The preparation of a activating solution:
At ambient temperature, the hydrochloric acid of to be the nickelous sulfate of 0.02 ~ 0.1g/mL and concentration by concentration be 0.01 ~ 0.05mol/L is made into acid nickel sulfate solution, for subsequent use;
The NaOH of to be the sodium borohydride of 0.005 ~ 0.01g/mL and concentration by concentration be 0.01 ~ 0.05g/mL is made into alkaline sodium borohydride solution, for subsequent use;
The acid nickel sulfate solution loading of preparing through a step is placed with in first reactor (1) of atomizer by b, being loaded by alkaline sodium borohydride solution is placed with in the 3rd reactor (3) of atomizer, first reactor (1), the 3rd reactor (3) are inserted in cooling bath respectively, are placed at by the fabric cleaned up (5) in the second reactor (2);
First connect the atomizer in the first reactor (1) and the air-flow bottle opening connection first reactor (1), making the acid nickel sulfate solution of the first reactor (1) be atomized into hanging drop is equipped with in second reactor (2) of fabric (5) with air-flow through pipeline importing, to fabric (5) atomization 10 ~ 40min, close the atomizer in the first reactor (1) and the air-flow bottle being connected the first reactor (1), connect the atomizer in the 3rd reactor (3) and the air-flow bottle opening connection the 3rd reactor (3), making the alkaline sodium borohydride solution in the 3rd reactor (3) be atomized into hanging drop imports in the second reaction vessel (2) with air-flow through pipeline, atomizer and the air-flow bottle being connected the 3rd reactor (3) in the 3rd reactor (3) is closed to after fabric (5) atomization 10 ~ 40min, take out the fabric (5) in the second reactor (2), by washed with de-ionized water, fabric (5) after cleaning is put into 60 DEG C of dry 30min of thermostatic drying chamber.
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CZ308348B6 (en) * | 2018-11-06 | 2020-06-10 | Bochemie A.S. | Process for continuously metallizing a textile material, the apparatus for carrying out the process, metallized textile material and its use |
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CN104975277A (en) * | 2015-06-10 | 2015-10-14 | 上海大学 | Preparation method of copper/nickel iron phosphorus alloy plating double-plating-layer fabric |
CN105803433B (en) * | 2016-04-20 | 2019-07-30 | 青岛科技大学 | A kind of alumina ceramic face no-palladium activating nickel chemical plating technology |
CN106337172B (en) * | 2016-08-30 | 2019-03-01 | 辽宁科技学院 | A kind of method of carbon steel surface no-palladium activating electroless copper |
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CN1334358A (en) * | 2001-08-09 | 2002-02-06 | 华南师范大学 | Process for preparing concentrated liquid specially adapted for chemical spray coating of Ni and its application method |
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CZ308348B6 (en) * | 2018-11-06 | 2020-06-10 | Bochemie A.S. | Process for continuously metallizing a textile material, the apparatus for carrying out the process, metallized textile material and its use |
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