CN109161876A - A kind of silver-plated method of nylon fiber surface chemistry - Google Patents
A kind of silver-plated method of nylon fiber surface chemistry Download PDFInfo
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- CN109161876A CN109161876A CN201811160943.5A CN201811160943A CN109161876A CN 109161876 A CN109161876 A CN 109161876A CN 201811160943 A CN201811160943 A CN 201811160943A CN 109161876 A CN109161876 A CN 109161876A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/28—Sensitising or activating
- C23C18/285—Sensitising or activating with tin based compound or composition
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/20—Pretreatment of the material to be coated of organic surfaces, e.g. resins
- C23C18/2006—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30
- C23C18/2046—Pretreatment of the material to be coated of organic surfaces, e.g. resins by other methods than those of C23C18/22 - C23C18/30 by chemical pretreatment
- C23C18/2073—Multistep pretreatment
- C23C18/2086—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/42—Coating with noble metals
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- Chemical Or Physical Treatment Of Fibers (AREA)
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Abstract
The invention belongs to conductive technical fields, disclose a kind of silver-plated method of nylon fiber surface chemistry, the following steps are included: (1) oil removing: taking quantitative fiber to be put into clean container, the alkaline degreaser of the surface tension for reducing fiber is added into container；(2) sensitizing solution A sensitized treatment: step (1) resulting fiber is totally submerged in the sensitizing solution A now matched, and fiber surface is made to adsorb one layer of metal with catalytic activity；(3) sensitizing solution B sensitized treatment: step (2) resulting fiber is totally submerged in the sensitizing solution B now matched, and the carbonyl functional group of fiber surface and the hydroxy functional group in sensitizing solution B is made to form hydrogen bond；(4) it activates: step (3) resulting fiber is totally submerged in the silver ammino solution now matched；(5) quantitative glucose reducing solution is added into step (4) resulting solution.The available firm silver coating of coating, to obtain the preferable conductive fiber of electric conductivity.
Description
Technical field
The invention belongs to conductive technical fields, and in particular to a kind of silver-plated method of nylon fiber surface chemistry.
Background technique
PA, is called nylon, and chemical name is Fypro.The nylon scientist Tomas Carothers outstanding by the U.S.
(Carothers) and its seminar is in the first in the world kind fiber of synthesis in 1938.1958, first domestic caprolactam examination
It tests sample to trial-produce successfully in Liaoning Province Jinxi chemical plant, this synthetic fibers pull open Liao Zhong Guohe also referred to as " polyamide fibre ", from this
At the prelude of fiber industry.With the miniaturization of automobile, the high performance of electronic electric equipment, the light-weighted process of mechanical equipment
Accelerate, the demand to nylon is higher and higher, and especially nylon has tough, heat-resisting, wear-resistant, resistance toization as structural material
The advantages that product, coefficient of friction be low, self-lubricating, fire-retardant, use temperature range are wide and easy processing is widely used in a kind of industry
Engineering plastics, can be used to replace non-ferrous metal copper production machinery, chemical industry, electrical component, such as diesel engine fuel-firing pump
Gear, water pump, high-pressure seal ring or petroleum pipeline etc..
The advantages of Fypro, is numerous, but as a kind of organic high molecular polymer, its electric conductivity is poor, limitation
, in the application in the fields such as electronics, electric power, military affairs, the electric conductivity that how to improve Fypro has become a hot topic of research for it.
Summary of the invention
In order to solve the above problems existing in the present technology, it is an object of that present invention to provide a kind of nylon fiber surface chemistries
Silver-coating method.
The technical scheme adopted by the invention is as follows:
A kind of silver-plated method of nylon fiber surface chemistry the following steps are included:
(1) oil removing: taking quantitative nylon fiber to be put into clean container, is added into container for reducing nylon fiber
Surface tension alkaline degreaser, ultrasonic treatment then impregnated with dilute acid soln, and finally being cleaned with deionized water to pH value is 7；
(2) sensitizing solution A sensitized treatment: step (1) resulting nylon fiber is totally submerged in the sensitizing solution A now matched,
Make one layer of the nylon fiber adsorption metal with catalytic activity；
(3) sensitizing solution B sensitized treatment: step (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched,
The carbonyl functional group on nylon fiber surface and the hydroxy functional group in sensitizing solution B is set to form hydrogen bond；
(4) it activates: step (3) resulting nylon fiber being totally submerged in the silver ammino solution now matched, room temperature ultrasound one
Section time, the silver ion in silver ammino solution form coordinating with the amino in sensitizing solution B；
(5) quantitative glucose reducing solution is added into step (4) resulting solution, then adjusting pH value is 11-13, equal power
Container is rocked, solution becomes clarification by clarifying to become cloudy again, and nylon fiber surface is completed silver-plated.
Further, in step (1), the alkaline degreaser includes sodium hydroxide, sodium carbonate and anion surface active
Agent.
Further, in step (2), the composition of sensitizing solution A are as follows: 65% concentrated nitric acid of 5-15g/L SnCl2 and 5-15g/L,
Step (1) resulting nylon fiber is totally submerged in the sensitizing solution A now matched, room temperature ultrasound 4-6min, first with 5-15g/L's
NaOH impregnates 0.5-1.5min, then being cleaned with deionized water to pH value is 7.
Further, in step (3), sensitizing solution B's the preparation method comprises the following steps: 50mL 0.1mol/L trihydroxy methyl amino first
Alkane adds deionized water to be diluted to 100mL, and 65% 0.5~1g of nitric acid is added, and adjusting solution ph is 2~7, adds 3,4- bis-
Step (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched ultrasonic at room temperature by hydroxyphenethylamine 0.05g
4-6min。
Further, the process for preparation of the silver ammino solution of step (4) are as follows: 1-4.18gAgNO3 is added to a small amount of deionization
It is dissolved in water, concentrated ammonia liquor is added dropwise to tan precipitate is generated, continue that the tan precipitate disappearance of concentrated ammonia liquor to generation is added dropwise, then be added dropwise dense
The NaOH that degree is 5-15g/l is in dark brown to solution, and then concentrated ammonia liquor to dark brown is added dropwise again and disappears by pH value 11-13, solution
In clear, it is settled to 250ml.
Further, in step (5), the process for preparation of glucose reducing solution are as follows: by 5-15g glucose and 1-3g tartaric acid
It being added in container, adds deionized water and be settled to 500ml, heating stirring keeps 5-15min, is cooled to room temperature to slightly boiled,
Ethyl alcohol 40-60ml is added, sodium carbonate 0.1-0.2mol/l is stirred evenly.
Further, the nylon fiber is PA6 fiber.
The invention has the benefit that
(1) nylon fiber is sensitized first with sensitizing solution A, makes one layer of nylon fiber adsorption there is catalytic activity
Metal, then with sensitizing solution B sensitized treatment make nylon fiber surface carbonyl functional group and sensitizing solution B in hydroxy functional group shape
At hydrogen bond, then carry out chemical plating, the silver ion in silver ammino solution formed with the amino in sensitizing solution B it is good coordinating, point
The good coordinating silvering that improves of interaction force and amino and silver ion between son is in the heavy of nylon fiber surface
Product ability, the change of matrix surface chemical structure result in the enhancing of coating adhesion, the firm silver coating of available coating,
To obtain the preferable conductive fiber of electric conductivity, effectively approach is provided to improve the electric conductivity of Fypro.
(2) resistance of nylon fiber overlay coating works as silver with the raising of the concentration of silver ammino solution in the trend risen afterwards is first dropped
When the mass percent of ammonia solution is 1.1%, resistance value is minimum, is 0.5~0.7 Ω cm-1。
(3) electric conductivity of conductive fiber made from the silver-plated method of nylon fiber surface chemistry of the invention is excellent, anti-electricity
Electromagnetic wave radiation ability is excellent, and the PA6 of plating silver layer has significant electromagnetic shielding action to mobile phone 2G signal.
Specific embodiment
Further explaination is done to the present invention combined with specific embodiments below.
Embodiment 1:
The present embodiment provides a kind of silver-plated methods of nylon fiber surface chemistry, comprising the following steps:
(1) oil removing: taking quantitative nylon fiber to be put into clean container, is added into container for reducing nylon fiber
Surface tension alkaline degreaser, be ultrasonically treated 4-6min, then with mass percentage be 1% dilute nitric acid solution immersion,
Finally being cleaned with deionized water to pH value is 7.Wherein, alkaline degreaser includes that sodium hydroxide, sodium carbonate and anionic surface are living
Neopelex can be selected in property agent, anionic surfactant, and the content of alkaline degreaser each component is respectively as follows: hydrogen-oxygen
The content for changing sodium is 1%, and the content of sodium carbonate is 0.5%, and the content of neopelex is 0.1%；It can also be in alkalinity
Ethanol in proper amount is added in degreaser as defoaming agent.Nylon fiber surface tension significantly reduces after oil removing, is easy to postorder sensitization.
The replacement cycle of degreaser is 15~30 days.
PA6 fiber is selected in the present embodiment.
(2) sensitizing solution A sensitized treatment: step (1) resulting nylon fiber is totally submerged in the sensitizing solution A now matched,
Room temperature ultrasound 4-6min first impregnates 0.5-1.5min with the NaOH of 5-15g/L, then being cleaned with deionized water to pH value is 7, makes Buddhist nun
Imperial fiber surface adsorbs one layer of metal with catalytic activity；Wherein, the composition of sensitizing solution A are as follows: 5-15g/L SnCl2And 5-
65% concentrated nitric acid of 15g/L.It is tetravalence tin ion since stannous ion is oxidizable, tetravalence tin ion easily occurs to hydrolyze and generate glue
Shape precipitating makes sensitizing solution fail, so answering ready-to-use, use is finished as far as possible in for 24 hours.
(3) sensitizing solution B sensitized treatment: step (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched,
Ultrasound 4-6min at room temperature makes the carbonyl functional group on nylon fiber surface and the hydroxy functional group in sensitizing solution B form hydrogen bond；
Wherein, sensitizing solution B's the preparation method comprises the following steps: 50mL 0.1mol/L trishydroxymethylaminomethane, add deionized water to be diluted to
65% 0.5~1g of nitric acid is added in 100mL, and adjusting solution ph is 2~7, adds 3,4- dihydroxy benzenes ethamine 0.05g, will walk
Suddenly (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched.
3,4- dihydroxy benzenes ethamine stability in sensitizing solution B is poor, especially under strongly alkaline conditions, molecule easily occurs
Between polymerization reaction, and trishydroxymethylaminomethane is highly basic, and needing acid adding to adjust solution ph is 2~7, can make 3,4- dihydroxy
Base phenyl ethylamine is stabilized, and the replacement cycle of sensitizing solution B is 7~15 days.
(4) it activates: step (3) resulting nylon fiber being totally submerged in the silver ammino solution now matched, room temperature ultrasound one
Section time, the silver ion in silver ammino solution form good coordinating with the amino in sensitizing solution B；Wherein, silver ammino solution is matched
Process processed are as follows: by 1gAgNO3It is added in a small amount of deionized water and dissolves, concentrated ammonia liquor is added dropwise to tan precipitate is generated, continues to be added dropwise
Concentrated ammonia liquor to the tan precipitate generated disappears, then NaOH that concentration is 10g/l is added dropwise to solution in dark brown, pH value 11-13,
Then concentrated ammonia liquor to dark brown is added dropwise again to disappear, solution is in clear, is settled to 250ml.The quality of resulting silver ammino solution
Percentage is 0.4%.
(5) quantitative glucose reducing solution is added into step (4) resulting solution, then adjusting pH value is 11-13, it is best
Equal power rocks container to same direction, and solution becomes clarification by clarifying to become cloudy again, and nylon fiber surface is completed silver-plated.Wherein, Portugal
The process for preparation of grape sugar reducing solution are as follows: 5-15g glucose and 1-3g tartaric acid are added in container, it is fixed to add deionized water
Hold to 500ml, heating stirring keeps 5-15min, is cooled to room temperature, ethyl alcohol 40-60ml, sodium carbonate 0.1- is added to slightly boiled
0.2mol/l is stirred evenly.
Embodiment 2:
The present embodiment provides a kind of silver-plated methods of nylon fiber surface chemistry, comprising the following steps:
(1) oil removing: taking quantitative nylon fiber to be put into clean container, is added into container for reducing nylon fiber
Surface tension alkaline degreaser, be ultrasonically treated 4-6min, then with mass percentage be 1% dilute nitric acid solution immersion,
Finally being cleaned with deionized water to pH value is 7.Wherein, alkaline degreaser includes that sodium hydroxide, sodium carbonate and anionic surface are living
Neopelex can be selected in property agent, anionic surfactant, and the content of alkaline degreaser each component is respectively as follows: hydrogen-oxygen
The content for changing sodium is 1%, and the content of sodium carbonate is 0.5%, and the content of neopelex is 0.1%；It can also be in alkalinity
Ethanol in proper amount is added in degreaser as defoaming agent.Nylon fiber surface tension significantly reduces after oil removing, is easy to postorder sensitization.
The replacement cycle of degreaser is 15~30 days.
PA6 fiber is selected in the present embodiment.
(2) sensitizing solution A sensitized treatment: step (1) resulting nylon fiber is totally submerged in the sensitizing solution A now matched,
Room temperature ultrasound 4-6min first impregnates 0.5-1.5min with the NaOH of 5-15g/L, then being cleaned with deionized water to pH value is 7, makes Buddhist nun
Imperial fiber surface adsorbs one layer of metal with catalytic activity；Wherein, the composition of sensitizing solution A are as follows: 5-15g/L SnCl2And 5-
65% concentrated nitric acid of 15g/L.It is tetravalence tin ion since stannous ion is oxidizable, tetravalence tin ion easily occurs to hydrolyze and generate glue
Shape precipitating makes sensitizing solution fail, so answering ready-to-use, use is finished as far as possible in for 24 hours.
(3) sensitizing solution B sensitized treatment: step (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched,
Ultrasound 4-6min at room temperature makes the carbonyl functional group on nylon fiber surface and the hydroxy functional group in sensitizing solution B form hydrogen bond；
Wherein, sensitizing solution B's the preparation method comprises the following steps: 50mL 0.1mol/L trishydroxymethylaminomethane, add deionized water to be diluted to
65% 0.5~1g of nitric acid is added in 100mL, and adjusting solution ph is 2~7, adds 3,4- dihydroxy benzenes ethamine 0.05g, will walk
Suddenly (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched.
3,4- dihydroxy benzenes ethamine stability in sensitizing solution B is poor, especially under strongly alkaline conditions, molecule easily occurs
Between polymerization reaction, and trishydroxymethylaminomethane is highly basic, and needing acid adding to adjust solution ph is 2~7, can make 3,4- dihydroxy
Base phenyl ethylamine is stabilized, and the replacement cycle of sensitizing solution B is 7~15 days.
(4) it activates: step (3) resulting nylon fiber being totally submerged in the silver ammino solution now matched, room temperature ultrasound one
Section time, the silver ion in silver ammino solution form good coordinating with the amino in sensitizing solution B；Wherein, silver ammino solution is matched
Process processed are as follows: by 2gAgNO3It is added in a small amount of deionized water and dissolves, concentrated ammonia liquor is added dropwise to tan precipitate is generated, continues to be added dropwise
Concentrated ammonia liquor to the tan precipitate generated disappears, then NaOH that concentration is 10g/l is added dropwise to solution in dark brown, pH value 11-13,
Then concentrated ammonia liquor to dark brown is added dropwise again to disappear, solution is in clear, is settled to 250ml.The quality of resulting silver ammino solution
Percentage is 0.8%.
(5) quantitative glucose reducing solution is added into step (4) resulting solution, then adjusting pH value is 11-13, it is best
Equal power rocks container to same direction, and solution becomes clarification by clarifying to become cloudy again, and nylon fiber surface is completed silver-plated.Wherein, Portugal
The process for preparation of grape sugar reducing solution are as follows: 5-15g glucose and 1-3g tartaric acid are added in container, it is fixed to add deionized water
Hold to 500ml, heating stirring keeps 5-15min, is cooled to room temperature, ethyl alcohol 40-60ml, sodium carbonate 0.1- is added to slightly boiled
0.2mol/l is stirred evenly.
Embodiment 3:
The present embodiment provides a kind of silver-plated methods of nylon fiber surface chemistry, comprising the following steps:
(1) oil removing: taking quantitative nylon fiber to be put into clean container, is added into container for reducing nylon fiber
Surface tension alkaline degreaser, be ultrasonically treated 4-6min, then with mass percentage be 1% dilute nitric acid solution immersion,
Finally being cleaned with deionized water to pH value is 7.Wherein, alkaline degreaser includes that sodium hydroxide, sodium carbonate and anionic surface are living
Neopelex can be selected in property agent, anionic surfactant, and the content of alkaline degreaser each component is respectively as follows: hydrogen-oxygen
The content for changing sodium is 1%, and the content of sodium carbonate is 0.5%, and the content of neopelex is 0.1%；It can also be in alkalinity
Ethanol in proper amount is added in degreaser as defoaming agent.Nylon fiber surface tension significantly reduces after oil removing, is easy to postorder sensitization.
The replacement cycle of degreaser is 15~30 days.
PA6 fiber is selected in the present embodiment.
(2) sensitizing solution A sensitized treatment: step (1) resulting nylon fiber is totally submerged in the sensitizing solution A now matched,
Room temperature ultrasound 4-6min first impregnates 0.5-1.5min with the NaOH of 5-15g/L, then being cleaned with deionized water to pH value is 7, makes Buddhist nun
Imperial fiber surface adsorbs one layer of metal with catalytic activity；Wherein, the composition of sensitizing solution A are as follows: 5-15g/L SnCl2And 5-
65% concentrated nitric acid of 15g/L.It is tetravalence tin ion since stannous ion is oxidizable, tetravalence tin ion easily occurs to hydrolyze and generate glue
Shape precipitating makes sensitizing solution fail, so answering ready-to-use, use is finished as far as possible in for 24 hours.
(3) sensitizing solution B sensitized treatment: step (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched,
Ultrasound 4-6min at room temperature makes the carbonyl functional group on nylon fiber surface and the hydroxy functional group in sensitizing solution B form hydrogen bond；
Wherein, sensitizing solution B's the preparation method comprises the following steps: 50mL 0.1mol/L trishydroxymethylaminomethane, add deionized water to be diluted to
65% 0.5~1g of nitric acid is added in 100mL, and adjusting solution ph is 2~7, adds 3,4- dihydroxy benzenes ethamine 0.05g, will walk
Suddenly (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched.
3,4- dihydroxy benzenes ethamine stability in sensitizing solution B is poor, especially under strongly alkaline conditions, molecule easily occurs
Between polymerization reaction, and trishydroxymethylaminomethane is highly basic, and needing acid adding to adjust solution ph is 2~7, can make 3,4- dihydroxy
Base phenyl ethylamine is stabilized, and the replacement cycle of sensitizing solution B is 7~15 days.
(4) it activates: step (3) resulting nylon fiber being totally submerged in the silver ammino solution now matched, room temperature ultrasound one
Section time, the silver ion in silver ammino solution form good coordinating with the amino in sensitizing solution B；Wherein, silver ammino solution is matched
Process processed are as follows: by 2.75gAgNO3It is added in a small amount of deionized water and dissolves, concentrated ammonia liquor is added dropwise to tan precipitate is generated, continues to drip
Enriching ammonium hydroxide to the tan precipitate generated disappears, then NaOH that concentration is 10g/l is added dropwise to solution in dark brown, pH value 11-
13, concentrated ammonia liquor to dark brown is then added dropwise again and disappears, solution is in clear, is settled to 250ml.The matter of resulting silver ammino solution
Measuring percentage is 1.1%.
(5) quantitative glucose reducing solution is added into step (4) resulting solution, then adjusting pH value is 11-13, it is best
Equal power rocks container to same direction, and solution becomes clarification by clarifying to become cloudy again, and nylon fiber surface is completed silver-plated.Wherein, Portugal
The process for preparation of grape sugar reducing solution are as follows: 10g glucose and 2g tartaric acid are added in container, deionized water is added and is settled to
500ml, heating stirring keep 5-15min, are cooled to room temperature to slightly boiled, and ethyl alcohol 50ml, sodium carbonate 0.1-0.2mol/l is added,
It stirs evenly.
Embodiment 4:
The present embodiment provides a kind of silver-plated methods of nylon fiber surface chemistry, comprising the following steps:
(1) oil removing: taking quantitative nylon fiber to be put into clean container, is added into container for reducing nylon fiber
Surface tension alkaline degreaser, be ultrasonically treated 4-6min, then with mass percentage be 1% dilute nitric acid solution immersion,
Finally being cleaned with deionized water to pH value is 7.Wherein, alkaline degreaser includes that sodium hydroxide, sodium carbonate and anionic surface are living
Neopelex can be selected in property agent, anionic surfactant, and the content of alkaline degreaser each component is respectively as follows: hydrogen-oxygen
The content for changing sodium is 1%, and the content of sodium carbonate is 0.5%, and the content of neopelex is 0.1%；It can also be in alkalinity
Ethanol in proper amount is added in degreaser as defoaming agent.Nylon fiber surface tension significantly reduces after oil removing, is easy to postorder sensitization.
The replacement cycle of degreaser is 15~30 days.
PA6 fiber is selected in the present embodiment.
(2) sensitizing solution A sensitized treatment: step (1) resulting nylon fiber is totally submerged in the sensitizing solution A now matched,
Room temperature ultrasound 4-6min first impregnates 0.5-1.5min with the NaOH of 5-15g/L, then being cleaned with deionized water to pH value is 7, makes Buddhist nun
Imperial fiber surface adsorbs one layer of metal with catalytic activity；Wherein, the composition of sensitizing solution A are as follows: 5-15g/L SnCl2And 5-
65% concentrated nitric acid of 15g/L.It is tetravalence tin ion since stannous ion is oxidizable, tetravalence tin ion easily occurs to hydrolyze and generate glue
Shape precipitating makes sensitizing solution fail, so answering ready-to-use, use is finished as far as possible in for 24 hours.
(3) sensitizing solution B sensitized treatment: step (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched,
Ultrasound 4-6min at room temperature makes the carbonyl functional group on nylon fiber surface and the hydroxy functional group in sensitizing solution B form hydrogen bond；
Wherein, sensitizing solution B's the preparation method comprises the following steps: 50mL 0.1mol/L trishydroxymethylaminomethane, add deionized water to be diluted to
65% 0.5~1g of nitric acid is added in 100mL, and adjusting solution ph is 2~7, adds 3,4- dihydroxy benzenes ethamine 0.05g, will walk
Suddenly (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched.
3,4- dihydroxy benzenes ethamine stability in sensitizing solution B is poor, especially under strongly alkaline conditions, molecule easily occurs
Between polymerization reaction, and trishydroxymethylaminomethane is highly basic, and needing acid adding to adjust solution ph is 2~7, can make 3,4- dihydroxy
Base phenyl ethylamine is stabilized, and the replacement cycle of sensitizing solution B is 7~15 days.
(4) it activates: step (3) resulting nylon fiber being totally submerged in the silver ammino solution now matched, room temperature ultrasound one
Section time, the silver ion in silver ammino solution form good coordinating with the amino in sensitizing solution B；Wherein, silver ammino solution is matched
Process processed are as follows: by 4.18gAgNO3It is added in a small amount of deionized water and dissolves, concentrated ammonia liquor is added dropwise to tan precipitate is generated, continues to drip
Enriching ammonium hydroxide to the tan precipitate generated disappears, then NaOH that concentration is 10g/l is added dropwise to solution in dark brown, pH value 11-
13, concentrated ammonia liquor to dark brown is then added dropwise again and disappears, solution is in clear, is settled to 250ml.The matter of resulting silver ammino solution
Measuring percentage is 1.67%.
(5) quantitative glucose reducing solution is added into step (4) resulting solution, then adjusting pH value is 11-13, it is best
Equal power rocks container to same direction, and solution becomes clarification by clarifying to become cloudy again, and nylon fiber surface is completed silver-plated.Wherein, Portugal
The process for preparation of grape sugar reducing solution are as follows: 5-15g glucose and 1-3g tartaric acid are added in container, it is fixed to add deionized water
Hold to 500ml, heating stirring keeps 5-15min, is cooled to room temperature, ethyl alcohol 40-60ml, sodium carbonate 0.1- is added to slightly boiled
0.2mol/l is stirred evenly.
To sum up, the chemical reaction of silver-colored ammonia is as follows:
2AgNO3+2[NH3·H2O]→Ag2O+2NH4NO3+H2O (1)
Ag2O+4[NH3·H2O]→2[Ag(NH3)2OH]+3H2O (2)
Ag(NH3)2OH+NH4NO3→Ag(NH3)2N03+NH3·H2O (3)
2[Ag(NH3)2N03]+C6H1206→2Ag+C5H11O5COONH4+2NH4N03+NH3 (4)
The study found that be mainly derived from H+ in initial stage solution dense for the unstable factor of plating solution in nylon fiber chemical plating process
The raising of degree declines the pH value of plating solution sharply, therefore chemical plating initial stage needs to adjust the pH value of plating solution, and plating solution is made to keep stablizing.This
In test, by being added at one time enough dilute NaOH before plating, make the pH of plating solution during entire plating maintain 11~13 it
Between, avoiding leads to the discontinuous of reaction process because repeatedly adding alkali halfway, coating it is uneven.
It is stirred in such a way that even power rocks container instead of mechanical stirring or ultrasonic wave, it both can be to avoid due to physical impacts
Lead to falling off for coating during plating, but can guarantee will not because of part the excessively high reaction of pH it is fierce, lead to dividing for plating solution
Solution.
Under the silver ammino solution of various concentration (embodiment 1-4), pass through the coating resistance of multimeter detection fiber surface, tool
Body result such as table 1.
Table 1: pass through the result table of the coating resistance of multimeter detection fiber surface under the silver ammino solution of various concentration
| Testing program | Silver ammino solution mass percent (%) | Resistance/Ω cm-1 |
| Embodiment 1 | 0.4 | 50~70 |
| Embodiment 2 | 0.8 | 1~2 |
| Embodiment 3 | 1.1 | 0.5~0.7 |
| Embodiment 4 | 1.67 | 1~2 |
As it can be seen that silvery white coating is partially thin, is unevenly distributed under the silver ammino solution of low concentration, lead to resistance fluctuation model
It encloses larger；When the mass percent of silver ammino solution is increased to 0.8% from 0.4%, silvery white coating is obviously partially thick, is evenly distributed,
Resistance value significantly reduces, and is 1~2 Ω cm-1；The mass percent of silver ammino solution is improved to 1.1%, coating is thicker, color
It is partially dark, it is more evenly distributed, resistance value continues to reduce, and can reach 1 Ω cm-1Within；Continue the quality percentage of raising silver ammino solution
Than to 1.67%, dark yellow coating is thicker, and distribution uniform, resistance value slightly rises, and is 1~2 Ω cm-1.Result above is said
Bright, it is best when the mass percent of silver ammino solution is 1.1% that resistance and the silver ammino solution concentration of coating, which are not in a linear relationship,
Condition goes up not down more than this threshold value coating resistance, it may be possible to because the mass percent of silver ammino solution is more than after 1.1%,
Thickness of coating obviously increases, and declines the adhesive force of outermost layer silver layer obvious, causes partial exfoliation occur or not deposit, make to plate
Silver-colored actual content is lower than theoretical value in layer, and resistance increases.
Adhesive force without sensitizing solution B processing and the chemical plating silver layer of the fiber handled through sensitizing solution B is detected, is led to
The case where 3M tape method examination silver coating falls off is crossed, the results are shown in Table 2.
Table 2 is the contrast table of the adhesive force of the chemical plating silver layer without sensitizing solution B processing and the fiber handled through sensitizing solution B
| Testing program | Adhesive force |
| It is handled through sensitizing solution B | It does not fall off |
| Without sensitizing solution B processing | It falls off |
3,4- dihydroxy benzenes ethamine have good adhesion characteristics to dielectric surface, it can be adsorbed on dielectric surface, change
The structure of kind dielectric surface, as the hydroxy functional group in 3,4- dihydroxy benzenes ethamine can with the carbonyl functional group in polyamide it
Between form " hydrogen bond ", the good coordinating silvering that improves of interaction force and amino and silver ion between molecule exists
The deposition capability of PA6 fiber surface, the change of matrix surface chemical structure result in the enhancing of coating adhesion.
The electromagnetic shielding performance of fiber coating is as shown in table 3, and test condition is 25 DEG C of environment temperature, envionmental humidity 40
~50%, 86~106kPa of atmospheric pressure, 48h is kept before sample testing in above-mentioned environment, and environment electromagnetic noise ties measurement
Fruit should not have an impact.
Shielding properties of 3 different materials of table to 2G signal
| Sample | Mobile phone 2G signal attenuation/% |
| PA6 fabric | 0 |
| PA6 silver-plated fiber fabric (embodiment 1) | 50% |
| PA6 silver-plated fiber fabric (embodiment 4) | 50% |
| Aluminium foil | 50% |
As seen from the above table, using conductive fiber made from the silver-plated method of nylon fiber surface chemistry of the invention to 2G signal
Shielding properties connect and be equal to aluminium foil to the shielding properties of 2G signal, the silver-plated method of nylon fiber surface chemistry of the invention is made
Conductive fiber can be widely applied on the cabinet, shell, component or panel of electronic equipment etc., to avoid its electromagnetic radiation
Surrounding instruments and personnel are damaged, human health is protected, ensure that instrument and equipment works normally.
The present invention is not limited to above-mentioned optional embodiment, anyone can show that other are each under the inspiration of the present invention
The product of kind form.Above-mentioned specific embodiment should not be understood the limitation of pairs of protection scope of the present invention, protection of the invention
Range should be subject to be defined in claims, and specification can be used for interpreting the claims.
Claims (7)
1. a kind of silver-plated method of nylon fiber surface chemistry, it is characterised in that: the following steps are included:
(1) oil removing: taking quantitative nylon fiber to be put into clean container, and the table for reducing nylon fiber is added into container
The alkaline degreaser of face tension, ultrasonic treatment, then impregnated with dilute acid soln, finally being cleaned with deionized water to pH value is 7；
(2) sensitizing solution A sensitized treatment: step (1) resulting nylon fiber is totally submerged in the sensitizing solution A now matched, Buddhist nun is made
Imperial fiber surface adsorbs one layer of metal with catalytic activity；
(3) sensitizing solution B sensitized treatment: step (2) resulting nylon fiber is totally submerged in the sensitizing solution B now matched, Buddhist nun is made
The carbonyl functional group of imperial fiber surface and the hydroxy functional group in sensitizing solution B form hydrogen bond；
(4) it activates: step (3) resulting nylon fiber is totally submerged in the silver ammino solution now matched, when room temperature is one section ultrasonic
Between, the silver ion in silver ammino solution forms coordinating with the amino in sensitizing solution B；
(5) quantitative glucose reducing solution is added into step (4) resulting solution, then adjusting pH value is 11-13, equal power is rocked
Container, solution become clarification by clarifying to become cloudy again, and nylon fiber surface is completed silver-plated.
2. the silver-plated method of nylon fiber surface chemistry according to claim 1, it is characterised in that: in step (1), the alkali
Property degreaser includes sodium hydroxide, sodium carbonate and anionic surfactant.
3. the silver-plated method of nylon fiber surface chemistry according to claim 2, it is characterised in that: in step (2), sensitizing solution
The composition of A are as follows: 5-15g/L SnCl2And 65% concentrated nitric acid of 5-15g/L, by step (1) resulting nylon fiber be totally submerged in
In the sensitizing solution A now matched, room temperature ultrasound 4-6min first impregnates 0.5-1.5min with the NaOH of 5-15g/L, then clear with deionized water
Being washed till pH value is 7.
4. the silver-plated method of nylon fiber surface chemistry according to claim 3, it is characterised in that: in step (3), sensitizing solution
B's the preparation method comprises the following steps: 50mL 0.1mol/L trishydroxymethylaminomethane, add deionized water to be diluted to 100mL, be added 65%
0.5~1g of nitric acid, adjusting solution ph is 2~7,3,4- dihydroxy benzenes ethamine 0.05g is added, by step (2) resulting Buddhist nun
Imperial fiber is totally submerged in the sensitizing solution B now matched ultrasound 4-6min at room temperature.
5. the silver-plated method of nylon fiber surface chemistry according to claim 4, it is characterised in that: the silver-colored ammonia of step (4) is molten
The process for preparation of liquid are as follows: by 1-4.18gAgNO3It is added in a small amount of deionized water and dissolves, it is heavy to brown is generated that concentrated ammonia liquor is added dropwise
It forms sediment, continues concentrated ammonia liquor to the tan precipitate generated is added dropwise and disappear, then NaOH that concentration is 5-15g/l is added dropwise to solution in deep brown
Then concentrated ammonia liquor to dark brown is added dropwise again and disappears by color, pH value 11-13, solution is in clear, is settled to 250ml.
6. the silver-plated method of nylon fiber surface chemistry according to claim 5, it is characterised in that: in step (5), glucose
The process for preparation of reducing solution are as follows: 5-15g glucose and 1-3g tartaric acid are added in container, deionized water is added and is settled to
500ml, heating stirring keep 5-15min, are cooled to room temperature to slightly boiled, and ethyl alcohol 40-60ml, sodium carbonate 0.1-0.2mol/ is added
L is stirred evenly.
7. the silver-plated method of nylon fiber surface chemistry described in any one of -6 claims according to claim 1, it is characterised in that:
The nylon fiber is PA6 fiber.
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| CN114774895A (en) * | 2022-03-31 | 2022-07-22 | 莫纶(珠海)新材料科技有限公司 | Al2O3Composite functional fiber and its prepn |
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