CN106436290A - Method for preparing silver antibacterial agent textile by complexing aminoacetic acid and silver nitrate - Google Patents
Method for preparing silver antibacterial agent textile by complexing aminoacetic acid and silver nitrate Download PDFInfo
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- CN106436290A CN106436290A CN201611173152.7A CN201611173152A CN106436290A CN 106436290 A CN106436290 A CN 106436290A CN 201611173152 A CN201611173152 A CN 201611173152A CN 106436290 A CN106436290 A CN 106436290A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
Abstract
The invention relates to a method for preparing a silver antibacterial agent textile by complexing aminoacetic acid and silver nitrate. Carbon fibers (textiles) are infiltrated into a silver nitrate and aminoacetic acid complexing solution, and heating decomposition and reduction are carried out to obtain high-stability nano-silver adsorbed on surfaces of the carbon fibers (textiles). The silver nitrate-aminoacetic acid complexing solution with the Ag ion concentration of 0.01 percent to 0.6 percent and the mol ratio of (2 to 1.5) : 1 is prepared firstly; then the carbon fibers (textiles) are immersed into the complexing solution for 6 to 24 hours at the ratio of 0.25Kg to 1Kg per liter; under the protection of circulating nitrogen gas, heat is preserved at 160 DEG C to 260 DEG C for 0.5h to 6h for carrying out the heating decomposition; after being washed with clean water, the carbon fibers (textiles) are dried, wherein the grain diameter of obtained nano-silver is 10nm to 60nm, and the silver carrying amount is 0.01 weight percent to 0.45 weight percent. By adopting the method provided by the invention, a process flow is shortened and a reaction temperature is lowered; the sterilization efficiency of the silver-carried carbon fibers (textiles) is improved, and the silver utilization amount is reduced.
Description
Technical field
The present invention relates to a kind of carry silver-colored Carbon fibe（Fabric）Method.It is by molten with silver nitrate and glycine complexation
Liquid, then infiltrate Carbon fibe（Fabric）, through heat resolve and reduction, using silver nitrate and the reaction heat of alanine complex,
Obtain the Carbon fibe of high stability（Fabric）Surface adsorption nanometer silver, for preparing the side such as efficient silver-series antibacterial agent fabric product
Face.
Technical background
The invention belongs to the load silver process of silver-series antibacterial agent fabric product is processed.
Textile is one of requisite product of human lives, and its daily life daily with people is closely bound up.So
And, as most of textiles itself have stronger moisture pick-up propertiess and larger specific surface area, so easily becoming various
The place of microbial growth.The textile for growing antibacterial or other microorganisms can not only affect intensity, the color and luster of its own
With resistance to performance of waiting so long, the medium of the virus that spreads germs is will also become, endangers the healthy of user.So, antibacterial of weaving
Research and development with using just day by day becoming emphasis of concern.
Silver system textile antibacterial agent has the anti-microbial property of broad-spectrum high efficacy, has relatively broad answering in medicine and hygiene fieldses
With the such as medical treatment such as medical device and operation dress, clothing of nurses, Wound dressing, binder, mask such as surgical instrumenties, contraception apparatus, artificial limb
Protective articless.Under high pathogenic environmental, the wide spectrum of silver-series antibacterial agent, efficient, safe, lasting antibacterial functions contribute to resisting disease
Infringement of the bacterium to human body.Silver-series antibacterial agent can also be used for filter medium, add silver system anti-in water filtration or air filter
Microbial inoculum, not only can effectively reduce antibacterial, funguses and other harmful microorganisms of water or in the air, can also kill and remain in
Antibacterial inside filter device, improves its safety for using the service life for extending filter element.
According to carrier difference, the silver-colored silicate antibacterial of load can be divided into, carry silver-colored phosphate-based antibacterial, load silver Carbon fibe
（Fabric）The silver-colored organic polymer antibacterial of antibacterial, load and the silver-colored photocatalyst-type anti-biotic agent of load etc..
Carry silver-colored Carbon fibe（Fabric）Preparation method be divided into front bearing silver method and rear bearing silver method.Front bearing silver method is mainly presoma
Carry silver-colored method, i.e., precursor fibre on be loaded with silver-colored source, subsequently carry out activation charring process.The problem that front bearing silver method is present
Silver ion mainly in solution is difficult to load in precursor fibre, and after carbonization, activation, carbon fiber surface Argent grain divides
Cloth is irregular, particle diameter is not of uniform size, and anti-microbial property is poor.
Rear bearing silver method is to load silver by the method such as physics, chemistry on the fabric for having prepared, such as dipping thermal decomposition method,
Immersion reduction method, composite spinning method, chemical deposition and physical sputtering method etc..Wherein dipping thermal decomposition method, immersion reduction method are
Relatively common load silver method：1. dipping thermal decomposition method is knitted using the film containing silver particles aqueous solution soaking such as silver nitrate, silver nitrate
Thing, dries post-heating to～700 DEG C, obtains argent using silver oxide pyrolytic.Require to calcine under inert gas shielding,
Free air infiltration can not be to enter in calcination process and temperature-fall period, once there is free air infiltration to enter, the argent for easily being formed can be oxidized to again
Silver oxide, its end product quality is wayward.Infusion process process is simple, low cost, pollution-free, silver is distributed in fabric face,
Be conducive to sterilization.But the silver particles that the method is prepared are mainly physical absorption, silver is easily lost in, it is impossible to reach lasting sterilization
Effect.2. immersion reduction method is to soak the fabric into a period of time in Ag-containing solution, then with a kind of reducing agent silver ion also
Original becomes the process of elemental silver.With NaBH4As a example by reduction, detailed process is fabric activation processing, is soaked under the conditions of lucifuge for a long time
Stain is to AgNO3In solution, afterwards with distilled water wash until no silver ion detection in cleaning mixture, is then immersed in NaBH again4Solution
In, washing removes unnecessary NaBH4, dry in cryogenic vacuum long-time.The method can realize the good combination of fabric and Argent grain.
But reducing process process flow is long；Need repeatedly to wash, water consumption is big, and water resource has high demands；The techniques such as lucifuge, vacuum are used, if
Standby have high demands；And Argent grain is mainly distributed in the outer surface and hole of fabric with reunion shape, the Argent grain of load than larger, and
Germicidal efficiency is not high.
Nanometer silver is 30 × 10 in concentration-6When, with preferable antibacterial activity, but there is potential cytotoxicity；?
3×10-6Under concentration, 2 grades of cytotoxicity.How to reduce its cytotoxicity problem and should give attention.At present, reduce silver system antibacterial
The strategy of agent toxicity mainly controls its release concentration of silver ions higher than minimum inhibitory concentration, less than human body highest safe concentration.
For the silver-series antibacterial agent for being applied to the fields such as medical dressing, air and purification of water quality, it should also be noted that coming off for Argent grain is avoided,
Because the amount of coming off of Argent grain directly affects silver ion burst size, service life and the antibacterial persistence of antibacterial can be also affected.
Content of the invention
It is an object of the invention to provide a kind of load silver Carbon fibe with efficient, lasting bactericidal action（Fabric）Preparation side
Method.
The technical solution adopted for the present invention to solve the technical problems is that with silver particles, complexing can occur using one kind
Reducing agent, by silver ion with complex form adsorb in Carbon fibe（Fabric）Surface and micropore in, then in relatively low temperature
Degree lower fast restore, decomposition, the load silver Carbon fibe for obtain good dispersion, not easily runing off（Fabric）, comprise the following steps that：
(1) prepared by silver nitrate-glycine complex liquid：A certain amount of silver nitrate crystal and glycine crystal is weighed, with distillation
Water dissolution, obtains silver-colored ammonium nitrate complex liquid.Wherein, silver nitrate is 2 with the molar ratio of glycine:1～1.5:Between 1, join
In the aqueous solution of system, Ag mass of ion concentration is 0.01～0.6%.
(2) silver ion soaks, dries Carbon fibe（Fabric）：Shaken with the silver nitrate for preparing-alanine complex liquid room temperature
Swing, soak the Carbon fibe after carbonization, activation processing（Fabric）, soak time is 6～24 hours；Carbon fibe during immersion（Fabric）
Ratio with complex liquid is 0.25～1Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；Then in hot blast, such as electric heating
Air dry oven, 50～100 DEG C of dryings to constant weight, removing water and water of crystallization.
(3) pyrolysis：Carbon fibe after drying will be soaked（Fabric）It is warming up at 160-260 DEG C, temperature retention time is
0.5～6 hour.Using dry circulating nitrogen gas protection during thermal decomposition, may also be employed when having ready conditions decomposing ammonia protection.Using pushing away boat
The continuous furnaces such as stove, net belt type drying oven, rotary furnace can achieve continuous production.Programming rate controls at 0.1～2 DEG C/min,
Pyrolysis are avoided excessively acutely to affect nanometer silver dispersibility and and Carbon fibe（Fabric）The interface binding power on surface.
(4) wash：By above-mentioned Carbon fibe（Fabric）With pure water washing 2～4 times, the reactant of remnants is washed away.In order to keep away
Exempt from silver particles oxidation, the baking temperature after cleaning controls at 50～120 DEG C.Silver-colored remaining quantity≤the 10ppb of the water after cleaning（Micro-
Grams per liter), reach the standard of drinking water.
(5) detect：Sodium rhodanate standard solution titration determination silver carrying amount, scanning electron microscopic observation Argent grain are adopted per batch
Pattern and size, and in 25 DEG C, 150 r/min, constant temperature oscillation is after 600 hours, is swollen the anti-of Spectrophotometric Determination of Silver with double sulfur
Flow and failure property, turnover rate≤25% of silver, silver carrying amount is by Carbon fibe specific surface and absorption property, complex liquid silver content, soaking technology
With the impact of the parameter of thermal decomposition process, when silver carrying amount is less than the 0.01～0.45wt.% for requiring, repeat step（2）Silver ion
Soak, dry Carbon fibe and step（3）Pyrolysis are to increase silver carrying amount.
Silver nitrate is 1.8～1.5 with the mol ratio of glycine:1.
In the aqueous solution of preparation, Ag ion concentration is 0.01～0.1%.
By silver nitrate (AgNO3) as oxidant, glycine (C2H5NO2) as complexation reducing agent, be configured to water-soluble
Liquid；Solution is gradually evaporated and can form gel.This gel can react rapidly, release a large amount of gases and heat at 160～260 DEG C
Amount, is obtained scattered nano level superfine silver powder.Glycine (H there occurs during this first2N-CH2- COOH)
, there is NH in hydrolysis4 +.With the carrying out of heating, water evaporation, the NH in solution4 +And NO3 -Ion is then with NH4NO3The shape of crystal
Formula is separated out, and finally gives AgOH, Ag2O and NH4NO3The mixture of crystal.Above-mentioned mixed crystal is heated further, it may occur that
The decomposition reaction of complexity, obtains nanometer silver and CO2、H2O、N2O、N2Deng gas.
When silver nitrate and glycine are 2 in molar ratio:Reaction equation when 1 is as follows：
4AgNO3+2C2H5NO2→4Ag+4CO2+5H2O+3N2O
When silver nitrate and glycine are 3 in molar ratio:Reaction equation when 2 is as follows：
6AgNO3+4C2H5NO2→6Ag+8CO2+10H2O+5N2
When silver nitrate excess, reaction occurs the oxide of silver, but due to exothermic heat of reaction, local temperature is raised, the oxidation of silver
Decomposition product and obtain elemental silver；When reducing agent glycine is excessive further, needs oxygen that reaction is participated in, or discharge
Ammonia.
The present invention is used for producing the silver-colored Carbon fibe of load（Fabric）, have the characteristics that the low and efficiency high of reaction temperature, generally exist
Between 160-260 DEG C, the heat of decomposition reaction release promotes reaction to carry out.Compared with conventional dipping and thermal decomposition process, contracting
Short technological process, is reduced reaction temperature, avoids the occurrence of the Ag granule for being caused due to pyroreaction and combined not with carbon surface
Jail and the problem for silver oxide easily occur.Compared with conventional reduction method, dipping number of times is reduced, and due to of the present invention
Complexation Ag compound decomposes a large amount of gas such as NH of generation3、H2O、CO2、N2, N2O etc., disperses the Ag nano particles to be formed, overcomes
General N aBH4Reduction prepares Ag particle agglomeration phenomenon, carries high silver supported Carbon fibe（Fabric）Germicidal efficiency, reduce silver-colored consumption.
Present invention process process is simple, easily operated, yield is high, be easy to industrialized production, with clean, environmental protection and
Characteristics of energy saving.Gained nanometer silver particle diameter is 10 ~ 60nm；0.01～0.45wt.% of silver carrying amount；Argent grain and Carbon fibe（Fabric）Knot
High with joint efforts, 150r/min, vibrate in 25 DEG C of thermostatted waters, after 600 hours, turnover rate≤25% of silver；Argent grain good dispersion, kill
Bacterium efficiency high.
Specific embodiment
Below by way of specific embodiment, the present invention is elaborated.
Embodiment 1
(1) prepared by silver nitrate-glycine complex liquid：17g silver nitrate and 5.0g glycine is weighed, with distillation water dissolution, is obtained
Obtain 100 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate is 3 with the molar ratio of glycine:2, in the aqueous solution of preparation Ag from
Sub- concentration is about 0.01%.
(2) silver ion soaks, dries Carbon fibe（Fabric）By the Carbon fibe after carbonization, activation processing（Fabric）With steaming
Distilled water is cleaned, dries, is cooled.It is about 0.01% with Ag ion concentration, molar ratio is 3:2 silver nitrate-glycine complex liquid
Shaken at room temperature, immersion Carbon fibe（Fabric）, soak time is 6 hours；Carbon fibe during immersion（Fabric）Ratio with complex liquid is
1Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；In electric drying oven with forced convection, 50 DEG C of dryings to constant weight, removing water and
Water of crystallization.
(3) pyrolysis：Carbon fibe after drying will be soaked（Fabric）It is warming up at 160 DEG C, temperature retention time is 6 hours.
Using drying in dry circulating nitrogen gas protection tube furnace during thermal decomposition, programming rate is 2 DEG C/min.
(4) wash：By above-mentioned Carbon fibe（Fabric）With pure water washing 2 times, the reactant of remnants is washed away.After cleaning
Electric drying oven with forced convection, 50 DEG C of dryings are to constant weight.
(5) detect：Gained nanometer silver particle diameter is 25nm；Silver carrying amount 0.01%；Argent grain and Carbon fibe（Fabric）Adhesion
Height, 150r/min, vibrate in 25 DEG C of thermostatted waters, after 600 hours, the turnover rate of silver is 12%.
Embodiment 2
(1) prepared by silver nitrate-glycine complex liquid：17g silver nitrate and 5.0g glycine is weighed, with distillation water dissolution, is obtained
Obtain 18 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate is 3 with the molar ratio of glycine:2, in the aqueous solution of preparation Ag from
Sub- concentration is about 0.6%.
(2) silver ion soaks, dries Carbon fibe（Fabric）：By the Carbon fibe after carbonization, activation processing（Fabric）With steaming
Distilled water is cleaned, dries, is cooled.It is about 0.6% with Ag ion concentration, molar ratio is 3:2 silver nitrate-glycine complex liquid
Shaken at room temperature, immersion Carbon fibe（Fabric）, soak time is 24 hours；Carbon fibe during immersion（Fabric）Ratio with complex liquid is
1Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；In electric drying oven with forced convection, 100 DEG C of dryings to constant weight, remove water
And water of crystallization.
(3) pyrolysis：Carbon fibe after drying will be soaked（Fabric）It is warming up at 260 DEG C, temperature retention time is little for 0.5
When.Controlled at 0.1 DEG C/min using net belt type drying oven, programming rate during thermal decomposition, protected using dry circulating nitrogen gas.
(4) wash：By above-mentioned Carbon fibe（Fabric）With pure water washing 4 times, the reactant of remnants is washed away.Use after cleaning
In net belt type drying oven, 120 DEG C of dryings are to constant weight.
(5) detect：Gained nanometer silver particle diameter is 58nm；Silver carrying amount 0.44%；Argent grain and Carbon fibe（Fabric）Adhesion
Height, 150r/min, vibrate in 25 DEG C of thermostatted waters, after 600 hours, the turnover rate of silver is 24%.
Embodiment 3
(1) prepared by silver nitrate-glycine complex liquid：17g silver nitrate and 3.8g glycine is weighed, with distillation water dissolution, is obtained
Obtain 18 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate is 2 with the molar ratio of glycine:1, in the aqueous solution of preparation Ag from
Sub- concentration is about 0.6%.
(2) silver ion soaks, dries Carbon fibe（Fabric）：By the Carbon fibe after carbonization, activation processing（Fabric）With steaming
Distilled water is cleaned, dries, is cooled.It is about 0.6% with Ag ion concentration, molar ratio is 2:1 silver nitrate-glycine complex liquid
Shaken at room temperature, immersion Carbon fibe（Fabric）, soak time is 12 hours；Carbon fibe during immersion（Fabric）Ratio with complex liquid is
0.25Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；In 80 DEG C of hot air drying cylinders drying to constant weight, water and knot is removed
Brilliant water.
(3) pyrolysis：Carbon fibe after drying will be soaked（Fabric）It is warming up at 200 DEG C, temperature retention time is 3 hours.
Using boat drying oven, programming rate control is pushed away automatically at 0.5 DEG C/min during thermal decomposition, protected using dry circulating nitrogen gas.
(4) wash：By above-mentioned Carbon fibe（Fabric）With pure water washing 3 times, the reactant of remnants is washed away.Use after cleaning
Boat drying oven is being pushed away automatically, and 110 DEG C of dryings are to constant weight.
(5) detect：Gained nanometer silver particle diameter is 60nm；Silver carrying amount 0.32%；Argent grain and Carbon fibe（Fabric）In conjunction with
Power height, 150r/min, vibrate in 25 DEG C of thermostatted waters, after 600 hours, the turnover rate of silver is 14%.
Embodiment 4
(1) prepared by silver nitrate-glycine complex liquid：Weigh 17g silver nitrate and 4.68g glycine, with distillation water dissolution,
Obtain 36 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate is 1.6 with the molar ratio of glycine:1, in the aqueous solution of preparation
Ag ion concentration is about 0.3%.
(2) silver ion soaks, dries Carbon fibe（Fabric）：By the Carbon fibe after carbonization, activation processing（Fabric）With steaming
Distilled water is cleaned, dries, is cooled.It is about 0.3% with Ag ion concentration, molar ratio is 1.6:1 silver nitrate-glycine complexation
Liquid shaken at room temperature, immersion Carbon fibe（Fabric）, soak time is 12 hours；Carbon fibe during immersion（Fabric）Ratio with complex liquid
For 0.5Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；In 100 DEG C of hot air drying cylinders drying to constant weight, remove water and
Water of crystallization.
(3) pyrolysis：Carbon fibe after drying will be soaked（Fabric）It is warming up at 220 DEG C, temperature retention time is 3 hours.
Using boat drying oven, programming rate control is pushed away automatically at 0.5 DEG C/min during thermal decomposition, protected using dry circulating nitrogen gas.
(4) wash：By above-mentioned Carbon fibe（Fabric）With pure water washing 2 times, the reactant of remnants is washed away.Use after cleaning
Boat drying oven is being pushed away automatically, and 120 DEG C of dryings are to constant weight.
(5) detect：Gained nanometer silver particle diameter is 30nm；Silver carrying amount 0.3%；Argent grain and Carbon fibe（Fabric）Adhesion
Height, 150r/min, vibrate in 25 DEG C of thermostatted waters, after 600 hours, the turnover rate of silver is 14%.
Embodiment 5
(1) prepared by silver nitrate-glycine complex liquid：Weigh 8.5g silver nitrate and 4.4g glycine, with distillation water dissolution,
Obtain 36 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate is 1.7 with the molar ratio of glycine:1, in the aqueous solution of preparation
Ag ion concentration is about 0.15%.
(2) silver ion soaks, dries Carbon fibe（Fabric）：By the Carbon fibe after carbonization, activation processing（Fabric）With steaming
Distilled water is cleaned, dries, is cooled.It is about 0.15% with Ag ion concentration, molar ratio is 1.7:1 silver nitrate-glycine complexation
Liquid shaken at room temperature, immersion Carbon fibe（Fabric）, soak time is 9 hours；Carbon fibe during immersion（Fabric）Ratio with complex liquid
For 0.25Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；In 90 DEG C of hot air drying cylinders drying to constant weight, remove water and
Water of crystallization.
(3) pyrolysis：Carbon fibe after drying will be soaked（Fabric）It is warming up at 200 DEG C, temperature retention time is little for 2
When.Using dry circulating nitrogen gas protection tube furnace during thermal decomposition, programming rate controls at 1 DEG C/min.
(4) wash：By above-mentioned Carbon fibe（Fabric）With pure water washing 2 times, the reactant of remnants is washed away.Use after cleaning
90 DEG C of air dry oven dryings are to constant weight.
(5) detect：Gained nanometer silver particle diameter is 25nm；Silver carrying amount 0.03%；Argent grain and Carbon fibe（Fabric）In conjunction with
Power height, 150r/min, vibrate in 25 DEG C of thermostatted waters, after 600 hours, the turnover rate of silver is 9%.
Claims (3)
1. a kind of method that glycine prepares silver-series antibacterial agent fabric product with silver nitrate complexation, it is characterised in that including following step
Suddenly：
(1) prepared by silver nitrate-glycine complex liquid：A certain amount of silver nitrate crystal and glycine crystal is weighed, with distillation
Water dissolution, obtains silver-colored ammonium nitrate complex liquid, and silver nitrate is 2～1.5 with the mol ratio of glycine:1, Ag in the aqueous solution of preparation
Mass of ion concentration is 0.01～0.6%；
(2) silver ion soaks, dries Carbon fibe：With the silver nitrate for preparing-alanine complex liquid shaken at room temperature, soak warp
Carbon fibe after carbonization, activation processing, soak time is 6～24 hours；During immersion, the ratio of Carbon fibe and complex liquid is 0.25
～1Kg/ liter；It is filtered dry in ventilation, light protected environment after immersion；Then in hot blast, such as electric drying oven with forced convection, 50～100 DEG C of dryings
To constant weight, water and water of crystallization is removed；
(3) pyrolysis：Carbon fibe after drying will be soaked 160-260 DEG C is warming up to, insulation carries out heat point for 0.5～6 hour
Solution, adopts dry circulating nitrogen gas protection, or is protected using ammonia is decomposed during thermal decomposition；Using push away boat stove, net belt type drying oven or
Rotary furnace continuous furnace, realizes continuous production；Programming rate controls at 0.1～2 DEG C/min, it is to avoid pyrolysis are excessively
Acutely nanometer silver dispersibility and the interface binding power with carbon fiber surface are affected；
(4) wash：By above-mentioned Carbon fibe pure water washing 2～4 times, the reactant of remnants is washed away；In order to avoid silver particles oxygen
Change, the control of baking temperature after cleaning at 50～120 DEG C, the silver-colored remaining quantity≤10ppb of the water after cleaning, reach the mark of drinking water
Accurate；
(5) detect：Sodium rhodanate standard solution titration determination silver carrying amount, scanning electron microscopic observation Argent grain pattern are adopted per batch
And size, and in 25 DEG C, 150 r/min, constant temperature oscillation was lost with the anti-current of the swollen Spectrophotometric Determination of Silver of double sulfur after 600 hours
Performance, turnover rate≤25% of silver, silver carrying amount is by Carbon fibe specific surface and absorption property, complex liquid silver content, soaking technology and warm
The impact of the parameter of decomposition technique, when silver carrying amount is less than the 0.01～0.45wt.% for requiring, repeat step（2）Silver ion soaks
Steep, dry Carbon fibe and step（3）Pyrolysis are to increase silver carrying amount.
2. the method that glycine as claimed in claim 1 prepares silver-series antibacterial agent fabric product with silver nitrate complexation, its feature
It is：Silver nitrate is 1.8～1.5 with the mol ratio of glycine:1.
3. the method that glycine as claimed in claim 1 prepares silver-series antibacterial agent fabric product with silver nitrate complexation, its feature
It is：Step（1）In the aqueous solution of preparation, Ag mass of ion concentration is 0.01～0.1%.
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| CN201611173152.7A CN106436290B (en) | 2016-12-18 | 2016-12-18 | A kind of method that amion acetic acid prepares silver-series antibacterial agent fabric product with silver nitrate complexing |
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| CN201611173152.7A CN106436290B (en) | 2016-12-18 | 2016-12-18 | A kind of method that amion acetic acid prepares silver-series antibacterial agent fabric product with silver nitrate complexing |
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|---|---|---|---|---|
| JPH02185901A (en) * | 1988-08-22 | 1990-07-20 | Fukuda Metal Foil & Powder Co Ltd | Copper-silver-coated metal sulfide powder and manufacture thereof |
| JPH08325844A (en) * | 1995-05-24 | 1996-12-10 | Unitika Ltd | Antimicrobial fiber |
| CN1376822A (en) * | 2002-04-30 | 2002-10-30 | 中山大学 | Process for preparing antibacterial fibre of activated carbon containing nano silver particles |
| CN101368331A (en) * | 2008-09-25 | 2009-02-18 | 湖南多喜爱纺织科技有限公司 | Cotton fabric inorganic nanometer antibiotic finishing agent and preparation method thereof |
-
2016
- 2016-12-18 CN CN201611173152.7A patent/CN106436290B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02185901A (en) * | 1988-08-22 | 1990-07-20 | Fukuda Metal Foil & Powder Co Ltd | Copper-silver-coated metal sulfide powder and manufacture thereof |
| JPH08325844A (en) * | 1995-05-24 | 1996-12-10 | Unitika Ltd | Antimicrobial fiber |
| CN1376822A (en) * | 2002-04-30 | 2002-10-30 | 中山大学 | Process for preparing antibacterial fibre of activated carbon containing nano silver particles |
| CN101368331A (en) * | 2008-09-25 | 2009-02-18 | 湖南多喜爱纺织科技有限公司 | Cotton fabric inorganic nanometer antibiotic finishing agent and preparation method thereof |
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