CN106436291A - Method for preparing silver-carrying carbon fibers by aminopropionic acid serving as reducing agent - Google Patents
Method for preparing silver-carrying carbon fibers by aminopropionic acid serving as reducing agent Download PDFInfo
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- CN106436291A CN106436291A CN201611173166.9A CN201611173166A CN106436291A CN 106436291 A CN106436291 A CN 106436291A CN 201611173166 A CN201611173166 A CN 201611173166A CN 106436291 A CN106436291 A CN 106436291A
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- silver
- alanine
- carbon fibe
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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
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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
- 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 silver-carrying carbon fibers by aminopropionic acid serving as a reducing agent. By a silver nitrate and aminopropionic acid complex solution, carbon fibers (fabrics) are impregnated to obtain high-stability nano silver adsorbed on surfaces of the carbon fibers (fabrics) through heating decomposition and reduction. The method includes: preparing the silver nitrate and aminopropionic acid complex solution, wherein a mole ratio of the solution is 3.2-2.5:1, and the Ag ion mass concentration is 0.01-0.6%; soaking for 6-24h prior to thermal decomposition, wherein a proportion of the carbon fibers (fabrics) to the complex solution is 0.25-1Kg/liter; washing with clear water, and drying to obtain the nano silver in a particle size of 10-50nm, wherein the silver carrying amount is 0.01-0.4wt%. The method has advantages of shortening of process procedures, reduction of reaction temperature, improvement of bactericidal efficiency of the silver-carrying carbon fibers (fabrics) and reduction of silver consumption.
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 alanine 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-series antibacterial agent
The strategy of toxicity mainly controls its release concentration of silver ions higher than minimum inhibitory concentration, less than human body highest safe concentration.Right
In 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
Silver ion burst size is directly affected for the amount of coming off of Argent grain, can also affect service life and the antibacterial persistence of antibacterial.
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-alanine complex liquid：A certain amount of silver nitrate crystal and alanine crystal is weighed, with distillation
Water dissolution, obtains silver-colored ammonium nitrate complex liquid.Wherein, silver nitrate is 3.2～2.5 with the molar ratio of alanine:Between 1, join
In the aqueous solution of system, Ag mass of ion concentration is 0.01～0.6%.
(2) silver ion solution soaks：With the silver nitrate for preparing-alanine complex liquid shaken at room temperature, soak through charcoal
Carbon fibe after change, activation processing（Fabric）, 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 ventilated environment, light protected environment after immersion；Then in hot blast, such as electric drying oven with forced convection, 40～90
DEG C drying removes water and water of crystallization to constant weight.
(3) pyrolysis：Silver particles are soaked Carbon fibe after drying（Fabric）It is warming up at 160-300 DEG C, insulation
Between be 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
Push away the continuous furnaces such as boat stove, net belt type drying oven, rotary furnace and can achieve continuous production.Programming rate control 0.1～2 DEG C/
Minute, it is to avoid pyrolysis excessively acutely affect nanometer silver dispersibility and and Carbon fibe（Fabric）The interface cohesion on surface
Power.
(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 the leach resistance of the Spectrophotometric Determination of Silver that swells in 25 DEG C, 150 r/min constant temperature oscillation and double sulfur.Carry
Silver amount is by Carbon fibe（Fabric）Specific surface and absorption property, complex liquid silver content, the parameter of soaking technology and thermal decomposition process
Impact.When silver carrying amount is less than the 0.01～0.40wt.% for requiring, repeat step（2）Silver ion soaks and step（3）Thermal decomposition
Reaction is to increase silver carrying amount.
Silver nitrate is 3.0～2.5 with the mol ratio of alanine:1.
Silver ion mass concentration is 0.01～0.1%.
By silver nitrate (AgNO3) as oxidant, alanine (C3H7NO2) 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 160～300 DEG C
Amount, is obtained scattered nano level superfine silver powder.Alanine (CH there occurs during this first3CH(NH2)COOH)
Decomposition reaction, there is NH4 +.With the carrying out of heating, water evaporation, the NH in solution4 +And NO3 -Ion is then with NH4NO3Crystal
Form is separated out, and finally gives AgOH, Ag2O and NH4NO3The mixture of crystal.Above-mentioned mixed crystal is heated further, can be sent out
The decomposition reaction of complexity is given birth to, obtains nanometer silver and CO2、H2O、N2O、N2Deng gas.
When silver nitrate and alanine are 16 in molar ratio:Reaction equation when 5 is as follows：
32AgNO3+10C3H7NO2→32Ag+30CO2+35H2O+21N2O
When silver nitrate and alanine are 5 in molar ratio:Reaction equation when 2 is as follows：
10AgNO3+4 C3H7NO2→10Ag+12CO2+14H2O+7N2
When silver nitrate excess, reaction occurs the oxide of silver；When reducing agent alanine is excessive further, oxygen is needed
Reaction is participated in, or discharges 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 150-300 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 ~ 50nm；0.01～0.4wt.% 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≤20% 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-alanine complex liquid：Weigh 17g silver nitrate and 3.56g alanine, with distillation water dissolution,
Obtain 100 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate is 5 with the molar ratio of alanine:2, Ag in the aqueous solution of preparation
Mass of ion 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 mass of ion concentration, molar ratio is 5:2 silver nitrate-alanine network
Close liquid shaken at room temperature, soak Carbon fibe（Fabric）, soak time is 6 hours；Carbon fibe during immersion（Fabric）Ratio with complex liquid
Example is 1Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；In electric drying oven with forced convection, 40 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 10nm；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 3%.
Embodiment 2
(1) prepared by silver nitrate-alanine complex liquid：Weigh 17g silver nitrate and 3.56g alanine, with distillation water dissolution,
Obtain 18 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate is 5 with the molar ratio of alanine:2, Ag in the aqueous solution of preparation
Mass of ion 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 mass of ion concentration, molar ratio is 5:2 silver nitrate-alanine network
Close liquid shaken at room temperature, soak Carbon fibe（Fabric）, soak time is 24 hours；Carbon fibe during immersion（Fabric）Ratio with complex liquid
Example is 1Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；In electric drying oven with forced convection, 90 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 300 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 46nm；Silver carrying amount 0.4%；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 18%.
Embodiment 3
(1) prepared by silver nitrate-alanine complex liquid：Weigh 17g silver nitrate and 2.78g alanine, with distillation water dissolution,
Obtain 18 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate is 16 with the molar ratio of alanine:5, Ag in the aqueous solution of preparation
Mass of ion 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 mass of ion concentration, molar ratio is 16:5 silver nitrate-alanine network
Close liquid shaken at room temperature, soak Carbon fibe（Fabric）, soak time is 12 hours；Carbon fibe during immersion（Fabric）Ratio with complex liquid
Example 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 is removed
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 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 0.3%；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 10%.
Embodiment 4
(1) prepared by silver nitrate-alanine complex liquid：Weigh 17g silver nitrate and 3.34g alanine, with distillation water dissolution,
Obtain 36 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate is 8 with the molar ratio of alanine:3, Ag in the aqueous solution of preparation
Mass of 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 mass of ion concentration, molar ratio is 8:3 silver nitrate-alanine network
Close liquid shaken at room temperature, soak Carbon fibe（Fabric）, soak time is 12 hours；Carbon fibe during immersion（Fabric）Ratio with complex liquid
Example is 0.5Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；In 60 DEG C of hot air drying cylinders drying to constant weight, water is removed
And water of crystallization.
(3) pyrolysis：Carbon fibe after drying will be soaked（Fabric）It is warming up at 300 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 12%.
Embodiment 5
(1) prepared by silver nitrate-alanine complex liquid：Weigh 8.5g silver nitrate and 3.24g alanine, with distillation water dissolution,
Obtain 36 liters of silver-colored ammonium nitrate complex liquids.Wherein, silver nitrate is 11 with the molar ratio of alanine:4, Ag in the aqueous solution of preparation
Mass of 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 mass of ion concentration, molar ratio is 11:4 silver nitrate-alanine
Complex liquid shaken at room temperature, immersion Carbon fibe（Fabric）, soak time is 9 hours；Carbon fibe during immersion（Fabric）With complex liquid
Ratio is 0.25Kg/ liter；It is filtered dry in ventilated environment, light protected environment after immersion；In 40 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 2 hours.
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 30nm；Silver carrying amount 0.13%；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 11%.
Claims (3)
1. a kind of alanine prepares, for reducing agent, the method for carrying silver-colored Carbon fibe, it is characterised in that：
(1) prepared by silver nitrate-alanine complex liquid：Weigh silver nitrate crystal and alanine crystal, with distillation water dissolution,
Silver-colored ammonium nitrate complex liquid is obtained, silver nitrate is 3.2～2.5 with the mol ratio of alanine:1, Ag ion in the aqueous solution of preparation
Mass concentration is 0.01～0.6%；
(2) silver ion solution soaks：With the silver nitrate for preparing-alanine complex liquid shaken at room temperature, soak through carbonization, work
Carbon fibe after change process, soak time is 6～24 hours；During immersion, the ratio of Carbon fibe and complex liquid is 0.25～1Kg/
Rise；It is filtered dry in ventilation, light protected environment after immersion；Then dry in 40～90 DEG C of hot blast to constant weight, remove water and water of crystallization；
(3) pyrolysis：Silver particles are soaked Carbon fibe after drying 160-300 DEG C is warming up to, insulation is entered for 0.5～6 hour
Row thermal decomposition, using dry circulating nitrogen gas protection during thermal decomposition, or using ammonia protection is decomposed, is done using boat stove, net belt type is pushed away
Dry stove or rotary furnace continuous furnace, realize continuous production；Programming rate controls at 0.1～2 DEG C/min, it is to avoid thermal decomposition is anti-
Excessively acutely nanometer silver dispersibility and the interface binding power with carbon fiber surface should be 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
Oxidation, the baking temperature control after cleaning at 50～120 DEG C, the silver-colored remaining quantity≤10ppb of the water after cleaning, reach drinking water
Standard；
(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≤20% 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 0.01～0.40wt.% for requiring, repeat step（2）Silver ion soaks
And step（3）Pyrolysis are to increase silver carrying amount.
2. alanine as claimed in claim 1 prepares, for reducing agent, the method for carrying silver-colored Carbon fibe, it is characterised in that：Silver nitrate
Mol ratio with alanine is 3.0～2.5:1.
3. alanine as claimed in claim 1 prepares, for reducing agent, the method for carrying silver-colored Carbon fibe, it is characterised in that：Silver ion
Concentration is 0.01～0.1%.
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| CN201611173166.9A CN106436291B (en) | 2016-12-18 | 2016-12-18 | A kind of alanine is the method for the silver-colored Carbon fibe of reducing agent preparation load |
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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 CN201611173166.9A patent/CN106436291B/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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