CN106436290B - A kind of method that amion acetic acid prepares silver-series antibacterial agent fabric product with silver nitrate complexing - Google Patents
A kind of method that amion acetic acid prepares silver-series antibacterial agent fabric product with silver nitrate complexing Download PDFInfo
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- CN106436290B CN106436290B CN201611173152.7A CN201611173152A CN106436290B CN 106436290 B CN106436290 B CN 106436290B CN 201611173152 A CN201611173152 A CN 201611173152A CN 106436290 B CN106436290 B CN 106436290B
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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 present invention relates to a kind of method that amion acetic acid and silver nitrate complexing prepare silver-series antibacterial agent fabric product, by with silver nitrate and amion acetic acid complex solution, then Carbon fibe is infiltrated（Fabric）, by heat resolve and reduction, obtain the Carbon fibe of high stability（Fabric）Adsorption nano silver.It is 2~1.5 first to prepare molar ratio:The silver nitrate amion acetic acid complex liquid that 1, Ag ion concentration is 0.01~0.6%；Carbon fibe（Fabric）Ratio with complex liquid is that 0.25~1Kg/ rises immersion 6~24 hours；160 260 DEG C under circulating nitrogen gas protection, heat preservation thermal decomposition in 0.5~6 hour；Dry after clear water washing, gained nano silver grain size is 10 ~ 60nm；0.01~0.45wt.% of silver carrying amount.Present invention reduces technological processes, reduce reaction temperature, improve the silver-colored Carbon fibe of load（Fabric）Germicidal efficiency, reduce silver-colored dosage.
Description
Technical field
The present invention relates to a kind of silver-colored Carbon fibes of load（Fabric）Method.It is molten by being complexed with silver nitrate and amion acetic acid
Liquid, then infiltrate Carbon fibe（Fabric）, by heat resolve and reduction, using the reaction heat of silver nitrate and alanine complex compound,
Obtain the Carbon fibe of high stability（Fabric）Adsorption nano silver is used to prepare the side such as efficient silver-series antibacterial agent fabric product
Face.
Technical background
The invention belongs to the processing of the load silver process of silver-series antibacterial agent fabric product.
Textile is one of essential product of human lives, its daily life daily with people is closely bound up.So
And since most of textiles itself have stronger moisture pick-up properties and larger specific surface area, so easily becoming various
The place of microbial growth.Intensity, the color and luster of its own can not only be influenced by growing the textile of bacterium or other microorganisms
With resistance to performance of waiting so long, the medium for the virus that spreads germs is will also become, the health of user is endangered.So weaving antiseptic
Research and development with using just increasingly become emphasis of people's attention.
Silver system textile antibacterial agent has the anti-microbial property of broad-spectrum high efficacy, has relatively broad answer in medicine and hygiene fields
With, such as surgical instruments, contraception instrument, artificial limb medical equipment and operation dress, clothing of nurses, Wound dressing, bandage, mask etc. be medical
Protective articles.Under high pathogenic environmental, the wide spectrum of silver-series antibacterial agent, efficient, safe, lasting antibacterial functions help to resist disease
Infringement of the bacterium to human body.Silver-series antibacterial agent can also be used for filter medium, and it is anti-that silver system is added in water filtering or air filter
Microbial inoculum can not only effectively reduce bacterium, fungi and other harmful microorganisms in water or air, can also kill and remain in
The bacterium inside device is filtered, the safety that it is used and the service life for extending filter core are improved.
According to carrier difference, the silver-colored silicate antiseptic of load can be divided into, carry the phosphate-based antiseptic of silver, load silver Carbon fibe
（Fabric）Antiseptic carries silver-colored organic polymer antiseptic 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, then carry out activation charring process.Front bearing silver method there are the problem of
Silver ion mainly in solution is not easy to load in precursor fibre, and after carbonizing, activating, carbon fiber surface Argent grain point
Cloth is irregular, particle diameter is not of uniform size, and anti-microbial property is poor.
Rear bearing silver method be on the fabric prepared by the methods of physics, chemistry load silver, such as impregnate thermal decomposition method,
Immersion reduction method, composite spinning method, chemical deposition and physical sputtering method etc..Wherein impregnate thermal decomposition method, immersion reduction method is
Relatively common load silver method：1. dipping thermal decomposition method is knitted using film containing silver particles aqueous solution soakings such as silver nitrate, silver nitrates
Object is heated to~700 DEG C after dry, metallic silver is obtained using silver oxide pyrolytic.It is required that calcine under inert gas protection,
There cannot be free air infiltration to enter in calcination process and temperature-fall period, once there is free air infiltration to enter, the metallic silver easily formed can be oxidized to again
Silver oxide, end product quality are not easy to control.Infusion process simple process and low cost, pollution-free, silver is distributed in fabric surface,
Be conducive to sterilize.But the silver particles that the method prepares are mainly physical absorption, and silver is easy to be lost in, and cannot reach and persistently to sterilize
Effect.2. immersion reduction method is to soak the fabric into Ag-containing solution a period of time, then with a kind of reducing agent silver ion also
Original at elemental silver process.With NaBH4For reduction, detailed process is fabric activation process, is soaked for a long time under the conditions of being protected from light
Stain is to AgNO3In solution, it is washed with distilled water later until without silver ion detection in cleaning solution, is then immersed in NaBH again4Solution
In, washing removes extra NaBH4, dry for a long time in cryogenic vacuum.The good combination of fabric and Argent grain may be implemented in the method.
But reduction method process flow is long；It needs repeatedly to wash, water consumption is big, and water resource requires high；Use be protected from light, the techniques such as vacuum, if
It is standby to require height；And Argent grain is mainly distributed in reunion shape in the outer surface and hole of fabric, and the Argent grain of load is bigger, and
Germicidal efficiency is not high.
Nano silver is a concentration of 30 × 10-6When, there is preferable antibacterial activity, but there are potential cytotoxicities；
3×10-6Under concentration, 2 grades of cytotoxicity.How to reduce its cytotoxicity problem and should give attention.Currently, reducing silver system antibacterial
The strategy of agent toxicity mainly controls it and discharges concentration of silver ions higher than minimum inhibitory concentration, is less than human body highest safe concentration.
For the silver-series antibacterial agent applied to fields such as medical dressing, air and purification of water quality, it should also be noted that falling off for Argent grain is avoided,
Because the amount of falling off of Argent grain directly affects silver ion burst size, the service life and antibacterial duration of antiseptic can be also influenced.
Invention content
The object of the present invention is to provide a kind of load silver Carbon fibes with efficient, lasting bactericidal effect（Fabric）Preparation side
Method.
The technical solution adopted by the present invention to solve the technical problems is complexing to occur with silver particles using a kind of
Reducing agent, silver ion is adsorbed on Carbon fibe with complex form（Fabric）Surface and micropore in, then in lower temperature
The lower quickly reduction of degree is decomposed, the load silver Carbon fibe for obtaining good dispersion, not easily runing off（Fabric）, it is as follows：
(1) prepared by silver nitrate-amion acetic acid complex liquid：A certain amount of silver nitrate crystal and amion acetic acid crystal are weighed, is used
Water dissolution is distilled, silver-colored ammonium nitrate complex liquid is obtained.Wherein, the molar ratio of silver nitrate and amion acetic acid is 2:1~1.5:1 it
Between, Ag mass of ions a concentration of 0.01~0.6% in the aqueous solution of preparation.
(2) silver ion immersion, dry Carbon fibe（Fabric）：It is shaken with prepared silver nitrate-alanine complex liquid room temperature
It swings, impregnate the Carbon fibe after charing, activation process（Fabric）, soaking time is 6~24 hours；Carbon fibe when immersion（Fabric）
Ratio with complex liquid is 0.25~1Kg/ liters；It is filtered dry in ventilated environment, light protected environment after immersion；Then in hot wind, such as electric heating
Air dry oven, 50~100 DEG C of dryings to constant weight remove water and the crystallization water.
(3) pyrolysis：Carbon fibe after drying will be impregnated（Fabric）It is warming up at 160-260 DEG C, soaking time is
0.5~6 hour.It is protected using dry circulating nitrogen gas when thermal decomposition, can also be used when having ready conditions and decompose ammonia protection.Using pushing away boat
The continuous furnaces such as stove, net belt type drying oven, rotary furnace can realize continuous production.Heating rate is controlled at 0.1~2 DEG C/min,
Pyrolysis is avoided excessively acutely to influence nano silver dispersibility and and Carbon fibe（Fabric）The interface binding power on surface.
(4) it washs：By above-mentioned Carbon fibe（Fabric）With pure water washing 2~4 times, remaining reactant is washed away.In order to keep away
Exempt from silver particles oxidation, the drying temperature after cleaning is controlled at 50~120 DEG C.Silver-colored remaining quantity≤10ppb of water after cleaning（It is micro-
Grams per liter), reach the standard of drinking water.
(5) it detects：Every batch of is using sodium sulfocyanate standard solution titration determination silver carrying amount, scanning electron microscopic observation Argent grain
Morphology and size, and in 25 DEG C, 150 r/min, constant temperature oscillation is after 600 hours, with resisting for the swollen Spectrophotometric Determination of Silver of double sulphur
Flow and failure property, silver-colored turnover rate≤25%, silver carrying amount is by Carbon fibe specific surface and absorption property, complex liquid silver content, soaking technology
With the influence of the parameter of thermal decomposition process step is repeated when silver carrying amount is less than 0.01 desired~0.45wt.%（2）Silver ion
Immersion, dry Carbon fibe and step（3）Pyrolysis is to increase silver carrying amount.
The molar ratio of silver nitrate and amion acetic acid is 1.8~1.5:1.
Ag ion concentrations are 0.01~0.1% in the aqueous solution of preparation.
By silver nitrate (AgNO3) as oxidant, amion acetic acid (C2H5NO2) as complexing reducing agent, it is configured to water-soluble
Liquid；Solution, which is gradually evaporated, can form gel.This gel can react rapidly at 160~260 DEG C, release bulk gas and heat
Amount, the nano level superfine silver powder that can be disperseed.Amion acetic acid (H has occurred first during this2N-CH2- COOH)
There is NH in hydrolysis4 +.With the progress of heating, water evaporation, the NH in solution4 +And NO3 -Ion is then with NH4NO3The shape of crystal
Formula is precipitated, and finally obtains AgOH, Ag2O and NH4NO3The mixture of crystal.Above-mentioned mixed crystal further heats, it may occur that
Complicated decomposition reaction, nano silver and CO are obtained2、H2O、N2O、N2Equal gases.
When silver nitrate and amion acetic acid are 2 in molar ratio:Reaction equation when 1 is as follows：
4AgNO3+2C2H5NO2→4Ag+4CO2+5H2O+3N2O
When silver nitrate and amion acetic acid are 3 in molar ratio:Reaction equation when 2 is as follows：
6AgNO3+4C2H5NO2→6Ag+8CO2+10H2O+5N2
When silver nitrate excess, reaction will appear the oxide of silver, but due to exothermic heat of reaction, local temperature increases, silver-colored
Oxidation product decomposes and obtains elemental silver；When reducing agent amion acetic acid is further excessive, oxygen is needed to participate in reaction, or release
Release ammonia.
The present invention carries silver-colored Carbon fibe for producing（Fabric）, have the characteristics that reaction temperature is low and efficient, usually 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, reduce reaction temperature, avoid the occurrence of due to pyroreaction and caused by Ag particles combined not with carbon surface
Jail and easily there is the problem of silver oxide.Compared with conventional reduction method, reduce dipping time, and due to of the present invention
Ag compounds are complexed and decompose generation bulk gas such as NH3、H2O、CO2、N2, N2O etc. makes the Ag nano particles to be formed disperse, overcomes
General N aBH4Reduction prepares Ag particle agglomeration phenomenons, carries high silver supported Carbon fibe（Fabric）Germicidal efficiency, reduce silver-colored dosage.
Present invention process process is simple, easily operated, yield is high, is easy to industrialized production, have it is clean, environmentally protective and
Characteristics of energy saving.Gained nano silver grain size is 10 ~ 60nm；0.01~0.45wt.% of silver carrying amount；Argent grain and Carbon fibe（Fabric）Knot
Resultant force is high, 150r/min, is vibrated in 25 DEG C of thermostatted waters, after 600 hours, silver-colored turnover rate≤25%；Argent grain good dispersion kills
Bacterium is efficient.
Specific implementation mode
It elaborates to the present invention below by way of specific embodiment.
Embodiment 1
(1) prepared by silver nitrate-amion acetic acid complex liquid：17g silver nitrates and 5.0g amion acetic acids are weighed, it is water-soluble with distilling
Solution obtains 100 liters of silver-colored ammonium nitrate complex liquids.Wherein, the molar ratio of silver nitrate and amion acetic acid is 3:2, the aqueous solution of preparation
Middle Ag ion concentrations are about 0.01%.
(2) silver ion immersion, dry Carbon fibe（Fabric）By the Carbon fibe after charing, activation process（Fabric）With steaming
Distilled water is cleaned, dries, is cooled.It is about 0.01% with Ag ion concentrations, molar ratio 3:2 silver nitrate-amion acetic acid complex liquid
Shaken at room temperature impregnates Carbon fibe（Fabric）, soaking time is 6 hours；Carbon fibe when immersion（Fabric）Ratio with complex liquid is
1Kg/ liters；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
The crystallization water.
(3) pyrolysis：Carbon fibe after drying will be impregnated（Fabric）It is warming up at 160 DEG C, soaking time is 6 hours.
Using drying in dry circulating nitrogen gas protection tube furnace when thermal decomposition, heating rate is 2 DEG C/min.
(4) it washs：By above-mentioned Carbon fibe（Fabric）With pure water washing 2 times, remaining reactant is washed away.After cleaning
Electric drying oven with forced convection, 50 DEG C of dryings to constant weight.
(5) it detects：Gained nano silver grain size is 25nm；Silver carrying amount 0.01%；Argent grain and Carbon fibe（Fabric）Binding force
Height, 150r/min vibrate in 25 DEG C of thermostatted waters, and after 600 hours, silver-colored turnover rate is 12%.
Embodiment 2
(1) prepared by silver nitrate-amion acetic acid complex liquid：17g silver nitrates and 5.0g amion acetic acids are weighed, it is water-soluble with distilling
Solution obtains 18 liters of silver-colored ammonium nitrate complex liquids.Wherein, the molar ratio of silver nitrate and amion acetic acid is 3:2, in the aqueous solution of preparation
Ag ion concentrations are about 0.6%.
(2) silver ion immersion, dry Carbon fibe（Fabric）：By the Carbon fibe after charing, activation process（Fabric）With steaming
Distilled water is cleaned, dries, is cooled.It is about 0.6% with Ag ion concentrations, molar ratio 3:2 silver nitrate-amion acetic acid complex liquid
Shaken at room temperature impregnates Carbon fibe（Fabric）, soaking time is 24 hours；Carbon fibe when immersion（Fabric）Ratio with complex liquid is
1Kg/ liters；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 the crystallization water.
(3) pyrolysis：Carbon fibe after drying will be impregnated（Fabric）It is warming up at 260 DEG C, soaking time is 0.5 small
When.It is protected using dry circulating nitrogen gas at 0.1 DEG C/min using net belt type drying oven, heating rate control when thermal decomposition.
(4) it washs：By above-mentioned Carbon fibe（Fabric）With pure water washing 4 times, remaining reactant is washed away.It is used in after cleaning
In net belt type drying oven, 120 DEG C of dryings to constant weight.
(5) it detects：Gained nano silver grain size is 58nm；Silver carrying amount 0.44%；Argent grain and Carbon fibe（Fabric）Binding force
Height, 150r/min vibrate in 25 DEG C of thermostatted waters, and after 600 hours, silver-colored turnover rate is 24%.
Embodiment 3
(1) prepared by silver nitrate-amion acetic acid complex liquid：17g silver nitrates and 3.8g amion acetic acids are weighed, it is water-soluble with distilling
Solution obtains 18 liters of silver-colored ammonium nitrate complex liquids.Wherein, the molar ratio of silver nitrate and amion acetic acid is 2:1, in the aqueous solution of preparation
Ag ion concentrations are about 0.6%.
(2) silver ion immersion, dry Carbon fibe（Fabric）：By the Carbon fibe after charing, activation process（Fabric）With steaming
Distilled water is cleaned, dries, is cooled.It is about 0.6% with Ag ion concentrations, molar ratio 2:1 silver nitrate-amion acetic acid complex liquid
Shaken at room temperature impregnates Carbon fibe（Fabric）, soaking time is 12 hours；Carbon fibe when immersion（Fabric）Ratio with complex liquid is
0.25Kg/ liters；It is filtered dry in ventilated environment, light protected environment after immersion；It is dried to constant weight in 80 DEG C of heated-air drying cylinders, removes water and knot
Brilliant water.
(3) pyrolysis：Carbon fibe after drying will be impregnated（Fabric）It is warming up at 200 DEG C, soaking time is 3 hours.
Boat drying oven, heating rate control are pushed away at 0.5 DEG C/min using automatic when thermal decomposition, are protected using dry circulating nitrogen gas.
(4) it washs：By above-mentioned Carbon fibe（Fabric）With pure water washing 3 times, remaining reactant is washed away.It is used in after cleaning
Automatically boat drying oven, 110 DEG C of dryings to constant weight are pushed away.
(5) it detects：Gained nano silver grain size is 60nm；Silver carrying amount 0.32%；Argent grain and Carbon fibe（Fabric）Binding force
Height, 150r/min vibrate in 25 DEG C of thermostatted waters, and after 600 hours, silver-colored turnover rate is 14%.
Embodiment 4
(1) prepared by silver nitrate-amion acetic acid complex liquid：17g silver nitrates and 4.68g amion acetic acids are weighed, it is water-soluble with distilling
Solution obtains 36 liters of silver-colored ammonium nitrate complex liquids.Wherein, the molar ratio of silver nitrate and amion acetic acid is 1.6:1, the aqueous solution of preparation
Middle Ag ion concentrations are about 0.3%.
(2) silver ion immersion, dry Carbon fibe（Fabric）：By the Carbon fibe after charing, activation process（Fabric）With steaming
Distilled water is cleaned, dries, is cooled.It is about 0.3% with Ag ion concentrations, molar ratio 1.6:1 silver nitrate-amion acetic acid complexing
Liquid shaken at room temperature impregnates Carbon fibe（Fabric）, soaking time is 12 hours；Carbon fibe when immersion（Fabric）With the ratio of complex liquid
For 0.5Kg/ liters；It is filtered dry in ventilated environment, light protected environment after immersion；Dried to constant weight in 100 DEG C of heated-air drying cylinders, removing water and
The crystallization water.
(3) pyrolysis：Carbon fibe after drying will be impregnated（Fabric）It is warming up at 220 DEG C, soaking time is 3 hours.
Boat drying oven, heating rate control are pushed away at 0.5 DEG C/min using automatic when thermal decomposition, are protected using dry circulating nitrogen gas.
(4) it washs：By above-mentioned Carbon fibe（Fabric）With pure water washing 2 times, remaining reactant is washed away.It is used after cleaning
Automatically boat drying oven, 120 DEG C of dryings to constant weight are being pushed away.
(5) it detects：Gained nano silver grain size is 30nm；Silver carrying amount 0.3%；Argent grain and Carbon fibe（Fabric）Binding force is high,
150r/min vibrates in 25 DEG C of thermostatted waters, and after 600 hours, silver-colored turnover rate is 14%.
Embodiment 5
(1) prepared by silver nitrate-amion acetic acid complex liquid：8.5g silver nitrates and 4.4g amion acetic acids are weighed, it is water-soluble with distilling
Solution obtains 36 liters of silver-colored ammonium nitrate complex liquids.Wherein, the molar ratio of silver nitrate and amion acetic acid is 1.7:1, the aqueous solution of preparation
Middle Ag ion concentrations are about 0.15%.
(2) silver ion immersion, dry Carbon fibe（Fabric）：By the Carbon fibe after charing, activation process（Fabric）With steaming
Distilled water is cleaned, dries, is cooled.It is about 0.15% with Ag ion concentrations, molar ratio 1.7:1 silver nitrate-amion acetic acid complexing
Liquid shaken at room temperature impregnates Carbon fibe（Fabric）, soaking time is 9 hours；Carbon fibe when immersion（Fabric）With the ratio of complex liquid
For 0.25Kg/ liters；It is filtered dry in ventilated environment, light protected environment after immersion；Dried to constant weight in 90 DEG C of heated-air drying cylinders, removing water and
The crystallization water.
(3) pyrolysis：Carbon fibe after drying will be impregnated（Fabric）It is warming up at 200 DEG C, soaking time is 2 hours.
Tube furnace, heating rate is protected to control at 1 DEG C/min using dry circulating nitrogen gas when thermal decomposition.
(4) it washs：By above-mentioned Carbon fibe（Fabric）With pure water washing 2 times, remaining reactant is washed away.It is used after cleaning
90 DEG C of air dry ovens are dried to constant weight.
(5) it detects：Gained nano silver grain size is 25nm；Silver carrying amount 0.03%；Argent grain and Carbon fibe（Fabric）Binding force
Height, 150r/min vibrate in 25 DEG C of thermostatted waters, and after 600 hours, silver-colored turnover rate is 9%.
Claims (3)
1. a kind of method that amion acetic acid prepares silver-series antibacterial agent fabric product with silver nitrate complexing, it is characterised in that including following step
Suddenly：
(1) prepared by silver nitrate-amion acetic acid complex liquid：A certain amount of silver nitrate crystal and amion acetic acid crystal are weighed, with distillation
The molar ratio of water dissolution, acquisition silver nitrate-amion acetic acid complex liquid, silver nitrate and amion acetic acid is 2~1.5:1, the water of preparation
Ag mass of ions a concentration of 0.01~0.6% in solution；
(2) silver ion immersion, dry Carbon fibe：With prepared silver nitrate-amion acetic acid complex liquid shaken at room temperature, impregnate warp
Carbon fibe after charing, activation process, soaking time are 6~24 hours；The ratio of Carbon fibe and complex liquid is 0.25 when immersion
~1Kg/ liters；It is filtered dry in ventilation, light protected environment after immersion；Then in electric drying oven with forced convection, 50~100 DEG C of dryings to constant weight,
Remove water and the crystallization water；
(3) pyrolysis：Carbon fibe is warming up to 160-260 DEG C after drying will be impregnated, and keeps the temperature 0.5~6 hour and carries out heat point
Solution is protected using dry circulating nitrogen gas when thermal decomposition, or using decomposing ammonia protection；Using push away boat stove, net belt type drying oven or
Rotary furnace realizes continuous production；Heating rate is controlled at 0.1~2 DEG C/min, and pyrolysis is avoided excessively acutely to influence
Nano silver dispersibility and the interface binding power with carbon fiber surface；
(4) it washs：Above-mentioned Carbon fiber Wesy pure water is washed 2~4 times, remaining reactant is washed away；In order to avoid silver particles oxygen
Change, the drying temperature after cleaning is controlled at 50~120 DEG C, and silver-colored remaining quantity≤10ppb of the water after cleaning reaches the mark of drinking water
It is accurate；
(5) it detects：Every batch of is using sodium sulfocyanate standard solution titration determination silver carrying amount, scanning electron microscopic observation Argent grain pattern
And size, and in 25 DEG C, 150 r/min, constant temperature oscillation after 600 hours, lose by the anti-current that silver is measured with dithizone spectrophotometry
Performance, silver-colored turnover rate≤25%, silver carrying amount is by Carbon fibe specific surface and absorption property, complex liquid silver content, soaking technology and heat
The influence of the parameter of decomposition technique repeats step when silver carrying amount is less than 0.01 desired~0.45wt.%（2）Silver ion soaks
Bubble, dry Carbon fibe and step（3）Pyrolysis is to increase silver carrying amount.
2. the method that amion acetic acid as described in claim 1 prepares silver-series antibacterial agent fabric product with silver nitrate complexing, feature
It is：The molar ratio of silver nitrate and amion acetic acid is 1.8~1.5:1.
3. the method that amion acetic acid as described in claim 1 prepares silver-series antibacterial agent fabric product with silver nitrate complexing, feature
It is：Step（1）Ag ion concentrations are 0.01~0.1% in the aqueous solution of preparation.
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| 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 |
-
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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