CN102717094A - In-situ synthesis method of nanosilver - Google Patents
In-situ synthesis method of nanosilver Download PDFInfo
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- CN102717094A CN102717094A CN2012101908486A CN201210190848A CN102717094A CN 102717094 A CN102717094 A CN 102717094A CN 2012101908486 A CN2012101908486 A CN 2012101908486A CN 201210190848 A CN201210190848 A CN 201210190848A CN 102717094 A CN102717094 A CN 102717094A
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Abstract
The invention discloses an in-situ synthesis method of nanosilver, which comprises the following steps: carrying out surface treatment on a carrier with aminosilane, immersing the carrier in a silver ion solution, and reducing the silver ions attached to the carrier surface into neutral silver particles by using a strong reducer. Aminosilane is hydrolyzed in anhydrous alcohol to generate silanol, and the silanol is combined with hydroxy group and carboxy group on the carrier surface to implement dehydration, so that the aminosilane is firmly attached onto the carrier surface and the carrier surface obtains the amino group; under the interaction between the amino group and the silver ion, the silver ions are firmly attached onto the carrier surface; and after the silver ions are reduced into silver atoms, since the amino group carries high-density negative charges, the charge density on the carrier surface is increased, so that the migration rate of the silver atoms on the carrier surface is limited, and the reduced silver atoms can only generate small nano silver particles on the restricted carrier surface.
Description
Technical field
The invention belongs to field of new, be specifically related to the method that a kind of Nano Silver is uploaded carrier.
Background technology
Nano Silver be a kind of particle diameter in 100 nanometers with interior particle, wire or flake nano material.Different with traditional silver powder material, this material shows good physical and chemical performance and comes into one's own on nanoscale.General many sizes that obtains Nano Silver and control Nano Silver with reducing agent and coating material.The size of Nano Silver directly influences the application characteristic of Nano Silver.And be Nano Silver key in application place with firm the uploading or be adhered on the carrier of Nano Silver.
Nano Silver extensively is used as the disinfecting, antimicrobial material at present, also can do electrocondution slurry.General Nano Silver is used chemical reduction method as anti-biotic material and electrocondution slurry more.As antibiotic and antibacterial material, mainly be to obtain nano silver colloid through chemical reduction method or electrolytic method.This colloid can be directly or dilution after be used for sterilization or antibacterial processing, also can be used for relevant Nano Silver product, as mix Nano Silver plastic products, mix the textile of Nano Silver and mix the coating etc. of Nano Silver.When Nano Silver was uploaded carrier material, Nano Silver was attached on the carrier.Because the restriction of carrier surface Nano Silver concentration will cause the antibacterial ability of the Nano Silver of unit mass to descend greatly.Though also can nano silver colloid be adhered to relevant carrier surface through bonding agent, limit by the carrier surface chemical property, the adhesive force that causes Nano Silver very a little less than, make the antibacterial bacteriostatic ability drop of unit mass Nano Silver.
In addition; Though can improve carrying capacity on the Nano Silver of textile surface through textile being carried out surface treatment (as handling) through surface conditioning agent; But the adhesive force of its Nano Silver is still limited, can not satisfy the repeatedly requirement of conventional washing of Nano Silver textile.
Summary of the invention
The purpose of this invention is to provide the in-situ synthetic method that is stated from different carriers on a kind of Nano Silver.
According to an aspect of the present invention, a kind of method of original position synthesizing nano-silver is provided, concrete preparation process is following:
Step 1: it is dry that water and alcohol clean up the back with carrier, and the carrier of drying is carried out preliminary treatment, makes carrier surface obtain hydroxyl and carboxyl, and the ethanol solution of more said carrier being put into amino silane soaks, and it is amino that carrier surface is obtained;
Step 2: the carrier impregnation that will pass through step 1 processing makes said carrier surface absorption silver ion in silver ion solution;
Step 3: the carrier impregnation that will pass through step 2 processing makes the silver ion reduction of carrier surface become the center nano silver particles in reducing agent.
In some embodiments, make carrier surface obtain hydroxyl and carboxyl through plasma discharge method or acid and alkali corrosion method.
In some embodiments, carrier is all-cotton fabric or sponge or nylon wire or aluminium flake or pottery.
In some embodiments, the volume fraction of the ethanol solution of the amino silane in the step 1 is 2～10%.
In some embodiments, all-cotton fabric soak time in the ethanol solution of amino silane is 100～110 minutes.
In some embodiments, the silver ion solution concentration in the step 2 is 0.2～20mmol/L.
In some embodiments, all-cotton fabric dip time in silver ion solution of handling through step 1 is 5～6 minutes.
In some embodiments, the reducing agent in the step 3 is sodium borohydride or hydrazine hydrate or ammoniacal liquor.
In some embodiments, the concentration of the strong reductant in the step 3 is 8～12mmol/L.
In some embodiments, 4～5 minutes time that the all-cotton fabric of handling through step 2 soaks in reducing agent.
Amino silane hydrolysis in absolute ethyl alcohol generates silanol, and silanol combines dehydration with the hydroxyl and the carboxyl of carrier surface, thereby amino silane makes carrier surface obtain amino firmly attached on the carrier surface; Amino interaction with silver ion makes the silver ion firm attachment at carrier surface; Silver ion is reduced into silver atoms; Because of amino has highdensity negative electrical charge; Increased the charge density of carrier surface, made silver atoms limited in the migration velocity of carrier surface, the silver atoms of reduction can only generate less nano silver particles at the carrier surface that is obstructed.
Description of drawings
The sem photograph of the product that Fig. 1 obtains for embodiment one;
Sem photograph after the product that Fig. 2 obtains for embodiment one washs through 50 national standards;
The nano silver particles transmission electron microscope photo that the product that Fig. 3 obtains for embodiment one has been washed after through the washing of 50 national standards;
Fig. 4 relation of the concentration of the last carrying capacity of Nano Silver and liquor argenti nitratis ophthalmicus on the carrier when being carrier with the all-cotton fabric.
The specific embodiment
Below in conjunction with specific embodiment the present invention is further described.
Instance one
The cotton textile that Nano Silver is handled: use pure water and alcohol to distinguish ultrasonic cleaning 5 minutes all-cotton fabric, so that clean its surperficial pollutant and greasy dirt, air dry.The all-cotton fabric surface itself has hydroxyl and carboxyl.Then all-cotton fabric being put into volume fraction is that the ethanol solution of 5% 3-aminopropyltriethoxywerene werene soaked 100 minutes; Then air dry; Then the liquor argenti nitratis ophthalmicus of putting into 6mmol/L behind the fabric was flooded 5 minutes, then all-cotton fabric is thrown away unnecessary silver nitrate through roll.Then treated all-cotton fabric being put into concentration is that the sodium borohydride solution of 10mmol/L soaks reaction 5 minutes, uses water rinse at last, and 120 ° of C are dry down.Just can just obtain the neutral nano silver particles of growth in situ after accomplishing on the surface of all-cotton fabric.The hydrolysis in absolute ethyl alcohol of 3-TSL 8330 generates silanol, and silanol combines dehydration with the hydroxyl on all-cotton fabric surface with carboxyl, thereby amino silane firmly on the surface attached to all-cotton fabric makes the surperficial acquisition amino of all-cotton fabric.Because amino interaction with silver ion makes silver ion pass through amino securely attached on the all-cotton fabric.Silver ion is reduced into silver atoms; Because of amino has highdensity negative electrical charge; Increased the charge density of carrier surface, made silver atoms limited in the migration velocity on all-cotton fabric surface, the silver atoms of reduction can only generate less nano silver particles on the all-cotton fabric surface of being obstructed.
The last carrying capacity of measuring Nano Silver on the cotton fabric with atomic absorption spectrography (AAS) can be up to 800 micrograms/square centimeter/gram.
Fig. 1 is the sem photograph of the Nano Silver of the growth in situ on the carrier all-cotton fabric, can find out that a large amount of Nano Silvers is attached on the carrier.
Fig. 2 is the sem photograph after the Nano Silver of growth in situ on the carrier all-cotton fabric washs through 50 national standards, can find out after washing, more a large amount of Nano Silvers is still arranged attached on the carrier.
As shown in Figure 3, the transmission electron microscope picture of the nano silver particles that is washed down on the all-cotton fabric, as can be seen from the figure, the particle diameter of nano silver particles is between 5 ~ 25nm.
Can find out that by Fig. 4 along with the rising of liquor argenti nitratis ophthalmicus concentration, carrying capacity is also increasing on the Nano Silver on the all-cotton fabric, and as can be seen from Figure 4 on the carrier the last carrying capacity of Nano Silver all higher.
Instance two
The cotton textile that Nano Silver is handled: use pure water and alcohol to distinguish ultrasonic cleaning 5 minutes all-cotton fabric, so that clean its surperficial pollutant and greasy dirt, air dry.The cotton textile surface has hydroxyl and carboxyl.Then all-cotton fabric being put into volume fraction is that the ethanol solution of 5% 3-aminopropyltriethoxywerene werene soaked 110 minutes; Then air dry; Wait in the liquor argenti nitratis ophthalmicus that puts it into 6mmol/L after the fabric cools down dipping then 6 minutes, and then all-cotton fabric was thrown away unnecessary silver nitrate through roll.Then treated all-cotton fabric being put into concentration is that the sodium borohydride solution of 10mmol/L soaks reaction 4 minutes, uses water rinse at last, and 120 ° of C are dry down.Just can just obtain the neutral nano silver particles of growth in situ after accomplishing on the surface of all-cotton fabric.The hydrolysis in absolute ethyl alcohol of 3-TSL 8330 generates silanol, and silanol combines dehydration with the hydroxyl on all-cotton fabric surface with carboxyl, thereby amino silane firmly on the surface attached to all-cotton fabric makes the surperficial acquisition amino of all-cotton fabric.Because amino the interaction with silver ion makes silver ion pass through amino securely attached on the all-cotton fabric.Silver ion is reduced into silver atoms; Because of amino has highdensity negative electrical charge; Increased the charge density of carrier surface, made silver atoms limited in the migration velocity on all-cotton fabric surface, the silver atoms of reduction can only generate less nano silver particles on the all-cotton fabric surface of being obstructed.
Instance three
The sponge that Nano Silver is handled: use pure water and alcohol to distinguish ultrasonic cleaning 5 minutes sponge, so that it is clean its surperficial pollutant and greasy dirt, dry under 80 ° of C conditions.Make the sponge surface obtain hydroxyl and carboxyl through the acid corrosion method in the present embodiment.It is 10% sulfuric acid that sponge is put into concentration, soaks 5 minutes, then sponge is immersed in the water washing 10 minutes, at last under 60 ℃ condition, dries, and makes sponge surface acquisition hydroxyl and carboxyl.Then sponge being put into volume fraction is that the ethanol solution of 2% aminoethyl aminopropyl triethoxysilane soaked 120 minutes; Then dry under the condition of 80 ° of C; Put it in the liquor argenti nitratis ophthalmicus that concentration is 2mmol/L after waiting sponge to cool off then and soaked 10 minutes, the sponge that then will adsorb silver nitrate dries on 6 rev/mins drier.Put it into then in the hydrazine hydrate solution that concentration is 12mmol/L and to soak reaction 3 minutes, use purified rinse water at last, 120 ° of C dryings just obtain the nano silver particles of growth in situ on the surface of sponge.The hydrolysis in absolute ethyl alcohol of aminoethyl aminopropyl triethoxysilane generates silanol, and silanol combines dehydration with the hydroxyl on sponge surface with carboxyl, thereby amino silane firmly on the surface attached to sponge makes the surperficial acquisition amino of sponge.Because amino interaction with silver ion makes silver ion pass through amino securely attached on the sponge.Silver ion is reduced into silver atoms; Because of amino has highdensity negative electrical charge; Increased the charge density of carrier surface, made silver atoms limited in the migration velocity on sponge surface, the silver atoms of reduction can only generate less nano silver particles on the sponge surface of being obstructed.
Instance four
The nylon wire that Nano Silver is handled: use pure water and alcohol to distinguish ultrasonic cleaning 6 minutes nylon wire, so that clean its surperficial pollutant and greasy dirt, air dry.Make the surface of nylon wire obtain hydroxyl and carboxyl with the plasma discharge method in the present embodiment.Present embodiment adopts oxygen plasma treatment in the PDC-002 plasma surface treatment appearance of German Harrick Plasma company; The setup parameter radio frequency is 200 watts; Oxygen pressure is 266.644 handkerchiefs, and the spacing of discharge target and processing unit is 15 millimeters, and the processing time is 30 seconds.Processing makes the nylon wire surface obtain hydroxyl and carboxyl.Then nylon wire being put into volume fraction is that the ethanol solution of N-aminoethyl-3-aminopropyl methyl dimethoxysilane of 6% soaked 80 minutes; Then air dry; Put it in the liquor argenti nitratis ophthalmicus that concentration is 0.2mmol/L after waiting nylon wire to cool off then and soaked 20 minutes, the nylon wire that then will adsorb silver nitrate dries on 5 rev/mins drier.Put it into then and soak reaction 10 minutes in the ammoniacal liquor that concentration is 8mmol/L, at last with running water flushing, 120 ° of C dryings.Just obtain the nano silver particles of growth in situ on the nylon wire surface.The hydrolysis in absolute ethyl alcohol of N-aminoethyl-3-aminopropyl methyl dimethoxysilane generates silanol, and silanol combines dehydration with the hydroxyl on nylon wire surface with carboxyl, thereby amino silane firmly on the surface attached to nylon wire makes the surperficial acquisition amino of nylon wire.Because amino the interaction with silver ion makes silver ion pass through amino securely attached on the nylon wire.Silver ion is reduced into silver atoms; Because of amino has highdensity negative electrical charge; Increased the charge density of carrier surface, made silver atoms limited in the migration velocity on nylon wire surface, the silver atoms of reduction can only generate less nano silver particles on the nylon wire surface of being obstructed.
Embodiment five
The aluminium flake that Nano Silver is handled: use pure water and alcohol to distinguish ultrasonic cleaning 5 minutes aluminium flake, so that it is clean its surperficial pollutant and greasy dirt, dry under the condition of 80 ° of C.The aluminium flake surface itself just has hydroxyl and carboxyl.Then aluminium flake being put into volume fraction is that the ethanol solution of γ-aminoethyl aminopropyl trimethoxysilane of 8% soaked 60 minutes; Then dry under the condition of 80 ° of C; Put it in the liquor argenti nitratis ophthalmicus that concentration is 20mmol/L after waiting aluminium flake to cool off then and soaked 25 minutes; Then, again large quantity of moisture on the aluminium flake is got rid of, put it into then and soak reaction 10 minutes in the sodium borohydride solution that concentration is 8mmol/L with the silver nitrate flush away of pure water with not complexing residual on the aluminium flake.At last with running water flushing, 120 ° of C dryings.On aluminium flake, just get the nano silver particles of growth in situ.The hydrolysis in absolute ethyl alcohol of γ-aminoethyl aminopropyl trimethoxysilane generates silanol, and silanol combines dehydration with the hydroxyl and the carboxyl on aluminium flake surface, thereby amino silane makes that firmly attached on the aluminium flake surface acquisition of aluminium flake surface is amino.Because amino the interaction with silver ion makes silver ion pass through amino securely attached on the aluminium flake.Silver ion is reduced into silver atoms; Because of amino has highdensity negative electrical charge; Increased the charge density of carrier surface, made silver atoms limited in the migration velocity on aluminium flake surface, the silver atoms of reduction can only generate less nano silver particles on the aluminium flake surface of being obstructed.
Embodiment six
The pottery that Nano Silver is handled: use pure water and alcohol to distinguish ultrasonic cleaning 5 minutes potsherd, so that clean its surperficial pollutant and greasy dirt, air dry.Make ceramic surface obtain a large amount of hydroxyl and carboxyl through alkaline etching in the present embodiment.It is that 0.3% sodium hydroxide solution soaked 3 minutes that the pottery of drying is put into concentration, cleans up the back and takes out oven dry, can obtain hydroxyl and carboxyl on the ceramic surface.Then potsherd being put into volume fraction is that the ethanol solution of 10% 3-aminopropyltriethoxywerene werene soaked 40 minutes; Then air dry; Put it in the liquor argenti nitratis ophthalmicus that concentration is 16mmol/L after waiting potsherd to cool off then and soaked 30 minutes; Then, get rid of going up large quantity of moisture on the aluminium flake again, put it into then and soak reaction 6 minutes in the sodium borohydride solution that concentration is 10mmol/L with the silver nitrate flush away of pure water with not complexing residual on the aluminium flake.Use purified rinse water at last, 120 ° of C dryings.On potsherd, obtain the nano silver particles of growth in situ.The hydrolysis in absolute ethyl alcohol of 3-aminopropyltriethoxywerene werene generates silanol, and silanol combines dehydration with the hydroxyl and the carboxyl of ceramic surface, thereby amino silane makes ceramic surface obtain amino firmly attached on the ceramic surface.Because amino interaction with silver ion makes silver ion pass through amino securely attached on the pottery.Silver ion is reduced into silver atoms; Because of amino has highdensity negative electrical charge; Increased the charge density of carrier surface, made silver atoms limited in the migration velocity of ceramic surface, the silver atoms of reduction can only generate less nano silver particles at the ceramic surface that is obstructed.
Claims (10)
1. the method for original position synthesizing nano-silver, concrete preparation process is following:
Step 1: it is dry that water and alcohol clean up the back with carrier, and the carrier of drying is carried out preliminary treatment, makes carrier surface obtain hydroxyl and carboxyl, and the ethanol solution of more said carrier being put into amino silane soaks, and it is amino that carrier surface is obtained;
Step 2: the carrier impregnation that will pass through step 1 processing makes said carrier surface absorption silver ion in silver ion solution;
Step 3: the carrier impregnation that will pass through step 2 processing makes the silver ion reduction of carrier surface become neutral nano silver particles in reducing agent.
2. the method for original position synthesizing nano-silver according to claim 1 is characterized in that, makes carrier surface obtain hydroxyl and carboxyl through plasma discharge method or acid and alkali corrosion method.
3. the method for original position synthesizing nano-silver according to claim 1 is characterized in that, said carrier is all-cotton fabric or sponge or nylon wire or aluminium flake or pottery.
4. the method for original position synthesizing nano-silver according to claim 1 is characterized in that, the volume fraction of the ethanol solution of the amino silane in the said step 1 is 2～10%.
5. the method for original position synthesizing nano-silver according to claim 3 is characterized in that, said all-cotton fabric soak time in the ethanol solution of amino silane is 100～110 minutes.
6. the method for original position synthesizing nano-silver according to claim 1 is characterized in that, the silver ion solution concentration in the said step 2 is 0.2～20mmol/L.
7. the method for original position synthesizing nano-silver according to claim 3 is characterized in that, said all-cotton fabric dip time in silver ion solution of handling through step 1 is 5～6 minutes.
8. the method for original position synthesizing nano-silver according to claim 1 is characterized in that, the reducing agent in the said step 3 is sodium borohydride or hydrazine hydrate or ammoniacal liquor.
9. according to the method for claim 1 or 8 described original position synthesizing nano-silvers, it is characterized in that the concentration of the reducing agent in the said step 3 is 8～12mmol/L.
10. the method for original position synthesizing nano-silver according to claim 3 is characterized in that, 4～5 minutes time that the said all-cotton fabric of handling through step 2 soaks in reducing agent.
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Cited By (8)
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| CN104878587A (en) * | 2015-05-08 | 2015-09-02 | 四川大学 | Pretreatment of supercritical fluid nano silver textile fabric and microwave preparation method of supercritical fluid nano silver textile fabric |
| CN104988720A (en) * | 2015-07-22 | 2015-10-21 | 上海晨隆纺织新材料有限公司 | Nano silver in-situ formation silver-plating method based on plasma modification and silver-plated fabric |
| CN105921173A (en) * | 2016-04-21 | 2016-09-07 | 河南大学 | Nano-silver composite textile catalyst and application thereof |
| CN105970611A (en) * | 2016-05-30 | 2016-09-28 | 四川大学 | Supercritical fluid preparation method of nano-silver-coated textile fabric |
| CN107190399A (en) * | 2017-07-28 | 2017-09-22 | 合肥布竹梦依服装贸易有限公司 | A kind of manufacture method of Nano Silver weaving face fabric |
| WO2017181380A1 (en) * | 2016-04-21 | 2017-10-26 | 河南大学 | Silver nanoparticle-composite fabric-supported catalyst, and use thereof |
| CN107343505A (en) * | 2016-05-06 | 2017-11-14 | 识骅科技股份有限公司 | Has the CNT composite construction of Nano particles of silicon dioxide and Nano silver grain |
| CN114645459A (en) * | 2022-03-25 | 2022-06-21 | 武汉工程大学 | Stretchable conductive antibacterial modified polyamide and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104878587A (en) * | 2015-05-08 | 2015-09-02 | 四川大学 | Pretreatment of supercritical fluid nano silver textile fabric and microwave preparation method of supercritical fluid nano silver textile fabric |
| CN104988720A (en) * | 2015-07-22 | 2015-10-21 | 上海晨隆纺织新材料有限公司 | Nano silver in-situ formation silver-plating method based on plasma modification and silver-plated fabric |
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| CN107343505A (en) * | 2016-05-06 | 2017-11-14 | 识骅科技股份有限公司 | Has the CNT composite construction of Nano particles of silicon dioxide and Nano silver grain |
| CN105970611A (en) * | 2016-05-30 | 2016-09-28 | 四川大学 | Supercritical fluid preparation method of nano-silver-coated textile fabric |
| CN107190399A (en) * | 2017-07-28 | 2017-09-22 | 合肥布竹梦依服装贸易有限公司 | A kind of manufacture method of Nano Silver weaving face fabric |
| CN114645459A (en) * | 2022-03-25 | 2022-06-21 | 武汉工程大学 | Stretchable conductive antibacterial modified polyamide and preparation method thereof |
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Application publication date: 20121010 |