CN101875130A - Method for preparing nano silver particles - Google Patents
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- CN101875130A CN101875130A CN2009102731034A CN200910273103A CN101875130A CN 101875130 A CN101875130 A CN 101875130A CN 2009102731034 A CN2009102731034 A CN 2009102731034A CN 200910273103 A CN200910273103 A CN 200910273103A CN 101875130 A CN101875130 A CN 101875130A
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Abstract
The invention provides a method for preparing and separating nano silver particles. The method comprises the following steps of: preparing mixed aqueous solution of AgNO3 and a complexing agent of AgNO3 first, adding a certain amount of surfactant, adjusting the pH value of the system then, stirring the system to completely dissolve the added surfactant, adding a reducer into the solution dropwise with vigorous stirring, controlling the reaction temperature to be room temperature and continuously stirring the mixed solution after the reducer is completely dropped to obtain nano solver sol till the end of the reaction; and adjusting the pH value of the nano solver sol to be subacid or neutral (pH=2-7) by adopting a pH value regulator, allowing solids to be dissolved, separating the solids, washing the solids with an organic solvent, separating the mixed liquid again to obtain 'wet' nano silver particles and drying the 'wet' nano silver particles under vacuum to obtain the nano silver particles. The nano silver particles prepared by the method are small in particle size (less than 50 nanometers), the preparation process has mild reaction conditions (room temperature), and the subsequent separation steps are simple (centrifugal separation is not required).
Description
Technical field
The invention belongs to the preparation field of nano material, be specifically related to a kind of preparation method of nano-Ag particles.
Background technology
Nano-metal particle demonstrates performances such as the heat different with block materials, light, electricity, magnetic, catalysis owing to having small-size effect, skin effect and quantum size effect, so it has potential application prospect in fields such as photoelectronics, catalysis, chemical sensor, magnetic material, lifestyle medicals.
Silver be in all metals the best a kind of metal of electric conductivity (electrical conductivity is 6.62 * 10
5Scm
-1), be the most cheap noble metal of price, and have good chemical inertness again.Therefore be that bulk metal silver or different shape (sheet, spherical etc.) and the silver-colored particle of size (micron, sub-micron, nanometer etc.) have all obtained application very widely.
About the preparation method of nano-Ag particles, can be divided into physics method and chemical method substantially.The physics method mainly contains gas evaporation coacervation, polishing and atomization etc., but physics method production efficiency is low, cost costliness, energy consumption height; Chemical method comprises reduction protection method, microemulsion method, phase transfer method etc., and it is simple to have preparation technology, the productive rate advantages of higher.
Utilize that the electronation Protection Code can prepare that Size Distribution is more single, particle size and the controlled Nano silver grain of shape.This method mainly is to make surfactant by specific big molecule or polymer substance, in the growth course of the nucleation of nano-Ag particles and nuclear, selectively adsorb or be bonded in the surface of silver-colored particle, thereby form metastable colloidal dispersion, afterwards colloid is destroyed, through separation means such as super centrifugal, filtrations, nano-Ag particles is disperseed out.
As people such as Wu Qingsong (SCI, 2005, Vol.26, No.3, pp407-411) adopt the electronation Protection Code, be surfactant with the polyoxyethylene lauryl ether, preparation and centrifugation have gone out the nano-Ag particles of particle diameter greater than 100nm; People such as Niu Man (Materials Science and Engineering of Powder Metallurgy, 2007, Vol.12; No.3; pp183-186) also adopting the electronation Protection Code, is surfactant with polyvinylpyrrolidone (PVP), and preparation and centrifugation go out the silver-colored particle of particle diameter at 60～133nm in the time of 180 ℃.The preparation scheme that above-mentioned as can be seen example adopts, perhaps Zhi Bei silver-colored particle bigger (as particle diameter greater than 100nm), or (as 180 ℃) prepare under hot conditions.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nano-Ag particles, the prepared nano-Ag particles particle diameter of this method is little and distribute and concentrate, and preparation process reaction condition gentleness, later separation step are simple.
The preparation method of nano-Ag particles provided by the invention is characterized in that this method comprises the steps:
(1) stirs down, in silver nitrate aqueous solution, add complexing agent, form the complex solution of silver nitrate, in this complex solution, add surfactant again, and regulate between pH value to 9～12, obtaining homogeneous phase solution, the total concentration of silver nitrate is 5～100g/L in this homogeneous phase solution; Described complexing agent be in water-soluble organic amine, ammoniacal liquor and the disodium EDTA any or several, the addition of complexing agent is the amount that the precipitation that generates in the adition process is just dissolved; Described surfactant is C
8～C
18Aliphatic acid or in the soap any or several, the consumption of surfactant is on its critical micelle concentration;
(2) low whipping speed dropwise drips reductant solution greater than under the 300rpm condition in above-mentioned homogeneous phase solution, and reaction temperature is controlled at room temperature; Described reducing agent be in sodium borohydride, hydrazine hydrate, formaldehyde and the ascorbic acid any or several, many 0.01～2 times of the amount that its amount ratio calculates by the reaction equivalent.
(3) after reaction is finished, reduce mixing speed to 300rpm, add phosphoric acid in the system that step (2) obtains, the concentration of volume percent of this phosphoric acid is 15～25%, is between 2～7 in order to the pH value of regulation system, leaves standstill afterwards, and nano-Ag particles is separated out.Adopt filter method to separate again, isolated solid is used organic solvent washing again, separates once more, obtains particle diameter at " wetting " nano-Ag particles less than 50nm; Promptly get nano-Ag particles of the present invention through vacuum drying.Described organic solvent be in methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, acetone, the ethyl acetate any or several.
Regulate pH value agents useful for same and can be NaOH, potassium hydroxide or ammoniacal liquor.
The preparation method of the nano-Ag particles that the present invention proposes is that the complex compound with silver nitrate is main salt, at aqueous phase, with long-chain fat alkyl acid or long-chain fat alkyl hydrochlorate is surfactant, isolates nano-Ag particles by changing the solubility of surfactant in system.Described method has the nano-Ag particles particle diameter little (less than 50nm) of preparation, the advantage of preparation process reaction condition gentleness (room temperature), later separation step simple (not needing to adopt centrifugation).
Description of drawings
Fig. 1 is transmission electron microscope (TEM) photo of the nano-Ag particles that makes;
The specific embodiment
Embodiment 1
The 60g silver nitrate is dissolved in the 500mL water, and, forms silver ammonia complex solution, in above-mentioned solution, add the 15g laurate, add the 120mL concentrated ammonia liquor under stirring and regulate its pH value, to promote lauric dissolving to the concentrated ammonia liquor that wherein adds 60mL 25%.After treating that laurate dissolves fully, strengthen mixing speed to 800rpm, to wherein dripping the 400mL aqueous solution that contains the 4g sodium borohydride, whole dropping process continues 30min, waits to dropwise the back and continues stirring reaction 20min, and entire reaction course maintains room temperature.After this reduce mixing speed to 100rpm, to the phosphoric acid that wherein slowly adds 200mL 20% (V/V).Leave standstill after adding, filter black solid.The black solid that obtains is washed with 250mL methyl alcohol, 250mL ethanol successively, filter once more, promptly get " wetting " nano-Ag particles, after vacuum drying, get the about 27g of nano-Ag particles.
Embodiment 2
The 100g silver nitrate is dissolved in the 1000mL water, and to the methylamine water solution that wherein adds 125mL 40%, forms silver ammonia complex solution, add 16g caprylic acid sodium in above-mentioned solution, stirring is dissolved caprylic acid sodium fully.After this strengthen mixing speed at 500rpm, and to the formalin that wherein dropwise drips 48g 37%, whole dropping process continues 30min, wait to dropwise the back and continue stirring reaction 60min.Reduce mixing speed to 200rpm, in system, slowly inject the phosphoric acid of 150mL 25% (V/V).Leave standstill after adding, filter black solid.The black solid that obtains is washed with 250mL ethanol, 250mL acetone successively, filter once more, promptly get " wetting " nano-Ag particles, after vacuum drying, get the about 45g of nano-Ag particles.
Embodiment 3
The 60g silver nitrate is dissolved in the 1200mL water, to wherein adding 90g disodium EDTA (EDTA), form silver complex solution, in above-mentioned solution, add the 15g laurate, stir the NaOH aqueous solution that adds 100g 10% down and regulate its pH value, to promote lauric dissolving.After treating that laurate dissolves fully, strengthen mixing speed again to 1200rpm, to the hydrazine hydrate that wherein dropwise drips 20mL 40%, whole dropping process continues 30min, waits to dropwise the back and continues stirring reaction 20min, and entire reaction course maintains room temperature.After this reduce mixing speed to 150rpm, to the phosphoric acid that wherein slowly adds 250mL 15% (V/V).Leave standstill after adding, filter black solid.With the black solid that obtains 500mL ethanol washed twice (each 250mL), filter once more, promptly get " wetting " nano-Ag particles, after vacuum drying, get the about 27g of nano-Ag particles.
Embodiment 4
The 60g silver nitrate is dissolved in the 2000mL water, and to wherein adding the 15mL isopropylamine, forms silver ammonia complex solution, add the 17g sodium laurate in above-mentioned solution, stirring is dissolved sodium laurate fully.After treating that sodium laurate dissolves fully, strengthen mixing speed again to 1000rpm, to wherein dropwise dripping the 400mL aqueous solution that contains the 7g ascorbic acid, whole dropping process continues 30min, wait to dropwise the back and continue stirring reaction 20min, entire reaction course maintains room temperature.After this reduce mixing speed to 250rpm, to the phosphoric acid that wherein slowly adds 150mL 20% (V/V).Leave standstill after adding, filter black solid.With the black solid that obtains 500mL ethyl acetate washed twice (each 250mL), filter once more, promptly get " wetting " nano-Ag particles, after vacuum drying, get the about 27g of nano-Ag particles.
Embodiment 5
The 30g silver nitrate is dissolved in the 2500mL water, and, forms silver ammonia complex solution, in above-mentioned solution, add 9g octadecyl carboxylic acid, add the 60mL concentrated ammonia liquor under stirring and regulate its pH value, to promote the dissolving of octadecyl carboxylic acid to wherein adding the 25mL ethylenediamine.After treating that the octadecyl carboxylic acid dissolves fully, strengthen mixing speed again to 700rpm, to the aqueous solution that wherein dropwise drips the 400mL that contains the 1.5g sodium borohydride, whole dropping process continues 30min, wait to dropwise the back and continue stirring reaction 20min, entire reaction course maintains room temperature.After this reduce mixing speed to 100rpm, to the phosphoric acid that wherein slowly adds 100mL22% (V/V).Leave standstill after adding, filter black solid.With the black solid that obtains 200mL normal propyl alcohol washed twice (each 250mL), filter once more, promptly get " wetting " nano-Ag particles, after vacuum drying, get the about 13.5g of nano-Ag particles.
Embodiment 6
The 50g silver nitrate is dissolved in the 3000mL water, and to the ethylamine solution that wherein adds 100mL 50%, form silver ammonia complex solution, in above-mentioned solution, add 20g octadecyl carboxylic acid sodium, stirring is dissolved the octadecyl carboxylic acid sodium fully, strengthens mixing speed afterwards to 2000rpm, and to the formalin that wherein dropwise drips 30g 37%, whole dropping process continues 30min, waits to dropwise the back and continues stirring reaction 60min.Reduce mixing speed afterwards to 200rpm, in system, slowly inject the phosphoric acid of 200mL 20% (V/V).Leave standstill after adding, filter black solid.The black solid that obtains is washed with 250mL ethanol, 250mL acetone successively, filter once more, promptly get " wetting " nano-Ag particles, after vacuum drying, get the about 22g of nano-Ag particles.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment.So everyly do not break away from the equivalence of finishing under the spirit disclosed in this invention or revise, all fall into the scope of protection of the invention.
Claims (2)
1. the preparation method of a nano-Ag particles is characterized in that this method comprises the steps:
(1) under agitation, in silver nitrate aqueous solution, add complexing agent, form the complex solution of silver nitrate, in this complex solution, add surfactant again, and regulate between pH value to 9～12, obtaining homogeneous phase solution, the total concentration of silver nitrate is 5～100g/L in this homogeneous phase solution; Described complexing agent be in water-soluble organic amine, ammoniacal liquor and the disodium EDTA any or several, the addition of complexing agent is the amount that the precipitation that generates in the adition process is just dissolved; Described surfactant is C
8～C
18Aliphatic acid or in the soap any or several, the consumption of surfactant is on its critical micelle concentration;
(2) strengthen mixing speed to more than the 300rpm, dropwise drip reductant solution in above-mentioned homogeneous phase solution, reaction temperature is controlled at room temperature; Described reducing agent be in sodium borohydride, hydrazine hydrate, formaldehyde and the ascorbic acid any or several, many 0.01～2 times of the amount that its amount ratio calculates by the reaction equivalent.
2. preparation method according to claim 1 is characterized in that, after reaction is finished, reduce mixing speed to 300rpm, add phosphoric acid in the system that step (2) obtains, the concentration of volume percent of this phosphoric acid is 15～25%, is 2～7 in order to the pH value of regulation system; Leave standstill afterwards, nano-Ag particles is separated out, separate again, use organic solvent washing again, separate once more, obtain particle diameter, after vacuum drying, promptly get nano-Ag particles of the present invention at " wetting " nano-Ag particles less than 50nm; Described organic solvent be in methyl alcohol, ethanol, normal propyl alcohol, isopropyl alcohol, acetone, the ethyl acetate any or several.
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| CN102179526A (en) * | 2011-04-18 | 2011-09-14 | 东华大学 | Method for preparing cubic crystal nano silver material by oil-water interface method |
| CN102335751A (en) * | 2011-09-22 | 2012-02-01 | 上海交通大学 | Method for preparing highly dispersed ultrafine spherical silver powder |
| CN103203467A (en) * | 2013-04-17 | 2013-07-17 | 苏州冷石纳米材料科技有限公司 | Method for preparing silver nanowires |
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