CN104985175B - A kind of method for removing nano metal powder surface anion - Google Patents
A kind of method for removing nano metal powder surface anion Download PDFInfo
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Abstract
The invention provides a kind of method for removing nano metal powder surface anion, including（1）The nano metal powder that liquid phase reduction is prepared pure water is cleaned, centrifugation 23 times；（2）Under conditions of stirring, with wet 15 30min of nano metal powder of the ultrasonication of certain power, frequency, ammonium hydrogen carbonate or ammonium bisulfite is added, then is sufficiently stirred for and ultrasonically treated rear addition pure water, centrifugation；（3）With pure water, the wet nano metal powder of centrifugation, when pH value≤9 for measuring supernatant liquor, stop washing, outwell the stillness of night；（4）Mercaptan is added under stirring and ul-trasonic irradiation, continue ultrasonically treated 15 60min of stirring, pure water is added, is sufficiently stirred for and centrifugation after ultrasonic wave decentralized processing；（5）Nano metal powder is washed with organic solution, centrifugation 23 times, be put in high-temperature hydrogen reduction stove, be passed through hydrogen, dry at 200 300 DEG C, obtain required product.The method of the present invention, reasonable in design, process conditions temperature, simple to operate, the Anion-adsorption amount of the nano metal powder processed through the method greatly reduces.
Description
Technical field
The present invention relates to a kind of processing method of nano-material surface, more particularly to a kind of nano metal or sub-micron metal
The processing method on surface, specifically relates to a kind of method for removing nano metal or sub-micron metal powder surface anion.
Background technology
The research of nano material has become the focus in investigation of materials field at this stage.Nano material becomes ultramicro powder material again
Material, it is at least one-dimensional in nanoscale scope on three dimension scale（1-100nm, is 0.1-100nm in engineering）Or be
Material as basic structural unit.Nano-metal particle is due to larger specific surface area, good electric conductivity and change
Activity is learned, is widely used in the fields such as powder metallurgy, magnetic material, electrocondution slurry, battery material, catalyst.
The preparation method of nano-metal particle is varied, is broadly divided into Physical and two big class of chemical method.Physical has
High-energy ball milling method, high-voltage arc method；Chemical method has electrolysis, high pressure hydrogen reduction method, normal pressure liquid phase reduction etc..Due to Physical
Higher to equipment requirement, high energy consumption, and there is the unmanageable shortcoming of granularity, therefore be restricted in application.In chemical method
High pressure hydrogen reduction method needs high-tension apparatus and expensive noble metal catalyst, also restrained in application；And electrolysis is prepared
The shape of nano metal powder, size irregular, the active surface area of powder is big, production, storage, is also easy to produce during use
Problem, thus also limit the heavy industrialization of the method to a certain extent；Normal pressure liquid phase reduction is gone back by oxidation
Original reacts to prepare nano metal particles, as reaction condition is gentle, easy to operate, receives the very big pass of domestic and international researcher
Note.
Normal temperature liquid phase reduction is typically with the hydrochloride of metal, sulfate, nitrate or acetate etc. as presoma, molten
In water or absolute ethyl alcohol, with ammoniacal liquor or NaOH as pH adjusting agent, with the organic reducing agents such as glucose, ethylene glycol or water
The inorganic reducing agents such as hydrazine are closed, nano metal powder is prepared as protective agent with SDS, CTAB or PVP.Prepared by normal temperature liquid phase reduction
Nano metal powder need centrifuge washing multiple through pure water, to remove chlorion, sulfate ion or the hydroxyl of residual
Ion, but as the specific surface area of nano-metal particle is very big, surface energy is also very high, and chlorion and sulfate ion are inhaled very well
Be attached to nano-metal particle surface, conventional physical cleaning is difficult preferably removal, and increases the number of times of cleaning, can not make cloudy from
Son amount is decreased obviously, and nano-metal particle can be caused on the contrary to hydrolyze.X-ray light XPS Analysis result shows：Cleaning time
Number is excessive, has hydroxide to generate on nano-metal particle surface.Such nano-metal particle is as conductive material in sintering
When, hydroxide decomposes generation metal oxide and produces a large amount of holes, can have a strong impact on electric conductivity.
Content of the invention
It is an object of the invention to provide a kind of method for removing nano metal powder surface anion, the method can be gone very well
Anion except the nano metal powder surface that normal temperature liquid phase reduction is prepared.
For realizing object above, the method for removing nano metal powder surface anion of the present invention, include successively as follows
Step：
（1）The nano metal powder that liquid phase reduction is prepared pure water is cleaned, centrifugation 2-3 time, outwell
Layer clear liquid, obtains wet nano metal powder；
（2）Under conditions of stirring, with power be 50-2000W, frequency be 50KHZ-5MHZ the wet nanometer of ultrasonication
Metal-powder 15-30min, being kept stirring for, with conditions of ultrasonic wave decentralized processing, adding ammonium hydrogen carbonate or ammonium bisulfite,
It is sufficiently stirred for, with after ultrasonically treated 20-30min, adding appropriate pure water, being centrifugally separating to obtain wet metal-powder, ammonium hydrogen carbonate or Asia
The addition of ammonium hydrogen sulfate is added for the ratio of 0.001-1 1 in the mol ratio of ammonium hydrogen carbonate or ammonium bisulfite metal；
（3）With pure water, step with centrifugal separation（2）The wet nano metal powder for obtaining, as the pH for measuring supernatant liquor
During value≤9, stop washing, supernatant liquor is outwelled, obtains wet nano metal powder；
（4）Using with step（2）Identical stirring and ultrasonic wave, to step（3）The wet nano metal powder for obtaining is carried out
Decentralized processing, is simultaneously introduced mercaptan, continues the ultrasonically treated 15-60min of stirring, adds appropriate pure water, is sufficiently stirred for and ultrasound
After ripple decentralized processing 15-45min, nano metal powder is centrifugally separating to obtain, the addition of mercaptan presses the mol ratio of mercaptan metal
Add for the ratio of 0.001-1 1；
（5）By step（4）The nano metal powder for obtaining organic solution is washed, centrifugation 2-3 time, is put into high temperature hydrogen
In reduction furnace, hydrogen is passed through, 0.5-2 hour is dry at 200-300 DEG C, you can obtain few high-purity of surface Anion-adsorption and receive
Rice metal-powder.
In order to more preferably remove the anion on nano metal powder surface, in said method, step（4）Repeat once.
Above-mentioned steps（2）The preferred ammonium hydrogen carbonate of the addition of middle ammonium hydrogen carbonate or ammonium bisulfite or ammonium bisulfite gold
The mol ratio of category is 0.05-0.5 1.
Above-mentioned steps（4）The mol ratio of the preferred mercaptan metal of the addition of middle mercaptan is 0.1-0.5.
Above-mentioned steps（4）The preferred propanethiol of the mercaptan of middle addition, isopropyl mercaptan, allyl mercaptan, butyl mercaptan, tert-butyl mercaptan,
Sec-butyl thioalcohol, isobutyl mercaptan, alkene butyl mercaptan, one or more of 2- butene-1-mercaptan, amyl hydrosulfide or hexyl mercaptan.
Above-mentioned steps（5）The preferred absolute methanol of the organic solvent of middle employing, absolute ethyl alcohol, acetone, ether any one or
Multiple.
Above-mentioned steps（2）The preferred 100-500W of the power of middle ultrasonic wave, the preferred 50KHZ-5MHZ of frequency.
The preferred gold, silver of nano metal powder in said method, copper or nickel.
The method for removing nano metal powder surface anion of the present invention, first with ammonium hydrogen carbonate or ammonium bisulfite
Ammonium ion, bicarbonate radical or the sulfite ion for ionizing out in aqueous, is easier to absorption on nano-metal particle surface, subtracts
The adsorbance of other anion few, and ammonium ion, bicarbonate radical or sulfite ion easily decompose under conditions of heating,
And catabolite is all gas；Then using mercaptan one end be hydrophilic sulfydryl (- SH), the other end be oleophylic alkyl, hydrophilic
Sulfydryl (- SH) activity higher, can react with nano metal, generate corresponding mercaptide in metal surface, tie up the moon from
The absorption position of son, makes the anion of physical absorption reenter in the aqueous solution, as mercaptan metal object is stable alkyl sulfide
Alcohol thing, will not hydrolyze, and stay in surface of metal particles is non-polar group, it is possible to reduce the suction again of anionic group
Attached；Finally metal simple-substance is decomposed at a certain temperature again using mercaptan metal object.The method of the present invention, reasonable in design, work
Skill condition temperature, simple to operate, the anion mass fraction of the nano metal powder processed through the method, can be from original thousand of
Ppm drops to tens ppm, is a kind of fine side for removing the nano metal powder surface anion that liquid phase reduction is prepared
Method.
Specific embodiment
Embodiment 1
（1）The nm of gold that tetra- chloride hydrate of 0.05mol gold is prepared through liquid phase reduction, is cleaned with pure water, is centrifuged
Separate 2 times, supernatant liquor is outwelled, obtains wet nano-gold powder；
（2）Under conditions of stirring, with power be 100W, frequency be 1MHZ the wet nano-gold powder 10min of ultrasonication,
It is kept stirring for and ultrasonic wave decentralized processing, 0.4 gram of ammonium hydrogen carbonate is added, is sufficiently stirred for, with after ultrasonically treated 20min, adding in right amount
Pure water, is centrifugally separating to obtain wet nano-gold powder；
（3）With pure water, step with centrifugal separation（2）After the wet nano gold powder for obtaining 2 times, measured with accurate pH test paper
The pH of supernatant liquor is 8.5, stops washing, outwells supernatant liquor, obtain wet nano-gold powder；
（4）Using step（2）Stirring and power, frequency identical ultrasonic wave, to step（3）The wet nano-gold powder for obtaining
Body carries out decentralized processing, adds 2 grams of propanethiols, continues the ultrasonically treated 20min of stirring, adds appropriate pure water, then be sufficiently stirred for
After ultrasonic wave decentralized processing 15min, nano-gold powder is centrifugally separating to obtain；
（5）Repeat step（4）Operation once, the nano gold powder for obtaining is cleaned, is centrifuged with absolute ethyl alcohol or acetone
Separate twice, place in hydrogen reduction furnace, hydrogen is passed through, dry 0.5 hour at 300 DEG C, the nano-gold powder for obtaining, through inspection
Survey, its chlorine ions fraction drops to 70ppm by original 6000ppm.
Embodiment 2
（1）The Nanometer Copper that 0.05mol Salzburg vitriol is prepared through liquid phase reduction, is cleaned with pure water, is centrifuged
Separate 2 times, supernatant liquor is outwelled, obtains wet copper nanoparticle；
（2）Under conditions of stirring, with power be 200W, frequency be 500KHZ the wet copper nanoparticle of ultrasonication
20min, is kept stirring for and ultrasonic wave decentralized processing, add 0.6 gram of ammonium hydrogen carbonate, be sufficiently stirred for after ultrasonically treated 20min, plus
Enter appropriate pure water, be centrifugally separating to obtain wet copper nanoparticle；
（3）With pure water, step with centrifugal separation（2）After the wet copper nanoparticle for obtaining 3 times, measured with accurate pH test paper
The pH of layer clear liquid is 9, stops washing, outwells supernatant liquor, obtain wet copper nanoparticle；
（4）Using step（2）Stirring and power, frequency identical ultrasonic wave, to step（3）The wet copper nanoparticle for obtaining
Decentralized processing is carried out, 1.35 grams of butyl mercaptan are added, continue the ultrasonically treated 20min of stirring, appropriate pure water is added, is sufficiently stirred for
After ultrasonic wave decentralized processing 15min, nano-metallic copper powder is centrifugally separating to obtain；
（5）Repeat step（4）Operation once, the copper nanoparticle for obtaining is cleaned with absolute ethyl alcohol or acetone, is centrifuged point
From twice, place in hydrogen reduction furnace, hydrogen is passed through, dry 1 hour at 240 DEG C, the copper nanoparticle for obtaining, after testing, its
Sulfate radical mass fraction declines for about 60ppm by original 5000ppm.
Embodiment 3
（1）The Nano Silver that 0.05mol nitric acid galactic longitude liquid phase reduction is prepared, is cleaned with pure water, centrifugation 2
Secondary, supernatant liquor is outwelled, obtains wet nano-silver powder；
（2）Under conditions of stirring, with power be 200W, frequency be 1MHZ the wet nano-silver powder 15min of ultrasonication,
It is kept stirring for and ultrasonic wave decentralized processing, 0.5 gram of ammonium bisulfite is added, is sufficiently stirred for, with after ultrasonically treated 20min, adding and fitting
Amount pure water, is centrifugally separating to obtain wet nano-silver powder；
（3）With pure water, step with centrifugal separation（2）After the wet nano-silver powder for obtaining 2 times, measured with accurate pH test paper
The pH of layer clear liquid is 8, stops washing, outwells supernatant liquor, obtain nano-silver powder stand-by；
（4）Using step（2）Stirring and power, frequency identical ultrasonic wave, to step（3）The wet copper nanoparticle for obtaining
Decentralized processing is carried out, 1.5 grams of propylene mercaptan are added, continue the ultrasonically treated 20min of stirring, appropriate pure water is added, is fully stirred
After mixing and stirring ultrasonic wave decentralized processing 15min, nano-silver powder is centrifugally separating to obtain；
（5））Repeat step（4）Operation once, by the nano-silver powder absolute ethyl alcohol for obtaining or acetone cleaning, centrifugation
Twice, place in hydrogen reduction furnace, hydrogen is passed through, dry 1 hour at 270 DEG C, the nano-silver powder for obtaining, its nitrate anion quality
Fraction drops to 60ppm by original 5000ppm.
Embodiment 4
（1）The nano nickel that 0.05mol nickel acetate is prepared through liquid phase reduction, is cleaned with pure water, centrifugation 2
Secondary, supernatant liquor is outwelled, obtains wet nano-nickel powder；
（2）Under conditions of stirring, with power be 300W, frequency be 1MHZ the wet nano-nickel powder 15min of ultrasonication,
It is kept stirring for and ultrasonic wave decentralized processing, 0.6 gram of ammonium hydrogen carbonate is added, is sufficiently stirred for, with after ultrasonically treated 20min, adding in right amount
Pure water, is centrifugally separating to obtain wet nano-nickel powder；
（3）With pure water, step with centrifugal separation（2）After the wet nano-nickel powder for obtaining 3 times, measured with accurate pH test paper
The pH of layer clear liquid is 9, stops washing, outwells supernatant liquor, obtain wet nano-nickel powder stand-by；
（4）Using step（2）Stirring and power, frequency identical ultrasonic wave, to step（3）The wet copper nanoparticle for obtaining
Carry out decentralized processing, add 1.2 to restrain oneself mercaptan, continue the ultrasonically treated 20min of stirring, appropriate pure water is added, is sufficiently stirred for
After ultrasonic wave decentralized processing 10min, nano-nickel powder is centrifugally separating to obtain；
（5）Repeat step（4）Operation once, the nano-nickel powder for obtaining is cleaned with absolute ethyl alcohol or acetone, is centrifuged point
From twice, place in hydrogen reduction furnace, hydrogen is passed through, dry 2 hours at 200 DEG C.The nano-nickel powder for obtaining, its acetate matter
Amount fraction drops to 40ppm by original 5000ppm.
" adding appropriate pure water " in technique scheme and each embodiment, generally refers to add the amount of pure water to be less than
2/3rds of container height.
Claims (8)
1. a kind of method for removing nano metal powder surface anion, in turn includes the following steps：
（1）The nano metal powder that liquid phase reduction is prepared pure water is cleaned, centrifugation 2-3 time, to outwell upper strata clear
Liquid, obtains wet nano metal powder；
（2）Under conditions of stirring, with power be 50-2000W, frequency be 50KHZ-5MHZ the wet nano metal of ultrasonication
Powder 15-30min, is being kept stirring for, with conditions of ultrasonic wave decentralized processing, adding ammonium hydrogen carbonate or ammonium bisulfite, fully
After stirring and ultrasonically treated 20-30min, appropriate pure water is added, is centrifugally separating to obtain wet metal-powder, ammonium hydrogen carbonate or sulfurous acid
The addition of hydrogen ammonium is added for the ratio of 0.001-1 1 in the mol ratio of ammonium hydrogen carbonate or ammonium bisulfite metal；
（3）With pure water, step with centrifugal separation（2）The wet nano metal powder for obtaining, when pH value≤9 for measuring supernatant liquor
When, stop washing, supernatant liquor is outwelled, obtains wet nano metal powder；
（4）Using with step（2）Identical stirring and ultrasonic wave, to step（3）The wet nano metal powder for obtaining is disperseed
Process, mercaptan is simultaneously introduced, continue the ultrasonically treated 15-60min of stirring, appropriate pure water is added, be sufficiently stirred for and ultrasonic wavelength-division
Dissipate after processing 15-45min, nano metal powder is centrifugally separating to obtain, the addition of mercaptan by the mol ratio of mercaptan metal is
The ratio of 0.001-1 1 is added；
（5）By step（4）The nano metal powder for obtaining organic solution is washed, centrifugation 2-3 time, is put into high-temperature hydrogen reduction
In stove, hydrogen is passed through, 0.5-2 hour is dry at 200-300 DEG C, you can obtain the few high-purity nm gold of surface Anion-adsorption
Category powder.
2. the method for removing nano metal powder surface anion according to claim 1, it is characterised in that：Methods described
In, step（4）Repeat once.
3. the method for removing nano metal powder surface anion according to claim 1 and 2, it is characterised in that：Described
Step（2）The addition of middle ammonium hydrogen carbonate or ammonium bisulfite is that the mol ratio of ammonium hydrogen carbonate or ammonium bisulfite metal is
0.05-0.5 1.
4. the method for removing nano metal powder surface anion according to claim 3, it is characterised in that：The step
（4）The addition of middle mercaptan is 0.1-0.5 1 for the mol ratio of mercaptan metal.
5. the method for removing nano metal powder surface anion according to claim 4, it is characterised in that：The step
（4）The mercaptan of middle addition be propanethiol, isopropyl mercaptan, allyl mercaptan, butyl mercaptan, tert-butyl mercaptan, sec-butyl thioalcohol, isobutyl mercaptan,
Alkene butyl mercaptan, one or more of 2- butene-1-mercaptan, amyl hydrosulfide or hexyl mercaptan.
6. the method for removing nano metal powder surface anion according to claim 5, it is characterised in that：The step
（5）The organic solvent of middle employing is any one or more of absolute methanol, absolute ethyl alcohol, acetone, ether.
7. the method for removing nano metal powder surface anion according to claim 6, it is characterised in that：The step
（2）The preferred 100-500W of the power of middle ultrasonic wave, frequency are 50KHZ-5MHZ.
8. according to the arbitrary described method for removing nano metal powder surface anion of claim 1-7, it is characterised in that：Institute
It is gold, silver, copper or nickel to state the nano metal powder in method.
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| US6660058B1 (en) * | 2000-08-22 | 2003-12-09 | Nanopros, Inc. | Preparation of silver and silver alloyed nanoparticles in surfactant solutions |
| CN1483540A (en) * | 2003-08-12 | 2004-03-24 | 北京科技大学 | Method for mfg nano copper powder |
| WO2006082844A1 (en) * | 2005-02-02 | 2006-08-10 | National Institute For Materials Science | Process for producing nanometer-size particles |
| EP1844883A1 (en) * | 2005-02-02 | 2007-10-17 | DOWA Electronics Materials Co., Ltd. | Silver particle powder and process for producing the same |
| CN101698496A (en) * | 2009-10-28 | 2010-04-28 | 广东光华化学厂有限公司 | Preparation method of electronic grade high-purity copper oxide superfine powder |
| CN103785826A (en) * | 2014-02-19 | 2014-05-14 | 南京林业大学 | Method for preparing modified nanometer nickel powder |
-
2015
- 2015-07-02 CN CN201510378844.4A patent/CN104985175B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6660058B1 (en) * | 2000-08-22 | 2003-12-09 | Nanopros, Inc. | Preparation of silver and silver alloyed nanoparticles in surfactant solutions |
| CN1483540A (en) * | 2003-08-12 | 2004-03-24 | 北京科技大学 | Method for mfg nano copper powder |
| WO2006082844A1 (en) * | 2005-02-02 | 2006-08-10 | National Institute For Materials Science | Process for producing nanometer-size particles |
| EP1844883A1 (en) * | 2005-02-02 | 2007-10-17 | DOWA Electronics Materials Co., Ltd. | Silver particle powder and process for producing the same |
| CN101698496A (en) * | 2009-10-28 | 2010-04-28 | 广东光华化学厂有限公司 | Preparation method of electronic grade high-purity copper oxide superfine powder |
| CN103785826A (en) * | 2014-02-19 | 2014-05-14 | 南京林业大学 | Method for preparing modified nanometer nickel powder |
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