CN107552069A - A kind of preparation method of Research of Silver Copper Oxide Composite - Google Patents
A kind of preparation method of Research of Silver Copper Oxide Composite Download PDFInfo
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- CN107552069A CN107552069A CN201710801026.XA CN201710801026A CN107552069A CN 107552069 A CN107552069 A CN 107552069A CN 201710801026 A CN201710801026 A CN 201710801026A CN 107552069 A CN107552069 A CN 107552069A
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Abstract
The invention discloses a kind of preparation method of Research of Silver Copper Oxide Composite, including：(1) silver nitrate solution is added in the ethanol solution containing reducing agent with certain rate of addition, stirring, lucifuge and it is closed under conditions of, 6~72h is reacted under 30~60 DEG C of water bath conditions, obtains silver sol；(2) finite concentration copper nitrate solution is added in above-mentioned silver sol, under conditions of stirring, it is 10~12 to add aqueous slkali regulation pH value, obtains silver-colored Kocide SD colloidal sol；(3) above-mentioned silver-colored Kocide SD colloidal sol is aged 5~8h at room temperature, filtered, absolute ethyl alcohol is respectively adopted and deionized water is washed 3~5 times, dries, 2~3h is calcined under the conditions of 300~500 DEG C, obtains Research of Silver Copper Oxide Composite.In the present invention, preparation technology is simple, cost is low, and in the Research of Silver Copper Oxide Composite being prepared using this method, particle is uniformly dispersed, and its catalytic performance is substantially better than pure zirconia copper.
Description
Technical field
The present invention relates to field of material technology, more particularly to a kind of preparation method of silver-oxidation carbon/carbon-copper composite material.
Background technology
Precious metal doping can form Schottky barrier so as to suppress its hole-recombination in composite material surface.Therefore, your gold
The doping of category is the chemically active important means such as lifting composite catalytic activity, adsorption activity.At present mainly study be
The noble metals such as Pt, Au, Ag, Pd.Wherein, Ag with its cost is low, bio-toxicity is small, it is not soluble in water, not with oxidant reaction, catalysis
The advantages that performance is good and be widely used.It is living in magnetic, light absorbs, chemistry because nano cupric oxide is compared with common cupric oxide
Property, show peculiar physical and chemical properties in terms of thermal resistance, catalyst and fusing point.Therefore, nano cupric oxide is being catalyzed, surpassed
Lead, the field such as ceramics is widely used, so as to cause the concern of researcher.But at present both at home and abroad on load
The report of the oxidation carbon/carbon-copper composite material of silver is also very rare.
Although the method for preparing silver metal nanoparticles is a lot, because the metallic particles of nano-scale is with higher
Specific surface area, easily assemble, so the problem of how keeping its stability to be always relatively difficult.The system of nano cupric oxide
It is standby also to have many methods, but process conditions harshness, industrial flow length are usually present, or particle is easily reunited, made in preparation process
The defects of standby with high costs.Therefore a kind of efficient, cleaning, the synthetic method for aoxidizing carbon/carbon-copper composite material of the silver load of green are found
Have important practical significance.
For this reason, it is necessary in view of the above-mentioned problems, proposing a kind of preparation method of silver-oxidation carbon/carbon-copper composite material, it can be solved
Certainly problems of the prior art.
The content of the invention
It is an object of the invention to provide a kind of preparation method of silver-oxidation carbon/carbon-copper composite material, to overcome in the prior art
Deficiency.
To achieve the above object, the present invention provides following technical scheme：
A kind of preparation method of silver-oxidation carbon/carbon-copper composite material, including：
(1) silver nitrate solution is added in the ethanol solution containing reducing agent with certain rate of addition, in stirring, lucifuge
Under conditions of closed, 6~72h is reacted under 30~60 DEG C of water bath conditions, obtains silver sol；
(2) finite concentration copper nitrate solution is added in above-mentioned silver sol, under conditions of stirring, adds aqueous slkali regulation
PH value is 10~12, obtains silver-Kocide SD colloidal sol；
(3) above-mentioned silver-Kocide SD colloidal sol is aged 5~8h at room temperature, filter, be respectively adopted absolute ethyl alcohol and go from
Sub- water washing 3~5 times, dry, 2~3h is calcined under the conditions of 300~500 DEG C, obtains silver-oxidation carbon/carbon-copper composite material.
Preferably, in step (1), the reducing agent in formaldehyde, formic acid, formic acid esters, glucose, maltose one
Kind.
Preferably, in step (1), the rate of addition is per second 1 drop.
Preferably, in step (2), the preparation method of the silver nitrate solution includes：By 0.001~0.01mol silver nitrates
It is dissolved in 1L absolute ethyl alcohols, obtains the silver nitrate solution that concentration is 0.001~0.01mol/L.
Preferably, in step (2), the aqueous slkali is in ammonia spirit, sodium hydroxide solution, potassium hydroxide solution
It is a kind of.
Preferably, the mol ratio of the silver nitrate and the copper nitrate is 1:15~25.
Compared with prior art, the advantage of the invention is that：In the present invention, preparation technology is simple, cost is low, using the party
In the silver that method is prepared-oxidation carbon/carbon-copper composite material, particle is uniformly dispersed, and its catalytic performance is substantially better than pure zirconia copper.
Embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used
In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
The present invention discloses a kind of preparation method of silver-oxidation carbon/carbon-copper composite material, including：
(1) silver nitrate solution is added in the ethanol solution containing reducing agent with certain rate of addition, in stirring, lucifuge
Under conditions of closed, 6~72h is reacted under 30~60 DEG C of water bath conditions, obtains silver sol；
(2) finite concentration copper nitrate solution is added in above-mentioned silver sol, under conditions of stirring, adds aqueous slkali regulation
PH value is 10~12, obtains silver-Kocide SD colloidal sol；
(3) above-mentioned silver-Kocide SD colloidal sol is aged 5~8h at room temperature, filter, be respectively adopted absolute ethyl alcohol and go from
Sub- water washing 3~5 times, dry, 2~3h is calcined under the conditions of 300~500 DEG C, obtains silver-oxidation carbon/carbon-copper composite material.
In above-mentioned steps (1), the one kind of the reducing agent in formaldehyde, formic acid, formic acid esters, glucose, maltose is excellent
Choosing, the reducing agent is selected from glucose.
In above-mentioned steps (1), the rate of addition is per second 1 drop.
In above-mentioned steps (2), the aqueous slkali in ammonia spirit, sodium hydroxide solution, potassium hydroxide solution one
Kind, it is preferred that the aqueous slkali is selected from ammonia spirit.
In above-mentioned steps, the mol ratio of the silver nitrate and the copper nitrate is 1:15~25, it is preferred that the silver nitrate
Mol ratio with the copper nitrate is 1:20.
In one embodiment, the preparation method of the silver nitrate solution includes：0.001~0.01mol silver nitrates are dissolved in
In 1L absolute ethyl alcohols, the silver nitrate solution that concentration is 0.001~0.01mol/L is obtained.
Embodiment
1st, silver nitrate solution is prepared
0.005mol silver nitrates are dissolved in 1L absolute ethyl alcohols, obtain the silver nitrate solution that concentration is 0.005mol/L.
2nd, silver-oxidation carbon/carbon-copper composite material is prepared
(1) silver nitrate solution is added in the ethanol solution containing reducing agent glucose sugar with the rate of addition of per second one drop,
Stirring, lucifuge and it is closed under conditions of, react 36h under 40 DEG C of water bath conditions, obtain silver sol；
(2) finite concentration copper nitrate solution is added in above-mentioned silver sol, under conditions of stirring, adds ammonia spirit and adjust
It is 11 to save pH value, obtains silver-Kocide SD colloidal sol；
(3) above-mentioned silver-Kocide SD colloidal sol is aged 6h at room temperature, filters, absolute ethyl alcohol and deionization is respectively adopted
Water washing 3~5 times, dry, calcine 2.5h under the conditions of 400 DEG C, obtain silver-oxidation carbon/carbon-copper composite material.
In above-mentioned steps, the mol ratio of the silver nitrate and the copper nitrate is 1:20.
Preparation method in above-described embodiment is simple, cost is low, and the silver that the method in above-described embodiment is prepared-
Aoxidize in carbon/carbon-copper composite material, silver particles can be evenly dispersed in copper oxide particle, using the composite pair in the present invention
Hydrogen peroxide carries out catalytic decomposition experiment and understands that the catalytic performance of the silver-oxidation carbon/carbon-copper composite material is substantially better than urging for pure zirconia copper
Change performance.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant be intended to it is non-exclusive
Property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and
Also include the other element that is not expressly set out, or also include for this process, method, article or equipment inherently
Key element.
Claims (6)
- A kind of 1. preparation method of silver-oxidation carbon/carbon-copper composite material, it is characterised in that including：(1) silver nitrate solution is added in the ethanol solution containing reducing agent with certain rate of addition, in stirring, lucifuge and close Under conditions of closing, 6~72h is reacted under 30~60 DEG C of water bath conditions, obtains silver sol；(2) finite concentration copper nitrate solution is added in above-mentioned silver sol, under conditions of stirring, adds aqueous slkali regulation pH value For 10~12, silver-Kocide SD colloidal sol is obtained；(3) above-mentioned silver-Kocide SD colloidal sol is aged 5~8h at room temperature, filters, absolute ethyl alcohol and deionized water is respectively adopted Washing 3~5 times, dry, 2~3h is calcined under the conditions of 300~500 DEG C, obtains silver-oxidation carbon/carbon-copper composite material.
- 2. the preparation method of silver according to claim 1-oxidation carbon/carbon-copper composite material, it is characterised in that in step (1), institute State the one kind of reducing agent in formaldehyde, formic acid, formic acid esters, glucose, maltose.
- 3. the preparation method of silver according to claim 1-oxidation carbon/carbon-copper composite material, it is characterised in that in step (1), institute Rate of addition is stated as per second 1 drop.
- 4. the preparation method of silver according to claim 1-oxidation carbon/carbon-copper composite material, it is characterised in that in step (1), institute Stating the preparation method of silver nitrate solution includes：0.001~0.01mol silver nitrates are dissolved in 1L absolute ethyl alcohols, obtaining concentration is 0.001~0.01mol/L silver nitrate solution.
- 5. the preparation method of silver according to claim 1-oxidation carbon/carbon-copper composite material, it is characterised in that in step (2), institute State the one kind of aqueous slkali in ammonia spirit, sodium hydroxide solution, potassium hydroxide solution.
- 6. the preparation method of silver according to claim 1-oxidation carbon/carbon-copper composite material, it is characterised in that the silver nitrate with The mol ratio of the copper nitrate is 1:15~25.
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| CN201710801026.XA CN107552069A (en) | 2017-09-07 | 2017-09-07 | A kind of preparation method of Research of Silver Copper Oxide Composite |
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| CN201710801026.XA CN107552069A (en) | 2017-09-07 | 2017-09-07 | A kind of preparation method of Research of Silver Copper Oxide Composite |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121204A (en) * | 2007-09-14 | 2008-02-13 | 北京首创纳米科技有限公司 | Method for preparing nanometer silver composite sol |
| CN101633045A (en) * | 2009-08-24 | 2010-01-27 | 北京崇高纳米科技有限公司 | Nanometer silver collosol, preparation method and application thereof |
| CN102706936A (en) * | 2012-03-15 | 2012-10-03 | 安徽师范大学 | Preparation method of copper-copper oxide composite electrode |
| CN106732654A (en) * | 2017-01-13 | 2017-05-31 | 昆明理工大学 | A kind of preparation method of the oxidation carbon/carbon-copper composite material of loading nano silvery |
| CN107127353A (en) * | 2017-05-20 | 2017-09-05 | 皖西学院 | A kind of nano silver colloidal sol and preparation method thereof |
-
2017
- 2017-09-07 CN CN201710801026.XA patent/CN107552069A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101121204A (en) * | 2007-09-14 | 2008-02-13 | 北京首创纳米科技有限公司 | Method for preparing nanometer silver composite sol |
| CN101633045A (en) * | 2009-08-24 | 2010-01-27 | 北京崇高纳米科技有限公司 | Nanometer silver collosol, preparation method and application thereof |
| CN102706936A (en) * | 2012-03-15 | 2012-10-03 | 安徽师范大学 | Preparation method of copper-copper oxide composite electrode |
| CN106732654A (en) * | 2017-01-13 | 2017-05-31 | 昆明理工大学 | A kind of preparation method of the oxidation carbon/carbon-copper composite material of loading nano silvery |
| CN107127353A (en) * | 2017-05-20 | 2017-09-05 | 皖西学院 | A kind of nano silver colloidal sol and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| GUIJING LI, ET AL.: "Formation and effects of CuO nanoparticles on Ag/SnO2 electrical contact materials", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
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