CN107186222A - A kind of method that supersonic liquid phase reduction prepares Nanometer Copper - Google Patents
A kind of method that supersonic liquid phase reduction prepares Nanometer Copper Download PDFInfo
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- CN107186222A CN107186222A CN201710332267.4A CN201710332267A CN107186222A CN 107186222 A CN107186222 A CN 107186222A CN 201710332267 A CN201710332267 A CN 201710332267A CN 107186222 A CN107186222 A CN 107186222A
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The invention discloses a kind of method that supersonic liquid phase reduction prepares Nanometer Copper, belong to technical field of nano material.The present invention is using under the conditions of ultrasonic reaction, and using copper nitrate as copper source, ascorbic acid is reducing agent, and ethanol is organic solvent, and polyvinylpyrrolidone is protective agent, and liquid-phase reduction prepares Nanometer Copper.Nanometer Copper particle size distribution range prepared by the present invention is narrow, dispersed and stability is good, safe, available for fields such as medicine, food, feeds.Secondly, simple production process of the present invention, production cost are relatively low and environmentally friendly, it is easy to large-scale production, and with important economy and social effect, development prospect is wide.
Description
Technical field
The invention belongs to technical field of nano material, and in particular to a kind of method that supersonic liquid phase reduction prepares Nanometer Copper.
Background technology
Nano material refer in three dimensions at least one dimension be in nanoscale scope (1~100nm) or by
The material that they are constituted as basic component units.When normality material is machined into extremely fine nanoscale, it may appear that
Special small-size effect, skin effect, quantum size effect and macro quanta tunnel effect etc., therefore can show special
Physics and the chemical property such as light, magnetic, electricity.Nanometer Copper can replace noble silver preparing conduction as the important raw material of industry
Cost is substantially reduced in terms of material, effective catalyst, lube oil additive and antiseptic, is had broad application prospects.Cause
This, the research to preparation and the application of Nanometer Copper in recent years has caused extensive concern both domestic and external.But it is due to Nanometer Copper
Easily be oxidized, and existence and stability and it is dispersed poor the problems such as, therefore, prepare dispersiveness and have good stability, pattern and
The controllable copper nano material of size turns into the study hotspot of field of nanometer material technology.
Preparing the method for Nanometer Copper in recent years mainly has solid phase method (ball-milling method, mechanochemical reaction), vapor phase method (plasma
Method, gamma-radiation method, physical vaporous deposition), liquid phase method (microemulsion method, chemical precipitation method, electrolysis, reducing process).Solid phase method
Obtained nano material particle diameter is larger, and is easily introduced during mechanically actuated impurity；Plasma method preparation temperature is high, reaction
Speed is fast, can obtain uniform, short grained nano-powder, it is easy to accomplish mass production, but the capacity usage ratio of the method is low,
The stability of product is poor；Gamma-radiation method preparation technology is simple, and operation is easy, can at normal temperatures and pressures carry out, can preferably expand
Large-scale production, but cupric must be step by step reduced into elemental metals copper particle under ray intense irradiation；Sedimentation pair is set
It is standby to require higher, and equipment is expensive, is awkward；Microemulsion method can prepare the product of single-size and pattern, but remove production
The surfactant on thing surface needs exacting terms and a large amount of detergent, and production cost is higher and easily pollutes environment；Chemistry is heavy
Shallow lake method course of reaction is simple, be easy to promote and industrialized production, but the composition situation of solid solution sediment be it is fairly limited,
Such as to obtain product micro mist, it is necessary to focus on the Composition Control of solution and the management of precipitation composition, cost relative increase；Electrolysis is given birth to
Produce purity high, but particle diameter is big, in irregular shape；The most toxic side effect of reducing agent that liquid phase reduction is used, if using careless
Environment may be polluted, such as hydrazine hydrate, sodium borohydride, formaldehyde and hydroxylamine hydrochloride are harmful.By simply
Raw material, gentle reaction condition simultaneously obtain the good Nanometer Copper of anti-microbial property with relatively low cost, have become engineering research neck
One direction in domain.
The content of the invention
It is an object of the invention to solve shortcoming and defect present in above-mentioned existing preparation method, there is provided a kind of ultrasonic liquid
The method that phase reduction prepares Nanometer Copper, the preparation method is simple and easy to do, repeated good, granular size is controllable, production cost compared with
Low and environmentally friendly, with important economy and social effect, development prospect is wide.
The present invention is achieved through the following technical solutions：
A kind of method that supersonic liquid phase reduction prepares Nanometer Copper, comprises the following steps：
(1) copper nitrate solution and ascorbic acid solution are prepared respectively；
(2) a certain amount of polyvinylpyrrolidone is weighed, is dissolved in copper nitrate solution, the water-bath under magnetic agitation effect
It is heated to 30~70 DEG C；
(3) ascorbic acid solution is added into step (2) resulting solution, be well mixed, be placed in ultrasonic reactor and react
After a period of time, room temperature is gradually cooling to；
(4) high speed centrifugation after the solution ethanol of cooling is diluted, removes supernatant liquor, and this process is repeated 3 times；
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, it is pure nanometer to obtain red-brown powder
Copper particle.
Preferably, copper nitrate solution preparation method is in step (1)：Take a certain amount of copper nitrate to be dissolved in ethanol, configure dense
Spend the copper nitrate solution for 0.06~0.35mol/L.
Preferably, ascorbic acid solution manufacturing method is in step (1)：Take a certain amount of ascorbic acid to be dissolved in ethanol, match somebody with somebody
Put the ascorbic acid solution that concentration is 0.5~1.5mol/L.
Preferably, copper nitrate and polyvinylpyrrolidone mol ratio are 1 in step (2)：1~1：30.
Preferably, copper nitrate and ascorbic acid mol ratio are 1 in step (3)：1~1：3.
Preferably, the ultrasonic reaction time is 10~40min in step (3).
Preferably, centrifugal condition is in step (4)：Rotating speed 10000rpm/min, centrifugation time 10min.
Nanometer Copper：Nanometer Copper has that size is small, specific surface area is big, resistance is small, quantum size effect, macroscopic quantum are imitated with road
The features such as answering, can replace noble silver big in terms of conductive material, effective catalyst, lube oil additive and antiseptic is prepared
Cost is reduced greatly, with important economic and social benefit.Secondly, medicine is made by raw material of copper nanoparticle, and (weight ratio is
0.2%~0.4%), with obvious reduction mda content, improve the lipid peroxidation infringement caused by oxygen radical,
Strengthen body superoxide dismutase levels, the characteristic of its functional activity expression is adjusted, so as to intervene, postpone body tissue structure
Converted to aging.Research finds that Nanometer Copper also has significant curative effect to cerebral ischemia, cerebral embolism sequela, osteoporosis etc..
Polyvinylpyrrolidone：Polyvinylpyrrolidone abbreviation PVP, is a kind of non-ionic macromolecule compound, has
Hypotoxicity, physiological compatibility and excellent solubility property, are widely used in fields such as medicine, food, cosmetics.In PVP molecules
O, N lone pair electrons can be with Cu2+Between form covalent bond, PVP-Cu is formed in reaction system2+Complicated complexing body, when also
Former agent is Cu2+When being reduced into copper nano-particle, the steric hindrance of this complexing body formation can play the work for preventing copper particle from reuniting
With.Copper nanoparticle is smaller due to particle, and the atom number for being in wafer surface areas is more so that its activity is than in crystal
The atom in portion is high, extremely unstable.Therefore, appropriate PVP is added in preparation process as protective agent, can effectively be prevented
Only nano copper particle is reunited, and is increased granule stability, is preferably received so as to obtain narrow particle size distribution range, good dispersion, crystal formation
Rice copper powder.
Ascorbic acid：Ascorbic acid is a kind of high water soluble compound, with very strong polarity, in its molecular structure by
Carboxylic acid double bond, hydroxyl lone pair electrons, carbonyl double bond one conjugated system of formation of lactonic ring, the system can provide enough electricity
Son, Cu2+Elemental copper is reduced into, and ascorbic acid is then oxidized to hydroascorbic acid.
Beneficial effects of the present invention：
1st, the present invention is by the way that copper nitrate and ascorbic acid are dissolved in ethanol, and the synthesis that inorganic matter is carried out in organic phase is anti-
Should, reaction rate can be better controled over, the monodispersity of Nanometer Copper size is improved.
2nd, the present invention reduces copper nitrate by ascorbic acid and prepares Nanometer Copper, adopt simultaneously using under the conditions of ultrasonic reaction
With polyvinylpyrrolidone as protective agent, the formation of nano copper particle and disperseing in the solution can be effectively facilitated, prevents from receiving
Rice copper particle agglomeration, increases granule stability, so as to obtain the preferable Nanometer Copper of narrow particle size distribution range, good dispersion, crystal formation
Powder.
3rd, simple production process of the present invention, production cost are relatively low and environmentally friendly, it is easy to large-scale production, with weight
The economy and social effect wanted, development prospect are wide.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
A kind of method that supersonic liquid phase reduction prepares Nanometer Copper, comprises the following steps：
(1) 0.06mol copper nitrates and 1.5mol ascorbic acid are weighed respectively, is dissolved in respectively in 1L ethanol, and configuration concentration is
0.06mol/L copper nitrate solution and concentration is 1.5mol/L ascorbic acid solution；
(2) 1.8mol polyvinylpyrrolidones are weighed, is dissolved in 1L0.06mol/L copper nitrate solutions, makes copper nitrate
It is 1 with polyvinylpyrrolidone mol ratio：30, heating water bath is to 50 DEG C under magnetic agitation effect；
(3) 40mL 1.5mol/L ascorbic acid solution is added into step (2) resulting solution, make copper nitrate with it is anti-bad
Hematic acid mol ratio is 1：1, it is well mixed, is placed in ultrasonic reactor and reacts after 40min, be gradually cooling to room temperature；
(4) after the solution ethanol of cooling is diluted, 10000rpm/min centrifugation 10min remove supernatant liquor, this process
It is repeated 3 times；
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, it is pure nanometer to obtain red-brown powder
Copper particle.
Embodiment 2
A kind of method that supersonic liquid phase reduction prepares Nanometer Copper, comprises the following steps：
(1) 0.2mol copper nitrates and 1.0mol ascorbic acid are weighed respectively, is dissolved in respectively in 1L ethanol, and configuration concentration is
0.2mol/L copper nitrate solution and concentration is 1.0mol/L ascorbic acid solution；
(2) 4mol polyvinylpyrrolidones are weighed, are dissolved in 1L 0.2mol/L copper nitrate solutions, make copper nitrate with
Polyvinylpyrrolidone mol ratio is 1：20, heating water bath is to 30 DEG C under magnetic agitation effect；
(3) 400mL 1.0mol/L ascorbic acid solution is added into step (2) resulting solution, make copper nitrate with it is anti-bad
Hematic acid mol ratio is 1：2, it is well mixed, is placed in ultrasonic reactor and reacts after 20min, be gradually cooling to room temperature；
(4) after the solution ethanol of cooling is diluted, 10000rpm/min centrifugation 10min remove supernatant liquor, this process
It is repeated 3 times；
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, it is pure nanometer to obtain red-brown powder
Copper particle.
Embodiment 3
A kind of method that supersonic liquid phase reduction prepares Nanometer Copper, comprises the following steps：
(1) 0.35mol copper nitrates and 0.5mol ascorbic acid are weighed respectively, is dissolved in respectively in 1L ethanol, and configuration concentration is
0.35mol/L copper nitrate solution and concentration is 0.5mol/L ascorbic acid solution；
(2) 0.35mol polyvinylpyrrolidones are weighed, is dissolved in 1L0.35mol/L copper nitrate solutions, makes copper nitrate
It is 1 with polyvinylpyrrolidone mol ratio：1, heating water bath is to 70 DEG C under magnetic agitation effect；
(3) into step (2) resulting solution add 2100mL0.5mol/L ascorbic acid solution, make copper nitrate with it is anti-bad
Hematic acid mol ratio is 1：3, it is well mixed, is placed in ultrasonic reactor and reacts after 10min, be gradually cooling to room temperature；
(4) after the solution ethanol of cooling is diluted, 10000rpm/min centrifugation 10min remove supernatant liquor, this process
It is repeated 3 times；
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, it is pure nanometer to obtain red-brown powder
Copper particle.
Comparative example 1
Protected in a kind of method that supersonic liquid phase reduction prepares Nanometer Copper, preparation process without polyvinylpyrrolidone
Agent, comprises the following steps：
(1) 0.2mol copper nitrates and 1.0mol ascorbic acid are weighed respectively, is dissolved in respectively in 1L ethanol, and configuration concentration is
0.2mol/L copper nitrate solution and concentration is 1.0mol/L ascorbic acid solution；
(2) by 1L0.2mol/L copper nitrate solutions magnetic agitation effect under heating water bath to 30 DEG C；
(3) 400mL 1.0mol/L ascorbic acid solution is added into step (2) resulting solution, make copper nitrate with it is anti-bad
Hematic acid mol ratio is 1：2, it is well mixed, is placed in ultrasonic reactor and reacts after 20min, be gradually cooling to room temperature；
(4) after the solution ethanol of cooling is diluted, 10000rpm/min centrifugation 10min remove supernatant liquor, this process
It is repeated 3 times；
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, it is pure nanometer to obtain red-brown powder
Copper particle.
Comparative example 2
Replace organic solvent second using distilled water in a kind of method that supersonic liquid phase reduction prepares Nanometer Copper, preparation process
Alcohol, comprises the following steps：
(1) 0.2mol copper nitrates and 1.0mol ascorbic acid are weighed respectively, is dissolved in respectively in 1L distilled water, and configuration concentration is
0.2mol/L copper nitrate solution and concentration is 1.0mol/L ascorbic acid solution；
(2) 4mol polyvinylpyrrolidones are weighed, are dissolved in 1L 0.2mol/L copper nitrate solutions, make copper nitrate with
Polyvinylpyrrolidone mol ratio is 1：20, heating water bath is to 30 DEG C under magnetic agitation effect；
(3) 400mL 1.0mol/L ascorbic acid solution is added into step (2) resulting solution, make copper nitrate with it is anti-bad
Hematic acid mol ratio is 1：2, it is well mixed, is placed in ultrasonic reactor and reacts after 20min, be gradually cooling to room temperature；
(4) after the solution ethanol of cooling is diluted, 10000rpm/min centrifugation 10min remove supernatant liquor, this process
It is repeated 3 times；
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, it is pure nanometer to obtain red-brown powder
Copper particle.
Test example 1
The measure of Nanometer Copper average grain diameter
1st, test objective：Detect the Nanometer Copper as obtained by a kind of supersonic liquid phase reduction of the present invention prepares the method for Nanometer Copper
Average grain diameter.
2nd, sample is detected：The nanometer copper sample prepared by above-described embodiment 1~3 and comparative example 1~2.
3rd, detection method：Using laser particle size analyzer detection sample particle diameter distribution and average grain diameter.
4th, testing result：Testing result is as shown in table 1 below.
The Nanometer Copper average grain diameter measurement result of table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | |
| Nanometer Copper average grain diameter (nm) | 47 | 35 | 43 | 96 | 87 |
5th, conclusion
After testing, compared with comparative example 1, the average grain of Nanometer Copper prepared by the embodiment of the present invention 1, embodiment 2, embodiment 3
Footpath reduces 49nm, 61nm, 53nm respectively；Compared with comparative example 2, prepared by the embodiment of the present invention 1, embodiment 2, embodiment 3 receives
Rice copper average grain diameter reduces 40nm, 52nm, 44nm respectively, wherein the best results of embodiment 2, shows a kind of ultrasonic liquid of the present invention
The method that phase reduction prepares Nanometer Copper can effectively prevent the reunion of copper nano particles, suppress the continued growth of copper, reach and control it
The purpose of size.
Test example 2
The measure of Nanometer Copper dispersion stabilization
1st, test objective：Detect the Nanometer Copper as obtained by a kind of supersonic liquid phase reduction of the present invention prepares the method for Nanometer Copper
Dispersion stabilization.
2nd, sample is detected：The nanometer copper sample prepared by above-described embodiment 1~3 and comparative example 1~2.
3rd, detection method：Settling methods.The copper nanoparticle that will be prepared is configured to the Cu-H that mass fraction is 5%2O
Nano-colloid, is placed in being carved with the test tube of scale after ultrasound 20min of same size, stands one week, measures clarified solution above
Then divided by liquid surface total height H obtains settling ratio height h, settling ratio is smaller, and dispersion stabilization is better.
4th, testing result：Testing result is as shown in table 2 below.
The Nanometer Copper dispersion stabilization measurement result of table 2
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | |
| Settling ratio | 0.07 | 0.05 | 0.07 | 0.21 | 0.13 |
5th, conclusion
After testing, compared with comparative example 1, Nanometer Copper settling ratio prepared by the embodiment of the present invention 1, embodiment 2, embodiment 3
Reduce 0.14,0.16,0.14 respectively；Compared with comparative example 2, nanometer prepared by the embodiment of the present invention 1, embodiment 2, embodiment 3
Copper settling ratio reduces 0.06,0.08,0.06 respectively, wherein the best results of embodiment 2, shows that Nanometer Copper prepared by the present invention disperses
Stability is good.
Claims (7)
1. a kind of method that supersonic liquid phase reduction prepares Nanometer Copper, it is characterised in that comprise the following steps：
(1) copper nitrate solution and ascorbic acid solution are prepared respectively；
(2) a certain amount of polyvinylpyrrolidone is weighed, is dissolved in copper nitrate solution, the heating water bath under magnetic agitation effect
To 30~70 DEG C；
(3) ascorbic acid solution is added into step (2) resulting solution, be well mixed, be placed in ultrasonic reactor and react one section
After time, room temperature is gradually cooling to；
(4) high speed centrifugation after the solution ethanol of cooling is diluted, removes supernatant liquor, and this process is repeated 3 times；
(5) step (4) products therefrom is dried in vacuo 24h at room temperature, it is pure Nanometer Copper to obtain red-brown powder
Grain.
2. the method that a kind of supersonic liquid phase reduction according to claim 1 prepares Nanometer Copper, it is characterised in that the step
Suddenly copper nitrate solution preparation method is in (1)：A certain amount of copper nitrate is taken to be dissolved in ethanol, configuration concentration is 0.06~0.35mol/
L copper nitrate solution.
3. the method that a kind of supersonic liquid phase reduction according to claim 1 prepares Nanometer Copper, it is characterised in that the step
Suddenly ascorbic acid solution manufacturing method is in (1)：Take a certain amount of ascorbic acid to be dissolved in ethanol, configuration concentration be 0.5~
1.5mol/L ascorbic acid solution.
4. the method that a kind of supersonic liquid phase reduction according to claim 1 prepares Nanometer Copper, it is characterised in that the step
Suddenly copper nitrate and polyvinylpyrrolidone mol ratio are 1 in (2)：1~1：30.
5. the method that a kind of supersonic liquid phase reduction according to claim 1 prepares Nanometer Copper, it is characterised in that the step
Suddenly copper nitrate and ascorbic acid mol ratio are 1 in (3)：1~1：3.
6. the method that a kind of supersonic liquid phase reduction according to claim 1 prepares Nanometer Copper, it is characterised in that the step
Suddenly the ultrasonic reaction time is 10~40min in (3).
7. the method that a kind of supersonic liquid phase reduction according to claim 1 prepares Nanometer Copper, it is characterised in that the step
Suddenly centrifugal condition is in (4)：Rotating speed 10000rpm/min, centrifugation time 10min.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109122720A (en) * | 2018-09-20 | 2019-01-04 | 安徽江淮汽车集团股份有限公司 | A kind of antibacterial agent and preparation method thereof |
| CN109822090A (en) * | 2017-11-23 | 2019-05-31 | 中国科学院化学研究所 | A kind of preparation method of the copper nanoparticle of in-stiu coating organic matter |
| CN110153443A (en) * | 2019-07-11 | 2019-08-23 | 中国科学院深圳先进技术研究院 | A kind of copper nanometer sheet and its preparation method and application |
| CN111496266A (en) * | 2020-05-09 | 2020-08-07 | 哈尔滨工业大学(深圳)(哈尔滨工业大学深圳科技创新研究院) | Environment-friendly conductive nano copper ink and preparation method thereof |
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| CN111922360A (en) * | 2020-10-19 | 2020-11-13 | 西安宏星电子浆料科技股份有限公司 | Preparation method of nano copper powder |
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| CN109822090A (en) * | 2017-11-23 | 2019-05-31 | 中国科学院化学研究所 | A kind of preparation method of the copper nanoparticle of in-stiu coating organic matter |
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| CN111687408A (en) * | 2020-06-29 | 2020-09-22 | 太原师范学院 | Fluorescent copper nanocluster, preparation method and application thereof |
| CN111922360A (en) * | 2020-10-19 | 2020-11-13 | 西安宏星电子浆料科技股份有限公司 | Preparation method of nano copper powder |
| CN114672305A (en) * | 2022-03-23 | 2022-06-28 | 中电华创电力技术研究有限公司 | Preparation method of copper nanocluster fluorescent probe and detection method of hypochlorite in water environment |
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| CN115141423B (en) * | 2022-07-07 | 2023-11-21 | 沪本新材料科技（上海）有限公司 | Preparation method of core-shell structured nano copper particle polyethylene ball antibacterial master batch |
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