CN101664810B - Method for synthetizing nano-copper in microemulsion system - Google Patents

Method for synthetizing nano-copper in microemulsion system Download PDF

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CN101664810B
CN101664810B CN2009100923519A CN200910092351A CN101664810B CN 101664810 B CN101664810 B CN 101664810B CN 2009100923519 A CN2009100923519 A CN 2009100923519A CN 200910092351 A CN200910092351 A CN 200910092351A CN 101664810 B CN101664810 B CN 101664810B
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microemulsion
copper
water
kbh
cuso
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CN101664810A (en
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张敬畅
曾婷
杨秀英
曹维良
李海平
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Beijing University of Chemical Technology
Hainan Institute of Science and Technology
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Beijing University of Chemical Technology
Hainan Institute of Science and Technology
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Abstract

The invention provides a method for synthetizing nano-copper in a microemulsion system. Under the alkaline condition, nano-copper with the particle size of about 10-20 nm, uniform particle size distribution and high purity is prepared in the microemulsion system with a specific ratio by using KBH4 as a reducing agent and using CuSO4-5H2O as a copper source; and at the same time of synthesis, the surface of the nano-copper is coated by a surfactant so that the nano-copper has high dispersibility, can not be easily oxidized and can be stored conveniently. The process has the advantages of mild preparation condition, simple preparation process, no toxicity or pollution, low cost, small particle size and uniform dispersion of the prepared nano-copper, and the like.

Description

The method of synthetizing nano-copper in a kind of microemulsion system
Technical field
The present invention relates to the nano material synthesis technical field, be specifically related to a kind of in microemulsion system the method for synthetizing nano-copper.
Technical background
In various wires and metal nano-rod, copper is the most frequently used, because copper has superior conductivity of heat and high electrical conductivity.Copper is used as the important devices that is interconnected in electronic circuit always for a long time, because it is a kind of good conductor.Because the price of copper powder is more much lower than the price of noble metal silver powder, palladium powder, thereby more and more is subject to people's attention, and has broad application prospects.In today that the nano material development is maked rapid progress, the application of nanometer copper also receives much concern, and has obtained utilization widely.For example: superfine cupper powder can be used as raw material, electrode material of electrically-conducting paint and conducing composite material etc.; Copper nanoparticle is good catalyst at metallurgy and petrochemical industry in the reactions such as the hydrogenation of high molecular polymer and dehydrogenation; Nanometer copper also has the little cut of filling as lubricated oil additive, reduces the effect of friction and wear; Copper nanoparticle also is preparation high conductivity, the indispensable basic material of the brilliant copper of high-strength nano; In addition, nanometer copper also plays an important role in fields such as medicine, bioengineering.Therefore preparation technology and the technology of furtheing investigate nanometer copper have great importance, and are to promote the extensively motive power of utilization of nanometer copper.
It is simple that micro-emulsion method for preparing nano copper has preparation process, less demanding to equipment, advantage such as cost is low, and is pollution-free.Be to study focus at present.When preparing nano material, normally two kinds of reactants are dissolved in respectively and form in identical two microemulsion systems, mix the microemulsion system of two reactions, make to react mass exchange between the reactant, generate product with microemulsion.After the reaction, nanoparticle is separated with microemulsion, obtain nano material after the washing drying by centrifugation or adding demulsifier.Microemulsion system is by transparent, isotropic thermodynamic stable system of surfactant, cosurfactant, the phase composition of oil phase Heshui.The type of microemulsion has: oil-in-water type (O/W), water-in-oil type (W/O) and co-continuous facies type (or in the micro emulsion mutually).Wherein, W/O is for the most common aspect preparation, the micro emulsion granular size that the monolayer that surfactant and cosurfactant constituted in the w/o type microemulsion is surrounded as several between tens nanometers, these small " ponds " are separated from one another, these drops do not stop diffusion and collision in continuous phase, and the continuous exchange of carrying out material between " pond " has formed good " microreactor ", so makes in the process of micro-emulsion method for preparing nano copper that the particle diameter of copper powder has controllability.Choose certain surfactant and can make nanometer copper prepare the hydrophilic or lipophilic group that the rear surface connects surfactant, make nanometer copper obtain preliminary surface modification.
Document: Xu Jiansheng, Cai Yifei, Yuan Xiaohui. microemulsion method prepares the research [J] of oil solubility nanometer metallic copper. Wuhan Institute of Chemical Technology's journal, 2006,28 (1): among the 50-53, employing is aided with triethanolamine again with Si Ban and tween mixed surfactant and is mixed with microemulsion system in lubricating oil, with NaBH 4For reducing agent prepares nanometer copper, it is good to obtain oil-soluble, the product about the about 10nm of particle diameter.But this method obtains nanometer copper in lubricating oil, is not easy away unreacted reactant, influences the performance of lubricating oil, and, be difficult to obtain the copper nanoparticle body, be not easy to nanometer copper and be used for other aspects.
Document: Hao Chuncheng, Xiao Feng, Yuan Shenli. utilize prepared by reverse microemulsion method nanometer copper particle [J]. the material Leader, 2007,21 (5): 65-66.] make surfactant with enuatrol, isooctane is an oil phase preparation microemulsion system, is that reducing agent prepares nanometer copper with the hydrazine hydrate, obtains the product that particle diameter is 10-50nm.This method can be controlled the particle diameter of synthetizing nano-copper by the content that changes the surfactant enuatrol, but hydrazine hydrate is poisonous, does not meet the standard of Green Chemistry.
Summary of the invention
The purpose of this invention is to provide a kind of Cu that in microemulsion system, reduces 2+The method for preparing nanometer copper, the copper nanoparticle body particle diameter that obtains is little, and particle diameter is evenly distributed, and purity height, and the nanometer copper that obtains surface absorption upper surface activating agent can be considered preliminary modification has been carried out on the surface of nanometer copper.
Method provided by the present invention is with KBH 4Be reducing agent, in microemulsion system, alkali condition is reduction CuSO down 45H 2O, preparation nanometer copper.
Concrete preparation process is as follows:
A.CuSO 45H 2The preparation of O microemulsion: with CuSO 45H 2O is dissolved in ammoniacal liquor, and to be mixed with concentration be 0.1-0.5mol/L cuprammonium complex ion solution, is water with this solution, and according to surfactant: cosurfactant: oil phase: the water mass ratio is 1: 5-20: 2-44: 0.2-1.4 prepares CuSO 45H 2The O microemulsion system, and disperse to mix with ultrasonic wave;
B.KBH 4The preparation of microemulsion: with KBH 4Being dissolved in deionized water and being mixed with the reducing solution that concentration is 0.25-1mol/L, add KOH and regulate pH=12, is water with this solution, and according to surfactant: cosurfactant: oil phase: the water mass ratio is 1: 5-20: 2-44: 0.2-1.4 prepares KBH 4Microemulsion, and disperse to mix with ultrasonic wave;
The microemulsion with steps A that C. will prepare places reactor, keeps 5-30 ℃ of temperature, and wherein 15-20 ℃ is optimal reaction temperature, under the vigorous stirring according to mol ratio CuSO 45H 2O: KBH 4=1: 0.25-2 drips the microemulsion of step B in the reactor, and reaction system becomes brownish red very soon, and has bubble to generate, carry out centrifugation behind the reaction 0.5-1.5h, with deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains powder in the vacuum.
Surfactant described in steps A and the B is lauryl alcohol polyethylene glycol oxide (a 3) ether; Described cosurfactant is n-butanol, n-amyl alcohol or n-hexyl alcohol; Described oil phase is n-hexane or cyclohexane; The CuSO of steps A wherein 45H 2The B KBH of O microemulsion and step 4Surfactant, cosurfactant and oil-phase component used in the microemulsion are identical with ratio.
The sample that obtains is characterized: Fig. 1 is an X-ray powder diffraction spectrogram, is found out by Fig. 1, has only the characteristic peak of nanometer copper among the figure, does not have other assorted peaks, illustrates that nanometer copper purity is good; Calculating its particle diameter by Scherrer formula (Scherrer equation) is 11nm.
Fig. 2 is infrared (IR) spectrogram of the nanometer copper of embodiment 1 preparation; Find out that by Fig. 2 there is the characteristic peak of tangible surfactant A EO-3 on nanometer copper surface, illustrate that nanometer copper surface is coated with AEO-3, make nanometer copper have good dispersiveness, be difficult for oxidized, the convenient preservation, and help the nanometer copper surface modification that improves.
The invention has the beneficial effects as follows:
1) reaction condition gentleness, the reaction time is short, pollutes gently, and the three wastes are few, and preparation process and aftertreatment technology are simple.
2) the nanometer shot copper that obtains of prepared in reaction directly is 10-20nm, and particle diameter is evenly distributed, and purity is good.
3) problems such as no equipment corrosion and environmental pollution require lowly to equipment is corrosion-resistant, and technological process is short, the production process environmental friendliness, and equipment investment and operating cost are low.
Description of drawings
Fig. 1 is X-ray powder diffraction (XRD) spectrogram of the nanometer copper of embodiment 1 preparation
Fig. 2 is infrared (IR) spectrogram of the nanometer copper of embodiment 1 preparation;
The specific embodiment
Embodiment 1
A.CuSO 45H 2The preparation of O microemulsion (A liquid): with 0.1873g CuSO 45H 2O is dissolved in 1.5ml, is mixed with cuprammonium complex ion solution (0.5mol/L) in the ammoniacal liquor of 3mol/L, is that water and AEO-3, n-butanol, cyclohexane mix with this solution, disperses with ultrasonic wave.Wherein, AEO-3, n-butanol, cyclohexane, water mass ratio are 1: 10: 3.33: 0.94.
B.KBH 4The preparation of microemulsion (B liquid): with 0.0404g KBH 4Being dissolved in the 1.5ml deionized water with KOH and being mixed with reducing solution, make pH=12, is that water and AEO-3, n-butanol, cyclohexane mix with this solution, disperses with ultrasonic wave.Wherein, AEO-3, n-butanol, cyclohexane, water mass ratio are 1: 10: 3.33: 0.94.
C. the A liquid for preparing is placed reactor, keep temperature T=15 ℃ in the water-bath, following B drop of vigorous stirring added in the A liquid, reaction system becomes brownish red very soon, and have bubble to generate, and carry out centrifugation behind the reaction 1h, use deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains 0.0288g powder nanometer copper in the vacuum.Recording its particle diameter is 11nm.
Embodiment 2
A.CuSO 45H 2The preparation of O microemulsion (A liquid): with 0.1225g CuSO 45H 2O is dissolved in 1.0ml, in the ammoniacal liquor of 3mol/L, add the 0.5ml deionized water again, be mixed with cuprammonium complex ion solution (0.3mol/L), with this solution is that water and AEO-3, n-butanol, cyclohexane mix, disperse with ultrasonic wave, wherein, AEO-3, n-butanol, cyclohexane, water mass ratio are 1: 10: 3.33: 0.94;
B.KBH 4The preparation of microemulsion (B liquid): with 0.0529g KBH 4Be dissolved in the 1.5ml deionized water with KOH and be mixed with reducing solution, making pH=12, is that water and AEO-3, n-butanol, cyclohexane mix with this solution, disperses with ultrasonic wave, wherein, AEO-3, n-butanol, cyclohexane, water mass ratio are 1: 10: 3.33: 0.94;
C. the A liquid for preparing is placed reactor, keep temperature T=15 ℃ in the water-bath, following B drop of vigorous stirring added in the A liquid, reaction system becomes brownish red very soon, and have bubble to generate, and carry out centrifugation behind the reaction 1h, use deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains 0.0179g powder nanometer copper in the vacuum.Recording its particle diameter is 11nm.
Embodiment 3
A.CuSO 45H 2The preparation of O microemulsion (A liquid): with 0.1615g CuSO 45H 2O is dissolved in 1.0ml, in the ammoniacal liquor of 3mol/L, add the 0.5ml deionized water again, be mixed with cuprammonium complex ion solution (0.43mol/L), with this solution is that water and AEO-3, n-amyl alcohol, cyclohexane mix, disperse with ultrasonic wave, wherein, AEO-3, n-amyl alcohol, cyclohexane, water mass ratio are 1: 10: 2.57: 0.38;
B.KBH 4The preparation of microemulsion (B liquid): with 0.0349g KBH 4Be dissolved in the 1.5ml deionized water with KOH and be mixed with reducing solution, making pH=12, is that water and AEO-3, n-amyl alcohol, cyclohexane mix with this solution, disperses with ultrasonic wave, wherein, AEO-3, n-amyl alcohol, cyclohexane, water mass ratio are 1: 10: 2.57: 0.38;
C. the A liquid for preparing is placed reactor, keep temperature T=15 ℃ in the water-bath, following B drop of vigorous stirring added in the A liquid, reaction system becomes brownish red very soon, and have bubble to generate, and carry out centrifugation behind the reaction 1h, use deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains 0.0211g powder nanometer copper in the vacuum.Recording its particle diameter is 11nm.
Embodiment 4
A.CuSO 45H 2The preparation of O microemulsion (A liquid): with 0.1102g CuSO 45H 2O is dissolved in 1.0ml, in the ammoniacal liquor of 3mol/L, add the 1.0ml deionized water again, be mixed with cuprammonium complex ion solution (0.22mol/L), with this solution is that water and AEO-3, n-amyl alcohol, n-hexane mix, disperse with ultrasonic wave, wherein, AEO-3, n-amyl alcohol, n-hexane, water mass ratio are 1: 5: 3.48: 0.44;
B.KBH 4The preparation of microemulsion (B liquid): with 0.0238g KBH 4Be dissolved in the 2.0ml deionized water with KOH and be mixed with reducing solution, making pH=12, is that water and AEO-3, n-amyl alcohol, n-hexane mix with this solution, disperses with ultrasonic wave, wherein, AEO-3, n-amyl alcohol, n-hexane, water mass ratio are 1: 5: 3.48: 0.44;
C. the A liquid for preparing is placed reactor, keep temperature T=15 ℃ in the water-bath, following B drop of vigorous stirring added in the A liquid, reaction system becomes brownish red very soon, and have bubble to generate, and carry out centrifugation behind the reaction 1h, use deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains 0.0144g powder nanometer copper in the vacuum.Recording its particle diameter is 18nm.
Embodiment 5
A.CuSO 45H 2The preparation of O microemulsion (A liquid): with 0.1639g CuSO 45H 2O is dissolved in 1.0ml, in the ammoniacal liquor of 3mol/L, add the 0.5ml deionized water again, be mixed with cuprammonium complex ion solution (0.44mol/L), with this solution is that water and AEO-3, n-butanol, cyclohexane mix, disperse with ultrasonic wave, wherein, AEO-3, n-butanol, cyclohexane, water mass ratio are 1: 20: 31.4: 0.8;
B.KBH 4The preparation of microemulsion (B liquid): with 0.0354g KBH 4Be dissolved in the 1.5ml deionized water with KOH and be mixed with reducing solution, making pH=12, is that water and AEO-3, n-butanol, cyclohexane mix with this solution, disperses with ultrasonic wave, wherein, AEO-3, n-butanol, cyclohexane, water mass ratio are 1: 20: 31.4: 0.8;
C. the A liquid for preparing is placed reactor, keep temperature T=15 ℃ in the water-bath, following B drop of vigorous stirring added in the A liquid, reaction system becomes brownish red very soon, and have bubble to generate, and carry out centrifugation behind the reaction 1h, use deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains 0.0218g powder nanometer copper in the vacuum.Recording its particle diameter is 15nm.
Embodiment 6
A.CuSO 45H 2The preparation of O microemulsion (A liquid): with 0.2247g CuSO 45H 2O is dissolved in 1.0ml, in the ammoniacal liquor of 3mol/L, add the 0.5ml deionized water again, be mixed with cuprammonium complex ion solution (0.5mol/L), with this solution is that water and AEO-3, n-butanol, cyclohexane mix, disperse with ultrasonic wave, wherein, AEO-3, n-butanol, cyclohexane, water mass ratio are 1: 15: 10.66: 0.96;
B.KBH 4The preparation of microemulsion (B liquid): with 0.0364g KBH 4Be dissolved in the 1.5ml deionized water with KOH and be mixed with reducing solution, making pH=12, is that water and AEO-3, n-butanol, cyclohexane mix with this solution, disperses with ultrasonic wave, wherein, AEO-3, n-butanol, cyclohexane, water mass ratio are 1: 15: 10.66: 0.96;
C. the A liquid for preparing is placed reactor, keep temperature T=5 ℃ in the water-bath, following B drop of vigorous stirring added in the A liquid, reaction system becomes brownish red very soon, and have bubble to generate, and carry out centrifugation behind the reaction 1h, use deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains 0.0204g powder nanometer copper in the vacuum.Recording its particle diameter is 10nm.
Embodiment 7
A.CuSO 45H 2The preparation of O microemulsion (A liquid): with 0.1873g CuSO 45H 2O is dissolved in 1.0ml, in the ammoniacal liquor of 3mol/L, add the 0.5ml deionized water again, be mixed with cuprammonium complex ion solution (0.5mol/L), with this solution is that water and AEO-3, n-hexyl alcohol, cyclohexane mix, disperse with ultrasonic wave, wherein, AEO-3, n-hexyl alcohol, cyclohexane, water mass ratio are 1: 5: 2.57: 0.24;
B.KBH 4The preparation of microemulsion (B liquid): with 0.0405g KBH 4Be dissolved in the 1.5ml deionized water with KOH and be mixed with reducing solution, making pH=12, is that water and AEO-3, n-hexyl alcohol, cyclohexane mix with this solution, disperses with ultrasonic wave, wherein, AEO-3, n-hexyl alcohol, cyclohexane, water mass ratio are 1: 5: 2.57: 0.24;
C. the A liquid for preparing is placed reactor, keep temperature T=15 ℃ in the water-bath, following B drop of vigorous stirring added in the A liquid, reaction system becomes brownish red very soon, and have bubble to generate, and carry out centrifugation behind the reaction 1h, use deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains 0.0219g powder nanometer copper in the vacuum.Recording its particle diameter is 13nm.
Embodiment 8
A.CuSO 45H 2The preparation of O microemulsion (A liquid): with 0.1498g CuSO 45H 2O is dissolved in 1.0ml, in the ammoniacal liquor of 3mol/L, add the 0.5ml deionized water again, be mixed with cuprammonium complex ion solution (0.4mol/L), with this solution is that water and AEO-3, n-hexyl alcohol, n-hexane mix, disperse with ultrasonic wave, wherein, AEO-3, n-hexyl alcohol, n-hexane, water mass ratio are 1: 10: 7.33: 0.88;
B.KBH 4The preparation of microemulsion (B liquid): with 0.0324g KBH 4Be dissolved in the 1.5ml deionized water with KOH and be mixed with reducing solution, making pH=12, is that water and AEO-3, n-hexyl alcohol, n-hexane mix with this solution, disperses with ultrasonic wave, wherein, AEO-3, n-hexyl alcohol, n-hexane, water mass ratio are 1: 10: 7.33: 0.88;
C. the A liquid for preparing is placed reactor, keep temperature T=15 ℃ in the water-bath, following B drop of vigorous stirring added in the A liquid, reaction system becomes brownish red very soon, and have bubble to generate, and carry out centrifugation behind the reaction 0.5h, use deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains 0.0193g powder nanometer copper in the vacuum.Measuring its particle diameter is 14nm.
Embodiment 9
A.CuSO 45H 2The preparation of O microemulsion (A liquid): with 0.1873g CuSO 45H 2O is dissolved in 1.0ml, in the ammoniacal liquor of 3mol/L, add the 0.5ml deionized water again, be mixed with cuprammonium complex ion solution (0.5mol/L), with this solution is that water and AEO-3, n-butanol, n-hexane mix, disperse with ultrasonic wave, wherein, AEO-3, n-butanol, n-hexane, water mass ratio are 1: 15: 16: 1.11;
B.KBH 4The preparation of microemulsion (B liquid): with 0.0405g KBH 4Be dissolved in the 1.5ml deionized water with KOH and be mixed with reducing solution, making pH=12, is that water and AEO-3, n-butanol, n-hexane mix with this solution, disperses with ultrasonic wave, wherein, AEO-3, n-butanol, n-hexane, water mass ratio are 1: 15: 16: 1.11;
C. the A liquid for preparing is placed reactor, keep temperature T=15 ℃ in the water-bath, following B drop of vigorous stirring added in the A liquid, reaction system becomes brownish red very soon, and have bubble to generate, and carry out centrifugation behind the reaction 1.5h, use deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains 0.0259g powder nanometer copper in the vacuum.Recording its particle diameter is 19nm.
Embodiment 10
A.CuSO 45H 2The preparation of O microemulsion (A liquid): with 0.1124g CuSO 45H 2O is dissolved in 1.0ml, in the ammoniacal liquor of 3mol/L, add the 1.0ml deionized water again, be mixed with cuprammonium complex ion solution (0.3mol/L), with this solution is that water and AEO-3, n-butanol, n-hexane mix, disperse with ultrasonic wave, wherein, AEO-3, n-butanol, n-hexane, water mass ratio are 1: 20: 21: 1.4;
B.KBH 4The preparation of microemulsion (B liquid): with 0.0243g KBH 4Be dissolved in the 2.0ml deionized water with KOH and be mixed with reducing solution, making pH=12, is that water and AEO-3, n-butanol, n-hexane mix with this solution, disperses with ultrasonic wave, wherein, AEO-3, n-butanol, n-hexane, water mass ratio are 1: 20: 21: 1.4;
C. the A liquid for preparing is placed reactor, keep temperature T=30 ℃ in the water-bath, following B drop of vigorous stirring added in the A liquid, reaction system becomes brownish red very soon, and have bubble to generate, and carry out centrifugation behind the reaction 1h, use deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains 0.0138g powder nanometer copper in the vacuum.Recording its particle diameter is 19nm.

Claims (2)

1. the method for synthetizing nano-copper in the microemulsion system, concrete preparation process is as follows:
A.CuSO 45H 2The preparation of O microemulsion: with CuSO 45H 2O is dissolved in ammoniacal liquor, and to be mixed with concentration be 0.1-0.5mol/L cuprammonium complex ion solution, is water with this solution, and according to surfactant: cosurfactant: oil phase: the water mass ratio is 1: 5-20: 2-44: 0.2-1.4 prepares CuSO 45H 2The O microemulsion system, and disperse to mix with ultrasonic wave;
B.KBH 4The preparation of microemulsion: with KBH 4Being dissolved in deionized water and being mixed with the reducing solution that concentration is 0.25-1mol/L, add KOH and regulate pH=12, is water with this solution, and according to surfactant: cosurfactant: oil phase: the water mass ratio is 1: 5-20: 2-44: 0.2-1.4 prepares KBH 4Microemulsion, and disperse to mix with ultrasonic wave;
The microemulsion with steps A that C. will prepare places reactor, keeps 5-30 ℃ of temperature, under the vigorous stirring according to mol ratio CuSO 45H 2O: KBH 4=1: 0.25-2 drips the microemulsion of step B in the reactor, and reaction system becomes brownish red very soon, and has bubble to generate, carry out centrifugation behind the reaction 0.5-1.5h, with deionized water centrifuge washing 2 times, absolute ethyl alcohol centrifuge washing 2 times, drying obtains powder in the vacuum;
Surfactant described in steps A and the B is lauryl alcohol polyethylene glycol oxide (a 3) ether; Described cosurfactant is n-butanol, n-amyl alcohol or n-hexyl alcohol; Described oil phase is n-hexane or cyclohexane.
2. the method for synthetizing nano-copper in the microemulsion system according to claim 1 is characterized in that the described CuSO of steps A 45H 2O microemulsion and the described KBH of step B 4Surfactant in the microemulsion, cosurfactant and oil-phase component are identical with ratio;
The described reaction temperature of step C is 15-20 ℃.
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CN105598464B (en) * 2016-01-06 2017-10-24 哈尔滨工业大学（威海） The in-situ preparation method of copper nano-wire in a kind of microchannel
CN105880625B (en) * 2016-05-04 2018-05-25 四川大学 The method that liquid-liquid two-phase method prepares nano-cobalt powder
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1662447A (en) * 2002-04-25 2005-08-31 通用电气公司 Preparation of nanosized copper (I) compounds
CN101077529A (en) * 2007-07-05 2007-11-28 中南大学 Method for preparing nano copper powder and copper slurry

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1662447A (en) * 2002-04-25 2005-08-31 通用电气公司 Preparation of nanosized copper (I) compounds
CN101077529A (en) * 2007-07-05 2007-11-28 中南大学 Method for preparing nano copper powder and copper slurry

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
徐建生等.微乳液法制备油溶性纳米金属铜的研究.《武汉化工学院学报》.2006,第28卷(第1期),50-53. *
马丽果等.微乳液法制备纳米铜粉及其在润滑油中的应用研究.《润滑与密封》.2004,(第4期),87-88. *

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