CN112238002A - Method for differential separation of nano copper powder with different particle sizes - Google Patents
Method for differential separation of nano copper powder with different particle sizes Download PDFInfo
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- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
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Abstract
The invention relates to a method for differential separation of nanometer copper powder, which comprises the following steps: mixing the nano copper powder to be separated with a first dispersing agent to obtain a mixed solution; carrying out centrifugal separation on the mixed solution to obtain a 1 st precipitate and a 1 st upper layer liquid; continuously carrying out centrifugal separation on the 1 st upper layer liquid to obtain a 2 nd precipitate and a 2 nd upper layer liquid, and repeating the step (N-2) times to obtain an Nth precipitate and an Nth upper layer liquid; and respectively mixing the 1 st to Nth precipitates with a second dispersing agent, and performing centrifugal separation to respectively obtain 1 st to Nth solids. The method has the advantages of simplicity, convenience, economy, good separation effect, less copper powder loss and environmental protection.
Description
Technical Field
The invention relates to a method for separating nano copper powder, in particular to a method for separating nano copper powder with different particle sizes by adopting a differential speed, and belongs to the technical field of copper powder separation.
Background
The nanometer copper powder has larger specific surface area and more surface active centers, and is a better catalyst in metallurgy, petrochemical industry and high polymer reaction, for example, the nanometer copper powder is used as the catalyst in the purification treatment of automobile exhaust. Meanwhile, the nano copper powder is widely used for conductive coatings and electrode materials due to the excellent electrical properties of the nano copper powder. In addition, the ultra-fine thick film slurry prepared by the nano copper powder plays an important and most important role in some larger-scale integrated circuits.
The existing nano copper powder is mainly prepared by a liquid phase method, and the main principle is that a proper soluble salt is selected to dissolve the copper powder, and copper ions exist in a solution in a certain form through treatment, so that the nano copper powder is formed. In addition to the liquid phase method, the solid phase method can also be used for preparing the nano copper powder, such as the ball milling method, the principle is that a ball mill is used for grinding or impacting to separate and polish raw materials into finer particles, and compared with the liquid phase method, the method has the advantages of high yield and simple process, but the polished particles need to be separated.
The particle size separation methods commonly used in industry can be classified into two types, screening and classification, wherein screening is to separate materials on different screen surfaces by using screens, and classification is to separate materials by using the difference of the sedimentation velocity of particles in a fluid medium, and common classification equipment comprises a hydraulic cyclone, a hydraulic classifier, a mechanical classifier and the like. Although the separation effect of the methods is good, the separation equipment is expensive and heavy, and the separation steps are also extremely complicated.
Therefore, it is necessary to research the separation of the copper nanoparticles and find a low-cost, simple and feasible separation method.
Disclosure of Invention
In order to overcome the problems, the inventor of the invention makes a keen study to design a method for separating nano copper powder with different particle sizes in a differential mode, and the method has the advantages of low equipment price, simplicity in operation and good separation effect.
The method comprises the following steps:
step 1: mixing the nano copper powder to be separated with a first dispersing agent to obtain a mixed solution;
step 2: carrying out centrifugal separation on the mixed solution to obtain a 1 st precipitate and a 1 st upper layer liquid;
and step 3: continuously carrying out centrifugal separation on the 1 st upper layer liquid to obtain a 2 nd precipitate and a 2 nd upper layer liquid, and repeating the step (N-2) times to obtain an Nth precipitate and an Nth upper layer liquid;
and 4, step 4: and respectively mixing the 1 st to Nth precipitates with a second dispersing agent, and performing centrifugal separation to respectively obtain 1 st to Nth solids.
Further, drying the No. 1 solid to the No. N solid respectively to obtain the nano copper powder with different particle sizes.
The invention has the advantages that:
(1) simple and economical, and does not need expensive large-scale equipment;
(2) the separation effect is good, and the particle size range of the separated copper powder is narrow;
(3) no chemical reaction, and less copper powder loss in the separation process;
(4) the environment is protected, and the dispersing agent can be recycled in the process.
Drawings
FIG. 1 shows the IR spectra of copper powders obtained in example 1 by separation at different speeds;
FIG. 2 shows a scanning electron micrograph of copper powder before separation in example 1;
FIG. 3 shows an electron micrograph of the copper powder isolated at 500rpm in example 1;
FIG. 4 shows an electron micrograph of copper powder isolated at 3000rpm in example 1;
FIG. 5 shows the electron microscopy of the copper powder isolated at 5000rpm in example 1.
Detailed Description
The present invention will be described in further detail below with reference to examples. The features and advantages of the present invention will become more apparent from the description.
The word "exemplary" is used exclusively herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments.
The invention provides a method for separating nano copper powder with different particle sizes by a differential separation method, which comprises the following steps:
step 1: mixing the nano copper powder to be separated with a first dispersing agent to obtain a mixed solution;
the inventor finds that the viscosity of the dispersant has direct influence on the separation effect, and the high viscosity of the dispersant can cause the copper powder not to precipitate and cannot be separated; the viscosity of the dispersant is too low, so that the dispersant can not achieve the dispersing effect, the copper powder is precipitated too fast and can not be separated effectively,
in the present invention, the first dispersant is a mixture of a low viscosity dispersant and a high viscosity dispersant,
wherein the low viscosity dispersant is a dispersant having a viscosity of from 1 mPaS (20 ℃) to 10 mPaS (20 ℃), preferably a low boiling point, readily volatile dispersant such as ethanol, and the high viscosity dispersant is a dispersant having a viscosity of from 15 mPaS (20 ℃) to 25 mPaS (20 ℃), preferably a dispersant having a viscosity of from 18 mPaS (20 ℃) to 22 mPaS (20 ℃), such as ethylene glycol;
further, the volume ratio of the low-viscosity dispersant to the high-viscosity dispersant is 1: (0.5-2), preferably 1:1,
the mass ratio of the nano copper powder to be separated to the first dispersing agent is 1 (50-200), preferably 1:100, so that the copper powder can be completely dispersed in the dispersing agent;
although the first dispersing agent can provide a good separation effect during centrifugal separation, certain agglomeration phenomenon can occur when the first dispersing agent is mixed with the nano copper powder to be separated, so that stirring ultrasound is required to assist the uniform dispersion of the copper powder in the first dispersing agent during mixing,
in the invention, the time of stirring and ultrasonic treatment is 0.5 to 20 minutes, preferably 1.5 to 10 minutes, and more preferably 2.5 to 5 minutes.
Step 2: carrying out centrifugal separation on the mixed solution to obtain a 1 st precipitate and a 1 st upper layer liquid;
the centrifugal rotating speed of the centrifugal separation is 100-1000 rpm, preferably 300-700 rpm, more preferably 400-600 rpm,
when the rotating speed is lower than 100rpm, the centrifugal force is too small, the copper powder can be rapidly precipitated, effective separation cannot be realized, and when the rotating speed is higher than 1000rpm, the obtained nano copper powder has a wider particle size range and a poor separation effect.
And step 3: continuously carrying out centrifugal separation on the 1 st upper layer liquid to obtain a 2 nd precipitate and a 2 nd upper layer liquid, and repeating the step (N-2) times to obtain an Nth precipitate and an Nth upper layer liquid;
and (2) performing centrifugal separation on the upper layer liquid at the speed 1, wherein the rotation speed is greater than the centrifugal rotation speed in the step 2, repeating the step (N-2 times), wherein the rotation speed of each centrifugal separation is greater than the previous centrifugal rotation speed until the centrifugal rotation speed is increased to more than 3000rpm, preferably more than 4000rpm, more preferably more than 5000rpm, and N is a positive integer not less than 3, preferably N is a positive integer not less than 5.
In the invention, the centrifugal rotating speed is gradually increased to gradually separate the nano copper powder with different particle sizes, the nano copper powder can be effectively separated when the centrifugal rotating speed is increased to more than 3000rpm, and the particle size range of the separated nano copper powder is narrower when the N is larger and the repetition times are more;
furthermore, the Nth upper layer liquid mainly comprises the first dispersing agent and can be repeatedly used.
And 4, step 4: mixing the 1 st to Nth precipitates with a second dispersing agent respectively, and performing centrifugal separation to obtain 1 st to Nth solids respectively;
a small amount of small-particle copper powder and part of the first dispersing agent are adsorbed in the 1 st to the Nth precipitates, the particle size of the small-particle copper powder is far smaller than the particle size range of the 1 st to the Nth precipitates, the small-particle copper powder and the first dispersing agent can be removed by adopting a method of respectively mixing the second dispersing agent with lower viscosity with the 1 st to the Nth precipitates and then separating again to obtain the nano copper powder with higher purity,
the second dispersant is a low viscosity dispersant, preferably from 1 mPaS (20 ℃) to 10 mPaS (20 ℃), more preferably the low viscosity dispersant from the first dispersant, to reduce the introduction of impurities during the separation process,
wherein the mass ratio of the second dispersing agent to the 1 st to Nth precipitates is (100-300): 1, preferably 200:1, and carrying out stirring ultrasound in the same way during mixing, wherein the stirring ultrasound time is 1-5 minutes, preferably 3 minutes;
the inventor finds that the centrifugation at higher rotating speed is more beneficial to the rapid separation of particles with large particle size difference,
in step 4, the centrifugal separation is performed at a high rotation speed, preferably 3000rpm or more, more preferably 4000rpm, for example 5000 rpm.
In the step 2, the step 3 and the step 4, the centrifugal separation time is 1-5 minutes
Furthermore, the No. 1 solid to the No. N solid contain copper powder, and also contain a small amount of a first dispersing agent and a second dispersing agent, and the copper nanoparticles with different particle sizes can be obtained after drying.
Example 1
Respectively measuring 15mL of absolute ethyl alcohol and 15mL of ethylene glycol by using a measuring cylinder, pouring the absolute ethyl alcohol and the ethylene glycol into a beaker, uniformly stirring to prepare a first dispersing agent, sampling 0.5g of copper powder from a sample by using an electronic balance, mixing the copper powder with the first dispersing agent, and stirring and ultrasonically treating for 3 minutes to obtain a mixed solution;
carrying out centrifugal separation on the mixed solution, wherein the centrifugal rotation speed is 500rpm, and the centrifugal time is 3 minutes, so as to obtain a 1 st precipitate and a 1 st upper layer liquid;
continuously centrifuging the 1 st upper layer liquid at the centrifugal rotation speed of 1000rpm for 3 minutes to obtain a 2 nd precipitate and a 2 nd upper layer liquid, and repeating the step 8 times, wherein the centrifugal rotation speeds are 2000rpm, 2500rpm, 3000rpm, 35000rpm, 4000rpm, 4500rpm and 5000rpm respectively, and the centrifugal time is 3 minutes to obtain 3 rd to 10 th precipitates and 3 rd to 10 th upper layer liquids;
mixing the 1 st sediment to the 10 th sediment with 10ml of ethanol respectively, stirring and ultrasonically treating for 3 minutes, and then centrifuging at the centrifugal speed of 5000rpm respectively to obtain 1 st solid to 10 th solid respectively;
and drying the obtained 1 st solid to 10 th solid to obtain the nano copper powder at the rotating speeds of 500rpm, 1000rpm, 1500rpm, 2000rpm, 2500rpm, 3000rpm, 35000rpm, 4000rpm, 4500rpm and 5000 rpm.
The particle sizes of the copper powder sample and the obtained nano copper powder at different rotating speeds are respectively detected, the detection results are shown in table 1,
TABLE 1
As can be seen from the data in Table 1, the method of the present invention can obtain the copper nanoparticles with different particle sizes at different centrifugal rotation speeds.
The nano copper powder is subjected to energy spectrum detection at the rotating speed of 500rpm, as shown in table 2,
energy spectrum data distribution table of nano copper powder at 2500 r/min
As can be seen from table 2, the copper powder content is higher and less impurities are introduced during the separation process.
The copper powder separated in example 1 was measured by using a fourier infrared spectrometer Nicolet Is50, and as shown in fig. 1, it can be seen that the obtained nano copper powder Is pure and has only a few impurities.
When the copper powder before separation was observed by using a scanning electron microscope CARL ZEISS, as shown in fig. 2, the difference in the particle size distribution of the copper powder before separation was large, and the particle size distribution of the copper powder before separation was very uneven. After the copper powder is separated by the centrifugal method, the copper powder is observed by using a scanning electron microscope, as shown in figures 2 to 5, the particle size distribution of the copper powder is relatively uniform, and the effect of separating the copper powder by the differential centrifugal method is better.
The present invention is described in detail with reference to the above-mentioned embodiments. It should be noted that the above embodiments are only for illustrating the present invention. Numerous alternatives and modifications can be devised by those skilled in the art without departing from the spirit and scope of the invention, which should be construed as within the scope of the invention.
Claims (10)
1. The method for differential separation of the nano copper powder with different particle sizes is characterized by comprising the following steps:
step 1: mixing the nano copper powder to be separated with a first dispersing agent to obtain a mixed solution;
step 2: carrying out centrifugal separation on the mixed solution to obtain a 1 st precipitate and a 1 st upper layer liquid;
and step 3: continuously carrying out centrifugal separation on the 1 st upper layer liquid to obtain a 2 nd precipitate and a 2 nd upper layer liquid, and repeating the step (N-2) times to obtain an Nth precipitate and an Nth upper layer liquid;
and 4, step 4: and respectively mixing the 1 st to Nth precipitates with a second dispersing agent, and performing centrifugal separation to respectively obtain 1 st to Nth solids.
2. The method of claim 1 wherein in step 1, the first dispersant is a mixture of a low viscosity dispersant and a high viscosity dispersant,
wherein the low viscosity dispersant is a dispersant having a viscosity of 1 mPaS (20 ℃) to 10 mPaS (20 ℃), and the high viscosity dispersant is a dispersant having a viscosity of 15 mPaS (20 ℃) to 25 mPaS (20 ℃);
the volume ratio of the low-viscosity dispersant to the high-viscosity dispersant is 1: (0.5-2).
3. The method according to claim 1 or 2, wherein, in step 1,
and stirring and ultrasonically treating the nano copper powder to be separated while mixing the nano copper powder with the first dispersing agent, wherein the stirring and ultrasonically treating time is 0.5-20 minutes, preferably 1.5-10 minutes, and more preferably 2.5-5 minutes.
4. The method according to any one of claims 1 to 3, wherein in step 2, the centrifugation speed of the centrifugation is 100 to 1000rpm, preferably 300 to 700rpm, more preferably 400 to 600 rpm.
5. The method according to one of claims 1 to 4, characterized in that, in step 3,
the number of revolutions of centrifugal separation of the 1 st upper layer liquid is larger than the centrifugal speed in the step 2, and the step is repeated for (N-2) times, and the number of revolutions of each centrifugal separation is larger than the previous centrifugal speed until the centrifugal speed is increased to more than 3000rpm, preferably more than 4000rpm, and more preferably more than 5000 rpm.
6. Process according to one of claims 1 to 5, characterized in that in step 3 N.gtoreq.3 is a positive integer, preferably N.gtoreq.5 is a positive integer.
7. Method according to one of claims 1 to 6, characterized in that, in step 4,
the second dispersant is a dispersant having a viscosity of 1 mPaS (20 ℃) to 10 mPaS (20 ℃), and is preferably the same as the low viscosity dispersant in the first dispersant;
in step 4, the centrifugation is performed at a relatively high rotation speed, preferably 3000rpm or more, more preferably 4000rpm, for example 5000 rpm.
8. The method as claimed in any one of claims 1 to 7, wherein in step 4, the No. 1 solid to the No. N solid are respectively dried to obtain the nano copper powder with different particle sizes.
9. The method according to any one of claims 1 to 8, wherein the time for the centrifugation in step 2, step 3 and step 4 is 1 to 5 minutes.
10. Copper nanopowder obtained according to the process of any one of claims 1 to 9, having a particle size difference of less than 800nm, preferably less than 300nm, more preferably less than 200 nm.
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| DE102005022639A1 (en) * | 2005-05-11 | 2006-11-16 | Technische Universität Clausthal | Extraction of particles ranging from nanoparticles to microparticles from liquefied phase or suspension entails creating second liquefied phase by addition of fluid which is basically not mixable with first phase |
| CN1958167A (en) * | 2006-11-28 | 2007-05-09 | 厦门大学 | Method for separating micro Nano material |
| CN105233968A (en) * | 2015-06-17 | 2016-01-13 | 陶栋梁 | Method for separating nano particles of different particle sizes |
| CN106040589A (en) * | 2016-07-11 | 2016-10-26 | 阜阳师范学院 | Method for separating nanometer aluminum powder with different particle sizes |
| CN106607180A (en) * | 2016-12-30 | 2017-05-03 | 广东工业大学 | Separation method of nanoparticles |
| CN109133129A (en) * | 2018-11-01 | 2019-01-04 | 大连海事大学 | A kind of fractionation method of AlON transparent ceramic powder |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005022639A1 (en) * | 2005-05-11 | 2006-11-16 | Technische Universität Clausthal | Extraction of particles ranging from nanoparticles to microparticles from liquefied phase or suspension entails creating second liquefied phase by addition of fluid which is basically not mixable with first phase |
| CN1958167A (en) * | 2006-11-28 | 2007-05-09 | 厦门大学 | Method for separating micro Nano material |
| CN105233968A (en) * | 2015-06-17 | 2016-01-13 | 陶栋梁 | Method for separating nano particles of different particle sizes |
| CN106040589A (en) * | 2016-07-11 | 2016-10-26 | 阜阳师范学院 | Method for separating nanometer aluminum powder with different particle sizes |
| CN106607180A (en) * | 2016-12-30 | 2017-05-03 | 广东工业大学 | Separation method of nanoparticles |
| CN109133129A (en) * | 2018-11-01 | 2019-01-04 | 大连海事大学 | A kind of fractionation method of AlON transparent ceramic powder |
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Application publication date: 20210119 |