CN112238001A - Method for differential separation of nano aluminum powder with different particle sizes - Google Patents
Method for differential separation of nano aluminum powder with different particle sizes Download PDFInfo
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Abstract
The invention provides a method for differential separation of nano aluminum powder with different particle sizes, which comprises the following steps: preparing a dispersant 1 and a dispersant 2; fully mixing aluminum powder to be separated with a dispersing agent 1 to obtain a mixed solution, centrifuging the mixed solution at different rotating speeds to obtain multiple groups of primary products, fully mixing the obtained multiple groups of primary products with a dispersing agent 2 respectively, then carrying out secondary separation to obtain multiple groups of secondary products, and drying the secondary products to obtain multiple groups of nano aluminum powder with different particle sizes. The method has the advantages of simplicity, convenience, economy, good separation effect, narrower distribution range of the particle size after separation, less aluminum powder loss in the separation process, environmental protection and the like.
Description
Technical Field
The invention relates to a method for separating aluminum powder with different nano-particle sizes, in particular to a method for separating the aluminum powder with different nano-particle sizes by adopting a differential speed.
Background
Due to the rapid development of the aluminum industry, aluminum products are used in a large amount in our national lives, but problems are brought about, and the rapid increase of the amount of aluminum waste becomes a problem which seriously affects the environmental protection, destroys the ecological environment and affects the national survival. Bauxite energy and resource have been the two largest stumbling stones that have blocked the development of the aluminum industry in china for a long time. Bauxite, electrolytic aluminum, alumina and the like have a particularly high degree of dependence on energy and resources. Therefore, a circular economy system taking the recycled aluminum as a core is built, the circular use of aluminum resources is realized, the dependence on mineral resources and resources can be reduced, the negative influence on the ecological environment is reduced, the aluminum industry in China is free from the energy and resource constraints, and the sustainable development is realized.
The aluminum powder is widely applied to the fields of agriculture, catalysts, solid rocket propellants, gunpowder, metal flashing coatings, photovoltaic solar cell slurry and the like, and plays an important role in the industries of aerospace, national defense, metallurgy, coatings, buildings and the like. The aluminum powder with different particle size ranges has different action fields, and the separation of the aluminum powder with different particle size ranges is the basis and the premise for the application of the aluminum powder in different fields.
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.
The existing centrifugal separation method solves part of problems, and has the advantages of simple operation, no need of filtration, less aluminum powder loss in the separation process, environmental protection and saving, recyclable intermediate auxiliary materials and the like, but the separation effect still has a certain difference from the particle size separation method commonly used in industry, and the purity of the aluminum powder after separation still needs to be improved.
Therefore, there is an urgent need for further improvement of the method for centrifugal separation of aluminum powder to improve the separation effect and obtain aluminum powder with a narrower particle size distribution effect and higher purity.
Disclosure of Invention
In order to overcome the problems, the inventor of the invention carries out intensive research and designs a method for differentially separating nano aluminum powder with different particle sizes, the method firstly needs to be provided with a dispersing agent, the aluminum powder to be separated is fully mixed with the dispersing agent 1, different primary products are obtained by continuously improving centrifugal force, then the primary products are fully mixed with the dispersing agent 2, the secondary products are obtained by purification in a high-speed centrifugal mode, and the aluminum powder with narrower particle size distribution and higher purity is obtained by heating treatment.
Specifically, the invention aims to provide a method for differential separation of nano aluminum powder with different particle sizes, which comprises the following steps:
step 1: preparing a dispersing agent 1;
step 2: mixing the aluminum powder to be separated with the dispersant 1 to obtain a mixed solution, and centrifuging the mixed solution at different rotating speeds to obtain a plurality of groups of primary products;
and step 3: mixing the obtained multiple groups of primary products with the dispersing agent 2 respectively, and then carrying out secondary separation to obtain multiple groups of secondary products;
and 4, step 4: and drying the secondary product to obtain a plurality of groups of nano aluminum powder.
In the step 1, the dispersant 1 is formed by mixing a low-viscosity dispersant and a high-viscosity dispersant according to a certain proportion.
In step 2, centrifuging at different rotating speeds, and performing centrifugation in multiple groups;
a first set of centrifugation: centrifuging the mixed solution at an initial rotating speed for a certain time to obtain a first group of precipitates and liquid, wherein the precipitates are primary products,
second group centrifugation: increasing the rotation speed, centrifuging the liquid obtained in the first group, obtaining a second group of primary products and liquid after a certain time,
repeating the above process, increasing rotation speed each time until reaching the highest rotation speed to obtain multiple groups of primary products,
the initial rotating speed and the highest rotating speed are respectively 300rpm and 6000rpm, preferably 500rpm and 5000rpm, and the increasing rotating speed is 300-700 rpm, preferably 500rpm, increased each time;
the certain time is the time for fully separating the aluminum powder, the aluminum powder cannot be completely separated if the time is too short, the content of the aluminum powder with smaller particle size in the precipitate is increased if the time is too long, and the concentration ratio is reduced, and according to multiple tests of an inventor, the separation time can reach a good effect within 3-10 minutes, and the most preferable time is5 minutes.
Further, in the step 2 and the step 3, stirring, ultrasonic dispersion and/or temperature control are carried out while mixing;
and 3, performing high-speed centrifugation as the secondary separation in the step 3, wherein the rotation speed of the secondary separation is 4000-6000 rpm, preferably 5000rpm, and the secondary product is a precipitate after the secondary centrifugation.
And 4, drying the secondary product in a drying device, preferably drying at a low temperature of 50-100 ℃, preferably 60-80 ℃, for 40-60 minutes.
In a preferred embodiment, low-oxidation-degree aluminum powder is selected for separation, the primary product obtained in the step 2 is quickly and fully mixed with a dispersing agent, and the secondary product obtained in the step 3 is quickly placed in a vacuum drying device for drying treatment in the step 4, so that a plurality of groups of low-oxidation-degree nano aluminum powder with different particle size ranges can be obtained.
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 average particle size of the separated aluminum powder is closer to the median of the particle size range;
(3) the particle size distribution range after separation is narrower;
(4) the aluminum powder loss is less in the separation process;
(5) the environment is protected, and the dispersing agent can be recycled in the process.
Drawings
FIG. 1 shows the IR spectra of the aluminum powders obtained by the separation at different rotation speeds in example 1;
FIG. 2 shows a scanning electron microscope image of aluminum powder before non-separation in example 1;
FIG. 3 shows an electron microscope image of the aluminum powder separated at 1000rpm in example 1;
FIG. 4 shows an electron microscope of the aluminum powder separated at 5000rpm in example 1.
Detailed Description
The invention is explained in more detail below with reference to the figures and 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 aluminum powder with different particle sizes by a differential separation method, which comprises the following steps:
step 1: dispersant 1 was prepared.
Step 2: mixing the aluminum powder to be separated with the dispersant 1 to obtain a mixed solution, and centrifuging the mixed solution at different rotating speeds to obtain a plurality of groups of primary products;
and step 3: mixing the obtained multiple groups of primary products with the dispersing agent 2 respectively, and then carrying out secondary separation to obtain multiple groups of secondary products;
and 4, step 4: and drying the secondary product to obtain a plurality of groups of nano aluminum powder.
The inventor finds that the dispersants with different viscosities directly influence the centrifugal separation effect of the aluminum powder, the low viscosity can cause the particle size range of the separated aluminum powder to be too large, the high viscosity can cause the aluminum powder to be incapable of being separated and incapable of being obtained, and when the viscosity is moderate, the separation effect of the aluminum powder with different particle sizes is good.
In the step 1, the dispersant 1 is formed by mixing a low-viscosity dispersant and a high-viscosity dispersant according to a certain proportion;
further, the low viscosity dispersant is a dispersant having a viscosity of 0.5 to 10 mPaS (20 ℃), preferably 0.5 to 5 mPaS (20 ℃), more preferably 1 to 2 mPaS (20 ℃), such as absolute ethanol,
the high viscosity dispersant is a dispersant having a viscosity of 10 to 30 mPaS (20 ℃), preferably 15 to 25 mPaS (20 ℃), more preferably 18 to 22 mPaS (20 ℃), such as ethylene glycol,
the certain proportion refers to that the volume ratio of the low-viscosity dispersant to the high-viscosity dispersant is 1: (1-4), preferably in a volume ratio of 1: (1-2), more preferably the volume ratio is 1: 1.
Step 2: and mixing the aluminum powder to be separated with the dispersant 1 to obtain a mixed solution, and centrifuging the mixed solution at different rotating speeds to obtain multiple groups of primary products.
The inventor finds that different centrifugal forces are generated at different rotating speeds, the centrifugal force is increased by continuously increasing the rotating speed, the centrifugal force required by particles with large mass is small, the particles can sink at low rotating speed, and the centrifugal force required by the particles with small mass is large, so the particles can sink at high rotating speed. Thus, the particles with different particle sizes can be well separated at different rotating speeds.
The centrifuge inevitably passes through the low rotating speed in the process of reaching the high rotating speed state from the stop state, the aluminum powder with large particle size is partially precipitated at the low rotating speed, and if the small-particle-size aluminum powder is obtained after separation at the high rotating speed, a small amount of large-particle-size aluminum powder is contained in the obtained aluminum powder. Based on the above, the invention starts to separate from low rotating speed, and relatively narrower particle size range of the aluminum powder is obtained.
According to the invention, the centrifugation is carried out in groups at different rotation speeds, the centrifugation rotation speed is gradually changed from low rotation speed to high rotation speed,
a first set of centrifugation: centrifuging the mixed solution at an initial rotating speed for a certain time to obtain a first group of precipitates and liquid, wherein the precipitates are primary products,
second group centrifugation: increasing the rotation speed, centrifuging the liquid obtained in the first group, obtaining a second group of primary products and liquid after a certain time,
repeating the above process, increasing rotation speed each time until reaching maximum rotation speed to obtain multiple groups of primary products and a separation solution,
further, the separation liquid can be recycled as the dispersant 1.
Further, the initial rotating speed and the highest rotating speed are respectively 300rpm and 6000rpm, preferably 500rpm and 5000rpm, and the increasing rotating speed is 300-700 rpm, preferably 500rpm, increased each time;
in step 2 and step 3, stirring, ultrasonic dispersion and/or temperature control are performed while mixing.
The inventors found that the mixing process of the aluminum powder and the dispersant has a great influence on the centrifugal effect, and in order to ensure the separation stability, the inventors studied the mixing process and carried out stirring, ultrasonic dispersion and/or temperature control while mixing.
When the aluminum powder is mixed with the dispersing agent, particularly when a large amount of aluminum powder is added into the dispersing agent at the same time, the aluminum powder can be agglomerated to generate adverse effect on separation, and the aluminum powder can be initially uniformly distributed in the dispersing agent by clockwise and anticlockwise alternate stirring for 1-10 minutes, preferably 3-7 minutes, and more preferably 5 minutes.
Because the particle size of the aluminum powder is smaller, part of the aluminum powder can be agglomerated after stirring, and an ultrasonic dispersion mode can be adopted, so that the aluminum powder particles are dispersed more uniformly, the ultrasonic frequency has a direct relation with the particle size of the aluminum powder, the frequency is lower than 5kHz, the nano aluminum powder cannot be dispersed, the frequency is too high, and the requirement on equipment is higher although the dispersion effect can be achieved.
The ultrasonic frequency of the invention is 5-60 kHz, preferably 10-50 kHz, more preferably 20-30 kHz, and the ultrasonic time is 10-120 minutes, preferably 20-60 minutes, more preferably 30 minutes.
The temperature of the mixed liquid can also influence the separation effect during centrifugation, when the temperature is high, a large amount of precipitates are generated, the particle size range of the aluminum powder is widened, when the temperature is low, the precipitates are generated less, and a large amount of aluminum powder is still dispersed in the mixed liquid, so that incomplete separation is caused.
In the invention, the temperature during centrifugation is 17-25 ℃, and 20 ℃ is preferred.
The centrifugal time is too short, the aluminum powder is not completely separated, and the time is too long, so that the temperature in the centrifuge is increased, and the centrifugal effect is deviated.
And (3) obtaining a plurality of groups of primary products in the step (2), wherein the primary products inevitably contain dispersant components and a small amount of small-particle-size aluminum powder, and adopting a secondary centrifugation method, a low-viscosity dispersant and a high-rotation-speed centrifugation method to improve the purity of the aluminum powder and reduce the distribution range of the separated aluminum powder.
And step 3: fully mixing the obtained multiple groups of primary products with the dispersing agent 2 respectively, and then carrying out secondary separation to obtain multiple groups of secondary products;
in the step 3, the secondary separation is separation at a high rotating speed, the rotating speed is 4000-6000 rpm, preferably 5000rpm, and the secondary product is a precipitate after secondary centrifugation.
The dispersant 2 is a low-viscosity dispersant or a mixture of several low-viscosity dispersants, the low viscosity is favorable for removing tiny particles brought by primary centrifugal separation, so that the particle size range of the aluminum powder is narrower, and the dispersant with the viscosity of 0.5-10 mPa & S (20 ℃) is selected in the invention.
Further, in order to improve the purity of the separated aluminum powder and minimize the introduction of impurities during the separation process, the dispersant 2 is preferably the same as the low viscosity dispersant in the dispersant 1, such as absolute ethanol.
And 4, step 4: and (3) drying the secondary product, namely drying the secondary product in a drying device, wherein the drying device is closed, the dispersing agent 2 volatilizes to a limited space in the drying process, and the high temperature can cause an explosion phenomenon, so that the drying at a low temperature is preferred to obtain a plurality of groups of pure nano aluminum powder with different particle size ranges.
The low temperature is 50-100 ℃, preferably 60-80 ℃, and the drying time is 40-60 minutes.
Examples
Example 1
Taking 15mL of absolute ethyl alcohol and 15mL of ethylene glycol respectively to prepare a dispersing agent 1, taking 15mL of absolute ethyl alcohol as a dispersing agent 2, and preparing a multi-component dispersing agent 2.
0.5478g of aluminum powder is weighed on an electronic balance and placed in the dispersing agent 1, the mixture is placed in an ultrasonic machine for ultrasonic treatment for 30 minutes after being alternately stirred clockwise and anticlockwise for 5 minutes, and the mixture is centrifuged for 5 minutes at the rotating speed of 500r/min after the temperature of a beaker is reduced to 20 ℃, so that the group 1 primary product and the liquid 1 are obtained.
And stirring the liquid 1 for 5 minutes, carrying out ultrasonic treatment at 25kHz for 30 minutes, cooling to 20 ℃, centrifuging for 5 minutes at 1000r/min to obtain liquid 2 and group 2 primary products, repeating the steps, and sequentially increasing the rotating speed to obtain group 3-10 primary products and liquid 3-10 at 1500r/min-5000 r/min.
And respectively mixing the obtained 1 st to 10 th groups of primary products with a dispersing agent 2, stirring for 5 minutes, carrying out 25kHz ultrasonic treatment for 30 minutes, cooling to 20 ℃, and then centrifuging at the speed of 5000r/min to obtain 1 st to 10 th groups of secondary products.
And (3) respectively placing the 1 st to 10 th groups of secondary products in an oven for drying for 60 minutes at the temperature of 60 ℃ to obtain 1 st to 10 th groups of nano aluminum powder, and referring to the following experimental examples 1-4 for characterization and test of the nano aluminum powder.
Examples of the experiments
Experimental example 1
Quality change of aluminum powder before and after separation in example 1
The particle sizes and the mass conditions of the 1 st to 10 th groups of nano aluminum powder obtained in the example 1 and the aluminum powder before separation at different rotating speeds are shown in table 1:
TABLE 1 aluminum powder particle size and Mass distribution Table at different rotation speeds
As can be seen from Table 1, the difference between the total mass of the aluminum powder before and after separation is not large, and the loss rate of the aluminum powder is low during the separation process.
Experimental example 2
Particle size distribution of 1 st to 10 th groups of aluminum nanopowder obtained in example 1
The group 1 nano aluminum powder obtained in example 1 was measured by using a laser particle size analyzer 90Plus, and the results are as follows: the particle size distribution range of the 1 st group of nano aluminum powder is 1190.5nm-1591.0nm, and the average particle size is 1390.8 nm;
the group 2 of nano aluminum powder has the particle size distribution range of 1487.9nm-1507.7nm and the average particle size of 1496.6 nm;
the 3 rd group of nano aluminum powder has the particle size distribution range of 1070.1-1331.0nm and the average particle size of 1200.55 nm;
the 4 th group of nano aluminum powder has the particle size distribution range of 1024.3-1035.7nm and the average particle size of 1030.0 nm;
the 5 th group of nano aluminum powder has the particle size distribution range of 921.0-934.5nm and the average particle size of 927.5 nm;
the 6 th group of nano aluminum powder has the particle size distribution range of 858.3-871.2nm and the average particle size of 864.8 nm;
the 7 th group of nano aluminum powder has the particle size distribution range of 716.8-742.0nm and the average particle size of 730.0 nm;
the 8 th group of nano aluminum powder has the particle size distribution range of 393.1-610.2nm and the average particle size of 501.7 nm;
the 9 th group of nano aluminum powder has the particle size distribution range of 249.2-330.2nm and the average particle size of 289.7 nm;
the 10 th group of nano aluminum powder has the particle size distribution range of 193.6-237.8nm and the average particle size of 215.7 nm;
according to the detection result, 193.6-1591.0 nm aluminum powder can be separated according to the particle size range by the method, the particle size range of the separated aluminum powder is narrow, and the average particle size is close to the median of the particle size range.
Experimental example 3
Purity of aluminum powder separated at different rotating speeds in examples
The aluminum powder separated in different embodiments Is measured by using a Fourier infrared spectrometer Nicolet Is50, and as shown in FIG. 2, it can be known that the alcohol Is completely volatilized and the aluminum powder Is relatively pure in the drying process of the prepared aluminum powder in a drying box.
Experimental example 4
Scanning electron microscope for aluminum powder particle sizes separated at different rotating speeds in embodiment
When the aluminum powder before and after separation was observed using a scanning electron microscope CARL ZEISS (as shown in fig. 3), the particle size distribution of the aluminum powder before separation was very different, and the particle size distribution of the aluminum powder before separation was very uneven. After the aluminum powder is separated by the centrifugal method, the particle size distribution of the aluminum powder is relatively uniform by observing an electron microscope picture (as shown in figure 4), which shows that the differential centrifugal method has better effect on separating the aluminum powder.
The present invention has been described in detail with reference to the specific embodiments and experimental examples, but the description should not be construed as limiting the present invention. Those skilled in the art will appreciate that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present invention and its embodiments without departing from the spirit and scope of the present invention, which fall within the scope of the present invention. The scope of the invention is defined by the appended claims.
Claims (10)
1. A method for differential separation of nano aluminum powder with different particle sizes is characterized by comprising the following steps:
step 1, preparing a dispersant 1;
step 2: mixing the aluminum powder to be separated with the dispersant 1 to obtain a mixed solution, and centrifuging the mixed solution at different rotating speeds to obtain a plurality of groups of primary products;
and step 3: mixing the obtained multiple groups of primary products with the dispersing agent 2 respectively, and then carrying out secondary separation to obtain multiple groups of secondary products;
and 4, step 4: and drying the secondary product to obtain a plurality of groups of nano aluminum powder.
2. The method of claim 1 wherein in step 1 dispersant 1 is a low viscosity dispersant and a high viscosity dispersant mixed in proportions.
3. The method according to claim 2, wherein, in step 1,
the low viscosity dispersant is a dispersant having a viscosity of 0.5 to 10 mPaS (20 ℃), preferably 0.5 to 5 mPaS (20 ℃), more preferably 1 to 2 mPaS (20 ℃), such as absolute ethanol,
the high viscosity dispersant is a dispersant having a viscosity of 10 to 30 mPaS (20 ℃), preferably 15 to 25 mPaS (20 ℃), more preferably 18 to 22 mPaS (20 ℃), such as ethylene glycol,
the volume ratio of the low-viscosity dispersant to the high-viscosity dispersant is 1: (1-4), preferably in a volume ratio of 1: (1-2), more preferably the volume ratio is 1: 1.
4. A method according to claim 1, characterized in that in step 2, the centrifugation at different speeds is carried out in groups, the centrifugation speed being stepwise from a low speed to a high speed,
a first set of centrifugation: centrifuging the mixed solution at an initial rotating speed for a certain time to obtain a first group of precipitates and liquid, wherein the precipitates are primary products,
second group centrifugation: increasing the rotation speed, centrifuging the liquid obtained in the first group, obtaining a second group of primary products and liquid after a certain time,
repeating the above process, increasing the rotation speed each time until reaching the highest rotation speed, and obtaining multiple groups of primary products.
5. The method according to claim 4, wherein, in step 2,
the initial rotating speed and the highest rotating speed are respectively 300rpm and 6000rpm, preferably 500rpm and 5000rpm, and the increasing rotating speed is 300-700 rpm, preferably 500rpm, increased each time;
the certain time is 3-10 minutes, preferably 5 minutes.
6. The method of claim 1, wherein the mixing is performed simultaneously with stirring, ultrasonic dispersion and/or temperature control in steps 2 and 3.
7. The method of claim 6, wherein:
stirring for 1-10 minutes, preferably 3-7 minutes, more preferably 5 minutes, by using a stirring device along clockwise and anticlockwise alternately during stirring, wherein the ultrasonic frequency during ultrasonic treatment is 5-60 kHz, preferably 10-50 kHz, more preferably 20-30 kHz, and the certain time is 10-120 minutes, preferably 20-60 minutes, more preferably 30 minutes;
the ultrasonic dispersion is that the mixed solution after stirring and mixing is placed in an ultrasonic device for ultrasonic dispersion;
the temperature is controlled to be 17-25 ℃ and preferably 20 ℃ when the mixed solution after ultrasonic treatment is stirred.
8. The method according to claim 1, wherein, in step 3,
the secondary separation is separation at a high rotating speed of 4000-6000 rpm, preferably 5000rpm, the secondary product is sediment after secondary centrifugation,
the dispersant 2 is a low-viscosity dispersant or a mixture of several low-viscosity dispersants, preferably a low-viscosity dispersant, more preferably a dispersant having a viscosity of 0.5 to 10 mPas (20 ℃), particularly preferably the same as the low-viscosity dispersant in the dispersant 1, and is, for example, absolute ethanol.
9. The method according to claim 1, wherein, in step 4,
and drying the secondary product in a drying device, preferably drying at a low temperature of 50-100 ℃, preferably 60-80 ℃, for 40-60 minutes.
10. Nano-aluminum powder obtained by the process according to one of claims 1 to 9, having a particle size difference of less than 500nm, preferably limited to 250nm, more preferably less than 150 nm.
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