CN117585683A - Method for precisely separating nano-micro powder particles - Google Patents
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- CN117585683A CN117585683A CN202310283057.6A CN202310283057A CN117585683A CN 117585683 A CN117585683 A CN 117585683A CN 202310283057 A CN202310283057 A CN 202310283057A CN 117585683 A CN117585683 A CN 117585683A
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- 239000000843 powder Substances 0.000 title claims abstract description 74
- 239000002245 particle Substances 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 109
- 239000000243 solution Substances 0.000 claims abstract description 64
- 238000004062 sedimentation Methods 0.000 claims abstract description 18
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 13
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims abstract description 11
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- 230000005484 gravity Effects 0.000 claims abstract description 7
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 10
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 3
- 229920002134 Carboxymethyl cellulose Polymers 0.000 abstract description 2
- 235000010643 Leucaena leucocephala Nutrition 0.000 abstract description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 2
- 229910019142 PO4 Inorganic materials 0.000 abstract description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 abstract description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 abstract description 2
- 235000010948 carboxy methyl cellulose Nutrition 0.000 abstract description 2
- 239000008112 carboxymethyl-cellulose Substances 0.000 abstract description 2
- 229920000609 methyl cellulose Polymers 0.000 abstract description 2
- 239000001923 methylcellulose Substances 0.000 abstract description 2
- 235000010981 methylcellulose Nutrition 0.000 abstract description 2
- 239000001814 pectin Substances 0.000 abstract description 2
- 235000010987 pectin Nutrition 0.000 abstract description 2
- 229920001277 pectin Polymers 0.000 abstract description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract description 2
- 239000010452 phosphate Substances 0.000 abstract description 2
- -1 polyoxyethylene Polymers 0.000 abstract description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 abstract description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 abstract description 2
- 229940080313 sodium starch Drugs 0.000 abstract description 2
- 241000220479 Acacia Species 0.000 abstract 1
- 239000011858 nanopowder Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000007865 diluting Methods 0.000 description 4
- 239000003550 marker Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 240000007472 Leucaena leucocephala Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010332 dry classification Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Separation Of Solids By Using Liquids Or Pneumatic Power (AREA)
Abstract
The invention provides a method for precisely separating nano-micro powder particles, which comprises the following steps: weighing one of carboxymethyl cellulose, sodium carboxymethyl cellulose, polyvinyl alcohol, methyl cellulose, sodium starch phosphate, polyoxyethylene, acacia or pectin, and preparing into viscosity separation solution with viscosity ranging from 0.01 Pa.s to 1000 Pa.s; transferring the viscosity separation solution to a separation vessel to form a viscosity gradient separation system; forming a viscosity gradient mixed solution in a viscosity gradient separation system of the powder solution to be separated; the invention adopts gravity sedimentation and centrifugal separation to combine the viscosity gradient solution to carry out multistage powder on the powder solution to be separated, the separation precision is as high as 50-100nm, and compared with the traditional centrifugal or sedimentation separation mode, the invention has higher separation efficiency, simultaneously reduces the separation energy consumption and separation cost, and widens the fine preparation and application scene of the powder material.
Description
Technical Field
The invention relates to the technical field of powder engineering, in particular to a method for precisely separating nano-micro powder particles.
Background
The powder material is a base material of a plurality of materials, the preparation and separation of the powder material are one of the most critical technologies for industrial development, the traditional powder classification is carried out after the powder material is powder, the classified powder is applied to different fields according to parameters such as particle size and the like, in the powder classification field, a wet process and a dry process are usually adopted, the wet process usually adopts gravity sedimentation or centrifugation, and the separation precision is high and is usually applied to the classification of some special powder materials, but the post-processing process is complex, waste water and the like are easy to generate, the large-scale application of the special powder materials is limited, the dry classification usually adopts air as a carrier, the process is simple, the cost is low, the classification precision is low, and the obtained particles are wide in distribution;
a centrifuge-assisted small-size nanomaterial separation method of the prior art disclosed under publication No. CN114682347a, comprising: obtaining nano powder by using a planetary ball mill method; obtaining centrifugal parameters through theoretical calculation; starting a stirring motor according to the centrifugal parameters to drive a stirring paddle to rotate, and setting the rotating speed of the stirring motor to be a fixed value; injecting the nano powder into water rotating at a high speed; then under the action of centrifugal force, the nano powder is gradually precipitated and collected by a first collecting bottle below the centrifugal container, and when the separation time is reached, the nano powder is collected by a second collecting bottle; the nano powder aqueous solution in the second collecting bottle is placed in a drying box, and after the nano powder aqueous solution is completely dried, the small-particle-size rice powder is obtained.
The above-mentioned powder is separated by adopting centrifugal separation mode, but the above-mentioned centrifugal auxiliary small-size nano material separation method still has obvious defect in the course of use: the device adopts a centrifugal mode to separate only nano powder, large granular substances after separation are subjected to gravity sedimentation, and lighter small granules float on the upper layer of the liquid level, and although the layering separation of large and small granules is realized to a certain extent, the separation precision is lower, and simultaneously, the particles with the micrometer size are difficult to separate, if the powder separation with higher precision is required, the centrifugal parameters are regulated to perform secondary or even more times of re-separation operation on the separated solution, the separation process is complicated, the energy consumption is higher, and the large-scale commercial application is difficult to perform.
Disclosure of Invention
The present invention is directed to a method for precisely separating nano-micro powder particles, which solves the above-mentioned problems in the prior art.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a method for precisely separating nano-micro powder particles, comprising the steps of:
step one: weighing sodium carboxymethylcellulose, and uniformly mixing the sodium carboxymethylcellulose with water or ethanol at room temperature to prepare a plurality of groups of viscosity separation solutions with the viscosity range of 0.01-1000 Pa.s;
step two: sequentially transferring a plurality of groups of viscosity separation solutions into the same separation container from bottom to top according to the sequence from the high viscosity to the low viscosity to form a viscosity gradient separation system;
step three: slowly adding the powder solution to be separated which is uniformly dispersed by ultrasonic into a viscosity gradient separation system, standing, gravity settling or centrifugal separation operation of a centrifugal machine is carried out on a separation container, and the powder solution to be separated and the viscosity gradient separation system are subjected to viscosity gradient separation in the separation container to form a viscosity gradient mixed solution;
step four: and sequentially extracting a plurality of groups of viscosity gradient mixed solutions from top to bottom, and washing after dilution, sedimentation or drying to obtain uniform powder particles.
Preferably, the viscosity values of several sets of said viscosity separation solutions differ by a factor of not less than 2.
Preferably, the viscosity separation solutions of the groups are designed into 3-6 gradient grades according to the separation precision and the separation efficiency.
Preferably, the viscosity separation solution is subjected to viscosity measurement by a rotational viscometer.
Preferably, a plurality of groups of viscosity separation solutions are added close to the liquid level of the upper layer in the process of adding the viscosity separation solutions into the separation container, so that liquid level disturbance among the viscosity separation solutions of each component is avoided, and normal layering of the viscosity gradient separation system is ensured.
Preferably, the uppermost layer of the viscosity gradient separation system has a greater volume of viscosity separation solution than the remaining layers.
Preferably, the powder solution to be separated is slowly added near the upper liquid level of the viscosity gradient separation system, so that disturbance to each layered liquid level of the viscosity gradient separation system is prevented.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts gravity sedimentation and centrifugal separation combined with viscosity gradient solution to carry out multistage powder on the powder solution to be separated, has been successfully applied to separation of spherical silicon dioxide powder materials, has high separation precision of 50-100nm, has higher separation efficiency compared with the traditional centrifugal or sedimentation separation mode, obtains multistage particle size products through one-step separation, reduces separation energy consumption and separation cost, and widens the fine preparation and application scenes of the powder materials.
Drawings
FIG. 1 is a graph showing a particle size distribution in a state where a powder solution to be separated is uniformly mixed;
FIG. 2 is a distribution diagram of particle size distribution of uniform powder particles according to the first embodiment;
FIG. 3 is a distribution diagram of the particle size of uniform powder particles according to the second embodiment;
FIG. 4 is a distribution diagram of the particle size of uniform powder particles according to the third embodiment;
fig. 5 is a distribution diagram of the particle size of the uniform powder particles of the control group.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples:
referring to fig. 1-5, the present invention provides a technical solution:
the sodium carboxymethyl cellulose used in the examples is prepared by using the characteristic that the sodium carboxymethyl cellulose forms colloid in the solution, and one of carboxymethyl cellulose, polyvinyl alcohol, methyl cellulose, sodium starch phosphate, polyoxyethylene, acacia and pectin can be selected as required to prepare viscosity separation solution, and spherical silica is selected as the powder to be separated in the examples.
Embodiment one:
1) Weighing sodium carboxymethylcellulose by adopting a rotary viscometer at the room temperature of 25-35 ℃ to prepare 5 groups of viscosity separation solutions with the viscosity of 0.1, 1, 5, 10 and 20 Pa.s into 6mL each;
2) Sucking the viscosity gradient solution, sequentially adding the viscosity gradient solution into a 50mL centrifuge tube from bottom to top according to the sequence of the viscosity from top to bottom to form a viscosity gradient separation system, and marking at the corresponding layering position by a marker;
3) Slowly adding 10mL of the powder solution to be separated, which is well dispersed by ultrasonic, into a viscosity gradient separation system at a position close to the upper liquid level, and centrifugally separating for 10 minutes by 8000r/min to form a viscosity gradient mixed solution;
4) And sucking the solution in the system according to the marked position after centrifugation, diluting, settling or washing after drying to obtain high-uniformity powder particles, and measuring the particle size distribution by a powder particle size analyzer.
Embodiment two:
1) Weighing sodium carboxymethylcellulose by adopting a rotary viscometer at the room temperature of 25-35 ℃ to prepare 4 groups of viscosity separation solutions with the viscosity of 10, 50, 200 and 1000 Pa.s, wherein 50mL each;
2) Absorbing the viscosity gradient solution, sequentially adding the viscosity gradient solution into 500mL centrifuge tubes from bottom to top according to the sequence of the viscosity from top to bottom to form a viscosity gradient separation system, and marking at the corresponding layering position by a marker;
3) Slowly adding 100mL of the powder solution to be separated, which is well dispersed by ultrasonic, into a viscosity gradient separation system at a position close to the upper liquid level, and forming a viscosity gradient mixed solution by adopting a gravity sedimentation mode of standing for 24 hours;
4) And (3) sucking the solution in the system according to the marked position after centrifugation, diluting, settling or drying, washing to obtain high-uniformity powder particles respectively, and measuring the particle size distribution by a powder particle size analyzer.
Embodiment III:
1) Weighing sodium carboxymethylcellulose by adopting a rotary viscometer at the room temperature of 25-35 ℃ to prepare 4 groups of viscosity separation solutions with the viscosity of 0.01, 0.1, 1 and 10 Pa.s into 6mL each;
2) Sucking the viscosity gradient solution, sequentially adding the viscosity gradient solution into a 50mL centrifuge tube from bottom to top according to the sequence of the viscosity from top to bottom to form a viscosity gradient separation system, and marking at the corresponding layering position by a marker;
3) Slowly adding 10mL of the powder solution to be separated, which is well dispersed by ultrasonic, into a viscosity gradient separation system at a position close to the upper liquid level, and centrifugally separating for 15 minutes by 10000r/min to form a viscosity gradient mixed solution;
4) And sucking the solution in the system according to the marked position after centrifugation, diluting, settling or washing after drying to obtain high-uniformity powder particles, and measuring the particle size distribution by a powder particle size analyzer.
Control group:
slowly adding 10mL of the ultrasonic-dispersed powder solution to be separated into a 30mL water system, marking at a corresponding position by a marker pen, centrifugally separating for 10 minutes by 8000r/min to form a viscosity gradient mixed solution, centrifuging, sucking the solution in the system according to the marked position, diluting, settling or drying, washing to obtain high-uniformity powder particles, and measuring the particle size distribution by a powder particle size analyzer.
Conclusion of test analysis: the uniform powder formed by the three groups of examples and the control group is measured by a powder particle size analyzer to obtain the powder particles with the particle size ranging from 150nm to 700nm, wherein the powder particles with the particle size ranging from 150nm to 350nm in the figure 2 of the first corresponding example are concentrated near 350nm, the powder particles with the particle size ranging from 200nm to 500nm can be concentrated and separated by analyzing the colloidal viscosity separation solution with the particle size ranging from 0.1 Pa.s to 20 Pa.s, the powder particles with the particle size ranging from 200nm to 1000nm in the figure 3 of the second corresponding example are concentrated near 500nm, and the powder particles with the particle size ranging from 400 Pa.s to 800nm can be concentrated and separated by analyzing the colloidal viscosity separation solution with the particle size ranging from 10 Pa.s to 1000 Pa.s; in the figure 4 of the specification corresponding to the third embodiment, the particle size of the separated powder is between 80nm and 200nm, and is concentrated near 130nm, and the analysis shows that the colloidal viscosity separation solution with the particle size of 0.01 to 10 Pa.s can concentrate and separate the powder particles with the particle size near 100 to 150nm, and the separation precision reaches 50nm; in order to verify whether the three groups of embodiments play a role in separation, the invention also introduces a control group, the particle size of the powder to be separated corresponding to the control group is compared with that of the first embodiment, the particle size of the powder to be separated is widely distributed in each interval of 50-3000nm, the centrifugal separation mode is not provided with a remarkable separation effect, the comparison of the control group with the first embodiment shows that the colloidal solution formed by sodium carboxymethylcellulose has a significant separation effect on the basis of the viscosity gradient of the solution to be separated, the separation precision reaches 50-100nm, the colloidal viscosity gradient separation mode introduced by the three groups of embodiments is compared with the conventional centrifugal sedimentation separation mode, the invention also introduces a control group, the particle size of the powder to be separated corresponding to the control group is widely distributed in each interval of 50-3000nm, the colloidal solution to be separated does not have a remarkable separation effect, the colloidal solution formed by sodium carboxymethylcellulose is stressed on the separation mode of the viscosity system, the colloidal solution is better than the conventional centrifugal force viscosity gradient of the control group, the colloidal solution is better than the conventional viscosity gradient viscosity of the contrast group, the dynamic viscosity of the colloidal solution is better than the conventional viscosity gradient sedimentation system, or the dynamic sedimentation system is better than the dynamic sedimentation system, the dynamic sedimentation system is more difficult to realize the effect of the dynamic sedimentation system, and the particles are more difficult to realize by combining the principle of the dynamic sedimentation system and the dynamic sedimentation system has a small dynamic sedimentation effect, the large particles settle in the bottom and the small particles float on the upper part of the water body, the particle size of the powder trapped in the middle layering is less, the separation particle size is low, and the viscosity value of the colloidal viscosity separation mode adopted by the application can be properly adjusted according to the particle size distribution condition of the powder to be separated, and the viscosity gradient difference value can be configured according to the separation precision, so that the separation precision can be effectively ensured.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for precisely separating nano-micro powder particles, comprising the steps of:
step one: weighing sodium carboxymethylcellulose, and uniformly mixing the sodium carboxymethylcellulose with water at room temperature to prepare a plurality of groups of viscosity separation solutions with the viscosity range of 0.01-1000 Pa.s;
step two: sequentially transferring a plurality of groups of viscosity separation solutions into the same separation container from bottom to top according to the sequence from the high viscosity to the low viscosity to form a viscosity gradient separation system;
step three: slowly adding the powder solution to be separated which is uniformly dispersed by ultrasonic into a viscosity gradient separation system, standing, gravity settling or centrifugal separation operation of a centrifugal machine is carried out on a separation container, and the powder solution to be separated and the viscosity gradient separation system are subjected to viscosity gradient separation in the separation container to form a viscosity gradient mixed solution;
step four: and sequentially extracting a plurality of groups of viscosity gradient mixed solutions from top to bottom, and washing after dilution, sedimentation or drying to obtain uniform powder particles.
2. A method for precisely separating nano-micro powder particles according to claim 1, wherein: the viscosity values of several groups of said viscosity separation solutions differ by a factor of not less than 2.
3. A method for precisely separating nano-micro powder particles according to claim 2, wherein: the viscosity separation solutions of a plurality of groups are designed into 3-6 gradient grades according to the separation precision and the separation efficiency.
4. A method for precisely separating nano-micro powder particles according to claim 1 or 3, wherein: the viscosity of the viscosity separation solution was measured by a rotary viscometer.
5. A method for precisely separating nano-micro powder particles according to claim 1 or 3, wherein: the viscosity separation solutions of a plurality of groups are added close to the liquid level of the upper layer in the process of adding the viscosity separation solutions into the separation container, so that the liquid level disturbance among the viscosity separation solutions of all the components is avoided, and the normal layering of the viscosity gradient separation system is ensured.
6. A method for precisely separating nano-micro powder particles according to claim 3, wherein: the uppermost layer of the viscosity gradient separation system has a greater volume of viscosity separation solution than the remaining layers.
7. A method for precisely separating nano-micro powder particles according to claim 1 or 6, wherein: the powder solution to be separated is slowly added near the upper liquid level of the viscosity gradient separation system, so that disturbance to each layered liquid level of the viscosity gradient separation system is prevented.
8. A method for precisely separating nano-micro powder particles according to claim 7, wherein: when the centrifugal separation operation is carried out by adopting a centrifugal machine, the separation rotating speed of the centrifugal machine is 1000-10000r/min, and the centrifugal separation time is 10-15min.
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