CN113333734A - Method for separating metal nanoparticles and nano-alloy from solution - Google Patents

Method for separating metal nanoparticles and nano-alloy from solution Download PDF

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Publication number
CN113333734A
CN113333734A CN202110482808.8A CN202110482808A CN113333734A CN 113333734 A CN113333734 A CN 113333734A CN 202110482808 A CN202110482808 A CN 202110482808A CN 113333734 A CN113333734 A CN 113333734A
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nano
alloy
solvent
nickel
solution
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黄博
谭喆
刘俞含
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Xian Jiaotong University
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Xian Jiaotong University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • 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

Abstract

The invention relates to a method for separating metal nanoparticles from a solution, in particular to a method for separating metal nanoparticles by adding a first solvent and a second solvent into a metal nanoparticle solution and centrifuging to obtain the metal nanoparticles. The volume ratio of the metal nanoparticle solution to the first solvent to the second solvent is 1: (0.1 to 10)7)：(0.1～107)。

Description

Method for separating metal nanoparticles and nano-alloy from solution
Technical Field
The invention relates to the technical field of nano material separation, in particular to a method for separating metal nano particles from a solution.
Background
Nanometer materials (also called ultrafine particle materials) have structural units with a size ranging from 1nm to 100 nm. The properties of the nano material in the aspects of optics, thermal, electricity, magnetism, mechanics, chemistry and the like are obviously different from those of the non-nano material. Nanomaterials, such as metal nanoparticle materials, have a wide range of applications in the fields of composites, nanocatalysts, nanooptics, and semiconductors.
At present, the common method for preparing metal nano particles is a chemical reduction method, and the chemical reduction method has the advantages of simplicity and rapidness. However, since the metal nanoparticle solution obtained by the chemical reduction method also contains a plurality of reagents participating in the chemical reduction reaction, post-treatment is required to obtain metal nanoparticles. The usual process is repeated high speed centrifugation, however the metal nanoparticles are extremely small in size and have a unique morphology, making the separation efficiency of centrifugation low.
Disclosure of Invention
Based on this, the invention provides a method for separating metal nanoparticles from a solution with high separation efficiency.
A method of separating metal nanoparticles from a solution, comprising:
adding a first solvent and a second solvent into the metal nanoparticle solution, and performing centrifugal separation to obtain metal nanoparticles;
wherein the volume ratio of the metal nanoparticle solution, the first solvent and the second solvent is 1: (0.1 to 10)7)：(0.1～107)。
Preferably, the volume ratio of the metal nanoparticle solution, the first solvent and the second solvent is 1: (0.1-3): (0.1-5).
Preferably, the first solvent and the second solvent are each independently selected from any one of ethyl acetate, acetone, pentane, 1, 2-trichlorotrifluoroethane, cyclopentane, heptane, N-hexane, isooctane, petroleum ether, cyclohexane, N-butyl chloride, toluene, methyl tert-butyl ether, o-xylene, chlorobenzene, o-dichlorobenzene, diethyl ether, dichloromethane, dichloroethane, N-butanol, isopropanol, N-butyl acetate, isobutanol, methyl isoamyl ketone, N-propanol, tetrahydrofuran, chloroform, methyl isobutyl ketone, methyl N-propyl ketone, methyl ethyl ketone, 1, 4-dioxane, methanol, pyridine, 2-methoxyethanol, acetonitrile, propylene carbonate, N-dimethylformamide, dimethylacetamide, N-methylpyrrolidone, and dimethylsulfoxide; wherein the first solvent and the second solvent are different solvents.
Preferably, the metal nanoparticles are monometallic nanoparticles or nanoalloys.
Has the advantages that:
compared with the existing method for separating the metal nanoparticles from the solution, the method adopts a two-solvent system to be added into the metal nanoparticle solution for centrifugal separation. The solvent is less in use variety, repeated centrifugation is not needed in the separation method, the use amount of the solvent is reduced, and the effect of environmental protection is achieved. The separation efficiency achieved by the separation method in the invention is more than 99%, and the yield of the metal nanoparticles is increased.
Drawings
Fig. 1 illustrates a separation process of metal nanoparticles according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the embodiments of the present invention and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
Provided herein is a method for separating metal nanoparticles from a solution, comprising adding a first solvent and a second solvent to a metal nanoparticle solution, and centrifuging to obtain metal nanoparticles; the volume ratio of the metal nanoparticle solution to the first solvent to the second solvent is 1: (0.1 to 10)7)：(0.1～107)。
The concentration of the metal nanoparticles in the metal nanoparticle solution herein may be in the full concentration range. For example, the concentration of the metal nanoparticles may be 0.067mol/L or 0.0265 mol/L.
Herein, the volume ratio of the metal nanoparticle solution, the first solvent, and the second solvent may be 1: (0.1-3): (0.1-5). For example, the volume ratio of the metal nanoparticle solution, the first solvent, and the second solvent may be 1:3:5, or the volume ratio of the metal nanoparticle solution, the first solvent, and the second solvent may be 1:1: 1.
In other embodiments, the metal nanoparticle solution, the volume ratio of the first solvent to the second solvent may be 1: (0.9-1): (0.2-0.6). Preferably, the volume ratio of the metal nanoparticle solution, the first solvent and the second solvent is 1:0.9: 0.6; or the volume ratio of the metal nanoparticle solution, the first solvent, and the second solvent is 1:1:0.2, 1:1:0.4, or 1:1: 0.6.
As a two-solvent system to be added to the metal nanoparticle solution, the first solvent and the second solvent are each independently selected from ethyl acetate, acetone, pentane, 1, 2-trichlorotrifluoroethane, cyclopentane, heptane, n-hexane, isooctane, petroleum ether, cyclohexane, n-butyl chloride, toluene, methyl tert-butyl ether, o-xylene, chlorobenzene, o-dichlorobenzene, diethyl ether, dichloromethane, dichloroethane, n-butanol, any one of isopropanol, N-butyl acetate, isobutanol, methyl isoamyl ketone, N-propanol, tetrahydrofuran, chloroform, methyl isobutyl ketone, methyl N-propyl ketone, methyl ethyl ketone, 1, 4-dioxane, methanol, pyridine, 2-methoxyethanol, acetonitrile, propylene carbonate, N-dimethylformamide, dimethylacetamide, N-methylpyrrolidone and dimethylsulfoxide. The first solvent and the second solvent are different solvents.
The two-solvent system can effectively separate the metal nanoparticles from the solution, for example, as shown in fig. 1, the metal nanoparticle solution, the first solvent and the second solvent are mixed to form a three-solvent system containing the metal nanoparticles, and after shaking and centrifuging, the metal nanoparticles are separated from the three-solvent system.
Preferably, the first solvent is diethyl ether, ethyl acetate, pentane, n-butanol or toluene; the second solvent is acetone, 1, 2-trichlorotrifluoroethane, isopropanol, chloroform or chlorobenzene.
The first solvent and the second solvent may be added to the single metal nanoparticle solution to separate the single metal nanoparticles, or the first solvent and the second solvent may be added to the nano alloy solution to separate the nano alloy.
After the single-metal nanoparticle solution or the nano-alloy solution is added into the first solvent and the second solvent, the first solvent and the second solvent can be vibrated to be uniformly mixed.
In some embodiments, the single metal nanoparticles are selected from any one of nanogold, nanogsilver, nanogalladium, nanognickel, nanogcobalt, nanogchromium, nanogmanganese, nanogmolybdenum, nanogruthenium, nanogrhodium, nanogtungsten, nanoggermanium, nanogtin, nanogrhenium, nanogosmium, nanogiridium, nanogplatinum, nanogbismuth, nanogcopper and nanogiron, and are preferably nanogold or nanogold.
In some embodiments, the monometallic nanoparticles are prepared by chemically reducing a metal salt containing the monometallic metal. The metal salt may be a metal salt containing any one of gold, silver, palladium, nickel, cobalt, chromium, manganese, molybdenum, ruthenium, rhodium, tungsten, germanium, tin, rhenium, osmium, iridium, platinum, bismuth, copper, and iron.
In some embodiments, the nano-alloy is selected from at least any two combinations of nano-gold, nano-silver, nano-palladium, nano-nickel, nano-cobalt, nano-chromium, nano-manganese, nano-molybdenum, nano-ruthenium, nano-rhodium, nano-tungsten, nano-germanium, nano-tin, nano-rhenium, nano-osmium, nano-iridium, nano-platinum, nano-bismuth, nano-copper and nano-iron, for example, the nano alloy is selected from any one of non-miscible nano palladium-rhodium alloy, gold-silver alloy, gold-chromium alloy, gold-tungsten alloy, nickel-ruthenium alloy, nickel-rhodium alloy, copper-ruthenium alloy, copper-tin alloy, osmium-rhodium alloy, palladium-nickel alloy, silver-palladium-nickel alloy, gold-chromium-tungsten alloy, nickel-ruthenium-tin alloy, palladium-nickel-molybdenum-rhodium alloy, and silver-cobalt-tin-osmium alloy.
The nano alloy can be prepared by mixing two different metal salts and carrying out chemical reduction.
In some embodiments, the centrifugation is performed at a speed of 1000 to 15000 rpm. Preferably, the rotating speed of the centrifugation is 3000-12000 rpm; more preferably 9000 rpm.
In some embodiments, the time of centrifugation is 1-600 min. Preferably, the centrifugation time is 1-10 min; more preferably 3 min.
In some embodiments, after centrifuging to remove the upper layer liquid, the lower layer precipitate is dried at 60-80 ℃, preferably 60 ℃, and the drying time can be 2-12 h.
The contents of this document are further illustrated below with reference to specific examples.
EXAMPLE 1 separation of Nano Pd-Rh alloy
Will K2PdCl4(88mg，0.27mmol)、Na3RhCl6·12H2A mixture of O (157mg, 0.26mmol) and DEG solution (20mL) was added to a solution of PVP (275mg) in DEG (80 mL). Magnetically stirring at 220 ℃ for 15min, and cooling to room temperature to obtain a DEG solution (dark brown) of the nano Pd-Rh alloy.
At room temperature, a DEG solution (10mL) of a nano Pd-Rh alloy, ethyl acetate (10mL) and acetone (2mL) were added to a centrifuge tube, the centrifuge tube was shaken until bubbles were generated in the tube, centrifuged (9000rpm, 3min), then the upper layer liquid was removed, and the remaining lower layer precipitate was dried in an oven (60 ℃, 12h) (yield: 100%).
EXAMPLE 2 separation of Nano Pd-Rh alloy
This example is substantially the same as example 1 except that acetone was added in an amount of 4mL (yield: 100%).
EXAMPLE 3 separation of Nano Pd-Rh alloy
This example is substantially the same as example 1 except that acetone was added in an amount of 6mL (yield: 100%).
EXAMPLE 4 separation of Nano Pd-Rh alloy
Will K2PdCl4(88mg，0.27mmol)、Na3RhCl6·12H2A mixture of O (157mg, 0.26mmol) and DEG solution (20mL) was added to a solution of PVP (275mg) in DEG (80 mL). Magnetically stirring at 220 ℃ for 15min, and cooling to room temperature to obtain a DEG solution (dark brown) of the nano Pd-Rh alloy.
At room temperature, a DEG solution (10mL) of a nano Pd-Rh alloy, ether (10mL) and acetone (2mL) are added into a centrifuge tube, the centrifuge tube is shaken until foams are generated in the tube, the tube is centrifuged (9000rpm, 3min), then an upper layer liquid is removed, and a remaining lower layer precipitate is placed into an oven (60 ℃, 12h) to be dried (yield: 100%).
EXAMPLE 5 separation of Nano Pd-Rh alloy
This example is substantially the same as example 4 except that diethyl ether was added in an amount of 9mL (yield: 100%).
EXAMPLE 6 separation of Nano Pd-Rh alloy
This example is substantially the same as example 4 except that in this example, diethyl ether was added in an amount of 30mL and acetone was added in an amount of 50mL (yield: 100%).
Example 7 separation of gold nanoparticles
Mixing AuCl3(151.7mg, 0.5mmol) of TEG solution (10mL) was added to a solution of PVP (1.1g) in TEG (100 mL). Stirring magnetically at 220 deg.C for 5min, and cooling to room temperature to obtain TEG solution (dark brown) of nanogold.
At room temperature, a TEG solution of nanogold (10mL), ethyl acetate (10mL) and acetone (2mL) were added to the centrifuge tube, the centrifuge tube was shaken until a foam was generated in the tube, centrifuged (9000rpm, 3min), then the upper liquid was removed, and the remaining lower precipitate was dried in an oven (60 ℃, 12h) (yield: 100%).
Example 8 separation of gold nanoparticles
This example is substantially the same as example 7 except that acetone was added in an amount of 4mL (yield: 100%).
Example 9 separation of gold nanoparticles
This example is substantially the same as example 7 except that acetone was added in an amount of 6mL (yield: 100%).
Comparative example 1 separation of Nano Pd-Rh alloy
Will K2PdCl4(88mg，0.27mmol)、Na3RhCl6·12H2A mixture of O (157mg, 0.26mmol) and DEG solution (20mL) was added to a solution of PVP (275mg) in DEG (80 mL). Magnetically stirring at 220 deg.C for 15min, cooling to room temperature to obtain the DEG solution of nanometer Pd-Rh alloyLiquid (dark brown).
At room temperature, a DEG solution (10mL) of a nano Pd-Rh alloy and ethyl acetate (15mL) were added to a centrifuge tube, the centrifuge tube was shaken until bubbles were generated in the tube, centrifuged (9000rpm, 3min), then the upper layer liquid was removed, and the remaining lower layer precipitate was dried in an oven (60 ℃, 12h) (yield: 85%).
Comparative example 2 separation of Nano Pd-Rh alloy
The scheme of this example is substantially the same as that of comparative example 1 except that the amount of the DEG solution of the nano Pd-Rh alloy added in this example is 10mL and the amount of acetone added is 15mL (yield: 85%).
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields within the spirit of the present invention are included in the scope of the present invention.

Claims (10)

1. A method of separating metal nanoparticles from a solution, comprising:
adding a first solvent and a second solvent into the metal nanoparticle solution, and performing centrifugal separation to obtain metal nanoparticles;
wherein the volume ratio of the metal nanoparticle solution, the first solvent and the second solvent is 1: (0.1 to 10)7)：(0.1～107)。
2. The method of claim 1, wherein the volume ratio of the metal nanoparticle solution, the first solvent, and the second solvent is 1: (0.1-3): (0.1-5).
3. The method of claim 1, wherein the volume ratio of the metal nanoparticle solution, the first solvent, and the second solvent is 1: (0.9-1): (0.2-0.6).
4. The method according to claim 1, wherein the first solvent and the second solvent are each independently selected from the group consisting of ethyl acetate, acetone, pentane, 1, 2-trichlorotrifluoroethane, cyclopentane, heptane, n-hexane, isooctane, petroleum ether, cyclohexane, n-butyl chloride, toluene, methyl tert-butyl ether, o-xylene, chlorobenzene, o-dichlorobenzene, diethyl ether, dichloromethane, dichloroethane, n-butanol, any one of isopropanol, N-butyl acetate, isobutanol, methyl isoamyl ketone, N-propanol, tetrahydrofuran, chloroform, methyl isobutyl ketone, methyl N-propyl ketone, methyl ethyl ketone, 1, 4-dioxane, methanol, pyridine, 2-methoxyethanol, acetonitrile, propylene carbonate, N-dimethylformamide, dimethylacetamide, N-methylpyrrolidone and dimethylsulfoxide; wherein the first solvent and the second solvent are different solvents.
5. The method of claim 1, wherein the metal nanoparticles are monometallic nanoparticles or nanoalloys.
6. The method as claimed in claim 5, wherein the single metal nanoparticles are selected from any one of nano gold, nano silver, nano palladium, nano nickel, nano cobalt, nano chromium, nano manganese, nano molybdenum, nano ruthenium, nano rhodium, nano tungsten, nano germanium, nano tin, nano rhenium, nano osmium, nano iridium, nano platinum, nano bismuth, nano copper and nano iron.
7. The method of claim 5, wherein the nano-alloy is selected from at least any two combinations of the single-metal nanoparticles of claim 6;
preferably, the nano alloy is selected from any one of non-miscible nano palladium-rhodium alloy, gold-silver alloy, gold-chromium alloy, gold-tungsten alloy, nickel-ruthenium alloy, nickel-rhodium alloy, copper-ruthenium alloy, copper-tin alloy, osmium-rhodium alloy, palladium-nickel alloy, silver-palladium-nickel alloy, gold-chromium-tungsten alloy, nickel-ruthenium-tin alloy, palladium-nickel-molybdenum-rhodium alloy and silver-cobalt-tin-osmium alloy.
8. The method according to claim 1, wherein the centrifugation is carried out at a speed of 1000 to 15000 rpm.
9. The method according to claim 8, wherein the centrifugation time is 1-600 min.
10. The method of claim 1, further comprising:
after centrifugation, the upper layer liquid is removed and the lower layer precipitate is dried at 60-80 ℃.
CN202110482808.8A 2021-04-30 2021-04-30 Method for separating metal nanoparticles and nano-alloy from solution Pending CN113333734A (en)

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Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040115345A1 (en) * 2002-07-23 2004-06-17 Xueying Huang Nanoparticle fractionation and size determination
US20060159603A1 (en) * 2005-01-14 2006-07-20 Cabot Corporation Separation of metal nanoparticles
CN101104204A (en) * 2006-07-10 2008-01-16 三星电机株式会社 Method for manufacturing metal nanoparticles
CN1958167A (en) * 2006-11-28 2007-05-09 厦门大学 Method for separating micro Nano material
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