CN113084155A - Green, mild and efficient purification method of nano silver wires - Google Patents
Green, mild and efficient purification method of nano silver wires Download PDFInfo
- Publication number
- CN113084155A CN113084155A CN202110339822.2A CN202110339822A CN113084155A CN 113084155 A CN113084155 A CN 113084155A CN 202110339822 A CN202110339822 A CN 202110339822A CN 113084155 A CN113084155 A CN 113084155A
- Authority
- CN
- China
- Prior art keywords
- nano silver
- nano
- green
- silver wire
- purification method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 58
- 238000000746 purification Methods 0.000 title claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002245 particle Substances 0.000 claims abstract description 28
- 239000000725 suspension Substances 0.000 claims abstract description 28
- 239000012452 mother liquor Substances 0.000 claims abstract description 25
- 239000012535 impurity Substances 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000002244 precipitate Substances 0.000 claims abstract description 18
- 239000002042 Silver nanowire Substances 0.000 claims abstract description 14
- 239000002105 nanoparticle Substances 0.000 claims abstract description 12
- 238000004062 sedimentation Methods 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 27
- 230000008569 process Effects 0.000 claims description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000010413 mother solution Substances 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- GSNUFIFRDBKVIE-UHFFFAOYSA-N DMF Natural products CC1=CC=C(C)O1 GSNUFIFRDBKVIE-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- CEOWTYWOQSHEQI-UHFFFAOYSA-N butan-2-one;2-propan-2-yloxypropane Chemical compound CCC(C)=O.CC(C)OC(C)C CEOWTYWOQSHEQI-UHFFFAOYSA-N 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 238000001016 Ostwald ripening Methods 0.000 claims 2
- 230000005070 ripening Effects 0.000 abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- 229910052709 silver Inorganic materials 0.000 description 5
- 239000004332 silver Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 238000000502 dialysis Methods 0.000 description 3
- 238000001962 electrophoresis Methods 0.000 description 3
- 229920005862 polyol Polymers 0.000 description 3
- 150000003077 polyols Chemical class 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 238000011282 treatment Methods 0.000 description 2
- 241000700605 Viruses Species 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 238000000703 high-speed centrifugation Methods 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0547—Nanofibres or nanotubes
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
-
- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/148—Agglomerating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- 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
- B22F2301/00—Metallic composition of the powder or its coating
- B22F2301/25—Noble metals, i.e. Ag Au, Ir, Os, Pd, Pt, Rh, Ru
- B22F2301/255—Silver or gold
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a green mild high-efficiency purification method of a nano silver wire, which comprises the following operation steps: the method comprises the following steps: adding pure water in a certain proportion into the obtained nano silver wire mother liquor, uniformly stirring, and settling for 1-48 h; step two: carefully collecting the upper layer of the nano-silver wire suspension, and discarding nano-particle impurities settled after curing at the bottom of the container; the suspension was slowly dropped with PVP insoluble solvent under stirring until the color of the above solution also changed slowly from grayish green to yellow or orange and flocculent precipitate of silver nanowires appeared, and the dropping of the solvent was stopped and allowed to settle by standing. According to the invention, through the flow cooperation of the first step, the second step and the third step, the Oswald ripening principle is utilized to drive small particles to coarsen into large particles, and the particles can be removed through simple sedimentation, so that the aim of improving the solution purity is achieved.
Description
Technical Field
The invention relates to the technical field of nano silver wires, in particular to a green, mild and efficient purification method of a nano silver wire.
Background
The traditional separation and purification method of the nano silver wire mainly comprises a centrifugal sedimentation method, a filtration method (pressure filtration, pressure reduction filtration, centrifugal filtration), an electrophoresis method, a dialysis method, a natural sedimentation method, a selective sedimentation method and the like, according to actual experience, the centrifugal process is easy to settle nano silver particles and the nano silver wire together due to overlong centrifugal time and overhigh centrifugal speed, the separation and purification effect cannot be achieved, and the most important is that the nano silver wire has high probability and irreversibly forms agglomerates (locking agglomerates), after multiple centrifugal purification treatments, the yield of the nano silver wire can be seriously influenced, the filtration method is simple to operate, fast and efficient, but only small-diameter particles in a system can be removed, large-diameter nano particle impurities are difficult to remove, and irreversible agglomerates caused by formed nano silver wire filter cakes are difficult to redisperse, so the method has certain limitation;
the limitation of the electrophoresis method is that the gel treatment is needed firstly, and then the gel is exchanged into a proper solvent, the concentration needs to be kept low, otherwise the nanometer coat keeps the colloid stability of the nanometer silver wire, which greatly limits the application in the industrial scale production, and the dialysis method is mostly used for removing substances below 10nm, such as small molecules, polymer chains and viruses, and limits the application in the purification of the nanometer silver wire;
the traditional methods are large in limitation and difficult to be applied in large scale in industrial production, and an acetone selective precipitation method is proposed in the market, in the process of synthesizing the nano silver wire, PVP is needed as a polymerization inhibitor and a dispersing agent, the crystal faces 110 and 100 of the nano silver wire have higher activation energy and are combined with PVP to be protected, the silver wire can only grow along the crystal face 111, the nano silver wire in the mother solution is coated by the PVP, the acetone is slowly added into the mother solution containing the nano silver wire by utilizing the complementary intermiscibility of the acetone and the PVP, so that the nano silver wire can be deposited on the bottom of a container in a flocculation shape, the color of the solution is slowly changed from grey green to yellow or orange, the addition amount of the acetone can be judged according to the change of the color, after the acetone heats the mother solution, the nano silver wire is deposited on the bottom, the suspension containing particles and the nano rod on the top is removed, the method provided by the team is also a common method for synthesizing and purifying the nano silver wire at present, the effect is obvious, the quantity of impurity products of nano particles and short rods of the purified nano silver wire is obviously reduced, and the method is suitable for industrial amplification production, but the defects of the method are obvious: the whole operation is too fine, the process is complicated, the consumed time is long, most importantly, a large amount of toxic acetone is used, the environment is not protected, the waste liquid is difficult to recycle, the cost is high, and the method is only suitable for small-scale implementation at present;
in the process of purifying the nano silver wires, acetone sedimentation, ultrasound and high-speed centrifugation are involved, the whole method is only suitable for operation in a laboratory, particularly, the ultrasonic dispersion of the nano silver wire precipitation lumps is not good in dispersion effect and difficult to control strength, re-agglomeration of the nano silver wires is easy to cause, the precision requirement on the operation process is too high, and the method is difficult to apply to industrial production in a large range.
Therefore, it is highly desirable to design a green, mild and efficient purification method of silver nanowires to solve the above problems.
Disclosure of Invention
The invention aims to provide a green mild high-efficiency purification method for a nano silver wire, which aims to solve the problems that small particles cannot be driven to be coarsened into large particles by using an Ostwald curing principle in the using process of the traditional nano silver wire separation and purification method provided by the background art, the environment is poor in economical efficiency, links such as centrifugation, filtration, electrophoresis and dialysis are involved, and high shearing and special equipment and instruments are required in the whole process.
In order to achieve the purpose, the invention provides the following technical scheme: a green mild high-efficiency purification method of nano silver wires comprises the following operation steps:
the method comprises the following steps: adding pure water in a certain proportion into the obtained nano silver wire mother liquor, uniformly stirring, and settling for 1-48 h;
step two: carefully collecting the upper layer of the nano-silver wire suspension, and discarding nano-particle impurities settled after curing at the bottom of the container; slowly dripping PVP insoluble solvent into the suspension under stirring until the color of the solution is slowly changed from grayish green to yellow or orange and flocculent precipitate of the nano silver wires appears, stopping dripping the solvent, and standing for settling;
step three: carefully removing the upper suspension, collecting the precipitate, re-dispersing in 0.01-1% PVP aqueous solution, stirring and shaking up; repeating the steps 1-3 for at least 2-4 times to obtain the high-purity nano silver wire product.
Preferably, in the step one process, the pure water is one of distilled water, deionized water and pure water obtained by three times of distillation, and the purity of the pure water is more than 99%.
Preferably, in the step one process, the nano silver wire mother liquor added with the pure water is stirred uniformly by a glass stirring rod manually, and during stirring, the glass stirring rod is stirred clockwise for 3 circles, then is stirred anticlockwise for 3 circles, and the steps are repeated.
Preferably, the sedimentation of the nano silver wire mother solution during the step one is based on the oswald ripening principle, and the oswald ripening principle: because the solution is in a thermodynamic imbalance state and the required surface energy tends to be reduced, small particles in the solution are continuously reduced and then completely disappear and dissolved, and large particles are larger and larger in diameter, so that the small particles are dissolved and deposited on the surface of the large particles again to achieve the effect of reducing the surface energy, and meanwhile, the conservation of quality is ensured.
Preferably, during the second step, the PVP insoluble solvent is one of ethyl acetate, tetrahydrofuran, DMF, DMSO, ethanol, isopropanol, isopropyl ether and primary butanone, and the volume ratio between the mother liquor and the solvent is 1: 0.1 to 10.
Preferably, during step three, the supernatant suspension contains nanoparticles and short rod impurities and is removed using a strainer embedded with a fine mesh.
Preferably, during the third step, the model of the PVP is one of K30, K40, K50, K60 and K90.
Compared with the prior art, the invention has the beneficial effects that:
1. the green mild high-efficiency purification method of the nano silver wire has the advantages that through the flow matching of the first step, the second step and the third step, the Ostwald curing principle is utilized to drive small particles to be coarsened into large particles, the particles can be removed through simple sedimentation, and the aim of improving the purity of the solution is fulfilled.
2. This silver nanowire's green gentle high-efficient purification method adopts the distilled water that obtains after the cubic distillation through the pure water, deionized water, one of them and the purity of pure water is greater than 99%, the foreign particles who carries in the greatly reduced pure water, prevent that impurity from causing the influence to the preparation of silver nanowire mother liquor, through stirring 3 circles clockwise with the glass stirring rod earlier, then stir 3 circles anticlockwise again, so reciprocating cycle can, can be fully to the stirring of the silver nanowire mother liquor of adding the pure water, prevent that the silver nanowire mother liquor of adding the pure water from appearing deposiing, improve the stirring degree of uniformity of silver nanowire mother liquor solution.
3. The green mild high-efficiency purification method of the nano silver wires is based on the Ostwald curing principle through the sedimentation of the mother liquor solution of the nano silver wires, can quickly and simply settle precipitates, meets the aim of purifying solution impurities, simply eliminates residual impurities in the solution, adopts one of ethyl acetate, tetrahydrofuran, DMF, DMSO, ethanol, isopropanol and isopropyl ether butanone through a PVP insoluble solvent, and the volume ratio of the mother liquor to the solvent is 1: 0.1 ~ 10, satisfy the manifold selection demand of PVP insoluble solvent, can carry out accurate selection according to the on-the-spot condition, promote the precision of volume ratio between mother liquor and the solvent, contain nanometer particulate matter and short stick pole impurity through upper suspension, and use the strainer that has inlayed fine and close filter screen to remove, strengthen the manual edulcoration effect of solution, guarantee the purity requirement of solution, the model through PVP adopts K30, K40, K50, one of them of K60 and K90, the selectivity of various PVP models is provided, the person of facilitating the use carries out the pertinence selection according to actual requirement, further strengthen the purification effect of nanometer silver line.
Drawings
FIG. 1 is a flow chart of the steps of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, 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.
Referring to fig. 1, an embodiment of the present invention:
a green mild high-efficiency purification method of nano silver wires comprises the following operation steps:
the method comprises the following steps: adding pure water in a certain proportion into the obtained nano silver wire mother liquor, uniformly stirring, and settling for 1-48 h;
step two: carefully collecting the upper layer of the nano-silver wire suspension, and discarding nano-particle impurities settled after curing at the bottom of the container; slowly dripping PVP insoluble solvent into the suspension under stirring until the color of the solution is slowly changed from grayish green to yellow or orange and flocculent precipitate of the nano silver wires appears, stopping dripping the solvent, and standing for settling;
step three: carefully removing the upper suspension, collecting the precipitate, re-dispersing in 0.01-1% PVP aqueous solution, stirring and shaking up; repeating the steps 1-3 for at least 2-4 times to obtain a high-purity nano silver wire product, driving small particles to coarsen into large particles by utilizing the Oswald ripening principle through the flow matching of the step one, the step two and the step three, and removing particles through simple sedimentation to achieve the aim of improving the purity of the solution, meanwhile, adopting an acetone-free selective sedimentation method to collect the high-purity nano silver wire as far as possible and improve the yield, and the green color is environment-friendly and safe in the implementation process, and no harmful substances and gas are separated out.
In the first step, the pure water is one of distilled water, deionized water and pure water obtained after three times of distillation, the purity of the pure water is more than 99%, impurity particles carried in the pure water are greatly reduced, and the influence of impurities on the preparation of the nano silver wire mother liquor is prevented.
In the first step of process, use the glass stirring rod manual to carry out the stirring to the nanometer silver line mother liquor that adds the pure water, and during the stirring, stir 3 circles clockwise with the glass stirring rod earlier, then stir 3 circles anticlockwise, so reciprocating bad can, can be fully to the nanometer silver line mother liquor stirring of adding the pure water, prevent that the nanometer silver line mother liquor that adds the pure water from appearing deposiing, improve the stirring degree of consistency of nanometer silver line mother liquor solution.
During step one, the sedimentation of the nano silver wire mother solution is based on the oswald ripening principle, which is: because the solution is in a thermodynamic imbalance state, the required surface energy tends to be reduced, small particles can be continuously reduced and then completely disappear and dissolved in the solution, the diameter of large particles can be larger and larger, the small particles are dissolved and deposited on the surface of the large particles again to achieve the effect of reducing the surface energy, the conservation of quality is ensured, precipitates can be quickly and simply settled, the aim of purifying solution impurities is fulfilled, and residual impurities in the solution are simply removed.
In the second step, the PVP insoluble solvent is one of ethyl acetate, tetrahydrofuran, DMF, DMSO, ethanol, isopropanol and isopropyl ether primary butanone, and the volume ratio of the mother liquor to the solvent is 1: 0.1 ~ 10, satisfy the manifold selection demand of PVP insoluble solvent, can carry out accurate selection according to the on-the-spot condition, promote the precision of volume ratio between mother liquor and the solvent.
In the third step, the upper suspension contains nano-particles and short rod impurities, and is removed by using a strainer embedded with a fine filter screen, so that the manual impurity removal effect of the solution is enhanced, and the purity requirement of the solution is ensured.
In the third step, the model of the PVP adopts one of K30, K40, K50, K60 and K90, so that the selectivity of various PVP models is provided, a user can conveniently perform targeted selection according to actual requirements, and the purification effect of the silver nanowire is further enhanced.
According to the above embodiments, the present invention also has the following embodiments, and each embodiment is a limitation of the above embodiments;
example 1
1. The synthesis of the nano silver wire adopts a high-temperature reduction method of a polyol/PVP/halogen salt construction system, pure water in equal proportion is added into the obtained nano silver wire mother liquor, the mixture is stirred and mixed uniformly, and the mixture is settled for 12 hours;
2. carefully collecting the upper layer of the nano-silver wire suspension, and discarding nano-particle impurities settled after curing at the bottom of the container; the suspension was added slowly dropwise to tetrahydrofuran at room temperature with stirring, suspension: tetrahydrofuran ═ 1: 0.5 (volume ratio), slowly changing the color of the upper solution from grayish green to yellow and generating flocculent precipitate of the nano silver wires, stopping dripping, standing and settling for 3 hours;
3. carefully removing the upper suspension, collecting flocculent precipitate, re-dispersing the nano silver wire precipitate in 0.05% PVP (K30) aqueous solution, stirring and shaking up;
repeating the step 1-3 for 3 times to obtain the high-purity nano silver wire product.
Example 2
1. The synthesis of the nano silver wire adopts a high-temperature reduction method of a polyol/PVP/halogen salt construction system, pure water in equal proportion is added into the obtained nano silver wire mother liquor, the mixture is stirred and mixed uniformly, and the mixture is settled for 24 hours;
2. carefully collecting the upper layer of the nano silver wire suspension, abandoning nano particle impurities, short wires, rods and the like settled after curing the bottom of the container; suspension DMF was added slowly dropwise at room temperature with stirring, suspension: DMF ═ 1: 1 (volume ratio), slowly changing the color of the upper solution from grayish green to orange yellow, starting to generate flocculent precipitate of the nano silver wires, stopping dripping, standing and settling for 2 hours;
3. carefully removing the upper suspension, collecting flocculent precipitate, re-dispersing the nano silver wire precipitate in 0.02% PVP (K60) aqueous solution, stirring and shaking up;
repeating the steps 1-3 for 4 times to obtain the high-purity nano silver wire product.
Example 3
1. The synthesis of the nano silver wire adopts a high-temperature reduction method of a polyol/PVP/halogen salt construction system, pure water in equal proportion is added into the obtained nano silver wire mother liquor, the mixture is stirred and mixed uniformly, and the mixture is settled for 36 hours;
2. carefully collecting the upper layer of the nano silver wire suspension, abandoning nano particle impurities, short wires, rods and the like settled after curing the bottom of the container; the suspension was slowly added dropwise to butanone under stirring at room temperature, suspension: butanone 1: 0.8 (volume ratio), slowly changing the color of the upper solution from grayish green to orange yellow, starting to generate flocculent precipitate of the nano silver wires, stopping dripping, standing and settling for 2 hours;
3. carefully removing the upper suspension, collecting flocculent precipitate, redispersing the nano silver wire precipitate in 0.01% PVP (K90) aqueous solution, stirring and shaking up;
repeating the step 1-3 for 3 times to obtain the high-purity nano silver wire product.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (7)
1. A green mild high-efficiency purification method of nano silver wires is characterized by comprising the following steps: the operation steps are as follows:
the method comprises the following steps: adding pure water in a certain proportion into the obtained nano silver wire mother liquor, uniformly stirring, and settling for 1-48 h;
step two: carefully collecting the upper layer of the nano-silver wire suspension, and discarding nano-particle impurities settled after curing at the bottom of the container; slowly dripping PVP insoluble solvent into the suspension under stirring until the color of the solution is slowly changed from grayish green to yellow or orange and flocculent precipitate of the nano silver wires appears, stopping dripping the solvent, and standing for settling;
step three: carefully removing the upper suspension, collecting the precipitate, re-dispersing in 0.01-1% PVP aqueous solution, stirring and shaking up; repeating the steps 1-3 for at least 2-4 times to obtain the high-purity nano silver wire product.
2. The green mild high-efficiency purification method of the silver nanowires of claim 1, which is characterized in that: in the step one process, the pure water is one of distilled water, deionized water and pure water obtained by three times of distillation, and the purity of the pure water is more than 99%.
3. The green mild high-efficiency purification method of the silver nanowires of claim 1, which is characterized in that: in the step one process, the nano silver wire mother liquor added with the pure water is stirred uniformly by using a glass stirring rod manually, and during stirring, the glass stirring rod is stirred clockwise for 3 circles, then is stirred anticlockwise for 3 circles, and the steps are repeated.
4. The green mild high-efficiency purification method of the silver nanowires of claim 1, which is characterized in that: during the step one, the sedimentation of the nano silver line mother solution is based on the Ostwald ripening principle, and the Ostwald ripening principle is as follows: because the solution is in a thermodynamic imbalance state and the required surface energy tends to be reduced, small particles in the solution are continuously reduced and then completely disappear and dissolved, and large particles are larger and larger in diameter, so that the small particles are dissolved and deposited on the surface of the large particles again to achieve the effect of reducing the surface energy, and meanwhile, the conservation of quality is ensured.
5. The green mild high-efficiency purification method of the silver nanowires of claim 1, which is characterized in that: in the second step, the PVP insoluble solvent is one of ethyl acetate, tetrahydrofuran, DMF, DMSO, ethanol, isopropanol and isopropyl ether methyl ethyl ketone, and the volume ratio of the mother liquor to the solvent is 1: 0.1 to 10.
6. The green mild high-efficiency purification method of the silver nanowires of claim 1, which is characterized in that: during step three, the supernatant suspension contained nanoparticles and short rod impurities and was removed using a strainer embedded with a fine screen.
7. The green mild high-efficiency purification method of the silver nanowires of claim 1, which is characterized in that: and in the third step, the model number of the PVP adopts one of K30, K40, K50, K60 and K90.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110339822.2A CN113084155A (en) | 2021-03-30 | 2021-03-30 | Green, mild and efficient purification method of nano silver wires |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110339822.2A CN113084155A (en) | 2021-03-30 | 2021-03-30 | Green, mild and efficient purification method of nano silver wires |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113084155A true CN113084155A (en) | 2021-07-09 |
Family
ID=76671166
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110339822.2A Pending CN113084155A (en) | 2021-03-30 | 2021-03-30 | Green, mild and efficient purification method of nano silver wires |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113084155A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115194143A (en) * | 2022-06-22 | 2022-10-18 | 深圳先进电子材料国际创新研究院 | Method for separating and purifying nano particles in suspension of polyvinyl pyrrolidone coated nano particles |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105345022A (en) * | 2015-10-22 | 2016-02-24 | 东华大学 | Purification method for silver nanowire |
| CN106001544A (en) * | 2016-07-08 | 2016-10-12 | 合肥微晶材料科技有限公司 | Method for purifying silver nanowires through settling separation |
| CN107486561A (en) * | 2017-07-27 | 2017-12-19 | 南京邮电大学 | A kind of method that extensive normal pressure prepares and separates nano silver wire |
| CN109434132A (en) * | 2018-12-07 | 2019-03-08 | 陕西煤业化工技术研究院有限责任公司 | A method of purifying ultra-fine silver nanowires |
| CN109482900A (en) * | 2018-12-14 | 2019-03-19 | 浙江加州国际纳米技术研究院台州分院 | A kind of method high-volume synthesis and efficiently purify ultra-fine silver nanowires |
| CN109545476A (en) * | 2018-11-21 | 2019-03-29 | 哈尔滨工业大学 | The method of atomic deposition zinc oxide promotion silver nanowires electrode stability |
-
2021
- 2021-03-30 CN CN202110339822.2A patent/CN113084155A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105345022A (en) * | 2015-10-22 | 2016-02-24 | 东华大学 | Purification method for silver nanowire |
| CN106001544A (en) * | 2016-07-08 | 2016-10-12 | 合肥微晶材料科技有限公司 | Method for purifying silver nanowires through settling separation |
| CN107486561A (en) * | 2017-07-27 | 2017-12-19 | 南京邮电大学 | A kind of method that extensive normal pressure prepares and separates nano silver wire |
| CN109545476A (en) * | 2018-11-21 | 2019-03-29 | 哈尔滨工业大学 | The method of atomic deposition zinc oxide promotion silver nanowires electrode stability |
| CN109434132A (en) * | 2018-12-07 | 2019-03-08 | 陕西煤业化工技术研究院有限责任公司 | A method of purifying ultra-fine silver nanowires |
| CN109482900A (en) * | 2018-12-14 | 2019-03-19 | 浙江加州国际纳米技术研究院台州分院 | A kind of method high-volume synthesis and efficiently purify ultra-fine silver nanowires |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115194143A (en) * | 2022-06-22 | 2022-10-18 | 深圳先进电子材料国际创新研究院 | Method for separating and purifying nano particles in suspension of polyvinyl pyrrolidone coated nano particles |
| CN115194143B (en) * | 2022-06-22 | 2023-11-14 | 深圳先进电子材料国际创新研究院 | Method for separating and purifying nano particles in suspension of polyvinylpyrrolidone coated nano particles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| KR101197386B1 (en) | Process for manufacture of nanometric, monodisperse, and stable metallic silver and product obtained therefrom | |
| Pradel et al. | Cross‐flow purification of nanowires | |
| CN103170645B (en) | The preparation method of nano silver wire | |
| CN106893722B (en) | Stimulus-responsive nucleic acid nanostructure carrier chiral noble metal nano-composite and preparation method and application thereof | |
| CN103586461B (en) | A kind of nano silver colloidal sol and preparation and purification method thereof | |
| CN104209538B (en) | A kind of method preparing nano-silver thread in an aqueous medium | |
| CN107127333B (en) | A method of by vibrating and settling purification silver nanowires | |
| CN107377993B (en) | A kind of metal nanometer line, dispersion liquid and preparation method thereof | |
| CN110576193B (en) | Method for preparing superfine silver nanowires by using citrate as reducing agent | |
| CN109650350A (en) | A kind of method and application of large scale preparation polyose modification nanometer selenium | |
| CN104308169B (en) | A kind of preparation method of the concave surface silver nano-grain with high miller index surface | |
| CN113084155A (en) | Green, mild and efficient purification method of nano silver wires | |
| CN104591305B (en) | A kind of purification devices of nano wire and purification process | |
| CN112605392A (en) | Method for preparing silver nanowires | |
| CN107802845B (en) | Method for phase conversion of hydrophobic nanoparticles by using silk fibroin molecules | |
| CN110170644A (en) | A method of by being centrifuged and settling purification silver nanowires | |
| CN105820277B (en) | A kind of PBCA nanowire preparation method | |
| CN112743099A (en) | Preparation method of gold nanorod material with length-diameter ratio regulated and controlled by hydrochloric acid | |
| CN102728831B (en) | Method for dispersing, purifying and/or assembling nano gold rods | |
| CN110814361A (en) | Silver nanowire purification method | |
| CN108213459B (en) | Preparation method of glucan/nano gold-silver alloy compound | |
| CN112809017A (en) | Large-scale preparation and purification method of superfine silver nanowires | |
| JPH04240112A (en) | Production of silica particulates | |
| CN110845746A (en) | Preparation method of nano starch | |
| CN103342768B (en) | A kind of method utilizing emulsifier-free emulsion polymerization to prepare PMMA microsphere |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210709 |