CN115138858B - Preparation method of silver nanowire - Google Patents
Preparation method of silver nanowire Download PDFInfo
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- CN115138858B CN115138858B CN202210914600.3A CN202210914600A CN115138858B CN 115138858 B CN115138858 B CN 115138858B CN 202210914600 A CN202210914600 A CN 202210914600A CN 115138858 B CN115138858 B CN 115138858B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 238000003756 stirring Methods 0.000 claims abstract description 121
- 238000001914 filtration Methods 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000004140 cleaning Methods 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims description 55
- 239000005416 organic matter Substances 0.000 claims description 39
- 239000007864 aqueous solution Substances 0.000 claims description 32
- 239000002270 dispersing agent Substances 0.000 claims description 25
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 25
- 238000007599 discharging Methods 0.000 claims description 22
- 239000013049 sediment Substances 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 15
- 239000012266 salt solution Substances 0.000 claims description 13
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 4
- 229940071536 silver acetate Drugs 0.000 claims description 4
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 2
- 239000002244 precipitate Substances 0.000 abstract description 8
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 9
- 238000011068 loading method Methods 0.000 description 8
- 238000010924 continuous production Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 239000002070 nanowire Substances 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000004038 photonic crystal Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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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
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/01—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor with flat filtering elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D29/00—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor
- B01D29/88—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor having feed or discharge devices
- B01D29/94—Filters with filtering elements stationary during filtration, e.g. pressure or suction filters, not covered by groups B01D24/00 - B01D27/00; Filtering elements therefor having feed or discharge devices for discharging the filter cake, e.g. chutes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/10—Maintenance of mixers
- B01F35/11—Maintenance of mixers using fluids
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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
- 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
- B22F1/0545—Dispersions or suspensions of nanosized particles
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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
- 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
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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- 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
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- 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
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention discloses a preparation method of silver nanowires, which belongs to the technical field of nano material preparation, wherein a silver nanowire is prepared by adopting a silver nanowire preparation machine, a cleaning mechanism arranged in the silver nanowire preparation machine is matched with a filtering mechanism, the interior of a stirring tank is cleaned by the cleaning mechanism through deionized water while a precipitate in a mixed solution is separated by the filtering mechanism, so that the preparation efficiency of the silver nanowires is improved, and meanwhile, when the deionized water in the stirring tank is discharged into the filtering tank of the filtering mechanism after cleaning, the precipitate on the filtering tank can be washed to remove soluble impurities on the surface of the precipitate, thereby being convenient for preparing pure silver nanowires, improving the preparation quality of the silver nanowires.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation method of silver nanowires.
Background
Among nanomaterials, one-dimensional metallic nanomaterials having an axial-to-radial ratio have been attracting attention due to their unique electrical, magnetic, thermal, optical properties and potential applications in microelectronic devices, optoelectronic devices, sensors, etc. Among these one-dimensional metal nanowires, silver nanowires are the most studied because of their very high electrical and thermal conductivity properties. Silver has potential applications in many fields of application, such as silver nanowires, which have been used in the fields of polarizing devices, photonic crystals, catalysts, as well as biological and chemical sensors.
The existing preparation methods of silver nanowires mainly comprise a physical template method and a liquid phase reduction method, wherein the template is removed by using a stronger corrosion reaction for synthesizing the nanowires by the physical template method, which not only can pollute the metal nanowires, but also can bring a large amount of waste liquid. The liquid phase reduction method is classified into a hydrothermal method and an oil bath heating method, wherein the hydrothermal method requires a reaction kettle to react in a closed system, and the prepared silver nanowire has a higher length-diameter ratio, but the reaction is affected by the volume ratio of air and solution in the reaction kettle, so that the repeatability is poor, and continuous production cannot be realized.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method of silver nanowires, which solves the following technical problems: the existing silver nanowire has low preparation efficiency and cannot be continuously produced.
The aim of the invention can be achieved by the following technical scheme:
a method for preparing silver nanowires, comprising the following steps:
step one: 15-20 parts of water-soluble silver salt, 1.5-2.5 parts of dispersing agent, 100-150 parts of aqueous solution A of polyhydroxy liquid organic matter and 15-60 parts of aqueous solution B of polyhydroxy liquid organic matter are weighed according to weight parts;
step two: adding an aqueous solution A of a polyhydroxy liquid organic matter into a first feeding box of a silver nanowire preparation machine, and adding water-soluble silver salt into the first feeding box to obtain a water-soluble silver salt solution;
step three: adding an aqueous solution B of polyhydroxy liquid organic matters into a second feeding box of the silver nanowire preparation machine, and adding a dispersing agent into the second feeding box to obtain a dispersing agent solution;
step four: when the heating belt heats and maintains the temperature of the stirring tank to 150-250 ℃, opening a connecting pipe communicated with the first feeding box and a control valve on the connecting pipe communicated with the second feeding box, enabling the water-soluble silver salt solution and the dispersing agent solution to fall into the stirring tank through the connecting pipes respectively, simultaneously starting a stirring motor, driving a stirring shaft to rotate by an output shaft of the stirring motor, driving a plurality of stirring blades to rotate by the stirring shaft, and stirring the dispersing agent solution and the water-soluble silver salt solution in the stirring tank by the stirring blades to obtain mixed solution;
step five: opening the control valve on the discharging pipe, enabling mixed liquid to fall into the filter tank through the discharging pipe, filtering sediment in the mixed liquid through the filter screen, then remaining on the surface of the filter screen, discharging liquid from the filter screen along the filter tank, introducing deionized water to a plurality of cleaning pipes on the mounting seat, cleaning the residual mixed liquid in the stirring tank, discharging cleaning water to the filter tank, washing the sediment on the filter tank, starting the rotating motor, and driving the filter tank on the rotating shaft to rotate by the output shaft of the rotating motor, so that the filter tank is turned over, collecting the sediment on the filter screen in the filter tank, and obtaining silver nanowires.
Further, the water-soluble silver salt is one or more of silver nitrate, silver chlorate and silver acetate which are mixed according to any proportion; the dispersing agent is polyvinylpyrrolidone.
Further, the aqueous solution A of the polyhydroxy liquid organic matter and the aqueous solution B of the polyhydroxy liquid organic matter are both formed by mixing the polyhydroxy liquid organic matter and water, and the volume ratio of the polyhydroxy liquid organic matter to the water in the aqueous solution A of the polyhydroxy liquid organic matter to the aqueous solution B of the polyhydroxy liquid organic matter is 1:3.
Further, the polyhydroxy liquid organic matter is one or more of glycol and glycerol which are mixed in any proportion.
Further, the stirring time in the fourth step is 30-70 min.
Further, the silver nanowire preparation machine comprises a stirring tank, wherein the bottom of the stirring tank is arranged in a fixed tank, the stirring tank is fixedly arranged in the fixed tank through a plurality of connecting rings, a gap is arranged between the fixed tank and the stirring tank, the gap is filled with a plurality of heating belts for heating the stirring tank, a first feeding box is arranged on a first feeding frame arranged on one side of the stirring tank, a second feeding box is arranged on a second feeding frame arranged on the other side of the stirring tank, and the first feeding box and the second feeding box are respectively communicated with the top of the stirring tank through connecting pipes;
the stirring tank is characterized in that an output shaft of a stirring motor fixedly arranged at the top of the stirring tank is fixedly connected with the end part of a stirring shaft, the stirring shaft is rotatably arranged in the stirring tank, and a plurality of stirring blades are fixedly arranged on the stirring shaft;
the stirring tank is characterized in that a filtering mechanism is arranged at the bottom of the stirring tank and comprises a filtering tank, a filter screen for filtering sediment is arranged in the filtering tank, the filtering tank is arranged above the fixing base, rotating shafts fixedly arranged on two sides of the filtering tank are respectively rotatably arranged on two sides of the fixing base, and one rotating shaft end part of the rotating motor is fixedly connected with an output shaft of the rotating motor fixedly arranged on one side of the fixing base.
Further, fixed tank outer wall fixed mounting has the carrier, the carrier bottom is fixed with a plurality of support frames that are used for supporting the fixed tank, is fixed with the link between a plurality of support frames, fixing base fixed mounting is on the link.
Further, a cleaning mechanism is arranged on one side of the stirring tank and comprises a mounting seat, the mounting seat is fixedly arranged on one side of the top of the stirring tank, and a plurality of cleaning pipes communicated with the water tank are arranged on the mounting seat.
Further, the stirring tank bottom is provided with the discharging pipe, the discharging pipe runs through the fixed tank and sets up in the filtration jar top, all be provided with the control valve on discharging pipe and the two connecting pipes.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the silver nanowire is prepared by adopting the silver nanowire preparation machine, the cleaning mechanism arranged in the silver nanowire preparation machine is matched with the filtering mechanism, the cleaning mechanism cleans the interior of the stirring tank through deionized water while the filtering mechanism separates the precipitate in the mixed solution, so that the next silver nanowire preparation is convenient, the preparation efficiency of the silver nanowire is improved, and meanwhile, when the deionized water in the stirring tank is completely cleaned and discharged into the filtering tank of the filtering mechanism, the precipitate on the filtering tank can be washed, the soluble impurities on the surface of the precipitate are removed, so that the pure silver nanowire can be conveniently prepared, the preparation quality of the silver nanowire is improved, and meanwhile, the continuous production of the silver nanowire is convenient;
the rotatable filter tank on the filter mechanism is convenient for recovering the prepared silver nanowire, manual collection is not needed, the preparation process of the silver nanowire is simple, the cost is low, the silver nanowire prepared by the silver nanowire preparation machine is high in preparation efficiency and preparation quality, and the large-scale and continuous production of the silver nanowire is convenient.
Drawings
Fig. 1 is a schematic structural view of a silver nanowire manufacturing machine according to the present invention.
FIG. 2 is a schematic view of the structure of the inside of the stirring tank in the present invention.
FIG. 3 is a schematic diagram of a filtering mechanism according to the present invention.
Fig. 4 is a schematic structural view of a cleaning mechanism in the present invention.
In the figure: 1. a stirring tank; 2. a fixed tank; 3. a stirring motor; 4. a stirring shaft; 5. stirring blades; 6. a filtering mechanism; 61. a filter tank; 62. a filter screen; 63. a rotating motor; 64. a fixing seat; 7. a cleaning mechanism; 71. a mounting base; 72. cleaning the tube; 8. a first feeding frame; 9. a first feeding box; 10. a second feeding frame; 11. a second feeding box; 12. a carrier; 13. a support frame; 14. a heating belt; 15. and a discharging pipe.
Detailed Description
The invention will be described in further detail with reference to the drawings and the detailed description. The embodiments of the invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
As shown with reference to figures 1-4,
example 1:
a method for preparing silver nanowires, comprising the following steps:
step one: 15 parts of water-soluble silver salt, 1.5 parts of dispersing agent, 100 parts of aqueous solution A of polyhydroxy liquid organic matter and 15 parts of aqueous solution B of polyhydroxy liquid organic matter are weighed according to weight parts;
step two: adding an aqueous solution A of polyhydroxy liquid organic matters into a first feeding box 9 of a silver nanowire preparation machine, and adding water-soluble silver salt into the first feeding box 9 to obtain a water-soluble silver salt solution;
step three: adding an aqueous solution B of polyhydroxy liquid organic matters into a second feeding box 11 of the silver nanowire preparation machine, and adding a dispersing agent into the second feeding box 11 to obtain a dispersing agent solution;
step four: when the heating belt 14 heats and maintains the temperature of the stirring tank 1 to 150 ℃, a control valve on a connecting pipe of the first feeding box 9 and a connecting pipe of the second feeding box 11 is opened, the water-soluble silver salt solution and the dispersing agent solution fall into the stirring tank 1 through the connecting pipes respectively, meanwhile, a stirring motor 3 is started, an output shaft of the stirring motor 3 drives a stirring shaft 4 to rotate, the stirring shaft 4 drives a plurality of stirring blades 5 to rotate, and the stirring blades 5 stir the dispersing agent solution and the water-soluble silver salt solution in the stirring tank 1 to obtain a mixed solution;
step five: the control valve on the discharging pipe 15 is opened, the mixed solution falls into the filter tank 61 through the discharging pipe 15, the sediment in the mixed solution is filtered by the filter screen 62 and then is left on the surface of the filter screen 62, the liquid passes through the filter screen 62 and is discharged along the filter tank 61, deionized water is introduced into a plurality of cleaning pipes 72 on the mounting seat 71, the residual mixed solution in the stirring tank 1 is cleaned, meanwhile, cleaning water is discharged onto the filter tank 61, the sediment on the filter screen 62 is washed, the rotating motor 63 is started, the output shaft of the rotating motor 63 drives the filter tank 61 on the rotating shaft to rotate, the filter tank 61 is turned over, and the sediment on the filter screen 62 in the filter tank 61 is collected, so that silver nanowires are obtained.
Specifically, the water-soluble silver salt is one or more of silver nitrate, silver chlorate and silver acetate which are mixed in any proportion; the dispersing agent is polyvinylpyrrolidone; the aqueous solution A of the polyhydroxy liquid organic matter and the aqueous solution B of the polyhydroxy liquid organic matter are both formed by mixing the polyhydroxy liquid organic matter and water, and the volume ratio of the polyhydroxy liquid organic matter to the water in the aqueous solution A of the polyhydroxy liquid organic matter to the aqueous solution B of the polyhydroxy liquid organic matter is 1:3; the polyhydroxy liquid organic matter is one or more of glycol and glycerol mixed in any proportion; the stirring time in the fourth step is 30min.
Example 2:
a method for preparing silver nanowires, comprising the following steps:
step one: weighing 20 parts of water-soluble silver salt, 2.5 parts of dispersing agent, 150 parts of aqueous solution A of polyhydroxy liquid organic matter and 60 parts of aqueous solution B of polyhydroxy liquid organic matter according to parts by weight;
step two: adding an aqueous solution A of polyhydroxy liquid organic matters into a first feeding box 9 of a silver nanowire preparation machine, and adding water-soluble silver salt into the first feeding box 9 to obtain a water-soluble silver salt solution;
step three: adding an aqueous solution B of polyhydroxy liquid organic matters into a second feeding box 11 of the silver nanowire preparation machine, and adding a dispersing agent into the second feeding box 11 to obtain a dispersing agent solution;
step four: when the heating belt 14 heats and keeps the temperature of the stirring tank 1 to 250 ℃, a control valve on a connecting pipe of the first feeding box 9 and a connecting pipe of the second feeding box 11 is opened, the water-soluble silver salt solution and the dispersing agent solution fall into the stirring tank 1 through the connecting pipes respectively, meanwhile, a stirring motor 3 is started, an output shaft of the stirring motor 3 drives a stirring shaft 4 to rotate, the stirring shaft 4 drives a plurality of stirring blades 5 to rotate, and the stirring blades 5 stir the dispersing agent solution and the water-soluble silver salt solution in the stirring tank 1 to obtain mixed solution;
step five: the control valve on the discharging pipe 15 is opened, the mixed solution falls into the filter tank 61 through the discharging pipe 15, the sediment in the mixed solution is filtered by the filter screen 62 and then is left on the surface of the filter screen 62, the liquid passes through the filter screen 62 and is discharged along the filter tank 61, deionized water is introduced into a plurality of cleaning pipes 72 on the mounting seat 71, the residual mixed solution in the stirring tank 1 is cleaned, meanwhile, cleaning water is discharged onto the filter tank 61, the sediment on the filter screen 62 is washed, the rotating motor 63 is started, the output shaft of the rotating motor 63 drives the filter tank 61 on the rotating shaft to rotate, the filter tank 61 is turned over, and the sediment on the filter screen 62 in the filter tank 61 is collected, so that silver nanowires are obtained.
Specifically, the water-soluble silver salt is one or more of silver nitrate, silver chlorate and silver acetate which are mixed in any proportion; the dispersing agent is polyvinylpyrrolidone; the aqueous solution A of the polyhydroxy liquid organic matter and the aqueous solution B of the polyhydroxy liquid organic matter are both formed by mixing the polyhydroxy liquid organic matter and water, and the volume ratio of the polyhydroxy liquid organic matter to the water in the aqueous solution A of the polyhydroxy liquid organic matter to the aqueous solution B of the polyhydroxy liquid organic matter is 1:3; the polyhydroxy liquid organic matter is one or more of glycol and glycerol mixed in any proportion; the stirring time in the fourth step is 70min.
The silver nanowire preparation machine comprises a stirring tank 1, wherein the bottom of the stirring tank 1 is arranged in a fixed tank 2, the stirring tank 1 is fixedly arranged in the fixed tank 2 through a plurality of connecting rings, a gap is arranged between the fixed tank 2 and the stirring tank 1, the gap is filled with a plurality of heating belts 14 for heating the stirring tank 1, a bearing frame 12 is fixedly arranged on the outer wall of the fixed tank 2, a plurality of supporting frames 13 for supporting the fixed tank 2 are fixed at the bottom of the bearing frame 12, and a feeding pipe for feeding materials is arranged at the top of the stirring tank 1;
the stirring tank 1 is fixedly provided with a stirring motor 3, an output shaft of the stirring motor 3 is fixedly connected with the end part of a stirring shaft 4, the stirring shaft 4 is rotatably arranged in the stirring tank 1, and a plurality of stirring blades 5 are fixedly arranged on the stirring shaft 4; when the stirring tank is used, the stirring motor 3 is started, the output shaft of the stirring motor 3 drives the stirring shaft 4 to rotate, the stirring shaft 4 drives the stirring blades 5 to rotate, and the stirring blades 5 stir the dispersing agent solution and the water-soluble silver salt solution in the stirring tank 1 to obtain mixed solution.
The agitator tank 1 one side is provided with wiper mechanism 7, wiper mechanism 7 includes mount pad 71, mount pad 71 fixed mounting is in agitator tank 1 top one side, be provided with a plurality of wash pipes 72 on the mount pad 71, a plurality of wash pipes 72 all communicate with external water tank through connecting line, the water tank passes through connecting line with deionized water and inputs to wash on the pipe 72, in the input agitator tank 1 through wash pipe 72, clean agitator tank 1 inside, the preparation of silver nanowire that makes things convenient for next time, when the deionized water that has cleaned agitator tank 1 discharges to filter tank 61 simultaneously, can wash the precipitate on the filter tank 61, get rid of the soluble impurity in precipitate surface, obtain pure silver nanowire, the preparation quality of silver nanowire has been improved.
The agitator tank 1 one side is provided with first material loading frame 8, is provided with first material loading case 9 on the first material loading frame 8, and agitator tank 1 opposite side is provided with second material loading frame 10, is provided with second material loading case 11 on the second material loading frame 10, and first material loading case 9 and second material loading case 11 communicate with agitator tank 1 top through the connecting pipe respectively, and agitator tank 1 bottom is provided with discharging pipe 15, and discharging pipe 15 runs through fixed tank 2 and sets up in filtering tank 61 top, all is provided with the control valve on discharging pipe 15 and the two connecting pipes.
The bottom of the stirring tank 1 is provided with a filtering mechanism 6, the filtering mechanism 6 comprises a filtering tank 61, a filter screen 62 for filtering sediment is arranged in the filtering tank 61, the filtering tank 61 is arranged above a fixed seat 64, two sides of the filtering tank 61 are fixedly provided with rotating shafts, the two rotating shafts are respectively and rotatably arranged on two sides of the fixed seat 64, one side of the fixed seat 64 is fixedly provided with a rotating motor 63, an output shaft of the rotating motor 63 is fixedly connected with one rotating shaft end part, a connecting frame is fixedly arranged between a plurality of supporting frames 13, and the fixed seat 64 is fixedly arranged on the connecting frame;
when the silver nanowire collecting device is used, the rotating motor 63 is started, the output shaft of the rotating motor 63 drives the filter tank 61 on the rotating shaft to rotate, so that the filter tank 61 is turned over, sediment on the filter screen 62 in the filter tank 61 can be collected, silver nanowires can be obtained, the rotatable filter tank 61 is convenient to recover the silver nanowires after preparation, manual collection is not needed, and the silver nanowire collecting device is convenient and quick; the preparation process of the silver nanowire is simple, the cost is low, the silver nanowire prepared by the silver nanowire preparation machine has high preparation efficiency and preparation quality, and the large-scale and continuous production of the silver nanowire is convenient.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (1)
1. A method for preparing silver nanowires, which is characterized by comprising the following steps:
step one: 15-20 parts of water-soluble silver salt, 1.5-2.5 parts of dispersing agent, 100-150 parts of aqueous solution A of polyhydroxy liquid organic matter and 15-60 parts of aqueous solution B of polyhydroxy liquid organic matter are weighed according to weight parts;
step two: adding an aqueous solution A of a polyhydroxy liquid organic matter into a first feeding box (9) of a silver nanowire preparation machine, and adding water-soluble silver salt into the first feeding box (9) to obtain a water-soluble silver salt solution;
step three: adding an aqueous solution B of a polyhydroxy liquid organic matter into a second feeding box (11) of the silver nanowire preparation machine, and adding a dispersing agent into the second feeding box (11) to obtain a dispersing agent solution;
step four: when the heating belt (14) heats and maintains the temperature of the stirring tank (1) to 150-250 ℃, a control valve on a connecting pipe of the first feeding box (9) and a connecting pipe of the second feeding box (11) is opened, the water-soluble silver salt solution and the dispersing agent solution fall into the stirring tank (1) through the connecting pipes respectively, meanwhile, an output shaft of the stirring motor (3) drives a plurality of stirring blades (5) to rotate through a stirring shaft (4), and the stirring blades (5) stir the dispersing agent solution and the water-soluble silver salt solution in the stirring tank (1) to obtain mixed solution;
step five: opening a control valve on a discharging pipe (15), enabling mixed liquid to fall into a filter tank (61) through the discharging pipe (15), filtering sediment in the mixed liquid through a filter screen (62), then, keeping on the surface of the filter screen (62), discharging liquid from the filter screen (62) along the filter tank (61), introducing deionized water into a plurality of cleaning pipes (72) on a mounting seat (71), cleaning the mixed liquid remained in the stirring tank (1), discharging cleaning water onto the filter tank (61), washing sediment on the filter screen (62), and rotating the filter tank (61) on a rotating shaft driven by an output shaft of a rotating motor (63), so that the filter tank (61) is turned over, and collecting sediment on the filter screen (62) in the filter tank (61), thus silver nanowires are obtained;
the water-soluble silver salt is one or more of silver nitrate, silver chlorate and silver acetate which are mixed in any proportion; the dispersing agent is polyvinylpyrrolidone;
the aqueous solution A of the polyhydroxy liquid organic matter and the aqueous solution B of the polyhydroxy liquid organic matter are both formed by mixing the polyhydroxy liquid organic matter and water, and the volume ratio of the polyhydroxy liquid organic matter to the water in the aqueous solution A of the polyhydroxy liquid organic matter to the aqueous solution B of the polyhydroxy liquid organic matter is 1:3;
the polyhydroxy liquid organic matter is one or more of glycol and glycerol which are mixed in any proportion;
the stirring time in the fourth step is 30min-70min;
the silver nanowire preparation machine comprises a stirring tank (1), wherein the bottom of the stirring tank (1) is arranged in a fixed tank (2), the stirring tank (1) is fixedly arranged in the fixed tank (2) through a plurality of connecting rings, a gap is formed between the fixed tank (2) and the stirring tank (1), a plurality of heating belts (14) for heating the stirring tank (1) are filled in the gap, a first feeding box (9) is arranged on a first feeding frame (8) arranged on one side of the stirring tank (1), a second feeding box (11) is arranged on a second feeding frame (10) arranged on the other side of the stirring tank (1), and the first feeding box (9) and the second feeding box (11) are respectively communicated with the top of the stirring tank (1) through connecting pipes;
an output shaft of a stirring motor (3) fixedly arranged at the top of the stirring tank (1) is fixedly connected with the end part of a stirring shaft (4), the stirring shaft (4) is rotatably arranged in the stirring tank (1), and a plurality of stirring blades (5) are fixedly arranged on the stirring shaft (4);
the stirring tank is characterized in that a filtering mechanism (6) is arranged at the bottom of the stirring tank (1), the filtering mechanism (6) comprises a filtering tank (61), a filter screen (62) for filtering sediment is arranged in the filtering tank (61), the filtering tank (61) is arranged above a fixed seat (64), rotating shafts fixedly arranged on two sides of the filtering tank (61) are respectively rotatably arranged on two sides of the fixed seat (64), and an output shaft of a rotating motor (63) fixedly arranged on one side of the fixed seat (64) is fixedly connected with one rotating shaft end part;
the outer wall of the fixed tank (2) is fixedly provided with a bearing frame (12), a plurality of supporting frames (13) for supporting the fixed tank (2) are fixed at the bottom of the bearing frame (12), connecting frames are fixed between the supporting frames (13), and the fixing seat (64) is fixedly arranged on the connecting frames;
a cleaning mechanism (7) is arranged on one side of the stirring tank (1), the cleaning mechanism (7) comprises a mounting seat (71), the mounting seat (71) is fixedly arranged on one side of the top of the stirring tank (1), and a plurality of cleaning pipes (72) communicated with the water tank are arranged on the mounting seat (71);
the stirring tank is characterized in that a discharging pipe (15) is arranged at the bottom of the stirring tank (1), the discharging pipe (15) penetrates through the fixed tank (2) and is arranged above the filtering tank (61), and control valves are arranged on the discharging pipe (15) and the two connecting pipes.
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