CN114029500A - Nano silver wire apparatus for producing suitable for hundred kilograms are grades - Google Patents
Nano silver wire apparatus for producing suitable for hundred kilograms are grades Download PDFInfo
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- CN114029500A CN114029500A CN202111318508.2A CN202111318508A CN114029500A CN 114029500 A CN114029500 A CN 114029500A CN 202111318508 A CN202111318508 A CN 202111318508A CN 114029500 A CN114029500 A CN 114029500A
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- Prior art keywords
- liquid
- hundred kilograms
- heating
- pipeline
- silver nanowire
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 43
- 238000010438 heat treatment Methods 0.000 claims abstract description 39
- 238000004519 manufacturing process Methods 0.000 claims abstract description 19
- 239000002042 Silver nanowire Substances 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 12
- 238000002347 injection Methods 0.000 claims abstract description 11
- 239000007924 injection Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000011084 recovery Methods 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 3
- 238000004064 recycling Methods 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 238000004804 winding Methods 0.000 claims 1
- 239000002243 precursor Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 2
- 229920006362 Teflon® Polymers 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000011020 pilot scale process Methods 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000005406 washing Methods 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
- 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
- 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
Abstract
The invention discloses a silver nanowire production device suitable for hundred kilogram level, which comprises a storage tank, a propeller, a liquid mixer, a liquid distributor, a liquid drop generator, a heating device and a cooling recovery device which are sequentially connected through a pipeline; the propeller pushes the solution in the storage tank to the liquid mixer for mixing, the mixed solution is divided into a plurality of strands of solutions by the liquid separator, then flows to the liquid drop generator, is heated by the heating device for reaction, and finally is collected by the cooling and recycling device; the drop generator is additionally and independently connected with a branch, is propelled by the injection pump and is merged with the main channel at the drop generator. The invention realizes that the daily output of the nano silver wire reaches hundreds of kilograms, and realizes the large-scale mass production of the nano silver wire.
Description
Technical Field
The invention belongs to the field of synthesis of nano materials, and particularly relates to a production device of a silver nanowire suitable for hundred kilogram level.
Background
At present, the touch screen is still made of ITO transparent conductive materials, but with the rise of flexible foldable mobile phones and education integrated machines, the defects of height prevention, brittleness prevention and the like of ITO are undoubtedly avoided, and the touch screen cannot keep pace with emerging markets.
The silver nanowires are considered as the best alternative material for ITO due to their low cost and high electrical conductivity, but the way of industrialization is extremely difficult, and one of the major problems is that the silver nanowires cannot be industrially prepared on a large scale. The reason is that the traditional nano silver wire production still adopts the kettle type reaction to prepare, and has the problems of low yield, large batch reaction error, no scale amplification and the like.
The synthesis of the nano silver wire and the continuous flow reaction are combined, so that the problems of low yield, large batch error and the like in the kettle type reaction are effectively solved. On the basis of laboratory lab bench test parameters, how to further amplify the pilot test is a problem to be solved.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a silver nanowire production device which can improve productivity and reduce cost and is suitable for hundred kilogram levels.
The technical scheme is as follows: the invention comprises a storage tank, a propeller, a liquid mixer, a liquid distributor, a liquid drop generator, a heating device and a cooling recovery device which are connected in sequence through pipelines; wherein, the number of the storage tanks and the propellers is a plurality; the propeller pushes the solution in the storage tank to the liquid mixer for mixing, the mixed solution is divided into a plurality of strands of solutions by the liquid separator, then flows to the liquid drop generator, is heated by the heating device for reaction, and finally is collected by the cooling and recycling device; the drop generator is additionally and independently connected with a branch, is propelled by the injection pump and is merged with the main channel at the drop generator.
The heating device comprises a heating column, a plurality of heating pipes are wound on the inner wall of the heating column, and an insulating layer is wrapped on the outer wall of the heating column.
Dimethyl silicone oil is filled between the heating column and the insulating layer to keep the local temperature constant.
Each outlet of the liquid separator is connected with one pressure reducing channel, and the inner diameter of the pressure reducing channel is 10-20 mm.
The injection pump is filled with water phase solution which has boiling point lower than 120 ℃ and can be mixed with glycol.
And the liquid outlet of the injection pump and the liquid outlet of the heating device are respectively provided with a flow divider.
The storage tank is made of high-molecular polymer plastics.
The pipeline is a polytetrafluoroethylene pipeline, a quartz glass pipeline or a silicon carbide pipeline.
The inner diameter of the heating pipe is 4-10 mm, and the inner diameter of a pipeline between the liquid mixer and the liquid distributor is 20-30 mm.
The propelling speeds of the plurality of propellers are kept consistent and are all 30-60 mL/min.
Has the advantages that: compared with the prior art, the invention has the beneficial effects that: (1) the scale mass production capacity of the nano silver wire is increased by one hundred times, the unit daily output reaches one hundred kilograms, and the effects of improving the quality and reducing the cost are achieved; (2) compared with the traditional pilot scale production line, the pilot scale production line has the advantages that the number of the current-carrying phase circulating devices is reduced, and the device cost is reduced.
Drawings
FIG. 1 is a schematic structural view of the present invention;
fig. 2 is an SEM image of the nano silver wire manufactured by using the nano silver wire manufacturing apparatus of the present invention.
Detailed Description
The technical scheme of the invention is described in detail in the following with the combination of the detailed description and the attached drawings.
As shown in fig. 1, the present invention includes a storage tank 1, a propeller 2, a liquid mixer 3, a dispenser 4, a droplet generator 5, a heating device 6, and a cooling recovery device 11, which are connected in sequence via a pipe 9. Wherein, the quantity of storage tank 1, propeller 2 is two, inserts the input port of liquid mixer 3 after every storage tank is connected with corresponding propeller. The storage tank 1 is made of high molecular polymer plastics, such as polytetrafluoroethylene, polyethylene, polypropylene, polystyrene, butyl rubber, styrene butadiene rubber, silicon rubber, epoxy resin and the like. The storage tank cannot be a stainless steel or metal storage tank. The speeds of the two propellers are kept consistent and are both 30mL/min to 60 mL/min. Each outlet of the liquid separator 4 is connected with a pressure reduction channel 8. The liquid drop generator 5 is additionally and independently connected with a branch, is propelled by the injection pump 7, is divided into five strands through the flow divider 10, and is converged with the main pipeline at the liquid drop generator 5. The syringe pump 7 contains an aqueous solution having a boiling point below 120 ℃ and being miscible with ethylene glycol, preferably deionized water and an ethanol solution. The pushing speed of the injection pump 7 is only one hundred and fifty times of that of the propeller 2 and is 200-400 uL/min. The liquid outlet of the injection pump 7 and the liquid outlet of the heating device 6 are respectively provided with a flow divider 10. The pipe 9 is a teflon pipe, a quartz glass pipe or a silicon carbide pipe, preferably a teflon pipe, which cannot be made of metal or stainless steel. The cooling recovery device 11 is used as a rapid cooling region, and an ice water bath is selected. The storage tank 1 is connected with the propeller 2, precursor solution flows through the liquid mixer 3 in the storage tank 1 under the action of the propeller 2 and is uniformly mixed and then divided into five strands in the liquid distributor 4, the five strands enter the heating device 6 through the pressure reduction channel 8 and the liquid drop generator 5 to react, and the five strands are collected together through the flow divider 10 after the reaction is finished.
The heating device 6 specifically comprises a heating column 61, heating pipes 62 and an insulating layer 63, five heating pipes 62 are wound on the inner wall of the heating column 61, and the heating pipes 62 can keep constant temperature reaction; the outer wall of the heating column 61 is covered by an insulating layer 63 for protection. Dimethyl silicone oil is filled between the heating column 61 and the insulating layer 63 for keeping local temperature constant, and after heating is finished, the heating column can be quickly cooled by using dimethyl silicone oil circulation heat exchange, and the reaction is stopped. The heating pipe 62 has an inner diameter of 4 mm to 10 mm and a length of 50 m to 100 m; the inner diameter of the pipeline between the liquid mixer 3 and the liquid distributor 4 is 20 mm-30 mm; the inner diameter of the pipeline of the pressure reduction channel 8 is 10 mm-20 mm; the inner diameters of the rest pipelines are 4 mm-10 mm; preferably, the heating zone pipe has an inner diameter of 6 mm and a length of 80 m; the inner diameter of the pipeline between the mixed gas and the liquid separator is 30 mm; the inner diameter of the pressure reduction channel is 12 mm, and the inner diameters of the rest channels are 6 mm.
After the device is installed, preparing nano silver wire precursor solutions, respectively placing the nano silver wire precursor solutions in two storage tanks 1, starting the device, when the temperature of a heating zone of a heating device 6 reaches 160 ℃, setting the flow rates of two propellers at 45mL/min and setting the flow rate of an injection pump at 300uL/min, collecting a product in a product collecting zone after about 60 minutes, and obtaining a nano silver wire product through centrifugal washing. The microscopic morphology is shown in figure 2, and through the design of the device, the daily output of the nano silver wire reaches hundreds of kilograms, and the large-scale mass production of the nano silver wire is realized.
Claims (10)
1. The utility model provides a nanometer silver line apparatus for producing suitable for hundred kilograms are grades which characterized in that: comprises a storage tank (1), a propeller (2), a liquid mixer (3), a liquid distributor (4), a liquid drop generator (5), a heating device (6) and a cooling recovery device (11) which are connected in sequence through a pipeline (9); wherein, the number of the storage tanks (1) and the propellers (2) is a plurality;
the solution in the storage tank (1) is pushed to the liquid mixer (3) by the propeller (2) to be mixed, the mixed solution is divided into a plurality of strands of solutions by the liquid distributor (4), then flows to the liquid drop generator (5), is heated by the heating device (5) for reaction, and finally is collected by the cooling and recycling device (11); the liquid drop generator (5) is additionally and independently connected with a branch, is propelled by the injection pump (7) and is merged with the main channel at the liquid drop generator (5).
2. The silver nanowire production device suitable for hundred kilograms according to claim 1, which is characterized in that: heating device (6) are including heating post (61), and many heating pipes (62) of heating post (61) inner wall winding, heating post (61) outer wall parcel insulating layer (63).
3. The silver nanowire production device suitable for hundred kilograms according to claim 2, which is characterized in that: dimethyl silicone oil is filled between the heating column (61) and the insulating layer (63) to keep the local temperature constant.
4. The silver nanowire production device suitable for hundred kilograms according to claim 1, which is characterized in that: each outlet of the liquid separator (4) is connected with one pressure reducing channel (8), and the inner diameter of the pipeline of the pressure reducing channel (8) is 10-20 mm.
5. The silver nanowire production device suitable for hundred kilograms according to claim 1, which is characterized in that: the injection pump (7) is filled with water phase solution which has boiling point lower than 120 ℃ and can be mixed with glycol.
6. The silver nanowire production device suitable for hundred kilograms according to claim 1, which is characterized in that: and a flow divider (10) is respectively arranged at the liquid outlet of the injection pump (7) and the liquid outlet of the heating device (6).
7. The silver nanowire production device suitable for hundred kilograms according to claim 1, which is characterized in that: the storage tank (1) is made of high-molecular polymer plastics.
8. The silver nanowire production device suitable for hundred kilograms according to claim 1, which is characterized in that: the pipeline (9) is a polytetrafluoroethylene pipeline, a quartz glass pipeline or a silicon carbide pipeline.
9. The silver nanowire production device suitable for hundred kilograms according to claim 2, which is characterized in that: the inner diameter of the heating pipe (62) is 4-10 mm, and the inner diameter of a pipeline between the liquid mixer (3) and the liquid distributor (4) is 20-30 mm.
10. The silver nanowire production device suitable for hundred kilograms according to claim 1, which is characterized in that: the propelling speeds of the plurality of propellers (2) are kept consistent and are all 30 mL/min-60 mL/min.
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CN202111318508.2A CN114029500B (en) | 2021-11-09 | 2021-11-09 | Production device and production method of silver nanowires suitable for hundred kilogram level |
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CN202111318508.2A CN114029500B (en) | 2021-11-09 | 2021-11-09 | Production device and production method of silver nanowires suitable for hundred kilogram level |
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CN114029500A true CN114029500A (en) | 2022-02-11 |
CN114029500B CN114029500B (en) | 2023-01-06 |
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Cited By (1)
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CN114932231A (en) * | 2022-03-21 | 2022-08-23 | 苏州六材新材料科技有限公司 | Nano silver wire production device |
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