CN114029500B - Production device and production method of silver nanowires suitable for hundred kilogram level - Google Patents
Production device and production method of silver nanowires suitable for hundred kilogram level Download PDFInfo
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- CN114029500B CN114029500B CN202111318508.2A CN202111318508A CN114029500B CN 114029500 B CN114029500 B CN 114029500B CN 202111318508 A CN202111318508 A CN 202111318508A CN 114029500 B CN114029500 B CN 114029500B
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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
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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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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 silver nanowire production device suitable for hundred kilogram levels.
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 high resistance, brittleness and the like of ITO are undoubtedly prevented, 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 parameters, how to further amplify the pilot scale 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 kilograms.
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 sequentially connected 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 beneficial effects that: compared with the prior art, the invention has the beneficial effects that: (1) The mass production capacity of the nano silver wire is increased by one hundred times, the daily output per unit reaches one hundred kilograms, and the effects of improving quality and reducing cost are achieved; (2) Compared with the traditional pilot scale production line, the pilot scale production line has the advantages that the current-carrying phase circulating device is omitted, and the device cost is reduced.
Drawings
FIG. 1 is a schematic view of the structure 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 30 mL/min-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 uL/min-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 a pipeline between the liquid mixer 3 and the liquid distributor 4 is 20-30 mm; the inner diameter of the pipeline of the pressure reduction channel 8 is 10-20 mm; the inner diameters of the rest pipelines are 4-10 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 45 mL/min and setting the flow rate of an injection pump at 300 uL/min, collecting a product in a product collecting zone after about 60 minutes, and obtaining a nano silver wire product through centrifugal washing. The microcosmic topography 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 (7)
1. A production method of silver nanowires suitable for hundred kilogram levels is characterized by adopting the following production devices: 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 (6) 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 converged with the main trunk at the liquid drop generator (5);
deionized water and an ethanol solution which have boiling points lower than 120 ℃ and are miscible with ethylene glycol are filled in the injection pump (7);
the heating device (6) comprises a heating column (61), a plurality of heating pipes (62) are wound on the inner wall of the heating column (61), and an insulating layer (63) is wrapped on the outer wall of the heating column (61);
the inner diameter of the heating pipe (62) is 4-10 mm;
preparing nano silver wire precursor solutions, respectively placing the prepared nano silver wire precursor solutions in two storage tanks (1), starting the device, setting the flow rate of two propellers to be 45 mL/min when the temperature of a heating zone of a heating device (6) reaches 160 ℃, setting the flow rate of an injection pump (7) to be 300 uL/min, collecting a product in a product collecting zone after 60 minutes, and obtaining a nano silver wire product through centrifugal washing.
2. The method for producing silver nanowires applicable to the hundred kilogram level as claimed in claim 1, wherein: dimethyl silicone oil is filled between the heating column (61) and the insulating layer (63) to keep the local temperature constant.
3. The method for producing silver nanowires applicable to the hundred kilogram level as claimed in claim 1, wherein: 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.
4. The method for producing silver nanowires on a hundred kilogram scale according to claim 1, wherein the method comprises the following steps: and a liquid outlet of the injection pump (7) and a liquid outlet of the heating device (6) are respectively provided with a flow divider (10).
5. The method for producing silver nanowires on a hundred kilogram scale according to claim 1, wherein the method comprises the following steps: the storage tank (1) is made of high-molecular polymer plastics.
6. The method for producing silver nanowires applicable to the hundred kilogram level as claimed in claim 1, wherein: the pipeline (9) is a polytetrafluoroethylene pipeline, a quartz glass pipeline or a silicon carbide pipeline.
7. The method for producing silver nanowires applicable to the hundred kilogram level as claimed in claim 1, wherein: the inner diameter of a pipeline between the liquid mixer (3) and the liquid distributor (4) is 20-30 mm.
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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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| CN101957383A (en) * | 2010-08-10 | 2011-01-26 | 浙江大学 | Micro-fluid control liquid drop generation system based on liquid drop sequence assembly technology and use method |
| CN104741158B (en) * | 2015-04-03 | 2019-04-12 | 北京天天极因科技有限公司 | A kind of method and apparatus generating microlayer model using inertia force |
| CN106893109B (en) * | 2017-02-17 | 2020-12-01 | 中国石油大学(华东) | Continuous synthesis method of metal organic framework compound with stepped pore structure |
| CN107866577B (en) * | 2017-10-26 | 2020-05-12 | 北京科技大学 | Method for preparing monodisperse silver powder by instant micro-flow reactor |
| CN108927231B (en) * | 2018-07-17 | 2021-07-23 | 晋江精纯科技有限公司 | Multichannel liquid drop generation device and method based on macroporous perfusion microspheres |
| KR102164022B1 (en) * | 2018-11-23 | 2020-10-12 | 경희대학교 산학협력단 | Method for Synthesizing Nanoparticles Using Mircrodroplet-based Microfluidic Device Integrated with In-situ Quenching Zone |
| CN111014720A (en) * | 2019-12-27 | 2020-04-17 | 华北电力大学（保定） | Method and device for synthesizing nano silver on line |
| CN112024905A (en) * | 2020-07-08 | 2020-12-04 | 南京大学 | Method for large-scale synthesis of nano silver wire based on continuous flow technology |
| CN112126416A (en) * | 2020-10-14 | 2020-12-25 | 北京工业大学 | Microfluidic synthesis method and device for silver nanofluid |
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