CN213135053U

CN213135053U - Silver nanowire preparation facilities based on thermal centrifugation method

Info

Publication number: CN213135053U
Application number: CN202021733472.5U
Authority: CN
Inventors: 刘松青
Original assignee: Shenzhen Jindasheng Chemical Co ltd
Current assignee: Shenzhen Jindasheng Chemical Co ltd
Priority date: 2020-08-19
Filing date: 2020-08-19
Publication date: 2021-05-07
Anticipated expiration: 2030-08-19

Abstract

The utility model relates to a silver nanowire preparation facilities based on hot centrifugation method, including raw materials storage container, reaction vessel, full-automatic centrifuge, mother liquor recovery jar, raw materials storage container and reaction vessel pass through the peristaltic pump and communicate, reaction vessel and full-automatic centrifuge feed inlet communicate, full-automatic centrifuge's liquid phase discharge gate and mother liquor recovery jar communicate, mother liquor recovery jar and raw materials storage container communicate; still include finished product collection device, finished product collection device is equipped with collection tank, baffle, the collection container of unloading, and full automatic centrifuge's solid phase discharge gate and finished product collection device intercommunication. Compared with the prior art, the device adopts a thermal centrifugation technology, can realize the recycling of the polyalcohol solvent in the process of preparing the silver nanowires by the polyalcohol method, and simultaneously obtains the silver nanowires with excellent quality; the device can be used for continuously producing the silver nanowires on line, the production period is shortened, the production cost is reduced, the operation is simple, the environment is protected, and the industrial application is easy.

Description

Silver nanowire preparation facilities based on thermal centrifugation method

Technical Field

The utility model belongs to the technical field of the nano-material preparation, concretely relates to silver nano-wire preparation facilities based on hot centrifugation method.

Background

The transparent electrode is indispensable in the fields of displays, touch screens, solar cells and the like, and the market demand is huge. The high-quality flexible transparent electrode is the key point for realizing the popularization and application of a new generation of folding screen mobile phone, future wearable equipment and the like.

Almost all transparent conductive materials currently used for transparent electrodes are Indium Tin Oxide (ITO), or Tin-doped Indium Oxide. However, ITO transparent electrodes have several disadvantages: (1) indium is expensive and has limited supply. The content of indium in earth crust is 1 × 10^-5% and relatively dispersed, and no over-rich ore has been found so far, but is present as an impurity in zinc and other metal ores. Indium is therefore classified as a rare metal. Worldwide indium reserves are estimated to be only 5 million tons, with 50% being recoverable. Because independent indium ores are not found, the industrial production of metallic indium by a method for purifying waste zinc and waste tin has a recovery rate of about 50-60%, and the indium actually obtained is only 1.5-1.6 ten thousand tons (which is not 1/50 of silver). This will certainly affect the stable supply of ITO transparent electrodes in the future. (2) The ITO film lacks flexibility and is difficult to apply to a flexible transparent electrode. An ITO film having a thickness of about 100 μm has an unbreakable limit radius of curvature of about 6 mm. Therefore, the ITO transparent electrode is liable to be broken when it is bent excessively. This is a fatal drawback for its application to flexible transparent electrodes of increasing importance. (3) The film is prepared by vacuum sputtering, the process cost is high, and certain requirements are imposed on the heat resistance of the substrate material, which limits the application of the flexible transparent electrode. Therefore, the development of the next generation transparent conductive material suitable for the flexible transparent electrode is urgently needed to replace the ITO.

At present, the alternative technologies of the ITO conductive glass mainly include graphene, conductive polymers, carbon nanotubes, metal grids, silver nanowires, and the like. Theoretically, the transmittance and the resistance of graphene are dominant, but due to the complex process, huge early investment is required in the aspects of equipment improvement, process optimization and the like, and the price is also very high. For a long time, the graphene does not have mass production conditions. The industrial mass production technology of carbon nanotubes is not perfect, and the conductivity of the prepared film product can not reach the level of the common ITO film. Conductive polymers also have the problem of insufficient conductivity and, because of aging problems, have a limited service life. For the metal grid scheme, in order to make the metal grid invisible to naked eyes, the metal line width is less than 5 microns, so that the process difficulty is high, and the cost is high; even if the line width is reduced to be less than 5 microns, the resolution is low due to the Morie interference problem, and the method is not suitable for high-resolution products such as smart phones and tablet computers. In summary, silver nanowire technology will be the most promising ITO alternative from the technological and marketing perspectives.

At present, silver nanowires also have their own problems, namely high price, which severely limits their development applications. In order to realize the popularization and application of the silver nanowire transparent electrode, the key is to prepare the high-quality silver nanowire in a large scale and at low cost. The preparation method of the silver nanowire is various, and comprises an ultraviolet radiation reduction method, a DNA template method, a mesoporous material template method, a hydrothermal synthesis method, a polyol method and the like. Among them, the polyol method has significant advantages over other methods: mild reaction conditions, high reaction speed, no need of additional templates, simple process and the like. In the traditional process of preparing silver nanowires by using a polyol method, the polyol solvent cannot be recycled, so that a large amount of waste liquid is formed, the production cost is increased, and the environment is polluted.

Therefore, it is necessary to design a new and efficient method for preparing silver nanowires in a recyclable manner.

SUMMERY OF THE UTILITY MODEL

The utility model aims to provide a: aiming at the defects of the prior art, the device for preparing the silver nanowires based on the thermal centrifugation method is provided, the device adopts the thermal centrifugation technology, can realize the recycling of the polyol solvent in the process of preparing the silver nanowires by the polyol method, and simultaneously obtains the silver nanowires with excellent quality.

In order to achieve the above purpose, the utility model adopts the following technical scheme:

a silver nanowire preparation device based on a thermal centrifugation method comprises a raw material storage container, a reaction container, a full-automatic centrifuge and a mother liquor recovery tank, wherein the raw material storage container is communicated with the reaction container through a peristaltic pump, the reaction container is communicated with a feed inlet of the full-automatic centrifuge, a liquid phase discharge outlet of the full-automatic centrifuge is communicated with the mother liquor recovery tank, and the mother liquor recovery tank is communicated with the raw material storage container;

the finished product collecting device is sequentially provided with a collecting tank, an unloading baffle and a collecting container from top to bottom, and a solid-phase discharge hole of the full-automatic centrifuge is communicated with the finished product collecting device to collect centrifuged solid-phase silver nanowires.

As an improvement of silver nano wire preparation facilities based on hot centrifugation method, raw materials storage container's the mouth of outflowing with be equipped with between reaction container's the influent stream mouth and be used for communicateing first connecting tube between them, reaction container's the mouth of outflowing with be equipped with between full-automatic centrifuge's the feed inlet and be used for communicateing second connecting tube between them, the mother liquor recovery jar with be equipped with between the raw materials storage container and be used for communicateing third connecting tube between them.

As an improvement of silver nanometer line preparation facilities based on hot centrifugation method, be equipped with on the first connecting line and be used for controlling its first ooff valve that switches on or cuts off and be used for controlling feed rate's peristaltic pump.

As an improvement of silver nanometer line preparation facilities based on hot centrifugation method, be equipped with the first water pump that is used for controlling its second ooff valve that switches on or cuts off and is used for driving the fluid motion on the second connecting line.

As an improvement of silver nanometer line preparation facilities based on hot centrifugation method, be equipped with the second water pump that is used for controlling its third ooff valve that switches on or cuts off and is used for driving the fluid motion in the third connecting line.

As an improvement of silver nano wire preparation facilities based on hot centrifugation method, be equipped with the agitator in the reaction vessel, be used for measuring the temperature sensor of its interior temperature and be used for maintaining reaction temperature's hot plate, the agitator comprises motor, (mixing) shaft, impeller triplex, the hot plate pastes on the reaction vessel inner wall.

As an improvement of silver nano wire preparation facilities based on hot centrifugation method, full automatic centrifuge is equipped with three interface, is feed inlet, liquid phase discharge gate, solid phase discharge gate respectively, full automatic centrifuge passes through the feed inlet will the solid-liquid mixture who contains silver nano wire and polyol solution after the reaction vessel reaction pours into full automatic centrifuge accomplishes the back at the centrifugation, through the solid phase discharge gate is with silver nano wire discharge, through polyol solution discharge is gone out to the liquid phase discharge gate.

As an improvement of silver nano wire preparation facilities based on hot centrifugation method, will through feed inlet closing means, liquid phase discharge gate closing means, solid phase discharge gate closing means full-automatic centrifuge seals in order to carry out the centrifugation.

As an improvement of silver nanometer line preparation facilities based on hot centrifugation, be equipped with the charge door in the raw materials storage container, the charge door is arranged in silver nanometer line production initial solution to add and the circulation in supplementary solution.

Compared with the prior art, the beneficial effects of the utility model include but are not limited to: the utility model discloses can realize the cyclic utilization of polyol solvent in the silver nano-wire technology of polyol method preparation, obtain the silver nano-wire of high quality simultaneously. The utility model discloses process flow is short, shortens production cycle, can realize automated production and mother liquor cyclic utilization, can reduction in production cost, easy operation, green, easily industrialization is used.

Drawings

Fig. 1 is a schematic structural diagram of the present invention.

Wherein: 1-a raw material storage container; 11-a feed inlet; 2-a reaction vessel; 21-a stirrer; 22-a temperature sensor; 23-heating plate; 3-full automatic centrifuge; 31-a feed inlet; 32-feed inlet closing means; 33-liquid phase discharge port; 34-liquid phase discharge port closing device; 35-solid phase discharge port; 36-solid phase discharge port closing device; 4-mother liquor recovery tank; 5-finished product collecting device; 51-a collection tank; 52-discharge baffles; 53-a collection vessel; 61-first connecting line; 62-a second connecting line; 63-a third connecting line; 7-a peristaltic pump; 81-a first water pump; 82-a second water pump; 91-a first on-off valve; 92-a second on-off valve; 93-third on-off valve.

Detailed Description

As used in the specification and in the claims, certain terms are used to refer to particular components. As one skilled in the art will appreciate, manufacturers may refer to a component by different names. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. "substantially" means within an acceptable error range, within which a person skilled in the art can solve the technical problem to substantially achieve the technical result.

In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", horizontal "and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.

In the present invention, unless otherwise expressly specified or limited, the terms "mounted," "connected," and "fixed" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood according to specific situations by those skilled in the art.

The present invention will be described in further detail with reference to the accompanying drawings, which are not intended to limit the present invention.

Referring to fig. 1, the utility model provides a silver nanowire preparation facilities based on thermal centrifugation method, including raw materials storage container 1, reaction vessel 2, full-automatic centrifuge 3, mother liquor recovery tank 4, raw materials storage container 1 communicates through peristaltic pump 7 with reaction vessel 2, reaction vessel 2 communicates with feed inlet 31 of full-automatic centrifuge 3, liquid phase discharge gate 33 and mother liquor recovery tank 4 of full-automatic centrifuge 3 communicate, mother liquor recovery tank 4 communicates with raw materials storage container 1;

the device is characterized by further comprising a finished product collecting device 5, wherein the finished product collecting device 5 is sequentially provided with a collecting tank 51, a discharging baffle 52 and a collecting container 53 from top to bottom, and a solid-phase discharge port 35 of the full-automatic centrifuge 3 is communicated with the finished product collecting device 5 to collect centrifuged solid-phase silver nanowires.

Further, a first connecting pipeline 61 for communicating the outflow port of the raw material storage container 1 and the inflow port of the reaction container 2 is arranged between the outflow port of the reaction container 2 and the feed inlet 31 of the full-automatic centrifuge 3, a second connecting pipeline 62 for communicating the outflow port of the reaction container 2 and the feed inlet 31 of the full-automatic centrifuge 3 is arranged between the outflow port of the reaction container 2 and the feed inlet 31 of the full-automatic centrifuge 3, and a third connecting pipeline 63 for communicating the outflow port of the mother liquid recovery tank 4 and the raw material storage container 1 is arranged.

Furthermore, the first connecting pipeline 61 is provided with a first switch valve 91 for controlling the conduction or the interruption of the first connecting pipeline and a peristaltic pump 7 for controlling the feeding speed.

Furthermore, a second switch valve 92 for controlling the connection or disconnection of the second connecting pipeline 62 and a first water pump 81 for driving the fluid to move are provided on the second connecting pipeline 62.

Further, a third on/off valve 93 for controlling the opening and closing of the third connecting pipeline 63 and a second water pump 82 for driving the movement of the fluid are provided in the third connecting pipeline 63.

Further, a stirrer 21, a temperature sensor 22 for measuring the internal temperature thereof, and a heating plate 23 for maintaining the reaction temperature are provided in the reaction vessel 2, the stirrer 21 is composed of a motor, a stirring shaft, and an impeller, and the heating plate 23 is attached to the inner wall of the reaction vessel 2. Specifically, the stirrer 21 is used for uniform mixing of raw materials and better shaping of silver nanowires during the reaction process, the temperature sensor 22 is used for feedback of temperature parameters in the reaction container 2 to the controller, and the heating plate 23 is used for providing a heat source required by the reaction and maintaining the reaction temperature.

Further, the full-automatic centrifuge 3 is used for solid-liquid phase separation in the reaction product, the full-automatic centrifuge 3 is provided with three interfaces, namely a feed inlet 31, a liquid phase discharge outlet 33 and a solid phase discharge outlet 35, the full-automatic centrifuge 3 injects a solid-liquid mixture containing silver nanowires and polyol solution after the reaction in the reaction container 2 into the full-automatic centrifuge 3 through the feed inlet 31, and after the centrifugation is completed, the silver nanowires are discharged through the solid phase discharge outlet 35, and the polyol solution is discharged through the liquid phase discharge outlet 33.

Further, the fully automatic centrifuge 3 is sealed by the inlet port closing device 32, the liquid phase outlet port closing device 34, and the solid phase outlet port closing device 36 to perform centrifugation. The sealing environment of the full-automatic centrifuge during operation can be realized by opening the feed inlet closing device 32, the liquid phase discharge outlet closing device 34 and the solid phase discharge outlet closing device 36.

Further, a feed inlet 11 is arranged in the raw material storage container 1, and the feed inlet 11 is used for adding the initial solution for silver nanowire production and replenishing the solution in circulation. The raw material storage container 1 is used for storing the raw material added through the feed port 11 and the hot filtered mother liquor.

Further, a stirring device can be added into the raw material storage container 1, so that the raw materials and the filtered mother liquor are uniformly mixed.

Further, a cleaning device and a heating element can be installed in the collecting tank 51 of the finished product collecting device 5, the cleaning device cleans the silver nanowires to remove the polyol solution and impurities, and the heating element can dry the silver nanowires.

Further, the full-automatic centrifuge 3 can have a heating function, and the thermal centrifugation can more effectively separate a solid-liquid mixture after reaction.

The utility model discloses a working process specifically as follows:

(1) sequentially filling polyol, silver nitrate, a surfactant and a polyol solution of a halide salt into the raw material storage container 1 through a feeding port 11, and filling the polyol solution into the reaction container 2 through a peristaltic pump 7;

(2) uniformly stirring the polyalcohol solution by a stirrer 21 to obtain a reaction solution, heating the reaction solution to 100-200 ℃ by using a heating plate 23 in the reaction container 2, and reacting for 40-120 min to form a solid-liquid mixture in which the silver nanowires and the mixed solution coexist;

(3) opening a second switch valve 92 and a first water pump 81, closing the feed inlet sealing device 32 to enable the full-automatic centrifuge 3 to feed materials, ensuring that a liquid phase discharge port 33 and a solid phase discharge port 35 of the full-automatic centrifuge 3 are in a sealed state, and filling the solid-liquid mixture after reaction into the full-automatic centrifuge 3;

(4) opening a second switch valve 92 and a first water pump 81, opening a feed inlet closing device 32, starting a full-automatic centrifuge 3, adjusting the temperature in the full-automatic centrifuge 3 to be about 100 ℃, operating at 10000 rpm for 15 minutes, then leading out a separated solid phase and a separated liquid phase, closing a liquid phase discharge outlet closing device 34, leading the liquid phase into a mother liquor recovery tank 4, opening a liquid phase discharge outlet closing device 34, closing a solid phase discharge outlet closing device 36, and leading the solid phase into a collection tank 51, wherein the solid-liquid separation operation is different due to different types and working modes of the full-automatic centrifuge 3;

(5) opening the solid-phase discharge port closing device 36, cleaning and drying the silver nanowires in the collection tank 51, opening the discharge baffle 52, and collecting the silver nanowire finished products into the collection container 53;

(6) opening the third on-off valve 93 and the second water pump 82, injecting the polyhydric alcohol solution in the mother liquor recovery tank 4 into the raw material storage container 1, and closing the third on-off valve 93 and the second water pump 82 after the injection is completed;

(7) replenishing a silver nitrate polyalcohol solution and a halide salt polyalcohol solution into the raw material storage container 1 through a feed inlet 11, and filling a newly replenished solution in the raw material storage container 1 and a filtered solution into the reaction container 2 through a peristaltic pump 7;

(8) and (4) repeating the steps (2) to (7) to realize the continuous production of the silver nanowires and the recycling of the polyhydric alcohol.

The inlet port closing means 32, the liquid phase outlet port closing means 34, and the solid phase outlet port closing means 36 are closed when opened, and are not closed when closed.

While the foregoing description shows and describes several preferred embodiments of the invention, it is to be understood, as noted above, that the invention is not limited to the forms disclosed herein, but is not intended to be exhaustive of other embodiments, and is capable of use in various other combinations, modifications, and environments and is capable of changes within the scope of the inventive concept as expressed above, or as otherwise known in the relevant art. But that modifications and variations may be effected by those skilled in the art without departing from the spirit and scope of the invention, which is to be limited only by the claims appended hereto.

Claims

1. A silver nanowire preparation device based on a thermal centrifugation method, which is characterized in that,

the device comprises a raw material storage container (1), a reaction container (2), a full-automatic centrifuge (3) and a mother liquor recovery tank (4), wherein the raw material storage container (1) is communicated with the reaction container (2) through a peristaltic pump (7), the reaction container (2) is communicated with a feed inlet (31) of the full-automatic centrifuge (3), a liquid phase discharge port (33) of the full-automatic centrifuge (3) is communicated with the mother liquor recovery tank (4), and the mother liquor recovery tank (4) is communicated with the raw material storage container (1);

the silver nanowire collection device is characterized by further comprising a finished product collection device (5), wherein the finished product collection device (5) is sequentially provided with a collection tank (51), a discharge baffle (52) and a collection container (53) from top to bottom, and a solid phase discharge hole (35) of the full-automatic centrifuge (3) is communicated with the finished product collection device (5) to collect centrifuged solid phase silver nanowires.

2. The silver nanowire preparation apparatus based on the thermal centrifugation method according to claim 1, wherein a first connecting pipeline (61) for communicating the outflow port of the raw material storage container (1) and the inflow port of the reaction container (2) is provided therebetween, a second connecting pipeline (62) for communicating the outflow port of the reaction container (2) and the feed port (31) of the fully automatic centrifuge (3) is provided therebetween, and a third connecting pipeline (63) for communicating the mother liquor recovery tank (4) and the raw material storage container (1) is provided therebetween.

3. The silver nanowire production apparatus based on the thermal centrifugation method according to claim 2, wherein the first connecting pipe (61) is provided with a first switch valve (91) for controlling the connection or disconnection thereof and a peristaltic pump (7) for controlling the feeding speed.

4. The silver nanowire preparation apparatus based on the thermal centrifugation method according to claim 2, wherein a second switch valve (92) for controlling the connection or disconnection of the second connection pipeline (62) and a first water pump (81) for driving the fluid to move are provided on the second connection pipeline.

5. The silver nanowire manufacturing apparatus based on the thermal centrifugation method according to claim 2, wherein a third on/off valve (93) for controlling the on/off of the third connecting pipeline (63) and a second water pump (82) for driving the fluid to move are provided in the third connecting pipeline (63).

6. The silver nanowire manufacturing apparatus based on the thermal centrifugation method as claimed in claim 1, wherein an agitator (21), a temperature sensor (22) for measuring the temperature therein and a heating plate (23) for maintaining the reaction temperature are provided in the reaction vessel (2), the agitator (21) is composed of a motor, an agitating shaft and an impeller, and the heating plate (23) is attached to the inner wall of the reaction vessel (2).

7. The silver nanowire preparation apparatus based on the thermal centrifugation method according to claim 1, wherein the full-automatic centrifuge (3) is provided with three ports, namely a feed inlet (31), a liquid phase discharge outlet (33) and a solid phase discharge outlet (35), the full-automatic centrifuge (3) injects the solid-liquid mixture containing the silver nanowires and the polyol solution after the reaction in the reaction container (2) into the full-automatic centrifuge (3) through the feed inlet (31), discharges the silver nanowires through the solid phase discharge outlet (35) after the centrifugation is completed, and discharges the polyol solution through the liquid phase discharge outlet (33).

8. The silver nanowire manufacturing apparatus based on the thermal centrifugation method according to claim 1, wherein the fully automatic centrifuge (3) is sealed for centrifugation by a feed inlet closing means (32), a liquid phase outlet closing means (34), and a solid phase outlet closing means (36).

9. The apparatus for preparing silver nanowires based on the thermal centrifugation method according to claim 1, wherein a feed port (11) is provided in the raw material storage container (1), and the feed port (11) is used for adding an initial solution for silver nanowire production and replenishing the solution in circulation.