A continuous preparation method and device for nano-silver wire

A nano-silver wire and filtering device technology, applied in nanotechnology and other directions, can solve problems such as unfavorable industrial production, many steps required, harsh reaction conditions, etc., and achieve convenient production or basic research, simple and feasible steps, and safe and simple equipment. Effect

Active Publication Date: 2017-01-18
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese patent CN102689018A discloses a production method for synthesizing nano-silver wire material. The process of this method is simple and equipped with a reverse osmosis membrane filter device, which greatly simplifies the extraction steps of nano-silver wire, and the size of nano-silver wire is single; but in this method The pore size of the ceramic membrane is not large, and some silver wires may not be filtered out, resulting in loss
Chinese patent CN102259190A discloses a method for rapidly and mass-preparing nano-silver wires with high aspect ratio. grow into silver wires; the disadvantage is that there are many steps involved in the reaction process, and the types of additives added are also relatively large.
And although the diameter of the nano-silver wire prepared by this method is controlled, it is found that the diameter is larger when the silver wire is longer, so the long wire is not conducive to obtaining a high aspect ratio.
Chinese patent CN102161102A discloses a method for preparing nano-silver wires by adding the inducer polyvinylpyrrolidone dropwise in two steps. However, the centrifugal purification treatment method is adopted in the later stage, which not only increases the cost of post-processing, but also the silver wire itself is easy to agglomerate. It is difficult to disperse after centrifugation, which will also cause the loss of product
However, most of them are batch-type preparations, which require many steps and many auxiliary technologies, and most of the preparation methods stay in the laboratory stage, which is not conducive to industrial production.
Some methods have harsh reaction conditions, take a long time, and the process is cumbersome, and it is difficult to meet the requirements for large-scale production of silver nanowires in industrial applications.

Method used

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  • A continuous preparation method and device for nano-silver wire

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Raw material premixing

[0038] According to the mass ratio of ethylene glycol: polyvinylpyrrolidone: silver nitrate is 1:0.024:0.018 to take materials; 2 liters (density is 1.111 g / ml) ethylene glycol, 80.00 grams of polyvinylpyrrolidone and 2.7 mg of sodium chloride from the feed Port 4 is put into the reaction kettle 5 with a capacity of 5 liters for mixing, and the stirrer 3 is started to stir and the temperature is raised to 160°C. At this time, the stirring speed is 180r / min, and the stirring time is 1h. Observe the color change of the solution (preliminary judgment of the degree of mixing) , to obtain liquid A; 1 liter of ethylene glycol and 60.00 grams of silver nitrate were stirred and dissolved, the stirring speed was 200r / min, and the stirring time was 1h, and liquid B was obtained for subsequent use; wherein the number average molecular weight of polyvinylpyrrolidone was 58000;

[0039] (2) Liquid phase reduction

[0040] Add liquid B obtained in step (...

Embodiment 2

[0048] (1) Raw material premixing

[0049] According to the mass ratio of ethylene glycol: polyvinylpyrrolidone: silver nitrate is 1:0.027:0.024. Put 2 liters (density 1.111 g / ml) of ethylene glycol, 90.00 g of polyvinylpyrrolidone and 3.6 mg of potassium chloride into a reactor with a capacity of 5 liters from the feed port and mix, stir and heat up to 160 ° C, then stir The speed is 180r / min, the stirring time is 1h, observe the color change of the solution (preliminary judgment of the degree of mixing), and obtain liquid A; stir and dissolve 1 liter of ethylene glycol and 80.00 grams of silver nitrate. The stirring speed is 200r / min, and the stirring time is 1h. Obtain liquid B; wherein the number average molecular weight of polyvinylpyrrolidone is 58000;

[0050] (2) Liquid phase reduction

[0051] Add liquid B obtained in step (1) dropwise from the feed port to liquid A obtained in step (1) at a constant speed (the drop rate is 0.6mL / s), keep the reaction temperature at...

Embodiment 3

[0059] (1) Raw material premixing

[0060] According to the mass ratio of ethylene glycol: polyvinylpyrrolidone: silver nitrate is 1:0.030:0.024 to take materials. Put 2 liters (density 1.111 g / ml) of ethylene glycol, 100.00 g of polyvinylpyrrolidone and 3.6 mg of ferric chloride into a reactor with a capacity of 5 liters from the feed port and mix, stir and heat up to 160 ° C, then stir The speed is 180r / min, the stirring time is 1h, observe the color change of the solution (preliminary judgment of the degree of mixing), and obtain liquid A; stir and dissolve 1 liter of ethylene glycol and 80.00 grams of silver nitrate. The stirring speed is 200r / min, and the stirring time is 1h. Obtain liquid B; wherein the number average molecular weight of polyvinylpyrrolidone is 58000;

[0061] (2) Liquid phase reduction

[0062] Add liquid B obtained in step (1) dropwise from the feed port to liquid A obtained in step (1) at a constant speed (the drop rate is 0.6mL / s), keep the reactio...

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Abstract

The invention discloses a continuous preparation method and a continuous preparation device for a nano-silver wire. The continuous preparation method comprises the following steps: adding polyvinylpyrrolidone, halide salt and ethylene glycol into a reactor to stir and mix, thereby obtaining a solution A; adding part of ethylene glycol and adding silver nitrate to stir and disperse, thereby preparing a solution B; adding the solution B into the solution A, continuously stirring, thereby obtaining a nano-silver wire original solution C; guiding out the solution C from the reactor, filtering, retaining the grown nano-silver wire through a filter net, returning filtrate into the reactor to continuously react, then repeatedly filtering for 2-4 times; getting out the filter net, eluting the nano-silver wire on the filter net, standing the precipitates, thereby obtaining the nano-silver wire. The continuous preparation method can be used for realizing continuous production, is low in production cost, simple and safe in equipment, and short in production period.

Description

technical field [0001] The invention belongs to the field of nano-silver wire production technology, and in particular relates to a continuous preparation method and device for nano-silver wire. Background technique [0002] Silver nanowires are one-dimensional nanomaterials with good mechanical properties, electrical properties, optical properties, magnetic properties, thermal properties and catalytic properties. They are widely used in microelectronics, metallurgy, electronics, national defense, catalysis and bioengineering, etc. At the same time, silver nanowires are also valued because of their small size, large specific surface area, and unique physical and chemical properties. From the perspective of electrical properties alone, it is well known that silver is the metal with the best electrical conductivity. Wu Haiping synthesized silver nanowires with an aspect ratio of 50-60, added them to the conductive adhesive, and carried out electrical and mechanical properties ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/24B82Y40/00
Inventor 胡继文吴丹罗洪盛齐键邹海良
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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