Method for preparing and separating silver nanowires under normal pressure in large scale
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A silver nanowire, large-scale technology, applied in the direction of nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve the problems of nanomaterial agglomeration, limited production capacity, etc., to avoid damage, reduce costs, avoid The effect of pretreatment on spoilage
Active Publication Date: 2017-12-19
NANJING UNIV OF POSTS & TELECOMM
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This scheme uses a microwave oven as a heating device, which greatly limits the production capacity of a single batch, and adopts a centrifugal-drying process, which is ver
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Embodiment 1
[0033] A method for preparing and separating silver nanowires under normal pressure on a large scale, comprising the following steps:
[0034] Step 1: Add 0.0963g of ammonium chloride to 1,000ml of 1,2-propanediol, heat to 80°C and stir for 1 hour to dissolve, then cool to obtain an ammonium chloride / 1,2-propanediol solution for use. Mix 3,000ml of propylene glycol, 68g of PVP, 800ml of Add the ammonium chloride / 1,2-propanediol solution into a 50L glass reactor with a reflux condensing device, stir and raise the temperature to 160°C to obtain the first mixture;
[0035] Step 2, in a quartz glass grinder, add 54g of silver nitrate crystals to 70ml of 1,2-propanediol for rapid grinding, and when no silver nitrate crystals are observed in the grinder, quickly transfer the silver nitrate suspension to the high position of the reaction kettle tank and ready to be added dropwise to the first mixture in the reactor, the first drop rate is 1 drop / second, when the suspension in the rea...
Embodiment 2
[0038] Step 1: Add 0.12 g of ammonium chloride to 1.2 kg of 1,2-propanediol, heat to 100°C and stir for 20 minutes to dissolve, then cool to obtain an ammonium chloride / 1,2-propanediol solution for use;
[0039] Add 5.5 kg of propylene glycol, 80 g of PVP, and 1.2 kg of ammonium chloride / 1,2-propylene glycol solution into a 50 L glass reactor with a reflux condensing device, stir and raise the temperature to 140°C to obtain the first mixture;
[0040] Step 2, in a quartz glass grinder, add 82g of silver nitrate to 0.09 kg of 1,2-propanediol for rapid grinding, and when no silver nitrate crystals are observed in the grinder, quickly transfer the suspension of silver nitrate to the high position of the reaction kettle tank and ready to be added dropwise to the first mixture in the reactor, the first drop rate is 1 drop / second, when the suspension in the reactor gradually turns dark brown, and gradually becomes black and opaque as the crystal seeds increase, the crystal Seed grow...
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Abstract
The invention discloses a method for preparing and separating silver nanowires under normal pressure in a large scale. Firstly, a crystal type control agent is prepared into a solution, then the solution of the crystal type control agent, polyvinylpyrrolidone and polyhydric alcohol are taken and added into a reaction kettle to be stirred and subjected to temperature rise, and a first mixture is obtained, wherein with silver nitrate crystals as reference, the mass ratio of the crystal type control agent, the polyvinylpyrrolidone and the polyhydric alcohol in the reaction kettle is (5*10<-4>-2*10<-3>): (0.7-1.4): (50-100); the silver nitrate crystals are dispersed to obtain a silver nitrate/polyatomic alcohol solution which is added into the first mixture in three times, and after heat preserving, cooling is performed till normal temperature is achieved so that a second mixture can be obtained; and absolute ethyl alcohol with the volume being 3-6 times of the volume of the second mixture then is added in, after stirring, the second mixture and the absolute ethyl alcohol are transferred into a settling tank, by setting the height of the settling tank, standing separation is performed in a manner that both ends are broken off, and a material of the settling tank is not soluble with the silver nanowires. The preparation method is simple, and the obtained silver nanowires are good in dispersing performance and wide in application range.
Description
technical field [0001] The invention belongs to the field of preparation of silver nanowires, in particular to a method for preparing and separating silver nanowires under normal pressure on a large scale. Background technique [0002] Silver nanowire is a material in the nanometer range in at least one dimension. It has excellent optical / electrical / chemical properties. It can be used to prepare flexible transparent electrodes to replace ITO conductive glass, and can also be used for catalysis, etc., but No large-scale preparation method of silver nanowires has been disclosed in the current large-scale synthesis. [0003] Application No. 201610420466.6, titled a method for macro-preparation of monodisperse silver nanowires, specifically discloses that the method includes the following steps: 1) Silver salt, surfactant and reducing polyol solution according to 1: (0.2- 5): (0.4-50) mass ratio mixed to form a uniform reaction solution A; 2) To the reaction solution A, add a...
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