Method for preparing nanometer nickel powder by micro passage reaction vessel

A micro-channel reactor, nano-nickel powder technology, applied in the fields of nanotechnology, nanotechnology, nanotechnology for materials and surface science, can solve the problems of low intermittent production efficiency, microchannel blockage, etc., and achieve low cost of raw materials , The particle size distribution is narrow, and the effect of subsequent separation processing is convenient

Inactive Publication Date: 2010-08-18
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the shortcoming of low intermittent production efficiency, and utilize the flow form of the gas-liquid two-phase block flow formed by the partial vaporization of the solvent to solve the problem of particle blockage in the microchannel during the synthesis process, and provide a A kind of method utilizing microchannel reactor to prepare nano-nickel powder

Method used

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  • Method for preparing nanometer nickel powder by micro passage reaction vessel
  • Method for preparing nanometer nickel powder by micro passage reaction vessel
  • Method for preparing nanometer nickel powder by micro passage reaction vessel

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Dissolve 4.75g of nickel chloride in 50ml of ethanol to configure liquid A, add 4.71g of hydrazine hydrate and 3.2g of sodium hydroxide to 50ml of ethanol to configure liquid B, and inject liquid A and liquid B through a pump at a temperature of 70°C and a channel diameter of 100μm Mix in a micro-mixer (purchased from German IMM company), and after staying for 60ms, the feed liquid is directly injected into a microchannel reactor (purchased from Nanjing Wanqing Industrial Co., Ltd.) with a reaction temperature of 70 ° C and an inner diameter of 2 mm and stays for 3.5 minutes for reaction. , the product was collected, and the product was separated by centrifugation, washed to pH = 7, and stored in isolation from air. The XRD characterization shows that the product is nickel metal, and the nano-nickel average particle diameter obtained is 73nm, and the X-ray diffraction pattern (XRD) of the sample of this sample is as follows figure 2 Shown, TEM image see image 3 shown...

Embodiment 2

[0024] Dissolve 9.51g of nickel chloride in 100ml of ethanol to configure liquid A, add 8.83g of hydrazine hydrate and 6g of sodium hydroxide to 100ml of ethanol to configure liquid B, and inject liquid A and liquid B through a pump at a temperature of 70°C and a channel diameter of 100μm Mixed in a micro-mixer (purchased from IMM Company of Germany), after staying for 80ms, the feed liquid was directly injected into a microchannel reactor (purchased from Nanjing Wanqing Industrial Co., Ltd.) with a reaction temperature of 70 ° C and an internal diameter of 2 mm to react for 5 minutes. The products were collected, and the products were separated by centrifugation, washed to pH=6.5, and the obtained samples were kept in air isolation. The XRD characterization shows that the sample is nickel metal, and the average particle size of the obtained nano-nickel is 65nm. The FESEM figure of the sample is shown in Figure 4 shown.

Embodiment 3

[0026] Dissolve 2.08g of nickel chloride in 50ml of ethanol to configure liquid A, add 4.12g of hydrazine hydrate and 2.8g of sodium hydroxide to 50ml of ethanol to configure liquid B, and inject liquid A and liquid B through a pump at a temperature of 68°C. The channel diameter is Mix in a 50 μm micro-mixer (purchased from German IMM Company), and the feed liquid after staying for 50 ms is directly injected into a microchannel reactor (purchased from Nanjing Wanqing Industrial Company) with a reaction temperature of 68 ° C and an inner diameter of 2 mm (purchased from Nanjing Wanqing Industrial Company) for 4 min. React and collect the products, and the products are separated by centrifugation, washed to pH=6.5, and the obtained samples are kept in air isolation. The XRD characterization showed that the sample was nickel metal, and the average particle size of the obtained nano-nickel was 45nm.

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Abstract

The invention relates to a method for preparing nanometer nickel powder by a micro passage reaction vessel, which comprises the following steps: preparing a soluble nickel salt alcoholic solution and an alkaliferous hydrazine hydrate alcoholic solution; injecting the two solutions into a micro passage mixer to be mixed according to the mol rate requirements of the hydrazine hydrate / nickel; directly injecting the mixed material solutions into the micro passage reaction vessel for reaction; and storing products in an air insulation mode respectively through separation and washing. Through adopting solvents for partial vaporization to form a flowing form of gas phase and liquid phase section flows, the method can solve the problem of blockage of the micro passage reaction vessel in the process of synthesizing the nanometer granules, the continuous synthesis of the nanometer nickel granules is realized, in addition, the preparation process does not need the addition of any surface active agents such as dispersing agents and the like, the cost of raw materials is low, the operation is simple, and the synthesized nanometer nickel granules have the characteristics of uniform granule size, good dispersivity and the like.

Description

technical field [0001] The invention relates to a preparation method for preparing nanometer nickel powder, in particular to a method for continuously preparing nanometer nickel powder through a microchannel reactor. Background technique [0002] Nanomaterials are currently one of the most active research fields. Due to their unique physical and chemical properties, nano-nickel has been widely used in many fields such as catalysts, battery materials, magnetic materials, and nano-coating materials. [0003] At present, the preparation methods of nano-nickel mainly include carboxyl thermal decomposition method, evaporation condensation method, physical preparation method, hydrothermal method, electrolysis method, mechanical pulverization method, microemulsion method and chemical reduction method. Among these preparation methods, the liquid-phase chemical reduction method has become the focus of researchers because of its advantages such as simple process, easy operation, and u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/054
CPCB22F9/24B22F2998/00B22F1/0018B82Y30/00B22F2303/01B22F2301/15
Inventor 张利雄张钰王重庆董利徐南平
Owner NANJING UNIV OF TECH
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