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Preparation method of high-specific surface area micro-nano cerium dioxide

A high specific surface area, ceria technology, applied in the field of nanomaterial manufacturing, can solve the problems of high production equipment requirements, affecting product quality, difficult operation, etc., to achieve the effect of low production cost, easy operation, and pollution reduction

Inactive Publication Date: 2018-07-03
NEIJIANG NORMAL UNIV +1
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  • Abstract
  • Description
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Problems solved by technology

This method has simple process and less pollution, but consumes more energy and has higher temperature
[0009] Other methods, such as spray pyrolysis, prepare a high-concentration solution of cerium salt, atomize it in a pyrolysis tower at a certain flow rate through a spray nozzle, collect and roast it, and obtain cerium dioxide. This method has higher requirements for production equipment, and Empty shell particles are prone to appear, affecting product quality
[0010] Among the existing preparation methods, the liquid phase method is the main method. In the hydrothermal method, sol-gel method, precipitation method, etc., the ceria powder prepared by the hydrothermal method has high purity and good dispersibility. and other characteristics, but it needs to be carried out under high temperature and high pressure conditions, high energy consumption and difficult operation

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  • Preparation method of high-specific surface area micro-nano cerium dioxide

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preparation example Construction

[0026] The preparation method adopted in some embodiments of the present invention is as follows: take cerium carbonate and dissolve it in inorganic acid, add inorganic salt mineralizer, surfactant and hydrogen peroxide, stir to form cerium salt solution (A solution), weigh the precipitate Prepare a precipitant solution (B solution), drop B solution at a rate of 1-3mL / min into A solution with a stirring rate of 200-500r / min, stir at a constant temperature of 25-80°C for 0.5h-5h, and form cerium salt Slurry, cerium salt slurry is hydrothermally reacted at 80-95°C for 2h-24h, centrifugally washed, oven-dried, ground, then roasted at 200-600°C for 1-3h, cooled to obtain nano cerium dioxide.

[0027] More preferably, the preparation method adopted in other embodiments of the present invention is as follows: weigh cerium carbonate and dissolve it in inorganic acid, weigh mineralizer and add it to the solution for dissolution, add hydrogen peroxide, and stir to form a cerium salt sol...

Embodiment 1

[0030]Weigh 18.2g of cerium carbonate, dissolve it in 14mL of concentrated nitric acid, add water to dilute to 50mL, and prepare a 1.6mol / L cerium nitrate solution, weigh 2.6g of potassium sulfate and add to the solution to dissolve, add 5mL of hydrogen peroxide, and stir for 5min to obtain (A liquid ), measure 16mL ammonia water and add 34mL aqueous solution containing 13.5g urea (B liquid), weigh 0.1g of cetyltrimethylammonium bromide and dissolve it in 88mL ethanol solution (C liquid), mix A liquid and B liquid At a rate of 3mL / min, drop it into liquid C with a stirring rate of 450r / min at the same time, and stir at 25°C for 30min to form a cerium salt slurry. The cerium salt slurry is hydrothermally reacted at 95°C for 4h, centrifugally washed, and dried in an oven. Drying, grinding, calcination in air at 500°C for 2 hours, and cooling to obtain nano-cerium dioxide. Specific surface area up to 164m 2 / g, the particle size is about 180nm.

Embodiment 2

[0032] Weigh 11.4g of cerium carbonate and dissolve it in 10mL of concentrated nitric acid, add water to dilute to 100mL, weigh 0.9g of potassium chloride and add to the solution to dissolve, add 5mL of hydrogen peroxide to prepare a 0.5mol / L cerium nitrate solution (liquid A), measure Take 36mL of ammonia water and add water to dilute to 100mL (solution B), weigh 4g of sodium lauryl sulfate and add it to a mixed solution containing 40mL of water and 10mL of ethanol to dissolve (solution C), and mix liquid A and liquid B simultaneously at a rate of 3mL / min. Drop into liquid C with a stirring rate of 450r / min, stir at 25°C for 4h, undergo a hydrothermal reaction at 80°C for 4h, centrifugally wash, dry in an oven, grind, then roast in air at 300°C for 2h, and cool to obtain di Ceria. Specific surface area up to 172m 2 / g, the particle size is about 100nm.

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Abstract

The invention discloses a preparation method of high-specific surface area micro-nano cerium dioxide. The preparation method comprises the steps of preparing a cerium-containing inorganic acid solution, adding an inorganic salt mineralization agent, a surfactant and hydrogen peroxide, stirring to obtain a cerium salt solution, dropwise adding a precipitator solution into the cerium salt solution,stirring at constant temperature to form cerium salt slurry, reacting by virtue of the cerium salt slurry at 80-95 DEG C for 2-24 hours, carrying out centrifugal washing, drying by virtue of a dryingtank, adequately grinding the dried material, and carrying out high-temperature roasting, so as to obtain high-specific surface area micro-nano cerium dioxide. Compared with a traditional hydrothermalmethod, the method disclosed by the invention has the advantages that the reaction temperature is low, the conditions are mild, the operation is easy, prepared micro-nano cerium dioxide is high in specific surface area and small in particle size, and the industrial production is relatively easily realized.

Description

technical field [0001] The invention belongs to the field of nanomaterial manufacturing, and in particular relates to a method for preparing micro-nano ceria with a high specific surface area. Background technique [0002] Cerium dioxide is widely used as a functional material due to its excellent redox ability. Cerium dioxide has been widely used in the fields of catalysis, polishing and energy conversion. The nanostructure of ceria greatly improves the redox ability of ceria, and with the development of human science and technology, the demand for nano ceria is increasing. For example, cerium oxide as a polishing agent, as people have higher and higher requirements for the size of silicon electronic devices, the distance between the components is getting smaller and smaller, which requires more and more size requirements for cerium oxide as a polishing agent. Come higher. Therefore, the preparation of nano ceria with high reactivity and catalytic efficiency is the direct...

Claims

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Application Information

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IPC IPC(8): C01F17/00B82Y40/00
CPCB82Y40/00C01F17/206C01P2004/62C01P2006/12
Inventor 郑小刚康富彦周艳娇王福海刘敏曹锟张金洋付孝锦刘勇
Owner NEIJIANG NORMAL UNIV
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