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Nanometer zirconium dioxide with high specific surface area and preparation method thereof

A technology of nano zirconia and high specific surface area, which is applied in nanotechnology, zirconia, nanotechnology, etc. for materials and surface science, and can solve the unpublished primary particle size of zirconia, which is unfavorable for industrial production and preparation process cumbersome and other problems, to achieve the effect of eliminating post-processing, low cost, and simple post-processing

Inactive Publication Date: 2019-08-09
CHANGZHOU GEOQUIN NANO NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The patent application publication number CN108083334A discloses a preparation method of monodisperse spherical nano-zirconia powder, but the primary particle size obtained by this method is larger than 100nm, and it must be carried out under an inert gas. The process is more cumbersome and the cost increases
[0004] The application publication number is: CN108190950A patent discloses a preparation method and device of zirconium dioxide. This method must have a set of special devices, which is not conducive to industrial production, and the primary particle size of zirconium dioxide has not been announced.

Method used

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  • Nanometer zirconium dioxide with high specific surface area and preparation method thereof
  • Nanometer zirconium dioxide with high specific surface area and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0030] Weigh 1383.5g of zirconium oxychloride, add water to dilute to a concentration of 0.4mol / l, take 10.15L of the solution, add PEG20000-10g, the molar ratio of zirconium oxychloride to ammonia water is 1:3.5, take 1.1L of ammonia water, and dilute to 14.2L, positive sedimentation, dropping time 2h, after precipitation, add 2% sodium dodecylbenzenesulfonate, stir for 1h, age at room temperature for 2h, suction filter, wash with water, water temperature 60℃, wash until pH is about 7 , and then washed with 10L ethanol, baked at 90°C for 15 hours, burned at 500°C, kept for 2 hours, and sieved to obtain nano-zirconia.

[0031] After TEM detection, the primary particle size is: 10-30nm, the particles are uniformly dispersed, and the BET is 68m 2 / g.

[0032] figure 1 For the TEM figure of the nano zirconium dioxide that this embodiment makes, from figure 1 It can be seen that the particles are well dispersed and relatively uniform in size, with a size of 10-30nm.

Embodiment 2

[0034] Weigh 2767g of zirconium oxychloride, add water to dilute to a concentration of 0.5mol / l, take 16.23L of the solution, add 30g of n-butanol, the molar ratio of zirconium oxychloride to sodium hydroxide is 1:3.0, and take 974g of sodium hydroxide , dilute to 48.7L, positively settle, add dropwise for 5 hours, add 3% sodium dodecylbenzenesulfonate after precipitation, stir for 1 hour, age at room temperature for 3 hours, filter with suction, wash with water, water temperature 70°C, wash to pH 7, then wash with 25L of ethanol, bake at 90°C for 18 hours, burn at 550°C, keep warm for 2 hours, and sieve to obtain nano-zirconia.

[0035] After TEM detection, the primary particle size is: 10-30nm, the particles are uniformly dispersed, and the BET is 80m 2 / g.

Embodiment 3

[0037] Weigh 5534g of zirconium oxychloride and prepare it to a concentration of 0.8mol / l. Take 20.3L of this solution, add 80g of n-butanol, the molar ratio of zirconium oxychloride to ammonia water is 1:4, take 5L of ammonia water, and dilute to 43.17L , is settling, and the dropping time is 5 hours. After the precipitation, add 5% sodium lauryl sulfate, stir for 1 hour, age at room temperature for 3 hours, filter with suction, wash with water, and wash at a water temperature of 80°C until the pH is about 7, and then use Wash with 30L ethanol, bake at 90°C for 20 hours, burn at 600°C, keep warm for 3 hours, and sieve to obtain nano-zirconia.

[0038] After TEM detection, the primary particle size is: 10-30nm, the particles are uniformly dispersed, and the BET is 75m 2 / g.

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Abstract

The invention belongs to the technical field of preparation of nano materials and particularly relates to a preparation method of nanometer zirconium dioxide with a high specific surface area. An inorganic zirconium source is diluted with water, an alcohol dispersing agent is added to obtain a solution A, an alkaline precipitating agent is added into water to prepare a solution B, and then the solution B is dropped into the solution A; after the dropwise addition is completed, an anionic surfactant is added for stirring, aging is carried out at the room temperature, suction filtration, washing, drying, burning and sieving are carried out, and then nanometer zirconium oxide powder is obtained. According to the method, by adding the anionic surfactant after completion of a precipitation reaction, the size and uniformity of particles can be controlled, so that BET is increased as much as possible; meanwhile, the concentration of a material liquid and the concentration of a precipitant arecooperatively controlled, the alcohol dispersing agent is added to control the size and uniformity of the particles, and the BET of the particles is further increased.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to nano zirconium dioxide with small particle size, high dispersion and high specific surface area and a preparation method thereof. Background technique [0002] Zirconium dioxide has good thermal and chemical stability, high strength and fracture toughness, low thermal conductivity, good wear resistance and corrosion resistance, etc., so in addition to being used in traditional refractory materials, it is also widely used in compression Electrical components, ceramic capacitors and other functional ceramics, as well as advanced structural ceramics, functional coatings, oxygen sensors and catalyst carriers, and the applications in metallurgy, chemical industry, cosmetics and medicine are also increasing, with broad application prospects. Especially as a three-way catalyst for automobile exhaust purification, it has received extensive attention. Since th...

Claims

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Application Information

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IPC IPC(8): C01G25/02B82Y30/00
CPCB82Y30/00C01G25/02C01P2004/04C01P2004/64C01P2006/12
Inventor 杨应亚
Owner CHANGZHOU GEOQUIN NANO NEW MATERIALS
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