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 for materials and surface science, and can solve the unpublished primary particle size of zirconia, which is unfavorable for industrial production and preparation process cumbersome and other problems, to achieve the effect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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  • 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

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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

Examples

Experimental program
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Example Embodiment

[0029] Example 1

[0030] Weigh 1383.5g of zirconium oxychloride, dilute with water to a concentration of 0.4mol / l, take 10.15L of the solution, add PEG20000-10g, the molar ratio of zirconium oxychloride to ammonia is 1:3.5, take 1.1L of ammonia, and dilute to 14.2L, normal precipitation, dripping time 2h, add 2% sodium dodecylbenzene sulfonate after precipitation, stir for 1h, aging at room temperature for 2h, suction filter, wash with water, water temperature 60℃, wash until PH is about 7 , Then use 10L ethanol for alcohol washing, bake at 90°C for 15h, burn at 500°C, keep for 2h, sieving to obtain nano-zirconia.

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

[0032] figure 1 The TEM image of nano zirconia prepared in this example, from figure 1 It can be seen that the particles are well dispersed and relatively uniform in size, with a size of 10-30 nm.

Example Embodiment

[0033] Example 2

[0034] Weigh 2767g of zirconium oxychloride, dilute with water 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, take 974g of sodium hydroxide , Diluted to 48.7L, normal precipitation, dripping time 5h, after precipitation, add 3% sodium dodecylbenzene sulfonate, stir for 1h, aging at room temperature for 3h, suction filter, wash with water, water temperature 70℃, wash to PH It is about 7, and then washed with 25L ethanol, bake at 90°C for 18h, burn at 550°C, keep for 2h, and sieving to obtain nano-zirconia.

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

Example Embodiment

[0036] Example 3

[0037] Weigh 5534 g of zirconium oxychloride and prepare a concentration of 0.8 mol / l. Take 20.3L of the solution, add 80g of n-butanol, and the molar ratio of zirconium oxychloride to ammonia is 1:4. Take 5L of ammonia and dilute to 43.17L. , Precipitation, dripping time 5h, after precipitation, add 5% sodium lauryl sulfate, stir for 1h, aging at room temperature for 3h, suction filter, wash with water, water temperature 80℃, wash until PH is about 7, then use 30L of ethanol is washed with alcohol, baked at 90°C for 20 hours, burned at 600°C, kept for 3 hours, and sieved to obtain nano-zirconia.

[0038] Detected by TEM, the primary particle size is 10-30nm, the particles are evenly 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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