Synthetic method of water medium dispersed cerium zirconium oxide nano material

Abstract

The invention provides a synthetic method of a water medium dispersed cerium zirconium oxide nano material. The synthetic method comprises the following steps: (1) performing a precipitation reaction by using an inorganic salt aqueous solutios of Ce and Zr and an inorganic base aqueous solution of Ce and Zr to prepare a Ce-Zr mixed hydroxide precipitate; (2) heating and refluxing the Ce-Zr mixed hydroxide precipitate to prepare a Ce-Zr hydroxide cosolubilization body; (3) filtering and washing the Ce-Zr hydroxide cosolubilization body to prepare a Ce-Zr hydroxide hydrogel; (4) mixing the Ce-Zr hydroxide hydrogel with organic alcohol, organic acid and high polymer to prepare a Ce-Zr oxide synthetic sizing material; and (5) heating and further performing hydro-thermal synthesis on the Ce-Zr oxide synthetic sizing material to obtain the water medium dispersed cerium zirconium oxide nano material. The cerium zirconium oxide nano particles obtained by the method provided by the invention are single crystals, have a nano scale of 2-8nm, and are monodispersed in a water medium; and the mass of cerium zirconium oxide accounts for 5-10% of the sol body volume of the nano material.

Description

technical field

[0001] The invention relates to a synthesis method of a rare earth cerium-based oxide nanometer material, in particular to a synthesis method of a cerium-zirconium oxide nanometer material. Background technique

[0002] Cerium-zirconium oxide, or a co-solution oxide of cerium oxide and zirconium oxide, is a rare earth cerium-based composite material that is widely used in industry. For example, it is used as polishing material for optical glass, quartz glass, semiconductor, LED, UV shielding material for cosmetics, textiles, light-transmitting glass, surface thermal barrier or wear-resistant material for special plates, catalytic accelerator for fuel cell anode, load Support or co-catalyst for type catalysts, and modifiers for materials such as hydrogen storage, sensing, luminescence, and ceramics.

[0003] Most of the industrial use of cerium-zirconium oxide is used as an oxygen storage / release material for three-way catalysts for the purification of mo...

Examples

preparation example Construction

[0055] Aqueous medium dispersed cerium zirconium oxide nanomaterials are sols with water as the dispersion medium and solid solution nanoparticles composed of cerium oxide and zirconia as the dispersed phase. The nanoparticles are single crystals with a nanometer size of 2-8nm. The medium is monodisperse; solid solution nanoparticles composed of ceria and zirconia are also called cerium-zirconium oxide nanoparticles, and the general formula is denoted as Ce x Zr 1-x o 2 , x=0.2~0.8, represents the mass fraction of Ce; Ce x Zr 1-x o 2The mass (w / g) of the mass (w / g) accounts for 5-10% of the sol body volume (V / ml); the synthesis method of the aqueous medium dispersion cerium zirconium oxide nanomaterial comprises the following steps: (1) using Ce and Zr inorganic Precipitation reaction between salt aqueous solution and inorganic alkali aqueous solution to prepare Ce-Zr mixed hydroxide precipitate; (2) heating Ce-Zr mixed hydroxide precipitate to reflux to prepare Ce-Zr hydr...

Embodiment 1

[0106] Dispersion of cerium zirconium oxide Ce in water medium 0.2 Zr 0.8 o 2 Synthesis of Nanomaterials:

[0107] Take 0.010mol Ce(NO 3 ) 3 ·6H 2 O was added to deionized water and stirred to dissolve, and 0.040mol Zr(NO 3 ) 4 ·5H 2 Add O into deionized water and stir to dissolve, mix cerium and zirconium salt solutions and add 0.61ml of hydrogen peroxide (30w%), dilute to 80ml with deionized water, and record it as liquid A; take 7.49ml of concentrated ammonia water (25w%), 9.60 Add 1 g of ammonium carbonate to deionized water to form an alkaline solution, dilute to 80 ml with deionized water, and record it as liquid B. Stir the liquid A and heat it to 60° C., drop the liquid B into the liquid A until the pH of the liquid A is 8.3-8.5, and obtain a Ce-Zr mixed hydroxide precipitate suspension. Stir the suspension at 80°C for 2h, add 40ml of ethylene glycol, use a reflux device to reflux at a heating temperature of 105°C with stirring for 2h, and cool to room tempera...

Embodiment 2

[0110] Dispersion of cerium zirconium oxide Ce in water medium 0.3 Zr 0.7 o 2 Synthesis of Nanomaterials:

[0111] Take 0.012mol Ce(NO 3 ) 3 ·6H 2 O was added to deionized water and stirred to dissolve, and 0.028mol ZrOCO 3 ·nH 2O (dissolved with nitric acid first) was added to deionized water and stirred to dissolve, mixed with cerium and zirconium salt solution, diluted to 80ml with deionized water, and recorded as solution A; take 3.32ml of concentrated ammonia water (25w%) and 1.77g of sodium hydroxide to add Make an alkaline solution in deionized water, add 0.73ml of hydrogen peroxide (30w%), dilute to 80ml with deionized water, and record it as solution B. Drop liquid A into liquid B under stirring, and adjust the pH to 8.5-8.8 with dilute ammonia water after dripping of liquid A to obtain Ce-Zr mixed hydroxide precipitate suspension. Let the suspension stand overnight, add 20ml of ethanol and 20ml of isopropanol, reflux at a heating temperature of 85°C with stir...

technical field

[0001] The invention relates to a synthesis method of a rare earth cerium-based oxide nanometer material, in particular to a synthesis method of a cerium-zirconium oxide nanometer material. Background technique

[0002] Cerium-zirconium oxide, or a co-solution oxide of cerium oxide and zirconium oxide, is a rare earth cerium-based composite material that is widely used in industry. For example, it is used as polishing material for optical glass, quartz glass, semiconductor, LED, UV shielding material for cosmetics, textiles, light-transmitting glass, surface thermal barrier or wear-resistant material for special plates, catalytic accelerator for fuel cell anode, load Support or co-catalyst for type catalysts, and modifiers for materials such as hydrogen storage, sensing, luminescence, and ceramics.

[0003] Most of the industrial use of cerium-zirconium oxide is used as an oxygen storage / release material for three-way catalysts for the purification of mo...

Examples

preparation example Construction

[0055] Aqueous medium dispersed cerium zirconium oxide nanomaterials are sols with water as the dispersion medium and solid solution nanoparticles composed of cerium oxide and zirconia as the dispersed phase. The nanoparticles are single crystals with a nanometer size of 2-8nm. The medium is monodisperse; solid solution nanoparticles composed of ceria and zirconia are also called cerium-zirconium oxide nanoparticles, and the general formula is denoted as Ce x Zr 1-x o 2 , x=0.2~0.8, represents the mass fraction of Ce; Ce x Zr 1-x o 2The mass (w / g) of the mass (w / g) accounts for 5-10% of the sol body volume (V / ml); the synthesis method of the aqueous medium dispersion cerium zirconium oxide nanomaterial comprises the following steps: (1) using Ce and Zr inorganic Precipitation reaction between salt aqueous solution and inorganic alkali aqueous solution to prepare Ce-Zr mixed hydroxide precipitate; (2) heating Ce-Zr mixed hydroxide precipitate to reflux to prepare Ce-Zr hydr...

Embodiment 1

[0106] Dispersion of cerium zirconium oxide Ce in water medium 0.2 Zr 0.8 o 2 Synthesis of Nanomaterials:

[0107] Take 0.010mol Ce(NO 3 ) 3 ·6H 2 O was added to deionized water and stirred to dissolve, and 0.040mol Zr(NO 3 ) 4 ·5H 2 Add O into deionized water and stir to dissolve, mix cerium and zirconium salt solutions and add 0.61ml of hydrogen peroxide (30w%), dilute to 80ml with deionized water, and record it as liquid A; take 7.49ml of concentrated ammonia water (25w%), 9.60 Add 1 g of ammonium carbonate to deionized water to form an alkaline solution, dilute to 80 ml with deionized water, and record it as liquid B. Stir the liquid A and heat it to 60° C., drop the liquid B into the liquid A until the pH of the liquid A is 8.3-8.5, and obtain a Ce-Zr mixed hydroxide precipitate suspension. Stir the suspension at 80°C for 2h, add 40ml of ethylene glycol, use a reflux device to reflux at a heating temperature of 105°C with stirring for 2h, and cool to room tempera...

Embodiment 2

[0110] Dispersion of cerium zirconium oxide Ce in water medium 0.3 Zr 0.7 o 2 Synthesis of Nanomaterials:

[0111] Take 0.012mol Ce(NO 3 ) 3 ·6H 2 O was added to deionized water and stirred to dissolve, and 0.028mol ZrOCO 3 ·nH 2O (dissolved with nitric acid first) was added to deionized water and stirred to dissolve, mixed with cerium and zirconium salt solution, diluted to 80ml with deionized water, and recorded as solution A; take 3.32ml of concentrated ammonia water (25w%) and 1.77g of sodium hydroxide to add Make an alkaline solution in deionized water, add 0.73ml of hydrogen peroxide (30w%), dilute to 80ml with deionized water, and record it as solution B. Drop liquid A into liquid B under stirring, and adjust the pH to 8.5-8.8 with dilute ammonia water after dripping of liquid A to obtain Ce-Zr mixed hydroxide precipitate suspension. Let the suspension stand overnight, add 20ml of ethanol and 20ml of isopropanol, reflux at a heating temperature of 85°C with stir...

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