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Method for preparing zirconate yttrium through tartaric acid-nitrate combustion method

A technology of tartaric acid and nitrate, applied in chemical instruments and methods, zirconium compounds, inorganic chemistry, etc., can solve the problems of high temperature of reactants, large size of products, and loss of stoichiometry, so as to promote low-temperature rapid synthesis and product Less loss rate and lower synthesis temperature

Active Publication Date: 2017-08-04
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the above methods, the disadvantage of the high-temperature solid-phase sintering method is that the synthesis temperature is high, the size of the generated product is large, the particle size cannot be controlled, and there is an impure phase due to uneven distribution of components, which has a stoichiometric loss; the simple sol-gel method The disadvantage is that the reaction temperature is higher and the reaction time is longer
The advantage of the hydrothermal method is that it overcomes the disadvantages of uneven distribution of components and stoichiometric loss. However, the requirements for equipment are higher and the reaction time is longer.

Method used

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  • Method for preparing zirconate yttrium through tartaric acid-nitrate combustion method
  • Method for preparing zirconate yttrium through tartaric acid-nitrate combustion method
  • Method for preparing zirconate yttrium through tartaric acid-nitrate combustion method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1) Weigh 2mmol of analytically pure Y(NO 3 ) 3 ·6H 2 O and ZrO(NO 3 ) 2 ·H 2 O, placed in an agate mortar and ground thoroughly to obtain a mixed powder.

[0028] 2) According to the molar ratio of tartaric acid: EDTA = 1: 1, take quantitative analysis of pure tartaric acid and ethylenediaminetetraacetic acid (EDTA), prepare a compound complexing agent with a tartaric acid concentration of 0.2mol / L, and adjust it with concentrated ammonia water Composite complexing agent pH=7, obtains complex complexing agent solution; Wherein, tartaric acid and Y(NO 3 ) 3 ·6H 2 The molar ratio of O is 2:1.

[0029] 3) After stirring with a magnetic stirrer at a speed of 350 rpm for 12 hours, add the complex complexing agent solution drop by drop into the mortar containing the mixed powder, grind while adding, and continue grinding for 15 minutes after the addition is completed , to obtain a pasty viscous intermediate.

[0030] 4) The obtained paste-like viscous intermediate w...

Embodiment 2

[0033] 1) Weigh 3mmol of analytically pure Y(NO 3 ) 3 ·6H 2 O and ZrO(NO 3 ) 2 ·H 2 O, placed in an agate mortar and ground thoroughly to obtain a mixed powder.

[0034] 2) According to the molar ratio of tartaric acid: EDTA = 1: 1, take quantitative analysis of pure tartaric acid and ethylenediaminetetraacetic acid (EDTA), prepare a compound complexing agent with a tartaric acid concentration of 0.2mol / L, and adjust it with concentrated ammonia water Composite complexing agent pH=6, obtains complex complexing agent solution; Wherein, tartaric acid and Y(NO 3 ) 3 ·6H 2 The molar ratio of O is 2:1.

[0035] 3) After stirring with a magnetic stirrer at a speed of 400 rpm for 8 hours, add the complex complexing agent solution drop by drop into the mortar containing the mixed powder, grind while adding, and continue grinding for 20 minutes after the addition is completed , to obtain a pasty viscous intermediate.

[0036] 4) The obtained paste-like viscous intermediate wa...

Embodiment 3

[0042] 1) Weigh 5mmol of analytically pure Y(NO 3 ) 3 ·6H 2 O and ZrO(NO 3 ) 2 ·H 2 O, placed in an agate mortar and ground thoroughly to obtain a mixed powder.

[0043] 2) According to the molar ratio of tartaric acid: EDTA = 1: 2, take quantitative analysis of pure tartaric acid and ethylenediaminetetraacetic acid (EDTA), prepare a compound complexing agent whose tartaric acid concentration is 0.2mol / L, and adjust it with concentrated ammonia water Composite complexing agent pH=5, obtains complex complexing agent solution; Wherein, tartaric acid and Y(NO 3 ) 3 ·6H 2 The molar ratio of O is 2:1.

[0044] 3) After stirring with a magnetic stirrer at a speed of 450 rpm for 8 hours, add the complex complexing agent solution drop by drop into the mortar containing the mixed powder, grind while adding, and continue grinding for 25 minutes after the addition is completed , to obtain a pasty viscous intermediate.

[0045] 4) The obtained paste-like viscous intermediate was...

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Abstract

The invention discloses a method for preparing zirconate yttrium through a tartaric acid-nitrate combustion method. The method comprises the steps of grinding ZrO(NO3)2.H2O to obtain mixed powder; mixing tartaric acid with ethylenediamine tetraacetic acid, adjusting the pH value to be 2-7, stirring and dropwise adding the mixed solution into a mortar containing mixed powder, grinding while adding, further grinding evenly and drying to obtain a gel block; and heating the gel block at a high temperature to obtain a fluffy block and carrying out thermal treatment on the fluffy block to obtain the zirconate yttrium. The method is simple in process, convenient, easy to operate and relatively low in preparation cost; a reaction system is mild and controllable, a combustion product is extremely few in impurity and is low in loss rate; CO2 generated during combustion of the tartaric acid can play roles in forming pores and improving the specific surface area of a solid oxide, improvement of the pphotocatalytic activity of powder is facilitated, low-temperature rapid synthesis of the material can be promoted by heat released by a compound complex agent during combustion within a short period of time, and the method has the advantages of energy-saving and environment-friendly in comparison with an existing high-temperature solid-phase method.

Description

technical field [0001] The invention belongs to the field of material preparation, and in particular relates to a method for preparing yttrium zirconate by a tartaric acid-nitrate combustion method. Background technique [0002] Due to their unique crystal structure, high ionic conductivity and high melting point, rare earth zirconates have good chemical stability and high catalytic activity, and have attracted extensive attention from researchers. It has been widely used in thermal barrier coatings, solid electrolytes, catalysts, and the treatment of radioactive nuclear waste [Xu Qiang, Pan Wei, et al. Pyrochlore-type Ln 2 Zr 2 o 7 Research Progress of Ceramics [J]. Rare Metal Materials and Engineering, 2005, (34): 1100-1104.]. [0003] Since the element yttrium and another element cerium are two kinds of rare earth elements with large content on the earth, compared with other kinds of rare earth zirconates, for yttrium zirconate (Y 2 Zr 2 o 7 ) application research h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00B01J23/10
CPCB01J23/10C01G25/00C01P2002/72C01P2004/03
Inventor 曹丽云罗艺佳黄剑锋吴建鹏李瑞梓
Owner SHAANXI UNIV OF SCI & TECH
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