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Hydrothermal preparation method of rod-like zinc germanate with adjustable size

A zinc germanate, rod-shaped technology, applied in the field of hydrothermal preparation of rod-shaped zinc germanate, to achieve the effect of mild conditions, high specific surface area, and simple process

Inactive Publication Date: 2016-12-07
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of amino acids as surfactants to synthesize rod-shaped zinc germanate with adjustable size and high yield has not been reported so far

Method used

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  • Hydrothermal preparation method of rod-like zinc germanate with adjustable size
  • Hydrothermal preparation method of rod-like zinc germanate with adjustable size
  • Hydrothermal preparation method of rod-like zinc germanate with adjustable size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The invention provides a hydrothermal preparation method of rod-shaped zinc germanate with adjustable size, comprising the following steps:

[0027] (1) Precursor preparation: Mix sodium carbonate and germanium oxide solid powder at a molar ratio of 1:1, grind for 30 at room temperature, place the mixture in a muffle furnace, heat up to 700°C at room temperature through 70°C, and keep warm After 8 hours, rapid decompression cooling, the obtained sodium germanate solid was further ground for 60 minutes;

[0028] (2) Using sodium germanate as the source of germanium, make it into a sodium germanate solution with a concentration of 0.01mol / L, and use arginine as a surfactant to add it to the sodium germanate solution, wherein the sodium germanate The molar ratio to arginine is 1:0.5; the mixed solution is placed at 40°C and stirred evenly;

[0029] (3) Using zinc acetate dihydrate as the zinc source, it is made into a zinc acetate solution with a concentration of 0.01mol / ...

Embodiment 2

[0033] The difference between embodiment 2 and embodiment 1 is:

[0034] (1) Precursor preparation: mix sodium carbonate and germanium oxide solid powder at a molar ratio of 1:1, grind for 40 minutes at room temperature, place the mixture in a muffle furnace, heat up to 800°C after 80 minutes at room temperature, and keep warm After 12 hours, rapid decompression cooling, the obtained sodium germanate solid was further ground for about 40 minutes;

[0035] (2) Using sodium germanate as the source of germanium, make it into a sodium germanate solution with a concentration of 0.02mol / L, and use tyrosine as a surfactant to add it to the sodium germanate solution, wherein the sodium germanate The molar ratio to tyrosine is 1:2; put the mixed solution at 50°C and stir evenly;

[0036] (3) Using zinc acetate dihydrate as the zinc source, it is made into a zinc acetate solution with a concentration of 0.02mol / L, and the zinc acetate solution is added to the mixed solution in step (2)...

Embodiment 3

[0040] The difference between embodiment 3 and embodiment 1 is:

[0041] (1) Precursor preparation: Mix sodium carbonate and germanium oxide solid powder at a molar ratio of 1:1, grind for 50 minutes at room temperature, place the mixture in a muffle furnace, heat up to 900°C after 90 minutes at room temperature, and keep warm After 16 hours, rapid cooling under reduced pressure, the obtained sodium germanate solid was further ground for about 50 minutes;

[0042] (2) Using sodium germanate as the germanium source, make it into a sodium germanate solution with a concentration of 0.04mol / L, use tryptophan as a surfactant, add it to the sodium germanate solution, wherein sodium germanate The molar ratio to tryptophan is 1:3; the mixed solution is placed at 60°C and stirred evenly;

[0043] (3) Using zinc acetate dihydrate as the zinc source, it is made into a zinc acetate solution with a concentration of 0.05mol / L, and the zinc acetate solution is added to the mixed solution in...

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Abstract

The invention discloses a hydrothermal preparation method of rod-like zinc germanate with an adjustable size. The hydrothermal preparation method comprises the following steps: (1) preparing a precursor: mixing sodium carbonate and germanium oxide solid powder at the mol ratio of 1 to 1; calcining under the condition that the temperature is 700 DEG C to 1000 DEG C for 8h to 24h to prepare sodium germanate solid powder; (2) taking the sodium germanate as a germanium source and adding amino acid into a sodium germanate solution, wherein the adding mol ratio of the sodium germanate to the amino acid is 1 to (0.5 to 5); uniformly stirring a mixed solution under the condition of 40 DEG C to 80 DEG C; (3) adding a zinc acetate solution into the mixed solution of the step (2), wherein the adding mol ratio of zinc acetate to the sodium germanate is 1 to 1; loading the mixed solution into a reaction kettle and carrying out a hydrothermal reaction for 3h to 12h under the condition that the temperature is 120 DEG C to 200 DEG C; washing a product with water until the product is neutral; drying under reduced pressure, and grinding to prepare the rod-like zinc germanate. The hydrothermal preparation method is simple and convenient to operate; a sodium germanate nano-rod has an adjustable size, can be synthesized in a large batch and is low in cost.

Description

technical field [0001] The invention belongs to the field of material synthesis, and in particular relates to a hydrothermal preparation method of rod-shaped zinc germanate with adjustable size. Background technique [0002] Zinc germanate is a compound containing p-region metal ions with a d10 electronic structure. The atoms are distributed along the c-axis, and each germanium atom and zinc atom is located in a tetrahedron composed of 4 oxygen atoms. Its special structure determines that zinc germanate has many advantages such as good thermal stability, high brightness and easy processing, so it becomes an ideal material for electroluminescence and field emission displays. Zinc germanate not only has good luminescent properties, but also is an excellent photocatalyst, which is mainly used to treat refractory organic pollutants, decompose water and reduce carbon dioxide. The microstructure of zinc germanate materials, especially the shape and size, has a great influence on ...

Claims

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Application Information

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IPC IPC(8): C01G17/00
CPCC01G17/00C01P2002/72C01P2004/03C01P2004/10C01P2004/60
Inventor 王冰杨则伟石莹莹
Owner NANJING UNIV
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