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Method for CO2-enriched hydro-thermal synthesis of flower-shaped terbium phosphate

A technology of hydrothermal synthesis and terbium phosphate, which is applied in the field of preparation of rare earth phosphate materials, can solve the problems of not very high crystallinity, not very uniform size, lack of crystal morphology and the like, and achieves uniform size, good crystallinity and environmental friendly effect

Active Publication Date: 2015-04-22
INST OF GEOCHEM CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A large number of studies have shown that pH is one of the most important factors controlling the crystal shape and appearance of rare earth phosphate nanomaterials. However, the current methods of synthesizing rare earth phosphates using aqueous solutions only adjust the pH in the initial aqueous solution without buffering the pH. Gradient physical and chemical conditions control its crystal shape and appearance, and there are problems such as the degree of crystallization is not very high, the size is not very uniform, and the controllability is not strong.

Method used

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  • Method for CO2-enriched hydro-thermal synthesis of flower-shaped terbium phosphate
  • Method for CO2-enriched hydro-thermal synthesis of flower-shaped terbium phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Weigh a certain mass of terbium nitrate [Tb(NO 3 ) 3 ·6H 2 O] and diammonium hydrogen phosphate [(NH 4 ) 2 HPO 4 ], and deionized water was used to make an aqueous solution of terbium nitrate and an aqueous solution of diammonium hydrogen phosphate with a concentration of 0.36mol / L respectively. The terbium nitrate solution and the diammonium hydrogen phosphate solution were added into the reaction kettle according to the volume ratio of 1:1, and stirred while adding, and the initial filling degree of the reaction kettle was controlled to be 70%, and the stirring was continued for 30 min to 1 h. Fill the autoclave with 1 MPa carbon dioxide gas and close the autoclave. The autoclave was heated to control the reaction temperature at 180 °C for 2 days, and then the autoclave was naturally cooled to room temperature. After the reaction kettle was depressurized, the product was filtered, centrifuged, and washed twice with deionized water and absolute ethanol alternatel...

Embodiment 2

[0016] Weigh a certain mass of terbium nitrate [Tb(NO 3 ) 3 ·6H 2 O] and diammonium hydrogen phosphate [(NH 4 ) 2 HPO 4 ], and deionized water was used to make an aqueous solution of terbium nitrate and an aqueous solution of diammonium hydrogen phosphate with a concentration of 0.36mol / L respectively. The terbium nitrate solution and the diammonium hydrogen phosphate solution were added into the reaction kettle according to the volume ratio of 1:1, and stirred while adding, and the initial filling degree of the reaction kettle was controlled to be 70%, and the stirring was continued for 30 min to 1 h. Fill the autoclave with 5 MPa carbon dioxide gas and close the autoclave. The autoclave was heated to control the reaction temperature at 180 °C for 2 days, and then the autoclave was naturally cooled to room temperature. After the reaction kettle was depressurized, the product was filtered, centrifuged, and washed twice with deionized water and absolute ethanol alternatel...

Embodiment 3

[0018] Weigh a certain mass of terbium nitrate [Tb(NO 3 ) 3 ·6H 2 O] and diammonium hydrogen phosphate [(NH 4 ) 2 HPO 4 ], and deionized water was used to make an aqueous solution of terbium nitrate and an aqueous solution of diammonium hydrogen phosphate with a concentration of 0.36mol / L respectively. The terbium nitrate solution and the diammonium hydrogen phosphate solution were added into the reaction kettle according to the volume ratio of 1:1, and stirred while adding, and the initial filling degree of the reaction kettle was controlled to be 70%, and the stirring was continued for 30 min to 1 h. Add dry ice (solid carbon dioxide) to the autoclave, control the pressure inside the autoclave to 10 Mpa, and close the autoclave. The autoclave was heated to control the reaction temperature at 180 °C for 2 days, and then the autoclave was naturally cooled to room temperature. After the reaction kettle was depressurized, the product was filtered, centrifuged, and washed t...

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Abstract

The invention discloses a method for CO2-enriched hydro-thermal synthesis of flower-shaped terbium phosphate. The method is characterized by comprising the following steps: preparing a Tb<3+> salt solution and a PO4<3+> salt solution respectively at room temperature; adding the two solutions into a reaction kettle in a volume ratio of 1:1 while stirring, and continuously stirring for 30 minutes to 1 hour; introducing CO2 gas or adding dry ice into the reaction kettle, controlling the pressure in the kettle to be 1-10Mpa, and sealing the high-pressure reaction kettle; heating the high-pressure reaction kettle, setting the reaction temperature to be 100-200 DEG C and the time of duration to be 12 hours to 2 days, and then naturally cooling the high-pressure reaction kettle to room temperature; filtering a product after reaction, and washing and centrifuging the product twice by using deionized water and anhydrous ethanol successively; and drying the washed and centrifuged product at 50-100 DEG C for more than 6 hours to obtain a final pure product.

Description

technical field [0001] The invention relates to a preparation method of a rare earth phosphate material, belonging to the technical field of functional material synthesis. Background technique [0002] In the periodic table of elements, terbium (Tb) is in group IIIB, with an atomic number of 65, and belongs to heavy rare earth elements. In addition, the elements with atomic numbers 57 to 71, which together with terbium are called lanthanides. The lanthanides and their congeners yttrium (Y) and scandium (Sc) are collectively referred to as rare earth elements. Rare earth elements have a special electron shell structure (4f 0-145 d 0-1 6s 2 ), their outer electrons are basically the same, and the inner 4f electron energy levels are very similar, and 4f is an unfilled shell, and ions with completely empty, half-filled and fully-filled electron orbits are optically inert and stable. , because of the characteristics of the outer electronic structure, it has special physical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/37
Inventor 陈柱周丽李和平李肃宁张为
Owner INST OF GEOCHEM CHINESE ACADEMY OF SCI
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