a rich co 2 Method for hydrothermally synthesizing yttrium phosphate nanospheres

A technology of hydrothermal synthesis and yttrium phosphate, which is applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problems of not very high degree of crystallization, uneven size, lack of crystal shape and appearance, etc., to achieve uniform size, Good crystallization degree, environmental friendly effect

Active Publication Date: 2016-07-13
INST OF GEOCHEM CHINESE ACADEMY OF SCI
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  • 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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  • a rich co <sub>2</sub> Method for hydrothermally synthesizing yttrium phosphate nanospheres
  • a rich co <sub>2</sub> Method for hydrothermally synthesizing yttrium phosphate nanospheres

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Effect test

Embodiment 1

[0014] Weigh a certain mass of yttrium nitrate [Y(NO 3 ) 3 ·6H 2 O] and diammonium hydrogen phosphate [(NH 4 ) 2 HPO 4 ], be made into the aqueous solution of the yttrium nitrate of 0.36mol / L and the aqueous solution of diammonium hydrogen phosphate respectively with deionized water. Add the yttrium nitrate solution and the diammonium hydrogen phosphate solution into the reactor according to the volume ratio of 1:1, stir while adding, control the initial filling degree of the reactor to 70%, and keep stirring for 30min to 1h. Fill the autoclave with 1MPa 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 alternately, and finally the product was dried at 70°C for 12 hours.

Embodiment 2

[0016] Weigh a certain mass of yttrium nitrate [Y(NO 3 ) 3 ·6H 2 O] and diammonium hydrogen phosphate [(NH 4 ) 2 HPO 4 ], be made into the aqueous solution of the yttrium nitrate of 0.36mol / L and the aqueous solution of diammonium hydrogen phosphate respectively with deionized water. Add the yttrium nitrate solution and the diammonium hydrogen phosphate solution into the reactor according to the volume ratio of 1:1, stir while adding, control the initial filling degree of the reactor to 70%, and keep stirring for 30min to 1h. Fill the autoclave with 5MPa 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 alternately, and finally the product was dried at 70°C for 12 hours.

Embodiment 3

[0018] Weigh a certain mass of yttrium nitrate [Y(NO 3 ) 3 ·6H 2 O] and diammonium hydrogen phosphate [(NH 4 ) 2 HPO 4 ], be made into the aqueous solution of the yttrium nitrate of 0.36mol / L and the aqueous solution of diammonium hydrogen phosphate respectively with deionized water. Add the yttrium nitrate solution and the diammonium hydrogen phosphate solution into the reactor according to the volume ratio of 1:1, stir while adding, control the initial filling degree of the reactor to 70%, and keep stirring for 30min to 1h. Add dry ice (solid carbon dioxide) to the autoclave, control the internal pressure of the autoclave to be 10Mpa, 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 alternately, and finall...

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Abstract

The invention discloses a method for hydrothermally synthesizing a yttrium phosphate nanosphere by using rich CO2. The method is characterized by comprising the following steps: respectively preparing a Y<3+> salt solution and a PO4<3+> salt solution at room temperature; adding the two solutions to a reaction kettle at a volume ratio of 1:1, stirring at the same time, and continuously stirring for 30 minutes to 1 hour; introducing CO2 gas or adding dry ice to the reaction kettle, controlling the pressure inside the reaction kettle to 1-10 Mpa, and sealing the high-pressure reaction kettle; heating the high-pressure reaction kettle, determining reaction temperature of 100-200 DEG C and duration time of 12 hours to 2 days, and then naturally cooling the high-pressure reaction kettle to room temperature; filtering a reacted product, and successively washing and centrifugalizing twice by using deionized water and absolute ethyl alcohol; and drying the washed and centrifugalized 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 nanometer material, belonging to the technical field of functional material synthesis. Background technique [0002] In the periodic table of elements, yttrium (Y) is in group IIIB, with an atomic number of 39, and belongs to heavy rare earth elements. Yttrium and another rare earth element, cerium, are the two most abundant rare earth elements in the earth's crust. The lanthanides with atomic numbers 57 to 71 are collectively referred to as rare earth elements together with the congeners yttrium (Y) and scandium (Sc). 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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/37B82Y30/00B82Y40/00
Inventor 周丽陈柱李和平李肃宁张为
Owner INST OF GEOCHEM CHINESE ACADEMY OF SCI
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