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Metal phosphate and preparation method thereof

A metal phosphate and metal technology, applied in the field of zirconium phosphate materials and their preparation, spherical titanium, can solve the problems of easy introduction of impurities

Active Publication Date: 2016-11-30
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of metal phosphate and preparation method thereof, to overcome the problem that metal phosphate is easy to introduce impurities in the preparation process

Method used

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  • Metal phosphate and preparation method thereof

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preparation example Construction

[0030] A kind of preparation method of metal phosphate provided by the invention comprises the steps:

[0031] (1) the soluble salt of metal is dissolved in the hydrochloric acid aqueous solution;

[0032] (2) adding the metal salt solution in the step (1) to the phosphoric acid aqueous solution under stirring;

[0033] (3) Heat the mixture system obtained in step (2) to a reflux state for reaction under stirring to obtain a solid precipitate, and after cooling to room temperature, wash with deionized water to remove unreacted acid to obtain a metal phosphate precipitate ;

[0034] (4) the metal phosphate precipitate obtained in step (3) is emulsified into a suspension by shearing;

[0035] (5) Spray drying the suspension obtained in step (4) to obtain spherical metal phosphate.

[0036] Aqueous hydrochloric acid:

[0037] In the present invention, the concentration of the aqueous hydrochloric acid solution is not particularly limited, and is usually 0-10 mol / L. If it is g...

Embodiment 1

[0048] Accurately weigh 10g ZrOCl 2 ·8H 2 O was dissolved in 40ml concentration of 3mol / L hydrochloric acid aqueous solution; at room temperature, under stirring, the above zirconium solution was added dropwise to 200ml concentration of 2mol / L phosphoric acid aqueous solution; kept stirring, the obtained mixture was heated to a reflux state, and the reaction 24h; cool to room temperature after the reaction, centrifuge the white precipitate of zirconium phosphate, wash with deionized water several times to remove unreacted acid, separate the wet sample of zirconium phosphate precipitate, and add a certain amount of deionized Ionized water, process the suspension with a shear emulsifier, the rotor speed is 5000rpm, and the treatment time is 4h to obtain a zirconium phosphate suspension, the solid content of the suspension is 10%; the zirconium phosphate suspension is molded by a spray dryer, The inlet temperature of the spray dryer is 190°C, and the outlet temperature is 120°C....

Embodiment 2

[0051] Accurately measure 5ml TiCl 4 Dissolve in 10ml of aqueous hydrochloric acid with a concentration of 8mol / L; at room temperature, add the above titanium solution dropwise to 230ml of aqueous phosphoric acid with a concentration of 6mol / L under stirring; keep stirring, and heat the obtained mixture to a reflux state, React for 4 hours; after the reaction, cool to room temperature, centrifuge and separate the white precipitate of titanium phosphate, wash with deionized water several times to remove unreacted acid, add a certain amount of deionized water to make titanium phosphate suspension liquid; process the suspension with a shear emulsifier, the rotor speed is 3000rpm, and the treatment time is 5h to obtain a titanium phosphate suspension, and the solid content in the suspension is 5%; the titanium phosphate suspension is molded by a spray dryer, sprayed The inlet temperature of the dryer is 260°C and the outlet temperature is 170°C.

[0052] The scanning electron mic...

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Abstract

The invention provides a metal phosphate and a preparation method thereof. The preparation method comprises the steps of: (1) dissolving a soluble salt of metal into a hydrochloric acid aqueous solution; (2) under stirring, adding the metal salt solution of step (1) into a phosphoric acid aqueous solution; (3) under stirring, heating the mixture system obtained in step (2) to a reflux state to carry out reaction so as to obtain a solid precipitate, performing cooling to room temperature, then conducting washing with deionized water to remove unreacted acid, thus obtaining a metal phosphate precipitate; (4) conducting shearing emulsification on the metal phosphate precipitate obtained in step (3) into a suspension; and (5) conducting spray drying on the suspension obtained in step (4) so as to obtain spherical metal phosphate. The metal phosphate has good sphericity and uniform shape, and does not contain other impurities. Also, the preparation method provided by the invention has the advantages of simple operation, low equipment requirement, low production cost and high safety.

Description

technical field [0001] The invention relates to a metal phosphate and a preparation method thereof, in particular to a spherical titanium and zirconium phosphate material and a preparation method thereof. Background technique [0002] Tetravalent metal phosphate compounds are a class of multifunctional materials, the most representative of which are titanium or zirconium phosphates, such as Zr(HPO 4 ) 2 ·H 2 O (abbreviated as α-ZrP), Ti (HPO 4 ) 2 ·H 2 O (abbreviated as α-TiP). Since Clearfield et al first synthesized α-ZrP in 1964, the structure and properties of tetravalent metal phosphate compounds have been extensively and deeply studied. [0003] α-ZrP or α-TiP and its derivatives are a layered material, and the laminates are passed through MO 6 Octahedral (M represents Zr or Ti metal atom) with 6 -PO 3 The group shares an oxygen atom, while each -PO 3 The group and three M atoms share oxygen atoms to form a layered structure between the laminates through hydro...

Claims

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Application Information

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IPC IPC(8): C01B25/37C01B25/45
Inventor 袁苑王仪森义建军祖凤华李志飞王科峰崔伟松
Owner PETROCHINA CO LTD