Micron-scale lamellar zirconium phosphate and preparation method thereof

A zirconium phosphate, lamellar technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of high reaction temperature, long reaction time, harsh reaction conditions, etc., and achieve high equipment safety factor and human body hazards The effect of large and low equipment investment

Inactive Publication Date: 2018-11-30
绵竹耀隆化工有限公司
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Problems solved by technology

[0004] The purpose of the present invention is to overcome the deficiencies of the prior art, to provide a micron-scale lamellar zirconium phosphate and its preparation method, which solves the problem of using a large amount of concentrated phosphoric acid or strongly corrosive hydrofluoric acid in the prior art zirconium phosphate preparation technology, and the reaction temperature Disadvantages such as high and long reaction time, harsh reaction conditions, etc.

Method used

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  • Micron-scale lamellar zirconium phosphate and preparation method thereof
  • Micron-scale lamellar zirconium phosphate and preparation method thereof
  • Micron-scale lamellar zirconium phosphate and preparation method thereof

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preparation example Construction

[0026] The preparation method of the above-mentioned micron-scale lamellar zirconium phosphate comprises the following steps:

[0027] Step 1, adding zirconium oxychloride octahydrate into deionized water and stirring evenly, then adding fluoride salt and stirring evenly, then adding phosphoric acid or / and phosphate salt and stirring evenly, after the reaction is completed, heat preservation and standing to obtain a mixed solution for use;

[0028] Step 2: Suction-filtering, washing and drying the above mixed solution to obtain micron-sized lamellar zirconium phosphate.

[0029] Specifically, the molar ratio of zirconium oxychloride octahydrate to deionized water is 1: (170-210); the molar ratio of zirconium oxychloride octahydrate to fluoride salt is 1: (1.0-6.0) ; The molar ratio of zirconium oxychloride octahydrate to phosphoric acid or / and phosphate is 1:(2.0-10.0.

[0030] Specifically, the fluoride salt is at least one of ammonium fluoride, potassium fluoride and / or sod...

Embodiment 1

[0035] After adding 0.155 mol of zirconium oxychloride octahydrate, 0.43 mol of potassium fluoride and 1.02 mol of phosphoric acid in 28 mol of deionized water, stir at 70°C and 100rpm for 3 hours, and finally filter, wash and dry at 85°C After 1.0h, lamellar zirconium phosphate was obtained. Then take samples for scanning electron microscope observation, X-ray diffraction analysis and particle size analysis, the result average particle size is 1.89 μm sheet structure α-Zr (HPO 4 ) 2 ·H 2 O.

Embodiment 2

[0037] After adding 0.806 mol of zirconium oxychloride octahydrate, 4.59 mol of ammonium fluoride and 3.57 mol of phosphoric acid in 167 mol of deionized water, stir at 80°C and 120rpm for 4 hours, and finally filter, wash and dry at 70°C After 2.0h, lamellar zirconium phosphate was obtained. Then take samples for scanning electron microscope observation, X-ray diffraction analysis and particle size analysis, the result average particle size is 1.68 μm sheet structure α-Zr (HPO 4 ) 2 ·H 2 O.

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Abstract

The invention relates to the technical field of zirconium phosphate and preparation thereof, particularly to micron-scale lamellar zirconium phosphate and a preparation method thereof, wherein the zirconium phosphate is alpha-Zr(HPO4)2.H2O, and the average particle size of the alpha-Zr(HPO4)2.H2O is 1.0-2.0 [mu]m. The preparation method comprises: adding zirconium oxychloride octahydrate to deionized water, stirring, adding a fluoride salt, stirring, adding phosphoric acid or / and phosphate, stirring, carrying out a reaction, carrying out thermal insulation standing, carrying out suction filtering, washing, and drying to obtain the micron-scale lamellar zirconium phosphate. According to the present invention, the disadvantages of use of a lot of concentrated phosphoric acid or strong corrosive hydrofluoric acid, high reaction temperature, long reaction time, harsh reaction conditions and the like of the zirconium phosphate preparation technology in the prior art are solved, and the method using the fluoride salt as the reaction catalyst is provided, and has advantages of low reaction temperature, short time, short cycle and wide application range.

Description

technical field [0001] The invention relates to the technical field of zirconium phosphate and its preparation, in particular to a micron-scale lamellar zirconium phosphate and a preparation method thereof. Background technique [0002] Zirconium phosphate α-Zr(HPO 4 ) 2 ·H 2 O is an excellent cation exchanger with strong catalytic, adsorption and ion exchange properties, and is widely used in ion exchangers, especially as a carrier for silver-loaded antibacterial agents. At present, there are mainly three methods for the preparation of zirconium phosphate. One is the reflux method proposed by Clearfield in 1964. In this method, zirconium oxychloride octahydrate is dissolved in hydrochloric acid, concentrated phosphoric acid is added, and the reaction is refluxed for 1 to 7 days to synthesize In the process, strong acid conditions are adopted, the reaction time is long, and a large amount of concentrated phosphoric acid is used. The other is the direct precipitation meth...

Claims

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Application Information

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IPC IPC(8): C01B25/37
CPCC01B25/372C01P2002/72C01P2004/03C01P2004/61
Inventor 周玉军陈林
Owner 绵竹耀隆化工有限公司
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