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Microwave-assisted preparation method for spherical transition metal and zirconium diphosphonate in one step

A zirconium bisphosphonate and transition metal salt technology, applied in the field of bisphosphonate preparation, can solve the problems of long process steps, environmental pollution, time-consuming, etc., and achieve low equipment requirements, high efficiency, and short reaction time Effect

Inactive Publication Date: 2015-07-01
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the above method, the stripping agents and adhesives such as ethylenediamine and diethylamine added in the stripping process and spray molding process will pollute the environment, and labor protection needs to be strengthened in actual operation, and the process operation steps Long, relatively complex, and time-consuming

Method used

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  • Microwave-assisted preparation method for spherical transition metal and zirconium diphosphonate in one step
  • Microwave-assisted preparation method for spherical transition metal and zirconium diphosphonate in one step

Examples

Experimental program
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Effect test

Embodiment 1

[0029] CoCl 2 , ZrOCl 2 , NaH 2 PO 4 and NH 4 F is formulated into aqueous solution respectively, mixes, wherein ZrOCl in the solution 2 The concentration of Zr / P is 0.005mol / L, the molar ratio of Zr / P is 1:20, the molar ratio of Zr / F is 1:6, and the molar ratio of Zr / Co is 1:1. The mixed solution was microwaved at 90°C for 30 min. After centrifugation, washing, and freeze-drying, spherical zirconium-cobalt bisphosphate ZrCo(PO 4 ) 2 4H 2 O, SEM characterization as figure 1 shown, where figure 2 yes figure 1 magnified view of .

Embodiment 2

[0031] Will Co(NO 3 ) 2 , ZrO(NO 3 ) 2 、Na 2 HPO 4 and NaF were prepared as aqueous solutions, mixed, wherein the solution ZrO(NO 3 ) 2 The concentration of Zr / P is 0.02mol / L, the molar ratio of Zr / P is 1:40, the molar ratio of Zr / F is 1:3, and the molar ratio of Zr / Co is 1:1. The mixed solution was microwaved at 85°C for 45min. After centrifugation, washing and drying at room temperature, spherical zirconium cobalt bisphosphate ZrCo(PO 4 ) 2 4H 2 O.

Embodiment 3

[0033] MnCl 2 , ZrOCl 2 , NH 4 h 2 PO 4 and NaF were formulated into aqueous solutions, mixed, wherein ZrOCl in the solution 2 The concentration of Zr / P is 0.005mol / L, the molar ratio of Zr / P is 1:40, the molar ratio of Zr / F is 1:6, and the molar ratio of Zr / Mn is 1:1. The mixed solution was microwaved at 90°C for 30 min. After centrifugation, washing, and freeze-drying, spherical zirconium manganese bisphosphate ZrMn(PO 4 ) 2 4H 2 O.

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Abstract

The invention relates to a microwave-assisted preparation method for spherical transition metal and zirconium diphosphonate in one step. The microwave-assisted preparation method comprises the following steps: preparing a water-soluble transition metal salt, a water-soluble zirconium, a water-soluble phosphoric acid source and water-soluble fluoride into an aqueous solution respectively, and mixing; then, performing microwave-assisted heating, centrifuging, washing and drying to obtain transition metal and zirconium diphosphonate. The microwave-assisted preparation method is simple, convenient to operate, less in time consumption and high in efficiency; the prepared transition metal and zirconium diphosphonate are regular in morphology, and can be used as a catalyst, an ion exchange material, an antibacterial material and the like without being roasted at a high temperature.

Description

technical field [0001] The invention belongs to the field of preparation methods of bisphosphonates, in particular to a method for preparing spherical transition metal and zirconium bisphosphates in one step with microwave assistance. Background technique [0002] Zirconium phosphate α-ZrP(α-Zr(HPO 4 ) 2 ·H 2 O) is a typical cationic layered structure compound. Zirconium phosphate and its derivatives have high thermal stability, chemical stability and strong acid and alkali resistance, as well as zeolite-like shape-selective adsorption and Catalytic performance, so it is widely used in intercalation chemistry, catalysis, adsorption, membrane, fuel cell, biology, photochemistry and other fields. [0003] Transition metal and zirconium bisphosphate ZrM(PO 4 ) 2 As a catalyst, it can be used to catalyze isomerization of alkanes, selective oxidation of methane to generate synthetic gas, oxidation of propane to dehydrogenation, selective oxidation of propylene to alcohols to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45B01J27/18B01J27/185B01J27/187B01J39/12A01N59/26A01P1/00
Inventor 邢彦军胡晓霞
Owner DONGHUA UNIV
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