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Preparation method of iron phosphomolybdate comprising keggin structure

A technology of phosphomolybdic acid and liquid phase method, which is applied in the direction of phosphorus oxyacids, etc., can solve the problems of no keggin structure iron phosphomolybdate compound, no report, etc., and achieve low impurity ion content, low price and high yield Effect

Active Publication Date: 2018-07-06
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At the same time, the content of its research and research in related fields have attracted widespread attention. The synthesis of phosphomolybdate containing keggin structure is still a major challenge in the field of chemistry.
[0004] Before the work of this patent application, there was no report of iron phosphomolybdate compound with keggin structure, neither in patent literature nor in scientific papers.

Method used

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  • Preparation method of iron phosphomolybdate comprising keggin structure
  • Preparation method of iron phosphomolybdate comprising keggin structure

Examples

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Effect test

Embodiment 1

[0019] Weigh 0.0119mol phosphomolybdic acid crystal and put it into a beaker, add distilled water, stir the glass, put it into a water bath with a temperature of 60°C and continue stirring until the turbid solution turns into a yellow clear liquid; weigh 0.0119mol Fe(OH) 3 Add it to the phosphomolybdic acid solution, start the stirrer, react in a water bath at a temperature of 60 °C, and continue to stir it fully. At the same time, add the phosphomolybdic acid solution dropwise to control the pH to about 1.0 to obtain a reddish-brown precipitate. Note that centrifugation or filtration is not allowed here. , because the obtained precipitate is very fine, centrifugation and filtration cannot separate the precipitate from the solution, but the solution containing the precipitate should be distilled under reduced pressure to obtain a reddish-brown paste, and finally dried at 80 °C for 4 hours by blasting to obtain brown phosphorus Iron molybdate 20.50g, in Fe[PMo 12 O 40 ], the y...

Embodiment 2

[0023] Weigh 0.0129mol of phosphomolybdic acid crystals into a beaker, add distilled water, stir in the glass, put into a water bath at 60°C and continue stirring until the turbid solution turns into a yellow clear liquid; weigh 0.0109mol Fe(OH) 3 Add it to the phosphomolybdic acid solution, start the stirrer, react in a water bath at a temperature of 65°C, and continue to stir thoroughly. At the same time, add the phosphomolybdic acid solution dropwise to control the pH to about 2.0 to obtain a reddish-brown precipitate. Note that centrifugation or filtration is not allowed here. , because the obtained precipitate is very fine, centrifugation and filtration cannot separate the precipitate from the solution, but the solution containing the precipitate should be distilled under reduced pressure to obtain a reddish-brown paste, and finally dried at 80 °C for 4 hours by blasting to obtain brown phosphorus Iron molybdate 20.38g, in Fe[PMo 12 O 40 ], the yield was 82.64%.

Embodiment 3

[0025] Weigh 0.01mol phosphomolybdic acid crystal and put it into a beaker, add distilled water, stir the glass, put it into a water bath with a temperature of 60°C and continue stirring until the turbid solution turns into a yellow clear liquid; weigh 0.0157mol Fe(OH) 3 Add it to the phosphomolybdic acid solution, start the stirrer, react in a water bath at a temperature of 55°C, and continue to stir thoroughly. At the same time, add the phosphomolybdic acid solution dropwise to control the pH to about 3.0 to obtain a reddish-brown precipitate. Note that centrifugation or filtration is not allowed here. , because the obtained precipitate is very fine, centrifugation and filtration cannot separate the precipitate from the solution, but the solution containing the precipitate should be distilled under reduced pressure to obtain a reddish-brown paste, and finally dried at 70 °C for 5 hours by blasting to obtain brown phosphorus Iron molybdate 15.47g, in Fe[PMo 12 O 40 ], the yi...

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Abstract

The invention belongs to the field of the preparation of phosphomolybdate, and relates to a preparation method of iron phosphomolybdate comprising a keggin structure. The preparation method comprisesthe following steps: by adopting a liquid phase synthesis method, adopting phosphomolybdic acid and iron hydroxide as raw materials, and adopting distilled water or ethanol as a solvent, controlling PH at 1.0 to 3.0, and performing the reaction under a water bath condition of 55 to 65 DEG C; and decompressing and distilling to obtain a pasty substance, and drying for 4 to 6 hours at 70 to 90 DEG C, thus obtaining the orange iron phosphomolybdate. The preparation method has the advantages of simple process, low price of reactant raw materials, low content of impurity ions, high yield and benefit to decreasing the production cost; and the prepared iron phosphomolybdate comprising the Keggin structure can meet the requirements on the application in the aspects of catalyst synthesis, medicinesynthesis, electrochemistry application, flame-retardant agent compounding and the like.

Description

technical field [0001] The invention belongs to the field of preparation of phosphomolybdate, and relates to a preparation method of iron phosphomolybdate containing keggin structure. Background technique [0002] With the successful synthesis of the first heteropolyacid salt, ammonium phosphomolybdate, polyacid chemistry has slowly become an important research field in inorganic chemistry. Heteropolyacid is a multimeric oxygen-containing ion formed by the condensation of two or more oxygen-containing acid ions of different types. Among them, the heteropoly compound has excellent characteristics: definite structure, good compatibility with polar solvents, It is acidic and oxidizing at the same time. Heteropolyacid salt-related reactions can generate "pseudo-liquid phase" behavior to form unique reaction fields, which can modulate molecules or atoms to make them multifunctional. [0003] Due to the special configuration of phosphomolybdate containing keggin structure, it ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/16
CPCC01B25/16C01P2002/82C01P2002/85
Inventor 陈绪煌
Owner HUBEI UNIV OF TECH
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