A kind of preparation method of zinc phosphomolybdate containing keggin structure

A technology of zinc phosphomolybdate and phosphomolybdic acid, applied in the direction of phosphorus oxo acid, etc., can solve the problems of no report, no keggin structure zinc phosphomolybdate compound, etc., and achieves low price, low impurity ion content, and reduced production cost. Effect

Active Publication Date: 2020-02-07
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 zinc phosphomolybdate compound with keggin structure, neither in patent literature nor in scientific papers.

Method used

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  • A kind of preparation method of zinc phosphomolybdate containing keggin structure
  • A kind of preparation method of zinc phosphomolybdate containing keggin structure

Examples

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Embodiment 1

[0019] Weigh 0.015mol phosphomolybdic acid crystals into a beaker, add enough distilled water, stir the glass, put it in a water bath at 60°C and continue stirring until the cloudy solution turns into a yellow clear liquid; weigh 0.0221mol zinc oxide and add phosphomolybdenum In the acid solution, start the stirrer and react in a water bath at 60°C. A small amount of bubbles appear as the reaction progresses. Add the phosphomolybdic acid solution dropwise to control the pH at about 1.0, and continue to stir until the bubbles are completely released and white The powder was completely dissolved, and when the solution turned yellow-green, the solution was distilled under reduced pressure to obtain an orange-red paste, and finally dried at 80°C for 8 hours to prepare 24.76 g of orange zinc phosphomolybdate powder. 3 [PMo 12 o 40 ] 2 Calculated, the yield is 84.85%.

[0020] Depend on figure 1 As shown in the infrared spectrogram data, 783.0cm -1 ,868.3cm -1 ,961.6cm -1 and...

Embodiment 2

[0023] Weigh 0.0128mol phosphomolybdic acid crystals into a beaker, add enough distilled water, stir the glass, put it in a water bath at 60°C and continue stirring until the cloudy solution turns into a yellow clear liquid; weigh 0.0192mol zinc oxide and add phosphomolybdenum In the acid solution, start the stirrer and react in a water bath at 65°C. A small amount of bubbles appear as the reaction progresses. Add the phosphomolybdic acid solution dropwise to control the pH at about 2.0, and continue to stir until the bubbles are completely released and white The powder was completely dissolved, and when the solution turned yellow-green, the solution was distilled under reduced pressure to obtain an orange-red paste, and finally dried at 80°C for 8 hours to prepare 22.07 g of orange zinc phosphomolybdate powder. 3 [PMo 12 o 40 ] 2 Calculated, the yield is 88.49%.

Embodiment 3

[0025] Weigh 0.01mol phosphomolybdic acid crystals into a beaker, add enough distilled water, stir the glass, put it in a water bath at 60°C and continue stirring until the cloudy solution turns into a yellow clear liquid; weigh 0.0271mol zinc oxide and add phosphomolybdenum In the acid solution, start the stirrer and react in a water bath at 55°C. A small amount of bubbles appear as the reaction progresses. Add the phosphomolybdic acid solution dropwise to control the pH at about 3.0, and continue to stir until the bubbles are completely released and white The powder was completely dissolved, and when the solution turned yellow-green, the solution was distilled under reduced pressure to obtain an orange-red paste, and finally dried at 70°C for 10 hours to prepare 17.51 ​​g of orange zinc phosphomolybdate powder. 3 [PMo 12 o 40 ] 2 Calculated, the yield is 85.04%.

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Abstract

The invention belongs to the field of preparation of phosphomolybdate and relates to a preparation method of zinc phosphomolybdate containing a keggin structure. The preparation method adopts a liquid-phase method to synthesize the zinc phosphomolybdate and comprises the following steps of: adopting phosphomolybdic acid and zinc oxide as raw materials, adopting distilled water or alcohol as a solvent, controlling PH to be 1.0-3.0, and reacting under a water-bathing condition with the temperature of 55-65 DEG C; carrying out reduced-pressure distillation to obtain pasty substance, and drying for 8-10 hours at the temperature of 70-90 DEG C to obtain orange zinc phosphomolybdate. The preparation method has the beneficial effects that the process is simple, the reactant raw materials are cheap in price, the impurity-ion content is low, the yield is high and the benefit for reducing the production cost is achieved; the prepared zinc phosphomolybdate containing the keggin structure can meetthe requirements of application in the aspects of catalyst synthesis, pharmaceutical synthesis, electrochemical application and flame-retardant compounding and the like.

Description

technical field [0001] The invention belongs to the field of phosphomolybdate preparation, and relates to a preparation method of zinc phosphomolybdate containing a keggin structure. Background technique [0002] With the successful synthesis of the first heteropolyacid salt, ammonium phosphomolybdate, polyacid chemistry has gradually become an important research field in inorganic chemistry. In the early days, it was believed that polyacids were condensed acids formed by the condensation of inorganic oxygen-containing acids such as sulfuric acid, phosphoric acid, and tungstic acid. However, isopolyacids and heteropolyacids belong to different categories. Isopolyacids and heteropolyacids are two major components of polyacid chemistry. Isopolyacids are formed by condensation of the same oxoacid ions; Different types of polymeric oxygen-containing ions formed by the condensation of two or more oxoacid ions. Among them, heteropoly compounds have excellent characteristics: the...

Claims

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Application Information

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