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Method for preparing protonated B-type Anderson-type heteropoly acid by aqueous phase method

A technology for protonation and heteropolyacids, which is applied in the field of synthesis and characterization of protonated B-type Anderson-type heteropolyacids by aqueous method, which can solve the problems of restricting the research of Anderson-type heteropolyacids, low stability, etc., and achieves a high yield High, high purity, economical effect

Inactive Publication Date: 2019-06-07
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since most Anderson-type heteropolyacids are synthesized under weakly acidic or neutral conditions, the stability is not high
This limits further and more in-depth research on Anderson-type heteropolyacids

Method used

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  • Method for preparing protonated B-type Anderson-type heteropoly acid by aqueous phase method
  • Method for preparing protonated B-type Anderson-type heteropoly acid by aqueous phase method
  • Method for preparing protonated B-type Anderson-type heteropoly acid by aqueous phase method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 2

[0055] Example 2 (NH 4 ) 3 [Mn(OH) 6 Mo 6 o 18 ]Synthesis

[0056] 741g ammonium molybdate (NH 4 ) 6 Mo 7 o 24 Dissolve in 1L of water, heat to 70-90°C, acidify the solution to pH 5.5 with 1M nitric acid, and add 50ml of oxidant H at the same time 2 o 2 , nitric acid not only plays an acidifying role, but also reacts with H 2 o 2 together to oxide Mn II Form Mn III role. Then 118gMnSO 4 Add it into the solution, stir vigorously and react for 15-20min, the orange-red B-type Anderson-type heteropolyacid powder is precipitated from the solution, and then the product is obtained by suction filtration. By infrared spectrum, 955, 896, 879, 806, 783cm -1 Indicating the formation of Anderson framework structure. If a non-oxidizing acid such as HCl is used, only Mn can be obtained as Mn II The product (NH 4 ) 4 [Mn(OH) 6 Mo 6 o 18 ], but the topology remains unchanged.

Embodiment 3

[0057] Example 3Li 3 [Fe(OH) 6 Mo 6 o 18 ]Synthesis

[0058] 726g lithium molybdate Li 2 MoO 4 Dissolve in 1L of water, heat to 70-90°C, and acidify the solution with 1M acetic acid to pH 5.5. Then 113gFeCl 3 Add it into the solution, stir vigorously and react for 15 minutes, the maroon type B Anderson type heteropolyacid powder is precipitated from the solution, and then the product is obtained by suction filtration. By infrared spectrum, 910, 758, 620cm -1 Indicating the formation of Anderson framework structure.

Embodiment 4

[0059] Embodiment 4 (NH 4 ) 3 [Co(OH) 6 Mo 6 o 18 ]Synthesis

[0060] 741g ammonium molybdate (NH 4 ) 6 Mo 7 o 24 Dissolve in 1L of water, heat to 70-90°C, acidify the solution to pH 5.0 with 1M nitric acid, and add 189g of oxidant K at the same time 2 S 2 o 8 , nitric acid not only plays an acidifying role, but also reacts with K 2 S 2 o 8 together to oxidized Co II Form Co III role. Then 128gCo(NO 3 ) 2 Add it into the solution, stir vigorously and react for 20-25min, dark green B-type Anderson-type heteropolyacid powder precipitates out of the solution, and then suction filter to obtain the product. By infrared spectrum, 977, 952, 884cm -1 Indicating the formation of Anderson framework structure. If a non-oxidizing acid such as HCl is used, only Co can be obtained as Co II The product (NH 4 ) 4 [Co(OH) 6 Mo 6 o 18 ], but the topology remains unchanged. The atomically accurate B-type Anderson-type heteropolyacid structure can be obtained by single ...

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Abstract

The invention provides a universal method for preparing a protonated B-type Anderson-type heteropoly acid by an aqueous phase method. A commercialized water-soluble molybdate is used as the reaction raw material, the heteropoly acid is prepared by adjusting pH in a system through an inorganic acid and adding a corresponding central heteroatom metal salt, and the central heteroatom includes most oftransition metals and main group metals. The method is highly controllable, and simple and easy to operate, the yield is up to 95%, the purity is high, and the large-scale production in a kilogram scale can be achieved. The topological structure of the heteropoly acid is determined by single crystal diffraction. The B-type Anderson-type heteropoly acid (NH4)n[Hy(XO6)Mo6O18] can be used as a special solid acid catalyst, and has broad application prospects in the fields of chemistry, life, environmental science and the like. Different from traditional methods that organic solvents are used in the production process, the method uses water as the solvent, and the preparation is carried out under mild conditions, so that the method is environmentally friendly, has economic benefits, and is inline with the development direction of green production advocated by the state.

Description

technical field [0001] The invention belongs to the field of inorganic nano synthesis, in particular to the synthesis and characterization of protonated B-type Anderson type heteropolyacids by aqueous phase method. Background technique [0002] Polyoxometalates, also known as polyoxometalates (ab.POMs), are composed of high-valence transition metal ions (such as Mo(VI), W(VI), V(V), Nb(V), Ta(V ), etc.) are highly polymerized with oxygen to form a "molecular state" inorganic nanocluster compound with a spatial network structure. Polyacid compounds have a wide variety, diverse structures, and rich and varied physical properties such as light, electricity, and magnetism. They are a class of shining star clusters, especially in catalytic oxidation, and are of great application value in fields such as energy chemistry. At present, it has important applications in academic basic research and industry. [0003] According to whether there is a central heteroatom in the multi-acid...

Claims

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Application Information

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IPC IPC(8): B01J27/24
Inventor 张江威李杲
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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