Transition-rare earth dissimilar metal cluster doped polyniobic acid compound and preparation method thereof

A transition metal and compound technology, applied in the field of polyniobium oxyacid compounds, can solve problems such as difficulty in crystallization, and achieve the effects of easy storage, good stability and simple preparation process

Active Publication Date: 2021-09-17
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Under relatively alkaline conditions, rare earth ions and transition metal ions are prone to hydrolysis to form precipitates, and are not easy to crystallize

Method used

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  • Transition-rare earth dissimilar metal cluster doped polyniobic acid compound and preparation method thereof
  • Transition-rare earth dissimilar metal cluster doped polyniobic acid compound and preparation method thereof
  • Transition-rare earth dissimilar metal cluster doped polyniobic acid compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Example 1: Na 6 h 20 {Cr 2 [Dy 3 O(μ 3 -OH) 3 (H 2 O) 3 ] 2 (Nb 6 o 19 ) 5} 40H 2 O transition-preparation of polyniobic acid clusters doped with rare earth heterometallic clusters. 0.27mmol potassium niobate tridehydrate, 0.14mmol dysprosium nitrate hexahydrate, 0.24mmol chromium chloride hexahydrate, 0.53mmol trishydroxymethylaminomethane Add it into 8ml of sodium carbonate-sodium bicarbonate solution and mix evenly, put the resulting mixture into a 25mL glass bottle, stir for 1 hour, then put it into an oven for hydrothermal reaction. After incubating at 90°C for 72 hours, it was lowered to room temperature, filtered, and the resulting mother liquor was placed at room temperature to volatilize naturally to obtain Na 6 h 20 {Cr 2 [Dy 3 O(μ 3 -OH) 3 (H 2 O) 3 ] 2 (Nb 6 o 19 ) 5} 40H 2 O transition-rare earth heterometallic cluster doped polynioboxoacid clusters.

Embodiment 2

[0032] Example 2: Na 6 h 20 {Mn 2 [Dy 3 O(μ 3 -OH) 3 (H 2 O) 3 ] 2 (Nb 6 o 19 ) 5} 44H 2 Preparation of Polyniobic Acid Clusters Doped with O Transition-Rare Earth Heterometallic Clusters

[0033] Add 0.27mmol potassium niobate thirteen hydrate, 0.14mmol dysprosium nitrate hexahydrate, 0.33mmol manganese chloride dihydrate, and 0.53mmol trishydroxymethylaminomethane to 8ml sodium carbonate-sodium bicarbonate solution and mix evenly, and the resulting mixture Put it into a 25mL glass bottle, stir for 1 hour, and put it into an oven for hydrothermal reaction. After being incubated at 90°C for 72 hours, it was lowered to room temperature, and after filtration, the resulting mother liquor was placed at room temperature to volatilize naturally to obtain Na 6 h 20 {Mn 2 [Dy 3 O(μ 3 -OH) 3 (H 2 O) 3 ] 2 (Nb 6 o 19 ) 5} 40H 2 O transition-rare earth heterometallic cluster doped polynioboxoacid clusters.

Embodiment 3

[0034] Example 3: Na 6 h 20 {Fe 2 [Dy 3 O(μ 3 -OH) 3 (H 2 O) 3 ] 2 (Nb 6 o 19 ) 5} 43H 2 Preparation of Polyniobic Acid Clusters Doped with O Transition-Rare Earth Heterometallic Clusters

[0035] Add 0.27mmol potassium niobate thirteen hydrate, 0.14mmol dysprosium nitrate hexahydrate, 0.23mmol ferrous sulfate heptahydrate, and 0.53mmol trishydroxymethylaminomethane to 8ml sodium carbonate-sodium bicarbonate solution and mix evenly. Put it into a 25mL glass bottle, stir for 1 hour, and put it into an oven for hydrothermal reaction. After being incubated at 90°C for 72 hours, it was lowered to room temperature, and after filtration, the resulting mother liquor was placed at room temperature to volatilize naturally to obtain Na 6 h 20 {Fe 2 [Dy 3 O(μ 3 -OH) 3 (H 2 O) 3 ] 2 (Nb 6 o 19 ) 5} 43H 2 O transition-rare earth heterometallic cluster doped polynioboxoacid clusters.

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Abstract

The invention discloses a transition-rare earth dissimilar metal cluster doped polyniobic acid compound, the molecular formula of the compound is Na6H20 {TM2 [Dy3O (<mu>3-OH) 3 (H2O) 3] 2 (Nb6O19) 5}. nH2O, six Dy < 3 + > ions and two TM < 3 + > ions form an 8-core transition-rare earth dissimilar metal cluster inside cluster anions in the crystal structure of the compound, a regular triangular bipyramid configuration is formed in the cubic axis direction, the upper end and the lower end of the dissimilar metal cluster and the equatorial plane of the dissimilar metal cluster successfully capture five {Nb6O19} (Nb6) cluster units, so that rare transition-rare earth dissimilar metal cluster doped polyniobic acid cluster anions are formed. According to the preparation method, a conventional hydrothermal method and a room-temperature volatilization method are combined, a sodium carbonate-sodium bicarbonate buffer solution is used as a solvent, the preparation process is simple, the pH value of a reaction system can be maintained in a proper and stable range, meanwhile, the problem that a niobate precursor and two dissimilar metals are incompatible when coexisting is solved, and the transition metal and rare earth ions are prevented from prematurely separating out a large amount of precipitates.

Description

technical field [0001] The invention relates to the field of magnetic materials and crystal materials, in particular to a polyniobic acid compound doped with transition-rare earth heterometallic clusters, a preparation method and an application. Background technique [0002] Polyoxometalate is a kind of metal oxo cluster anion formed by dehydration polycondensation of early transition metal oxides such as Mo, W, V, Nb, Ta, etc. It has high negative charge, oxygen-rich surface, rich redox performance and Interesting structural features such as nanoscale dimensions. Due to their potential applications in catalysis, medicine, magnetism, and materials science, researchers have continuously strived to synthesize new metal-doped polyoxometalates. Metal-substituted polyoxometallates, as one of the fastest-growing branches in the field of polyacids, have attracted the attention of many researchers due to their structural diversity and interesting applications in magnetism. [0003...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00H01F41/00
CPCC01G33/006H01F41/00C01P2002/77C01P2006/42C01P2004/01C01P2002/72C01P2006/10
Inventor 李新雄林玉雕郑寿添
Owner FUZHOU UNIV
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