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Mixed-valence hexavanadate alkoxyl derivative and preparation method thereof

A technology of hexavanadate and mixed valence state, which is applied in the direction of chemical instruments and methods, compounds of group 5/15 elements of the periodic table, organic compounds of group 5/15 without C-metal bonds, etc., to achieve structurally rich Effect

Inactive Publication Date: 2017-06-13
HUBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Previous studies on polyacid-based compounds mostly focused on structural design and synthesis, and their properties and practical applications have just started; however, there are few studies on the design and synthesis of polyvanadic acid-based materials, especially reduced polyvanadic acid derivatives. There are fewer reports on the synthesis, modification and properties of

Method used

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  • Mixed-valence hexavanadate alkoxyl derivative and preparation method thereof
  • Mixed-valence hexavanadate alkoxyl derivative and preparation method thereof
  • Mixed-valence hexavanadate alkoxyl derivative and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 (TRIS=trishydroxymethylaminomethane)

[0029] Compound 1 synthesis process: Weigh 1.6935g (14mmol) NaVO 3 , 0.8413g (7mmol) tris hydroxymethyl amino methane into the 50ml hydrothermal reaction kettle liner, then add 20ml deionized water and 150ul (4.6mmol) N 2 h 4 ∙ H 2 O, after stirring evenly, the reaction kettle was sealed and placed in an oven, reacted at 210°C for 24h, after cooling to room temperature, filtered the reaction mixture, and the filtrate was allowed to stand for 7 days to precipitate black blocky crystals. Use 20ml deionized water for crystals, 20ml anhydrous Naturally dry after washing with ethanol. IR (KBr-pellets, cm -1 ): 3475(s), 1608(m), 1534(m), 1111(s), 1049(s), 947(s), 745(s), 613(s); UV-Vis (H 2 O): λ max =347nm; Elemental analysis (%): theoretical value V 6 N 3 o 29 C 12 h 46 : N 4.19, C 14.38, H4.63; Test values: N 4.48, C 14.53, H 4.87

Embodiment 2

[0030] Example 2 (TRIS=pentaerythritol)

[0031] Compound 2 synthesis process: Weigh 1.6935g (14mmol) NaVO 3 , Add 0.9455g (7mmol) pentaerythritol into 50ml reactor liner, then add 20ml deionized water and 150ul (4.6mmol) N 2 h 4 ∙H 2 O, the reaction kettle was placed in an oven at 210°C for 24 hours. After cooling to room temperature, the reaction mixture was filtered, and the filtrate was allowed to stand for 7 days to precipitate blue flaky crystals. IR (KBr-pellets, cm -1 ): 3600(w), 3311(s), 1620(m), 1126(s), 1066(sh), 1033(s), 956(sh), 943(s), 798(w), 653(s ); UV-Vis (H 2 O): λ max =346nm; Elemental analysis (%): theoretical value forNa2V6O24C15H34: C 18.96, H 3.61; test value: C 19.52, H 3.21.

Embodiment 3

[0032] Example 3 (TRIS=trimethylolethane)

[0033] Compound 3 synthesis process: Weigh 1.6935g (14mmol) NaVO 3 , Add 0.8344g (7mmol) trimethylolethane into 50ml reactor liner, then add 20ml deionized water and 150ul (4.6mmol) N 2 h 4 ∙ H 2 O, the reaction kettle was placed in an oven at 210°C for 24 hours, and after cooling to room temperature, blue columnar crystals were precipitated. IR (KBr-pellets, cm -1 ):3594(w),2964(w),2893(m),2850(m),1403(m),1144(s),1047(s),974(s),943(sh),926(s ),847(s),617(s); UV-Vis (H 2 O): λmax=346nm; Elemental analysis (%): theoretical value V6N3O19C15H41: N 4.81, C20.63, H 4.73; test value: N 5.03, C 20.46, H 4.76.

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Abstract

The invention relates to a mixed-valence hexavanadate alkoxyl derivative and a preparation method thereof and belongs to the technical field of organic-inorganic hybrid materials. According to the structure of the alkoxyl derivative, three bridging oxygen atoms arranged to form a planar triangle on a Linqivist hexavanadate framework are substituted by three hydroxyl oxygens of a tri-hydroxymethyl compound molecule, three tri-hydroxymethyl compounds are adjacently distributed on the hexavanadate framework, and all vanadium is tetravalent vanadium or tetravalent and pentavalent vanadium distributed in a mixed mode. The tri-hydroxymethyl compounds are tri-hydroxymethyl aminomethane, pentaerythritol, trimethylolethane or trimethylolpropane. The tri-substituted hexavanadate alkoxyl derivative and a post-modification product thereof possibly have unique magnetism, catalytic activity and other properties. The properties make them have unique advantages on the aspect of the organic-inorganic hybrid materials rich in construction structure and property.

Description

technical field [0001] The invention relates to a mixed valence hexavanadate alkoxy derivative and a preparation method thereof, belonging to the technical field of organic-inorganic hybrid materials. Background technique [0002] my country is rich in vanadium resources, the price is relatively low, and there is no suitable process and route for deep processing and utilization of vanadium resources. Most of the vanadium is used for iron and steel smelting, etc., and the utilization level of vanadium resources is very low. These factors make the development and application of new vanadium-based materials of great significance. In recent years, research on vanadium oxides and vanadic acid compounds has achieved many fruitful results in the fields of catalysis, hydrogen storage, and electrode materials. For example, vanadium-based materials as electrode materials have outstanding advantages such as high specific capacity and large flow charge and discharge. Occhiuzzi et a...

Claims

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Application Information

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IPC IPC(8): C07F9/00H01M4/60H01M10/052
CPCC07F9/005H01M4/60H01M10/052Y02E60/10
Inventor 伍平凡胡勋亮肖滋成
Owner HUBEI UNIV OF TECH
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