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Preparation and application of stable niobium precursor

A stable and niobium salt technology, applied in the field of preparation of niobium-containing porous materials, can solve the problems of complex preparation process and low purity

Inactive Publication Date: 2013-03-06
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, most of the research on soluble niobium salts is in soluble organic acids. For example, Chinese patent (CN 1935772) has prepared niobium oxalate soluble niobium precursors using oxalic acid as a coordination organic acid, but the preparation process is complicated. The obtained niobium oxalate precursors Industrial grade, low purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Example 1 Mesoporous niobium silicon material was prepared by using niobium tartrate.

[0011] Prepare a hydrochloric acid aqueous solution with pH=1 with deionized water; weigh 1-2g P 123 Dissolve in the above hydrochloric acid solution, until P 123 After complete dissolution, a certain concentration of niobium tartrate solution is added, wherein the niobium content in the tartaric acid solution is fixed but the amount of tartaric acid is adjustable. After continuous stirring for 1h, add tetraethyl orthosilicate (TEOS) dropwise to ensure that the molar ratio of Nb / template / TEOS / solvent is 1 / 0.2-0.5 / 1-5 / 20-100, and stir at 35°C After 24 hours, the slurry was transferred to a stainless steel autoclave lined with polytetrafluoroethylene, and crystallized at 100°C for 24 hours. After centrifugation, the precipitate was washed with deionized water to pH = 7, then dried at 60°C overnight, ground, and then placed in a muffle furnace at 550°C for 6 hours to obtain the desire...

Embodiment 2

[0012] Example 2 Preparation of Mesoporous Niobium Oxide Material Using Niobium Tartrate

[0013] Weigh the organic surfactant (P 123 , F 127 , CTAB) 1-2g, dissolved in water (or ethanol) solution, after the surfactant is completely dissolved, adjust the pH value of the solution in the range of 1-2, then measure a certain concentration of niobium tartrate solution, you can add ammonia water to adjust For the pH value of the niobium precursor, add the niobium precursor solution to the above solution dropwise to ensure that the molar ratio of Nb / template agent / solvent is in the ratio range of 1 / 0.2-0.5 / 20-100. After that, the stirring was continued at 80°C for 24h, and then the slurry was transferred to a stainless steel autoclave lined with polytetrafluoroethylene, and crystallized at 100-180°C for 24h. After centrifugation, the precipitate was washed with deionized water to pH = 7, then dried overnight at 60°C, ground, and then baked in a muffle furnace at 550°C for 6 hours ...

Embodiment 3

[0014] Example 3 Preparation of Mesoporous Niobium Phosphate Material Using Niobium Tartrate

[0015] A mixed aqueous solution of niobium tartrate and sodium hydrogen phosphate was prepared with deionized water, and the coordination state of the niobium precursor could be regulated by adding ammonium oxalate. The organic template (P 123 ,CTAB,F 127 ) is dissolved in water (ethanol) solution, and the pH value of the solution is adjusted in the range of 1-10 after the surfactant is completely dissolved. Under continuous stirring, the mixed solution of Nb and P is added dropwise to the template solution, and the molar ratio of Nb / P / template / solvent is controlled in the ratio range of 1 / 1-5 / 0.1-0.6 / 20-100. After the dropwise addition was completed, the slurry was transferred to a stainless steel pressure vessel lined with polytetrafluoroethylene, and crystallized at 100-160° C. for 24 hours. After centrifugation, the precipitate was washed with deionized water to pH = 7, then d...

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PUM

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Abstract

The invention relates to a preparation method of stable water-soluble niobium precursor. Niobium pentoxide is dissolved in hydrofluoric acid solution to obtain niobium pentafluori solution. Niobium is precipitated in the form of niobic acid hydrate by alkali liquor. Precipitation is dissolved in tartaric acid solution to obtain stable soluble-niobium tartrate precursor solution which is faintly acid. The concentration of the niobium tartrate solution can be controlled according to the amount of the niobium pentoxide added in early regulation. The stable niobium tartrate solution can be used to synthesize mesoporous niobium oxide, mesoporous niobium phosphate and mesoporous niobium-silicon materials, and the materials are as excellent as commercial niobium chloride soluble salt in property. The highly stable water-soluble niobium tartrate precursor is obtained from low-cost materials in a simple and feasible synthesis path.

Description

technical field [0001] The invention relates to a preparation method of a soluble niobium precursor solution and its application in niobium-containing porous materials, especially for the preparation of niobium-containing porous materials. Background technique [0002] Niobium materials are a new type of functional materials, which have good applications in acid catalysis, oxidation, and hydrolysis reactions, and also have potential applications in electrochemistry, superconducting materials, and optical materials. Correspondingly, the soluble salts of niobium that can be applied in the material preparation process are only a limited number of halogen compounds, the most commonly used is niobium pentachloride, which is formed by the action of metal niobium and chlorine gas or hydrogen chloride gas or in the presence of carbon Anhydrous Nb 2 o 5 It is prepared by reacting with chlorine gas, so the cost is very high and cannot meet the requirements of industrial production. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G33/00C01B25/37
Inventor 王艳芹张宇卢冠忠刘晓晖任家文刘慧慧郭耘郭杨龙王筠松张志刚龚学庆
Owner EAST CHINA UNIV OF SCI & TECH
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