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Method for preparing KNbWO6.H2O

A technology of niobium tungstate and potassium niobium tungstate, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., to achieve low reaction temperature, improved product performance, and good crystallinity

Inactive Publication Date: 2013-11-20
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of niobium tungstate KNbWO by solvothermal method has not been reported in the literature 6 ·H 2 o

Method used

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  • Method for preparing KNbWO6.H2O
  • Method for preparing KNbWO6.H2O
  • Method for preparing KNbWO6.H2O

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1.0g Nb 2 o 5 Add 5.0 g of KOH to 60 ml of deionized water, and conduct a hydrothermal treatment at 180° C. for 2 days. Get 2.4ml hydrothermal reaction product in the upper layer [Nb 6 o 19 ] 8- solution (ICP test the Nb in the solution 5+ Concentration is 0.1116mol / L), then add 20ml octanol, according to the molar ratio Nb 5+ :W 6+ =1:2.5 ratio by adding 0.1673g H 2 WO 4 , and then use dilute hydrochloric acid to adjust the pH of the solution to 7.2, put it into a 40ml reaction kettle, and conduct hydrothermal treatment at 220°C for 2 days. The obtained product was washed by centrifugation with deionized water and dried.

[0023] This embodiment is the best embodiment. Figure 1 ~ Figure 2 The obtained KNbWO is given respectively 6 ·H 2 XRD and SEM pictures of O.

Embodiment 2

[0025] 1.0g Nb 2 o 5 Add 5.0 g of KOH to 60 ml of deionized water, and conduct a hydrothermal treatment at 180° C. for 2 days. Get 2.4ml hydrothermal reaction product in the upper layer [Nb 6 o 19 ] 8- solution (ICP test the Nb in the solution 5+ Concentration is 0.1116mol / L), then add 20ml octanol, according to the molar ratio Nb 5+ :W 6+ =1:2.5 ratio by adding 0.1673g H 2 WO 4 , and then use dilute hydrochloric acid to adjust the pH of the solution to 7.2, put it into a 40ml reaction kettle, and conduct hydrothermal treatment at 220°C for 1 day. The obtained product was washed by centrifugation with deionized water and dried.

[0026] Compared with Example 1, when the reaction time was changed to 1 day, the morphology of the prepared product had no obvious change, and there was an extremely weak miscellaneous peak at 22° in the XRD spectrum observation spectrum.

Embodiment 3

[0028] 1.0g Nb 2 o 5Add 5.0 g of KOH to 60 ml of deionized water, and conduct a hydrothermal treatment at 180° C. for 2 days. Get 2.4ml hydrothermal reaction product in the upper layer [Nb 6 o 19 ] 8- solution (ICP test the Nb in the solution 5+ Concentration is 0.1116mol / L), then add 20ml octanol, according to the molar ratio Nb 5+ :W 6+ =1:2.5 ratio by adding 0.1673g H 2 WO 4 , and then use dilute hydrochloric acid to adjust the pH of the solution to 7.2, put it into a 40ml reaction kettle, and conduct hydrothermal treatment at 220°C for 5 days. The obtained product was washed by centrifugation with deionized water and dried.

[0029] Compared with Example 1, when the reaction time was extended to 5 days, the morphology of the obtained product did not change significantly, and no miscellaneous peaks were found in the XRD spectrum, but the intensity of the diffraction peak was slightly stronger.

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Abstract

The invention relates to a method for preparing KNbWO6.H2O, belonging to the technical field of inorganic material preparation technology. The provided method comprises the following steps of: firstly processing Nb2O5 and KOH under hydrothermal condition to get [Nb6O19]8- solution; then adding a certain amount of octanol and H2WO4 in the [Nb6O19]8- solution, regulating the pH value of the reaction liquid by diluted hydrochloric acid, and then obtaining KNbWO6.H2O with a pyrochlore structure under the solvothermal condition. The method is simple, convenient, easy to carry out and low in cost, and overcomes the tedious steps of the conventional high temperature solid phase method, such as repeated high temperature firing and grinding; and the obtained KNbWO6.H2O is a monodispersed octahedron in appearance.

Description

technical field [0001] The invention provides a niobium tungstate KNbWO 6 ·H 2 The preparation method of O belongs to the technical field of inorganic material preparation technology. Background technique [0002] Solid acid catalytic materials are attracting more and more attention due to its unique structure, and niobium tungstate is a typical solid acid catalytic material, which shows good catalytic activity, selectivity and stability in some organic synthesis reactions. In addition, because of its unique structure and physical and chemical properties, niobium tungstate compounds have also attracted extensive research interest in piezoelectricity, dielectric, thermodynamics, etc. (Journal of Physics and Chemistry of Solids, 2001, 62, 1149- 1161). [0003] At present, niobium tungstate is prepared by high-temperature solid-phase method. The high-temperature solid-phase method requires repeated high-temperature burning and grinding, and the temperature is basically abov...

Claims

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Application Information

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IPC IPC(8): C01G41/00
Inventor 庞广生韩永男焦世惠
Owner JILIN UNIV
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