Method for preparing tantalum-based rare earth polyacid and nanocrystal of tantalum-based rare earth polyacid

A technology of rare earth polyacids and nanocrystals, which is applied in the direction of nanotechnology, nanotechnology, polycrystalline material growth, etc., can solve the problems of low efficiency and difficult recovery of catalysts, and achieve the effect of increasing the specific surface area

Inactive Publication Date: 2018-01-16
HENAN NORMAL UNIV
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  • Abstract
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Problems solved by technology

[0003] Rare earth polyacids have important research value in the field of catalysis, but there are also some problems. For example, in a homogeneous catalytic system, although rare earth polyacids have high catalytic efficiency, there is a problem that the catalyst is difficult to recycle.
However, in heterogeneous systems, rare earth polyacids are less efficient due to their larger size.

Method used

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  • Method for preparing tantalum-based rare earth polyacid and nanocrystal of tantalum-based rare earth polyacid
  • Method for preparing tantalum-based rare earth polyacid and nanocrystal of tantalum-based rare earth polyacid
  • Method for preparing tantalum-based rare earth polyacid and nanocrystal of tantalum-based rare earth polyacid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Preparation of rare earth polyacid Y-POM single crystal product

[0023] Will K 5 Na 4 [P 2 W 15 o 59 (TaO 2 ) 3 ]·17H 2 O (0.20 g, 0.04 mmol) was dissolved in 25 mL deionized water and heated to 75 °C to obtain a light yellow solution; add solid NaHSO 3 (0.04 g, 0.38 mmol) solution became colorless; Y(NO 3 ) 3 ·6H 2 O (0.05 g, 0.15 mmol) was added to the solution; 2 mL of glacial acetic acid (or 1 mL of 1 M hydrochloric acid solution) was added to the solution for acidification, cooled to room temperature and allowed to stand for a week to obtain a Y-POM single crystal product with a final yield of 82%, its structure is as attached figure 1 shown.

[0024] Preparation of other tantalum-based rare earth polyacid single crystal products

[0025] The synthesis conditions of Eu-POM, Gd-POM, Tb-POM, Dy-POM, Ho-POM, Er-POM, Tm-POM, Yb-POM and Lu-POM are the same as those of Y-POM, except that Y(NO 3 ) 3 ·6H 2 O is replaced by EuCl respectively 3 ·6H 2 O, Gd...

Embodiment 2

[0027] Preparation of Nanoscale Rare Earth Polyacid Y-POM

[0028] Will K 5 Na 4 [P 2 W 15 o 59 (TaO 2 ) 3 ]·17H 2 O (0.20 g, 0.04 mmol) was dissolved in 25 mL deionized water and heated to 75 °C to obtain a light yellow solution; add solid NaHSO 3 (0.04 g, 0.38 mmol) solution became colorless; Y(NO 3 ) 3 ·6H 2 O (0.1 g, 0.26 mmol) was added to the solution; 1 mL of 1M hydrochloric acid solution was added to the solution for acidification, and then 25 mL of ethanol solution was added, and the resulting solution was continuously stirred for 20 min and cooled naturally to room temperature (the speed was kept at 1000 r / min ), a large amount of fine powder product was formed during this process, the product was collected by filtration and washed with 2.0 mL deionized water and 2.0 mL ethanol, and the yield of the final product was 91%. as attached Figure 4 As shown, its powder XRD pattern is consistent with the single crystal sample, and the SEM electron microscope ph...

Embodiment 3

[0030] Mass Preparation of Nanoscale Rare Earth Polyacid Y-POM

[0031] Will K 5 Na 4 [P 2 W 15 o 59 (TaO 2 ) 3 ]·17H 2 O (2.0 g, 0.4 mmol) was dissolved in 250 mL of deionized water and heated to 75 °C to obtain a pale yellow solution. Add solid NaHSO 3 (0.4 g, 3.8 mmol) The solution became colorless. Then set Y(NO 3 ) 3 ·6H 2 O (1.0 g, 2.6 mmol) was added to the solution; 10 mL of 1M HCl solution was added to the solution for acidification, and 250 mL of ethanol was added. The resulting solution was continuously stirred for 20 minutes and cooled to room temperature naturally. During this process, a large number of fine powder products were formed. The product was collected by filtration and washed with 10 mL of deionized water and 5 mL of ethanol to finally obtain 1.75 g of nano-sized product with a yield of 80%. as attached Figure 4 As shown, its powder XRD is consistent with the single crystal sample. Its particle size and Figure 5 similar in .

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Abstract

The invention discloses a method for preparing tantalum-based rare earth polyacid and a nanocrystal of tantalum-based rare earth polyacid, and belongs to the technical field of synthesis of polytantalate. The key points of the technical scheme are as follows: the tantalum-based rare earth polyacid is composed of three rare earth ions and one polyacid anion which are bonded through three RE-O-Ta bonds, the tantalum-based rare earth polyacid is overall an electrically neutral cluster and the molecular formula of the tantalum-based rare earth polyacid is [REH2O)7]3P2W15Ta3O62.nH2O. The inventionalso specifically discloses the method for preparing the nanocrystal of the tantalum-based rare earth polyacid. A large amount of coordinated water on the rare earth ions in the tantalum-based rare earth polyacid is easily lost under heating, and thus Lewis acid catalytic active sites of the rare earth ions are exposed, so that the tantalum-based rare earth polyacid can be used as a Lewis acid catalyst; the tantalum-based rare earth polyacid is insoluble in water and a common organic solvent, and therefore the tantalum-based rare earth polyacid can be used as a heterogeneous catalyst; besides,since the specific surface area of the tantalum-based rare earth polyacid is increased due to nanoparticles of the tantalum-based rare earth polyacid, a catalytic reaction is promoted, and when Y-POMis used for catalyzing a reaction of benzaldehyde with trimethylsilyl cyanide, the conversion rate within 4 hours reaches 99% or above.

Description

technical field [0001] The invention belongs to the technical field of synthesis of polytantalates, and in particular relates to a preparation method of a class of tantalum-based rare earth polyacids and nanocrystals thereof. Background technique [0002] Rare earth polyacids have important potential applications in fluorescence, magnetism, electrochemistry, and especially catalysis, and have attracted more and more attention. The reaction of various vacant polyacids with rare earth ions is one of the most effective strategies for the synthesis of rare earth polyacids. In recent years, a large number of rare earth polyacids with new structure types have been synthesized by this method (CrystEngComm, 2015, 17, 8175). However, due to the strong basicity of vacancy polyacids and the strong oxophilicity and high coordination number of rare earth ions, the controllability of the reaction between vacancy polyacids and rare earth ions is poor. Slightly changing the pH value, reac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/30C30B7/14B01J27/195B01J31/18C01F17/00B82Y30/00B82Y40/00
Inventor 李书军王若雅彭青坡翟建新陈学年
Owner HENAN NORMAL UNIV
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