Polyoxometallate compound containing tetranuclear cadmium cluster and preparation method and application thereof
A technology of oxo-salt compounds and polymetals, which is applied in the field of poly-oxo-metal salt compounds containing tetranuclear cadmium clusters and its preparation, can solve the problems of no fluorescence detection of PAHs, etc.
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[0032] The present invention provides the preparation method of the tetranuclear cadmium cluster-containing polyoxometalate compound described in the above technical scheme, comprising the following steps:
[0033] Mixing tungstate, cadmium salt, arsenic-containing precursor and amine to obtain a suspension, the arsenic-containing precursor being arsenite or arsenate;
[0034] Adjust the pH value of the suspension to 4.50-6.50 with a pH regulator, and then perform a solvothermal reaction to obtain the polyoxometalate compound containing tetranuclear cadmium clusters; the cadmium salt or the pH regulator contains chlorine element.
[0035] In the present invention, unless otherwise specified, the required preparation materials are commercially available products well known to those skilled in the art.
[0036] In the present invention, the tungstate is preferably sodium tungstate (Na 2 WO 4 ) or potassium tungstate (K 2 WO 4 ); the cadmium salt preferably includes cadmium ...
Embodiment 1
[0044] 4.00g Na 2 WO 4 , 2.00g NaAsO 2 and 2.52g CdCl 2 Dissolve in water (150mL), stir and mix at 300r / min to obtain a suspension; add 8mL of 1,2-propylenediamine dropwise into the above mixture, stir and mix well, and use hydrochloric acid (6mol / L) Adjust the pH of the suspension to 5.66.
[0045] Take 15 mL of the suspension and pour it into a reaction kettle, and react at 150° C. for 3 days; after the reaction is completed, the resulting material is naturally cooled to room temperature to obtain colorless transparent crystals (polyoxometalate compounds containing tetranuclear cadmium clusters) , the chemical formula is (H 2 dap) 6 [Cd 4 Cl 2 (AsW 9 o 34 ) 2 ], denoted as CdAW; The yield is 40%.
Embodiment 2
[0047] 4.00g Na 2 WO 4 , 3.20g Na 3 AsO 4 and 2.52g CdCl 2 Dissolve in water (150mL), stir and mix at 600r / min to obtain a suspension; add 8mL of 1,3-propylenediamine dropwise into the above mixture, stir and mix well, and use nitric acid (6mol / L) Adjust the pH of the suspension to 5.80.
[0048] Take 15 mL of the suspension and pour it into a reaction kettle, and react at 130° C. for 5 days; after the reaction is completed, the resulting material is naturally cooled to room temperature to obtain colorless transparent crystals (polyoxometalate compounds containing tetranuclear cadmium clusters) , the chemical formula is (H 2 dap) 6 [Cd 4 Cl 2 (AsW 9 o 34 ) 2 ], the yield was 35%.
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