Four di(phenyl sulphinyl)alkane were synthesized by oxidation of corresponding sulfide with nitric acid and characterized by elemental analysis, IR and NMR spectroscopy. The method has the advantages of high purity of the intermediates and high yield of the end products.
The uranyl complex [UO2(PMBP)2(DMDBU)](HPMBP=1-phenyl-3-methy1-4-benzoyl-pyrazolone-5,DMDBU=N,N′-dimethyl-N,N′-dibenzenyl-urea)was synthesized and characterized.The structure was determined by single X-ray diffraction analysis.The crystal belongs to triclinic system,space group P(1)-.The crystallographic data are:a=9.5947(10),b=12.0531(11),c=20.002(2),α=77.167(7),β=80.090(8),γ=75.870(7)°,V=2170.1(4)3,Z=2,F(000)=1052,Mr=164.92,Dc=1.630 Mg/m3,μ=3.800mm-1,R1=0.0409,wR2=0.0770.In the crystal,the uranyl ion is coordinated by four oxygen atoms from two PMBP ligands and one oxygen atoms from one DMDBU to form a distorted pentagonal-bipyramid geometry.
The extraction behavior of N,N′ diethyl N,N′ dibenzenyl urea (DEDBU) to Uranium? and Thorium? from nitric acid solution was studied by using xylene as diluent. The effects of aqueous HNO3 concentration and extractant concentration on the extraction distribution ratio of U? and Th? were studied, and the results show that the extraction behavior of the extractant to U? is similar to tributyl phosphate (TBP), the solvation numbers for DEDBU and TBP are two, respectively. Under the experiment condition, the extractant does not show the extraction behavior to Th?, this result exhibits that the extractant has good application to separate U? and Th?. The crystal structure of the complex UO2(NO3)2[CH2(CH2)2CONC8H17]2 was determined by single crystal X ray diffraction. Crystal data: C24H46N4O10U, triclinic, space group , a = 8.662(2)?, b = 10.07(2)?, c = 10.895(3)?, α = 103.77(2)°, β = 92.01(2)°, γ = 96.23(2)°, V = 915.7(4)?3, Mr = 934.78, Z = 1, Dc = 1.695 g·cm-3, F(000) = 462, μ = 4.495mm-1, R= 0.0250, wR = 0.0591, observed reflections 3566 (I >2σ(I)).The central uranyl ions is coordinated by six oxygen atoms, two of them are from the carbonyl groups of N,N′ diethyl N,N′ dibenzenyl urea molecules, and the other four are from two nitrate groups.
The extraction behavior of N,N-diethyl-N,N-dibenzenyl-urea(DEDBU)and N,N-dimethyl-N,N-dibenzenyl-urea(DMDBU)to uranium(VI)and thorium(IV)from nitric acid solution was studied by using xylene or chloroform as diluent.The effect of aqueous HNO3 concentration,extractant concentration,salting-out agent concentration and aqueous UO2+2/Th4+concentration on extraction distribution ratio of U(VI)and Th(IV)was determined.The results show that the extraction behavior of the extractants DEDBU and DMDBU to U(VI)is similar to that of TBP,the solvation numbers both are two.Under the experimental condition,the extractants DEDBU and DMDBU do not show the extraction behatvior to Th(IV).This means that the estractants may have potential application to separate U(VI)and Th(IV).