Organic acid radical-pillared hydrotalcites of the type of M6Al2（OH）16〔CnH2n+1COO-〕（M=Mg,Zn;n=13,17）have been successfully assembled by calcination of M6Al2（OH）16CO3·mH2O〕（M=Mg,Zn）and rehydration of MgAlO and ZnAlO in tetradecylic acid solvent and stearic acid solvent respectively and characterized by IR and XRD.The experimental results show that the method of calcination-rehydration could be used to prepare the organic acid radical-pillared MAl-LKHs（M=Mg,Zn）which have good crystallinity,regular layered structure and large interlayer distance (d003(M6Al2（OH）16〔CnH2n+1COO-〕)=2.74nm（M=Zn,n=13）,2.90nm（M=Mg,n=13）,3.24nm（M=Zn,n=17）,3.22nm（M=Mg,n=17）.
