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As the intercalated LDHs was a sort of composites with super-molecular structure, it had many advantages of host and guest simultaneously, so it was widely used as adsorbent, catalyst, pharmaceutical, electrochemistry, photochemistry, pesticide and etc.Solid-state NMR spectroscopy is now well estabished as one of the most powerful tools available to study LDHs and related systems, providing detailed structural information on the local environment and dynamic behavior of the nucleus under investigation. Solid-state NMR, Combining with the techniques such as XRD and TG-DTA were applied to study on the intercalted LDHs in this paper, which mainly included two aspects as below:（1） The reconstruction process of Mg2Al-CO32- during calcine-reconstructing was investigated in the solution of sebaic acid. The result showed that, temperature was a decisive factor to the process. The same time, different temperatures and the same temperatures, different time had something similar, both of which consisted the same intermediate phase. All the sebacic acids were exist as the dianion, and there was no undissociated molecules.（2） The intercalated process of Mg2Al-NO3- with sodium dodecyl sulfate was studied, DS- anions were mainly adsorbing on the outer surface of the LDHs prior to the intercalation when the concentration of
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