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Hydroxy-copper montmorillonite was prepared by titrating copper solutions with sodium hydroxide in the presence of Na-montmorillonite. If a copper nitrate solution was used, basic copper nitrate Cu2(OH)3NO3 was precipitated without forming hydroxy-copper interlayers. If a copper acetate solution, however, was titrated similarly in the presence of montmorillonite, the basal spacing of the montmorillonite increased to 20.2 Å, and no basic copper acetate Cu2(OH)3(OCOCH3)H2O was detected until hydroxy-copper layers had fully developed in the interlayer spaces. Chemical analyses showed that the resulting hydroxy interlayers were basic copper acetate, although the amount of acetate ions was small compared with that in Cu2(OH)3(OCOCH3)H2O. A similar hydroxy-copper interlayering occurred in montmorillonite even when Na-montmorillonite was stirred together with freshly precipitated Cu2(OH)3(OCOCH3) H20 in water. The basic copper acetate interlayers decomposed on heating above 300°C, and CuO deposited on the outer surfaces of the montmorillonite.

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