The Organic Intercalates of HTiNbO

White solid KTiNbOj is prepared by heating an intimate mixture of K2CO3, TiOj, NbjOj in the molar ratio 1 2 1 at 1100° overnight. The reaction product ( 3 g) is treated with 2M HCI (200 mL) at 60° for 1 h to produce HTiNbOj. The sample is washed with distilled water several times, until a flame test shows no detectable potassium. Approximately 20 mg of the sample is sealed in a Pyrex tube, IS cm long and 1.5 cm in diameter with a wall thickness of 2.0 mm, which contains 3 mL of aliphatic amines CH3(CH2) NH2 and the mixture warmed at 60° for 5 h. The products are filtered and washed with acetone three times. The products have composition [CH3(CH2) NH + ]i 2 [TiNbOj-]. 

Both parent compounds (KTiNbOs and HTiNbOj) and amine-intercalated HTiNbOs belong to the orthorhombic system a = 6.44, b = 3.78, c = 17.52 A for HTiNbOs. The (TiNbOj) layer lies in the ab plane and intercalates amine in its protonated form. The interlayer distance c/2 expands on intercalation c = 9.02 A for ammonia, 22.96 A for methanamine, 26.78 A for ethanamine, 35.34 A for 1-propanamine, 36.82 A for 1-butanamine. 

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Herein are described the preparations of the charge-transfer-type intercalation compound FeOCl (pyridine derivative), of grafted-type intercalation compounds FeO(OCH3) and Fe0(02C2H4)1/2 and of some organic intercalates of HTiNbOs. 

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