TS-1 has been hydrothermally treated by aqueous solutions of triethylamine, characterized by a number of techniques and studied in the ammoximation of cyclohexanone with NH 3 and H 2 O 2 in a continuous system. Some irregular hollow cavities are created after the treatment by desilication. The catalytic activities of TS-1 are not affected, but the catalyst stabilities significantly increase after the treatment, which can be attributed to the generation of the cavities. The treatment conditions are optimized, with the catalyst stability being extended to ten times of the conventional TS-1. After the treatment, triethylamine can be separated simply through distillation and recycled. The causes of deactivation are elucidated to be the deposition of higher weight byproducts formed on the surface of the catalysts and the deactivated TS-1 can be effectively regenerated through calcination in air.