Effect of Extra-Framework Titanium in TS-1 on the Ammoximation of Cyclohexanone

Titanium silicalite (TS-1) without and with extra-framework titanium have been prepared and TiO_2 is also prepared under the same conditions.All the samples are characterized with XRD,FT-IR,and UV–Vis.The effects of extra-framework titanium in TS-1 on the ammoximation of cyclohexanone have been studied in a continuous slurry reactor.The characterization results reveal that the extra-framework titanium exists as anatase.The catalytic evaluation results show that the anatase has a positive effect on the ammoximation of cyclohexanone by extending the catalytic life because it also exhibits some activity,while the conversion of cyclohexanone and the selectivity to cyclohexanone oxime are not influenced.The anatase TiO_2 does not catalyze H_2O_2 decomposition appreciably compared with TS-1 without extra-framework titanium.The results are very useful in guiding the TS-1 production.

Preparation of aldoxime through direct ammoximation using titanium silicalite-1 catalyst

The liquid phase direct ammoximation of 5-isooctyl salicylaldehyde with ammonia and hydrogen peroxide was studied using titanium silicalite-1(TS-1)catalyst.The effect of reaction parameters on the yield of the product was studied,which include reaction temperature,reaction time,molar ratio of ammonia to aldehyde as well as hydrogen peroxide to aldehyde.The influence of the amount of catalyst on the reaction results was also investigated.The maximum 5-isooctyl salicylaldoxime yield of 98.76%was achieved under the following optimal reaction conditions:the molar ratio of 5-isooctylaldehyde to hydrogen peroxide and ammonia of 1:1.4:1.6,the reaction temperature of 70℃,the amount of TS-1 of 17.5 g·mol^(-1)(5-isooctyl salicylaldehyde),and the feeding time of 2 h.This method has the mild reaction conditions and avoids the shortcomings of traditional methods.Moreover,useless inorganic salts by-products are avoided,and there is no environmental pollution.