气相色谱-质谱法分析环己酮氨肟化体系中失活催化剂上可溶性沉积物的组成

利用气相色谱-质谱(GC-MS)联用技术,对环己酮氨肟化体系中失活催化剂上的可溶性沉积物进行了分析.分析液样品的制备采用了HF溶解-乙醚萃取法.GC条件:HP-5型石英毛细管色谱柱(30 m× 0.25 mm×0.25μm),载气为He,流速为0.8 mL/min;柱箱程序升温,初始温度为40℃,以20℃/min升至2...

Determination of soluble deposits on deactived catalyst of cyclohexanone ammoximation system by gas chromatographymass spectrometry

The soluble deposits on deactived catalyst of cyclohexanone ammoximation system were analyzed by gas chromatography-mass spectrometry（GC-MS）.Sample for analyzing was prepared by HF dissolution and ether extraction method.The GC conditions were as follows： an HP-5 quartz capillary column（30 m× 0.25 mm×0.25 μm）,flowrate of carrier gas helium 0.8 mL/min;oven temperature program started at 40 ℃,then increased to 240 ℃ at a rate of 20 ℃/min,finally held at this temperature for 5 min;inlet temperature 250 ℃,sample volume 0.2 μL.The MS conditions were that electron impact energy of mass spectrometer 70 eV,mass range 10~450 m/z,detector temperature 280 ℃.The result shows that the main soluble deposits on deactived TS-1 are products of cyclohexanone oxidation/ reduction,dimers of cyclohexanone,continuous reaction products of cyclohexanone oxime,tert-butylcyclohexanone and a small quantity of other organic compounds.The testing conclusion might be useful in solvent selection and mechanism investigation of deposits formation on TS-1.