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在5DX-FT型I R红外光谱仪上编制了获得微分光谱的程序。测得了高硅型ZSM-11分子筛在晶化过程中的I R微分光谱。结果表明:原来重叠在1100厘米~(-1)上的1223峰在二次微分谱上得到完全分离,其1100厘米~(-1)峰被分离成1126、1102、1051及980厘米~(-1)等几分峰,而550厘米~(-1)峰被分离成627、590、556、534厘米~(-1)等几个峰,在470厘米~(-1)峰上可以分出474、455、424等峰。在晶化过程中,1223、556、534、454厘米~(-1)等峰基本不发生位移,而1110、1072、796厘米~(-1)等峰有一定程度的位移现象产生。随着晶化时间的增加,这些峰的强度,都很有规律地发生变化;1110,474厘米~(-1)峰在晶化过程中明显地迅速降低,而1223、1051、556、534、454等峰却明显地成长。我们认为556与534厘米~(-1)两个峰是ZSM构型分子筛骨架中两种不同环境的五元环的特征振动;一种是处于分子筛十元环孔道的壁上的五元环以及介于十元环孔道之间的五元环的振动。通过实验我们认为IR微分光谱技术是解析谱峰严重重叠的IR谱图的有效工具,它将为分子筛的研究提供大量的内部结构信息。
In 5DX-FT I R infrared spectrometer prepared on the differential spectrum of the program. The I R differential spectra of high-ZSM-11 molecular sieve during crystallization were measured. The results show that the 1223 peak originally overlapped at 1100 cm -1 was completely separated on the second derivative spectrum and the 1100 cm -1 peak was separated into 1126, 1102, 1051 and 980 cm ~ (- 1), and the peak of 550 cm ~ (-1) was separated into several peaks of 627,590,556 and 534 cm ~ (-1), which could be separated on the peak of 470 cm ~ (-1) 474,455,424 other peaks. In the crystallization process, 1223,556,534,454 cm ~ (-1) peak basically did not shift, while the 1110,1072,796 cm ~ (-1) peak of a certain degree of displacement phenomenon. As the crystallization time increases, the intensity of these peaks changes regularly. The 1110 and 474 cm -1 peaks decrease rapidly and sharply during the crystallization process, while the peaks of 1223, 1051, 556 and 534, 454 other peaks have obviously grown. We consider that the two peaks of 556 and 534 cm -1 are the characteristic vibrations of the five-membered ring in two different environments in the molecular sieve framework of ZSM. One is the five-membered ring on the wall of the molecular sieve ten- Vibration between the five-membered ring between the ten-ring tunnel. Through experiments, we believe that IR differential spectroscopy is an effective tool for resolving the IR spectra of severely overlapping spectral peaks, which will provide a large amount of internal structure information for the study of molecular sieves.