通过红外光谱在线监测1,5-二乙酰基-3,7-二硝基-1,3,5,7-四氮杂环辛烷(简写DADN)合成奥克托今(HMX)的反应过程,利用渐进因子分析(EFA)、多元曲线分辨-交替最小二乘法(MCR-ALS)和直观推导式演进特征投影法(HELP)等化学计量学方法对反应过程获得的光谱信息进行解析,得到了各组分浓度变化曲线和对应的红外光谱,并将MCR-ALS和HELP两种方法的分析结果进行比较,得出可相互验证的一致结论,从而推测出该反应合理的反应机理.所得结果与文献报道吻合,表明化学计量学方法结合在线红外光谱是研究奥克托今合成机理的有效手段.
参考文献
| [1] | SONG Hongyan,WANG Peng,TAN Guangming,et al.Reaction Mechanism of One-Pot Synthesis of Dinitro Pentamethylene Tetramine[J].Chinese J Org Chem,2010,30(3):414-418(in Chinese).宋红燕,王鹏,覃光明,等.一锅法合成二硝基五亚甲基四胺反应机理的研究[J].有机化学,2010,30(3):414-418. |
| [2] | LI Quanliang.Study on the Technology of Synthesis of HMX[D].Shanxi:North University of China,2007(in Chinese).李全良.奥克托今的合成工艺研究[D].山西:中北大学,2007. |
| [3] | Li H,Zhang F,Josef Hovel.Quantification of Analyses in Overlapping Peaks from Capillary Electrophoresis Using Multivariate Curve Resolution-Alternating Least Squares Methods[J].Electrophoresis,2003,V24(18):3107-3115. |
| [4] | WANG Kang,ZHANG Fang,LI Hua.Analysis of the Catalytic Process of Enzyme by Using Heuristic Evolving Latent Projection(HELP)[J].Acta Chim Sin,2007,65(15):1493-1498(in Chinese).王康,张方,李华.直观推导式演进特征投影法对酶催化反应的过程分析[J].化学学报,2007,65(15):1493-1498. |
| [5] | Esteves da Silva J C G,Machado A A S C.Evolving Factor Analysis of Synchronous Fluorescence Spectra of Humic Substances in the Presence of Cu(Ⅱ)[J].Chemom Intell Lab Syst,1995,27:115. |
| [6] | Dohnal V,Zhang F,Li H,et al.Quantitative Chiral Analysis in Capillary Electrophoresis from Unresolved Peaks Using Derivative Electropherograms,Experimental Design,and Artificial Neural Networks[J].Electrophoresis,2003,V24(15):2462-2468. |
| [7] | Zhang F,Chen Y,Li H.Application of Multivariate Curve Resolution-Alternating Least Square Methods on the Resolution of Overlapping CE Peaks from Different Separation Conditions[J].Electrophoresis,2007,V28(20):3674-3683. |
| [8] | Bezemer E,Rutan S C.Analysis of Three-way and Four-way Data Using Multivariate Curve Resolution-Alternating Least Squares with Global Multi-way Kinetic Fitting[J].Chemom Intell Lab Syst,2006,81:82-93. |
| [9] | Pasamontes A,Callao M P.Determination of Amoxicillin in Pharmaceuticals Using Sequential Injection Analysis and Multivariate Curve Resolution[J].Anal Chim Acta,2004,V515(1):159-165. |
| [10] | QI Yunpeng,WU Yutian,LI Tonghua.Heuristical Evolving Latent Projections(HELP) and Its Application in Multicomponent Systems[J].J Anal Sci,2003,19(2):175-178(in Chinese).亓云鹏,吴玉田,李通化.直观推导式演进特征投影法及其在复杂体系分析中的应用[J].分析科学学报,2003,19(2):175-178. |
| [11] | Kvalheim O M,Liang Y Z.Heuriatical Evolving Latent Projections:Resolving Two-way Multicomponent Data[J].Anal Chem,1992,64(8):936-946. |
| [12] | Keller H,Massart D,Liang Y Z,et al.A Comparison of the Heuristic Evolving Latent Projections and Evolving Factor Analysis Methods for Peak Purity Control in Liquid Chromatography with Photodiode Array Detection[J].Anal Chim Acta,1992,V267(1):63-67. |
| [13] | DU Canping,LIANG Wensheng,LIU Lusheng,et al.Summary of the Seminar on "the Strategies for Developing China's Organic Chemistry in 21st Century"[J].Prog Chem,2001,13(4):323-327(in Chinese).杜灿屏,梁文生,刘鲁生,等."21世纪中国有机化学发展战略"研讨会纪要[J].化学进展,2001,13(4):323-327. |
| [14] | Azzouz T,Tauler R.Application of Multivariate Curve Resolution Alternating Least Squares(MCR-ALS) to the Quantitative Analysis of Pharmaceutical and Agricultural Samples[J].Talanta,2008,V74(5):1201-1210. |
| [15] | Winning H,Larsan F H,Bro R,et al.Quantitative Analysis of NMR Spectra with Chemometrics[J].J Magn Reson,2008,V190(1):26-32. |
| [16] | LI Ting,MENG Zihui,WANG Bozhou,et al.Using Multivariate Curve Resolution and Infrared Spectroscopy for Researching the Synthesizing Reaction Mechanism of 1,5-Methylene-3,7-dintro-1,3,5,7-tetraazacyclooctane[J].Acta Chim Sin,2010,68(20):2104-2110(in Chinese).李婷,孟子晖,王伯周,等.多元曲线分辨等方法和红外光谱用于二硝基五亚甲基四胺的合成反应机理研究[J].化学学报,2010,68(20):2104-2110. |
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