The complex is formed in an aqueous solution system of N-methylpyrrolidone(NMP) and lithium chloride. To scientifically develop the separation technology of this kind of solution system,a detailed study of the characteristics of these complex is quite necessary. However,the structure of this kind of complex has not been reported until now. In this study,the structure of this complex from a sample of the industrial wastewater was characterized initially by 1H NMR spectroscopy. The conditions of forming this complex was simulated and the same complex was successfully synthesized by our experiments. Then,the single crystals of the complex suitable for X-ray diffraction measurements were grown in the mixed solution of CH3OH and CH3CN with the volume ratio of 1∶1 and obtained by slow evaporation in air at low temperature. The analysis of the single-crystal indicates that this complex is constituted by two lithium ions,two NMP molecules,four coordinated water molecules and two chloride ions,showing a distorted tetrahedral configuration. Among them,the distance between the centers of two lithium ions is 2.737(9),and the related Li-O bond lengths are 1.903(5),1.929(5) and 1.960(5),respectively. In addition,the decomplexation method of the NMP-LiCl-H2O complex system has also been explored by experiments in this study.
Gao Ziya,Wang Baorong,Zhou Zheng,Zheng Limin,Zhang Zhibing*.
Structure and decomplexation study of NMP-LiCl-H2O complex[J]. Journal of Nanjing University(Natural Sciences), 2018, 54(4): 672
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参考文献
[1] 谢执中. 优良溶剂——NMP. 河南化工,1988(2):19-22.
[2] 欧玉静,王晓梅,李春雷等. N-甲基吡咯烷酮的应用进展. 化工新型材料,2017,45(8):241-243.(Ouyang Y J,Wang X M,Li C L,et al. Progress on application of N-methyl-2-pyrrolidone. New Chemical Materials,2017,45(8):241-243.)
[3] Bracamonte M V,Lacconi G I,Urreta S E,et al. On the nature of defects in liquid-phase exfoliated graphene. Journal of Physical Chemistry C,2014,118(28):15455-15459.
[4] Ren H M,Ding Y H,Chang F H,et al. Flexible free-standing TiO2/graphene/PVdF films as anode materials for lithium-ion batteries. Applied Surface Science,2012,263:54-57.
[5] Wang Z L,Zhao T,Takei M. Morphological structure characterizations in lithium-ion battery(LIB)slurry under shear rotational conditions by on-line dynamic electrochemical impedance spectroscopy(EIS)method. Journal of the Electrochemical Society,2017,164(9):A2268-A2276.
[6] Do M P,Neut C,Metz H,et al. Mechanistic analysis of PLGA/HPMC-based in-situ forming implants for periodontitis treatment. European Journal of Pharmaceutics and Biopharmaceutics,2015,94:273-283.
[7] Salavagione H J,Sherwood J,De Bruyn M,et al. Identification of high performance solvents for the sustainable processing of graphene. Green Chemistry,2017,19(11):2550-2560.
[8] Li H,Jiang Z J,Cao X L,et al. SPE/GC-MS determination of 2-pyrrolidone,N-methyl-2-pyrrolidone,and N-ethyl-2-pyrrolidone in liquid pesticide formulations. Chromato Graphia,2018,81(2):359-364.
[9] Li H,Jiang Z J,Cao X L,et al. Simultaneous determination of three pesticide adjuvant residues in plant-derived agro-products using liquid chromatography-tandem mass spectrometry. Journal of Chromatography A,2017,1528:53-60.
[10] Park J M,Jung C Y,Yao W,et al. Synthesis of yellow pyridonylazo colorants and their application in dye-pigment hybrid colour filters for liquid crystal display. Coloration Technology,2017,133(2):158-164.
[11] Niu H J,Wang C,Bai X D,et al. New perylene polyimides containing p-n diblocks for sensitization in TiO2 solar cells. Polymers for Advanced Technologies,2004,15(12):701-707.
[12] Koslitz S,Meier S,Schindler B K,et al. Biomonitoring of N-ethyl-2-pyrrolidone in automobile varnishers. Toxicology Letters,2014,231(2):142-146.
[13] Tiano A L,Gibbons L,Tsui M,et al. Thermodynamic approach to boron nitride nanotube solubility and dispersion. Nanoscale,2016,8(7):4348-4359.
[14] Van Thriel C,Blaszkewicz M,Schper M,et al. Chemosensory effects during acute exposure to N-methyl-2-pyrrolidone(NMP). Toxicology Letters,2007,175(1-3):44-56.
[15] kesson B,Jnsson B A G. Biological monitoring of N-methyl-2-pyrrolidone using 5-hydroxy-N-methyl-2-pyrrolidone in plasma and urine as the biomarker. Scandinavian Journal of Work,Environment & Health,2000,26(3):213-218.
[16] Ishii J,Akamatsu T. Organo-soluble low CTE polyimides and their applications to photosensitive cover layer materials in flexible printed circuit boards. High Performance Polymers,2009,21(2):123-128.
[17] Shimomura T,Yoshida K,Ito K,et al. Insulation effect of an inclusion complex formed by polyaniline and beta-cyclodextrin in solution. Polymers for Advanced Technologies,2000,11(8-12):837-839.
[18] Tanaka K,Oharada K,Yamada D,et al. Fatigue crack propagation in short-carbon-fiber reinforced plastics evaluated based on anisotropic fracture mechanics. International Journal of Fatigue,2016,92:415-425.
[19] Lee S W,Lee J,Choi H S,et al. Synthesis and analysis of flow modifiers for PPS flowability enhancement. Polymer-Korea,2017,41(5):889-895.
[20] 吴彦彬,刘俊广,宋国全等. 萃取法回收生产聚苯硫醚废液中的N-甲基吡咯烷酮溶剂的研究. 精细与专用化学品,2015,23(11):20-22.(Wu Y B,liu J G,Song G Q,et al. Study on extraction recovery of N-methy-2-pyrrplidone from waste liquid of the production process of p-phenylene sulfide. Fine and Specialty Chemicals,2015,23(11):20-22.)
[21] Zhou Q,Yang P. Crystal structure and DNA-binding studies of a new Cu(Ⅱ)complex involving benzimidazole. Inorganica Chimica Acta,2006,359(4):1200-1206.
[22] You S,Chen X T,Zheng C G,et al. Synthesis,crystal structure and properties of the dimeric copper(Ⅱ)complex,[Cu2(Hboa)2(H2O)2]?(ClO4)2,(H2boa=biacetyl oxime azine). Transition Metal Chemistry,2001,26(3):247-251.
[23] Dong H,Liu X,Yang J,et al. Assembling of transitional metal CuⅡ,and MnⅡ,with 4-pyridin-2-yl-pyrimidine-2-sulfonate adjusted by anions. Transition Metal Chemistry,2007,32(4):518-522.
[24] Rappoport Z,Marek I. 7. The lithium metal reduction of π-conjugated hydrocarbons and fullerenes. The chemistry of organolithium compounds. Hoboken:John Wiley & Sons,Ltd,2006,477-523.
[25] 彭雨新,甘逸涛,陶 涛等. 5,6-位烷氧基保护和3-/3,8-位三苯胺拓展1,10-菲咯啉衍生物与银离子识别. 无机化学学报,2017,33(11):2075-2082.(Peng Y X,Gan Y T,Tao T,et al. 5,6-alkoxyl protected and 3-/3,8-triphenylamine extended 1,10-phenanthroline derivatives and their selective silver ion recognition. Chinese Journal of Inorganic Chemistry,2017,33(11):2075-2082.)