[K(HTNR)(H_2O)]_n的制备、晶体结构和热分解机理  

Preparation, Crystal Structure and Thermal Decomposition Mechanism of [K(HTNR)(H_2O)]_n

作　　者：李玉锋[1] 张同来[1] 张建国[1] 马桂霞[1] 宋江闯[1] 郁开北[2] 

机构地区：[1]北京理工大学机电工程学院,北京100081 [2]中国科学院成都分院分析测试中心,成都610041

出　　处：《化学学报》2003年第7期1020-1024,共5页Acta Chimica Sinica

摘　　要：通过2,4,6-三硝基间苯二酚(斯蒂芬酸,TNR)与氢氧化钾在乙醇溶液中反应,首次合成出配位聚合物[K(HTNR)-(H_2O)]n,并测定了其晶体结构.该晶体属单斜晶系,P2_1/c空间群;晶胞参数:a=0.7888(1)nm,b=1.3800 (2) nm,c=0.9520(1)nm,β=8.91(1)°;V=1.0238(2)nm^3;D_c=1.954 g/cm^3;Z=4;F(000)=608;μ(Mo K_α)=0.575 mm^(-1) .用DSC,TG-DTG及FT-IR等分析方法研究了该配位聚合物的热分解机理.在线性升温条件下,该配合物的热分解包含两个重叠的弱吸热过程和两个强放热分解过程.分解残渣的红外分析表明,在271.9℃时,分解残渣中有KNCO与羧酸钾,357.1℃时,残渣中只有KNC存在.The new coordination polymer of potassium 2; 4, 6-trinitroresorcinate, [K(HTNR) (H2O)](n), was prepared by reacting 2, 4, 6-trinitroresorcinol with potassium hydroxide in alcohol solution. Its crystal structure was determined by X-ray single crystal diffraction analysis. The crystalline belongs to monoclinic with space group P2(1)/c. Its unit cell parameters are as follows: a = 0.7888(1) nm, b = 1.3800(2) nm, c = 0.9520(1) nm, beta = 8.91(1)degrees, V = 1.0238 (2) nm(3), D-c = 1.954 g/cm(3), Z = 4, F (000) = 608, mu ( Mo Ka) = 0.575 mm(-1). The thermal decomposition mechanism of the. complex was studied by using differential scanning calorimetry (DSC), thermogravimetry-derivative thermogravimetry (TG-DTG) and FT-IR techniques. At the linear heated rate the thermal decomposition of the complex contained two overlapped weak endothermic and two. intense exothermic processes. There are KNCO and RCOOK at 271. 9 degreesC, and KNC at 357.1 degreesC in the residue according to FT-IR analysis.

关 键 词：[K(HTNR)(H2O)]n 制备 晶体结构 热分解机理 2 4 6-硝基间苯二酚 钾配位聚合物 

分 类 号：O625[理学—有机化学]