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N,N'-二(5,5-二甲基-2-磷杂-2-硫代-1,3-二噁烷-2-基)乙二胺的热分解动力学研究 总被引:3,自引:0,他引:3
以TG-DTG为手段, 研究了N,N'-二(5,5-二甲基-2-磷杂-2-硫代-1,3-二噁烷-2-基)乙二胺(DPTDEDA)在氮气气氛中的热分解动力学, 利用 Kissinger法、Flynn-Wall-Ozawa(FWO)法对DPTDEDA进行了动力学分析, 求出了该物质的热分解动力学参数, 同时利用Satava-Sestak法研究了该物质的热分解机理. 结果表明, Kissinger法所求得的表观活化能为137.37 kJ•mol-1, 指前因子ln A=28.00; Flynn-Wall-Ozawa法所求得的活化能为139.83 kJ•mol-1. DPTDEDA的热分解机理为相边界反应, 其动力学方程为G(α)=1-(1-α)4, 反应级数n=4. 相似文献
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用TG-DTG-DSC热分析技术研究了三(O,O′-二异丙基二硫代磷酸酯)合钴(Ⅲ)、双(O,O′-二乙基二硫代磷酸酯)合镍(Ⅱ)及其后者与吡啶或4-甲基吡啶加合物在氮气气氛中的热行为;用传统的微商法(A-B-S)和积分法(C-R法)以及分别由Malek、Dollimore提出的两种新型的热分析动力学方法协同处理TG数据,获得了四种配合物的热分解反应动力学参数E和A,确定了反应机理。对它们的热行为和分子结构之间的关系进行了讨论;并试就本文所用的几种数据处理方法作了比较。 相似文献
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α-乙酰基二硫缩烯酮α碳原子的酰化反应 总被引:1,自引:0,他引:1
进行了α-乙酰基二硫缩烯酮与酰氯的酰化反应. 以干燥的二氯甲烷为溶剂, 在四氯化钛催化下, α-乙酰基环二硫缩烯酮(1)可与脂肪及芳酰氯(2)反应, 在化合物1的α-碳原子上发生酰化反应, 以较高的产率生成各种α-乙酰基-α-酰基二硫缩烯酮(3). 相似文献
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以TG-DTG为手段, 研究了N,N′-二(5,5-二甲基-2-磷杂-2-硫代-1,3-二噁烷-2-基)乙二胺(DPTDEDA)在空气中的热分解动力学,利用Friedman法、Flynn-Wall-Ozawa(FWO)法对DPTDEDA进行了动力学分析, 求出了该物质两个主要的热分解阶段的热分解动力学参数, 同时利用Coats-Redfern法、Achar法研究了该物质的热分解机理. 结果表明, 用Friedman法所求得的两个热分解阶段的表观活化能的平均值分别为128.03和92.59 kJ•mol-1; 而Flynn-Wall-Ozawa法所求得的两个热分解阶段的表观活化能的平均值分别为138.75和106.78 kJ•mol-1. 由Coats-Redfern法、Achar法得出DPTDEDA在空气中的热分解过程虽主要分为两段反应, 但经过推理其反应机理函数却是相同的, 为f(α)=3/2(1-α)4/3[(1-α)-1/3-1]-1. 相似文献
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基于热重分析、微商热重分析及示差热分析研究了N,N′-二苯胺基己二酰胺β-晶型成核剂在空气气氛中的热分解动力学;通过利用Friedman方程和Flynn-Wall-Ozawa(FWO)方程对其热分解过程进行动力学分析求得了其热分解表观活化能;同时利用Achar-Brindly-Sharp方程和Coats-Redfern方程研究了其热分解机理,用等温热重分析法测得了失重10%时的寿命方程.结果表明,N,N′-二苯胺基己二酰胺β-晶型成核剂的表观活化能为138.66kJ.mol-1,其热分解反应的机理函数符合Mample法则,反应级数n=3/2,动力学方程为G(α)=α3/2,寿命方程为:lnτ=-51.877+2.922 2×104/T. 相似文献
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α-硝基二硫缩烯酮的制备 总被引:1,自引:0,他引:1
近年来,结合烷硫基对α-羰基二硫缩烯酮反应的调控作用,我们开展了α-羰基二硫缩烯酮/二硫缩烯酮α-官能化(或α-位修饰)的研究,以期扩展二硫缩烯酮在合成中的应用。在用α-碘代脱羧和α-溴代脱乙酰基反应分别成功地制备了α-碘代-α’-肉桂酰基二硫缩烯酮Ⅲ和α-溴代二硫缩烯酮嘲的基础 相似文献
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双(6,7-二甲硫基四硫富瓦烯-2,3-二硫)金属配合物的合成 总被引:5,自引:0,他引:5
以6,7-二甲硫基四硫富瓦烯-2,3-二硫盐为配体合成了3种未见文献报道的双(6,7-二甲硫基四硫富瓦烯-2,3-二硫)金属配合物,为“桥式”四硫富瓦烯衍生物的合成创造出一种新方法,并对只得到中性产物提出了合理的解释。研究了其IR及室温电导率。 相似文献
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Crystal of the complex Ni2L (ClO4)2 was obtained by reaction of Ni(ClO4)2 and macrocyclic ligand H2L, where L2– is the dinucleating macrocycle with two 2,6-di(aminomethyl)-4-methyl phenolate entities combined by the same two lateral chains, –(CH2)2–NH–(CH2)2–, at the amino nitrogens. The thermal decomposition processes of the title complex were studied in a dynamic atmosphere of dry argon using TG-DTG. The kinetic analysis of the first and second thermal decomposition steps were performed via the TG-DTG curves, and the kinetic parameters were obtained from analysis of the TG-DTG curves with integral and differential methods. The most probable kinetic function was suggested by comparison of the kinetic parameters.This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献
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Chromium(III)isanessentialtraceelement.Inanactiveform.chronlium(III)asacomponentofglucosetolerancefactor(GTF)canimproveinsulinbiologicalactivity.CrsupplementationinhumansandanimalsreducessymptomsofTypeIIdiabetesandhypoglycemia.Forabetterunderstandingofthenatureofbiologicallyactivechromium(ill)complex,manyGTFmodelcomplexeshavebeenstudiedpreviously'.Here,oneGTFmodelcomplexofN,N'-ethylenebis(salicylideneiminato)diaquochromium(ill)chloride,[Cr(salen)(H,O)=]CIwaspreparedandcharacterized.a… 相似文献
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Daqing Wang Baoxue Zhou Yuanjang Jia Feng Shi Yiping Fan 《Journal of Thermal Analysis and Calorimetry》1995,45(1-2):221-226
The complex Mn(Nica)2Cl2 (Nica=nicotinamide) was prepared, and its decomposition was studied by means of TG and DSC. The IR spectra of the products
of thermal decomposition were examined at every stage. Kinetic analysis of the first stage of thermal decomposition was performed
via the TG-DTG curves, and the kinetic parameters were obtained from analysis of the TG-DTG curves with integral and differential
methods. The most probable kinetic function was suggested from a comparison of the kinetic parameters. Mathematical expressions
were derived for the kinetic compensation effect.
Zusammenfassung Der Komplex Mn(Nica)2Cl2 (Nica steht für Nikotinamid) wurde hergestellt und seine Zersetzung mittels TG und DSC untersucht. Die thermisch zersetzten Substanzen jedes Schrittes wurden mittels IR-Spektren untersucht. Anhand der TG-DTG-Kurven erstellte man eine kinetische Analyse des ersten Schrittes der thermischen Zersetzung, die kinetischen Parameter wurden aus den TG-DTG-Kurven unter Einsatz von Integrations- und Differentialmethoden ermittelt. Durch Vergleich der kinetischen Parameter wurde die wahrscheinlichste kinetische Funktion vorgeschlagen. Mathematische Ausdrücke für den kinetischen Kompensationseffekt wurden erhalten.相似文献
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Thermal Decomposition Kinetics and Mechanism of Tb(Ⅲ) m-Methylbenzoate Complex with 1,10-Phenanthroline in Static Air Atmosphere 总被引:3,自引:0,他引:3
ZHANG Jian-jun ** WANG Rui-fen ZHANG Jian-ling WANG Shu-ping . Experimental Center Hebei Normal University Shijiazhuang P. R. China . Department of Chemistry Hebei Normal University Shijiazhuang . P. R. China . 《高等学校化学研究》2002,18(1):25-29
IntroductionThe rare- earth carboxylic acid complexes havemany special structures and interesting spectro-scopic properties,which are of great interestin ex-traction,separation,germicide preparation,catal-ysis,luminescence and functional material prepara-tion.The preparation,crystal structure,fluores-cence spectroscopy and thermal properties of somerare- earth carboxylic acid complexes have beenstudied[1— 8] . In this work,on the basis of thestructural and fluorescence spectroscopicresearches… 相似文献
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Summary: An amorphous grade Poly (lactic acid) (PLA) was selected for an accelerated burial in soil test during 450 days. Thermogravimetric analyses were carried out to study the effects of degradation in soil on the thermal stability and the thermal decomposition kinetics. A single stage decomposition process is observed for all degradation times. It is shown that the thermal stability of PLA is slightly affected by degradation in soil. Concerning the study of the thermal decomposition kinetics, Criado master curves were plotted from experimental data to focus the study of the thermodegradation kinetic model.The kinetic methods proposed by Broido and Chang were used to calculate the apparent activation energies (Ea) of the degradation mechanism. These results were compared to the Ea values obtained by the method developed by Coats and Redfern in order to prove the applicability of the former methods to the kinetic study. As expected, non-linear tendency is found out for Ea variation along the degradation times, which can be explained as an evolution by stages. 相似文献
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Chen Donghua Yuan Yuhong Peng Zhenghe Jian Lihua Pan Qingcai Qin Zibin 《Thermochimica Acta》1998,320(1-2):291-295
Studies of the non-isothermal decomposition of M (mnt) (5-NO2-phen) (M=CoII, CuII, ZnII) were carried out by thermogravimetry. The thermal decomposition mechanisms and associated kinetics have been investigated. The kinetic parameters were obtained from an analysis of the TG–DTG curves by integral and differential methods. The most probable kinetic model functions were suggested by comparison of the kinetic parameters. Mathematical expressions for the kinetic compensation effect were derived. 相似文献
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Non-isothermal kinetics of the thermal degradation of poly(vinyl chloride) (PVC) prepared by a living radical polymerization (LRP) method was performed and compared with the results obtained from PVC prepared by the conventional free-radical process (FRP). Both differential and integral isoconversional methods were applied for determining the apparent activation energy of the dehydrochlorination stage. This study made clear noticeable differences in the thermal degradation of the PVC samples under analysis. The newly synthesized LRP-PVC material has a better thermal stability and presents substantial differences in the macroscopic kinetics of the dehydrochlorination process compared with conventional FRP-PVC. These differences were assessed in quantitative terms on the basis of the kinetic triplet [Ea,A,f(α)]. 相似文献
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J. J. Zhang L. G. Ge X. L. Zhang Y. J. Dai H. L. Chen L. P. Mo 《Journal of Thermal Analysis and Calorimetry》1999,58(2):269-278
The thermal decomposition of Zn[NFA]25H2O (NFA=C16H18FN3O3, norfloxacin) and its kinetics were studied under non-isothermal conditions in air by TG-DTG and DTA methods. The intermediate and residue for each decomposition were identified from the TG curve. The non-isothermal kinetic data were analyzed by means of the Achar method and the Madhusudanan-Krishnan-Ninan (MKN) method. The possible reaction mechanisms were investigated by comparing the kinetic parameters. The kinetic equation for the second stage can be expressed as d/dt=Aexp(–E/RT)(1–).This revised version was published online in November 2005 with corrections to the Cover Date. 相似文献