Multistage kinetic analysis of DMAA/MBAM polymer removal from gelcast ceramic parts using a multi-stage parallel reaction model and model-free method.
Multistage kinetic analysis of DMAA/MBAM polymer removal from gelcast ceramic parts using a multi-stage parallel reaction model and model-free method.
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本工作旨在开发一种有效的方法来研究从凝胶铸造陶瓷零件中去除N，N-二甲基丙烯酰胺/N，N‘-亚甲基双丙烯酰胺(DMAA/MBAM)聚合物的多级脱脂动力学和反应机理。采用热重分析(TG)和裂解气相色谱/质谱仪(Py-GC/MS)研究了DMAA/MBAM聚合物在绿色组分中的热降解特性和热解产物。提出了一个多阶段平行反应模型来分离dα/dt曲线中的重叠峰。利用无模型方法(Flynn-Wall-Ozawa、Starink、Friedman和KisSinger-Akahira-Sunose)和活化能变量模型计算了各阶段的动力学参数(活化能E和指前因子k0)。此外，还利用Málek过程和α的ŠEsták-Berggren(SB)模型，分析和讨论了各阶段最合适的动力学机理函数f(Sp)。结果表明，通过三阶段平行反应模型(3-PRM)，可以将绿色组分中的DMAA/MBAM聚合物燃耗分为三个子阶段。1~3期的E(α)=139.862−110.481α+156.161α2−88.714α3kJ−1，E(α)=160.791+152.496α−236.906α2+163.724α3 kJ mol−1，E(α)=72.132+452.830α−669.039α2+507.015α3 kJ ol−1。从第1级到第3级，E的平均值呈递增趋势，各亚级的E与k0之间也存在动态补偿效应。动力学机理分析表明，第1、3阶段的反应机理分别为f(α)=(1−α)0.668α3.049(−ln(1−α))−3.874)，f(α)=(1−α)0.700α3.177(−ln(1−α))−3.962)和f(α)=(1−α)1.049α−0.161(−ln(1−α))0.518)。该研究成果可望推广到各种胶体成型技术中粘结剂或聚合物的复合脱脂研究。本工作旨在开发一种有效的方法来研究从凝胶注模陶瓷制品中去除DMAA/MBAM聚合物的多级脱脂动力学和反应机理。
This work aims to develop an effective method for investigating the multistage debinding kinetics and reaction mechanisms of removing N,N-dimethylacrylamide/N,N′-methylenebisacrylamide (DMAA/MBAM) polymer from gelcast ceramic parts. Thermogravimetry (TG) and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) experiments were performed to investigate the thermal degradation characteristics and the main compounds produced during the pyrolysis of DMAA/MBAM polymer within green components. A multi-stage parallel reaction model (M-PRM) was proposed to separate the overlapping peaks in the dα/dT curves. The kinetic parameters (activation energy E and pre-exponential factor k0) of each substage were calculated using model-free methods (Flynn–Wall–Ozawa, Starink, Friedman and Kissinger–Akahira–Sunose) and an activation energy variable model. In addition, the most appropriate kinetic mechanism function f(α) of each substage was analyzed and discussed via Málek's procedure and the Šesták–Berggren (SB) model. The results showed that the DMAA/MBAM polymer burnout in green components can be divided into three substages through a three-stage parallel reaction model (3-PRM). The values of E (Friedman method) for substages 1 to 3 were E(α) = 139.862 − 110.481α + 156.161α2 − 88.714α3 kJ mol−1, E(α) = 160.791 + 152.496α − 236.906α2 + 163.724α3 kJ mol−1 and E(α) = 72.132 + 452.830α − 669.039α2 + 507.015α3 kJ mol−1, respectively. The average values of E showed an increasing tendency from substages 1 to 3, and a kinetic compensation effect was also observed between the E and k0 in each substage. The kinetic mechanism analysis revealed that the reaction mechanisms for substages 1 to 3 were f(α) = (1 − α)0.668α3.049(−ln(1 − α))−3.874, f(α) = (1 − α)0.700α3.177(−ln(1 − α))−3.962 and f(α) = (1 − α)1.049α−0.161(−ln(1 − α))0.518, respectively. It is expected that the research results can be extended to investigate the multiplex debinding of binders or polymers for various colloidal molding techniques. This work aims to develop an effective method to investigate the multistage debinding kinetics and the reaction mechanisms of removing DMAA/MBAM polymer from gelcast ceramic parts.
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