CAJ | 학술논문

通过共沉淀法制备了一系列不同镁铝比的水滑石样品,依据物相分析与热失重实验结果确认了合成的样品具有水滑石结构.以方解石型CaCO_3为内标,对水滑石样品碱性位的CO_2-程序升温脱附(TPD)定量表征进行校正,并比较了不同实验参数对方法精密度的影响.经过各测试参数的敏感性分析证实,用CaCO_3脱附峰面积校正后,水滑石碱密度测量结果的RSD分别由9.7%、12.3%下降为4.3%、7.3%,而汇总分析的RSD可从29.6%下降至6.6%.CO_2-TPD定量分析精密度明显提高,证实了内标法的优势及其应用于固体碱定量表征的可行性.将内标法所得结果与固体碱催化酯交换反应的性能关联,结果发现,水滑石催化性能受到活性相的碱强度与碱密度双重指标的调控,碱强度和碱密度越大,酯交换催化效率越高.
통과공침정법제비료일계렬불동미려비적수활석양품,의거물상분석여열실중실험결과학인료합성적양품구유수활석결구.이방해석형CaCO_3위내표,대수활석양품감성위적CO_2-정서승온탈부(TPD)정량표정진행교정,병비교료불동실험삼수대방법정밀도적영향.경과각측시삼수적민감성분석증실,용CaCO_3탈부봉면적교정후,수활석감밀도측량결과적RSD분별유9.7%、12.3%하강위4.3%、7.3%,이회총분석적RSD가종29.6%하강지6.6%.CO_2-TPD정량분석정밀도명현제고,증실료내표법적우세급기응용우고체감정량표정적가행성.장내표법소득결과여고체감최화지교환반응적성능관련,결과발현,수활석최화성능수도활성상적감강도여감밀도쌍중지표적조공,감강도화감밀도월대,지교환최화효솔월고.
A series of hydrotalcite samples with varied Mg/Al ratios were synthesized by coprecipitation route. Quantitative analysis on the basic sites of hydrotalcite samples was carried out by CO_2-TPD(temperature programmed desorption) technique which was calibrated by calcium carbonate internal standard,and the effects of various experimental factors on the precision of testing results were evaluated. The relative standard deviation(RSD) of the experiments shows that the precision of test is obviously improved under the condition that the internal standard calibration is applied. Moreover,combined with the internal standard quantitative CO_2-TPD-MS technique,the investigation on the catalytic performance of hydrotalcites in transesterification demonstrates that the solid base with the stronger alkalinity and the higher density of basic sites presents the higher catalytic activity.