Shahi Mahrzadi Noureen, Arshad Muhammad, Ullah Aman
Department of Agricultural, Food and Nutritional Sciences, University of Alberta, Edmonton, AB T6G 2P5, Canada.
Department of Chemistry, The Islamia University of Bahawalpur, Bahawalpur 63100, Pakistan.
Materials (Basel). 2017 Mar 20;10(3):315. doi: 10.3390/ma10030315.
Solvent-free copolymerization of epoxides derived from fatty esters of waste cooking oil with phthalic anhydride using (salen)CrCl as catalyst and n-Bu₄NCl/DMAP (tetrabutylammonium chloride/4-(dimethylamino)pyridine) as co-catalysts was carried out for the first time under microwave irradiation, where reaction time was reduced from a number of hours to minutes. The polyesters were obtained with molecular weight (w = 3100-6750 g/mol) and dispersity values (D = 1.18-1.92) when (salen)CrCl/n-Bu₄NCl was used as catalysts. Moreover, in the case of DMAP as a co-catalyst, polyesters with improved molecular weight (w = 5500-6950 g/mol) and narrow dispersity values (D = 1.07-1.28) were obtained even at reduced concentrations of (salen)CrCl and DMAP. The obtained products were characterized and evaluated by attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR), proton nuclear magnetic resonance (¹H-NMR) spectroscopy, gel permeation chromatography (GPC), thermogravimetric analysis (TGA) and differential scanning calorimetric (DSC) Techniques.
首次在微波辐射下,以(salen)CrCl为催化剂、n-Bu₄NCl/DMAP(四丁基氯化铵/4-(二甲氨基)吡啶)为共催化剂,使废食用油脂肪酸酯衍生的环氧化物与邻苯二甲酸酐进行无溶剂共聚反应,反应时间从数小时缩短至数分钟。当使用(salen)CrCl/n-Bu₄NCl作为催化剂时,得到的聚酯分子量(w = 3100-6750 g/mol)和分散度值(D = 1.18-1.92)。此外,在使用DMAP作为共催化剂的情况下,即使在(salen)CrCl和DMAP浓度降低的情况下,也能获得分子量提高(w = 5500-6950 g/mol)且分散度值较窄(D = 1.07-1.28)的聚酯。通过衰减全反射-傅里叶变换红外光谱(ATR-FTIR)、质子核磁共振(¹H-NMR)光谱、凝胶渗透色谱(GPC)、热重分析(TGA)和差示扫描量热法(DSC)技术对所得产物进行了表征和评估。