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探究了用二甲基亚砜(DMSO)氧化法对低分子质量聚乙二醇(PEG200~PEG1000)端羟基进行醛基化改性的工艺条件,发现使用“接种”的方法可有效提高低分子质量醛基化产物(Aldehyde-PEG-Aldehyde,APA)的析出产率。试验采用盐酸羟胺法对产物的醛基含量进行了检测,并进一步用红外光谱和核磁共振对产物APA进行了结构鉴定。通过对反应温度和DMSO氧化剂用量的考察,得到了制备低分子质量醛基化产物的最适反应温度、以及APA醛基含量与氧化剂(DMSO)用量之间的定量关系规律。
The process conditions for aldehyde modification of hydroxyl groups of low molecular mass polyethylene glycol (PEG200 ~ PEG1000) by dimethyl sulfoxide (DMSO) oxidation were explored. It was found that the method of “inoculation” could be effectively improved Precipitation yield of low molecular mass aldehyde-product (Aldehyde-PEG-Aldehyde, APA). The aldehyde content of the product was detected by the hydroxylamine hydrochloride method, and the structure of the product APA was further identified by infrared spectroscopy and nuclear magnetic resonance. Through the investigation of the reaction temperature and the amount of the oxidant, the optimal reaction temperature and the quantitative relationship between the amount of APA and oxidant (DMSO) were obtained.