| The analysis methods of impurities possible existed in monomer DAC solution were studied in this paper.Firstly, based on the literatures and existing foundation work in our group,15sorts of impurities, such as dimethylamine and others, possible existed in monomer solution were confirmed according to the impurity sources, and then classified into four categories on the basis of their volatility. The corresponding analysis methods were constructed for the different sorts of the impurities respectively. Here,6sorts of volatile impurities such as dimethylamine, methanol could be analyzed by gas chromatography. Acrylic acid with strong polarity might be analyzed by high performance liquid chromatography (HPLC). Organic amine salts such as acrylate of dimethylamine could be analyzed by gas chromatography after being changed into corresponding volatile amine. Involatile impurities PEG and choline chloride could be analyzed by visual spectrophotometry and difference method, respectively. Meanwhile, the precisions and the recovery rates of the methods were valuated and their reliability were fully verified.Secondly, a extraction method for7sorts of volatile impurities and3sorts of organic amine salts possible existed in monomer DAC solution was constructed by liquid-liquid extraction. Meanwhile, the reliability of the extraction was valuated.Finally, the impurities existed in monomers DAC solution both from lab-made and industry were analyzed practically by the constructed methods, so that the applicability of the above methods were well verified.The analytical method for all volatile impurities, invertible organic amine salts, part of involatile impurities, and the extraction method for volatile impurities were established based on above researches. The completed research work have constructed an essential basement for optimizing the monomer preparation and monomer purification, researching the influence of impurities in monomer on polymerization, and establishing the quality standard of monomers. |
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