药用辅料交联聚乙烯吡咯烷酮的合成

Synthesis of cross-linked polyvinylpyrrolidone for pharmaceutical excipients

以2-咪唑烷酮为原料,合成了1,3-二乙烯-2-咪唑烷酮(DVI)并进行了表征.结果表明,4-二甲氨基吡啶(DMAP)的比例对DVI的收率有很大影响;同时考察了自制的DVI与乙烯基吡咯烷酮(NVP)的爆米花聚合反应,并进行了相应表征.发现DVI用量在1%~2%范围内时,爆米花聚合非常容易进行,且随着DVI用量的增加,聚合物的交联程度也逐渐增加,但对水的溶胀度却下降.

Cross-linked polyvinyl pyrrolidone(PVPP)is a kind of cross-linked polymer that is insoluble in water,strong acid,strong base,and common organic solvents.PVPP is polymerized from vinyl pyrrolidone(NVP)monomer under specific conditions.It can be swollen by water,and has a non-toxic,physiologically inert,and strong adsorption capacity.Due to its special properties,PVPP is widely used in the food and pharmaceutical industries.Few research has been reported on the polymer,mainly patents,and the mechanism of its reaction is unclear.At present,in situ polymerization is the most commonly used production method in China.Because of the alkali and high-temperature reaction,the product is easy to color,which has a great influence on the yield and quality of the product,and the swelling degree and particle size are difficult to control.In order to solve these problems,1,3-divinyl-2-imidazolone(DVI)was successfully synthesized from 2-imidazolone as a cross-linking agent for popcorn polymerization.The structure of the product was characterized,and the effect of catalyst 4-dinethylaminopyridine(DMAP)on the reaction yield was explored.The results show that the higher the dosage of DMAP,the higher the yield of DVI.In summary,we successfully synthesized the crosslinking agent DVI and obtained the best synthesis method:reaction temperature was controlled at 100℃,and the mole of DMAP was twice or more than that of 2-imidazolane,consistent with the amount of ethylene propionate.Under these conditions,the yield of DVI was 33%and the separation purity was more than 98%by chromatography.The role of DVI in NVP popcorn polymerization was also investigated,and it was found that popcorn polymerization was easier when DVI was in the 1%to 2%range.As the amount of DVI increased,the resulting popcorn polymers were more crosslinked,had higher accumulation density,and were less soluble in water.