摘要
制备了交联的聚(2-丙烯酰胺基-2-甲基丙磺酸)(PAMPS)。测定了PAMPS的硫元素含量和H^+密度,用示差扫描量热仪测定了高吸水树脂PAMPS所吸收的结合水和自由水的量。以PAMPS为催化剂和吸水剂,未使用苯等共沸除水剂的条件下,芳香醛和邻二醇反应,合成了缩醛。与传统催化剂酸型732阳离子交换树脂相比较,PAMPS的用量少、催化产物产率更高。PAMPS易与反应物分离,可回收重复利用。测定了PAMPS作为催化剂在反应中吸收的醛、醇、缩醛和水的量。PAMPS易吸附邻二醇和水,吸附的醛和缩醛的量很少。不同条件下,PAMPS吸附的水与未吸附水比值越大,越有利于反应正向进行,产率越高。阐明了催化过程。芳香醛与1,2-丙二醇反应生成的缩醛顺反异构体的比例由1H NMR测定,反式结构量多于顺式结构。
Poly(2-acrylamido-2-methylpropanesulfonic acid)(PAMPS)was prepared.The sulfur element content and H^+ density of PAMPS were determined.The contents of free water and bound water absorbed by superabsorbent PAMPS were determined by differential scanning calorimetry.Acetal by the reaction of aldehyde and diol was synthesized using PAMPS as both catalyst and water-absorbent.Compared with traditional method,toluene was not used to remove water by azeotropy in the reaction.Compared with traditional catalystacidic 732 cation exchange resin,the dose of PAMPS was less,but the yield of product catalyzed by PAMPS was higher.It was easily to separate PAMPS from reaction mixtures,and PAMPS was recyclable.The contents of aldehyde,diol,acetal and water absorbed by PAMPS in the reaction mixtures were determined.The amounts of diol and water absorbed by PAMPS were large,the amounts of aldehyde and acetal absorbed by PAMPS were less.The larger the ratio of water absorbed by PAMPS to water unabsorbed by PAMPS,the higher the yield of acetal.The catalytic procedure was illustrated.There were cis-trans-isomers for acetal of aromatic aldehyde and 1,2-propanediol,the ratio of cis-isomer to that of trans-isomer was determined by 1H NMR,and the amount of trans-isomer was larger than that of cis-isomer.
作者
代红光
赵志浩
师兰
DAI Hong-guang;ZHAO Zhi-hao;SHI Lan(College of Science,Inner Mongolia Agricultural University,Hohhot 010018,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2020年第6期1030-1039,共10页
Chemical Research and Application
基金
国家自然科学基金项目(21607085)资助。
关键词
方法学
催化
吸水剂
methodology
catalysis
water-absorbent