CAJ | 학술논문

文章将蔗糖八乙酸酯的合成和分离提纯相结合,阐明了制备高纯度SOA的途径.采用无水吡啶为催化剂能够有效提高SOA的产率及粗产物的纯度,并讨论了反应条件对合成的影响,得出最佳反应条件为:蔗糖、乙酸酐、催化剂的摩尔比为1∶11∶0.8,保温时间120 min,反应温度130～135℃.采用醇-水重结晶的方法进行粗产物的提纯,当乙醇体积分数为25%～45%时,SOA易结晶析出,能够缩短重结晶的时间,提高产品回收率.重结晶6次后SOA纯度可达约99.9%,继续重结晶对纯度提高影响不大.采用IR、DSC、GC-MS、~1H NMR对SOA进行了表征.高纯度SOA满足了在国防上的应用,对标准物质的制备奠定了基础.
문장장자당팔을산지적합성화분리제순상결합,천명료제비고순도SOA적도경.채용무수필정위최화제능구유효제고SOA적산솔급조산물적순도,병토론료반응조건대합성적영향,득출최가반응조건위:자당、을산항、최화제적마이비위1∶11∶0.8,보온시간120 min,반응온도130～135℃.채용순-수중결정적방법진행조산물적제순,당을순체적분수위25%～45%시,SOA역결정석출,능구축단중결정적시간,제고산품회수솔.중결정6차후SOA순도가체약99.9%,계속중결정대순도제고영향불대.채용IR、DSC、GC-MS、~1H NMR대SOA진행료표정.고순도SOA만족료재국방상적응용,대표준물질적제비전정료기출.
High purity sucrose octaacetate(SOA) has been prepared by the combination of its synthesis and purification. Sucrose octaacetate was synthesized by the reaction between sucrose and acetic anhydride in the presence of anhydrous pyridine which reduced the amounts of by-products and improved yield to 96%. The optimum experiment conditions were as follows:molar ratio of sucrose to anhydride and pyridine 1∶11∶0.8, reaction temperature 130～135℃,and holding time 120 min. Compared with other catalysts, the anhydrous pyridine resulted in the best purity of SOA raw product which is determined by gas chromatography (GC) to be 99.03%. Purification was carried out by the recrystallization process. Ethanol-water including 25vol%～45vol% ethanol was selected as recrystallization solvent. The purity of SOA was improved from 99.1% to 99.9%, which is the highest level of SOA for purity reported so far in the open literature, by six purification processes. Furthermore, high purity SOA was characterized by FT-IR, DSC, GC-MS, ~1H NMR.