CAJ | 학술논문

以丙酮肟、盐酸为原料，经水解反应合成盐酸羟胺，研究建立了对水解可逆反应进程作定量检测的HPLC-氧化还原滴定组合分析方法，分析结果的平均回收率达99.64%，相对标准偏差≤2.04%（n=6）。建立了反应-蒸馏耦合工艺装置，研究和优化了丙酮肟水解反应制备盐酸羟胺的反应-蒸馏过程工艺条件，结果表明，当丙酮肟与盐酸的摩尔比为1∶2，盐酸质量分数为38%，加热温度为130℃，反应时间为3h时，丙酮肟原料转化率达到89%左右，盐酸羟胺产品收率达到84%左右。
이병동우、염산위원료，경수해반응합성염산간알，연구건립료대수해가역반응진정작정량검측적HPLC-양화환원적정조합분석방법，분석결과적평균회수솔체99.64%，상대표준편차≤2.04%（n=6）。건립료반응-증류우합공예장치，연구화우화료병동우수해반응제비염산간알적반응-증류과정공예조건，결과표명，당병동우여염산적마이비위1∶2，염산질량분수위38%，가열온도위130℃，반응시간위3h시，병동우원료전화솔체도89%좌우，염산간알산품수솔체도84%좌우。
Using acetone oxime and hydrochloric acid as raw materials,the hydrolysis of acetone oxime was carried out to prepare hydroxylamine hydrochloride. A quantitative analysis method by combining HPLC detection and redox titration was set up for the analysis of the reversible hydrolysis reaction equilibrium. The obtained analysis data of the combined method had a recovery of 99.64%and a RSD of no more than 2.04% (n=6). After that,a reactive distillation device was set up for the hydrolysis of acetone oxime,and the process technology of the reactive distillation was studied and optimized. The result showed that,at condition when the molar ratio of acetone oxime to HCl=1∶2, HCl mass fraction at 38%,heating temperature at 130℃ and reaction time at 3h,the raw material conversion of acetone oxime approached around 89% and the product yield of hydroxylamine hydrochloride reached about 84%.