三氯蔗糖-6-乙酸酯醇解制三氯蔗糖及结晶工艺优化

Study on the conversion process of sucralose-6-acetate to sucralose in methanol and recrystallized process improvement

以自制的三氯蔗糖-6-乙酸酯(Sucralose-6-acetate,TGS-6-A)为原料,在碱性条件下制得三氯蔗糖(Sucralose,TGS),采用DPS数据处理软件,通过对醇解温度、初始p H以及反应时间三个因素进行混合均匀实验设计,并以TGS含量作为指标,最终得出醇解的最佳条件:温度35.0℃,p H10.0,时间2.3 h,制得TGS平均收率为79.49%,与模型计算理论值相差1.26%,说明使用DPS数据处理软件设计TGS-6-A醇解实验模型以寻求最佳醇解条件可行。重结晶提纯过程采用乙酸乙酯、乙酸丁酯作为萃取剂,使用蒸馏水多次洗涤有机相,收集水相,依次经过活性炭脱色、过滤、超声、冷却重结晶、干燥等流程,得到TGS重结晶产品。经红外光谱及高效液相色谱分析,产品最高纯度可达99.23%,水分均低于1.0%。本文为醇解制备TGS工业化生产以及结晶工艺提供一种可行性方法。

Sucralose was obtained from sucralose-6-acetate under the conditions of alkaline content of sucralose as index,investigated the effects of reaction temperature,p H and reaction time on deacetylation by mixed-level uniform design. Data processing software（ DPS） was used to obtain the result that the average yield of sucralose was 79.49% at the reaction temperature 35.0 ℃,adjusted to p H = 10.0 and reaction time 2.3 h. The absolute deviation relative to model-calculated theoretical value was 1.26%.These results showed the feasibility for design the conversion process of sucralose-6-acetate and obtained the optimal conditions of the alcoholysis by DPS.In the recrystallization purification process,the ethyl acetate and butyl acetate were used as extracting agent,the organic phase was washed several times by distilled water and then the water phase was collected.Then the TGS product was obtained by the proceture of actived carbon decoloration,filtration,ultrasonic,cooling,recrystallization,drying and other processes. Analyzed by IR and HPLC,the highest purity of TGS was up to 99.23% and the water content was less than 1.0%. It had provided a feasible method for sucralose industrialized production and crystallization purification technology.