抗硫化返原剂二水合六亚甲基-1,6-二硫代硫酸二钠的制备  

Preparation of anti-reversion agent disodium hexamethylene-1,6-dithiosulfate dihydrate

作　　者：李天余 侯文杰 施云海[1] 余涛 LI Tian-yu;HOU Wen-jie;SHI Yun-hai;YU Tao(Research Centre of Chemical Engineering,East China University of Science and Technology,Shanghai 200237,China;BaoWu Carbon Technology Co Ltd,Shanghai 201999,China)

机构地区：[1]华东理工大学化学工程研究所,上海200237 [2]宝武碳业科技股份有限公司,上海201999

出　　处：《合成橡胶工业》2024年第1期63-67,共5页China Synthetic Rubber Industry

摘　　要：使用1,6-二氯己烷与五水合硫代硫酸钠合成出抗硫化返原剂二水合六亚甲基-1,6-二硫代硫酸二钠,通过正交试验和单因素实验考察其粗产品的合成工艺条件;对获得的产品进行重结晶纯化,结合硫代硫酸钠在乙醇-水溶液体系中不同温度的溶解度获得重结晶过程中溶剂的最优乙醇浓度、重结晶温度和结晶次数;最后对所合成产品进行了傅里叶变换红外光谱、X射线衍射及热重-差示扫描量热法的分析。结果表明,合成二水合六亚甲基-1,6-二硫代硫酸二钠的最佳反应条件为1,6-二氯己烷质量分数14%、乙醇与水的质量比3/4、反应体系pH值9、反应温度83℃,此时所合成粗产品的纯度和收率最高;使用质量分数为80%的乙醇溶液在20℃下重结晶精制2次,可制得纯度达97%以上、单程收率在80%以上的产品。Anti-reversion agent disodium hexa-methylene-1,6-dithiosulfate dihydrate was synthesized using 1,6-dichlorohexane and sodium thiosulfate pentahydrate.The synthesis conditions of its crude product were investigated through orthogonal experiment and single factor experiments.In the recrystallization purification experiment,the solubility of sodium thiosulfate in ethanol-water solution system at different temperatures was combined to obtain the optimal ethanol concentration,recrystallization temperature and crystallization times in the recrystallization process.Finally,the synthesized product was analyzed by Fourier transform infrared spectroscopy,X-ray diffraction and thermogravimetry analysis-differential scanning calorimetry.The results showed that the optimum reaction conditions for synthesizing disodium hexamethylene-1,6-dithiosulfate dihydrate were as follows:mass fraction of 1,6-dichlorohexane 14%,mass ratio of ethanol to water 3/4,pH value of reaction system 9,and reaction temperature 83℃.At this time,the purity and yield of the crude pro-duct were the highest.The product with purity of over 97%and one-pass yield of over 80%could be obtained by using ethanol solution with mass fraction of 80%and recrystallizing twice at 20℃.

关 键 词：二水合六亚甲基-1 6-二硫代硫酸二钠 抗硫化返原剂 1 6-二氯己烷 硫代硫酸钠 

分 类 号：TQ330.385[化学工程—橡胶工业]