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以山梨醇、3,4-二甲基苯甲醛为原料,硫酸水溶液为反应介质及催化剂,采用水相沉淀法合成了成核剂DMDBS,筛选出OP-10作为乳化剂,并对合成工艺进行了优化。考察了硫酸浓度、n(醛)∶n(醇)、温度和时间对反应的影响,得出较适宜的工艺条件为:反应温度15℃;反应时间10 h;ω(硫酸)为45%;n(醛)∶n(醇)为1.5∶1.0。粗产品经溶有十八烷基二甲基叔胺的丙酮溶液回流精制,在此条件下DMDBS收率达75.56%,纯度99%以上,熔点252～253℃,质量达到国内外产品水平。
Using sorbitol, 3,4-dimethylbenzaldehyde as raw materials and sulfuric acid aqueous solution as the reaction medium and catalyst, the nucleating agent DMDBS was synthesized by aqueous precipitation method, and OP-10 was screened as the emulsifier, and the synthesis process was carried out Optimized. The effects of concentration of sulfuric acid, n (aldehyde): n (alcohol), temperature and time on the reaction were investigated. The optimum reaction conditions were: reaction temperature 15 ℃, reaction time 10 h, ω (sulfuric acid) 45% n (aldehyde): n (alcohol) 1.5: 1.0. The crude product was purified by refluxing with acetone solution of octadecyl dimethyl tertiary amine. Under this condition, the yield of DMDBS reached 75.56%, the purity was over 99% and the melting point was 252 ~ 253 ℃. The quality of DMDBS reached the level of domestic and foreign products.