聚丙烯成核剂DMDBS的合成工艺研究

摘要以山梨醇、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。

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	段元超
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关键词： DMDBS 水相沉淀法 OP-10 精制

Abstract： The nucleation agent DMDBS was synthesized by aqueous precipitation and the optimization of the process was studied.Sorbitol and 3,4-dimethylbenzaldehyde were condensed in aqueous H₂SO₄ in presence of the emulsifier OP-10.Factors such as the sulfuric acid concentration，molar ratio of aldehyde to alcohol,reaction temperature and reaction time，were investigated；and the preferred preparation conditions were reaction temperature 15 ℃，reaction time 10 h，the sulfuric acid concentration 45%，molar ratio of aldehyde to alcohol 1.5∶1.0.The crude product was refined with N,N-dimethyl-n-octadecylamine and acetone.Under this condition，the DMDBS was obtained with the yield of 75.56%，purity above 99%，melting point of 252—253 ℃，giving the product with quality of a high level.

Keywords： DMDBS aqueous precipitation OP-10 refined

Received 2011-08-25;

About author: 段元超(1986-), 男, 山东莱芜人，现从事精细化工方向的研究。

引用本文:

段元超, 宋健, 庞晓敏, 孙树娟, 冯荣秀.聚丙烯成核剂DMDBS的合成工艺研究[J]. 化学工业与工程, 2012,29(01): 30-33

DUAN Yuan-Chao, SONG Jian, PANG Xiao-Min, SUN Shu-Juan, FENG Rong-Xiu.Synthesis of Polypropylene Nucleation Agent DMDBS[J]. Chemcial Industry and Engineering, 2012,29(01): 30-33