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以二甲胺、氯丙烯和液碱为原料,均质泵进行搅拌,分阶段控制反应温度,一步法合成二甲基二烯丙基氯化铵(DMDAAC)单体。粗DMDAAC溶液通过微量注射泵逐滴加碱进行减压蒸馏,控制溶液pH≈9。结果表明,利用均质泵,提高了物料混合效果,整个氯丙烯滴加过程由原来的5 h缩短为3.5 h,降低了副反应的发生,产物的收率最高达91.5%,比传统一步法工艺提高了21.11%。利用合成的单体进行均聚反应,均聚物的相对分子质量(简称分子量,下同)最高可达到12.5万,聚合产物的特征黏度值由原来的1.19 dL/g提高到2.80 dL/g,单体的转化率由90.08%提高到99.23%。该研究已经完成20 L规模扩试。
With dimethylamine, allyl chloride and caustic soda as raw materials, the homogeneous pump was stirred, and the reaction temperature was controlled in stages. One-step synthesis of dimethyldiallylammonium chloride (DMDAAC) monomer. Crude DMDAAC solution was added dropwise to the base by vacuum injection syringe, and the solution was controlled to pH≈9. The results showed that the use of a homogeneous pump increased the material mixing effect. The whole process of dropping propylene chloride was shortened from 5 hours to 3.5 hours and the side reactions were reduced. The yield of the product was up to 91.5% Technology increased by 21.11%. The homopolymerization reaction of the synthesized monomer, the molecular weight of the homopolymer (molecular weight, the same below) up to 125000, the intrinsic viscosity of the polymer product value from the original 1.19 dL / g increased to 2.80 dL / g, The monomer conversion increased from 90.08% to 99.23%. The study has completed the 20 L scale expansion.