氯甲氧基丁烷的合成及应用

Synthesis and Application of Chloromethoxy Butane

摘要:

摘 要 本文采用正丁醇、多聚甲醛及干燥的氯化氢气体为主要原料，合成氯甲基化试剂烷基氯甲醚-氯甲氧基丁烷(CMB)。采用红外光谱(FTIR)与核磁共振谱(1H-NMR)对产物进行了表征。考察了溶剂用量，物料摩尔比，反应温度及反应时间对CMB收率的影响。采用正交试验法获得的最佳反应条件为溶剂1，2-二氯乙烷50 mL，n(正丁醇)：n(CH2O)=3:2.00, 温度为0-5 ℃, 反应时间为7 h。在此条件下，氯甲氧基丁烷的收率可达92%。用制备的氯甲氧基丁烷氯甲基化交联度为10%的白球，用佛尔哈德滴定法测氯含量，测得制得氯球中氯含量为13%。

Abstract:

Abstract Preparation of new chloromethylation reagent- Chloromethoxy butane(CMB) with butanol,paraformaldehyde and dry hydrogen chloride as raw material was reported in this paper.The product was confirmed by FTIR and 1H-NMR. Effects of the volume of solvent, molar ratio of reactants, reaction temperature and reaction time on the reaction have been studied. The optimal reaction conditions obtained by orthogonal test were solvent 1,2-dichloroethane 50 mL, n(CH3CH2CH2CH2OH) : n(CH2O) =3:2.00, reaction temperature 0-5℃, reaction time 7 h. Under these conditions, the yield of Chloromethoxy butane(CMB) can reach 92%. The product was used to chlomethylate crosslinking polystyrene(10%divinylbenzene crosslinking). Chlorine content highest reach 13% which is detected by Volhard method.