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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———氯甲氧基丁烷(CMB)。采用傅里叶变换红外光谱(FTIR)与核磁共振氢谱(1HNMR)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。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(多聚甲醛)=3∶2,温度为0～5℃,反应时间为7 h;在该条件下,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%的白球得到氯甲基化聚苯乙烯微球,并用佛尔哈德滴定法测得其中氯的质量分数为13%。
With n-butanol, paraformaldehyde and dry hydrogen chloride gas as the main raw material, chloromethylation reagent chloromethoxy butane (CMB) was synthesized. The product was characterized by Fourier transform infrared spectroscopy (FTIR) and 1H nuclear magnetic resonance (1HNMR). The effects of solvent dosage, molar ratio of materials, reaction temperature and reaction time on the yield of CMB were investigated. The optimal reaction conditions were as follows: 50 mL of solvent 1,2-dichloroethane, n (n-butanol): n (paraformaldehyde) = 3: 2, temperature 0 ~ 5 ℃, reaction time 7 h Under this condition, the yield of chloromethoxybutane can reach 92%. The chloromethylated polystyrene microspheres were obtained by chloromethylation of chloromethylated butane with 10% cross-linking degree. The mass fraction of chlorine was 13%.