摘要
研究了以碳酸钠和碳酸氢钠混合碱溶液作为新的催化体系合成三羟甲基丙烷的方法,探讨了催化剂和助催化剂用量、原料配比、反应温度、反应时间等因素对反应的影响,得到了适宜的工艺条件:原料n(甲醛)∶n(正丁醛)=6∶1,催化剂n(碳酸氢钠)∶n(正丁醛)=1.5∶1,助催化剂三乙胺用量为催化剂总质量的1.0%~1.5%,缩合反应温度20~30℃,反应时间为50~70min;Can-nizzaro反应温度55~60℃,反应时间为100~120min,三羟甲基丙烷产率可达87.7%(以正丁醛计)。
The Synthesis of trimethylolpropane using a mixed solution of sodium carbonate and sodium hydrocarbonate as catalyst is introduced. The effects of the amount of catalyst and promoter, the ratio of reactants, the reaction temperature and the reaction time are investigated. The optimum conditions are: molar ratio of formaldehyde to n-butyraldehyde, 6∶1; molar ratio of sodium hydrocarbonate to n-butyraldehyde, 1.5∶1; mass ratio of promoter triethylamine to catalyst, 1.0%~1.5%; temperature of condensation reaction, 20~30℃; condensation reaction time 50~70 min; temperature of Cannizzaro reaction,55~60℃; Cannizzaro reaction time,100~120 min. The yield of TMP is 87.7% (based on n-butyraldehyde).
出处
《化学世界》
CAS
CSCD
北大核心
2004年第5期262-264,共3页
Chemical World
关键词
三羟甲基丙烷
催化
合成
催化剂
trimethylolpropane
catalysis
synthesis
catalyst