摘要
采用新制的正丁醛 (NBAL)和多聚甲醛 (PFA)在三乙胺 (TEA)催化下制备了合成三羟甲基丙烷(TMP)的中间产物 2 ,2 二羟甲基丁醛 (DMB) .探讨了原料配比和反应时间对DMB收率的影响 ,以及催化剂与含水量对反应体系升温速率及DMB收率的影响 .最佳工艺条件为 :N2 保护下 ,nNBAL∶nPFA∶nTEA为 1∶3∶ (0 0 5～ 0 1) ,含水量为 10 %～ 15 % (以总量计 ) ,反应温度为 5 0～ 80℃ ,反应时间为 2h .通过IR、GC、GC MS、1HNMR对DMB的结构进行了表征 ;经过GC分析 ,NBAL在上述条件下可反应完全 (>99% ) ,DMB收率达88%以上 .
2,2-dimethylol-l-butanal (DMB) was synthesized by n-butyraldehyde (NBAL) with paraformaldehyde (PFA) in the existence of triethylamine (TEA). NBAL reacted completely (>99%) and the yield of DMB reached 88%. The structure of DMB was characterized by IR, GC, GC-MS, 1HNMR. It was found that the concentration of TEA and H2O greatly affected the rate of temperature rise of the reaction system and the yield of DMB. The optimized reaction conditions were as follows; under the nitrogen atmosphere, nNBAL:nPFA:nTEA=1:3:(0.05-0.1) and 10%-15% water by weight, temperature 50-80°C, reaction time 2 h.
出处
《化工学报》
EI
CAS
CSCD
北大核心
2004年第7期1098-1102,共5页
CIESC Journal
基金
山西省科技攻关项目资助 (No 0 2 1111)~~
关键词
三羟甲基丙烷
2
2-二羟甲基丁醛
三乙胺
羟醛缩合
Aldehydes
Amines
Catalysis
Condensation reactions
Gas chromatography
Infrared spectrometers
Mass spectrometry
Nitrogen
Nuclear magnetic resonance spectroscopy
Temperature
