双丙酮丙烯酰胺的合成及提纯工艺  

Synthesis and Purification of Diacetone Acrylamide

作　　者：张梅[1] 唐林生[1] 欧强[1] 

机构地区：[1]青岛科技大学化工学院,青岛266042

出　　处：《精细石油化工进展》2004年第9期20-22,共3页Advances in Fine Petrochemicals

摘　　要：对以丙酮和丙烯腈为原料合成双丙酮丙烯酰胺(DAAM)及提纯工艺进行了研究。考察了合成DAAM过程中主要影响因素,找出最佳合成条件:丙酮／丙烯腈／硫酸摩尔比为1.00:0.45:1.02,反应时间5 h,反应温度50-60℃;产品提纯工艺采用水萃取-NaCl盐析-NaOH溶液碱洗-冷冻结晶-乙酸乙酯重结晶方法,实验选出最佳提纯工艺条件:萃取水用量80 mL／mol丙酮,30％NaOH溶液用量15 mL／mol丙酮,乙酸乙酯用量5 mL／g粗产品,所得DAAM的产率为52.7％,含量99.58％,熔点54-56℃。此提纯方法与减压蒸馏方法相比,产品在提纯过程中不易聚合。Synthesis of diacetone acrylamide (DAAM) from acetone and acrylonitrile as raw materials as well as its purification was studied. The effects of main reaction conditions on the yield of DAAM were examined. The optimum conditions were obtained as follows: the molar ratio of acetone to acrylonitrile and sulfuric acid 1.00:0.45:1.02, reaction time 5 h, reaction temperature 50 - 60 ℃ . The product was purified using a process consisted of water extraction , NaCl salting out, NaOH solution washing, freeze crystallization and recrystallization with ethyl acetate. The optimum conditions for purification seleced by experiment were as follows: the dosages of water for extraction, 30 % NaOH solution for washing and ethyl acetate for recrystallization were 80 mL per mol acetone, 15 mL per mole actone and 5 mL per gram crude product respectively. The yield and purity of the product were 52.7% and 99.58% respectively with m. p 54 - 56 ℃ .

关 键 词：提纯工艺 双丙酮丙烯酰胺 合成 丙烯腈 液碱 乙酸乙酯 冷冻结晶 产品 过程 考察 

分 类 号：TQ226[化学工程—有机化工]