河南科学
河南科學
하남과학
HENAN SCIENCE
2013年
9期
1365-1368
,共4页
邵国斌%霍二福%刘菲%张谦华%徐桦
邵國斌%霍二福%劉菲%張謙華%徐樺
소국빈%곽이복%류비%장겸화%서화
邻氯苯亚甲基丙二腈%工业合成新工艺%复合催化剂%循环利用
鄰氯苯亞甲基丙二腈%工業閤成新工藝%複閤催化劑%循環利用
린록분아갑기병이정%공업합성신공예%복합최화제%순배이용
o-Chlorobenzylidenemalononitrile%the new industrial synthesis process%composite catalyst%cyclic utilization
邻氯苯亚甲基丙二腈通过工业新工艺而合成,以邻氯苯甲醛和丙二腈为原料,以乙醇为溶剂,以氢氧化钠-四丁基溴化铵配制的复合催化剂为催化剂,室温反应30 min,析出物离心分离、干燥后即得到高纯度的白色晶体邻氯苯亚甲基丙二腈。此新工艺的优点:收率高,产品纯度高,结晶粒度均匀;无需用无水乙醇重结晶,工艺简单,反应、结晶和提纯同时进行;反应母液可以循环利用10次以上,并且产品的收率不会随着循环次数的增加而降低,合成工艺成本降低30%以上。
鄰氯苯亞甲基丙二腈通過工業新工藝而閤成,以鄰氯苯甲醛和丙二腈為原料,以乙醇為溶劑,以氫氧化鈉-四丁基溴化銨配製的複閤催化劑為催化劑,室溫反應30 min,析齣物離心分離、榦燥後即得到高純度的白色晶體鄰氯苯亞甲基丙二腈。此新工藝的優點:收率高,產品純度高,結晶粒度均勻;無需用無水乙醇重結晶,工藝簡單,反應、結晶和提純同時進行;反應母液可以循環利用10次以上,併且產品的收率不會隨著循環次數的增加而降低,閤成工藝成本降低30%以上。
린록분아갑기병이정통과공업신공예이합성,이린록분갑철화병이정위원료,이을순위용제,이경양화납-사정기추화안배제적복합최화제위최화제,실온반응30 min,석출물리심분리、간조후즉득도고순도적백색정체린록분아갑기병이정。차신공예적우점:수솔고,산품순도고,결정립도균균;무수용무수을순중결정,공예간단,반응、결정화제순동시진행;반응모액가이순배이용10차이상,병차산품적수솔불회수착순배차수적증가이강저,합성공예성본강저30%이상。
O-Chlorobenzylidenemalononitrile(CS) is synthesized via the new industrial synthesis process in the presence of sodium hydroxide/tetrabutylammonium bromide prepared composite catalyst as catalyst,using o-chlorobenzaldehyde and malononitrile as raw material and absolute ethyl alcohol as solvent. After the reaction at room temperature for 30 minutes,precipitation is separated and dried to obtain high purity white crystal CS. This new process has many advantages,such as high yield,high product purity,crystals with uniform size;without the use of anhydrous alcohol recrystallization;simple process,reaction,crystallization and purification at the same time. The reaction mother liquid can be recycled more than ten times,and the yield of the product is not reduced with cycle number increases. The production cost reduces more than 30%than the existing synthetic process.