化学研究与应用
化學研究與應用
화학연구여응용
CHEMICAL RESEARCH AND APPLICATION
2014年
10期
1584-1590
,共7页
谢昊%吴淑萍%何康丽%刘万毅%李锐
謝昊%吳淑萍%何康麗%劉萬毅%李銳
사호%오숙평%하강려%류만의%리예
邻苯二胺与芳香醛%缩合反应%1 ,2-取代苯并咪唑%太西煤%碳基磺酸固体酸
鄰苯二胺與芳香醛%縮閤反應%1 ,2-取代苯併咪唑%太西煤%碳基磺痠固體痠
린분이알여방향철%축합반응%1 ,2-취대분병미서%태서매%탄기광산고체산
o-phenylenediamine and aromatic aldehyde%condensation reaction%1,2-substituted benzimidazoles%Taixi coal%sulfonat-ing carbon-based solid acid
以太西煤为原料(其灰份为0.6%、目数大于200目),通过直接磺化得到煤基碳基磺酸( CHS-SA),以及通过对太西无烟煤粉末与煤质腐植酸钠粘合成型后的碳化物进行磺化而得的复配型煤基碳基固体酸( CCB-SA),考察了2种煤基碳基固体酸催化邻苯二胺(OPDA)与芳香醛缩合制备1,2取代苯并咪唑类衍生物的合成工艺参数。结果表明CCB-SA的催化活性优于CHS-SA。优化出的反应条件是:邻苯二胺与芳香醛的投料当量比为1mmol∶2mmol,乙醇与水2∶1体积比的混合溶剂5mL,CCB-SA用量为反应底物总重量的31%,在回流条件下反应35-70 min时,目标产物的收率可达78%-86%。该类催化剂在水介质中对反应具有较好的催化活性、且可以重复利用3次。
以太西煤為原料(其灰份為0.6%、目數大于200目),通過直接磺化得到煤基碳基磺痠( CHS-SA),以及通過對太西無煙煤粉末與煤質腐植痠鈉粘閤成型後的碳化物進行磺化而得的複配型煤基碳基固體痠( CCB-SA),攷察瞭2種煤基碳基固體痠催化鄰苯二胺(OPDA)與芳香醛縮閤製備1,2取代苯併咪唑類衍生物的閤成工藝參數。結果錶明CCB-SA的催化活性優于CHS-SA。優化齣的反應條件是:鄰苯二胺與芳香醛的投料噹量比為1mmol∶2mmol,乙醇與水2∶1體積比的混閤溶劑5mL,CCB-SA用量為反應底物總重量的31%,在迴流條件下反應35-70 min時,目標產物的收率可達78%-86%。該類催化劑在水介質中對反應具有較好的催化活性、且可以重複利用3次。
이태서매위원료(기회빈위0.6%、목수대우200목),통과직접광화득도매기탄기광산( CHS-SA),이급통과대태서무연매분말여매질부식산납점합성형후적탄화물진행광화이득적복배형매기탄기고체산( CCB-SA),고찰료2충매기탄기고체산최화린분이알(OPDA)여방향철축합제비1,2취대분병미서류연생물적합성공예삼수。결과표명CCB-SA적최화활성우우CHS-SA。우화출적반응조건시:린분이알여방향철적투료당량비위1mmol∶2mmol,을순여수2∶1체적비적혼합용제5mL,CCB-SA용량위반응저물총중량적31%,재회류조건하반응35-70 min시,목표산물적수솔가체78%-86%。해류최화제재수개질중대반응구유교호적최화활성、차가이중복이용3차。
In this study,sulfonating coaled carbon-based solid acid catalyst( CHS-SA) was prepared by means of Taixi coal( ash con-tent is 0. 6%,mesh>200)as the main raw resource directly,as well as get through sulfonating the carbides from Taixi coal powder bonded with coal-based sodium humate to form composite coaled carbon-based solid acid catalyst(CCB-SA). Both coaled carbon-based solid acid catalyst had been investigated for their synthesis parameters in the condensation reaction between o-phenylenedia-mine(OPDA)and aromatic aldehyde to synthesize 1,2-substituted benzimidazoles. The result showed the catalytic activity of CCB-SA was higher than CHS-SA. The optimization reaction conditions were:n(OPDA)∶n(aldehyde)=1∶2,V(EtOH)∶V(water)=2∶1 (5mL),the quantity of CCB-SA equaled to 31%feed stock,refluxing reaction time 35-70 min,its yield could reach 78%-86%. The catalyst had good catalytic performance in the aqueous media,and repeated for three times without loss of activity.