高校化学工程学报
高校化學工程學報
고교화학공정학보
JOURNAL OF CHEMICAL ENGINEERING OF CHINESE UNIVERSITIES
2015年
2期
334-339
,共6页
徐斌%刘艳秋%王俊格%任晓乾%马文明%武文良
徐斌%劉豔鞦%王俊格%任曉乾%馬文明%武文良
서빈%류염추%왕준격%임효건%마문명%무문량
磺酸型离子交换树脂%胺化%酸碱双功能%环己酮%缩合
磺痠型離子交換樹脂%胺化%痠堿雙功能%環己酮%縮閤
광산형리자교환수지%알화%산감쌍공능%배기동%축합
sulfonie acid ion exchange resin%amination%acid-base bifunctional%cyclohexanone%self-condensation
采用乙二胺对磺酸型阳离子交换树脂进行胺化改性,并运用CHNS元素分析及傅里叶变换红外光谱对改性树脂进行了表征。结果表明,胺化改性后树脂含氮量为0.94 mmol?g?1,改性后树脂骨架结构变化不大,胺基成功固载到树脂上,碱性增强,使氢型树脂成为具有酸碱双功能的催化剂。在催化环己酮缩合反应中考察了胺化量、催化剂用量、反应温度、反应时间、带水剂种类及用量等条件对反应的影响。实验结果表明,以甲苯为带水剂效果较好。在5%(wt)胺化量改性树脂,10%(wt)催化剂用量,7 mL甲苯为带水剂,120℃反应3 h的优化条件下,环己酮转化率为62.1%,二聚物选择性98.0%,体现出了酸碱协同催化环己酮缩合反应优异性能。改性树脂重复使用5次后,催化性能仍较稳定。
採用乙二胺對磺痠型暘離子交換樹脂進行胺化改性,併運用CHNS元素分析及傅裏葉變換紅外光譜對改性樹脂進行瞭錶徵。結果錶明,胺化改性後樹脂含氮量為0.94 mmol?g?1,改性後樹脂骨架結構變化不大,胺基成功固載到樹脂上,堿性增彊,使氫型樹脂成為具有痠堿雙功能的催化劑。在催化環己酮縮閤反應中攷察瞭胺化量、催化劑用量、反應溫度、反應時間、帶水劑種類及用量等條件對反應的影響。實驗結果錶明,以甲苯為帶水劑效果較好。在5%(wt)胺化量改性樹脂,10%(wt)催化劑用量,7 mL甲苯為帶水劑,120℃反應3 h的優化條件下,環己酮轉化率為62.1%,二聚物選擇性98.0%,體現齣瞭痠堿協同催化環己酮縮閤反應優異性能。改性樹脂重複使用5次後,催化性能仍較穩定。
채용을이알대광산형양리자교환수지진행알화개성,병운용CHNS원소분석급부리협변환홍외광보대개성수지진행료표정。결과표명,알화개성후수지함담량위0.94 mmol?g?1,개성후수지골가결구변화불대,알기성공고재도수지상,감성증강,사경형수지성위구유산감쌍공능적최화제。재최화배기동축합반응중고찰료알화량、최화제용량、반응온도、반응시간、대수제충류급용량등조건대반응적영향。실험결과표명,이갑분위대수제효과교호。재5%(wt)알화량개성수지,10%(wt)최화제용량,7 mL갑분위대수제,120℃반응3 h적우화조건하,배기동전화솔위62.1%,이취물선택성98.0%,체현출료산감협동최화배기동축합반응우이성능。개성수지중복사용5차후,최화성능잉교은정。
Sulfonie acid ion exchange resins were modified with ethylenediamine and characterized by FTIR and CHNS elemental analysis. The results show that resins with 0.94 mmol?g?1 nitrogen were obtained through amine modification. Moreover, the skeleton structure of the modified resin does not change and its basicity is strengthened to become an acid-base bifunctional resin catalyst. Effects of catalyst dosage, reaction temperature, reaction time, water carrier variety and dosage on self-condensation of cyclohexanone were investigated. Toluene was chosen as a good water carrier. Under optimum conditions (amination rate 5%(wt), catalyst dosage 10%(wt), toluene dosage 7mL, reaction time 3 h and reaction temperature 120℃), conversion of cyclohexanone and selectivity of dimer product are 62.1 % and 98.0 %, respectively. Furthermore, the modified resin shows good reusability after using for 5 times.