山东化工
山東化工
산동화공
SHANDONG CHEMICAL INDUSTRY
2014年
11期
113-117
,共5页
刘合梅%张和%宁玉玺%陈凑喜%李学强
劉閤梅%張和%寧玉璽%陳湊喜%李學彊
류합매%장화%저옥새%진주희%리학강
季铵盐模板剂%ZSM-5改性%催化%缩酮反应%绿色固体酸
季銨鹽模闆劑%ZSM-5改性%催化%縮酮反應%綠色固體痠
계안염모판제%ZSM-5개성%최화%축동반응%록색고체산
quaternary ammonium template%ZSM-5 modification%catalysis%ketalization%green solid acid
本文报道了新型双核含芳环季铵盐化合物的合成,经核磁共振和红外光谱表征其结构,首次利用芳环季铵盐为模板剂,制备了具有MFI型衍射特征峰的新型ZSM-5分子筛,并借助XRD、SEM、N2吸附脱附、NH3-TPD等方法对其进行了表征。详细研究了该新型HZSM-5分子筛在缩酮反应中的催化性能,考察了分子筛用量、反应时间、温度等因素对缩酮反应的影响,优化了反应条件,并考察了该分子筛的循环使用效果。为进一步提高HZSM-5分子筛的催化活性,对其进行了质子交换改性,结果表明,改性后的HZSM-5分子筛具有催化活性高、稳定性好、重复使用次数多、催化剂分离方便、环境污染小等特点,是一种高效绿色的环保型固体酸。
本文報道瞭新型雙覈含芳環季銨鹽化閤物的閤成,經覈磁共振和紅外光譜錶徵其結構,首次利用芳環季銨鹽為模闆劑,製備瞭具有MFI型衍射特徵峰的新型ZSM-5分子篩,併藉助XRD、SEM、N2吸附脫附、NH3-TPD等方法對其進行瞭錶徵。詳細研究瞭該新型HZSM-5分子篩在縮酮反應中的催化性能,攷察瞭分子篩用量、反應時間、溫度等因素對縮酮反應的影響,優化瞭反應條件,併攷察瞭該分子篩的循環使用效果。為進一步提高HZSM-5分子篩的催化活性,對其進行瞭質子交換改性,結果錶明,改性後的HZSM-5分子篩具有催化活性高、穩定性好、重複使用次數多、催化劑分離方便、環境汙染小等特點,是一種高效綠色的環保型固體痠。
본문보도료신형쌍핵함방배계안염화합물적합성,경핵자공진화홍외광보표정기결구,수차이용방배계안염위모판제,제비료구유MFI형연사특정봉적신형ZSM-5분자사,병차조XRD、SEM、N2흡부탈부、NH3-TPD등방법대기진행료표정。상세연구료해신형HZSM-5분자사재축동반응중적최화성능,고찰료분자사용량、반응시간、온도등인소대축동반응적영향,우화료반응조건,병고찰료해분자사적순배사용효과。위진일보제고HZSM-5분자사적최화활성,대기진행료질자교환개성,결과표명,개성후적HZSM-5분자사구유최화활성고、은정성호、중복사용차수다、최화제분리방편、배경오염소등특점,시일충고효록색적배보형고체산。
A novel binuclear aromatic quaternary ammonium template was synthesized,and its structure was characterized by NMR and IR. On this basis,a new type of ZSM-5 zeolite with MFI-type diffraction peaks was prepared. The ZSM-5 zeolite was characterized by XRD,SEM,NH3 -TPD and N2 -adsorption-desorption. The novel HZSM-5 zeolite’s catalytic performance in condensation reaction of ethylene glycol and cyclohexanone was studied in detail. Then,the influences of zeolite dosage,reaction time and temperature on the Ketalization were investigated in order to optimize the reaction condition. Furthermore, the recycling of molecular sieve was organized under optimal reaction conditions. Subsequently,the HZSM-5 zeolite was modified by chlorosulfonic acid in order to improve the catalytic activity. After that,the ketalization catalyzed by the modified HZSM-5 zeolite under the optimal reaction conditions was investigated. The results revealed that the zeolite had high catalytic activity,good stability,easy recycling,easy separation of catalyst and few pollution,which can be used as an efficient and environmentally friendly green solid acid.