详细信息
Natural montmorillonite modified cyclo-addition catalysis system used in preparing cyclic carbamate comprises using carboxyl functionalized ion liquids with different chain lengths for intercalation modification
文献类型:专利
英文题名:Natural montmorillonite modified cyclo-addition catalysis system used in preparing cyclic carbamate comprises using carboxyl functionalized ion liquids with different chain lengths for intercalation modification
作者:SHI Y;CAO T;WANG M;HOU Z;SUN L;ZHANG L
机构:[1]UNIV EAST CHINA SCI&TECHNOLOGY
申请号:CN102069010-B
公开日:2012-11-21
语种:英文
收录:DERWENT
摘要:NOVELTY - Natural montmorillonite modified cyclo-addition catalysis system comprises using carboxyl functionalized ion liquid (I) with different chain lengths for intercalation modification. USE - Natural montmorillonite modified cycloaddition catalysis system used in preparing cyclic carbamate. ADVANTAGE - The catalyst system cooperates with quat. ammonium salt to catalyze cycloaddition reaction of carbon dioxide and epoxy compound to generate cyclic carbamate. It has simple preparation method, low material cost, and has high activity and good stability. DETAILED DESCRIPTION - Natural montmorillonite modified cyclo-addition catalysis system comprises using carboxyl functionalized ion liquid (I) with different chain lengths for intercalation modification. n, m=alkyl chains with different lengths. Provided that: (1) when n is 3-11, it comprises butyl imidazole to dodecyl imidazole; (2) when n is 3, 5, 7, or 11, it comprises butyl imidazole, hexyl imidazole, octyl imidazole, or dodecyl imidazole;and (3) when m is 1-5, preferably 1, 3, it comprises ethyl bromoacetate and ethyl bromobutyrate. INDEPENDENT CLAIMS are included for: (1) preparation of intercalation modified montmorillonite of ion liquid by preparation of sodium-based montmorillonite by preparing 3 g original soil of purified montmorillonite as slurry, adding 3.5 g sodium chloride (NaCl) into 20 ml deionized water, stirring to completely dissolve, mixing montmorillonite slurry with prepared NaCl solution, stirring for 3 hours in oil bath at 80 degrees C to accomplish exchange course of positive ion, continuously exchanging for 3 times, centrifuging and dehydrating, drying for 16 hours in oven at 60 degrees C, and grinding to prepare sodium-based montmorillonite; preparation of ion liquid by feeding alkyl imidazole and Br(CH2)mCOOCH2CH3 based on 1:1 mol ratio and oil bath at 50 degrees C, stirring and reacting for 8 hours; stop stirring and cooling; washing for 3 times by diethyl ether, extracting in oil bath at 70 degrees C, hydrolyzing for 2 hours by 40% hydrogen bromide water solution in equal mol quantity, vacuum extracting, washing for 3 times by diethyl ether, and vacuum extracting to prepare carboxyl functionalized ion liquid; and preparation of functionalized ion intercalated montmorillonite by weighing 1.5 g sodium-based montmorillonite, dissolving 1.5 mmol functionalized ion liquid in 20 ml deionized water, reflowing and mixing for 4 hours in oil bath at 80 degrees C, cooling, centrifuging and dehydrating, washing with deionized water for 8-10 times until no bromide is detected, drying for 16 hours in oven at 60 degrees C, and grinding to prepare functionalized ion intercalated montmorillonite;and (2) catalyzing cyclo-addition reaction of carbon dioxide and epoxy compound in double-component system using catalyst and quat. ammonium salts.
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