高等学校化学学报
高等學校化學學報
고등학교화학학보
CHEMICAL JOURNAL OF CHINESE UNIVERSITIES
2014年
11期
2444-2450
,共7页
唐荣芝%王松林%张元卓%陈彤%王公应
唐榮芝%王鬆林%張元卓%陳彤%王公應
당영지%왕송림%장원탁%진동%왕공응
乙酸氧钛%碳酸二苯酯%苯酚%酯交换%多相催化剂%苯氧基钛合物
乙痠氧鈦%碳痠二苯酯%苯酚%酯交換%多相催化劑%苯氧基鈦閤物
을산양태%탄산이분지%분분%지교환%다상최화제%분양기태합물
Titanyl acetate%Diphenyl carbonate%Phenol%Transesterification%Heterogeneous catalyst%Phenoxytitanium complex
采用溶剂热法合成了乙酸氧钛,其对碳酸二甲酯( DMC)与苯酚的酯交换合成碳酸二苯酯( DPC)的催化反应显示出了很好的催化效果.乙酸氧钛用量0.10 g时,苯酚转化率即达到47.8%,酯交换选择性在99.9%以上,仅检测到微量副产物苯甲醚.傅里叶变换红外光谱(FTIR)和固体核磁共振(13C NMR)等表征结果显示,乙酸氧钛在反应过程中首先与苯酚反应,苯氧基取代乙酸根生成苯氧基钛合物.实验结果表明,苯氧基钛合物作为实际催化剂参与DMC和苯酚的酯交换反应,并且重复使用效果良好.
採用溶劑熱法閤成瞭乙痠氧鈦,其對碳痠二甲酯( DMC)與苯酚的酯交換閤成碳痠二苯酯( DPC)的催化反應顯示齣瞭很好的催化效果.乙痠氧鈦用量0.10 g時,苯酚轉化率即達到47.8%,酯交換選擇性在99.9%以上,僅檢測到微量副產物苯甲醚.傅裏葉變換紅外光譜(FTIR)和固體覈磁共振(13C NMR)等錶徵結果顯示,乙痠氧鈦在反應過程中首先與苯酚反應,苯氧基取代乙痠根生成苯氧基鈦閤物.實驗結果錶明,苯氧基鈦閤物作為實際催化劑參與DMC和苯酚的酯交換反應,併且重複使用效果良好.
채용용제열법합성료을산양태,기대탄산이갑지( DMC)여분분적지교환합성탄산이분지( DPC)적최화반응현시출료흔호적최화효과.을산양태용량0.10 g시,분분전화솔즉체도47.8%,지교환선택성재99.9%이상,부검측도미량부산물분갑미.부리협변환홍외광보(FTIR)화고체핵자공진(13C NMR)등표정결과현시,을산양태재반응과정중수선여분분반응,분양기취대을산근생성분양기태합물.실험결과표명,분양기태합물작위실제최화제삼여DMC화분분적지교환반응,병차중복사용효과량호.
Titanyl acetate was prepared through the solvothermal reaction between titanium(Ⅳ) n-butoxide, acetic anhydride and distilled water. Titanyl acetate was firstly used in the transesterification reaction of dime-thyl carbonate and phenol to diphenyl carbonate and exhibited excellent performance. When titanyl acetate amount is 0. 10 g, the phenol conversion reaches to 47. 8% and transesterification selectivity is 99. 9% with trace anisole. Based on the results of FTIR, solid state 13 C NMR, titanyl acetate reacts firstly with phenol. The acetate group of titanyl acetate is replaced by phenoxy group and generates phenoxy titanium complex. It could be considered that phenoxy titanium complex is the real catalyst for the transesterification of dimethyl carbonate and phenol with good resuability.