Bu_2SnO催化反应耦合法清洁合成苯氨基甲酸甲酯
Clean synthesis of methyl N-phenyl carbamate through coupling route with catalyst Bu_2SnO
查看参考文献18篇
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文摘
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加压条件下,对反应耦合法清洁合成苯氨基甲酸甲酯(MPC)的催化剂进行了筛选,对反应工艺优化、催化剂的循环使用和表征等方面进行了研究.在筛选的催化剂中,Bu_2SnO是较为理想的催化剂.在反应物碳酸二甲酯(DMC)和二苯基脲(DPU)的摩尔比为10:1,催化剂Bu_2SnO的用量为2%,160℃时,反应2 h,MPC的收率达到98%,远高于文献结果(77%).催化剂Bu_2SnO循环使用4次后,催化活性基本不变.对反应前后的Bu_2SnO进行了FTIR、XPS和XRD表征,结果表明,反应后从釜液中用水作沉淀剂絮凝沉淀出的催化剂绝大部分仍为Bu_2SnO,并可能含有其他微量未水解的催化剂中间体. |
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其他语种文摘
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Screening of catalyst for clean synthesis of methyl N-phenyl carbamate (MPC) through coupling route was performed under pressure, and process optimization, recycling of catalyst, and characterization of catalyst were also studied. The results showed that Bu_2SnO was the best one among the screened catalysts. Under the conditions that the molar ratio of dimethyl carbonate (DMC) to N,N'-diphenyl urea (DPU) was 10: 1, the amount of catalyst Bu_2SnO was 2% , reaction temperature was 160℃, and reaction time was 2 h, the yield of MPC reached 98%, which was more than 77%, the reported yield of MPC with catalyst Bu_2SnO in the literature. Catalytic performance of Bu_2SnO was constant after four cycles. Catalyst Bu_2SnO before reaction and after reaction was characterized with FTIR, XPS and XRD. The analysis of XRD and XPS showed that the catalyst separated by the precipitator water from reaction solvent was still Bu_2SnO, but FTIR showed presence of new compounds. Since trace components or amorphous compounds in samples can not be detected by XPS or XRD, it could be concluded that most of the catalyst separated by the precipitator water from reaction solvent was Bu_2SnO with a small amount of possibly catalytic intermediates. |
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来源
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化工学报
,2009,60(12):3019-3025 【核心库】
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关键词
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苯氨基甲酸甲酯
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反应耦合法
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清洁工艺
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工艺优化
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地址
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1.
清华大学, 清华大学化学工程联合国家重点实验室, 北京, 100084
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中国科学院过程工程研究所, 北京, 100190
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语种
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中文 |
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文献类型
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研究性论文 |
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ISSN
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0438-1157 |
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学科
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化学工业 |
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基金
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国家科技支撑计划重大项目
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中国博士后科学基金
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文献收藏号
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CSCD:3724944
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