Synthesis of hexamethylene-1,6-dicarbamate by methoxycarbonylation of 1,6-hexamethylene diamine with dimethyl carbonate over bulk and hybrid heteropoly acid catalyst

Synthesis of hexamethylene-1,6-dicarbamate by methoxycarbonylation of 1,6-hexamethylene diamine with dimethyl carbonate over bulk and hybrid heteropoly acid catalyst
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本体杂多酸催化剂下 1,6-己二胺与碳酸二甲酯甲氧基羰基化合成 1,6-二氨基己酸

DOI:
10.1007/s11164-017-3030-4
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发表时间:
2017-12-01
影响因子:
3.3
通讯作者:
Li, Huiquan
Li, Huiquan
中科院分区:
化学3区
文献类型:
--
作者:
Ammar, Muhammad;Cao, Yan;Li, Huiquan

文献摘要

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以杂多酸(HPA)为主体和杂化催化剂,研究了HDA与DMC的甲氧基羰基化合成HDC的反应。采用XRD、FTIR、SEM和NH3-TPD等技术对催化剂进行了系统表征。对反应过程中产生的副产物进行了分析,并提出了可能的反应途径。评价了本体和混合HPA催化剂的性能。H4[SiW 12 O 40]催化剂与其他催化剂相比显示出高性能,其高性能归因于其酸性。考察了反应参数对反应的影响,并考察了H4[SiW 12 O 40]催化剂的重复使用性能。在优化的反应条件下,HDA转化率达到93.2%,HDC选择性为64.8%,副产物选择性仅为3.8%。并对H4[SiW 12 O 40]催化合成HDC的反应机理进行了初步探讨。
Synthesis of HDC by methoxycarbonylation of HDA with DMC was carried out over the bulk and hybrid heteropoly acid (HPA) catalyst. The catalysts were systematically characterized by XRD, FTIR, SEM and NH3-TPD techniques. The by-products produced in the reaction were identified and a possible reaction pathway was proposed based on the by-products analysis. The performances of bulk and hybrid HPA catalysts were evaluated. The H4[SiW12O40] catalyst revealed high performance compared with other catalysts and its high performance was attributed to its acidic properties. Effects of reaction parameters and reusability of the H4[SiW12O40] catalyst were also investigated. Under the optimized reaction conditions, HDA conversion reached 93.2% with 64.8% HDC selectivity and only 3.8% by-product selectivity. Moreover, a possible reaction mechanism was proposed for the synthesis of HDC over H4[SiW12O40] catalyst.