The efficient hydroxyalkylation of phenol with formaldehyde to bisphenol F over a thermoregulated phase-separable reaction system containing a water-soluble Bronsted acidic ionic liquid
The efficient hydroxyalkylation of phenol with formaldehyde to bisphenol F over a thermoregulated phase-separable reaction system containing a water-soluble Bronsted acidic ionic liquid
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在含有水溶性布朗斯台德酸性离子液体的温控相分离反应体系中苯酚与甲醛高效羟烷基化生成双酚F
DOI：
10.1039/c4ra02827a
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发表时间：
2014-01-01
期刊：
影响因子：
3.9
通讯作者：
Liu, Yuejin
中科院分区：
文献类型：
--
作者：
Wang, Qing;Wu, Zhi Min;Liu, Yuejin
研究了在水溶性Bronsted酸性离子液体的温控相分离反应体系中苯酚和甲醛的羟烷基化反应。含水溶性IL的反应体系随IL烷基链长、温度和水量的变化而呈现温控两相行为。分别以磷酸二氢根[H2 PO 4]（-）、乙酸根[CH 3COO]（-）和硫酸氢根[HSO 4]（-）为阴离子的咪唑、铵、磷和吡啶四种水溶性离子液体作为Bronsted酸性催化剂和温控溶剂。其中，[C6 MIM][HSO 4]的双酚F产率为80.5%，选择性为96.9%，最佳反应条件为搅拌速度450 rpm，酚醛比6：1，IL催化剂摩尔浓度12.5%，反应温度90 ℃，反应时间1h。[C6 MIM][HSO 4]可以通过简单的倾析回收，并且即使在六次循环使用后也可以保持其原始活性，发现具有烷基链长n = 6的[CnMIM][HSO 4]最适合于合成双酚F，因为在90 ℃下形成温度调节的两相反应体系以提高反应效率，并且作为温度调节相。过渡溶剂，以促进其从反应体系中回收。
The efficient hydroxyalkylation of phenol with formaldehyde to bisphenol F over a thermoregulated phase-separable reaction system containing a water-soluble Bronsted acidic ionic liquid was studied. The reaction system containing the water-soluble IL showed thermoregulated biphasic behavior with change of the alkyl chain length of IL, temperature and water amount. Four types of imidazolium-, ammonium-, phosphonium-and pyridinium-based water-soluble ionic liquids with different anions of dihydrogen phosphate [H2PO4](-), acetate [CH3COO](-) and hydrogen sulfate [HSO4](-) were used as both Bronsted acidic catalysts and thermoregulated solvents. Among them, [C6MIM][HSO4] gave a high yield of 80.5% and a selectivity of 96.9% for bisphenol F, and the optimal reaction conditions were stirring speed 450 rpm, phenol-formaldehyde ratio 6 : 1, IL catalyst molar concentration 12.5%, reaction temperature 90 degrees C and reaction time 1 h. [C6MIM][HSO4] could be recovered by simple decantation and could retain its original activity even after six recycling-uses [CnMIM][HSO4] with the alkyl chain length n = 6 found to be the most suitable for the synthesis of bisphenol F because of both the formation of a thermoregulated monophasic reaction system at 90 degrees C to enhance the reaction efficiency and as a thermoregulated phase-transition solvent to facilitate its recovery from the reaction system.