Method for preparing acrolein through catalysis of glycerol liquid phase dehydration by using pyridine ion liquid
An ionic liquid, a technology for catalyzing glycerol, which is applied in the field of organic chemistry to achieve the effects of high activity, high product selectivity and yield, and low price
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Embodiment 1
[0017] Take 0.1 mol of pyridine in a four-neck flask, add equimolar n-bromobutane into a constant pressure titration funnel, 2 Stirred under protective conditions for 12 h, the product was washed with ethyl acetate and then vacuum-dried for 8 h to obtain 0.1 mol of brominated n-butylpyridine [Bpy]Br as light yellow viscous oily liquid. At 90 °C, equimolar concentrated sulfuric acid was added dropwise to [BPy]Br, stirred for 6 h, the product was washed with ether and then dried in vacuum to obtain the ionic liquid [BPy]HSO 4 .
[0018] Weigh the [BPy]HSO prepared above 4 Catalyst 5 mmol, glycerin 1.0 mol, stirred and heated up to 250 °C for batch reaction, fully reacted until no distillate was produced, then sampled for gas chromatographic analysis. Analysis showed that the conversion rate of glycerol was 100%, and the yield of acrolein was 32.5%.
Embodiment 2
[0020] [BPy]HSO 4 Synthesis as in Example 1. Weigh the [BPy]HSO prepared above 4 Catalyst 5 mmol, glycerin 1.0 mol, stirred and heated up to 300 °C for batch reaction, fully reacted until no distillate was produced, and samples were taken for gas chromatographic analysis. The analysis shows that the conversion rate of glycerol is 100%, and the yield of acrolein is 48.1%.
Embodiment 3
[0022] [BPy]HSO 4 Synthesis as in Example 1. Weigh the [BPy]HSO prepared above 4 Catalyst 0.012 mol, glycerol 1.0 mol, stirred and heated up to 250 °C for batch reaction, fully reacted until no distillate was produced, then sampled for gas chromatography analysis. Analysis showed that the conversion rate of glycerol was 100%, and the yield of acrolein was 50.3%.
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