A kind of br*nsted-lewis double-acidic ionic liquid and its catalytic method for synthesizing succinate
An ionic liquid, succinate technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problem of low catalytic efficiency of ionic liquids, and achieve low price, environmental friendliness, and catalytic efficiency. high effect
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Embodiment 1
[0021] 1. Synthesis of ionic liquids
[0022] (1) Mix 0.025 mol of zinc chloride and caprolactam in a molar ratio of 1:5, heat to 80°C in a collector-type constant temperature heating magnetic stirrer, and eutectic until all reactants are dissolved and become a clear and transparent liquid. At the end, a coordination intermediate is obtained.
[0023] (2) After the obtained coordination intermediate was cooled in an oil bath, 30 mL of toluene and 15 g of 1,3-propane sultone were added, and the mixture was refluxed in an oil bath at 80°C for 5 hours. After reaction finishes, take out oil bath, layering after reaction liquid cooling, pour out the mixture of upper strata toluene and unreacted raw material, lower floor is biacidic ionic liquid [4(C 3 SO 3 H-CPL)Zn]Cl 2 , and then distill off the remaining toluene in an oil bath at 120°C in a fume hood.
[0024] 2. Esterification reaction
[0025] Take by weighing respectively succinic acid 0.1mol, methyl alcohol 0.3mol, 0.12g...
Embodiment 2
[0027] 1. Synthesis of ionic liquids
[0028] (1) Mix 0.025 mol of zinc chloride and caprolactam in a molar ratio of 1:4, heat to 80°C in a collector-type constant-temperature heating magnetic stirrer, and eutecticly melt until all reactants are dissolved and become a clear and transparent liquid. At the end, a coordination intermediate is obtained.
[0029] (2) After cooling the obtained coordination intermediate out of the oil bath, 30 mL of toluene and 12.2 g of 1,3-propane sultone were added, and the mixture was refluxed in an oil bath at 80°C for 4 hours. After reaction finishes, take out oil bath, layering after reaction liquid cooling, pour out the mixture of upper strata toluene and unreacted raw material, lower floor is biacidic ionic liquid [4(C 3 SO 3 H-CPL)Zn]Cl 2 , and then distill off the remaining toluene in an oil bath at 120°C in a fume hood.
[0030] 2. Esterification reaction
[0031] Take respectively succinic acid 0.1mol, ethanol 0.3mol, 0.25g step 1 ...
Embodiment 3
[0033] 1. Synthesis of ionic liquids
[0034] Same as Example 2.
[0035] 2. Esterification reaction
[0036] Take by weighing respectively succinic acid 0.1mol, methyl alcohol 0.4mol, 0.5g [4(C 3 SO 3 H-CPL)Zn]Cl 2 Add ionic liquid and 20ml cyclohexane with water agent into a three-necked flask equipped with reflux condenser, water separator, and magnetic stirring, and reflux for 1.5h. During the reaction, water agent will separate the water generated by the reaction from the reaction system. After the reaction, the product dimethyl succinate was evaporated from the reaction solution, and the yield was 94.15%. The bis-acidic ionic liquid remains in the three-necked flask, which can be reused more than 6 times after being dried.
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