Preparation method of oxalic acid diisoamyl ester
A technology of diisoamyl oxalate and oxalic acid, which is applied in the field of ester preparation, can solve problems such as poor thermal stability, inapplicability to higher temperature esterification systems, and use restrictions, and achieve the effect of improving conversion rate
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[0010] Example one.
[0011] Add 2.5 moles of isoamyl alcohol and 1 mole of oxalic acid to the four-necked flask, mix well and heat slowly while stirring. After the reaction solution reaches the specified temperature, add 2% NKC-9 catalyst, continue heating to boiling, and control the temperature of the reaction solution 110℃ for 3.0 hours, finally cooling, filtering off the catalyst, and distilling under a vacuum degree of 0.084MPa, collecting the fractions at 184-190℃, and analyzing it by infrared spectroscopy and gas chromatography-mass spectrometry to prove that it is diisoamyl oxalate. 93.1%.
Example Embodiment
[0012] Example two.
[0013] Add 4.5 moles of isoamyl alcohol and 1 mole of oxalic acid to a four-necked flask, mix well and heat slowly while stirring. After the reaction solution reaches the specified temperature, add 1.5% NKC-9 catalyst, continue heating to boiling, and control the temperature of the reaction solution At 130°C for 3.5 hours, the catalyst was finally cooled and filtered, and distilled under a vacuum of 0.084MPa. The fractions at 184-190°C were collected and analyzed by infrared spectroscopy and gas chromatography-mass spectrometry. The conversion rate was proved to be diisoamyl oxalate. 94.5%.
Example Embodiment
[0014] Example three.
[0015] Add 4 moles of isoamyl alcohol and 1 mole of oxalic acid to the four-neck flask, mix well and heat slowly while stirring. After the reaction liquid reaches the specified temperature, add NKC-9 catalyst, continue heating to boiling, and control the temperature of the reaction liquid to 120℃ After 3.1 hours, the catalyst was finally cooled, filtered, and distilled under a vacuum of 0.084MPa. The fractions at 184-190°C were collected and analyzed by infrared spectroscopy and gas chromatography-mass spectrometry. The conversion rate was 94.7%. .
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