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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

Inactive Publication Date: 2013-02-06
SHAANXI ALLIANCE LOGISTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to its poor thermal stability, its use is subject to certain restrictions, and it is not suitable for esterification systems with higher temperatures.

Method used

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  • Preparation method of oxalic acid diisoamyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Add 2.5 moles of isoamyl alcohol and 1 mole of oxalic acid into the four-neck flask, mix well and then heat slowly while stirring. After the reaction liquid reaches the specified temperature, add 2% NKC-9 catalyst, continue heating to boiling, and control the temperature of the reaction liquid 110°C for 3.0 hours, finally cooled, filtered out the catalyst, and distilled at a vacuum of 0.084MPa to collect fractions at 184-190°C, which were proved to be diisoamyl oxalate by infrared spectroscopy, gas chromatography-mass spectrometry, and the conversion rate was 93.1%.

Embodiment 2

[0013] Add 4.5 moles of isoamyl alcohol and 1 mole of oxalic acid into the four-neck flask, mix well and then heat slowly while stirring. After the reaction liquid reaches the specified temperature, add 1.5% NKC-9 catalyst, continue heating to boiling, and control the temperature of the reaction liquid 130°C for 3.5 hours, finally cooled, filtered out the catalyst, and distilled at a vacuum of 0.084MPa to collect fractions at 184-190°C, which were proved to be diisoamyl oxalate by infrared spectroscopy, gas chromatography-mass spectrometry, and the conversion rate was 94.5%.

Embodiment 3

[0015] Add 4 moles of isoamyl alcohol and 1 mole of oxalic acid into the four-necked flask, mix well and then 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°C After 3.1 hours, cool down, filter out the catalyst, and distill at a vacuum of 0.084MPa to collect fractions at 184-190°C. It is proved to be diisoamyl oxalate by infrared spectrum, gas chromatography-mass spectrometry, and its conversion rate is 94.7%. .

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Abstract

The invention discloses a preparation method of oxalic acid diisoamyl ester and relates to a preparation method of ester. The preparation method of the oxalic acid diisoamyl ester comprises the steps of mixing isoamyl alcohol and oxalic acid, stirring and heating simultaneously, adding NKC-9 catalyst, continuing to heat till boiling, controlling the temperature of reaction liquid to be 110-130 DEG C for 3.0-3.5h, finally cooling, filtering and distilling, and collecting the fraction at 184-190 DEG C. The preparation method allows the conversion rate of the oxalic acid to be increased, and the conversion rate of the oxalic acid is not less than 93% and can still reach 90% after the catalyst is reused for 3 times.

Description

technical field [0001] The present invention relates to a kind of preparation method of ester. Background technique [0002] Diisoamyl oxalate is an ester diesel cetane number improver, which does not emit NO because it does not contain nitrogen. , clean combustion, conducive to environmental protection, so there is a certain room for development. In recent years, there have been many research reports on the synthesis of diisoamyl oxalate by solid acid catalysts, such as 732 type cation exchange resin, HF-101 type ion exchange membrane, solid superacid Fe 2 o 3 / SO 4 2- , zinc sulfate, etc. Macroporous styrene-based cation exchange resin (NKC-9) has the advantages of less volume impact by solvent action, suitable for packed column operation, easy to realize continuous production, etc., and is also easy to store and transport. However, due to its poor thermal stability, its use is limited, and it is not suitable for esterification systems with higher temperatures. Co...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/36
Inventor 王耀斌
Owner SHAANXI ALLIANCE LOGISTICS
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