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Method for preparing valeric acid and valerate from levulinic acid

A technology of levulinic acid and valeric acid ester, which is applied in the direction of carboxylate preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of environmental pollution, equipment corrosion, etc., achieve high utilization rate, mild reaction conditions, The effect of high catalytic efficiency

Active Publication Date: 2017-06-30
合肥利夫生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, concentrated sulfuric acid is severely corrosive to equipment, and the subsequent treatment process often produces waste acid and alkali, which pollutes the environment

Method used

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  • Method for preparing valeric acid and valerate from levulinic acid
  • Method for preparing valeric acid and valerate from levulinic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0027] A method for preparing valeric acid from levulinic acid, comprising: adding 0.1mol levulinic acid to a reaction vessel, then adding 100ml of n-octane as a reaction solvent and 0.5mol% Pd / C based on levulinic acid and 2mol% Hf(OTf) 4 , after 3 replacements with hydrogen gas, the temperature was raised to 150°C under stirring, and the hydrogenolysis reaction was catalyzed for 6 hours under a hydrogen atmosphere with a pressure of 5 MPa. After cooling to room temperature, the reaction solution was obtained, and valeric acid was obtained by distillation under reduced pressure.

[0028] Sampling was diluted, and the yield of valeric acid determined by gas chromatography (GC) was 95%, and the purity was 99%. Among them, gas chromatography detection conditions: Shimadzu GC-2014C, DM-wax column, gasification temperature: 260 °C, detector temperature: 280 °C, column temperature: 100 °C (5min) → 10 °C / min → 180 °C (3min )→20°C / min→240°C (10min).

Embodiment 2

[0030] A method for preparing valeric acid from levulinic acid, comprising: adding 0.1mol levulinic acid to a reaction vessel, then adding 100ml of n-octane as a reaction solvent and 0.1mol% Pd / C based on levulinic acid and 10mol% Al(OTf) 3 , after 4 substitutions with hydrogen gas, the temperature was raised to 200°C under stirring, and the hydrogenolysis reaction was catalyzed for 10 h under a hydrogen atmosphere with a pressure of 10 MPa. After cooling to room temperature, the reaction solution was obtained, and valeric acid was obtained by distillation under reduced pressure.

[0031] Sampling was diluted, and the yield of valeric acid determined by gas chromatography (GC) was 92%, and the purity was 99%.

Embodiment 3

[0033] A method for preparing valeric acid from levulinic acid, comprising: adding 0.1mol levulinic acid to a reaction vessel, then adding 100ml of dioxane as a reaction solvent and 5mol% Ru / C based on levulinic acid and 0.1mol% Zr(OTf) 4 , after replacing twice with hydrogen gas, the temperature was raised to 100°C under stirring, and the catalytic hydrogenolysis reaction was carried out under a hydrogen atmosphere with a pressure of 8 MPa for 4 hours. After cooling to room temperature, the reaction liquid was obtained, and then valeric acid was obtained by distillation under reduced pressure.

[0034]Sampling was diluted, and the yield of valeric acid determined by gas chromatography (GC) was 94%, and the purity was 99%.

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Abstract

The invention provides a method for preparing valeric acid and valerate from levulinic acid. The method comprises the following steps: by taking levulinic acid as a raw material, hydrogenated catalyst and trifluoromethanesulfonic acid metal salt as a catalyst, performing catalytic hydrogenolytic cleavage reaction under hydrogen atmosphere, to obtain valeric acid; continuously by taking valeric acid as a raw material and trifluoromethanesulfonic acid metal salt as a catalyst, adding alcohol compound to perform esterification reaction, to obtain valerate. The method for preparing valeric acid and valerate from levulinic acid has the characteristics of being simple in technology, mild in reaction conditions, high in product yield, easily purified, environment-friendly and the like, and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical products, in particular to a method for preparing valeric acid and valeric acid esters from levulinic acid. Background technique [0002] As a class of fine chemicals, valeric acid esters have a wide range of applications, not only as food flavors, food flavoring agents, but also in the synthesis of medicines, solvents, etc. At the same time, valeric acid ester is also a new type of biomass fuel, which has good energy density and more suitable polarity, and can be completely miscible with existing transportation fuels, so it has a good and wide application prospect. At present, valeric acid ester is mainly produced by the esterification reaction of valeric acid and alcohol, and valeric acid can be produced by hydrogenation of levulinic acid, a biomass platform molecule. In the current technology, the levulinic acid is first hydrogenated into γ-valerolactone, and then the γ-valerolactone is conve...

Claims

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Application Information

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IPC IPC(8): C07C51/377C07C53/126C07C67/08C07C69/24
Inventor 邓晋周剑朱瑞徐海张坤谢中玉
Owner 合肥利夫生物科技有限公司
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