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Method for preparing valeric acid and valerate from gama-valerolactone

A technology of valerolactone and valeric acid ester, applied in the field of chemical product preparation, can solve problems such as unfavorable industrialization and harsh reaction conditions, and achieve the effects of high utilization rate, mild reaction conditions and high product yield

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

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Problems solved by technology

[0004] Although the methods reported above can obtain valeric acid by hydrogenolysis of GVL with a higher yield, they are all high-temperature and high-pressure processes, and the reaction conditions are harsh, which is not conducive to industrialization.

Method used

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  • Method for preparing valeric acid and valerate from gama-valerolactone
  • Method for preparing valeric acid and valerate from gama-valerolactone

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Embodiment 1

[0029] A method for preparing valeric acid by gamma-valerolactone, comprising: adding 0.1mol gamma-valerolactone into a reaction vessel, then adding 0.5mol% of Pd / C and 2mol% of gamma-valerolactone as a benchmark Zr(OTf) 3 , after replacement with hydrogen for 3 times, the temperature was raised to 135°C under stirring, and the catalytic hydrogenolysis reaction was carried out under a hydrogen atmosphere with a pressure of 1 atm for 12 hours. After cooling to room temperature, the reaction solution was obtained, and valeric acid was obtained by distillation under reduced pressure.

[0030] Sampling was diluted, and the yield of valeric acid determined by gas chromatography (GC) was 99%, 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

[0032] A method for preparing valeric acid by gamma-valerolactone, comprising: adding 0.1mol gamma-valerolactone into a reaction vessel, then adding 0.1mol% Pd / C and 10mol% Pd / C based on gamma-valerolactone 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 atm. After cooling to room temperature, the reaction liquid was obtained, and valeric acid was obtained by distillation under reduced pressure.

[0033]Sampling was diluted, and the yield of valeric acid determined by gas chromatography (GC) was 95%, and the purity was 99%.

Embodiment 3

[0035] A method for preparing valeric acid by gamma-valerolactone, comprising: adding 0.1mol gamma-valerolactone into a reaction vessel, then adding 5mol% Ru / C and 0.1mol% Ru / C based on gamma-valerolactone Hf(OTf) 4 , after two replacements with hydrogen, the temperature was raised to 80°C under stirring, and the catalytic hydrogenolysis reaction was carried out under a hydrogen atmosphere with a pressure of 50 atm for 6 hours. After cooling to room temperature, the reaction solution was obtained, and valeric acid was obtained by distillation under reduced pressure.

[0036] Sampling was diluted, and the yield of valeric acid determined by gas chromatography (GC) was 98%, and the purity was 99%.

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Abstract

The invention provides a method for preparing valeric acid and valerate from gama-valerolactone. The method comprises the following steps: by taking gama-valerolactone 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 gama-valerolactone 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 product preparation, in particular to a method for preparing valeric acid and valeric acid ester from gamma-valerolactone. Background technique [0002] Valerate is considered to be a fuel that can replace gasoline, and has passed Shell's 250,000-kilometer road test, and is known as a new generation of cellulose-based transportation fuel. On the other hand, levulinic acid (Levulinic acid) is a renewable biomass resource hydrolyzate, and is also considered by the U.S. Department of Energy as one of the 12 platform compounds from cellulose biobased (Werpy, T. et al. Top value added chemicals from biomass. In Results of Screening for Potential Candidates from Sugars and Synthesis Gas Vol.1, 45-48, 2004). Levulinic acid can be hydrogenated to generate γ-valerolactone (GVL), and GVL is hydrogenated to obtain valeric acid, and valeric acid is finally esterified to obtain valeric acid ester. Therefore...

Claims

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Application Information

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IPC IPC(8): C07C53/126C07C51/09C07C69/24C07C67/08
CPCC07C51/09C07C67/08C07C53/126C07C69/24
Inventor 邓晋常善伟朱瑞徐海周剑张坤谢中玉
Owner 合肥利夫生物科技有限公司
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