Method for synthesizing gamma-valerolactone based on catalytic hydrogenation

A technology for catalytic hydrogenation and valerolactone, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve high production costs, expensive noble metal catalysts, etc. problems, achieve low cost, high activity and stability, and simple operation process

Active Publication Date: 2013-07-10
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, noble metal catalysts are exp

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Preparation of catalyst by impregnation method:

[0034] 1) Pretreatment of the carrier, 1g SiO 2 The carrier is calcined at 500°C for 3 hours;

[0035] 2) Load the active components, set the cobalt loading to 15%, calculate the required Co(NO 3 ) 2 ·6H 2 The theoretical amount of O is 0.74g, and 0.74g of Co(NO 3 ) 2 ·6H 2 O was dissolved in 5 mL of water to obtain an aqueous solution of cobalt nitrate. The carrier pretreated in step 1) was completely immersed in the aqueous solution of cobalt nitrate, and immersed for 12 hours at 20° C., and then the entire solution and SiO 2 After drying at 110°C for 12 hours, calcining at 500°C for 4 hours, and finally reducing at 500°C for 3 hours in a hydrogen atmosphere, Co / SiO with a loading capacity of 15% can be obtained 2 Catalyst 1.15g.

[0036] 3) Add 0.3 g of Co / SiO 2 Catalyst, 1.7 grams of levulinic acid, and 40 mL of solvent methanol were added to the autoclave. The reaction temperature was 140 ° C. The air in th...

Embodiment 2

[0038] Other operations are the same as in Example 1, except that the solvent in step 3) is 40 mL of water, the reaction time is 6 hours, and the conversion rate of levulinic acid is 100% as detected by gas chromatography, and the yield of γ-valerolactone is 99.9% .

Embodiment 3

[0040] Catalyst preparation process 1), 2) are the same as in Example 1, the difference is that the catalyst uses γ-Al 2 o 3 As a carrier, Co / γ-Al with a loading capacity of 15% was prepared 2 o 3 catalyst.

[0041] 3) Add 0.3 g Co / γ-Al 2 o 3 The catalyst was added into a 100 milliliter autoclave, other conditions were the same as in Example 1, and the reaction time was 6 hours. Gas chromatography detected that the conversion rate of levulinic acid was 100%, and the yield of gamma-valerolactone was 80.4%.

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PUM

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Abstract

The invention discloses a method for synthesizing gamma-valerolactone based on catalytic hydrogenation. According to the method, levulinic acid or levulinate derivatives in a reaction solvent is/are subject to catalytic hydrogenation for 1-10 hours by adding hydrogen gas and keeping the hydrogen gas pressure at 0.5-5.0 MPa under the action of a supported cobalt catalyst and the temperature of 50-240 DEG C, and the reaction liquid is treated to obtain the gamma-valerolactone. The cobalt catalyst prepared according to the method has excellent catalytic activity and selectivity, the conversion rate of levulinic acid or levulinate is 100 percent, the yield of the gamma-valerolactone reaches up to 99 percent above; and the method has a simple operation technology, and is low in cost, safe and environment-friendly.

Description

(1) Technical field [0001] The invention relates to a method for synthesizing gamma-valerolactone by liquid-phase catalytic hydrogenation of levulinic acid and its esters, in particular to synthesizing gamma-valerolactone by catalytic hydrogenation of levulinic acid and its esters under the action of a supported cobalt catalyst Methods. (2) Background technology [0002] γ-valerolactone (also known as 4-methylbutyrolactone), English name Gamma-Valerolactone, molecular formula C 5 h 8 o 2 . γ-valerolactone is a very versatile platform compound, which can be used as liquid fuel, food additive, organic solvent, intermediate of medicine and chemical synthesis, etc. [0003] γ-valerolactone can be generated by first condensation of malonic acid and propionaldehyde to generate corresponding β, γ-unsaturated acid, and then intramolecular condensation of β, γ-unsaturated acid under the catalysis of sulfuric acid. However, this method pollutes the environment more seriously duri...

Claims

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Application Information

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IPC IPC(8): C07D307/33B01J23/75
Inventor 刘迎新张琳陆晓蕾
Owner ZHEJIANG UNIV OF TECH
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