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A kind of method of synthesizing gamma-valerolactone by catalytic hydrogenation

A technology of valerolactone and cobalt catalysts, which is applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxides/metal hydroxide catalysts, etc., and can solve the problems of expensive and high production costs of noble metal catalysts, Achieve low cost, high activity and stability, and good selectivity

Active Publication Date: 2016-04-13
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 expensive and the production cost is high

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, 1gSiO 2 The carrier is calcined at 500°C for 3 hours;

[0035] 2) Load the active components, set the cobalt load to 15%, and 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 at 20°C for 12 hours, then all the solution and SiO 2 Dry at 110°C for 12 hours, calcinate at 500°C for 4 hours, and finally reduce in hydrogen atmosphere at 500°C for 3 hours to obtain Co / SiO with 15% loading 2 Catalyst 1.15g.

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

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, the conversion rate of levulinic acid detected by gas chromatography is 100%, and the yield of γ-valerolactone is 99.9% .

Embodiment 3

[0040] The catalyst preparation process 1) and 2) are the same as in Example 1, except that the catalyst uses γ-Al 2 O 3 As a carrier, Co / γ-Al with a loading amount of 15% was prepared 2 O 3 catalyst.

[0041] 3) Add 0.3 g Co / γ-Al 2 O 3 The catalyst was added to a 100 ml autoclave, other conditions were the same as in Example 1, the reaction time was 6 hours, the conversion rate of levulinic acid detected by gas chromatography was 100%, and the yield of γ-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 the catalytic hydrogenation of levulinic acid and its esters under the action of a supported cobalt catalyst to synthesize gamma-valerolactone 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 fuels, food additives, organic solvents, pharmaceutical and chemical synthesis intermediates, etc. [0003] γ-valerolactone can be formed by the first condensation of malonic acid and propionaldehyde to form the corresponding β, γ-unsaturated acid, and then β, γ-unsaturated acid undergoes intramolecular condensation under the catalysis of sulfuric acid. However, this method has serious environmental pollution d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/33B01J23/75
Inventor 刘迎新张琳陆晓蕾
Owner ZHEJIANG UNIV OF TECH