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Method for preparing valerolactone through catalytic hydrogenation of ethyl levulinate

A technology of ethyl levulinate and valerolactone, which is applied in the field of catalytic biomass, can solve the problems of harsh reaction conditions, unfavorable reuse, poor stability, etc., and achieve the effects of less environmental pollution, good reusability, and less trouble

Active Publication Date: 2017-10-13
GUIZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main purpose of the present invention is to provide a kind of method that catalytic hydrogenation ethyl levulinate prepares valerolactone, utilizes a kind of method that catalytic hydrogenation ethyl levulinate prepares valerolactone to solve traditional zirconium-based catalyst, relatively stable Poor, not conducive to repeated use, or harsh reaction conditions, high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Preparation of Microspherical Titanium-Zirconium Oxide Catalysts with Different Molar Ratio

[0030] First weigh a total of 10 mmol of C 12 h 28 o 4 Ti and C 12 h 28 o 4Zr (Ti:Zr=1:0; 8:2; 5:5; 2:8; 0:1) solution was dissolved in 10 ml of CH 3 CH 2 OH to obtain a solution, then 5 mmol (1.2071 g) of hexadecylamine was dissolved in 100 ml of CH 3 CH 2 OH, to which was added 0.55 mL of H 2 O with 0.45 mL of KCl (0.1 M) to obtain a solution of b. Drop the solution a into the solution b under vigorous stirring, and let it stand at room temperature for 18 h.

[0031] Centrifuge the white emulsion with CH 3 CH 2 The white solid was washed with OH, and dried at room temperature to obtain a titanium-zirconium oxide precursor. Weigh 1.2 g precursor and disperse in 15 mL CH 3 CH 2 OH with 7.5 mL H 2 O mixed solution at 160 o C water heat treatment for 16 h, and then filtered, with CH 3 CH 2 OH washing 3 times, 500 in the air o Calcined at C for 2 h t...

Embodiment 2

[0032] Example 2: Application of microspherical titanium-zirconium oxide catalyst in converting ethyl levulinate into valerolactone.

[0033] Weigh 0.072 g of titanium-zirconium oxide catalyst (Ti:Zr=2:8) into a 25-milliliter autoclave, and add 1 mmol (0.1442 g) ethyl levulinate in the reaction kettle, 5 mL iso Propanol (as hydrogen source and solvent), add 0.02 g naphthalene as internal standard, put the reaction kettle at 180 o After reacting for 6 h in C environment, the reaction was stopped, and the reactor was cooled to room temperature in tap water. After filtering the cooled reaction solution, the yield of the product was analyzed by high-performance gas chromatography, and the conversion rate of ethyl levulinate was calculated to be 100% and the yield of valerolactone was 90.1% using the external standard method.

Embodiment 3

[0034] Example 3: The difference from Example 2 is that the titanium-zirconium molar ratio, reaction temperature, and reaction time of the titanium-zirconium catalyst are different. The results are shown in Table 1.

[0035] Table 1

[0036] Catalyst (Ti:Zr)

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PUM

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Abstract

The present invention discloses a method for preparing valerolactone through catalytic hydrogenation of ethyl levulinate. The method comprises: placing ethyl levulinate and different molar ratios of titanium zirconium microsphere catalysts in a device, adding isopropanol as a solvent and a hydrogen source, and carrying out a reaction for 2-10 h at a temperature of 160-200 DEG C, wherein a molar ratio of the titanium zirconium microsphere catalyst is Ti / Zr of 1:0, 8:2, 5:5, 2:8, and 0:1. According to the present invention, the catalytic activity of the method is good, the ethyl levulinate can be completely converted, the yield of the valerolactone can achieve 90.1%, the production cost is reduced by using the alcohol as the hydrogen source, and the catalytic system can be recycled more than 6 times while the catalytic efficiency is not significantly reduced.

Description

technical field [0001] The invention relates to a method for preparing valerolactone by catalytic hydrogenation of ethyl levulinate, especially a method for preparing valerolactone by catalytic hydrogenation of ethyl levulinate under the action of a titanium-zirconium microsphere oxide catalyst, which belongs to catalytic biomass field. Background technique [0002] With the depletion of fuel resources and the continuous improvement of people's demand for energy, the production of biofuels and chemicals from renewable biological resources has attracted increasing attention. Among many valuable biomass chemicals, valerolactone can not only be used as a green solvent, fuel additive, and food additive, but also can be further hydrogenated into 2-methyltetrahydrofuran (2-MTHF) and japonica biofuel, so It has become a biomass platform small molecule that has attracted much attention (Zhang, Z.H. Synthesis of γ-valerolactone from carbohydrates and its applications. ChemSusChem 2...

Claims

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Application Information

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IPC IPC(8): C07D307/33B01J21/06
CPCB01J21/066C07D307/33Y02P20/584
Inventor 杨松杨婷婷李虎贺健刘彦修王忠伟赵文凤
Owner GUIZHOU UNIV
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