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Method for preparing biomass fuel oil molecules from biomass platform compound through hydrogenation

A technology of biomass fuel oil and compounds, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, biological raw materials, etc., can solve problems such as catalyst deactivation, and achieve simple preparation process and simple reaction process , highly selective effect

Active Publication Date: 2019-08-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the cycle test of the catalyst, the catalyst showed obvious deactivation in the third cycle reaction

Method used

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  • Method for preparing biomass fuel oil molecules from biomass platform compound through hydrogenation
  • Method for preparing biomass fuel oil molecules from biomass platform compound through hydrogenation
  • Method for preparing biomass fuel oil molecules from biomass platform compound through hydrogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The preparation of embodiment 1 catalyst

[0023] Experiments 1 and 2: Preparation of La-Y and Ce-Y modified carriers: add 0.8476g of LaCl to 100ml round bottom flasks respectively 3 , 0.8517g of CeCl 3 , add 30ml of ultrapure water to dissolve, then add 2.1524g and 2.1482g of Na-Y molecular sieve respectively, stir the obtained mixed solution in a water bath at 50°C for 2 hours, then stir overnight at 80°C until the water evaporates to dryness, and then Calcined at 600° C. for 2 hours to obtain 3 g of 16 wt % La-Y, 16 wt % Ce-Y carrier modified with rare earth elements.

[0024] Experiments 3 and 4: Preparation of H-Y and H-ZSM-5 modified carriers: Weigh 3g of Na-Y and ZSM-5 molecular sieves into 100ml round bottom flasks respectively, and then add 0.10mol / L NH 4 Cl solution 25ml, the resulting mixed solution was kept in a water bath at 50°C for 1 hour, filtered, washed, and then washed with 0.10mol / L NH 4 The Cl solution was ion-exchanged five times, filtered, wash...

Embodiment 2

[0030] Embodiment 2 levulinic acid ester hydrogenation prepares gamma-valerolactone reaction

[0031] Experiment 16-19: Add 5g of ethyl levulinate, or 5g of levulinic acid ester, 45g of solvent, and 0.5g of catalyst into a 50ml reaction kettle, replace the gas with nitrogen for three times, then replace with hydrogen for three times, and then fill Hydrogen to 6MPa, heated to 200°C and stirred for 6 hours. After the reaction was completed, it was lowered to room temperature, and the supernatant liquid was taken and filtered, and the product was detected on an Agilent 7890B gas chromatograph. Calculate the yield of valeric acid, ethyl valerate, gamma-valerolactone, levulinic acid, etc. in the product, and the experimental results are shown in Table 1 (Experiments 16-19).

[0032] The experimental results are shown in Table 1 (Experiments 16-19).

[0033] Table 1 Experimental results of selective hydrogenation of ethyl levulinate to γ-valerolactone with different catalysts.

...

Embodiment 3

[0036] Example 3 Preparation of valeric acid esters by selective hydrogenation of gamma-valerolactone

[0037] The preparation process of 1wt% Ru / La-Y, 1wt% Ru / Ce-Y, and 1wt% Ru / H-Y catalyst is the same as that described in Example 1.

[0038] Experiment 20-22: Add 5g of γ-valerolactone and 0.5g of catalyst into a 50ml reactor, pass through nitrogen to replace the gas three times, then pass through hydrogen to replace three times, then fill with hydrogen to 4MPa, heat up to 220°C and stir for 10 hours . After the reaction was completed, it was lowered to room temperature, and the supernatant liquid was taken and filtered, and the product was detected by Agilent 7890B gas chromatography. The yields of valeric acid, ethyl valerate, gamma-valerolactone, and levulinic acid in the product were calculated, and the experimental results were shown in Table 2 (Experiment 20-22).

[0039] Table 2 Experimental results of preparing valerate by hydrogenation of γ-valerolactone over metal...

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Abstract

The invention provides a method for preparing gamma-valerolactone, valeric acid and valerate from biomass platform molecules. According to the method, the gamma-valerolactone is prepared with levulinate as the reaction raw material, the valeric acid and valerate are prepared with the gamma-valerolactone or levulinate as the raw material, and the process of preparing the gamma-valerolactone from the levulinate, preparing the valeric acid and valerate from the gamma-valerolactone through hydrogenation or efficiently preparing the valeric acid and valerate from the levulinate at high selectivityand high yield through one step is realized. Valerate compounds can serve as biological fuel oil and have high compatibility with an existing fuel oil system; the valeric acid and valerate are prepared through the reaction, and the method has the remarkable advantages that the raw materials serve as the biomass resources and the atom economy is good. Meanwhile, compared with other technologies ofpreparing the valeric acid and valerate with levulinic acid as the raw material, the method has the advantages that the method is simple in reaction process, high in target product yield and mild in reaction condition and medium, and a catalyst is simple in preparing process and stable.

Description

technical field [0001] The present invention relates to a kind of preparation method of biomass fuel oil molecule, specifically prepare gamma-valerolactone by biomass platform compound levulinate, prepare valeric acid and valeric acid ester by hydrogenation of gamma-valerolactone or acetyl A method for preparing valeric acid and valerate by one-step hydrogenation of propionate. Background technique [0002] Valerate is a novel green energy liquid fuel molecule that can be prepared from renewable biomass resources. Lange et al. reported for the first time the preparation of a new type of "valeric acid ester biofuel" based on the hydrogenation conversion of levulinic acid, and conducted a comprehensive study on the properties of this type of fuel. Compared with other biomass-based fuel molecules such as ethanol, butanol, ethyl levulinate, γ-valerolactone, and 2-methyltetrahydrofuran, valerate-based fuels have higher energy density and lower polarity. It is more suitable as a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/33B01J29/12B01J29/44B01J29/14B01J23/46B01J23/652C10L1/02
CPCC07D307/33B01J29/126B01J29/44B01J29/146B01J23/462B01J23/6525C10L1/02C10L2300/20Y02P30/20
Inventor 罗文豪何江王爱琴张涛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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