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One-pot method for preparing methyl levulinate by mesoporous molecular sieve catalyzed furfural in a near-critical methanol medium

A molecular sieve technology for catalyzing furfural and methyl levulinate, which is applied in molecular sieve catalysts, chemical instruments and methods, preparation of organic compounds, etc. Industrialization and other issues, to achieve the effect of easy recycling, good industrial application prospects, and green process

Active Publication Date: 2018-12-25
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Catalytic hydrogenation of furfural combined with alcoholysis: There are few studies on the direct preparation of methyl levulinate from furfural, only HuX et al. (Hu X, Song Y, Wu L. One-pot synthesis of levulinic acid / ester from C5carbohydrates in a methanol medium .ACS Sustainable Chemistry&Engineering.2013,1(12):1593-1599.) Starting from furfural, in Pt / Al 2 o 3 and Amberlyst-70 catalyzed, H 2 Under the conditions, the yield of methyl levulinate prepared by one-pot method is up to 23%. The reaction has the problems of consuming high-energy-density clean hydrogen and low yield of methyl levulinate, which is difficult to industrialize

Method used

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  • One-pot method for preparing methyl levulinate by mesoporous molecular sieve catalyzed furfural in a near-critical methanol medium
  • One-pot method for preparing methyl levulinate by mesoporous molecular sieve catalyzed furfural in a near-critical methanol medium
  • One-pot method for preparing methyl levulinate by mesoporous molecular sieve catalyzed furfural in a near-critical methanol medium

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Experimental program
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Effect test

Embodiment 1

[0036] Such as figure 1 As shown, add 60g furfural and 300g methanol to a 500mL stirred high temperature and high pressure reactor, the mass ratio of methanol to furfural is 1:5, then add 30g Zr-SBA-15-10, furfural and Zr-SBA-15- The mass ratio of 10 is 2:1; start stirring, heat up to 280 ° C, and react in one pot for 1 h; after the reaction is completed, cool to room temperature, filter, and the filtrate (after sampling, analyzed by GC, the molar yield of methyl levulinate The yield is 18.8%) to obtain methyl levulinate product after distillation, methanol reuse; filter residue to obtain Zr-SBA-15-10 mesoporous molecular sieve, wash with methanol, dry and roast and reuse.

Embodiment 2

[0038] Add 30g of furfural and 300g of methanol into a 500mL stirred high-temperature and high-pressure reactor. The ratio is 3:1; start stirring, heat up to 270°C, and react in one pot for 6h; after the reaction is completed, cool to room temperature, filter, and the filtrate (analyzed by GC after sampling, the molar yield of methyl levulinate is 35.4 %) is distilled to obtain methyl levulinate product, and the methanol is reused; the filter residue is Zr-SBA-15-20 mesoporous molecular sieve, which is washed with methanol, dried and roasted, and then reused.

Embodiment 3

[0040] Add 15g of furfural and 300g of methanol into a 500mL stirred high-temperature and high-pressure reactor. The mass ratio of methanol to furfural is 1:20, and then add 3g of Zr-SBA-15-40. The ratio is 5:1; start stirring, heat up to 260°C, and react in one pot for 8h; after the reaction is completed, cool to room temperature, filter, and the filtrate (analyzed by GC after sampling, the molar yield of methyl levulinate is 35.9 %) is distilled to obtain methyl levulinate product, and the methanol is reused; the filter residue is Zr-SBA-15-40 mesoporous molecular sieve, which is washed with methanol, dried and roasted, and then reused.

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Abstract

The invention discloses a one-pot method for preparing methyl levulinate by catalyzing furfural through a Zr-SBA-15 mesoporous molecular sieve in a near-critical methanol medium. The method comprises the following steps: (1) adding furfural and methanol into a high-temperature and high-pressure reaction kettle with a stirring function, and adding the Zr-SBA-15 mesoporous molecular sieve, wherein the Si / Zr molar ratio of the Zr-SBA-15 mesoporous molecular sieve is 5-100; (2) stirring, heating to 200-280 DEG C, and carrying out one-pot method reaction for 1-16 hours; and (3) after the reaction, cooling to the room temperature, filtering, distilling filtrate to obtain a methyl levulinate product, recycling methanol for later use, collecting filter residues, namely the Zr-SBA-15 mesoporous molecular sieve, washing with methanol, and drying and roasting for later use. The one-pot method has the beneficial effects that the process is simple, the process is environmentally friendly, and the cost is low and further has a good industrial production prospect.

Description

technical field [0001] The invention relates to a method for preparing methyl levulinate from furfural, in particular to a method for preparing methyl levulinate in a near-critical methanol medium by Zr-SBA-15 mesoporous molecular sieves catalyzing furfural in one pot. Background technique [0002] Biomass is an important class of renewable resources. The preparation of chemicals or fuels from biomass resources has become an important way for countries to solve the energy crisis. Among them, lignocellulose-based biomass is widely used due to its large output and wide distribution. focus on. [0003] Methyl levulinate (molecular formula: C 6 h 10 o 3 , CAS No.: 624-45-3,) is a class of short-chain fatty acid esters, an important class of organic chemicals, can be directly used as spices, food additives, gasoline additives and biological liquid fuels, etc., its structural formula is as follows As shown in the figure. [0004] [0005] There are three main ways to prepa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/00C07C69/716B01J29/035
CPCB01J29/035C07C67/00C07C69/716
Inventor 吕秀阳阮厚航吕喜蕾王立新
Owner ZHEJIANG UNIV
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