A kind of technique for the continuous preparation of methyl levulinate by furfural two-step method

A technology of methyl levulinate and two-step method, which is applied in the field of continuous preparation of methyl levulinate by furfural two-step method, which can solve the problems of low yield of methyl levulinate, consumption of high-energy-density clean hydrogen, and difficulty in industrialization, etc. question

Active Publication Date: 2018-09-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Catalytic hydrogenation of furfural combined with alcoholysis: There are few studies on the direct preparation of methyl levulinate from furfural, currently 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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  • A kind of technique for the continuous preparation of methyl levulinate by furfural two-step method
  • A kind of technique for the continuous preparation of methyl levulinate by furfural two-step method
  • A kind of technique for the continuous preparation of methyl levulinate by furfural two-step method

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Experimental program
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Embodiment 1

[0038] like figure 1 As shown, in situ hydrogenation fixed bed reactor filled with Cu / MgO-Al 2 o 3 , Amberlyst-21 is filled in the acid-catalyzed alcoholysis fixed-bed reactor; furfural is dissolved in isopropanol to form a homogeneous solution, wherein the mass fraction of furfural is 10%, and the solution is pressurized by metering pump 1 and preheater 1 After preheating, it is continuously added to the in-situ hydrogenation fixed-bed reactor for reaction, wherein the reaction temperature of the in-situ hydrogenation fixed-bed reactor is 150°C, the reaction residence time is 60min, and the reactor pressure is 5MPa; the reaction liquid passes through the back pressure valve 1 Outflow, separated by rectification tower 1, furfuryl alcohol mixed with methanol to form a homogeneous solution at the bottom of the tower, wherein the mass fraction of furfuryl alcohol is 10%, the solution is pressurized by metering pump 2, preheated by preheater 2, and then acid-catalyzed alcohol is ...

Embodiment 2

[0040] Filling Cu / MgO-Al in a fixed-bed reactor for in-situ hydrogenation 2 o 3 , Amberlyst-70 is filled in the acid-catalyzed alcoholysis fixed-bed reactor; furfural is dissolved in isopropanol to form a homogeneous solution, wherein the mass fraction of furfural is 15%, and the solution is pressurized by metering pump 1 and preheater 1 After preheating, it is continuously added to the in-situ hydrogenation fixed-bed reactor for reaction, wherein the reaction temperature of the in-situ hydrogenation fixed-bed reactor is 170°C, the reaction residence time is 40min, and the reactor pressure is 5MPa; the reaction liquid passes through the back pressure valve 1 Outflow, separated by rectification tower 1, furfuryl alcohol mixed with methanol to form a homogeneous solution at the bottom of the tower, wherein the mass fraction of furfuryl alcohol is 15%, the solution is pressurized by metering pump 2, preheated by preheater 2, and then acid-catalyzed alcohol is added continuously ...

Embodiment 3

[0042] Filling Cu / MgO-Al in a fixed-bed reactor for in-situ hydrogenation 2 o 3 , Amberlyst-70 is filled in the acid-catalyzed alcoholysis fixed-bed reactor; furfural is dissolved in isopropanol to form a homogeneous solution, wherein the mass fraction of furfural is 20%, and the solution is pressurized by metering pump 1 and preheater 1 After preheating, it is continuously added to the in-situ hydrogenation fixed-bed reactor for reaction, wherein the reaction temperature of the in-situ hydrogenation fixed-bed reactor is 170°C, the reaction residence time is 40min, and the reactor pressure is 5MPa; the reaction liquid passes through the back pressure valve 1 Outflow, separated by rectification tower 1, furfuryl alcohol mixed with methanol to form a homogeneous solution at the bottom of the tower, wherein the mass fraction of furfuryl alcohol is 20%, the solution is pressurized by metering pump 2, preheated by preheater 2, and then acid-catalyzed alcohol is added continuously ...

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Abstract

The invention discloses a technique for continuously preparing methyl levulinate by a furfural two-step process. The technique comprises the following steps: 1) filling an in-situ hydrogenation fixed-bed reactor with a supported non-noble metal catalyst, and filling an acid-catalyzed alcoholysis fixed-bed reactor with a solid acid catalyst; 2) dissolving furfural in isopropanol to form a homogeneous solution, pressurizing the solution through a measuring pump 1, preheating the solution through a preheater 1, continuously adding the solution into the in-situ hydrogenation fixed-bed reactor, and reacting; 3) separating the reaction solution by a rectification tower 1, mixing the furfuryl alcohol obtained on the tower bottom with methanol to form a homogeneous solution, pressurizing the solution through a measuring pump 2, preheating the solution through a preheater 2, continuously adding the solution into the acid-catalyzed alcoholysis fixed-bed reactor, and reacting; and 4) separating the reaction solution by a rectification tower 2, and obtaining the methyl levulinate product from the tower bottom. The technique implements continuous production on the methyl levulinate, has the advantages of high treatment capacity, stable long-time operation catalytic activity and high product yield, is suitable for large-scale industrial application, and has favorable industrialization application prospects.

Description

technical field [0001] The invention relates to a process for continuously preparing methyl levulinate from furfural, in particular to a process for continuously preparing methyl levulinate with furfural in two steps. Background technique [0002] Biomass is an important renewable resource, and the preparation of important chemical platform compounds from biomass resources has become an important research topic in the chemical industry. my country's annual biomass output exceeds 2.1 billion tons, of which agricultural straw exceeds 700 million tons and forest biomass exceeds 1.4 billion tons. Biomass components are mainly cellulose, hemicellulose and lignin, and the content of the three accounts for more than 90% of the total biomass; among them, furfural is the most important primary product from hemicellulose. [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 chem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/716C07C67/00C07D307/44
CPCC07C67/00C07D307/44C07C69/716
Inventor 吕秀阳阮厚航吕喜蕾王立新
Owner ZHEJIANG UNIV
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