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Xylose one-pot furfuryl alcohol preparation method taking formic acid as hydrogen donor

A xylose and formic acid technology, applied in chemical recovery, organic chemistry, etc., can solve the problems of high energy density hydrogen consumption, no industrial application value, high cost of separation and recovery, low cost, good industrial application prospects, The effect of high yield of furfuryl alcohol

Active Publication Date: 2019-05-31
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following disadvantages: the catalyst Pt is a noble metal, which is expensive; it needs to consume a large amount of hydrogen with high energy density, so it does not have industrial application value
[0013] ·The precious metal Ir catalyst is used, which is expensive;
[0014] ·Using three organic solvents (DMSO, THF, triethylamine), the cost of separation and recovery is high;
[0015] Although the intermediate product does not need to be separated, the two-step reaction conditions are different and the process is complicated

Method used

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  • Xylose one-pot furfuryl alcohol preparation method taking formic acid as hydrogen donor
  • Xylose one-pot furfuryl alcohol preparation method taking formic acid as hydrogen donor
  • Xylose one-pot furfuryl alcohol preparation method taking formic acid as hydrogen donor

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Experimental program
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Effect test

Embodiment 1

[0035] Water and 1,4-dioxane are formulated into a mixed solvent first, and the volume fraction of water is 5%; 200 mL of mixed solvent, 10 g of xylose, 50.3 mL of formic acid, 3.3 g Co-N-C-700 catalyst, wherein the mass concentration of xylose is 50g / L mixed solvent, the mol ratio of xylose and formic acid is 1:20, and the mass ratio of xylose and Co-N-C-700 catalyst is 3:1; Start stirring, stirring speed 500rpm, heat up to 130°C, dehydration and hydrogen transfer one-pot reaction for 12h; after the reaction, cool to room temperature and filter; the filtrate (analyzed by GC-FID after sampling, the molar yield of furfuryl alcohol is 43.36%) to obtain furfuryl alcohol product after rectification, the organic solvent is reused; the filter residue is reused as a catalyst after being washed and dried.

Embodiment 2

[0037]Water and 1,4-dioxane are formulated into a mixed solvent first, and the volume fraction of water is 10%; 200 mL of mixed solvent, 10 g of xylose, 50.3 mL of formic acid, 3.3 g Co-N-C-700 catalyst, wherein the mass concentration of xylose is 50g / L mixed solvent, the mol ratio of xylose and formic acid is 1:20, and the mass ratio of xylose and Co-N-C-700 catalyst is 3:1; Start stirring, stirring speed 500rpm, heat up to 140 ° C, dehydration and hydrogen transfer one-pot reaction 10h; after the reaction, cool to room temperature, filter; filtrate (analyzed by GC-FID after sampling, the molar yield of furfuryl alcohol is 56.39%) after rectification to obtain furfuryl alcohol product, the organic solvent is reused; the filter residue is washed and dried and reused as a catalyst.

Embodiment 3

[0039] Water and 1,4-dioxane are formulated into a mixed solvent first, and the volume fraction of water is 15%; 200 mL of mixed solvent, 10 g of xylose, 50.3 mL of formic acid, 3.3 g Co-N-C-700 catalyst, wherein the mass concentration of xylose is 50g / L mixed solvent, the mol ratio of xylose and formic acid is 1:20, and the mass ratio of xylose and Co-N-C-700 catalyst is 3:1; Start stirring, stirring speed 500rpm, heat up to 140 ° C, dehydration and hydrogen transfer one-pot reaction 10h; after the reaction, cool to room temperature, filter; filtrate (analyzed by GC-FID after sampling, the molar yield of furfuryl alcohol is 65.08%) after rectification to obtain furfuryl alcohol product, the organic solvent is reused; the filter residue is washed and dried and reused as a catalyst.

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Abstract

The invention discloses a xylose one-pot furfuryl alcohol preparation method taking formic acid as a hydrogen donor. The method comprises following steps: (1) preparing a mixed solvent from water andan organic solvent, wherein the volume percentage of water is 5 to 50%; sequentially adding the mixed solvent, xylose, formic acid, and a metal supported nitrogen doped carbon catalyst into a high temperature high pressure reactor with a stirring function, wherein the mass concentration of xylose is 10 to 200 g / L (mixed solvent), the mole ratio of xylose to formic acid is 1:5-1:30, and the mass ratio of xylose to the metal supported nitrogen doped carbon catalyst is 1:1-5:1; (2) starting stirring, raising the temperature to 120 to 200 DEG C, and carrying out dehydration and hydrogen transfer reactions in one pot for 20 minutes to 15 hours; and (3) after reactions, cooling the reactor to the room temperature, filtering, rectifying the filtrate to obtain a furfuryl alcohol product, recovering the organic solvent, washing the filter residues, and drying to recover the catalyst. The technology is simple and green, the furfuryl alcohol yield is high, the cost is low, hydrogen with high energy density is not used, and the method has a good industrial application prospect.

Description

technical field [0001] The invention relates to a method for preparing furfuryl alcohol in a one-pot method using xylose under the hydrogen supply of formic acid. Background technique [0002] The preparation of chemicals from biomass is a major trend in the future, and furfuryl alcohol is an important platform chemical that can be prepared from biomass. [0003] Furfuryl alcohol (Furfuryl alcohol, CAS number: 98-00-0), the structural formula is as follows. [0004] [0005] Furfuryl alcohol is a colorless liquid that turns brown when exposed to sunlight or air. It is miscible with water and easily soluble in ethanol, ether, benzene and chloroform. Furfuryl alcohol is mainly used to produce various types of resins with excellent properties, and is also used to prepare fruit acids, plasticizers, solvents and rocket fuels. In addition, furfuryl alcohol is also widely used in industries such as dyes, synthetic fibers, rubber, pesticides and foundry. [0006] The tradition...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/44
CPCY02P20/584
Inventor 吕秀阳徐玲吕喜蕾王俊成徐海峰
Owner ZHEJIANG UNIV