2, 5-furandicarboxylic acid preparing method

A technology of furandicarboxylic acid and dimethyl sulfoxide, applied in the direction of organic chemistry and the like, can solve the problems of low efficiency and low concentration of reaction substrate, and achieve the effects of high efficiency, easy control of oxidation process and few by-products

Inactive Publication Date: 2019-04-23
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the deficiencies of the prior art, and provides a method for preparing 2,5-furandica

Method used

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  • 2, 5-furandicarboxylic acid preparing method
  • 2, 5-furandicarboxylic acid preparing method
  • 2, 5-furandicarboxylic acid preparing method

Examples

Experimental program
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Effect test

Example

[0024] Examples 1~6

[0025] Add 0.7g 5-hydroxymethylfurfural (substrate concentration of 10wt%), 1.57g water and 4.73g polar aprotic solvent to a 20mL autoclave, the polar aprotic solvent includes acetonitrile and dimethyl carbonate , Tetrahydrofuran, ethyl acetate, γ-valerolactone, 1,4-epoxy hexacyclic ring, N,N-dimethylformamide, dimethyl sulfoxide or methyl isobutyl ketone; Add 0.93g of sodium bicarbonate, then add 0.25g of ruthenium carbon (the molar ratio of 5-hydroxymethyl furfural to active component Ru is 40:1) as a catalyst, add it to a sealed reaction vessel, pass in 4MPa oxygen, and stir vigorously (500rpm), heat to 110°C and keep for 10 hours. After the reaction, cool to room temperature and take samples. Use HPLC (Water 2695) for qualitative and quantitative detection, including acetonitrile, dimethyl carbonate, tetrahydrofuran, ethyl acetate, dimethyl The test results of sulfoxide as a polar aprotic solvent are listed in Table 1 with serial numbers 1 to 6.

Example

[0026] Examples 7-9

[0027] Add 0.7g 5-chloromethylfurfural (substrate concentration of 10wt%), 1.57g water and 4.73g 1,4-epoxy hexacyclic ring to a 20mL autoclave, add 0.93g sodium bicarbonate, and then add 0.25g Ruthenium carbon (Ru loading 5%), Ru / ZrO 2 (Ru loading 5%), Pt / Al 2 O 3 (Pt load 5%), Pd / ZrO 2 (Pd load 5%), Ru / Co 3 O 4 (Ru loading 5%), Pt / Fe 3 O 4 (Pt loading 5%) (the molar ratio of 5-hydroxymethyl furfural to active component is 40:1) is used as a catalyst, added to a sealed reaction vessel, fed with 4MPa oxygen, and stirred vigorously (500rpm ), heated to 140°C and kept for 10 hours, finished the reaction, cooled to room temperature and sampled. HPLC (Water 2695) was used for qualitative and quantitative detection, in which ruthenium carbon (Ru loading 5%), Ru / ZrO 2 (Ru loading 5%), Pt / Al 2 O 3 (Pt loading 5%) The detection results of the catalyst are listed in Table 1 with numbers 7-9.

Example

[0028] Examples 10-14

[0029] Add 0.7g 5-hydroxymethyl furfural (substrate concentration is 10wt%), 1.57g water and 4.73g dimethyl sulfoxide into a 20mL autoclave, add 0.45g sodium hydroxide, 0.59g sodium carbonate, 0.77g Potassium carbonate, 1.11g potassium bicarbonate or 0.62g potassium hydroxide, add 0.25g ruthenium carbon (5-hydroxymethyl furfural to active component Ru, the molar ratio is 40:1) as a catalyst , Put into a sealed reactor, put in 4MPa oxygen, stir vigorously (500rpm), heat to 110℃ and keep for 10 hours, after the reaction, cool to room temperature and take samples, use HPLC (Water 2695) for qualitative and quantitative detection, the test results are listed in The serial numbers in Table 1 are 10-14.

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Abstract

The invention discloses a 2, 5-furandicarboxylic acid preparing method. The 2, 5-furandicarboxylic acid preparing method comprises adding a mixture of reaction substrate and a double-component solventsystem into a reactor, then adding in catalysts and alkali, sealing up the reactor, then passing the reactor through a gas source containing oxygen, heating the reactor for reaction to obtain 2, 5-furandicarboxylate, and after the reaction is completed, regulating the pH of reaction liquor with concentrated hydrochloric acid to obtain 2, 5-furandicarboxylic acid. The 2, 5-furandicarboxylic acid preparing method is high in concentration of the reaction substrate as well as yield and purity of target products, energy-efficient and environmentally friendly, thereby having a good application prospect.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and in particular relates to a method for preparing 2,5-furandicarboxylic acid. Background technique [0002] At present, the development of human society has entered the fast lane, and the demand for energy is increasing day by day. Fossil energy, which is the main energy source at present, is being depleted at an accelerated rate. High emissions and high pollution are incompatible. Biomass is the only renewable resource that can replace fossil energy to provide human beings with liquid fuels, materials and chemicals. As an important bio-based platform compound, 5-hydroxymethylfurfural can obtain many high-value chemicals through oxidation, reduction, condensation, and ring opening. Among them, 2,5-furandicarboxylic acid obtained by selective oxidation of 5-hydroxymethylfurfural and its derivatives is an important organic compound intermediate, and was listed as one of the 12 ...

Claims

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Application Information

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IPC IPC(8): C07D307/68
CPCC07D307/68
Inventor 唐兴刘淮孙勇曾宪海林鹿雷廷宙
Owner XIAMEN UNIV
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