Method for one-step synthesis of 5-hydroxymethylfurfural and derivatives thereof by using microwave-microreactor to catalyze fructose

A technology of hydroxymethyl furfural and microreactor, applied in chemical instruments and methods, chemical/physical process, chemical/physical/physical chemical process, etc., can solve the problem of poor catalyst stability, low HMF selectivity, difficult separation and purification, etc. problem, to achieve the effect of less by-products, low energy consumption and high selectivity

Pending Publication Date: 2022-04-12
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the traditional two-step route has high yield and selectivity, it has disadvantages such as cumbersome process and long extraction time. The preparation of HMF and its derivatives by one-step method has become a research hotspot and has attracted widespread attention.
Fructose is ketose and exists preferentially in the form of furanose. It is relatively easy to prepare HMF and subsequent derivatives. However, in the prior art, HMF has disadvantages such as low selectivity, many by-products, poor catalyst stability, and difficulty in separation and purification.

Method used

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  • Method for one-step synthesis of 5-hydroxymethylfurfural and derivatives thereof by using microwave-microreactor to catalyze fructose
  • Method for one-step synthesis of 5-hydroxymethylfurfural and derivatives thereof by using microwave-microreactor to catalyze fructose
  • Method for one-step synthesis of 5-hydroxymethylfurfural and derivatives thereof by using microwave-microreactor to catalyze fructose

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Embodiment 1: The preparation process of wave-absorbing catalyst MOx / CNTs is as follows:

[0039] Modified carbon nanotubes were obtained by vapor deposition: 5 g of multi-walled carbon nanotubes were placed in a corundum crucible and placed in a tube furnace. Vacuumize the tube furnace and feed pure argon gas, the argon gas flow rate is 100mL / min, and the temperature is raised to 900 °C at a heating rate of 5-10 °C / min; then feed ammonia gas with a volume fraction of 5%, and keep 2h to obtain nitrogen-doped carbon nanotubes, and slowly lower to room temperature after heating.

[0040] Preparation of MOx / CNTs catalyst by impregnation method: 0.5 g nitrogen-doped carbon nanotubes were impregnated in 5 mL metal salt solution (50 mmol AgCl, CeCl 3 , CuCl 2 , MnCl 2 、CoCl 2 , FeCl 3 , ZrCl 4 dissolved in 5mL deionized water), ultrasonicated for 30min, stirred for 2h to fully disperse, washed with deionized water and ethanol, and vacuum-dried for 2h; then calcined the ...

Embodiment 2

[0041] Embodiment 2: Carried out fructose one-step synthesis HMF in microwave-microreactor

[0042] 6g fructose and 0.5g Co 3 o 4 / CNTs were dissolved in 50 mL deionized water and ultrasonicated for 30 minutes; in the flow mode, the suspension of fructose and wave-absorbing catalyst was used as one phase, the flow rate was set at 0.05 mL / min, and 4-methyl-2-pentanone was used as the other phase. phase, the flow rate is set to 0.5mL / min, the two phases are mixed by a micro-mixer for 20 minutes, and then passed into a U-shaped spiral glass pipe in the heating medium in the microwave reactor. After the temperature of the heating medium is stable, react at 90°C 10 minutes.

[0043] After the reaction ended, the resulting reaction solution took out the organic phase 4-methyl-2-pentanone, and the gained organic phase was diluted with ethanol to a certain number of times. It was qualitatively observed that the main product was HMF by high performance liquid chromatography, and the ...

Embodiment 3

[0044] Embodiment 3: Carried out fructose one-step synthesis FDCA in microwave-microreactor

[0045] Mix 6g fructose and 0.5g CeO 2 / CNTs were dissolved in 50 mL dimethyl sulfoxide and ultrasonicated for 30 minutes; in the flow mode, the suspension of fructose and wave-absorbing catalyst was used as one phase, the flow rate was set at 0.02 mL / min, and pure oxygen was used as the other phase, and the oxygen pressure 2bar, the flow rate is set to 0.1mL / min, the two phases are mixed by a micro-mixer for 20min, and then passed into the U-shaped spiral glass pipe in the heating medium in the microwave reactor. After the temperature of the heating medium is stabilized, the React for 20 minutes.

[0046] After the reaction, the obtained reaction solution was diluted with ethanol to a certain number of times, and the main product was qualitatively observed by high performance liquid chromatography to be FDCA. The yield of FDCA was measured to be 88.61%, and the selectivity was 90.42%...

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Abstract

The invention discloses a method for one-step synthesis of 5-hydroxymethylfurfural and derivatives thereof by catalyzing fructose through a microwave-microreactor, which comprises the following steps: taking suspension containing fructose and a wave-absorbing catalyst as a first phase, and taking pure oxygen or pure hydrogen or 4-methyl-2-pentanone as a second phase, and introducing the first phase and the second phase into a microchannel reaction device, mixing through a micromixer, introducing into a microreactor, and carrying out microwave heating catalytic reaction to obtain 5-hydroxymethylfurfural or any 5-hydroxymethylfurfural derivative in the structure as shown in the formula I. The invention also discloses a preparation method of the 5-hydroxymethylfurfural derivative. According to the invention, by changing the variety of metal oxide nanoparticles loaded in the wave-absorbing catalyst, the selectivity of the product can be effectively controlled, and the generation of by-products is reduced; the catalyst is low in cost and easy to synthesize, and the catalytic effect is still good after multiple cycles; and the microwave reactor and the microreactor are combined, so that an eddy current effect is generated, the heat and mass transfer performance is improved, and continuous production is realized.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a method for one-step synthesis of 5-hydroxymethylfurfural and its derivatives from fructose by using a microwave-microreactor to catalyze fructose. Background technique [0002] With the rapid development of global industrialization, pressing environmental issues have prompted researchers to look for new renewable resources and environmentally friendly alternative resources to minimize the dependence on fossil energy. Biomass is expected to be a carbon source for the production of chemicals in the future. As a widely used platform chemical in biomass production, 5-hydroxymethylfurfural (hereinafter referred to as HMF) is considered as an intermediate connecting biomass resources and petrochemical industry. The derivatives of HMF selective oxidation include 2,5-di Formylfuran (DFF), 5-formyl-2-furancarboxylic acid (FFCA), 5-hydroxymethyl-2-furancarboxylic acid (HMFC...

Claims

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Application Information

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IPC IPC(8): C07D307/46C07D307/68C07D307/42C07D307/36B01J19/00
CPCY02P20/584
Inventor 郭凯张文艳何伟张皓宇唐薇薇
Owner NANJING UNIV OF TECH
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