One-pot 5-HMF (5-hydroxymethylfurfural) preparation method based on MTO (methyltrioxorhenium) composite catalyst

A composite catalyst, 5-HMF technology, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc. Repeated use, equipment corrosion environment and other problems, to achieve the effect of less catalyst dosage, simple reaction process and no environmental pollution

Active Publication Date: 2017-10-10
LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

5-HMF is usually directly prepared by dehydration of fructose, but fructose has less reserves and higher price in nature, which limits the large-scale production of 5-HMF
However, there are problems in t

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1 MTO / CrCl 3 Preparation of 5-HMF by Catalytic Degradation of Microcrystalline Cellulose with Composite Catalyst

[0020] Weigh 0.01g MTO, 0.005g CrCl 3 In 2.0g of 1-ethyl-3-methylimidazolium chloride ionic liquid, stir and dissolve at 90°C for 10min to form a composite catalyst, then add 0.1g of microcrystalline cellulose and 50μL of water, and heat at 140°C for 30min. After the reaction finishes, extract repeatedly with 10mL ethyl acetate respectively, until the 5-HMF in the reaction solution is completely separated, steam the ethyl acetate in the extraction phase, weigh the quality of 5-HMF, and calculate its separation yield as 45.2%.

[0021] The ethyl acetate in the raffinate was distilled off, and 0.1 g of microcrystalline cellulose was added to react again. The 5-HMF separation yields were 44.8%, 44.1%, 43.6%, 42.5% and 41.2% during the 5 degradation processes, which were reused 5 times.

Embodiment 2

[0022] Example 2 MTO / CuCl 2 -CrCl 3 Preparation of 5-HMF by Catalytic Degradation of Microcrystalline Cellulose with Composite Catalyst

[0023] Weigh 0.01g MTO, 0.003gCrCl 3 and 0.003g CuCl 2 In 2.0g of 1-ethyl-3-methylimidazolium chloride ionic liquid, stir and dissolve at 90°C for 10min to form a composite catalyst, then add 0.1g of microcrystalline cellulose and 50μL of water, and heat at 140°C for 30min. After the reaction finishes, extract repeatedly with 10mL ethyl acetate respectively, until the 5-HMF in the reaction solution is completely separated, steam the ethyl acetate in the extraction phase, weigh the quality of 5-HMF, and calculate its separation yield as 50.3%.

[0024] The ethyl acetate in the raffinate was distilled off, and 0.1 g of microcrystalline cellulose was added to react again. It was reused 5 times, and the separation yields of 5-HMF were 50.3%, 50.5%, 48.6%, 45.3% and 41.8% during the 5 degradation processes.

Embodiment 3

[0025] Example 3 MTO / FeCl 3 -CrCl 3 Preparation of 5-HMF by Catalytic Degradation of Microcrystalline Cellulose with Composite Catalyst

[0026] Weigh 0.01g MTO, 0.003gCrCl 3 and 0.003g FeCl 3 In 2.0g of 1-ethyl-3-methylimidazolium chloride ionic liquid, stir and dissolve at 90°C for 10min to form a composite catalyst, then add 0.1g of microcrystalline cellulose and 50μL of water, and heat at 140°C for 30min. After the reaction finishes, extract repeatedly with 10mL ethyl acetate respectively, until the 5-HMF in the reaction solution is completely separated, steam the ethyl acetate in the extraction phase, weigh the quality of 5-HMF, and calculate its separation yield as 48.3%.

[0027] The ethyl acetate in the raffinate was distilled off, and 0.1 g of microcrystalline cellulose was added to react again. The 5-HMF separation yields were 47.5%, 46.8%, 46.1%, 45.5% and 43.2% in the 5 degradation processes after repeated use for 5 times.

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PUM

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Abstract

The invention relates to a one-pot 5-HMF (5-hydroxymethylfurfural) preparation method based on an MTO (methyltrioxorhenium) composite catalyst. The method comprises steps as follows: an appropriate amount of MTO, a metal chlorine salt and an ionic liquid are taken and dissolved sufficiently at the temperature of 90-100 DEG C, the composite catalyst is prepared, an appropriate amount ofmicrocrystalline cellulose or lignocellulose is added, the mixture reacts for 10-60 min at the temperature of 110-150 DEG C, and the target product, namely, 5-HMF is obtained. 5-HMF is prepared with a one-step method through direct degradation of cellulose, the reaction process is simple, the yield of 5-HMF is higher, and the catalyst MTO is environment-friendly and free of environmental pollution.

Description

technical field [0001] The invention belongs to the field of chemical synthesis methods, and in particular relates to a method for preparing 5-HMF by degrading lignocellulose in one pot based on MTO composite catalyst. Background technique [0002] 5-Hydroxymethylfurfural (5-HMF) is a multifunctional platform compound that can be used in the synthesis of pharmaceutical intermediates, biofuels and polymer materials. For example, 5-HMF can be converted into 2,5-furandicarboxylic acid (FDCA), and FDCA can replace terephthalic acid to produce polyethylene terephthalate and polybutylene terephthalate. Moreover, 5-HMF is also the precursor of 2,5-dimethylfuran and 2-methylfuran, which are potential liquid fuels. 5-HMF is usually directly prepared by dehydration of fructose, but the storage of fructose in nature is low and the price is high, which limits the large-scale production of 5-HMF. Glucose can be isomerized into fructose, therefore, 5-HMF can be prepared from glucose. C...

Claims

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Application Information

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IPC IPC(8): C07D307/46B01J31/34
Inventor 王景芸门楠白雪周明东
Owner LIAONING UNIVERSITY OF PETROLEUM AND CHEMICAL TECHNOLOGY
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