A One-pot Method for Preparation of 5-HMF Based on MTO 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: 2019-10-11
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 the process that the catalyst is not easy to be reused and the reaction time is long, and the use of the protonic acid catalyst will cause problems such as equipment corrosion and environmental pollution.

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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Patent Type & Authority Patents(China)
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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