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Method for realizing continuous synthesis of 5-hydroxymethylfurfural through continuous extraction

A technology for extracting hydroxymethylfurfural, which is applied in the field of continuous synthesis of 5-hydroxymethylfurfural, can solve the problems of high single-pot yield, large reaction space, and inapplicability to large-scale production, and achieves improved yield and high efficiency. Effects of transformation and prolonging the usage period

Inactive Publication Date: 2017-06-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
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Problems solved by technology

However, the batch-type preparation of 5-hydroxymethylfurfural cannot guarantee a higher single-pot yield, and a large amount of extractant in the reactor takes up a large amount of reaction space, and after the reaction scale is enlarged, mutually incompatible Mass transfer between the two phases is also affected
Therefore, the above two production processes are not suitable for large-scale production

Method used

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  • Method for realizing continuous synthesis of 5-hydroxymethylfurfural through continuous extraction
  • Method for realizing continuous synthesis of 5-hydroxymethylfurfural through continuous extraction
  • Method for realizing continuous synthesis of 5-hydroxymethylfurfural through continuous extraction

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Effect test

Embodiment 1

[0051] Using the above method, the reaction phase composed of 15g glucose, 30g ionic liquid (BMIMCl), 0.74g, and 6.0g water was reacted for 1 hour at 90°C and a pressure of 0.2Mpa, and ethylene glycol dimethyl ether was preheated to 90°C During the reaction process, ethylene glycol dimethyl ether continuously flows through the reaction phase at a speed of 10ml / min, and 5-hydroxymethylfurfural is continuously extracted out of the reaction system, and then flows into the separation system through the extraction agent quiet system for separation. The conversion rate of glucose was 26.4%, and the selectivity of 5-hydroxymethylfurfural was 70.5%.

Embodiment 2

[0053] Using the above method, 15g glucose, 30g ionic liquid (monobutyltrimethylimidazole chloride (BMIMCl)), 1.1g CrCl 3 -6H 2 O. The reaction phase composed of 6g water was reacted for 15 minutes at 130°C and pressure 2.0MP. During the reaction, ethylene glycol dimethyl ether was continuously preheated to 130°C and continuously transported at a speed of 20ml / min to enter the continuous reaction The device continuously flows through the reaction phase for extraction, and flows into the separation system through the extraction agent static system for separation. The conversion rate of glucose obtained was 97.6%, and the selectivity of 5‐hydroxymethylfurfural was 50.29%. Adopt the same proportioning, under the same reaction temperature and reaction time, in the batch tank reactor of small-scale magnetic force agitation, under the reaction condition that adds the extraction agent of reaction phase system 3 times, the conversion rate of glucose is only 66%, 5- The selectivity o...

Embodiment 3

[0055] Adopt above-mentioned method, will be made of 33gBMIMCl, 1.2g CrCl 3 -6H 2 The reaction phase composed of O, 6g water and 15g glucose was reacted for 10 minutes at 182°C and a pressure of 2.8Mpa. During the reaction, ethylene glycol dimethyl ether was preheated to 200°C and continued at a speed of 30ml / min. Flowing through the reaction phase, 5-hydroxymethylfurfural is extracted from the reaction phase, and flows into the separation system through the extraction agent static system for separation. The obtained glucose conversion rate is 96.9%, and the selectivity is 57.8%.

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Abstract

The invention discloses a method for realizing continuous synthesis of 5-hydroxymethylfurfural through continuous extraction. The method comprises the following steps: in a reaction system for generating the 5-hydroxymethylfurfural, continuously feeding an extracting agent and continuously extracting the 5-hydroxymethylfurfural generated in the reaction system; bringing the 5-hydroxymethylfurfural out of the reaction system to realize continuous production of the 5-hydroxymethylfurfural. A production process of the 5-hydroxymethylfurfural by utilizing glucose, provided by the invention, can realize large-scale production of the 5-hydroxymethylfurfural under a green and clean production process condition, and has wide application prospect.

Description

technical field [0001] The invention relates to the technical field of chemical reaction, in particular to a method for realizing the continuous synthesis of 5-hydroxymethylfurfural through continuous extraction. Background technique [0002] With the depletion of fossil resources such as oil and natural gas in the world, it is imperative to seek alternative resources. Biomass resources (plants, animals, microorganisms) are produced by photosynthesis and are a renewable resource. Therefore, it is of great research significance to replace traditional fossil resources with biomass to prepare fine chemicals required by humans. 5-Hydroxymethylfurfural has a furan ring, an aldehyde group and a hydroxyl group. It is a chemical intermediate with active chemical properties. It can generate various derivatives through oxidation, hydrogenation and other reactions. It is a promising fine chemical raw material. The preparation of 5-hydroxymethylfurfural from biomass-based raw materials...

Claims

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Application Information

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IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 张宗超夏至毛燎原
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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