Method for preparing 5-hydroxymethylfurfural by degrading carbonhydrate through ionic liquid

A technology of carbohydrates and hydroxymethylfurfural, applied in the direction of organic chemistry, can solve the problem of difficult separation of products, achieve the effect of short reaction time, simple device, and promotion of degradation

Inactive Publication Date: 2012-04-04
ZHEJIANG UNIV
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  • Claims
  • Application Information

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Problems solved by technology

[0007] The invention provides a method for preparing 5-hydroxymethylfurfural (5-HMF) by degrading carbohydrates with an ionic liquid. The reaction-vacuum distillation coupling method based on entrainer enhancement is adopted to promote the degradation of carbohydrates and simultaneously obtain high yield and high yield. The pure 5-hydroxymethylfurfural crystal product solves the problem that the product is difficult to separate in the prior art

Method used

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  • Method for preparing 5-hydroxymethylfurfural by degrading carbonhydrate through ionic liquid
  • Method for preparing 5-hydroxymethylfurfural by degrading carbonhydrate through ionic liquid
  • Method for preparing 5-hydroxymethylfurfural by degrading carbonhydrate through ionic liquid

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Embodiment 1

[0028] use as figure 1 Shown reaction unit, a kind of method that ionic liquid degrades carbohydrate and prepares 5-hydroxymethylfurfural (5-HMF) is as follows:

[0029] Weigh 20 g of [OMIM]Cl and place it in reactor 3 of a three-necked flask, and raise the temperature of the oil bath to 180°C. Weigh 2g fructose and 0.065g IrCl 3 ·(1-2)H 2 O (approximately equivalent to 7 mol% of the amount of fructose) was quickly added to reactor 3 of the three-necked flask. Nitrogen gas was introduced as an entrainer, and the high vacuum oil pump was started to continuously evacuate the reaction system, maintaining the vacuum degree at 300Pa-500Pa, and the reaction was terminated after 10 minutes. The product deposited in the connecting pipe and the two-necked flask separator 8 and the product remaining in the three-necked flask reactor 3 were collected, and the absolute mass of the product was calculated by HPLC.

[0030] product through 1 H-NMR and 13 C-NMR to characterize, respecti...

Embodiment 2～16

[0034] Take the same method and process as Example 1 to prepare 5-hydroxymethylfurfural, the difference is only in the reaction substrate and reaction conditions.

[0035] In Examples 2-16, the ionic liquid is [OMIM]Cl, the entrainer is nitrogen, n-hexane or methyl isobutyl ketone organic vapor, and the vacuum degree of the reaction system is maintained at 300-500Pa.

[0036] When the carbohydrate is fructose, the raw material ratio is: 2g carbohydrate and 0.065g IrCl 3 ·(1-2)H 2 O is dissolved in 20 g [OMIM]Cl.

[0037] When the carbohydrate is glucose, sucrose, α-starch or cellulose, the raw material ratio is: 2g carbohydrate and 0.049g CrCl 3 ·6H 2 O is dissolved in 20 g [OMIM]Cl.

[0038] The reaction substrate, entrainer, reaction temperature and reaction time taken by each embodiment are listed in Table 2.

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Abstract

The invention discloses a method for preparing 5-hydroxymethylfurfural (HMF) by degrading carbonhydrate through ionic liquid. The method comprises the following steps of: adding the carbonhydrate, the ionic liquid and a cocatalyst into a reactor, introducing an entrainer, continuously vacuumizing a reaction system to make the vacuum degree kept between 100 and 500Pa, and performing catalysis reaction at the temperature of between 120 and 180DEG C for 10 to 60 minutes; and during reaction, putting a separator connected with a product outlet of the reactor into an ice bath for collecting a product, wherein the separator is communicated with the product outlet of the reactor through a heat insulating connecting tube, and the separator has the same vacuum degree as the reactor. The catalysis reaction and product separation are coupled, and high vacuum distillation is adopted and the entrainer is introduced in the reaction process to make the generated water and 5-HMF leave the reaction system, so that the aim of enhancing the generation of the 5-HMF and the product separation is fulfilled and a problem that the 5-HMF is hard to separate is effectively solved.

Description

technical field [0001] The invention belongs to the field of utilization of biomass resources, and in particular relates to a method for preparing 5-hydroxymethylfurfural by degrading carbohydrates with an ionic liquid. Background technique [0002] In recent years, due to the gradual depletion of fossil energy, the research on the synthesis of chemical substances from biomass to replace gasoline and chemical intermediates has attracted widespread attention. Among these chemicals synthesized from biomass, 5-hydroxymethylfurfural obtained through carbohydrate degradation is an important platform compound. For example, 5-hydroxymethylfurfural can be used to synthesize 2,5-furanddioic acid, 2,5-furandiol, 2,5-dimethylol Tetrahydrofuran, dimethylfuran, and liquid alkanes, etc. (such as patents: US2009124839, US2009156841, etc.). These synthetic products may be important polymer monomers or important fuel substances. [0003] As high molecular carbohydrates are generally polyc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
Inventor 魏作君李艳任其龙
Owner ZHEJIANG UNIV
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