Method for preparing 5-hydroxymethyl-furfural by microwave promotion

A technology of hydroxymethylfurfural and microwave, applied in the field of ionic liquid catalytic system, can solve the problems of lack of environmental friendliness, high efficiency, low-cost effective separation, continuous production, unfavorable HMF industrial production, large amount of silica gel usage, etc., to achieve catalyst and The effect of less solvent consumption, low cost, and shortened reaction time

Active Publication Date: 2009-06-17
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

Although the column chromatography method reported in this patent has realized the separation of HMF and ionic liquid and product purification, the column chromatography method involves the use of volatile organic solvents, the separation volume is small, the silica gel usage is large, the separation cost is high, and the reaction The process involves the use of corrosive acid catalysts such as sulfuric acid, hydr

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  • Method for preparing 5-hydroxymethyl-furfural by microwave promotion
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  • Method for preparing 5-hydroxymethyl-furfural by microwave promotion

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preparation example Construction

[0034] Preparation of ionic liquid solvent: refer to literature (Li C, Zhao Z.Adv.Synth.Catal.2007, 349, 1847; Webb P B, Sellin M F, Kunen TE, et al.J.Am.Chem.Soc.2003, 125 , 15577; Noda A, Watanabe M.Electrochimica Acta.2000, 45, 1265; Sheldrake G N, Schleck D.Green Chem.2007, 9, 1044.) and patent (WO 00 / 16902) prepared and purified dozens of pairs The six-carbon sugar or the ionic liquid containing six-carbon sugar biomass with strong dissolving ability is used for the implementation of the patent of the present invention.

[0035] Selective dehydration of six-carbon sugar or six-carbon sugar source biomass under microwave radiation to prepare HMF comprises the following steps:

[0036] ①Dissolve six-carbon sugar or biomass containing six-carbon sugar in a preheating dissolution system at 50°C to 100°C;

[0037] ②Transfer the aforementioned mixture to a microwave reaction system and react under microwave radiation conditions. The rated frequency used for microwave radiation...

Embodiment 1

[0042] 20 g of ionic liquid [C 4 MIm]Cl and 10 grams of fructose were heated to 100°C in a preheating dissolving system, and fully dissolved; the liquid material was transferred to a microwave reaction system, and reacted for 2 minutes under microwave radiation (frequency 2450MHz); Distillation device, depressurize to 5KPa, distill and remove low boiling point substances; continue to depressurize to 133Pa, distill to collect 114 ° C ~ 116 ° C fractions, obtain 6.6 grams of dark yellow liquid product, the nuclear magnetic resonance (NMR) analysis data of this product are: 1 H NMR (400MHz, CDCl 3 ): δ 9.49(s, 1H), 7.20(d, 1H), 6.48(d, 1H), 4.65(s, 2H); 13 C NMR (100MHz, CDCl 3 ): δ 178.2, 161.6, 152.5, 123.9, 110.4, 57.7. The measured data of the product is completely consistent with the NMR data obtained by using the HMF reagent provided by Sigma, and then analyzed by ultraviolet-visible spectroscopy, it is found that the absorption peak is 282nm, which is consistent with th...

Embodiment 2

[0045] 1 g of ionic liquid [C 4 MIm]Cl and 0.1 gram of fructose are heated to 80°C in the preheating dissolving system, fully dissolved; the liquid material is transferred to the microwave reaction system, and reacted for 60 seconds under the microwave radiation condition of power 400W and frequency 2450MHz; take 0.01 gram The sample was immediately quenched with cold water, and the resulting aqueous solution was analyzed by a standard curve method at 282 nm with a UV-visible spectrophotometer, and the yield of HMF was determined to be 99%.

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Abstract

The invention relates to a continuous preparation method for 5-hydroxymethylfurfural (HMF) transformed by a biomass saccharine source under microwave radiation condition by using an ionic liquid as a reaction medium, in particular to a method for continuously preparing and separating HMF. The method comprises the following concrete steps: mixing the ionic liquid and hexose or hexose source biomass as a raw material substrate in a preheating and dissolving system, preheating and dissolving the mixture, feeding the mixture into a microwave reaction system to react for 30 seconds to 30 minutes under the microwave radiation condition so as to efficiently generate the HMF; then feeding the reaction mixture into a depressurizing and distilling system, and distilling the mixture under the condition that an operation temperature is not higher than 180 DEG C to obtain the HMF, wherein the separation yield is as high as 94 percent; and re-feeding the distilled remainder into a preheating system, adding the biomass saccharine source, and then repeating steps of reaction and separation, so as to achieve the aims of recycling of an ionic liquid catalyst system and continuous preparation of the HMF. The method has the advantages of no extra-added catalyst, high HMF selectivity, mild operation condition, quick reaction, reusability of the ionic liquid, low cost, simple process, environmental protection and continuous production, provides a new method for industrialized production of the HMF based on the biomass saccharine source, and opens up a new path for preparing common chemicals in a large scale and replacing fuels.

Description

technical field [0001] The present invention relates to the continuous production of 5-hydroxymethylfurfural (HMF), specifically a kind of biomass sugar source (six-carbon sugar or biomass rich in six-carbon sugar) in ionic liquid under microwave radiation condition It is a process method of continuously and efficiently converting to HMF and recycling the ionic liquid catalytic system. Background technique [0002] 5-Hydroxymethylfurfural is an important fine chemical intermediate and is regarded as a new platform compound based on biomass resources. It is widely used in agricultural chemistry, electrochemistry, cosmetics industry, synthetic pharmaceutical intermediates and other industries. Recently, HMF has been considered as a bridge between carbohydrate resources and the petroleum industry, because 2,5-dimethylfuran (DMF) obtained after selective hydrodeoxygenation of HMF is a high-quality fuel with an energy density higher than that of Ethanol is 40% higher and has lit...

Claims

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Application Information

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IPC IPC(8): C07D307/46B01J31/02
Inventor 赵宗保李昌志
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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