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Method for converting cellulose into 5-hydroxymethylfurfural (HMF)

A technology of hydroxymethyl furfural and cellulose, applied in the direction of organic chemistry and the like, can solve the problems of high cost, low conversion efficiency, complex process conditions of 5-hydroxymethyl furfural, etc., and achieve the effects of mild reaction and simple process

Inactive Publication Date: 2012-07-11
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The embodiment of the present invention provides a method for converting cellulose into 5-hydroxymethylfurfural, which can solve the current problems of complex process conditions, high cost and low conversion efficiency for converting cellulose into 5-hydroxymethylfurfural

Method used

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  • Method for converting cellulose into 5-hydroxymethylfurfural (HMF)
  • Method for converting cellulose into 5-hydroxymethylfurfural (HMF)
  • Method for converting cellulose into 5-hydroxymethylfurfural (HMF)

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Embodiment 1

[0043] This embodiment provides a method for converting cellulose into 5-hydroxymethylfurfural, which specifically includes the following steps:

[0044] Weigh 100mg cellulose, 2.0g ZnCl 2 , put it into a 50ml round bottom flask, shake the flask carefully to make the two solid powders fully contact and mix evenly, put the flask into an oil bath at 95°C, after the heat balance, slowly add 1mol / L hydrochloric acid aqueous solution dropwise with a syringe 0.6ml. (The apparent stoichiometric ratio is: 79% ZnCl 2 Aqueous solution, 3.8wt% cellulose dissolved, the molar ratio of glucose (Glu) to hydrogen ions is 0.97. It takes 45 seconds from the beginning to the end of the dropwise addition to completely infiltrate the whole system, and then add a stirring magnet to stir at a high speed, with an interval of a certain period of time Finally, the reaction device was taken out, a large amount of distilled water was added, cooled and left standing. The water-soluble total carbon (TOC...

Embodiment 2

[0050] This embodiment provides a method for converting cellulose into 5-hydroxymethylfurfural, which specifically includes the following steps:

[0051] Pulverize the laboratory quantitative filter paper; take 100mg of the pulverized sample and 2gZnCl 2 Mix well in a 50ml round-bottomed flask, place in an oil bath at 95°C until the system is thermally balanced; put 0.62mmol of CrCl 3 Dissolve in 1mol / L hydrochloric acid aqueous solution, draw slowly with a syringe and add CrCl-containing 3 0.6ml of aqueous hydrochloric acid solution, start timing from the moment of dropping, and add a stirring magnet after 45s to stir rapidly; after stirring for 1 minute, slowly add 4ml DMSO dropwise; After 2 hours, remove the reaction device from the oil bath and add a large amount of distilled water to cool the reaction system; then remove the reaction solution to constant volume and measure the HMF content by HPLC. The HMF conversion of the filter paper was 27%.

Embodiment 3

[0053] This embodiment provides a method for converting cellulose into 5-hydroxymethylfurfural, which specifically includes the following steps:

[0054] After pulverizing the absorbent cotton; take 100mg of the pulverized sample and 2g ZnCl 2 Mix well in a 50ml round-bottomed flask, place in an oil bath at 95°C until the system is thermally balanced; put 0.62mmol of CrCl 3 Dissolve in 1mol / L hydrochloric acid aqueous solution, draw slowly with a syringe and add CrCl-containing 3 0.6ml of aqueous hydrochloric acid solution, start timing from the moment of dropping, add a stirring magnet after 45s and stir rapidly; after stirring for 1 minute, slowly add 4ml of DMSO dropwise. Add a reflux condenser at the mouth of the flask, and the oil bath temperature rises to 120°C; after 2 hours of reaction, remove the reaction device from the oil bath and add a large amount of distilled water to cool the reaction system; then remove the reaction solution to constant volume and measure the...

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Abstract

The invention discloses a method for converting cellulose into 5-hydroxymethylfurfural (HMF), and belongs to the fields of renewable energy synthesized by using biomass and preparation of chemicals. The method comprises the following steps of: degrading the cellulose in hydrated zinc chloride molten salt into glucose; and catalytically converting the glucose obtained by degrading into the 5-HMF. The 5-HMF is prepared by directly catalytically converting the glucose which is obtained by degrading the cellulose and taken as a raw material under the condition that the glucose is not separated or purified, the method has the advantages that: the method is quick, simple and convenient, the process is simple, reaction is mild and high-efficiency, and a valuable new way is provided for converting the cellulose into heavy chemicals.

Description

technical field [0001] The invention relates to the field of utilizing biomass to synthesize renewable energy and chemical preparation, in particular to a method for converting cellulose into 5-hydroxymethylfurfural. Background technique [0002] Fossil resources represented by petroleum are increasingly depleted, and biomass has attracted much attention as an alternative resource in the future. Its potential applications include the preparation of renewable energy and the synthesis of high-additional chemicals. The most abundant and cheapest biomass resource on the earth is cellulose. The world produces up to 150 billion tons of dry matter through photosynthesis of plants every year, of which the total amount of cellulose and hemicellulose is 85 billion tons. Cellulose is a linear macromolecule connected by glucose as a structural unit through β-1,4 glycosidic bonds. Due to the folding of the long chain of the macromolecule and the interaction of hydrogen bonds between the ...

Claims

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Application Information

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IPC IPC(8): C07D307/58
Inventor 闫立峰赵毅
Owner UNIV OF SCI & TECH OF CHINA
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