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Method for rapidly determining content of 5-HMF (hydroxymethylfurfural) in glucose dehydration reaction liquid

A technology of hydroxymethylfurfural and dehydration reaction, applied in the direction of color/spectral characteristic measurement, etc., can solve the problems of gas chromatograph and high performance liquid chromatograph damage, cumbersome operation steps, long detection time, etc., and achieve accurate and reliable measurement results , The operation process is simple and the detection time is short

Active Publication Date: 2015-05-13
HUAIYIN TEACHERS COLLEGE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the content of HMF in the glucose dehydration reaction solution is mostly determined by gas chromatography and high performance liquid chromatography, but the determination process of these two methods requires sophisticated and expensive instruments, a good experimental environment and well-trained operators , and their operation steps are relatively cumbersome, and the detection time is relatively long, which is time-consuming and labor-intensive
In addition, [BMIM]Cl has a certain damage effect on the gas chromatograph and high performance liquid chromatograph itself, so these two methods have certain application limitations in the actual operation process

Method used

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  • Method for rapidly determining content of 5-HMF (hydroxymethylfurfural) in glucose dehydration reaction liquid
  • Method for rapidly determining content of 5-HMF (hydroxymethylfurfural) in glucose dehydration reaction liquid
  • Method for rapidly determining content of 5-HMF (hydroxymethylfurfural) in glucose dehydration reaction liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: Determination of 5-hydroxymethylfurfural content in the glucose dehydration reaction solution according to the following steps

[0024] (a) Accurately prepare 0.010 mg / mL HMF standard solution and dilute it to 0.001, 0.002, 0.004, 0.006 and 0.008 mg / mL respectively, and perform full-band spectral scanning on the ultraviolet spectrophotometer respectively. The scanning results are as follows: figure 1 shown; from figure 1 It can be seen that, under different concentrations, the maximum ultraviolet absorption peak of HMF is at 284 nm, therefore, determine that 284 nm is the maximum absorption wavelength of HMF;

[0025] (b) Prepare 0.01 mg / mL glucose standard solution and 0.1 mg / mL [BMIM]Cl standard solution respectively, and perform full-band spectral scanning on the ultraviolet spectrophotometer respectively. The scanning results are as follows: figure 2 shown; from figure 2 It can be seen that glucose has no UV absorption in the wavelength range of 20...

Embodiment 2

[0037] Example 2: Step (a-c) is the same as embodiment 1; then , 100 mg glucose and 6.9 mg CrCl 2 Add it to 1 g of [BMIM]Cl, seal it, place it in an oil bath and heat it at 120 °C for 30 min; after the reaction is completed, quickly cool down to room temperature in an ice-water bath, add 4 mL of deionized water, and mix well Centrifuge at 10000 rpm for 5 min, and the upper layer is the glucose dehydration reaction solution; the above-mentioned glucose dehydration reaction solution is diluted 2000 times, and its absorbance is measured with a UV spectrophotometer, and the HMF content calculated according to the standard curve in Example 1 is 46.21 mg.

Embodiment 3

[0038] Example 3: Steps (a-c) are the same as in Example 1; then, 100 mg glucose and 14.9 mg CrCl 3 ?6H 2O was added to 1 g [BMIM]Cl, sealed and placed in an oil bath and heated at 120 °C for 30 min; after the reaction was completed, quickly cooled to room temperature in an ice-water bath, added 4 mL of deionized water, and mixed Uniform; centrifuge at 5000 rpm for 10 min, and the upper layer is the glucose dehydration reaction solution; dilute the above glucose dehydration reaction solution 2000 times, measure its absorbance with an ultraviolet spectrophotometer, and calculate the HMF content according to the standard curve in Example 1 to be 50.73 mg .

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Abstract

The invention discloses a method for rapidly determining the content of 5-HMF (hydroxymethylfurfural) in a glucose dehydration reaction liquid. The method comprises the following steps: (1), preparing a 5-HMF standard solution, a glucose standard solution and an ionic liquid standard solution; (2), determining the maximum absorption wavelength of 5-HMF; (3), establishing a 5-HMFstandard curve; (4), preparing the glucose dehydration reaction liquid; (5), performing absorbance detection and content calculation on 5-HMF in the glucose dehydration reaction liquid in the position of the maximum absorption wavelength. According to the method, a used instrument is low in cost, the detection cost is low, the operation process is simple, the detection time is shorter, the determination result is accurate and reliable, and one economical, fast, simple and reliable method is provided for determining the content of 5-HMF.

Description

technical field [0001] The invention belongs to the field of biomass chemical catalysis and quantitative analysis of chemical components, and relates to a determination method, in particular to a rapid determination method for the content of 5-hydroxymethylfurfural in a glucose dehydration reaction liquid. Background technique [0002] 5-Hydroxymethylfurfural (HMF) is a very important platform compound with multiple uses. It can be used to prepare various high-quality biofuels such as 5-ethoxymethylfurfural, ethyl levulinate, γ-valerolactone, 2,5-dimethylfuran and long-chain alkanes, etc., can also produce various high value-added chemicals such as levulinic acid, 2,5-dimethylfuran, 2,5- Furandicarbaldehyde and 2,5-furandicarboxylic acid, etc. Glucose is the most widely distributed and abundant six-carbon sugar in nature, and it is also one of the most commonly used and ideal raw materials for the preparation of HMF. However, because glucose has a special and stable pyra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N21/33
Inventor 胡磊吴真周守勇徐继明
Owner HUAIYIN TEACHERS COLLEGE