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A kind of preparation method of 5-hydroxymethylfurfural

A technology of hydroxymethyl furfural and 5-HMF, applied in the field of preparation of biological furfural, can solve the problems of high viscosity, long catalyst preparation time, long reaction time, etc., and achieves mild reaction conditions, good catalytic effect, and strong adjustable denaturation. Effect

Active Publication Date: 2020-11-17
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] As mentioned above, although many inorganic acids, organic acids, solid acids, metal salts, metal-loaded functional materials, etc. can be used as catalysts to realize the conversion of fructose into 5-HMF, the methods that have been publicly reported still have some problems as follows: For example: 1. Using a common water-organic solvent two-phase system, the temperature for effective conversion of fructose is relatively high, usually at 150-180 o C, and the pressure in the reaction system is relatively high; 2, using ionic liquid as solvent, although it is possible to reduce the fructose conversion temperature and shorten the reaction time, the cost of this type of solvent is higher, and the viscosity of ionic liquid is lower at a lower temperature 3. Using a common system, under the action of a catalyst, when selecting relatively mild reaction temperature, pressure and other conditions, although fructose can be effectively converted, the reaction time is relatively long and with the reaction conditions. 4. Although some special catalysts have good catalytic performance, can make the reaction conditions of fructose conversion milder, and the yield of 5-HMF is higher, but the preparation time of these catalysts is relatively long, and it is difficult to obtain , the cost is high, and more toxic substances will be used in the process of preparing the catalyst, etc.

Method used

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  • A kind of preparation method of 5-hydroxymethylfurfural
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  • A kind of preparation method of 5-hydroxymethylfurfural

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1~14

[0025] 60 mg of fructose was added to 1 mL of solvent DMSO with catalyst, some chloride and P 2 o 5 binary complexes of lithium chloride (LiCl), sodium chloride (NaCl), potassium chloride (KCl), zinc chloride (ZnCl) 2 ), magnesium chloride (MgCl 2 ), cobalt chloride (CoCl 2 ), indium chloride (InCl 3 ), tin chloride (SnCl 4 ), chromium chloride (CrCl 3 ), manganese chloride (MnCl 2 ), aluminum chloride (AlCl 3 ), nickel chloride (NiCl 2 ), lanthanum chloride (LaCl 3 ), yttrium chloride (YCl 3 ), the chloride and P in the catalyst 2 o 5 The molar ratio is 1:1, the chloride and P in the catalyst 2 o 5 The ratio of the total molar mass of fructose to the molar mass of fructose is 0.2:1, at 80 o The reaction was carried out at C for 30 min. After the reaction, the samples were tested by high-performance liquid chromatography, and the conversion rate of fructose and the yield of 5-HMF were calculated.

[0026] Table 1 Results of conversion of fructose to 5-HMF cataly...

Embodiment 15~17

[0029] With reference to the steps of implementation example 12, the difference is: NiCl 2 with P 2 o 5 The molar ratio is 0.5:1, 2:1, 3:1, NiCl in the catalyst 2 and P 2 o 5 The ratio of the total molar weight of the fructose to the molar weight of fructose is 0.15:1, 0.3:1, 0.4:1, repeat the above experiment, test the samples, and calculate the conversion rate of fructose and the yield of 5-HMF.

[0030] Table 2 Different NiCl 2 with P 2 o5 Effects of Compounds on Conversion of Fructose to 5-HMF

[0031]

Embodiment 18~19

[0033] With reference to the step of embodiment example 12, difference is: when temperature of reaction is 70 o C, the reaction time is 45 min, when the reaction is 90 o C, the reaction time is 15 min, repeat the above experiment, test the samples, calculate the conversion rate of fructose and the yield of 5-HMF.

[0034] Table 3 Results of conversion of fructose to 5-HMF at different temperatures

[0035]

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Abstract

A method for preparing 5-hydroxymethylfurfural, relating to a method for preparing biological furfural. The invention discloses a method for preparing 5-hydroxymethylfurfural (5-hydroxymethylfurfural) by catalytic conversion in a liquid phase system using fructose-based biomass as a raw material ‑HMF), which involves the efficient catalytic conversion of carbohydrates to produce high value-added chemicals, which belongs to the field of biomass resource conversion and utilization. The method adopts the binary compound of chloride and phosphorus oxide as a catalyst, and can effectively convert the fructose-based biomass raw material into 5‑HMF in an organic solvent under medium and low temperature conditions. The method can adopt many catalysts, the catalyst components are flexible and adjustable, the reaction conditions are mild, and 5-HMF can be obtained relatively quickly, and the yield of 5-HMF is high. The information provided by this method provides a valuable reference for the efficient conversion of sugars.

Description

technical field [0001] The invention relates to a preparation method of biological furfural, in particular to a preparation method of 5-hydroxymethyl furfural. Background technique [0002] Facing the contradiction between the increasing demand for energy from social and economic progress and the depletion of traditional fossil resources, the development and utilization of new renewable energy is an effective measure to alleviate the above problems. At present, research all over the world is focused on the effective utilization of renewable resources. Biomass resources are considered as a potential alternative energy source because of their large reserves, wide distribution, non-polluting, renewable, and ability to reduce carbon dioxide emissions. Utilizing carbohydrates in inedible biomass to produce high value-added fine and fuel chemicals is the main hotspot in the current research field ( Chem. Rev. 2007, 107, 2411-2502). [0003] In recent years, 5-hydroxymethylfurfu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 贾松岩何欣骏马娇王康军
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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