Method and device for preparing 5-hydroxymethylfurfural through high fructose corn syrup

A technology of hydroxymethylfurfural and fructose syrup, applied in the direction of organic chemistry, can solve the problems of high fructose price, complex system, low yield, etc., and achieve the effects of reducing the discharge of three wastes, simple equipment, and reducing production costs

Active Publication Date: 2019-06-14
LUOYANG NORMAL UNIV
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Problems solved by technology

[0003] At present, the production of 5-hydroxymethylfurfural is mainly prepared by dehydration of sugar compounds under acid-catalyzed conditions. Among them, fructose is the most suitable raw material for the preparation of 5-hydroxymethylfurfural. However, the price of fructose is relatively high, so the cost is also high; When glucose is used as raw material, an isomerization catalyst needs to be added to the system, resulting in complex system and relatively low yield
Therefore, the simple use of fructose and glucose as raw materials has great limitations.

Method used

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  • Method and device for preparing 5-hydroxymethylfurfural through high fructose corn syrup

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Experimental program
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Effect test

Embodiment 1

[0023] Such as figure 1 As shown, 0.25 L of HCl and 0.75 L of MIBK with a concentration of 0.5 mol / L were pre-added in the reactor I1; ZnCl was pre-added in the reactor II2 2 Concentration of 0.25mol / L aqueous solution 0.25L, MIBK 0.75L. Control the temperature of reactor Ⅰ1 and reactor Ⅱ2 to be 100 o C and 180 o c. Fructose and glucose with a total mass fraction of 25% fructose syrup solution (F55 type, HCl to adjust pH = 0.3) and MIBK were injected into the continuous reactor I1 with a pump, the residence time of the aqueous solution was 60 minutes, and the residence time of the organic phase was 6 minutes. At the same time, the reaction liquid in the continuous reactor I1 is pumped out to the liquid separation tower I3. After liquid separation, the organic phase is transferred to the vacuum distillation tower 5 to obtain the crude product 5-hydroxymethylfurfural after vacuum distillation, and the organic phase MIBK is reused. The water phase in the separator Ⅰ3 is adju...

Embodiment 2

[0025] The difference between this example and Example 1 is that in this example, the B acid added in advance in the reactor I1 is HCl with a concentration of 0.75 mol / L, and the L acid added in the reactor II2 has a concentration of 0.05 mol / L ZnCl 2 , and the organic phase MIBK is replaced by toluene, and the residence time of toluene in the double continuous reactor is 10min. Finally, the yield of crude 5-hydroxymethylfurfural obtained through continuous reaction was 72%.

Embodiment 3

[0027] The difference between this example and Example 1 is: in this example, the B acid added in advance in the reactor I1 is HCl with a concentration of 0.25 mol / L, and the L acid added in the reactor II2 has a concentration of 0.15 mol / L ZnCl 2 , and replace the organic phase MIBK with CH 2 Cl 2 , CH 2 Cl 2 The residence time in the double continuous reactor is 10min. Finally, the yield of crude 5-hydroxymethylfurfural obtained through continuous reaction was 76%.

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Abstract

The invention discloses a method and device for preparing 5-hydroxymethylfurfural through high fructose corn syrup. The high fructose corn syrup is used as a raw material, acid is used as a catalyst,and in an aqueous solution, through a continuous process reaction, fructose and glucose in the high fructose corn syrup are converted to generate the 5-hydroxymethylfurfural. According to the method and device for preparing the 5-hydroxymethylfurfural from the high fructose corn syrup, for the difference of the conversion conditions of the fructose and the glucose in the high fructose corn syrup,a mode of double-reaction-kettle in series is adopted, in the aqueous solution, the fructose and the glucose are converted to generate the 5-hydroxymethylfurfural through the continuous process reaction, in the reaction process, a pure organic solvent is added, the 5-hydroxymethylfurfural in a reaction system is transferred to an organic layer in real time to be extracted in real time, the yield of the 5-hydroxymethylfurfural is further increased, the continuously extracted organic solvent is recycled through reduced pressure distillation, a water phase can be recycled for many times after impurities of the water phase are removed through an adsorption tower, on the one hand, the production cost is effectively lowered, and on the other hand, emission of three wastes is reduced, and thus the pressure of environmental protection in the production process is decreased.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to a method and device for preparing 5-hydroxymethylfurfural from fructose syrup. Background technique [0002] 5-Hydroxymethylfurfural is an important organic chemical intermediate obtained by dehydration of six-carbon sugar, and is one of the important bridge compounds connecting biomass and organic chemicals. 5-Hydroxymethylfurfural contains various groups such as aldehyde group, hydroxyl group and furyl group, and can be used to produce various bulk organic chemicals such as polyester monomers, fuel additives, biofuels, flavors and fragrances, etc. [0003] At present, the production of 5-hydroxymethylfurfural is mainly prepared by dehydration of sugar compounds under acid-catalyzed conditions. Among them, fructose is the most suitable raw material for the preparation of 5-hydroxymethylfurfural. However, the price of fructose is relatively high, so the cost is a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
Inventor 段英邓冬生杨艳良郑敏李东密
Owner LUOYANG NORMAL UNIV
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