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Method for synthesizing 5-hydroxymethylfurfural

A technology of hydroxymethylfurfural and methyl isobutyl ketone, which is applied in the field of 5-hydroxymethylfurfural preparation, can solve the problems of difficult separation and purification of 5-HMF, achieve easy separation, simple post-treatment, and reduce production costs Effect

Inactive Publication Date: 2019-03-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

With the continuous deepening of research, a variety of solvent systems have been developed for the conversion of carbohydrates. Some researchers have generated 5-hydroxymethylfurfural in pure aqueous or organic phases. Compared with pure aqueous phases, in some chemical The result of hydrolysis of carbohydrates in organic solvents is relatively ideal. The reason is that the side reactions of 5-HMF degraded into lower acids such as levulinic acid can be suppressed to a certain extent in organic solvents, but the boiling point of the solvent is usually Higher, making the separation and purification of 5-HMF relatively difficult

Method used

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  • Method for synthesizing 5-hydroxymethylfurfural

Examples

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Comparison scheme
Effect test

Embodiment 1

[0026] Add 50 mg of cellobiose and 25 mg of niobium-modified montmorillonite catalyst into a thick-walled pressure-resistant bottle (15 mL) reactor containing 5 mL of biphasic solvent at the same time. The biphasic solvent is saturated saline and methyl isobutyl Base ketone, the volume ratio is 1.5:3.5, and the thick-walled pressure-resistant bottle is placed in a constant temperature oil bath for reaction, and the reaction temperature is measured by a thermocouple inserted into the oil bath. The reactor has a built-in magnet, and the stirring rate is kept at 500rpm. After a certain reaction time, immediately transfer the reaction vial to an ice-water bath to quench the reaction. Then it is transferred to a suction filter funnel for suction filtration, and the solid catalyst obtained by suction filtration is weighed after washing and drying to ensure that the reuse reaction keeps the same reactant and catalyst ratio as the original reaction, and continues to be used in the nex...

Embodiment 2

[0028] Add 50 mg of cellobiose and 25 mg of niobium-modified montmorillonite catalyst into a thick-walled pressure-resistant bottle (15 mL) reactor containing 5 mL of biphasic solvent at the same time. The biphasic solvent is saturated saline and methyl isobutyl base ketone, the volume ratio is 1:4, and the thick-walled pressure-resistant bottle is placed in a constant temperature oil bath for reaction, and the reaction temperature is measured by a thermocouple inserted into the oil bath. The reactor has a built-in magnet, and the stirring rate is kept at 500rpm. After a certain reaction time, immediately transfer the reaction vial to an ice-water bath to quench the reaction. Then it is transferred to a suction filter funnel for suction filtration, and the solid catalyst obtained by suction filtration is weighed after washing and drying to ensure that the reuse reaction keeps the same reactant and catalyst ratio as the original reaction, and continues to be used in the next st...

Embodiment 3

[0030] Add 50 mg of cellobiose and 25 mg of niobium-modified montmorillonite catalyst into a thick-walled pressure-resistant bottle (15 mL) reactor containing 5 mL of biphasic solvent at the same time. The biphasic solvent is saturated saline and methyl isobutyl base ketone, the volume ratio is 2:3, and the thick-walled pressure-resistant bottle is placed in a constant temperature oil bath for reaction, and the reaction temperature is measured by a thermocouple inserted into the oil bath. The reactor has a built-in magnet, and the stirring rate is kept at 500rpm. After a certain reaction time, immediately transfer the reaction vial to an ice-water bath to quench the reaction. Then it is transferred to a suction filter funnel for suction filtration, and the solid catalyst obtained by suction filtration is weighed after washing and drying to ensure that the reuse reaction keeps the same reactant and catalyst ratio as the original reaction, and continues to be used in the next st...

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Abstract

The invention provides a method for synthesizing 5-hydroxymethylfurfural, and belongs to the technical field of 5-hydroxymethylfurfural preparation. The method comprises the following steps: adding cellobiose, dissolvent saturated saline solution, methyl isobutyl ketone and niobium modified montmorillonite catalyst into a pressure bottle reactor, reacting in a constant-temperature oil bath, and performing dehydration reaction at a certain temperature with a stirring device in the reactor; cooling the temperature of the mixture to room temperature after reaction is completed, performing suctionfiltration, standing and layering the filtrate, and putting 5-hydroxymethylfurfural in dissolvent; taking the solid catalyst obtained in suction filtration for reacting in next cycle. The method hasthe advantages of low cost, simplicity in operation, small corrosion on equipment, recyclable catalyst, and high product yield reaching more than 60 percent.

Description

technical field [0001] The invention is a new method for synthesizing 5-hydroxymethylfurfural in a two-phase solvent with a niobium-modified montmorillonite catalyst, and belongs to the technical field of 5-hydroxymethylfurfural preparation. Background technique [0002] 5-Hydroxymethylfurfural, the English name 5-hydroxymethylfurfural is abbreviated as 5-HMF, light yellow needle crystal, molecular formula C 6 h 6 o 3 , molecular weight 126.11, melting point 28-34°C, boiling point 114-116°C, density 1.243g / mL (25°C), maximum absorption wavelength 284nm, is an important chemical raw material. 5-HMF is easily soluble in water, ethanol, methanol, ethyl acetate, methyl isobutyl ketone, acetone, dimethylformamide, dimethyl sulfoxide, etc.; soluble in chloroform, benzene, ether, etc.; slightly soluble In carbon tetrachloride; insoluble in petroleum ether. It has been recognized as one of the most promising new platform compounds in recent years. It has active chemical properti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
CPCC07D307/46Y02P20/584
Inventor 黄崇品邱果陈娜薇李广超
Owner BEIJING UNIV OF CHEM TECH
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