Inorganic salt catalytic synthesis method for 5-hydroxy methyl furfural

A technology for hydroxymethyl furfural and inorganic salts, applied in the field of catalyzing synthesis of 5-hydroxymethyl furfural with inorganic salts, can solve the problems of inability to realize large-scale industrial production, difficult recovery of separated products, and high cost of ionic liquids, and achieve a convenient reaction rate , low energy consumption, environmental friendly effect

Inactive Publication Date: 2016-02-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The use of homogeneous catalysts such as concentrated sulfuric acid and concentrated hydrochloric acid has many problems, including high toxicity and high corrosion
In addition, a large number of homogeneous catalysts will make the later separation and product recovery difficult
Later, ionic liquid was widely used due to its high conversion rate and high yield, and produced less impurities, but the cost of ionic liquid was too high to realize large-scale industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In this embodiment, the method for catalyzing the synthesis of 5-hydroxymethylfurfural by inorganic salts specifically comprises the following steps:

[0021] Weigh 1.1g (6mmol) of fructose and 162mg (3mmol) of ammonium chloride and add them into the sealed tube, then add 12mL of ethanol into the sealed tube, seal and react in an oil bath at 100°C for 12h;

[0022] After the reaction stopped, the excess ethanol was removed with a rotary evaporator, then a small amount of saturated sodium chloride solution was added, extracted with ethyl acetate and left to separate layers, the organic layer was collected and spin-dried on a rotary evaporator to obtain reddish-brown liquid, add quantitative mesitylene to it, use 1 HNMR calculated 33% yield of 5-hydroxymethylfurfural.

Embodiment 2

[0024] In this embodiment, the method for catalyzing the synthesis of 5-hydroxymethylfurfural by inorganic salts specifically comprises the following steps:

[0025] Weigh 1.1g (6mmol) of fructose and 510mg (3mmol) of nickel chloride and add them into the sealed tube, then add 12mL of ethanol into the sealed tube, seal and react in an oil bath at 100°C for 12h;

[0026] After the reaction stopped, the excess ethanol was removed with a rotary evaporator, then a small amount of saturated sodium chloride solution was added, extracted with ethyl acetate and left to separate layers, the organic layer was collected and spin-dried on a rotary evaporator to obtain reddish-brown liquid, add quantitative mesitylene to it, use 1 HNMR calculated 19% yield of 5-hydroxymethylfurfural.

Embodiment 3

[0028] In this embodiment, the method for catalyzing the synthesis of 5-hydroxymethylfurfural by inorganic salts specifically comprises the following steps:

[0029] Weigh 1.1g (6mmol) of fructose and 162mg (3mmol) of ammonium chloride and add them into the sealed tube, then add 12mL of ethyl acetate into the sealed tube, seal and react in an oil bath at 100°C for 12h;

[0030] After the reaction stopped, a small amount of saturated sodium chloride solution was added, extracted with ethyl acetate and left to separate layers, the organic layer was collected, and spin-dried on a rotary evaporator to obtain a reddish-brown liquid, to which a quantitative amount of mesitylene was added, use 1 HNMR calculated 19% yield of 5-hydroxymethylfurfural.

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Abstract

The invention discloses an inorganic salt catalytic synthesis method for 5-hydroxy methyl furfural. The method comprises the steps that sugar used as a raw material and inorganic salt used as a catalyst react under the effect of an organic solvent, the mole ratio of the sugar to the inorganic salt is 2:1, the heating temperature in the reaction process is controlled to 100-120 DEG C, the redundant organic solvent is removed through a rotary evaporator after the reaction is performed for 0.5-24 h, a sodium chloride saturated solution is added in, extraction is performed through ethyl acetate, organic phases are collected, and therefore the 5-hydroxy methyl furfural is obtained. Due to the fact that the inorganic salt is used as the catalyst, compared with traditional strong acid and other catalysts, produced by-products are reduced, the requirement for equipment corrosion resistance is greatly lowered, energy is saved, no waste liquid harmful to the environment is drained, and large-scale production produces no influence and damage to the environment.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for catalytically synthesizing 5-hydroxymethylfurfural with inorganic salts. Background technique [0002] 5-Hydroxymethylfurfural is a new platform compound based on biomass resources, which is expected to become a new generation of new energy or fuel additives. Its molecule contains an aldehyde group and a hydroxymethyl group, which are unsaturated compounds. Many useful compounds and new polymer materials can be synthesized through chemical reactions such as hydrogenation, oxidative dehydrogenation, halogenation, esterification, and polymerization, including pharmaceuticals. , resinous plastics, diesel fuel additives, etc., 2,5-dimethylfuran can be used as a diesel fuel additive to replace traditional fossil fuels. [0003] At present, the preparation method of 5-hydroxymethylfurfural is mainly biomass hydrolysis method, which has rich sources of raw materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/46
CPCC07D307/46
Inventor 马明肖寒姜鸣邹兵姜素霞
Owner CHINA PETROLEUM & CHEM CORP
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