Preparation method of modified polyaniline catalyst for synthesizing 5-hydroxymethyl furfural

A technology of hydroxymethyl furfural and polyaniline, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of low HMF selectivity and catalyst reuse rate Low catalyst active sites are easily deactivated, etc., to achieve the effects of high catalyst activity, low cost, and easy separation.

Active Publication Date: 2016-04-27
SICHUAN UNIV
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  • Abstract
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  • Claims
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AI Technical Summary

Problems solved by technology

[0007] The present invention aims to provide a method for preparing a high-efficiency and highly stable polyaniline catalyst for the catalytic dehydration of fructose to synthesize HMF, so as to overcome the easy deactivation of the active site of the catalyst, low HMF selectivity, and low catalyst reuse rate in the prior art and other shortcomings

Method used

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  • Preparation method of modified polyaniline catalyst for synthesizing 5-hydroxymethyl furfural
  • Preparation method of modified polyaniline catalyst for synthesizing 5-hydroxymethyl furfural
  • Preparation method of modified polyaniline catalyst for synthesizing 5-hydroxymethyl furfural

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Embodiment 1

[0012] 156mmol of sulfuric acid and 44mmol of freshly distilled aniline monomer were prepared into 200mL aqueous solution. The molar ratio of ammonium persulfate to aniline monomer is 1.4:1. Slowly drop solution B into solution A at a rate of 4 mL / min, and control the solution temperature at 5°C; after the addition is complete, continue stirring at 5°C for 40 minutes; then add 1L of distilled water to dilute and quench the reaction; filter out the solid, Wash with distilled water until the pH of the filtrate is neutral, then wash off the aniline oligomers that may be formed with methanol and ether, and dry the solid at 100°C for 12 hours in vacuum, then grind it into powder. Take 0.2 g of polyaniline salt powder, add 4 mL of 40% formaldehyde aqueous solution by mass percentage, and react at 140° C. for 4 hours. After the reaction, it was naturally cooled to room temperature, filtered, washed with water, sucked dry, and vacuum-dried at 100°C for 12 hours to obtain a modified p...

Embodiment 2-5

[0015] Prepare the catalyst according to the method of Example 1, change the molar ratio of ammonium persulfate to aniline monomer to 0.5, 0.9, 1.8 and 2.3, and use the prepared catalyst for the dehydration reaction of fructose. The reaction results are listed in Table 1.

[0016] Table 1.

[0017]

Embodiment 6-11

[0019] Prepare the catalyst according to the method of Example 1, change the mass ratio of formaldehyde and polyaniline salt to 0.4, 1.1, 2.2, 4.4, 13.2 and 17.6, and use the prepared catalyst for the dehydration reaction of fructose. The reaction results are listed in Table 2 .

[0020] Table 2.

[0021]

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Abstract

The invention relates to a preparation method of a modified polyaniline catalyst for synthesizing 5-hydroxymethyl furfural. The preparation method comprises the following steps of using fresh distilled aniline as a monomer, using ammonium persulfate as an oxidant, synthesizing into a polyaniline salt in a sulfate or hydrochloric acid water solution, and enabling the polyaniline salt and 40% by mass of formalin to react, so as to prepare the modified polyaniline solid base catalyst. The preparation method has the advantages that the preparation of the catalyst is easy, the cost is low, the activity and selectivity on the dewatering of fructose to synthesize the 5-hydroxymethyl furfural are high, the effect of repeated use for multiple times is realized, and the industrial application prospect is good.

Description

technical field [0001] The invention relates to a preparation method of a modified polyaniline catalyst used for synthesizing 5-hydroxymethylfurfural. Background technique [0002] 5-Hydroxymethylfurfural (HMF), molecular formula C 6 h 6 o 3 , Needle crystal, dark yellow liquid or powder, boiling point 114-116°C. HMF is the product of removing three molecules of water from hexose, and has a wide range of industrial applications. It is a monomer for the production of polymers, and can also be used as a raw material to synthesize drugs, drug intermediates, antifungal agents, macrocyclic ligands, and liquid fuels, so it is known as an important bridge compound connecting biomass chemical industry and petrochemical industry . [0003] The existing HMF production method is prepared by acid-catalyzed dehydration of glucose or fructose. However, HMF is thermally unstable at high temperature, and it is very easy to undergo condensation reaction with the reaction intermediate u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/02C07D307/46B01J31/06
CPCB01J31/06C07D307/46C08G73/0266
Inventor 祝良芳代金杭付兴胡常伟
Owner SICHUAN UNIV
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