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Preparation and application of dual-functional synergetic catalyst for catalyzing biomass reforming to selectively prepare 5-methylfurfural

The technology of methyl furfural and catalyst is applied in the field of preparation and application of bifunctional synergistic catalyst, can solve problems such as low yield of 5-MF, and achieve the effects of good catalytic effect, environmental friendliness and simple operation.

Active Publication Date: 2014-10-01
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are few studies on the preparation of 5-MF from biomass reported in the literature, and the existing catalytic systems are homogeneous reactions, the catalyst uses liquid acid, and the yield of 5-MF is low

Method used

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  • Preparation and application of dual-functional synergetic catalyst for catalyzing biomass reforming to selectively prepare 5-methylfurfural

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Step A: Synthesis of Ti by ion exchange method 4+ Ion intercalated montmorillonite Ti-MMT:

[0022] Add 3.0g Na-MMT to a 500ml four-necked bottle, and the concentration in 200ml is 3.3×10 -2 M acidic TiCl 4 The solution was kept at 50°C and reacted for 24 hours under mechanical stirring. After the reaction, the slurry was filtered and washed with 1 L of deionized water until no Cl ions were detected in AgCl. Samples were dried in a liquid nitrogen freeze dryer. The obtained solid powder was off-white. That is Ti-MMT.

[0023] Step B: load metal: take 1.0g Ti-MMT prepared in step A, add 6mg RuCl 3 Ethanol solution, shaker 200rpm reaction 24h, rotary evaporation to remove the solvent to dryness, add 10ml deionized water to disperse the solid, add NaBH dropwise under the condition of shaker 200rpm 4 , After 4h, the lotion is solid. Freeze dry samples. A catalyst of 0.22% Ru / Ti-MMT was obtained (the metal content was measured by ICP).

[0024] Add 180mg of glucose...

Embodiment 2

[0026] Step A: Synthesis of Ti by ion exchange method 4+ Intercalated montmorillonite Ti-MMT:

[0027] Add 3.0g Na-MMT to a 500ml four-necked bottle, and the concentration in 200ml is 3.3×10 -2 M acidic TiCl 4 The solution was kept at 50°C and reacted for 24 hours under mechanical stirring. After the reaction, the slurry was filtered and washed with 1 L of deionized water until no Cl ions were detected in AgCl. Samples were dried in a liquid nitrogen freeze dryer. The obtained solid powder was off-white. That is Ti-MMT.

[0028] Step B: load metal: take 1.0g Ti-MMT prepared in step A, add 6mg RuCl 3 Ethanol solution, shaker 200rpm reaction 24h, rotary evaporation to remove the solvent to dryness, add 10ml deionized water to disperse the solid, add NaBH dropwise under the condition of shaker 200rpm 4 , After 4h, the lotion is solid. Freeze dry samples. A catalyst of 0.22% Ru / Ti-MMT was obtained (the metal content was measured by ICP).

[0029] Glucose 180mg, NaI224.8m...

Embodiment 3

[0031] Step A: Synthesis of Ti by ion exchange method 4+ Intercalated montmorillonite Ti-MMT:

[0032] Add 3.0g Na-MMT to a 500ml four-necked bottle, and the concentration in 200ml is 3.3×10-2 M acidic TiCl 4 The solution was kept at 50°C and reacted for 24 hours under mechanical stirring. After the reaction, the slurry was filtered and washed with 1 L of deionized water until no Cl ions were detected in AgCl. Samples were dried in a liquid nitrogen freeze dryer. The obtained solid powder was off-white. That is Ti-MMT.

[0033] Step B: load metal: take the Ti-MMT prepared in step A, add 6mg RuCl 3 h 2 O ethanol solution, shaker 200rpm reaction 24h, rotary evaporation to remove the solvent to dryness, add 10ml deionized water to disperse the solid, add NaBH dropwise under the condition of shaker 200rpm 4 , After 4h, the lotion is solid. Freeze dry samples. A catalyst of 0.22% Ru / Ti-MMT was obtained (the metal content was measured by ICP).

[0034] Glucose 180mg, NaI22...

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Abstract

The invention discloses preparation and application of a dual-functional synergetic catalyst for catalyzing biomass reforming to selectively prepare 5-methylfurfural and belongs to the technical field of catalysts. The catalyst mainly consists of montmorillonite supported metal nanoparticles, wherein montmorillonite with cationic intercalation provides an acidic active center; the montmorillonite supported metal nanoparticles provide a metal active center; positive ions in montmorillonite interlayer intercalation are preferentially Ti4<+>, Al<3+> or H<+>; the metal active center is preferentially Ru, Pd, PdCu and PdRu. Glucose isomerization and dehydration are catalyzed in the acid center, the acid-metal center is synergetic with a broken C-O bond, 5-methylfurfural is prepared by catalyzing glucose through a heterogeneous one-step method in the presence of the acid-metal dual-functional catalyst in a synergetic mode, and a reaction is carried out at the temperature of 130 DEG C for 4 hours so as to obtain 5-methylfurfural with the yield of 35.7 percent. The yield of 5-methylfurfural obtained by reacting with 5-hydroxymethylfurfural as a substrate at the temperature of 130 DEG C for 16 hours is 90.9 percent.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular provides the preparation and application of a bifunctional synergistic catalyst for selectively preparing 5-methylfurfural by catalyzing biomass reforming. Background technique [0002] Today's world is facing a shortage of non-renewable resources such as oil and coal, and human beings need to seek sustainable resources. Biomass is a renewable resource that widely exists in nature. The preparation of chemical raw materials and energy from biomass is of great significance. 5-Methylfurfural (5-MF) is widely used in medicine, agrochemicals, cosmetics, etc., and is also a common aromatic compound in the food industry. 5-MF may also be used as a potential antitumor agent. [0003] The industrial large-scale production method of 5-methylfurfural is to react with 2-methylfuran, N,N-dimethylformamide and phosgene or phosphorus oxychloride. But the use of more than equivalent amount...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J23/44B01J23/89C07D307/46
Inventor 何静董肃花
Owner BEIJING UNIV OF CHEM TECH