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Catalyst for preparing 2-methyl furan through furfural gas phase hydrogenation, and preparation method thereof

A technology for the preparation of methyl furan and hydrogen, which is applied in the direction of metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problem of aggregation and growth of active component copper particles, experimental Conditions are difficult to control and other problems, to achieve the effect of simple components

Active Publication Date: 2021-10-01
ZHENGZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the selectivity of the catalyst is good, the copper particles of the active component will aggregate and grow during the co-precipitation process, and the experimental conditions are difficult to control

Method used

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  • Catalyst for preparing 2-methyl furan through furfural gas phase hydrogenation, and preparation method thereof
  • Catalyst for preparing 2-methyl furan through furfural gas phase hydrogenation, and preparation method thereof
  • Catalyst for preparing 2-methyl furan through furfural gas phase hydrogenation, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of catalyst 20wt% Cu / SiO for preparing 2-methylfuran by gas-phase hydrogenation of furfural 2 (The percentage in front of the catalyst represents the loading capacity of the active component, the same below) The preparation method, the steps are as follows:

[0036] Preparation of S1, Cu NPs solution:

[0037] S1.1. Weigh 3 mL of polyethylene glycol 200 into a beaker and add 1.4 mL of CuCl 2 solution (2 g / mL), stirred in an ice-water bath at 0 °C for 10 min;

[0038] S1.2. Dialysis bag pretreatment: cut the dialysis bag (molecular weight cut-off 1000 mesh) into small pieces with a length of 5 cm, and prepare NaHCO 3 solution (0.01g / mL) and EDTA disodium solution (0.1g / mL), take 100 mL each in a 250 mL beaker, put the dialysis bag in the beaker and boil for 30 min, wash the dialysis bag with deionized water, and then put the dialysis bag Put in 100 mL EDTA disodium solution (0.1g / mL) and boil for 20 min, cool to room temperature, store at 4 ℃ for later use;

...

Embodiment 2

[0046] Catalyst 20wt% Ni / SiO for preparing 2-methylfuran by gas-phase hydrogenation of furfural 2 The preparation method, the steps are as follows:

[0047] Preparation of S1, Ni NPs solution:

[0048] S1.1. Weigh 5 mL of polyethylene glycol 200 into a beaker and add 0.3 mL of NiCl 2 (10 g / mL) solution, stirred in an ice-water bath at 5°C for 15 min;

[0049] S1.2. Dialysis bag pretreatment: same as step S1.1 in Example 1;

[0050] S1.3. Under the condition of stirring in ice-water bath, add NaBH dropwise with a dropper 4 Solution (0.1 mol / L) solution 10 mL (ready to use), drop it within 10 minutes, continue to stir for 3 hours after the dropwise addition, pour the solution into the dialysis bag in step S1.2, put L deionized water as the dialysate) was stirred for 8 h, and the dialyzed aqueous solution was replaced for 4 h, and finally the solution in the dialyzed bag was transferred to a 500 mL beaker;

[0051] S1.4. Add NaOH solution (0.1 g / mL) dropwise to the solution ...

Embodiment 3

[0055] A kind of catalyst 20wt% Co / SiO for preparing 2-methylfuran by gas-phase hydrogenation of furfural 2 The preparation method, the steps are as follows:

[0056] Preparation of S1, Co NPs solution:

[0057] S1.1. Weigh 6 mL of polyethylene glycol 200 and add 0.15 mL of CoCl 2 (20 g / mL) solution, stirred in an ice-water bath at 2°C for 20 min;

[0058] S1.2. Dialysis bag pretreatment: same as step S1.1 in Example 1;

[0059] S1.3. Under the condition of stirring in ice-water bath, add NaBH dropwise with a dropper 4 solution (0.1 mol / L) solution 15 mL (ready to use), drop it within 10 min, continue to stir for 3 h after the dropwise addition, pour the solution into the dialysis bag in step S1.2, put L deionized water as the dialysate) was stirred for 7 h, the dialyzed aqueous solution was replaced for 3 h, and finally the solution in the dialyzed bag was transferred to a 500 mL beaker;

[0060] S1.4. Add NaOH solution (0.1 g / mL) dropwise to the solution obtained in ste...

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Abstract

The invention belongs to the field of biomass conversion, and discloses a catalyst for preparing 2-methyl furan through furfural gas phase hydrogenation, and a preparation method thereof. The catalyst is composed of a carrier SiO2 and an active component loaded on the carrier SiO2, and the loading amount of the active component is 10-40 wt%. And the active component is a metal simple substance Cu, Co or Ni. The preparation method comprises the following steps: mixing an active component precursor with water to prepare a precursor solution; then mixing the precursor solution and polyethylene glycol in proportion, and stirring for 10-60 min in an ice-water bath at 0-5 DEG C; maintaining the ice-water bath stirring condition, adding a NaBH4 solution, and continuously stirring for 2-4 h after adding is completed; carrying out dialysis treatment by adopting a dialysis bag; after dialysis, transferring the solution in the dialysis bag into a container, adjusting the pH value of the solution to 8-11 by adopting a NaOH solution, and then continuously stirring for 1-5 h; and adding a silicon source, stirring at 40-80 DEG C for 1-8 h, separating, washing, and drying to obtain the catalyst. The catalyst has high dispersity, high activity and high selectivity, the furfural conversion rate is 99%, and the 2-methyl furan selectivity is 90% or above.

Description

technical field [0001] The invention belongs to the field of biomass conversion, and in particular relates to a catalyst for preparing 2-methylfuran by gas-phase hydrogenation of furfural and a preparation method thereof. Background technique [0002] 2-Methylfuran is an important organic chemical raw material, which can be used to synthesize a series of organic chemical products, such as pentadiene, pentanediol, acetylpropanol and related ketones. At the same time, it can be used as a solvent for solution matching process. In addition, 2-methylfuran, as an important pharmaceutical intermediate, plays an important role in the synthesis of vitamins, chloroquine phosphate, and primary ammonium phosphate. [0003] Furfural is an important biomass-based platform compound, which has been industrially produced. my country is the largest furfural producer in the world, with an annual output of about 800,000 tons of furfural, accounting for more than 70% of the world's furfural pr...

Claims

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Application Information

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IPC IPC(8): B01J23/72B01J23/75B01J23/755C07D307/36
CPCB01J23/72B01J23/755B01J23/75C07D307/36
Inventor 刘仲毅刘巧云付鑫鑫
Owner ZHENGZHOU UNIV
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