Preparation method for Cu-based hydrogenation catalyst

A hydrogenation catalyst, copper-based technology, applied in the direction of organic chemistry, etc., can solve problems such as difficult to control the interface structure of copper and oxides, and achieve the effects of good product preparation uniformity, good universality, and high hydrogenation performance

Inactive Publication Date: 2015-12-16
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, traditional methods are difficult to control the interface structure of copper and oxides

Method used

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  • Preparation method for Cu-based hydrogenation catalyst
  • Preparation method for Cu-based hydrogenation catalyst
  • Preparation method for Cu-based hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] 1) Weigh 1.52g copper nitrate (Cu(NO 3 ) 2 .3H 2 O) and 1.5g of urea were dissolved in 10ml of water, 1.5g of multi-walled carbon nanotubes (CNTs) was added, and stirred at 150°C for 0.5h. Copper nitrate precursor (Cu / CNTs).

[0032] 2) The sample loaded with copper is mixed with ethanol to form a uniform suspension, the concentration of the sample is 0.1g / ml, coated on the surface of the glass sheet, evaporated to dryness and placed in the molecular layer deposition vacuum reaction chamber, the temperature of the chamber is 80°C, the cavity pressure is 50Pa, the cavity volume is 200ml, the carrier gas is nitrogen during the deposition process, and the flow rate is 1sccm-1000sccm, preferably 60sccm.

[0033] 3) Polyurea hybrid film deposited by molecular layer deposition technology:

[0034] (a) The first pulse of diethyl zinc vapor is chemically adsorbed on the surface of the Cu / CNTs sample, and the physically adsorbed part is removed by pumping;

[0035] (b) The ...

Embodiment 2

[0043] Adopt the same method of embodiment 1 to test, and the difference with embodiment 1 is that the number of deposition cycles increases by 120 cycles, and the yield of gamma-valerolactone in levulinic acid hydrogenation is improved to 74%, showing that Zn-poly The thickness of the urea hybrid film can change the number of Cu-ZnO binding sites, and its TOF is 11.2h -1 . This indicates that more Cu-ZnO interfaces can be obtained by increasing the thickness of molecular layer deposition, which improves the intrinsic activity of the catalyst. Example 3:

Embodiment 3

[0044] 1) Weigh 1.9g of copper acetate and dissolve it in 10ml of ethanol, add 7.9g of porous alumina, stir at room temperature for 12h, and dry at 60°C for 24h to prepare alumina-supported copper acetate precursor (Cu / Al 2 o 3 ).

[0045] 2) The sample loaded with copper is mixed with ethanol to form a uniform suspension, the concentration of the sample is 0.03g / ml, coated on the surface of the glass sheet, evaporated to dryness and placed in the molecular layer deposition vacuum reaction chamber, the temperature of the chamber is 90°C, the cavity pressure is 40Pa, the cavity volume is 200ml, the carrier gas is nitrogen during the deposition process, and the flow rate is 1sccm-1000sccm, preferably 50sccm.

[0046] 3) Polyurea hybrid film deposited by molecular layer deposition technology:

[0047] (a) The first pulse of dimethyl zinc vapor chemisorption on Cu / Al 2 o 3 On the surface of the sample, pump air to remove the physically adsorbed part;

[0048] (b) The second p...

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Abstract

A preparation method for a Cu-based hydrogenation catalyst comprises the following steps: dissolving soluble copper salt into water, then adding a carrier into the solution, and uniformly loading a copper precursor on the surface of the carrier to obtain a precursor sample; mixing the precursor sample and ethanol to form a suspending liquid, coating the suspending liquid on the surface of a glass sheet, impulsing polyisocyanate into an MLD reaction cavity, then impulsing an M precursor to be subjected to monomolecular layer reaction on the sample surface in sequence to obtain a hybrid membrane coated copper precursor compound; conducting heat treatment on the compound in air to obtain a nanometer CuO-MOx compound, and then conducting reduction in the reducing atmosphere to obtain the Cu-MOx interface catalyst. The preparation method has the advantage that the Cu-MOx interface structure can be regulated and controlled.

Description

technical field [0001] The invention relates to a method for preparing a metal copper-oxide hydrogenation catalyst by a molecular layer deposition method. Background technique [0002] Copper-based heterogeneous catalysts have high activity and selectivity in hydrogenation reactions of carbonyl compounds such as esters and aldehydes. However, copper has a low melting point, is easily corroded, and is easily deactivated due to loss and sintering during hydrogenation. Usually, copper-based catalysts use methods such as precipitation, ion exchange, and sol-gel to anchor copper nanoparticles on the oxide support, and improve the stability of copper nanoparticles through the channel effect of the support or the interaction between the support oxide and copper. Catalysts prepared by conventional methods are complex in composition and often require a variety of oxide promoters to improve the performance of the catalyst. For example, the Cu-Al-A-B-O catalyst disclosed in CN1037691...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/78B01J23/72B01J23/825C07D307/06C07D307/44C07D307/33
Inventor 覃勇张斌陈耀杨慧敏
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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