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Preparation of catalyst for synthesizing hydrotalcite thin film by alcohol oxidation reaction

A hydrotalcite, alcohol oxidation technology, applied in the preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve difficult reactants and reaction products, separation, subsequent activation Easy to fall off and other problems, to achieve uniform dispersion of wafers, increase contact area, and solve the effect of mass diffusion

Inactive Publication Date: 2007-03-07
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing a hydrotalcite-like thin-film catalyst for the synthesis of aldehydes or ketones by alcohol oxidation, which solves the problem that only LDHs powder can be used as a catalyst in the past, and the catalyst is easy to lose and difficult to react with reactants and reaction products. Separation makes it difficult to realize the problem of industrial application; solves the problem that when LDHs are deposited on the substrate, the adhesion of LDHs on the substrate is small, which leads to the problem that the subsequent activation treatment is easy to fall off
At the same time, it also solves the problem of integration of LDHs catalyst and reactor; solves the problem of catalyst recovery and loss of active components

Method used

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  • Preparation of catalyst for synthesizing hydrotalcite thin film by alcohol oxidation reaction
  • Preparation of catalyst for synthesizing hydrotalcite thin film by alcohol oxidation reaction
  • Preparation of catalyst for synthesizing hydrotalcite thin film by alcohol oxidation reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] A 9.0cm×7.0cm aluminum sheet (purity 99.5%) was ultrasonically cleaned with absolute ethanol and deionized water for 3 minutes, and then the surface oxide layer was removed with 0.1mol / L sodium hydroxide solution, and then cleaned with deionized water Put it into an electrolytic cell as an anode, use a lead plate as a cathode, and use 1.0ml / L sulfuric acid solution as an electrolyte. The working voltage is 16V, and the oxidation current is 1.4A. Rinse with deionized water for later use. By X-ray powder diffractometer (XRD) (see Fig. 1), scanning electron microscope (SEM) (see Fig. 2), the characterization result of X-ray energy spectrometer (EDS) (see Fig. 3), show through anodic oxidation in aluminum A porous aluminum oxide film was obtained on the sheet surface.

[0042] 0.4365gNi(NO 3 ) 2 ·6H 2 O and 6.0030g NH 4 NO 3 Dissolve in 150ml of deionized water, pour into a 250ml three-neck flask, and prepare the Ni ion concentration as 0.01mol / L, NH 4 NO 3 A soluti...

Embodiment 2

[0045] The preparation method of aluminum base anodized aluminum is the same as embodiment 1

[0046] 0.4372gNi(NO 3 ) 2 ·6H 2 O and 6.0012g NH 4 NO 3 Dissolve in 150ml of deionized water, pour into a 250ml three-neck flask, and prepare the Ni ion concentration as 0.01mol / L, NH 4 NO 3 A solution with a concentration of 0.5mol / L, cut the aluminum sheet (6.5cm×4.5cm) with anodized surface into small pieces and put them into the solution, stir and impregnate at 50°C for 5h, then add ammonia water dropwise to adjust the pH value to 6.61,80 The reaction was stirred and reacted at ℃ for 24 hours. After the reaction solution was cooled, the film-grown substrate was taken out, washed 5 times with deionized water, and dried at 70 ℃ to obtain NiAlNO 3 - LDHs thin film catalyst.

[0047] The XRD spectrogram of the obtained LDHs thin film catalyst is shown in Figure 10, and the SEM and EDS spectrograms are shown in Figure 11 and Figure 12. The Ni / Al molar ratio in the LDHs film lay...

Embodiment 3

[0049] The preparation method of aluminum-based anodized aluminum is the same as that in Example 1.

[0050] 0.4360gCo(NO 3 ) 2 ·6H 2 O and 5.9999g NH 4 NO 3 Dissolved in 150ml deionized water, poured into a 250ml three-neck flask, and prepared to have a Co ion concentration of 0.01mol / L, NH 4 NO 3 A solution with a concentration of 0.5mol / L, cut the aluminum sheet (6.5cm×4.5cm) with anodized surface into small pieces and put them in the solution, stir and impregnate at 50°C for 5h, then add ammonia water dropwise to adjust the pH value to 7.05, 70 Stir the reaction at ℃ for 12h. After the reaction solution is cooled, take out the substrate with long film, wash it with deionized water for 5 times, and dry it at 70℃ to obtain CoAlCO 3 - LDHs thin film catalyst.

[0051] The XRD spectrogram of the obtained LDHs thin film catalyst is shown in Figure 13, and the SEM and EDS spectrograms are shown in Figure 14 and Figure 15. The Co / Al molar ratio in the LDHs film layer is 1....

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Abstract

The invention relates to a hydrotalcite film catalyst used in alcohol oxidization reaction to compose aldehyde or ketone. Wherein, it uses NH3 .H2O as deposit agent, uses ammonia-ammonium nitrate buffer solution to control pH value, controls the ionization balance and coordination balance, and supplies anode alumina layer to supply aluminum resource, to make LDHs into core and grow on substrate, to obtain LDHs film catalyst whose substrate is aluminum anode alumina. The invention can increase the contact area between reactant and catalyst active component, reduces pressure, accelerates disperse, to disperse LDHs uniformly in the anode oxide surface of aluminum plate, combined with substrate.

Description

technical field [0001] The invention belongs to the technical field of hydrotalcite thin film catalysts, and in particular provides a preparation method for synthesizing hydrotalcite thin film catalysts by alcohol oxidation reaction, using ammonia water as a precipitant coprecipitation method, and preparing in situ on aluminum-based anodic alumina Hydrotalcite-like thin-film catalyst, and the catalyst is applied to alcohol oxidation reaction to synthesize aldehyde or ketone compound. Background technique [0002] Synthesis of aldehydes or ketones by alcohol oxidation is an important basis for modern industry and fine chemical processes. Although there are several methods for the conversion of alcohols to ketones and aldehydes, newer and more selective oxidation methods are still of interest. Oxygen is used as an oxidant to selectively oxidize alcohols to obtain aldehydes or ketones by activating oxygen molecules through catalysts, which is not only economical but also envir...

Claims

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Application Information

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IPC IPC(8): B01J23/835C07C205/44C07C201/12
Inventor 杨兰亢永珍张法智
Owner BEIJING UNIV OF CHEM TECH
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