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A kind of catalyst for cinnamaldehyde MPV reduction to prepare cinnamyl alcohol composite oxide and preparation method thereof

A catalyst, cinnamaldehyde technology, applied in the preparation of hydroxyl compounds, the preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve the problems that do not conform to atomic economy and green chemistry, the separation of catalysts and products is difficult, and the separation of products is difficult. Achieve the effects of good cinnamyl alcohol selectivity, low cost, and cheap and easy-to-obtain raw materials

Active Publication Date: 2018-10-02
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In industry, mainly through homogeneous catalysts such as CeCl 3 It is prepared by complex borohydride reduction method, but it has a significant disadvantage: it is difficult to separate the catalyst and product, and it is easy to inactivate after recovery, and the reaction produces a lot of waste, which is easy to cause environmental pollution
However, this type of reaction usually requires a stoichiometric catalyst, and the catalyst remaining in the medium after the reaction needs to be neutralized with a strong acid. Since the catalyst is a homogeneous catalyst, the separation of the product is difficult, which does not meet the requirements of atomic economy and green chemistry.

Method used

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  • A kind of catalyst for cinnamaldehyde MPV reduction to prepare cinnamyl alcohol composite oxide and preparation method thereof
  • A kind of catalyst for cinnamaldehyde MPV reduction to prepare cinnamyl alcohol composite oxide and preparation method thereof
  • A kind of catalyst for cinnamaldehyde MPV reduction to prepare cinnamyl alcohol composite oxide and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Accurately weigh 1.2g γ-Al 2 o 3 The nanotube powder was dried in an oven at 120° C. for 2 hours, and set aside. Measure 0.35 g of butyl titanate and dissolve in a mixed solution of ethanol and toluene (volume ratio 1:1). The dried γ-Al 2 o 3 The nanotubes were slowly added into a mixed solution of ethanol and toluene, stirred at 25° C. for 20 hours, and then centrifuged. The supernatant was discarded, and the lower layer was taken to precipitate. The centrifuged product was dried in an oven at 120° C. for 4 hours, and then ground into powder. Finally, the obtained powder was placed in a tube furnace, and the temperature was programmed to 400°C at a rate of 5°C / min in an air atmosphere, and after 2 hours of calcination, it was switched to 5% H 2 / N 2 Gas was programmed to heat up to 500°C at a rate of 10°C / min and calcined for 2 hours to prepare the MPV reduction catalyst. The composition and internal structure of the catalyst were characterized by X-ray powder d...

Embodiment 2

[0040] Accurately weigh 1.5g γ-Al 2 o 3 The nanotube powder was dried in an oven at 100° C. for 2 hours, and set aside. Measure 0.4 g of butyl titanate and dissolve in a mixed solution of ethanol and toluene (volume ratio 1:1). The dried γ-Al 2 o 3 The nanotubes were slowly added into a mixed solution of ethanol and toluene, stirred at 30° C. for 20 hours, and then centrifuged. The supernatant was discarded, and the lower layer was removed. The centrifuged product was dried in an oven at 100°C for 6 hours, and then ground into powder. Finally, the obtained powder was placed in a tube furnace, and the temperature was programmed to 500 °C at a rate of 5 °C / min in an air atmosphere, and after 4 hours of calcination, it was switched to 5% H 2 / N 2 Gas was programmed to heat up to 600°C at a rate of 10°C / min and calcined for 3 hours to prepare the MPV reduction catalyst. The morphology of the catalyst was characterized by high-power transmission electron microscopy, such as ...

Embodiment 3

[0042]Accurately weigh 2g γ-Al 2 o 3 The nanotube powder was dried in an oven at 120° C. for 2 hours, and set aside. Measure 0.6 g of butyl titanate and dissolve in a mixed solution of ethanol and toluene (volume ratio 1:1). The dried γ-Al 2 o 3 The nanotubes were slowly added into a mixed solution of ethanol and toluene, stirred at 20° C. for 24 hours, then centrifuged, the supernatant was poured off, and the lower layer was removed. The centrifuged product was dried in an oven at 120° C. for 4 hours, and then ground into powder. Finally, the obtained powder was placed in a tube furnace, and the temperature was programmed to 400 °C at a rate of 5 °C / min in an air atmosphere, and after 4 hours of calcination, it was switched to 5% H 2 / N 2 Gas was programmed to heat up to 600°C at a rate of 10°C / min and calcined for 4 hours to prepare the MPV reduction catalyst.

[0043] The hydrogenation reaction test of cinnamaldehyde was done in a liquid phase reactor. The MPV reduc...

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Abstract

The invention discloses a cinnamyl alcohol catalyst and a preparation method thereof through highly selective reduction of cinnamyl aldehyde by virtue of MPV (Meerwein-Ponndorf-Verley) reaction. The catalyst is composed of composite oxides, and is a supported catalyst with Ti<3+> in the surfaces of gamma-aluminum oxide nano tubes. In the presence of the catalyst, cinnamyl aldehyde can be hydrogenated to obtain cinnamyl alcohol with high conversion rate of 97% and high selectivity of nearly 100%, the catalytic reaction performance of the cinnamyl alcohol catalyst is superior to that of industrial MPV reduction catalyst, aluminum isopropoxide, the reaction process is green and is free of pollution, and the catalyst is easy to recycle. The invention also discloses other preparation methods.

Description

technical field [0001] The invention relates to an MPV (Meerwein-Ponndorf-Verley) reduction catalyst, a preparation method and application thereof. Background technique [0002] Cinnamyl alcohol is an important raw material and intermediate in the production of drugs, spices, pesticides and other fine chemicals, and it is also widely used in organic synthesis. At present, it is mainly prepared by oxidation of olefins or alkylation of unsaturated aldehydes, while another more common preparation method is by chemical reduction of aldehydes or ketones. In industry, mainly through homogeneous catalysts such as CeCl 3 It is prepared by complex borohydride reduction method, but it has a significant disadvantage: it is difficult to separate the catalyst and product, and it is easy to inactivate after recovery, and the reaction produces a lot of waste, which is easy to cause environmental pollution. Therefore, the development of heterogeneous catalysts for the selective hydrogenat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/04C07C33/32C07C29/141
CPCY02P20/584
Inventor 丁维平蔡威盟凌铁杨杰彭路明薛念华章浩龙陈懿
Owner NANJING UNIV