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Method for selectively catalytically oxidizing alcohol into aldehyde based on iridium nano particles

A technology for catalytic oxidation and oxidation of alcohols, which is applied in the field of catalysis, can solve problems that have not been reported, and achieve the effects of good selectivity, mild reaction conditions and high reaction rate

Active Publication Date: 2017-06-23
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Su et al.'s research team and our recent research work have demonstrated that IrNPs have good peroxidase-like activity, but the oxidase properties of IrNPs and the method of catalyzing the selective oxidation of DO to aldehydes have not been reported.

Method used

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  • Method for selectively catalytically oxidizing alcohol into aldehyde based on iridium nano particles
  • Method for selectively catalytically oxidizing alcohol into aldehyde based on iridium nano particles
  • Method for selectively catalytically oxidizing alcohol into aldehyde based on iridium nano particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Embodiment 1: Preparation and characterization of Ir NPs oxidase

[0042] (1) Mix 3mL of 1% sodium citrate solution with 20mL of 0.03% IrCl 3 The solutions were mixed, and the pH was adjusted to 7-9 with 1M NaOH solution.

[0043] (2) in N 2 Under protection, the solution was placed in an oil bath to reflux for 20min, the solution turned light yellow, and 1mL of freshly prepared 0.1M NaBH was added 4 Solution, turn off the heating switch, continue to reflux for 30min, the color of the solution turns black, indicating the formation of Ir NPs.

[0044] (3) Add an appropriate amount of ethanol for reverse precipitation, and centrifuge at 3357 rcf for 5 min, wash the precipitate repeatedly with ethanol and centrifuge three times, and finally place it in a vacuum drying oven at 45°C for drying.

[0045](4) An appropriate amount of Ir NPs crystal powder was weighed and dissolved in ultrapure water to prepare a 3 mg / mL Ir NPs stock solution, and the Ir content was determine...

Embodiment 2

[0048] Example 2: Ir NPs Catalyzed DO Oxidation of Lower Alcohols to the Corresponding Aldehydes or Ketones

[0049] (1) Prepare 3mg / mL Ir NPs stock solution with ultrapure water;

[0050] (2) An equal volume of Ir NPs stock solution was added to methanol, ethanol, propanol, and isopropanol, mixed well, and stirred at room temperature for 24 h.

[0051] (3) The solution after the reaction is centrifuged, and the supernatant is taken for GC analysis.

[0052] (4) Determination of conversion rate. Table 1 is the conversion rate of alcohol.

[0053] It can be seen from Table 1 that from the perspective of the conversion rate of lower alcohols, the catalytic efficiency of Ir NPs is very high, and the longer the alkyl chain, the stronger the electron-pushing energy of the alkyl group, and the higher the conversion rate, indicating that Ir NPs can catalyze DO Alcohol oxidation is related to electron transfer between substrates, Ir NPs, and DO.

[0054] The reaction solution was ...

Embodiment 3

[0057] Example 3: Verification of the catalytic mechanism of Ir NPs

[0058] (1) Prepare 3 identical 1,3-diphenylisobenzofuran (DPBF) solutions, dilute one of them to 5mL, and measure its fluorescence spectrum.

[0059] (2) Add Ir NPs to the second DPBF solution, make the volume to 5mL, and measure its fluorescence spectrum.

[0060] (3) Add ascorbic acid (Vc) and Ir NPs sequentially to the third DPBF solution, and also make the volume to 5mL, and measure the fluorescence spectrum.

[0061] (4) Prepare two identical TMB solutions.

[0062] (5) Add an appropriate amount of Ir NPs to one of the TMB solutions, set the volume to 5mL, and measure its UV-vis spectrum after reacting for 5min.

[0063] (6) Add appropriate amount of Ir NPs and benzoquinone solution to another part of TMB solution, set the volume to 5mL, and measure its UV-vis spectrum after the same reaction for 5min.

[0064] DPBF is an O 2 ˉ ·and 1 o 2 scavenger, and cannot capture other active oxygen radicals...

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Abstract

The invention discloses a method for selectively catalytically oxidizing alcohol into aldehyde based on iridium nano particles, which belongs to the technical field of catalysis. The method utilizes sodium citrate as a coating agent and NaBH4 as a reducing agent to synthesize water-soluble Ir NPs with a diameter of 2.5+ / -0.5nm. Since the synthesized Ir NPs has high-index crystal faces {200}, {220} and {311}, the catalytic activity is high, and the DO is catalyzed at the normal temperature and normal pressure to oxidize the alcohol into corresponding aldehyde or ketone. The Ir NPs with the oxidase-like activity is expected to become a substitute of bio-oxidase and has a potential application prospect in a wider application field.

Description

technical field [0001] The invention relates to a method for selectively catalytically oxidizing alcohols into aldehydes based on iridium nanoparticles, and belongs to the technical field of catalysis. Background technique [0002] The selective oxidation of alcohols to the corresponding aldehydes or ketones is a very important process no matter in organic synthesis, fine chemicals, or fuel cells. Dichromate and permanganate are traditional oxidants for converting alcohols to aldehydes, they are not only expensive, but also produce a large amount of heavy metal effluent. At present, low-toxic Ag or Cu are widely used as catalysts in industry to catalyze air oxidation of methanol to formaldehyde, but the conversion process can only be carried out at high temperature (600-700°C). Some metal compounds and nanoparticle catalysts have been synthesized to catalyze dissolved oxygen (Dissolved oxygen, DO) oxidation of alcohols into aldehydes or ketones. The by-product is only water...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/38C07C45/39C07C47/055C07C47/07C07C47/02C07C49/08B01J23/46B82Y40/00
CPCB01J23/46B82Y40/00C07C45/38C07C45/39C07C47/04C07C47/06C07C47/02C07C49/08
Inventor 宋启军崔玛琳王婵赵媛王巍巍
Owner JIANGNAN UNIV
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