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A preparation method of rh nanocrystals functionalized with hippocampus tail-shaped phosphonic acid

A phosphonic acid-like, functionalized technology, applied in the field of preparation of hippocampus tail-shaped Rh nanocrystals, to achieve good stability, excellent catalytic activity, and improved catalytic performance

Active Publication Date: 2019-10-25
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, compared with other PGMs such as Au, Ag, and Pd, the surface free energy of Rh is very high, so it is challenging to control the shape of Rh nanocrystals.

Method used

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  • A preparation method of rh nanocrystals functionalized with hippocampus tail-shaped phosphonic acid
  • A preparation method of rh nanocrystals functionalized with hippocampus tail-shaped phosphonic acid
  • A preparation method of rh nanocrystals functionalized with hippocampus tail-shaped phosphonic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0022] 0.5mL 0.08mol / L RhCl 3 Aqueous solution, 4.5mL 0.017mol / L ethylenediaminetetramethylenephosphonic acid aqueous solution was added to a 10mL beaker, mixed evenly, then the pH value of the resulting mixture was adjusted to 14 with 5mol / L KOH aqueous solution, and then added under stirring 1mL of 85% hydrazine hydrate aqueous solution, in which RhCl 3 The molar ratio of ethylenediamine tetramethylene phosphonic acid and hydrazine hydrate is 1:1.9:430, and the reaction is stirred at 80°C for 4 hours to obtain a black suspension, which is centrifuged, washed, and placed in a vacuum oven Dry at 60°C to obtain hippocampus-tail-shaped phosphonic acid-functionalized Rh nanocrystals. Depend on figure 1 and 2 It can be seen that the length of the prepared hippocampus tail-shaped phosphonic acid functionalized Rh nanocrystals is 300-500 nm, and the diameter of the tail end is about 25-40 nm. Depend on image 3 It can be seen that ethylenediaminetetramethylenephosphonic acid is...

Embodiment 2

[0024] 0.5mL 0.08mol / L RhCl 3 Aqueous solution, 3.5mL 0.017mol / L ethylenediaminetetramethylenephosphonic acid aqueous solution and 10mL beaker, mix uniformly, then use 5mol / L KOH aqueous solution to adjust the pH value of the resulting mixed solution to 13, and then Add 1.9 mL of 85% hydrazine hydrate aqueous solution, in which RhCl 3 The molar ratio of ethylenediaminetetramethylenephosphonic acid and hydrazine hydrate is 1:1.5:800, and the reaction is stirred at 70°C for 6 hours to obtain a black suspension, which is centrifuged, washed, and placed in a vacuum oven Dry at 60°C to obtain hippocampus-tail-shaped phosphonic acid-functionalized Rh nanocrystals (see Figure 4 ).

Embodiment 3

[0026] 0.5mL 0.08mol / L RhCl 3 Aqueous solution, 7mL 0.017mol / L ethylenediaminetetramethylene phosphonic acid aqueous solution was added to a 10mL beaker, mixed evenly, then the pH value of the resulting mixture was adjusted to 13 with 5mol / L KOH aqueous solution, and 0.9 mL mass fraction is 85% hydrazine hydrate aqueous solution, wherein RhCl 3 The molar ratio of ethylenediaminetetramethylenephosphonic acid and hydrazine hydrate is 1:3:400, stirring and reacting at 90°C for 3 hours to obtain a black suspension, which is centrifuged, washed, and placed in a vacuum oven Dry at 60°C to obtain hippocampus-tail-shaped phosphonic acid-functionalized Rh nanocrystals (see Figure 5 ).

[0027] In order to prove the beneficial effects of the present invention, the inventors used the hippocampus tail-shaped phosphonic acid functionalized Rh nanocrystals prepared in Example 1 to catalyze the oxidation reaction of o-phenylenediamine at 30°C, and tested with an ultraviolet absorption spe...

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Abstract

The invention discloses a preparation method for a hippocampal tail-shaped phosphonic acid functional Rh nanocrystalline. The method comprises the following steps: taking ethylenediamine tetramethylenephosphonic acid as a complexing agent and a surfactant, taking hydrazine hydrate as a reducing agent and adopting a method for heating in an aqueous solution for reducing RhIII into the hippocampal tail-shaped phosphonic acid functional Rh nanocrystalline in regular shape and uniform size. The preparation method is simple, economic and suitable for industrial large-scale production. The Rh nanocrystalline prepared according to the invention has a unique structure, high stability and water solubility and has an effective effect for concentrating o-phenylenediamine, so that the Rh nanocrystalline can be used as a catalyst for o-phenylenediamine oxidizing reaction and can increase the conversion rate of the o-phenylenediamine reaction.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and in particular relates to a preparation method of hippocampal tail-shaped Rh nanocrystals functionalized with ethylenediaminetetramethylenephosphonic acid (EDTMP). The Rh nanocrystals are used as catalysts in the oxidation reaction of o-phenylenediamine exhibited high catalytic activity. Background technique [0002] Due to the excellent catalytic activity and stability, the controllable synthesis of branched noble metal nanostructures has attracted great attention and has broad applications in industrial catalysis. Currently, aggregation-based nanocrystal growth is the simplest, where nanostructures are rapidly synthesized with the aid of polymeric surfactants. However, the degradation of catalytic activity is often caused by the strong adsorption of macromolecular polymers on metal surfaces. [0003] Rh, as a member of the platinum group metals (PGM), plays an indispensable ro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J23/46C07D241/46
CPCB01J23/464B01J31/0255C07D241/46
Inventor 陈煜朱婧怡
Owner SHAANXI NORMAL UNIV
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