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Fe nanorod, Pt@Fe nanorod catalyst, and synthesis and application

A nanorod and catalyst technology, applied in the field of preparation of Fe nanorods, can solve few problems and achieve the effects of simple synthesis method, suitable for batch scale-up, excellent catalytic performance and cycle stability

Active Publication Date: 2019-10-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the research on iron nanoparticles in magnetic separation catalysts has not yet been involved.
On the other hand, in the magnetic separation catalysts currently studied, the magnetic materials mainly play the role of dispersing metal nanoparticles and inhibiting the aggregation of the catalyst under the reaction conditions during the catalytic reaction process, and seldom directly participate in the catalytic reaction process.

Method used

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  • Fe nanorod, Pt@Fe nanorod catalyst, and synthesis and application
  • Fe nanorod, Pt@Fe nanorod catalyst, and synthesis and application
  • Fe nanorod, Pt@Fe nanorod catalyst, and synthesis and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 8.1g FeCl 3 ·6H 2 O was dissolved in 80 mL of deionized water. 6.6 g of KOH (purity >85%) was dissolved in 20 mL of deionized water. After complete dissolution, the KOH solution was added dropwise to FeCl3 In the solution, a reddish-brown flocculent precipitate was gradually produced in the solution, and the process was accompanied by strong magnetic stirring. After 3 hours, the magnetic stirring was stopped, and the temperature was raised to 80° C., kept for 4 hours, and then lowered to room temperature. The resulting mixed solution was filtered and washed with deionized water and ethanol four times respectively, and after being washed to neutrality, it was dried in air for 6 hours to obtain a khaki-yellow product. XRD results see figure 1 , all diffraction peaks can be attributed to α-FeOOH (JCPDS#29-0713), which has good crystallinity. TEM results see figure 2 , the synthesized α-FeOOH has a regular nano-rod structure with a diameter of 10-20nm and a length of ...

Embodiment 2

[0049] 8.1g FeCl 3 ·6H 2 O was dissolved in 80 mL of deionized water. Dissolve 3.3 g KOH in 20 mL deionized water. After complete dissolution, the KOH solution was dropped into FeCl 3 In the solution, a reddish-brown flocculent precipitate was gradually produced in the solution, and the process was accompanied by strong magnetic stirring. After 3 hours, the magnetic stirring was stopped, and the temperature was raised to 80° C., kept for 4 hours, and then lowered to room temperature. The obtained mixed solution was filtered and washed with deionized water and ethanol three times respectively, and after being washed to neutrality, it was dried in air for 6 hours to obtain a khaki-yellow product. TEM results see image 3 , the synthesized α-FeOOH has a regular nano-rod structure with a diameter of 20-30nm and a length of 200-300nm.

Embodiment 3

[0051] Ultrasonic dispersion of the α-FeOOH nanorods (27mg, 0.3mmol) obtained in Example 1 into 10mL deionized water, ultrasonication for 5min, and then under stirring, 80μL of 12mol / L concentrated HCl solution was added dropwise, and after stirring for 5min, the 5 mL of 0.8 mol / L sodium borohydride aqueous solution was added dropwise to the above solution, and reacted for 0.5 h. The black Fe nanorods were obtained, which were separated by a magnet and washed three times with water and ethanol, respectively. The electron microscope results are shown in Figure 4 , the obtained product still maintains rod-like morphology after reduction, and its size remains unchanged (diameter 10-20 nm, length 300-500 nm).

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Abstract

The invention discloses a synthetic method for preparing a Pt nanoparticle@Fe nanorod catalyst by firstly synthesizing a metal iron nanorod through liquid phase reduction and then utilizing a metal replacement reaction. The synthetic method comprises the steps that firstly, by controlling hydrolysis kinetics of iron ions, an alpha-FeOOH nanorod is synthesized; then in an aqueous solution, NaBH4 isused for reduction, a Fe nanorod with the diameter being 10-30 nm and the length being 200-500 nm is obtained; and after magnetic separation and washing, through the metal replacement reaction between Fe<0> and PtCl6<2->, the Pt nanoparticle@Fe nanorod composite catalyst is prepared, and the size of Pt nanoparticles is adjustable within the range being 1.0-3.0 nm. The prepared Pt@Fe nano structure catalyst has excellent nitrobenzene hydrogenation reaction performance and circulation using stability.

Description

technical field [0001] The invention relates to a preparation method of Fe nanorods. [0002] The invention also relates to a preparation method of the Pt nanoparticle@Fe nanorod composite catalyst. [0003] The invention also relates to catalytic applications of the magnetically separable composite materials described above. Background technique [0004] Pt nanoparticle catalysts supported by magnetic materials have the characteristics of separation and recovery under the action of an external magnetic field, so they are widely used in solid-liquid phase catalytic reaction processes (Chem. Rev. 111 (2011) 3036; Catalysts 5 (2015) 534). The magnetic materials currently studied are mainly based on Fe 3 o 4 , γ-Fe 2 o 3 Wait for the main. For example, Baiker et al. used spherical Fe 3 o 4 Nanoparticles as carriers, 5.2wt.%Pt / Fe prepared by impregnation method 3 o 4 Catalyst, the Pt particle size is 4.4nm, the catalyst is used for chiral hydrogenation of ketones, and ...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J37/16B01J37/34B82Y30/00B82Y40/00C07C209/36C07C211/46
CPCB01J23/8906B01J37/16B01J37/343B82Y30/00B82Y40/00C07C209/36B01J35/393C07C211/46
Inventor 李勇刘爽张恩磊申文杰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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