A method for quasi-continuous synthesis of single-atom catalysts

A catalyst and quasi-continuous technology, applied in the field of materials science and engineering, can solve the problems of low efficiency and achieve the effects of simple preparation method, increased output, good scalability and reproducibility

Active Publication Date: 2021-06-25
SUN YAT SEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Based on the characteristics and deficiencies of the metal single-atom preparation methods of wet chemical method, deposition method and pyrolysis method, the purpose of the present invention is to provide a method for quasi-continuous synthesis of single-atom catalysts to solve the intermittent production of single-atom catalyst synthesis methods and low efficiency

Method used

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  • A method for quasi-continuous synthesis of single-atom catalysts
  • A method for quasi-continuous synthesis of single-atom catalysts

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Experimental program
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Embodiment 1

[0030] Chitosan was dissolved in 300 mL of deionized water as the continuous phase, and 1.5 g of iron acetylacetonate was dissolved in 30 mL of ethyl acetate as the dispersed phase. Then the dispersed phase was added dropwise to the continuous phase solution and sheared at 13000 rpm for 5 min. The emulsion was injected into a quartz capillary device (550 μm in outer diameter) at a flow rate of 2000 μL / min using a syringe pump, and then dropped into a coagulation bath containing 2 w / v% SDS to form microcapsules. After continuous synthesis for 1 h, the microcapsules were washed with deionized water and then freeze-dried with a freeze dryer. The obtained microcapsules were in N 2 900 under the protection of atmosphere o C pyrolysis for 2 h. then at 80 o C with 0.5 MH 2 SO 4 The iron single-atom catalyst can be obtained after washing for 12 hours and drying.

Embodiment 2

[0032] Chitosan was dissolved in 300 mL of deionized water as the continuous phase, and 1.5 g of iron acetylacetonate was dissolved in 30 mL of ethyl acetate as the dispersed phase. Then the dispersed phase was added dropwise to the continuous phase solution and sheared at 13000 rpm for 5 min. The emulsion was injected into a quartz capillary device (550 μm in outer diameter) at a flow rate of 2000 μL / min using a syringe pump, and then dropped into a coagulation bath containing 2 w / v% SDS to form microcapsules. After continuous synthesis for 2 h, the microcapsules were washed with deionized water and then freeze-dried with a freeze dryer. The obtained microcapsules were in N 2 900 under the protection of atmosphere o C pyrolysis for 2 h. then at 80 o C with 0.5 MH 2 SO 4 The iron single-atom catalyst can be obtained after washing for 12 hours and drying.

Embodiment 3

[0034] Chitosan was dissolved in 300 mL of deionized water as the continuous phase, and 0.9 g of cobalt acetylacetonate was dissolved in 30 mL of ethyl acetate as the dispersed phase. Then the dispersed phase was added dropwise to the continuous phase solution and sheared at 13000 rpm for 5 min. The emulsion was injected into a quartz capillary device (550 μm in outer diameter) at a flow rate of 2000 μL / min using a syringe pump, and then dropped into a coagulation bath containing 2 w / v% SDS to form microcapsules. After continuous synthesis for 1 h, the microcapsules were washed with deionized water and then freeze-dried with a freeze dryer. The obtained microcapsules were in N 2 900 under the protection of atmosphere o C pyrolysis for 2 h. then at 80 o C with 0.5 MH 2 SO 4 The cobalt single-atom catalyst can be obtained after washing for 12 hours and drying.

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Abstract

The invention discloses a method for quasi-continuously synthesizing a single-atom catalyst. The invention encapsulates the metal precursor in the chitosan / sodium lauryl sulfate hydrogel encapsulation through the microcapsule technology, and further pyrolyzes and synthesizes the metal single-atom catalyst. The present invention adopts the pendant drop method in microcapsule technology, which can continuously produce homogeneous microcapsules, thereby realizing the quasi-continuous preparation of single-atom materials. The quasi-continuous synthesis process of the invention solves the problems of poor reproducibility, amplification effect and the like caused by batch synthesis. In addition, the present invention has good expandability, solves the problems of few metal types and low metal content in the prior art, and enriches the research in related fields such as metal single-atom material synthesis methodology.

Description

technical field [0001] The invention relates to the technical field of material science and engineering, in particular to a method for quasi-continuously synthesizing single-atom catalysts. Background technique [0002] Single-atom catalysts have attracted extensive attention in recent years because they have the characteristics of "isolated active sites" of homogeneous catalysts and the characteristics of easy recycling of heterogeneous catalysts. The catalytic sites of single-atom catalysts are highly uniform, and there is no influence of various interference sites such as different crystal planes, vertices, and interfaces in nanoparticles, which is conducive to obtaining high selectivity in catalytic reactions. At present, single-atom catalysts are suitable for various catalytic reactions, including oxygen reduction reaction, selective oxidation reaction, selective hydrogenation reaction, water vapor shift reaction, and hydrogenation reaction, showing great industrial app...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J23/755B01J23/75B01J23/745B22F9/30
CPCB01J23/745B01J23/75B01J23/755B01J27/24B22F9/30
Inventor 纪红兵何晓辉黄丽云何千
Owner SUN YAT SEN UNIV
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