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Preparation method and application of Cu/N doped carbon nanosheet catalyst with high stability

A technology of carbon nanosheets and high stability, which is applied in the field of catalyst preparation and application, can solve the problems of poor stability and low catalyst activity, and achieve the effect of solving deactivation factors

Active Publication Date: 2020-11-24
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the problems of low catalyst activity and poor stability, the present invention provides a preparation method and application of a highly stable Cu / N-doped carbon nanosheet catalyst

Method used

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  • Preparation method and application of Cu/N doped carbon nanosheet catalyst with high stability
  • Preparation method and application of Cu/N doped carbon nanosheet catalyst with high stability
  • Preparation method and application of Cu/N doped carbon nanosheet catalyst with high stability

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Embodiment 1

[0032] The chemical substance material used in this embodiment is: magnesium citrate, potassium citrate, ammonium oxalate, copper nitrate, concentrated hydrochloric acid, deionized water, methanol, nitrogen, hydrogen, carbon monoxide, oxygen, and its combined dosage is as follows: in grams, milliliters ,cm 3 is the unit of measurement.

[0033] Magnesium citrate: Mg 3 (C 6 h 5 o 7 ) 2 9H 2 O 4.00g±0.01g

[0034] Potassium citrate: K 3 C 6 h 5 o 7 ·H 2 O 1.00g±0.01g

[0035] Ammonium oxalate: (NH 4 ) 2 C 2 o 4 ·H 2 O 12.00g±0.01g

[0036] Copper nitrate: Cu(NO 3 ) 2 ∙3H 2 O 0.093.00g±0.001g

[0037] Concentrated hydrochloric acid: HCl 40 ml±1 ml

[0038] Deionized water: H 2 O 3000ml±50ml

[0039] Methanol: CH 3 OH 100ml±5ml

[0040] Nitrogen: N 2 10000cm 3 ±100cm 3

[0041] Hydrogen: H 2 10000cm 3 ±100cm 3

[0042] Carbon monoxide: CO 15000 cm 3 ±100cm 3

[0043] Oxygen: O 2 2500cm 3 ±10cm 3

[0044] Selection of the above-mentioned che...

Embodiment 2

[0082] A Cu / NCNS- 4-4 The preparation method and application of catalyst comprise the following steps:

[0083] (1) Weigh 1 g ± 0.001 g potassium citrate, 4 g ± 0.001 g magnesium citrate, 4 g ± 0.001 g ammonium oxalate, place them in a mortar, and grind them thoroughly. The resulting white powder was placed in a corundum boat and transferred to a high temperature tube furnace under N 2 Atmosphere at 2°C·min -1 The heating rate rises to 220, 350, 435 ° C and keeps the temperature for 1 h respectively, then continues to rise to 800 ° C and keeps the temperature for 2 h, after falling to room temperature, a black solid is obtained, and ground to powder, the black powder is placed in 280 Add mL of 2M hydrochloric acid solution, stir at room temperature for 1 h, filter with suction, wash with deionized water until the filtrate is neutral, collect the filter residue, and dry to obtain NCNS- 4-4 . Then implement the same steps (2) (3) (4) as in Example 1.

Embodiment 3

[0085] A Cu / NCNS- 4-8 The preparation method of catalyst comprises the following steps:

[0086] (1) Weigh 1 g ± 0.001 g potassium citrate, 4 g ± 0.001 g magnesium citrate, and 8 g ± 0.001 g ammonium oxalate, place them in a mortar, and grind them thoroughly. The resulting white powder was placed in a corundum boat and transferred to a high temperature tube furnace under N 2 Atmosphere at 2°C·min -1 The heating rate rises to 220, 350, 435 ° C and keeps the temperature for 1 h respectively, then continues to rise to 800 ° C and keeps the temperature for 2 h, after falling to room temperature, a black solid is obtained, and ground to powder, the black powder is placed in 280 Add mL of 2M hydrochloric acid solution, stir at room temperature for 1 h, filter with suction, wash with deionized water until the filtrate is neutral, collect the filter residue, and dry to obtain NCNS- 4-4 . Then implement the same steps (2) (3) (4) as in Example 1.

[0087] Table 2 shows the Cu / NCNS...

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Abstract

The invention discloses a preparation method and application of a Cu / N doped carbon nanosheet catalyst with high stability. The preparation steps include: first, weighing raw materials of magnesium citrate, potassium citrate and ammonium oxalate in a mass ratio of 1:(2-8):(1-16) to prepare an N-doped carbon nanosheet; and then, preparing a N-doped carbon nanosheet copper-carrying salt precursor, and finally, carrying high-temperature roasting to obtain the Cu / N doped carbon nanosheet catalyst with high stability. The obtained catalyst has multilevel pores in which micropores, mesopores and macropores coexist and has a nanosheet structure, and Cu nanoparticles are uniformly dispersed on the carrier; in addition, the multilevel porous nanosheet structure is rich in carbon vacancies, and at lower temperatures (70-300 DEG C), more carbon vacancies can be excited to anchor the Cu nanoparticles, so that the Cu nanoparticles are redispersed into single atoms and atomic clusters of -0.91 nm. The Cu / N doped carbon nanosheet catalyst can also be used in oxidative carbonylation of carbon monoxide to synthesize dimethyl carbonate.

Description

technical field [0001] The invention relates to a preparation method and application of a high-stability Cu / N-doped carbon nanosheet catalyst, belonging to the technical field of catalyst preparation and application. Background technique [0002] As a green basic chemical raw material, dimethyl carbonate (DMC) is widely used. Among the synthesis processes of DMC, the oxidative carbonylation of methanol has become a research hotspot at home and abroad in recent years because of its low production cost, high product selectivity, and environmental friendliness. At present, the catalyst mainly used in this process is carbon-supported copper catalyst. However, the agglomeration of Cu nanoparticles during the reaction seriously affects the stability of this type of catalyst, which hinders its industrialization process. At present, the commonly used treatment methods for the agglomeration of Cu nanoparticles are only to slow down the agglomeration of nanoparticles through spatial ...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/00B01J35/10C07C68/01C07C69/96
CPCB01J27/24C07C68/01B01J35/394B01J35/399B01J35/393B01J35/60C07C69/96
Inventor 任军裴永丽权燕红赵金仙
Owner TAIYUAN UNIV OF TECH
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