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Copper-based composite metal oxide mesocrystal microsphere as well as preparation method and application thereof

A copper-based composite and oxide technology, applied in the direction of metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, silicon compounds, etc., to improve catalytic activity and selectivity, efficient charge transport channels, simple process Effect

Active Publication Date: 2020-01-21
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

No catalyst is currently used in industrial production, SiHCl 3 80-85% selectivity to SiCl 4 Selectivity is 15-20% (CN101665254A, CN101279734B), therefore, further improve SiHCl 3 The selectivity of high-purity crystalline silicon reduces the production cost, which is of great significance to the healthy development of the solar energy industry

Method used

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  • Copper-based composite metal oxide mesocrystal microsphere as well as preparation method and application thereof
  • Copper-based composite metal oxide mesocrystal microsphere as well as preparation method and application thereof
  • Copper-based composite metal oxide mesocrystal microsphere as well as preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] This embodiment provides a CuO-ZnO binary mesogenic material, the mesogenic material is arranged by uniformly oriented nanoparticles and has a spherical hollow core-shell structure with a particle size of about 13 μm, and both the outer shell and the inner core are porous shape, a nanoscale interface is formed between CuO and ZnO.

[0082] The preparation method of the CuO-ZnO binary mesogenic material is as follows:

[0083] 1) 2.5mmol Cu(NO 3 ) 2 ·3H 2 O and 0.25mmol Zn(NO 3 ) 2 ·6H 2 O was dissolved in 70mL DMF, stirred and mixed for 0.1h;

[0084] 2) Add 0.7 g of acetic acid to the above homogeneously mixed solution, and stir for 0.1 h;

[0085] 3) Then put it into an 80mL closed reactor for solvothermal reaction at 140°C for 6h;

[0086] 4) The solid obtained from the reaction in step 3) was washed, dried at 60° C. for 24 hours, and calcined at 400° C. for 3 hours in an air atmosphere to obtain the CuO—ZnO binary mesogenic material.

[0087] figure 1 is t...

Embodiment 2

[0094] This embodiment provides a CuO-Co 3 o 4 Binary mesogenic material, the mesogenic material is a spherical hollow core-shell structure with a particle size of about 13 μm formed by the arrangement of uniformly oriented nanoparticles, the outer shell and the inner core are both porous, CuO and Co 3 o 4 A nanoscale interface is formed between them.

[0095] The CuO-Co 3 o 4 The preparation method of the binary mesogen material is as follows:

[0096] 1) 2.4mmol Cu(NO 3 ) 2 ·3H 2 O and 0.5mmol Co(NO 3 ) 2 ·6H 2 O was dissolved in 70mL DMF, stirred and mixed for 6h;

[0097] 2) Add 0.7 g of sodium acetate to the above homogeneously mixed solution, and stir for 12 hours;

[0098] 3) Then put it into a 100mL airtight reactor for solvothermal reaction at 140°C for 24h;

[0099] 4) The solid obtained from the reaction in step 3) was washed, dried at 120°C for 12h, and calcined at 200°C for 24h in an air atmosphere to obtain the CuO-Co 3 o 4 Binary mesogenic materia...

Embodiment 3

[0101] This embodiment provides a CuO-NiO binary mesogenic material, the mesogenic material is arranged by uniformly oriented nanoparticles and has a spherical hollow core-shell structure with a particle size of about 15 μm, and both the outer shell and the inner core are porous. shape, a nanoscale interface is formed between CuO and NiO.

[0102] The preparation method of the CuO-NiO binary mesogenic material is as follows:

[0103] 1) Add 10mmol Cu(NO 3 ) 2 ·3H 2 O and 10mmol Ni(NO 3 ) 2·6H 2 O was dissolved in 600mL DMF, stirred and mixed for 12h;

[0104] 2) Add 7 g of acetic acid to the above homogeneously mixed solution, and stir for 6 hours;

[0105] 3) Then put it into a 1000mL closed reactor for solvothermal reaction at 130°C for 30h;

[0106] 4) The solid obtained from the reaction in step 3) was washed, dried at 100° C. for 4 hours, and calcined at 900° C. for 2 hours in an air atmosphere to obtain the CuO—NiO binary mesogenic material.

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Abstract

The invention relates to a copper-based composite metal oxide mesocrystal microsphere as well as a preparation method and application thereof. The copper-based composite metal oxide mesocrystal microsphere has a hollow core-shell structure, and sequentially comprises an inner core, a gap and an outer shell from inside to outside. The inner core and the outer shell are both composed of nano particles with consistent orientation, the nano particles comprise copper oxide nano particles and oxide nano particles of metal M, and the metal M comprises any one or a combination of at least two of Ge, Sn, Pb, In or transition metal elements. The copper-based composite metal oxide mesocrystal microsphere is synthesized by adopting a solvothermal method, conditions are mild, a surfactant and a template agent are not used, and the copper-based composite metal oxide mesocrystal microsphere is low in cost and environmentally friendly. When the copper-based composite metal oxide mesocrystal microsphere is used as a catalyst for a synthesis reaction of trichlorosilane serving as a solar crystalline silicon raw material, compared with a traditional non-catalytic industrial production process, the selectivity of trichlorosilane can be remarkably improved and reaches 98.0 percent.

Description

technical field [0001] The invention relates to the technical field of synthesis of micro-nano materials, in particular to a copper-based composite metal oxide mesogenic microsphere and its preparation method and application. Background technique [0002] The hollow core-shell structure is a unique core-shell structure with a layer of space between the core and the shell. This special morphology has obvious structural advantages in catalytic applications: the reaction phase can enter the inner cavity through the pores of the shell, the core can fully contact with the reaction phase, and give full play to the function of the core, while the outer hard shell can The inner core provides full protection. The methods for synthesizing materials with hollow core-shell structure mainly include hard template method and soft template method, but the hard template method requires multi-step and multiple wrapping on the surface of the template to form a multilayer core-shell structure,...

Claims

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Application Information

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IPC IPC(8): B01J23/745B01J23/75B01J23/755B01J23/80B01J23/825B01J23/889B01J35/08B01J35/02C01B33/107
CPCB01J23/002B01J23/80B01J23/75B01J23/755B01J23/8892B01J23/745B01J23/825C01B33/10742B01J2523/00B01J35/396B01J35/51B01J35/40B01J2523/17B01J2523/33B01J2523/842B01J2523/847B01J2523/32B01J2523/27
Inventor 苏发兵纪永军翟世辉谭强强
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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