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Method for preparing hollow copper silicate microspheres

A copper silicate, hollow technology, applied in the field of preparation of copper silicate hollow microspheres, can solve the problems of complex process and low adsorption capacity

Active Publication Date: 2018-12-18
QUFU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention aims at the problems of complex synthesis process of copper silicate microspheres or the need for polymer surfactants and low adsorption capacity. The present invention provides a method for preparing copper silicate hollow microspheres without a template and in one step. At the same time, the microspheres After the balls are roasted, hierarchical porous copper oxide / silica composite hollow microspheres with high crystallinity and good shape can be obtained

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  • Method for preparing hollow copper silicate microspheres
  • Method for preparing hollow copper silicate microspheres
  • Method for preparing hollow copper silicate microspheres

Examples

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Embodiment 1

[0042] A preparation method of copper silicate hollow microspheres, comprising the following steps:

[0043] (1) Add 0.75 mmol CuCl 2 and 8 mmol NH 4 The Cl solid was dissolved in 10 mL and 20 mL deionized water respectively, and the obtained NH 4 Cl solution was added dropwise to 10 mL CuCl 2 solution, after stirring evenly, a light green solution A was obtained;

[0044] (2) Add 3 mL NH 3 ·H 2 O, quickly drop into the light green solution A, stir evenly, the solution becomes dark blue solution B;

[0045] (3) Prepare 20 mL of 0.050 mol / L Na 2 SiO 3 Add the aqueous solution dropwise to the dark blue solution B, and stir to obtain a suspension C;

[0046] (4) Put the suspension C in a hydrothermal reaction kettle, raise the temperature to 120 ºC at a heating rate of 8 ºC / min, react at a constant temperature for 12.0 h, and cool to room temperature naturally to obtain a hydrothermal product;

[0047] (5) The hydrothermal product was washed three times with deionized wa...

Embodiment 2

[0054] A preparation method of copper silicate hollow microspheres, comprising the following steps:

[0055] (1) Add 0.75 mmol CuSO 4 and 5 mmol (NH 4 ) 2 SO 4 The solid was dissolved in 10 mL and 20 mL deionized water respectively, and the obtained NH 4 Cl solution was added dropwise to 10 mL CuSO 4 solution, after stirring evenly, a light green solution A was obtained;

[0056] (2) Add 5 mL of ethylenediamine dropwise quickly to the light green solution A, stir evenly, and the solution turns into dark blue solution B;

[0057] (3) Prepare 10 mL of 0.050 mol / L Na 2 SiO 3 Add the aqueous solution dropwise to the dark blue solution B, and stir to obtain a suspension C;

[0058] (4) Put the suspension C in a hydrothermal reaction kettle, raise the temperature to 180 ºC at a heating rate of 5 ºC / min, react at a constant temperature for 6.0 h, and then naturally cool to room temperature to obtain a hydrothermal product;

[0059] (5) The hydrothermal product was washed thr...

Embodiment 3

[0062] A preparation method of copper silicate hollow microspheres, comprising the following steps:

[0063] (1) Add 0.75 mmol Cu(NO 3 ) 2 and 10 mmol NH 4 NO 3 The solid was dissolved in 10 mL and 20 mL deionized water respectively, and the obtained NH 4 Cl solution was added dropwise to 10 mL Cu(NO 3 ) 2 solution, after stirring evenly, a light green solution A was obtained;

[0064] (2) Add 1 mL NaOH dropwise quickly to the light green solution A, and after stirring evenly, the solution turns into dark blue solution B;

[0065] (3) Prepare 20 mL of 0.030 mol / L Na 2 SiO 3 Add the aqueous solution dropwise to the dark blue solution B, and stir to obtain a suspension C;

[0066] (4) Put the suspension C in a hydrothermal reaction kettle, raise the temperature to 90 ºC at a heating rate of 5 ºC / min, react at a constant temperature for 24.0 h, and cool to room temperature naturally to obtain a hydrothermal product;

[0067] (5) The hydrothermal product was washed three...

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Abstract

The invention provides a method for preparing hollow copper silicate microspheres. The method comprises the following steps: a soluble copper salt used as a copper source, soluble silicate used as a silicon source and an ammonium salt used as a mineralizer undergo a one-step hydrothermal reaction under an alkaline condition to obtain copper silicate hydrate CuSiO3.2H2O microspheres (having a diameter of 250-700 nm and an aperture of 1-30 nm), and the CuSiO3.2H2O microspheres are calcined to improve the crystallinity in order to obtain CuO / SiO2 composite microspheres (having a diameter of 300-800 nm and an aperture of 1-10 nm) with a good morphology and a uniform size. The hollow copper silicate microspheres are hopeful to be widely applied in the fields of dye-containing wastewater treatment and supported catalysis. The preparation method has the advantages of simplicity in operation, mild conditions, low energy consumption, low cost, easy control of the process, and suitableness for large-scale industrial production.

Description

technical field [0001] The invention relates to a method for preparing copper silicate hollow microspheres, which belongs to the technical field of preparation of inorganic chemical materials. Background technique [0002] As we all know, with the rapid development of the world economy, environmental pollution is becoming more and more serious. Environmental water pollution, especially water pollution caused by inorganic and organic pollutants discharged from factories, is an environmental problem that is generally concerned worldwide. For this reason, people try to use non-toxic, non-polluting, fast and effective nano-materials as adsorbents or catalysts to solve the problem of water pollution. [0003] In recent years, three-dimensional (3D) hierarchical porous hollow materials have been widely used in energy storage, catalysis, sewage treatment and other fields due to their unique structure, high specific surface area, and good mechanical properties. As an important func...

Claims

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Application Information

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IPC IPC(8): C01B33/20C01B33/18C01G3/02B82Y30/00B82Y40/00B01J13/02C02F1/28C02F101/36C02F101/38
CPCB01J13/02B82Y30/00B82Y40/00C01B33/181C01B33/20C01G3/02C02F1/281C01P2002/72C01P2004/34C01P2004/03C01P2004/04C02F2101/36C02F2101/40C02F2101/38C01P2006/12C01P2006/14C01P2004/62C01P2004/82
Inventor 朱万诚孙盼盼许林姜学珍
Owner QUFU NORMAL UNIV
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