A kind of preparation method of copper silicate hollow microsphere

A copper silicate and hollow technology is applied in the field of preparation of copper silicate hollow microspheres, which can solve the problems of complex process and low adsorption capacity, and achieve the effects of uniform material size, wide application and uniform size.

Active Publication Date: 2022-02-25
QUFU NORMAL UNIV
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  • 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

Method used

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  • A kind of preparation method of copper silicate hollow microsphere
  • A kind of preparation method of copper silicate hollow microsphere
  • A kind of preparation method of copper silicate hollow microsphere

Examples

Experimental program
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Effect test

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 preparation method of copper silicate hollow microspheres. The method adopts the soluble copper salt as the copper source, the soluble silicate as the silicon source, the ammonium salt as the mineralizer, and under alkaline conditions, through one-step hydrothermal reaction to obtain the hydrated copper silicate CuSiO of uniform size 3 ·2H 2 O microspheres (diameter 250-700 nm, pore size 1-30 nm), and then calcined to increase the crystallinity to obtain CuO / SiO with well-maintained morphology and uniform size 2 Composite microspheres (300-800 nm, pore size 1-10 nm) are expected to be widely used in dye-containing wastewater treatment, supported catalysis and other fields. The preparation method provided by the invention has the advantages of simple operation, mild conditions, low energy consumption, low cost and easy control of the process, and is suitable for large-scale industrial promotion.

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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Patent Type & Authority Patents(China)
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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