Preparation of potassium zirconium hexacyanoferrate using pellet silica-gel as carrier

A technology of potassium zirconium cyanide and silica gel, applied in chemical instruments and methods, other chemical processes, adsorbed water/sewage treatment, etc., can solve the problems of low particle strength, low specific surface, difficulty in granulating ferrocyanide, etc. , to achieve the effect of improving adsorption rate, efficient adsorption performance, and improving adsorption kinetic conditions

Active Publication Date: 2008-10-08
TSINGHUA UNIV
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Problems solved by technology

[0012] The purpose of the present invention is to overcome the shortcomings of ferrocyanide granulation difficulties, low particle strength and low specific surface area in the prior art, and use the ready-made high specific surface spherical silica gel as a carrier to develop a preparation that does not contain organic matter and has a low specific surface area. The method of zirconium potassium ferrocyanide material with high specific surface area, while ensuring that the material has good sphericity, and also has high adsorption capacity and selectivity

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  • Preparation of potassium zirconium hexacyanoferrate using pellet silica-gel as carrier

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[0025] A kind of preparation method of zirconium ferrocyanide potassium ferrocyanide provided by the invention is carrier with small ball silica gel, its specific preparation steps are as follows:

[0026] 1) Firstly prepare spherical silica gel loaded with amorphous zirconia

[0027] Dissolve zirconium oxychloride in water at a concentration of 0.01-0.1mol / L, add small balls of silica gel into the water of zirconium oxychloride solution, heat to 60-100°C under stirring and condensing and reflux, preferably 75-90°C After reacting for 2 to 24 hours, filter out the silica gel pellets, wash with water until the washing liquid does not contain chloride ions, and dry them in an air atmosphere to constant weight to prepare pellets of silica gel loaded with amorphous zirconia, zirconium dioxide The loading capacity is between 2% and 20%; the mass ratio of the mass of the silica gel to the zirconium oxychloride is 1:0.3 to 1:3; the silica gel is a silica pellet, and the specific surfa...

Embodiment 1

[0032] 10g small ball silica gel, its specific surface is 184.9m 2 / g, the pore volume is 0.565mL / g, and the average pore diameter is 12.23nm. Wash the silica gel in water, dry at 90°C for 10 hours, put it into an aqueous solution of zirconium oxychloride with a concentration of 0.01mol / L, in which 3g of zirconium oxychloride is dissolved, heat to reflux at 90°C, and react for 2 hours Finally, the pellets are filtered out, washed until the washing liquid does not contain chloride ions, dried in an air atmosphere to a constant weight, and the loaded amount of zirconium dioxide is 2% (by mass). Then immerse the spherical silica gel loaded with zirconium dioxide in 100mL of potassium ferrocyanide hydrochloric acid solution, the concentration of potassium ferrocyanide is 1M, the concentration of hydrochloric acid is 1M, react for 24hr under stirring, and then fully After washing, the potassium zirconium ferrocyanide / spherical silica gel hybrid material is obtained, and the loadin...

Embodiment 2

[0034] 10g small ball silica gel, its specific surface is 184.9m 2 / g, the pore volume is 0.565mL / g, and the average pore diameter is 12.23nm. Wash the small silica gel in water, dry it at 90°C for 10 hours, put it into an aqueous solution of zirconium oxychloride with a concentration of 0.05mol / L, in which 10g of zirconium oxychloride is dissolved, heat to reflux at 60°C, and react for 12 hours Finally, the pellets are filtered out, washed until the washing liquid does not contain chloride ions, dried in an air atmosphere to a constant weight, and the loading capacity of zirconia is 9.5% (by mass). Then immerse the spherical silica gel loaded with zirconium dioxide in 150mL of potassium ferrocyanide hydrochloric acid solution, the concentration of potassium ferrocyanide is 0.5M, the concentration of hydrochloric acid is 1.5M, react for 18hr under stirring, and then use deionized After fully washing with water, the potassium zirconium ferrocyanide / spherical silica gel hybrid ...

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Abstract

A preparation method for ferrocyanide zirconium Kalium taking bead silica gel as carrier relates to the preparation method for ferrocyanide zirconium Kalium with high specific surface and taking the bead silica gel as the carrier. In the method, fashioned porous bead silica gel react with the solution of zirconium oxychloride under the condition of heating and refluxing, acquired bead silica gel loaded with amorphous zirconium dioxide is dried and then dipped in the hydrochloric acid solution of yellow potassium ferrocyanide for reaction under stirring for 12-24 hours, thus the hybrid material of ferrocyanide zirconium Kalium with high specific surface and taking bead silica gel as the carrier is obtained. The load of ferrocyanide of the material can be adjusted and the material has strong adsorption capability for nuclide ion, high specific surface, good particle degree of sphericity, and being uneasy to break, which avoids the problem of oversized bed water resistance caused by using ferrocyanide zirconium Kalium particles separately; besides, owing to the existence of Zr-O-Si covalent bond, nano ferrocyanide zirconium Kalium particles can closely combine with the bead silica-gel, thus being uneasy to run away in the process of waste water treatment.

Description

technical field [0001] The invention relates to a preparation method of a radionuclide ion absorbing material, in particular to a preparation method of zirconium potassium ferrocyanide with small spherical silica gel as a carrier, and belongs to the technical field of material preparation and radioactive waste water treatment. Background technique [0002] my country's energy policy has changed from "moderately developing nuclear power" to "actively developing nuclear power". By 2020, the domestic nuclear power installed capacity will increase from the current 8 million kW to about 40 million kW. After 2020, there will be even greater development. Whether the radioactive wastewater produced by the nuclear industry can be properly disposed of is one of the key links related to nuclear safety. It is a very meaningful work in the field of nuclear industry to research and develop efficient and highly selective radioactive wastewater treatment technology to maximize the miniatu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/30C02F1/28
Inventor 刘海弟李福志赵璇
Owner TSINGHUA UNIV
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