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Method for preparing high-loading iron cyanide complex/silicon dioxide hybrid materials

A technology of ferrocyanide and silicon dioxide, which is applied in the direction of silicon compounds, inorganic chemistry, radioactive purification, etc., can solve the problems of insufficient fixation of potassium ferrocyanide, low particle strength, and difficulty in granulation, and achieve improvement Effects of adsorption kinetic conditions, increasing adsorption rate, and meeting strength requirements

Active Publication Date: 2007-09-26
TSINGHUA UNIV
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Problems solved by technology

[0009] The purpose of the present invention is to overcome the shortcomings of low ferrocyanide loading, difficult granulation, low particle strength, and insufficient fixation of potassium ferrocyanide (sodium) in the prior art, thereby providing a method for preparing high-loading ferrocyanide. A method for ferrocyanide / silica hybrid materials while ensuring high adsorption capacity and selectivity

Method used

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preparation example Construction

[0021] The preparation method of a ferrocyanide / silicon dioxide hybrid material with a high loading capacity provided by the present invention, its specific process steps are as follows:

[0022] 1) Preprecipitation: Dissolve potassium ferrocyanide or sodium ferrocyanide in deionized water, add Mn, Sn, Ti, Fe, Ni, Co, Cr, Zr, Cu, Pb, Soluble salt solution of Zn transition metal, the molar ratio of hexacyanoferrate to metal ion is 1:1~1:6, preferably 1:1.5~1:3; the precipitate is centrifuged and washed several times to obtain ferrous Cyanide nanoparticles;

[0023] 2) Gel fixation: fixation with silica sol in water system or polymeric alkyl siloxane in organic solvent:

[0024] 2.1) Fixed with silica sol in water system

[0025] Add alkaline silica sol aqueous solution to the obtained ferrocyanide nanoparticles under vigorous stirring, the silica content in the alkaline silica sol aqueous solution is 10-35wt%, wherein the silica particles have a particle size of 10-40nm and a d...

Embodiment 1

[0030] Dissolve 9 g of potassium ferrocyanide in 50 mL of deionized water, and slowly add 50 mL of Co(NO 3 ) 2 solution, K 4 [Fe(CN) 6 ]) and the molar ratio of Co ions=1:1.5, then the system was stirred for 30min, aged for 24hr, filtered and washed. The resulting nanoscale K 2 [CoFe(CN) 6 ] Particles are dispersed in 50mL deionized water, adding silica content is 30% (wt) alkaline silica sol 115mL, in the system K 2 [CoFe(CN) 6 ] and the mass ratio of silicon dioxide is 0.2 / 1. Stir well and mix evenly, heat to 80°C in a water bath, then add 35% concentrated hydrochloric acid under vigorous stirring, adjust the pH to 5, let the system stand still, gel after 1min, and dry the gel at 100°C To constant weight, grind and pass through a 60-mesh sieve. The radionuclide ion absorbing material is obtained, and its active component is K 2 [CoFe(CN) 6 ].

Embodiment 2

[0032] Dissolve 15g of sodium ferrocyanide in 80mL of deionized water, and slowly add 80mL of Zn(NO 3 ) 2 solution, Na 4 [Fe(CN) 6 ] and the molar ratio of Zn ions=1:2, then the system was stirred for 60min, aged for 12hr, filtered and washed. Na 2 [CoFe(CN) 6 ] Particles are dispersed in 80mL deionized water, then add the alkaline silica sol 50mL that silicon dioxide content is 25% (wt), in the system Na 2 [ZnFe(CN) 6 ] and the mass ratio of silicon dioxide is 0.9 / 1. After fully stirring and mixing evenly, heat to 40°C in a water bath, then add 65% concentrated nitric acid under vigorous stirring, adjust the pH to 4, let the obtained gel system stand still, and dry the gel at 120°C until constant heavy, ground, and passed through a 60-mesh sieve to obtain a radionuclide ion-absorbing material, whose active component is Na 2 [ZnFe(CN) 6 ].

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Abstract

The invention relates to a preparing method for ferrocyanide with high load / silica hybrid material, belonging to a preparing method for radionuclide ion absorbing material. The method uses the salt solution with metal ion such as Mn, Sn, Ti, Fe, and Ni so on to react with potassium (sodium) ferrocyanide so as to obtain nanometer particle of ferrocyannide. The particle is fixed by silica solution in water system or is fixed by polymerization siloxane in organic solvent and proper inorganic acid, organic amine or amine water is added to obtain hybrid gel. The hybrid gel is dried, rubbed and screened to obtain ferrocyanide with high load / silica hybrid material. The high load of the material is high and the absorption to nuclide ion is strong. In addition, the material intensity can satisfy the demand of packed bed. The particle diameter can be controlled so as to avoid the problem that the water resistance of bed layer generated by ferrocyanide used alone is overlarge.

Description

technical field [0001] The invention relates to a preparation method of a radionuclide ion absorption material, in particular to a preparation method of a ferrocyanide / silicon dioxide hybrid material with a high loading capacity, 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 miniatur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/10G21F9/12
Inventor 刘海弟赵璇李福志
Owner TSINGHUA UNIV
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