Process for producing ferrous iron titanium cyanide with spherule silica gel as carrier

A technology of titanium potassium ferrocyanide and potassium ferrocyanide, which is applied in the field of material preparation and radioactive wastewater treatment, and can solve the problems of difficult ferrocyanide granulation, low specific surface area, and low particle strength

Active Publication Date: 2008-07-16
TSINGHUA UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

[0010] 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 titanium 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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  • Process for producing ferrous iron titanium cyanide with spherule silica gel as carrier

Examples

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preparation example Construction

[0021] The preparation method of titanium potassium ferrocyanide provided by the present invention is the carrier of bead silica gel, and its concrete processing steps are as follows:

[0022] 1) Loading amorphous titanium dioxide in the microsphere silica gel channel

[0023]Dissolve tetrabutyl titanate in an organic solvent, the volume ratio of tetrabutyl titanate to organic solvent is 1:5-20; add small balls of silica gel into the organic solvent, the quality of the small balls of silica gel and the titanic acid in the system The mass ratio of tetrabutyl ester is 1:0.85~4.3; Heating to reflux under the protection of nitrogen, the reaction temperature is controlled at the boiling point of the organic solvent used, after 2~24 hours, filter out the silica gel of the pellets and wash them with n-hexane; Dry at 80-100°C in the atmosphere to constant weight to obtain white or light yellow spherical silica gel loaded with amorphous titanium dioxide; the specific surface of the sph...

Embodiment 1

[0028] 10g of coarse-porous pellet 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 pellets in water, dry them at 90°C for 10 hours, add 8.5g tetrabutyl titanate and 170mL cyclohexane, heat and reflux at 80°C under the protection of nitrogen, and filter the pellets out after 2 hours of reaction. It was dried at 80°C until constant weight, and the loading amount of titanium dioxide was 2% (mass). Then immerse the spherical silica gel loaded with titanium dioxide in 100mL of potassium ferrocyanide hydrochloric acid solution, the concentration of potassium ferrocyanide is 1M, the concentration of hydrochloric acid is 1M, react under stirring for 24hr, and then fully wash with deionized water, A dark blue titanium potassium ferrocyanide / spherical silica gel hybrid material is obtained, and the loading amount of the potassium titanium ferrocyanide is 4% (mass).

Embodiment 2

[0030] 10g of coarse-porous pellet 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 pellets in water, dry them at 90°C for 10 hours, add 43g of tetrabutyl titanate and 215mL of n-hexane, heat and reflux at 78°C under the protection of nitrogen, filter the pellets out after 24 hours of reaction, and put them in the air for 80 It was dried at ℃ to constant weight, and its loading capacity of titanium dioxide was 8% (mass). Then immerse the spherical silica gel loaded with titanium dioxide in 150mL potassium ferrocyanide hydrochloric acid solution, the concentration of potassium ferrocyanide is 0.5M, the concentration of hydrochloric acid is 1M, react under stirring for 24hr, and then fully wash with deionized water , to obtain a black blue titanium potassium ferrocyanide / small ball silica gel hybrid material, the loading of potassium titanium ferrocyanide is 23% (mass).

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Abstract

The invention provides a preparation method of potassium titanium hexacyanoferrate adopting tiny ball-shaped silicagel as carrier, which relates to a preparation method of high specific surface potassium titanium hexacyanoferrate adopting tiny ball-shaped silicagel as carrier. The method is that fashioned porous tiny ball-shaped silicagel under the protection of nitrogen and in the condition of heating and refluxing reacts with organic solvent solution of tetrabutyl titanate. The acquired tiny ball-shaped silicagel loaded with unformed titanium dioxide is dried, dipped in hydrochloric acid solution of kalium ferrocyanatum and then reacting for 12-24h to acquire the high specific surface potassium titanium hexacyanoferrate by adopting tiny the ball-shaped silicagel as carrier. Potassium titanium hexacyanoferrate in the material has adjustable loading amount, good adsorptivity to nuclides, high specific surface, good particle sphericility and solidity, and avoids over-limit moisture resistance of bed layer caused by exclusive use of potassium titanium hexacyanoferrate particles; moreover, owing to existence of Ti-O-Si covalent bond, potassium titanium hexacyanoferrate particles and tiny ball-shaped silicagel can link closely, and do not lose easily during the waste water disposal.

Description

technical field [0001] The invention relates to a preparation method of a radionuclide ion absorbing material, in particular to a preparation method of titanium 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 miniatur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/02B01J20/32G21F9/12
Inventor 刘海弟赵璇李福志
Owner TSINGHUA UNIV
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