Preparation method and application of a functionalized magnetic adsorption material

Abstract

The invention discloses a preparation method of a functionalized magnetic adsorption material, which is characterized in that: ethyl 2,5-dihydroxy-1,4-phenylene diphosphonate and / or 2,5-dihydroxyphenylphosphonic acid Add diethyl ester to solvent A, add nano-ferric oxide, react under certain temperature conditions, and obtain the reacted material; cool the reacted material, filter and separate, wash the solid with solvent B, and dry to obtain the functional magnetic adsorption material. The functionalized magnetic adsorption material prepared by the present invention has a porous structure, is formed by sparsely stacking spherical particles, and has abundant functional groups such as hydroxyl groups and phosphorus oxygen groups; the functionalized magnetic adsorption material prepared by the present invention has the advantages of simple synthesis, low cost, It has the advantages of good selectivity, large adsorption capacity, and easy collection after adsorption. It can be actually used for the adsorption, enrichment or removal of uranium in aqueous solution, and has strong practicability.

Description

technical field

[0001] The invention belongs to the adsorption, enrichment or treatment of radioactive element uranium, and relates to a preparation method and application of a functionalized magnetic adsorption material. The functionalized magnetic adsorption material prepared by the invention (or called the phosphate functionalized nano-iron tetroxide particle adsorption material) is especially suitable for the adsorption, enrichment or removal of radioactive element uranium in aqueous solution. Background technique

[0002] As one of the most important clean energy sources in the 21st century, nuclear energy has the advantages of high energy and higher energy supply stability than hydropower, thermal power, and wind power; less carbon emissions, lower than hydropower and wind power, and longer service life.

[0003] Uranium resources on land in China are actually not abundant, but the storage of uranium element is related to the sustainable development of China's nuclear ...

Examples

Embodiment 1

[0040] A preparation method of functionalized magnetic adsorption material, the steps are:

[0041] a. Add 0.01 mol 2,5-dihydroxy-1,4-benzenediphosphonic acid ethyl ester to 25 mL solvent A toluene (dissolve), add 0.005 mol nano-ferric oxide (powder), at a temperature of 80°C Under the condition of magnetic stirring reaction for 10 hours, obtain the material after reaction;

[0042] b. Cool the reacted material, filter and separate (can be separated by centrifugation or magnetic separation), wash the solid with solvent B (centrifugal wash 10 times with ethyl acetate), and dry to obtain a functionalized magnetic adsorption material (i.e. phosphoric acid Ester-functionalized nano-Fe3O4 particle adsorption material).

[0043] Performance Testing:

[0044](1) Take the functionalized magnetic adsorption material prepared in Example 1 and add it to a pre-configured concentration of 50 mg L -1 and a uranyl ion solution with a pH of 5, placed in a gyratory shaker at 30°C for 10 hou...

Embodiment 2

[0047] A preparation method of functionalized magnetic adsorption material, the steps are:

[0048] a. Add 0.01 mol ethyl 2,5-dihydroxy-1,4-benzenediphosphonate and 0.01 mol diethyl 2,5-dihydroxyphenylphosphonate to 60 mL of solvent A N,N-dimethylmethane Add 0.01 mol nano iron ferric oxide (powder) to the amide (dissolved), and react at a temperature of 30°C for 5 hours to obtain the reacted material;

[0049] b. After the reaction, the material is cooled, filtered and separated (by centrifugation or magnetic separation), and the solid is washed with solvent B ethanol (centrifugal washing 5 times) and dried to obtain a functionalized magnetic adsorption material (that is, a phosphate functionalized nanometer ferric oxide particle adsorption material).

[0050] Performance Testing:

[0051] Get the functionalized magnetic adsorption material prepared in Example 2, add it to a pre-configured concentration of 50 mg L -1 and a uranyl ion solution with a pH of 2-8, placed in a g...

Embodiment 3

[0053] A preparation method of functionalized magnetic adsorption material, the steps are:

[0054] a. Add 0.01mol diethyl 2,5-dihydroxyphenylphosphonate into 30ml solvent A pentane (dissolve), add 0.01mol nanometer ferric oxide (powder), under the condition of 120℃ Reacted for 15 hours to obtain the reacted material;

[0055] b. After the reaction, the material is cooled, filtered and separated (by centrifugation or magnetic separation), and the solid is washed with solvent B (centrifugal washing with ethyl acetate for 5 times, and then with water for 5 times), and then dried to obtain the function Magnetic adsorption material (that is, phosphate functionalized nano ferric oxide particle adsorption material).

[0056] Performance Testing:

[0057] 20 mg L at pH 5 in 1000 mL -1 Add 50 mg of the functionalized magnetic adsorption material (or phosphate-functionalized nanometer ferric oxide particle adsorption material) prepared in Example 3 to the uranyl ion solution, and sa...

technical field

[0001] The invention belongs to the adsorption, enrichment or treatment of radioactive element uranium, and relates to a preparation method and application of a functionalized magnetic adsorption material. The functionalized magnetic adsorption material prepared by the invention (or called the phosphate functionalized nano-iron tetroxide particle adsorption material) is especially suitable for the adsorption, enrichment or removal of radioactive element uranium in aqueous solution. Background technique

[0002] As one of the most important clean energy sources in the 21st century, nuclear energy has the advantages of high energy and higher energy supply stability than hydropower, thermal power, and wind power; less carbon emissions, lower than hydropower and wind power, and longer service life.

[0003] Uranium resources on land in China are actually not abundant, but the storage of uranium element is related to the sustainable development of China's nuclear ...

Examples

Embodiment 1

[0040] A preparation method of functionalized magnetic adsorption material, the steps are:

[0041] a. Add 0.01 mol 2,5-dihydroxy-1,4-benzenediphosphonic acid ethyl ester to 25 mL solvent A toluene (dissolve), add 0.005 mol nano-ferric oxide (powder), at a temperature of 80°C Under the condition of magnetic stirring reaction for 10 hours, obtain the material after reaction;

[0042] b. Cool the reacted material, filter and separate (can be separated by centrifugation or magnetic separation), wash the solid with solvent B (centrifugal wash 10 times with ethyl acetate), and dry to obtain a functionalized magnetic adsorption material (i.e. phosphoric acid Ester-functionalized nano-Fe3O4 particle adsorption material).

[0043] Performance Testing:

[0044](1) Take the functionalized magnetic adsorption material prepared in Example 1 and add it to a pre-configured concentration of 50 mg L -1 and a uranyl ion solution with a pH of 5, placed in a gyratory shaker at 30°C for 10 hou...

Embodiment 2

[0047] A preparation method of functionalized magnetic adsorption material, the steps are:

[0048] a. Add 0.01 mol ethyl 2,5-dihydroxy-1,4-benzenediphosphonate and 0.01 mol diethyl 2,5-dihydroxyphenylphosphonate to 60 mL of solvent A N,N-dimethylmethane Add 0.01 mol nano iron ferric oxide (powder) to the amide (dissolved), and react at a temperature of 30°C for 5 hours to obtain the reacted material;

[0049] b. After the reaction, the material is cooled, filtered and separated (by centrifugation or magnetic separation), and the solid is washed with solvent B ethanol (centrifugal washing 5 times) and dried to obtain a functionalized magnetic adsorption material (that is, a phosphate functionalized nanometer ferric oxide particle adsorption material).

[0050] Performance Testing:

[0051] Get the functionalized magnetic adsorption material prepared in Example 2, add it to a pre-configured concentration of 50 mg L -1 and a uranyl ion solution with a pH of 2-8, placed in a g...

Embodiment 3

[0053] A preparation method of functionalized magnetic adsorption material, the steps are:

[0054] a. Add 0.01mol diethyl 2,5-dihydroxyphenylphosphonate into 30ml solvent A pentane (dissolve), add 0.01mol nanometer ferric oxide (powder), under the condition of 120℃ Reacted for 15 hours to obtain the reacted material;

[0055] b. After the reaction, the material is cooled, filtered and separated (by centrifugation or magnetic separation), and the solid is washed with solvent B (centrifugal washing with ethyl acetate for 5 times, and then with water for 5 times), and then dried to obtain the function Magnetic adsorption material (that is, phosphate functionalized nano ferric oxide particle adsorption material).

[0056] Performance Testing:

[0057] 20 mg L at pH 5 in 1000 mL -1 Add 50 mg of the functionalized magnetic adsorption material (or phosphate-functionalized nanometer ferric oxide particle adsorption material) prepared in Example 3 to the uranyl ion solution, and sa...

Images