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Preparation method of adsorbent containing SnO2/Sb2O5, product and application of adsorbent

An adsorbent, H2O2 technology, applied in chemical instruments and methods, other chemical processes, nuclear engineering and other directions, can solve the problems of large-scale preparation of unfavorable materials, difficult to obtain, etc., and achieve the effect of good adsorption selectivity and good adsorption performance.

Active Publication Date: 2014-06-18
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

Due to SbCl 5 It is a highly toxic reagent and is highly volatile. There are many problems in the purchase, use and storage of the reagent, and it is not conducive to the large-scale preparation of materials.
Low-valence SbCl 3 The chemical properties are relatively stable and low toxicity, but with SbCl 3 Preparation of Sb as raw material 2 o 5 The process includes Sb 3+ Oxidized to Sb 5+ , then Sb 5+ Hydrolyzed to Sb 2 o 5 process, while the presence of Sb 3+ Rapid self-hydrolysis to form Sb 2 o 3 competing process, so it is difficult to obtain Sb with an oxidation rate close to 100% 2 o 5 ; on the other hand, Sb 5+ and Sn 4+ The difference in hydrolysis rate makes it difficult to form uniform Sn 4+ Substituted Sb 2 o 5

Method used

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  • Preparation method of adsorbent containing SnO2/Sb2O5, product and application of adsorbent
  • Preparation method of adsorbent containing SnO2/Sb2O5, product and application of adsorbent
  • Preparation method of adsorbent containing SnO2/Sb2O5, product and application of adsorbent

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Experimental program
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Effect test

Embodiment 1

[0038] Step 1: 4.56g of anhydrous SbCl 3 and 1.4g of SnCl 4 ·5H 2 O was dissolved in 20mL of anhydrous ethylene glycol, and then added to a 250mL three-necked flask equipped with electromagnetic stirring, oil bath heating, and a water-cooled condensing reflux tube. Heat in an oil bath to make the solution reach the set reaction temperature of 60°C. The molar ratio of Sn / Sb in the reaction system is 0.2.

[0039] Step 2: Keeping the temperature at 60°C, slowly add 20mL of 30wt% H 2 o 2 solution and 8 mL of concentrated hydrochloric acid with a concentration of 37%. A slight bumping phenomenon occurred at the beginning of the dropwise addition, but disappeared as the dropwise addition progressed. During the dropwise addition of the mixed solution, the system generates a colorless transparent colloidal solution.

[0040] Step 3: After the dropwise addition, set the reaction temperature to 80°C, turn on the ultraviolet lamp (254nm) placed outside the flask, and turn off the...

Embodiment 2

[0044] With reference to Example 1 in this embodiment, the SnCl in step 1 4 ·5H 2 The addition amount of O was adjusted to 5.6g, and the molar ratio of Sn / Sb in the reaction system was 0.8. Other operations are the same as in Comparative Example 1, and the material preparation is carried out.

[0045]The experimental results show that the obtained samples are detected by XPS, and the oxidation rates of Sb(III)→Sb(V) are all 100%. The Co ion adsorption performance of the material is measured. When the initial concentration of Co is 10mg / L, the distribution coefficient K of the material to Co is d-Co It is 1354362mg / L.

Embodiment 3

[0047] With reference to Example 1 in this embodiment, the SnCl in step 1 4 ·5H 2 The amount of O added was adjusted to 14.2 g, the molar ratio of Sn / Sb in the reaction system was 2.0, and the other operations were the same as in Comparative Example 1 for material preparation.

[0048] The experimental results show that the obtained samples are detected by XPS, and the oxidation rates of Sb(III)→Sb(V) are all 100%. The Co ion adsorption performance of the material is measured. When the initial concentration of Co is 10mg / L, the distribution coefficient K of the material to Co is d-Co It is 2766503mg / L.

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Abstract

The invention relates to a preparation method of an adsorbent containing SnO2 / Sb2O5. According to the method, SbCl3 with a stable chemical property and low toxicity is taken as a Sb source, sodium thiosulfate pentahydrate, namely SnCl4, is utilized as a Sn source, and a SnO2 / Sb2O5 binary composite oxide is prepared. The preparation method comprises the following steps of oxidizing Sb<3+> as Sb(V) in a non-water system taking alcohol as a solvent by adopting the combination of H2O2 oxidation and ultraviolet irradiation, further carrying out hydrolytic precipitation on Sb(V) and Sb<4+> by utilizing a small amount of water introduced by utilizing H2O2 solution as a reactant, and forming a binary SnO2 / Sb2O5 composite oxide. The method provided by the invention has the advantages that the hydrolyzing speed of Sb<3+> is slow, the generation of the Sb2O3 is effectively controlled, the Sn / Sb2O5 binary composite oxide with the Sb<3+> oxygenation efficiency being 100% is obtained, the adsorbent can remove the radioactive isotope Co ions and a complex thereof and stable isotope Co ions and a complex thereof, and the adsorptive property of the SnO2 / Sb2O5 binary composite oxide and pure Sb2O5 obtained by the introduction of Sb is improved by 200 times.

Description

technical field [0001] The invention relates to the field of inorganic materials, in particular to a 2 / Sb 2 o 5 The preparation method of the adsorbent and its products and applications. Background technique [0002] 58 Co / 60 Co is an important radionuclide in the radioactive waste liquid produced by nuclear power plants under normal operating conditions. 60 Co is one of the key targets of radioactive waste treatment because of its great harm to human body and environment. [0003] 58 Co / 60 Co mainly comes from the corrosion of structural materials, where 58 Co is 58 Ni is formed via the (n,p) reaction, while 60 Co is due to stainless steel and cobalt alloys 59 Co is formed by (n,p) reaction, the radioactivity of the two in the waste liquid is different, and the solubility characteristics are also different. Among the nuclear power plants in operation in Israel 58 Co / 60 The emission of Co and its activity contribution ratio in liquid radioactive effluents a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/02B01J20/30G21F9/12
Inventor 尉继英赵璇李福志张猛
Owner TSINGHUA UNIV
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