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Preparation method, products and application of Sb2O5 adsorbent containing doped metal ions

A metal ion and ion doping technology, applied in chemical instruments and methods, other chemical processes, inorganic chemistry, etc., can solve the problems of large-scale preparation and difficulty in obtaining unfavorable materials

Active Publication Date: 2014-06-18
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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, the competing process that exists is Sb 3+ Rapid self-hydrolysis to form Sb 2 o 3 , so it is difficult to obtain Sb with an oxidation rate close to 100% 2 o 5 ; on the other hand, Sb 5+ and Si 4+ The difference in hydrolysis rate makes it difficult to form a uniform Si(IV)-substituted Sb 2 o 5 Pyrochlore

Method used

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  • Preparation method, products and application of Sb2O5 adsorbent containing doped metal ions
  • Preparation method, products and application of Sb2O5 adsorbent containing doped metal ions
  • Preparation method, products and application of Sb2O5 adsorbent containing doped metal ions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Step 1: 4.56g of anhydrous SbCl 3Dissolve 4.46mL of TEOS in 20mL of anhydrous ethylene glycol, configure a solution containing Si(IV) / Sb(III) in a 250mL three-necked flask, and the flask is equipped with electromagnetic stirring, oil bath heating and water cooling to condense and reflux Tube. Heat in an oil bath to make the solution reach the set reaction temperature of 60°C.

[0048] Step 2: Keep the above set temperature at 60°C, slowly add 30% H at a rate of 5-10 drops / min 2 o 2 Solution 20mL. A slight bumping phenomenon occurred at the beginning of the dropwise addition, but disappeared as the dropwise addition progressed. During the dropwise addition of hydrogen peroxide, a colorless transparent colloidal solution was first generated, and then a white precipitate appeared in the reaction solution.

[0049] 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 u...

Embodiment 2

[0059] With reference to Example 1 in this embodiment, H in step 2 2 o 2 The addition amount of the solution is adjusted to 6mL, and other operations are the same as in Comparative Example 1, and the material preparation is carried out to obtain a solution containing Si / Sb 2 o 5 the adsorbent.

[0060] Add 30% H dropwise 2 o 2 The oxidation rate of Sb(III)→Sb(V) in 6mL of the solution was only 64%, which indicated that a higher dosage of hydrogen peroxide was beneficial to obtain a higher oxidation rate. The Sr ion adsorption performance of material is measured, under the state that the initial concentration of Sr ion is 10mg / L, the material of the present embodiment is to the distribution coefficient K of Sr ion d-sr It was 39754186mg / L, compared with Comparative Example 1, the adsorption performance decreased.

Embodiment 3

[0062] Step 1: 4.56g of anhydrous SbCl 3 and 4.46mL of TEOS were dissolved in 20mL of anhydrous ethylene glycol, and then the solution was added to a 250mL three-necked flask equipped with electromagnetic stirring, oil bath heating, and a water-cooled condensing reflux tube. Heat the oil bath to make the solution reach the set reaction temperature of 60°C

[0063] Step 2: Keep the above set temperature at 60°C, and slowly add 30% H2 to the three-necked flask at a rate of 5-10 drops / min. 2 o 2 Solution 20mL. A slight bumping phenomenon occurred at the beginning of the dropwise addition, but disappeared as the dropwise addition progressed. During the dropwise addition of hydrogen peroxide, a colorless transparent colloidal solution was first generated, and then a white precipitate appeared in the reaction solution.

[0064] 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 th...

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Abstract

The invention relates to a preparation method of a Sb2O5 adsorbent containing doped metal ions. The method comprises the steps of combining H2O2 oxidation and ultraviolet irradiation in a non-aqueous system which takes alcohol as a solvent to promote Sb (III) to be oxidized into Sb (V); further utilizing a small amount of water introduced by an H2O2 solution as a reactant to realize hydrolysis for the Sb (V) and metal ion Mn<+> (Si<4+> or Ti<4+>) and form metal ion partial substitution type Sb2O5; preparing a metal ion Si-doped Si / Sb2O5 adsorbent with a cubic pyrochlore structure and forming metal ion Ti-doped Ti / Sb2O5 adsorbent with a continuous solid solution structure within different Ti / Sb proportional ranges. The prepared adsorbent material can be used for effectively removing radioactive isotope Sr ions and complexes of the radioactive isotope Sr ions as well as stable isotope Sr ions and complexes of the stable isotope Sr ions.

Description

technical field [0001] The invention relates to the field of inorganic materials, in particular to a Sb doped with metal ions 2 o 5 Preparation methods of adsorbents and their products and applications. Background technique [0002] The Fukushima nuclear accident caused a large amount of radioactive waste to be discharged into the sea and caused pollution. This is a warning to the development of nuclear energy around the world: timely and effective disposal of radioactive waste is one of the important contents of establishing an emergency mechanism for nuclear power plant accidents. The main radioactive substances in radioactive waste liquid include long-lived fission products with β radioactivity 134 Cs / 137 Cs and 90 Sr, gamma radioactive 60 Co and α-radioactive 235+238 U 239+240 Pu, 241 Am, 242+244 Cm et al. in, 90 Sr is 235 One of the fission products of U, with a yield of 5.90%, a half-life of 28 years, and β radioactivity. After being absorbed by the human ...

Claims

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Application Information

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IPC IPC(8): B01J20/06B01J20/30C01G30/00G21F9/12
Inventor 赵璇尉继英李福志
Owner TSINGHUA UNIV
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