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CN-122006653-A - FeS/Fe2O3@LDH material, preparation method and application thereof in removal of antimonate in water

CN122006653ACN 122006653 ACN122006653 ACN 122006653ACN-122006653-A

Abstract

The preparation method comprises the steps of firstly mixing and reacting sodium sulfide solution and ferrous sulfate solution at normal temperature and normal pressure to generate FeS/Fe 2 O 3 precipitate, and then soaking FeS/Fe 2 O 3 precipitate in nitrate solution at normal temperature and normal pressure to modify to obtain the ferrous sulfide/ferric oxide@LDH material. The invention aims to provide a FeS/Fe 2 O 3 @LDH material, a preparation method and application thereof in removing antimonate in water, and the FeS/Fe 2 O 3 @LDH material can be prepared at normal temperature and normal pressure, has controllable morphology, has high-efficiency antimonate removing capability and can be reused.

Inventors

  • He Qiaochong
  • LI QINGQING
  • WAN DONGJIN
  • PAN CHUANQI
  • GUO DONGLI
  • SHEN YUNPENG
  • WU ZHENJUN

Assignees

  • 河南工业大学

Dates

Publication Date
20260512
Application Date
20251121

Claims (10)

  1. 1. A preparation method of FeS/Fe 2 O 3 @LDH material is characterized by firstly mixing sodium sulfide solution and ferrous sulfate solution at normal temperature and normal pressure and reacting to generate FeS/Fe 2 O 3 precipitate, and then soaking FeS/Fe 2 O 3 precipitate in nitrate solution at normal temperature and normal pressure for modification to obtain the ferrous sulfide/ferric oxide@LDH material.
  2. 2. The process for preparing FeS/Fe 2 O 3 @ LDH material as claimed in claim 1, wherein the molar ratio of sodium sulfide to ferrous sulfate is 1 (1-4), the concentration of the ferrous sulfate solution is 0.2-2mol/L, and the concentration of the sodium sulfide solution is 0.2-0.6mol/L.
  3. 3. The process for preparing FeS/Fe 2 O 3 @ LDH material as claimed in claim 1, wherein the sodium sulfide solution and the ferrous sulfate solution are added dropwise to the mixture, and the magnetic stirring is continued at a rate of 150 to 250r/min, and after the completion of the dropwise addition, the stirring is continued for 20 to 40 minutes for complete reaction.
  4. 4. The method for preparing FeS/Fe 2 O 3 @LDH material according to claim 1, wherein the produced FeS/Fe 2 O 3 precipitate is subjected to centrifugal separation and washing to remove impurities and then is soaked in nitrate solution for modification.
  5. 5. A process for preparing FeS/Fe 2 O 3 @LDH material as claimed in claim 1, wherein during the modification, magnetic stirring is carried out at a rate of 150-250r/min for 25-35min.
  6. 6. The method for preparing FeS/Fe 2 O 3 @LDH material according to claim 1, wherein the concentration of the nitrate solution is 1-10mg/L in terms of nitrogen element, and the nitrate solution is one or more of sodium nitrate solution, potassium nitrate solution or ammonium nitrate solution.
  7. 7. A FeS/Fe 2 O 3 @LDH material characterized in that the FeS/Fe 2 O 3 @LDH material is prepared by a preparation method of the FeS/Fe 2 O 3 @LDH material according to any one of claims 1 to 6.
  8. 8. Use of a FeS/Fe 2 O 3 @ LDH material according to claim 7 for removing antimonates from water.
  9. 9. The method for removing antimonate from water of claim 8 wherein FeS/Fe 2 O 3 @LDH material is added in an amount of 0.1-0.5g/L, and the initial pH of the water body is adjusted to 3.0-11.0.
  10. 10. The method of claim 8, wherein the FeS/Fe 2 O 3 @LDH material is recycled by repeatedly adding FeS/Fe 2 O 3 @LDH to the wastewater containing antimonate.

Description

FeS/Fe2O3@LDH material, preparation method and application thereof in removal of antimonate in water Technical Field The invention relates to the technical field of sewage treatment, in particular to a FeS/Fe 2O3 @LDH material, a preparation method and application thereof in removing antimonate in water. Background Antimony is used as a toxic heavy metal element and exists mainly in the form of antimonate in natural water, especially in the form of pentavalent antimony (Sb (V)), such as Sb (OH) 6 -. Long-term intake of water with excessive antimony can cause damage to organs such as human liver, kidney and the like, and threaten the stability of aquatic ecosystems. Therefore, developing a technology for efficiently removing antimonate in water becomes an important research direction in the field of water pollution control. The adsorption method is widely used for removing antimonate because of the advantages of simple operation, low cost, difficult secondary pollution and the like. Ferrous sulfide (FeS) is used as a typical metal sulfide adsorption material, has good reducibility and adsorption capacity, and is widely applied to heavy metal pollution treatment. However, feS materials synthesized by conventional methods generally exhibit a nanosphere or block structure with a smooth surface, have a limited specific surface area, and have insufficient adsorption active sites, resulting in low adsorption capacity and removal efficiency for antimonates. In addition, in complex water environments (such as pH fluctuation and coexisting anion interference), the removal performance stability is poor. More importantly, the traditional FeS material is difficult to realize effective regeneration, and is generally discarded after single use, so that the treatment cost is increased, the problem of solid waste pollution is possibly caused, and the large-scale application of the FeS material in actual water treatment engineering is limited. In view of the above problems, it is highly desirable to optimize the morphology, microstructure and regeneration performance of FeS materials, and to improve the specific surface area, adsorption activity and reusability thereof by a simple process. The conventional modification method is mostly dependent on high-temperature high-pressure reaction conditions (such as a hydrothermal method, a roasting method and the like), lacks of system design aiming at the material regeneration characteristic, has the problems of complex process, high energy consumption, high cost, poor cycle performance and the like, and is difficult to realize industrialized popularization Disclosure of Invention The invention aims to provide a FeS/Fe 2O3 @LDH material, a preparation method and application thereof in removing antimonate in water, and the FeS/Fe 2O3 @LDH material can be prepared at normal temperature and normal pressure, has controllable morphology, has high-efficiency antimonate removing capability and can be reused. In order to solve the technical problems, the preparation method of the FeS/Fe 2O3 @LDH material comprises the steps of firstly mixing and reacting sodium sulfide solution and ferrous sulfate solution at normal temperature and normal pressure to generate FeS/Fe 2O3 precipitate, and then soaking the FeS/Fe 2O3 precipitate in nitrate solution at normal temperature and normal pressure to modify to obtain the ferrous sulfide/ferric oxide@LDH material. Preferably, the molar ratio of sodium sulfide to ferrous sulfate is 1 (1-4), the concentration of ferrous sulfate solution is 0.2-2mol/L, and the concentration of sodium sulfide solution is 0.2-0.6mol/L. Preferably, during the process of mixing the sodium sulfide solution and the ferrous sulfate solution, the sodium sulfide solution is added into the ferrous sulfate solution in a dropwise manner, and is continuously magnetically stirred at a speed of 150-250r/min, and after the dropwise addition is finished, stirring is continued for 20-40 minutes for full reaction. Preferably, the FeS/Fe 2O3 precipitate is centrifugally separated, washed to remove impurities and then soaked in nitrate solution for modification. Preferably, during the modification, the magnetic stirring is carried out at a speed of 150-250r/min for 25-35min. Preferably, the concentration of the nitrate solution is 1-10mg/L in terms of nitrogen element, and the nitrate solution is one or more of sodium nitrate solution, potassium nitrate solution or ammonium nitrate solution. A FeS/Fe 2O3 @LDH material prepared by any one of the preparation methods. The application of the FeS/Fe 2O3 @LDH material in removing antimonate in water. Preferably, the addition amount of FeS/Fe 2O3 @LDH material is 0.1-0.5g/L, and the initial pH of the water body is adjusted to 3.0-11.0. Preferably, feS/Fe2O3@LDH is repeatedly added into the wastewater containing antimonate for recycling. The FeS/Fe 2O3 @LDH is prepared by a two-step method of normal temperature and normal pressure precipitation-nitr