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CN-121974468-A - Iron oxyhydroxide desulfurizing agent and preparation method thereof

CN121974468ACN 121974468 ACN121974468 ACN 121974468ACN-121974468-A

Abstract

The invention relates to the technical field of desulfurizing agents, in particular to a ferric hydroxide desulfurizing agent and a preparation method thereof. The iron oxyhydroxide desulfurizer is prepared by doping zinc oxide nano particles on the surface of iron oxyhydroxide, forming a core-shell structure with manganese dioxide as a shell and iron oxyhydroxide as a core with manganese dioxide, and finally loading the core-shell structure on carbon nano fibers. The iron oxyhydroxide desulfurizer of the invention has excellent sulfur removal performance, can still maintain excellent sulfur removal performance under the condition that interfering ions such as PO 4 3‑ 、SO 3 2‑ and the like exist in water, and can be widely applied to the field of industrial sulfur removal.

Inventors

  • HUANG RUIZHI

Assignees

  • 北京泰沧环保科技有限公司

Dates

Publication Date
20260505
Application Date
20260210

Claims (9)

  1. 1. The preparation method of the iron oxyhydroxide desulfurizer is characterized by comprising the following preparation steps: S1, mixing FeCl 3 solution and SDS solution, adding zinc oxide, adjusting the pH value to 10-11, reacting for 7-9h at 100-130 ℃, filtering, washing and drying to obtain iron oxyhydroxide nano particles; S2, adding the iron oxyhydroxide nano particles into deionized water, carrying out ultrasonic treatment for 0.5-1h at 230 ℃, then adding concentrated hydrochloric acid and potassium permanganate, reacting for 5-15 min at 20-30 ℃, finally transferring the iron oxyhydroxide nano particles into a reaction kettle, reacting for 4-8h at 100-120 ℃, cooling, filtering, washing and drying to obtain modified iron oxyhydroxide nano particles; s3, adding modified iron oxyhydroxide nano particles, PAN and PVP into DMF, stirring at 50-70 ℃ for 5-6 h and carrying out ultrasonic treatment for 20-30 min to obtain a mixed solution, and then carrying out electrostatic spinning on the mixed solution to obtain a primary product; s4, the initial product is firstly risen to 250 ℃ at a speed of 1 ℃ per minute in an air atmosphere, kept at 1h ℃, then heated to 600 ℃ at a speed of 5 ℃ per minute in a nitrogen atmosphere, kept at 1h, and cooled to obtain the iron oxyhydroxide desulfurizer.
  2. 2. The method for preparing a desulfurizing agent for iron oxyhydroxide according to claim 1, wherein the weight ratio of FeCl 3 solution, SDS solution and zinc oxide in step S1 is 20:15-25:0.3-0.5.
  3. 3. The method for preparing a desulfurizing agent for iron oxyhydroxide according to claim 1, wherein the particle size of the zinc oxide nanoparticles in step S1 is 20 to 40nm.
  4. 4. The method for producing a desulfurizing agent for iron oxyhydroxide according to claim 1, characterized in that the FeCl3 solution in step S1 has a molar concentration of 1mol/L.
  5. 5. The method for producing a desulfurizing agent for iron oxyhydroxide according to claim 1, characterized in that the molar concentration of the SDS solution in step S1 is 5mmol/L.
  6. 6. The method for preparing a desulfurizing agent for iron oxyhydroxide according to claim 1, wherein the weight ratio of the iron oxyhydroxide nanoparticles, deionized water, concentrated hydrochloric acid, and potassium permanganate in step S2 is 0.3-0.5:30-40:0.75:0.4-0.6.
  7. 7. The method for preparing a desulfurizing agent for iron oxyhydroxide according to claim 1, wherein the weight ratio of modified iron oxyhydroxide nanoparticles, PAN, PVP, and DMF in step S3 is 10-30:8:8:54-74.
  8. 8. The method for preparing a desulfurizing agent for iron oxyhydroxide according to claim 1, wherein specific parameters of the electrostatic spinning in the step S3 are 17G needle, 13/-1 kV applied voltage, 0.06-0.15 mm/min injection speed, and 120-180 mm receiving distance.
  9. 9. An iron oxyhydroxide desulfurizer prepared by the method for preparing an iron oxyhydroxide desulfurizer according to any one of claims 1 to 8.

Description

Iron oxyhydroxide desulfurizing agent and preparation method thereof Technical Field The invention relates to the technical field of desulfurizing agents, in particular to a ferric hydroxide desulfurizing agent and a preparation method thereof. Background With the continuous development of industry, a large number of industries closely related to life, such as oil refining, petrochemical industry, pharmacy, leather making and the like, can also generate a large amount of sulfur-containing wastewater in the production process. The sulfide exists in different states at different pH values, when the wastewater is acidic, most sulfide in the wastewater escapes from the water body in the form of H 2 S to be emitted into the air, when the pH value is between 5 and 7.5, S 2- generates a large amount of HS-to exist in the water body due to hydrolysis, and when the pH value is more than 7.5, the sulfide exists in the water body mainly in the form of S 2-、SO42-、SO32-. The pollutants are directly discharged into the environment after untreated, so that the water body is black, metal materials are corroded, the human health is damaged, and the environment is greatly harmed, so that the deep removal of sulfides is a problem to be solved in the world. The iron oxyhydroxide is an important desulfurizing agent and has wide application prospect in the fields of heavy metal particle adsorption, organic matter degradation treatment, solid phase/liquid phase desulfurization treatment, coal liquefaction and the like. The patent technical document CN202310514348.1 discloses a high-strength ferric oxide hydroxide desulfurizer and a preparation method thereof, wherein the high-strength ferric oxide hydroxide desulfurizer takes Fe-beta molecular sieve as a core layer and ferric oxide hydroxide as a shell layer, the outside of the Fe-beta molecular sieve is wrapped with ferric oxide hydroxide, and the molar ratio of SiO 2 and Al 2O3 in the Fe-beta molecular sieve is 40-50. The high-strength ferric hydroxide desulfurizer obtained by the method has high strength, large penetrating sulfur capacity, large specific surface area and high mechanical strength, is not pulverized after being soaked for a long time by common organic solvents in desulfurization, has high strength against organic solvents, and is suitable for recycling the ferric hydroxide desulfurizer after repeated desulfurization. However, when the sulfur removal agent is used for removing sulfur in water, the water contains more interfering ions such as PO 43-、SO32- and the like, and the interfering ions and S 2- can perform competition, so that the sulfur removal effect is greatly affected. Disclosure of Invention In view of the above, the invention aims to provide a ferric hydroxide desulfurizer and a preparation method thereof, so as to solve the problem that the traditional desulfurizer has poor desulfurization effect in water. Based on the above object, the present invention provides a method for preparing a desulfurizing agent of iron oxyhydroxide, comprising the following steps: S1, mixing FeCl 3 solution and SDS solution, adding zinc oxide, adjusting the pH value to 10-11, reacting for 7-9h at 100-130 ℃, filtering, washing and drying to obtain iron oxyhydroxide nano particles; S2, adding the iron oxyhydroxide nano particles into deionized water, carrying out ultrasonic treatment for 0.5-1h at 230 ℃, then adding concentrated hydrochloric acid and potassium permanganate, reacting for 5-15 min at 20-30 ℃, finally transferring the iron oxyhydroxide nano particles into a reaction kettle, reacting for 4-8h at 100-120 ℃, cooling, filtering, washing and drying to obtain modified iron oxyhydroxide nano particles; s3, adding modified iron oxyhydroxide nano particles, PAN and PVP into DMF, stirring at 50-70 ℃ for 5-6 h and carrying out ultrasonic treatment for 20-30 min to obtain a mixed solution, and then carrying out electrostatic spinning on the mixed solution to obtain a primary product; S4, firstly raising the initial product to 250 ℃ at a rate of 1 ℃ per minute in an air atmosphere, maintaining 1h ℃, then heating to 600 ℃ at a rate of 5 ℃ per minute in a nitrogen atmosphere, maintaining 1h, and cooling to obtain the iron oxyhydroxide desulfurizer; Preferably, the weight ratio of FeCl 3 solution, SDS solution and zinc oxide in the step S1 is 20:15-25:0.3-0.5. Preferably, the particle size of the zinc oxide nanoparticles in step S1 is 20-40nm. Preferably, the FeCl3 solution in step S1 has a molar concentration of 1mol/L. Preferably, the molar concentration of the SDS solution in step S1 is 5mmol/L. Preferably, the pH adjustment in step S1 is carried out with 1mol/L sodium hydroxide solution to a pH of 10-11. Preferably, the drying in step S1 is at 60 ℃ for 24 hours. Preferably, in the step S2, the weight ratio of the iron oxyhydroxide nanoparticles to the deionized water to the concentrated hydrochloric acid to the potassium permanganate is 0.3-0.5:30-40:0.75:0.4-0.6. Prefe