CN115028253A - Magnetic powder for efficiently degrading Cr (VI) wastewater and preparation method thereof - Google Patents

Magnetic powder for efficiently degrading Cr (VI) wastewater and preparation method thereof Download PDF

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Publication number
CN115028253A
CN115028253A CN202210716447.3A CN202210716447A CN115028253A CN 115028253 A CN115028253 A CN 115028253A CN 202210716447 A CN202210716447 A CN 202210716447A CN 115028253 A CN115028253 A CN 115028253A
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powder
heating
wastewater
preserving heat
fecl
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CN115028253B (en
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朱正吼
袁志芬
刘容羽
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Nanchang University
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Nanchang University
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/70Treatment of water, waste water, or sewage by reduction
    • C02F1/705Reduction by metals
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/48Treatment of water, waste water, or sewage with magnetic or electric fields
    • C02F1/488Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • C02F2101/22Chromium or chromium compounds, e.g. chromates
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
  • Water Treatment By Sorption (AREA)
  • Removal Of Specific Substances (AREA)

Abstract

The invention discloses a magnetic powder for treating heavy metal ion Cr (VI) wastewater and a preparation method thereof, wherein the magnetic powder comprises the following steps: polyvinyl alcohol (PVA) powder and Fe of more than or equal to 400 meshes 2 O 3 Fully mixing the powder according to the mass ratio of 1/3, adding water according to a proportion, soaking, heating, preserving heat and preparing into colloid; heating the colloid in an oven, preserving heat, cooling, and crushing into powder 1# with the particle size of 100-250 μm by using a blade type stirrer; taking 100g of powder 1# and 50-100 g of FeCl 2 Mixing with aqueous NiCl solution, FeCl 2 And the concentration of the NiCl aqueous solution is more than or equal to 10g/L, and the Fe/Ni molar ratio in the solution is 2/1. Heating in a baking oven, and drying to obtain powder 2 #; powder 2# in vacuum-N 2 Heating in an atmosphere furnace to 360-400 ℃, preserving heat, and introducing N in the heating process 2 Reacting to generate black powder 3# with the particle size of 100-250 μm; black tonerAnd magnetizing the body 3# in a direct current magnetic field of more than or equal to 0.5T for more than 30 seconds to finally generate magnetic powder. According to the invention, through organically modifying zero-valent iron, the prepared FMF powder not only maintains good water treatment activity, but also has strong oxidation resistance, and can be stored and used for a long time.

Description

Magnetic powder for efficiently degrading Cr (VI) wastewater and preparation method thereof
Technical Field
The invention belongs to the technical field of heavy metal ion wastewater treatment, and particularly relates to magnetic powder for heavy metal ion Cr (VI) wastewater treatment and a preparation method thereof.
Background
Compared with the traditional environment restoration technology, the surface effect, the volume effect, the quantum size and the macroscopic quantum tunneling effect endow the nano material with special performances such as huge specific surface area, super strong adsorption, catalysis and chelation capacity, so that the nano material not only overcomes the defects of the traditional restoration technology, but also shows extremely high restoration efficiency. Therefore, the remediation of polluted water and soil by using nano materials has become a research hotspot in the current environmental field.
The nano zero-valent iron particles have good treatment effect when treating pollutants such as chlorinated organic matters, polychlorobiphenyl, inorganic non-metallic ions, heavy metal ions and the like. The nano zero-valent iron has obvious advantages in the aspect of decontamination, and on one hand, due to the high specific surface area, the nano zero-valent iron can efficiently adsorb pollutants; on the other hand, the catalyst has higher reaction activity, and can chemically react with various pollutants, thereby achieving the effect of removing the pollutants.
With the progress of research, the single use of nano Fe is found 0 The outstanding problem of easy oxidation exists when the water body is repaired, and the nano Fe is generated in the storage and reaction processes 0 The nano Fe can be agglomerated and is unstable in air and water and easy to be oxidized along with the increase of the test time, and the problem seriously restricts the nano Fe 0 And (5) repairing the water body.
Disclosure of Invention
The invention aims to solve the problems and provides magnetic powder for treating heavy metal ions Cr (VI) wastewater and a preparation method thereof.
The invention is realized by the following technical scheme:
the invention provides a preparation method of magnetic powder for treating heavy metal ions Cr (VI), which comprises the following steps:
(1) polyvinyl alcohol (PVA) powder and Fe of more than or equal to 400 meshes 2 O 3 Fully mixing the powder according to the mass ratio of 1/3, adding water according to the proportion of (500 g-800 g)/L, soaking for more than 3h, heating to 95 ℃, and preserving heat for more than 1h to prepare colloid;
(2) heating the colloid in an oven to 200 deg.C, maintaining the temperature for more than 1h, cooling to below 100 deg.C, and pulverizing into powder (powder # 1) with particle size of 100-250 μm (60-250 meshes);
(3) taking 100g of powder 1# and 50-100 g of FeCl 2 Mixing with aqueous NiCl solution, FeCl 2 And the concentration of the NiCl aqueous solution is more than or equal to 10g/L, and the Fe/Ni molar ratio in the solution is 2/1. Heating to 150 deg.C in oven, and oven drying to obtain powder 2 #;
(4) powder 2# in vacuum-N 2 Heating in an atmosphere furnace to 360-400 ℃, preserving heat for more than 2h, and introducing N in the heating process 2 Gas reaction to produce black powder No. 3 with particle size of 100-250 micron;
(5) magnetizing the black powder 3# in a direct current magnetic field of more than or equal to 0.5T for more than 30 seconds to finally generate magnetic powder (FMF).
The invention also provides magnetic powder for treating heavy metal ions Cr (VI) wastewater, which is prepared by the method.
The invention has the beneficial effects that:
(1) through modifying the components of the nano iron, the prepared magnetic powder not only keeps good water treatment activity, but also has strong oxidation resistance and can be stored and used for a long time.
(2) The magnetic performance of the powder designed by the invention is stronger than that of pure iron powder, and the powder is easy to remove by a magnetic field after wastewater treatment.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1: a magnetic powder for efficiently degrading Cr (VI) wastewater and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
(1) preparing main raw materials: ferric chloride (FeCl) 2 ) Nickel chloride (NiCl), polyvinyl alcohol (PVA), Fe 2 O 3 Powder;
(2) polyvinyl alcohol (PVA) powder and Fe of more than or equal to 400 meshes 2 O 3 Fully mixing the powder according to the mass ratio of 1/3, adding water according to the proportion of 800g/L, soaking for more than 5 hours, heating to 95 ℃, and preserving heat for 1 hour to prepare colloid; the colloid was heated to 200 deg.C in an ovenKeeping the temperature for 1h, cooling to 30 deg.C, and pulverizing into powder (powder No. 1) with particle size of 250 μm (60 meshes) with blade type blender; 100g of powder 1# and 100g of FeCl are taken 2 Mixing with aqueous NiCl solution, FeCl 2 And the concentration of the NiCl aqueous solution is 100g/L, and the Fe/Ni molar ratio in the solution is 2/1. Heating to 150 deg.C in oven, and oven drying to obtain powder 2 #; powder 2# in vacuum-N 2 Heating in an atmosphere furnace to 360 ℃, preserving heat for 2 hours, and introducing N in the heating process 2 Reacting with gas to generate black powder 3# with the particle size of 250 mu m; magnetizing the black powder 3# in a 0.8T direct-current magnetic field for 30 seconds to finally generate magnetic powder (FMF); at normal temperature, adding a proper amount of FMF powder into wastewater (the concentration of Cr (VI) in the wastewater is 1.2g/L), stirring for 10S, and immediately clarifying the wastewater. Through chemical analysis, Cr (VI) in the wastewater is adsorbed on the FMF powder and reacts to generate Cr (III); the FMF powder can be repeatedly used for more than 10 times; the FMF powder can be conveniently recycled by using filter cloth or a magnet.
Example 2: a magnetic powder for efficiently degrading Cr (VI) wastewater and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
(1) preparing main raw materials: ferric chloride (FeCl) 2 ) Nickel chloride (NiCl), polyvinyl alcohol (PVA), Fe 2 O 3 Powder;
(2) polyvinyl alcohol (PVA) powder and Fe of more than or equal to 400 meshes 2 O 3 Fully mixing the powder according to the mass ratio of 1/3, adding water according to the proportion of 500g/L, soaking for more than 5h, heating to 95 ℃, and preserving heat for 1h to prepare colloid; heating the colloid in oven to 200 deg.C, maintaining the temperature for 1h, cooling to 30 deg.C, and pulverizing into powder (powder # 1) with particle size of 100 μm (250 meshes) with blade type blender; taking 100g of powder 1# and 100g of FeCl 2 Mixing with aqueous NiCl solution, FeCl 2 And the concentration of the NiCl aqueous solution is 50g/L, and the Fe/Ni molar ratio in the solution is 2/1. Heating to 150 deg.C in oven, and oven drying to obtain powder 2 #; powder 2# in vacuum-N 2 Heating to 400 ℃ in an atmosphere furnace, preserving heat for 2 hours, and introducing N in the heating process 2 Gas reaction to produce black powder No. 3 with particle size of 100 micron; the black powder 3# was magnetized in a 0.5T dc magnetic field for 30 seconds, and finally, magnetic powder (FMF) was produced. At normal temperature, adding a proper amount of FMF into wastewater (the concentration of Cr (VI) in the wastewater is 1.2g/L) containing Cr (VI)Powder, and the wastewater is immediately clarified after stirring for 10 seconds. Through chemical analysis, Cr (VI) in the wastewater is adsorbed on the FMF powder and reacts to generate Cr (III). The FMF powder can be repeatedly used for more than 5 times; the FMF powder can be conveniently recycled by using filter cloth or a magnet.
Example 3: a magnetic powder for efficiently degrading Cr (VI) wastewater and a preparation method thereof are disclosed, wherein the preparation method comprises the following steps:
(1) preparing main raw materials: ferric chloride (FeCl) 2 ) Nickel chloride (NiCl), polyvinyl alcohol (PVA), Fe 2 O 3 Powder;
(2) polyvinyl alcohol (PVA) powder and Fe of more than or equal to 400 meshes 2 O 3 Fully mixing the powder according to the mass ratio of 1/3, adding water according to the proportion of 500g/L, soaking for more than 5h, heating to 95 ℃, and preserving heat for 1h to prepare colloid; heating the colloid in oven to 200 deg.C, maintaining the temperature for 1h, cooling to 30 deg.C, and pulverizing into powder (powder # 1) with particle size of 100 μm (250 meshes) with blade type blender; 100g of powder 1# and 50g of FeCl are taken 2 Mixing with aqueous NiCl solution, FeCl 2 And the concentration of the NiCl aqueous solution is 100g/L, and the Fe/Ni molar ratio in the solution is 2/1. Heating to 150 deg.C in oven, and oven drying to obtain powder 2 #; powder 2# in vacuum-N 2 Heating to 380 ℃ in an atmosphere furnace, preserving heat for 2 hours, and introducing N in the heating process 2 Gas reaction to produce black powder No. 3 with particle size of 100 micron; the black powder 3# was magnetized in a 0.5T dc magnetic field for 30 seconds, and finally magnetic powder (FMF) was produced. At normal temperature, proper amount of FMF powder is added into waste water containing Cr (VI) (the concentration of Cr (VI) in the waste water is 1.2g/L), and the waste water is immediately clarified after being stirred for 10 seconds. Through chemical analysis, Cr (VI) in the wastewater is adsorbed on the FMF powder and reacts to generate Cr (III). The FMF powder can be repeatedly used for more than 5 times; the FMF powder can be conveniently recycled by using filter cloth or a magnet.
The present invention is not limited to the above embodiments, and it will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the concept and principle of the present invention, and these modifications and improvements are also considered to be within the scope of the present invention.

Claims (2)

1. A preparation method of magnetic powder for treating heavy metal ions Cr (VI) wastewater is characterized by comprising the following steps:
(1) polyvinyl alcohol PVA powder and Fe with mesh no less than 400 2 O 3 Fully mixing the powder according to the mass ratio of 1/3, adding water according to the proportion of (500 g-800 g)/L, soaking for more than 3h, heating to 95 ℃, and preserving heat for more than 1h to prepare colloid;
(2) heating the colloid in an oven to 200 deg.C, keeping the temperature for more than 1h, cooling to below 100 deg.C, and pulverizing into powder with particle size of 100-250 μm, i.e. powder # 1;
(3) taking 100g of powder 1# and 50-100 g of FeCl 2 Mixing with aqueous NiCl solution, FeCl 2 And the concentration of the NiCl aqueous solution is more than or equal to 10g/L, and the Fe/Ni molar ratio in the solution is 2/1; heating to 150 deg.C in oven, and oven drying to obtain powder 2 #;
(4) powder 2# in vacuum-N 2 Heating in an atmosphere furnace to 360-400 ℃, preserving heat for more than 2h, and introducing N in the heating process 2 Gas reaction to produce black powder No. 3 with particle size of 100-250 micron;
(5) and magnetizing the black powder 3# in a direct current magnetic field of more than or equal to 0.5T for more than 30 seconds to finally generate the magnetic powder.
2. A magnetic powder for treating wastewater containing heavy metal ions Cr (VI), which is prepared by the preparation method of claim 1.
CN202210716447.3A 2022-06-23 2022-06-23 Magnetic powder for degrading Cr (VI) wastewater and preparation method thereof Active CN115028253B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7622423B1 (en) * 2006-09-12 2009-11-24 The Hong Kong University Of Science & Technology Synthesis of modified maghemite and jacobsite nanoparticles
CN105858853A (en) * 2016-06-20 2016-08-17 南昌大学 Nano powder aqueous suspension for heavy metal ion wastewater treatment and preparation method thereof
WO2018151568A1 (en) * 2017-02-17 2018-08-23 한국가스공사 Catalyst for producing high-calorie synthetic natural gas and use thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7622423B1 (en) * 2006-09-12 2009-11-24 The Hong Kong University Of Science & Technology Synthesis of modified maghemite and jacobsite nanoparticles
CN105858853A (en) * 2016-06-20 2016-08-17 南昌大学 Nano powder aqueous suspension for heavy metal ion wastewater treatment and preparation method thereof
WO2018151568A1 (en) * 2017-02-17 2018-08-23 한국가스공사 Catalyst for producing high-calorie synthetic natural gas and use thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JINGYI CAI 等: "Carbon microfibers with tailored surface functionalities supporting iron/nickel bisalloy for highly efficient hexavalent chromium recovery", 《CARBON》, vol. 168, pages 640 - 649 *

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