CN105858853A - Nano powder aqueous suspension for heavy metal ion wastewater treatment and preparation method thereof - Google Patents

Nano powder aqueous suspension for heavy metal ion wastewater treatment and preparation method thereof Download PDF

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CN105858853A
CN105858853A CN201610436803.0A CN201610436803A CN105858853A CN 105858853 A CN105858853 A CN 105858853A CN 201610436803 A CN201610436803 A CN 201610436803A CN 105858853 A CN105858853 A CN 105858853A
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powder
water
powder body
fexniy
mmt
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CN105858853B (en
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朱正吼
宋晖
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Dayou Scientfic & Technical Co ltd
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Nanchang University
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C02F1/62—Heavy metal compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0545—Dispersions or suspensions of nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention discloses a nano powder aqueous suspension for treating heavy metal ion wastewater and a preparation method thereof, wherein the nano powder aqueous suspension comprises the following steps: mixing NiSO4And FeSO4Mixing the raw materials according to a molar ratio x/y, and carrying out redox reaction on the mixture and hydrazine hydrate under the conditions that the pH value of a solution is 13-15 and the temperature is 80-90 ℃ to generate FeNi magnetic alloy powder; then placing the beaker filled with the magnetic alloy powder aqueous suspension above the magnet, depositing the powder in a region close to the magnet, and pouring out residual water in the beaker; mixing and stirring the MMT, the FexNiy powder and water according to the mass ratio of FexNiy powder/MMT/purified water = 3/3/100. According to the invention, the nano iron component is modified, so that the prepared nano iron alloy powder not only maintains good water treatment activity, but also has strong oxidation resistance, and can be stored and used for a long time; meanwhile, the powder has stronger magnetic property than pure iron powder and is easy to remove by a magnetic field after wastewater treatment.

Description

A kind of effluent containing heavy metal ions processes with nano-powder water slurry and preparation method thereof
Technical field
The invention belongs to effluent containing heavy metal ions process field, be specifically related to a kind of effluent containing heavy metal ions process nano-powder water slurry and preparation method thereof.
Background technology
Compared with traditional environment remediation technology, skin effect, bulk effect, quantum size and macro quanta tunnel effect impart the distinctive performance of nano material, such as huge specific surface area, superpower absorption, catalysis and sequestering power, make nano material not only overcome the shortcoming of conventional repair techniques, but also show high remediation efficiency.Therefore, utilize nano material that polluted-water and soil are repaired and become the study hotspot of current environmental area.
Good treatment effect is shown during the pollutant such as nano zero-valence iron granules is processing chlorinated organics, PCB, inorganic non-metallic ion, heavy metal ion.Nano zero valence iron has significant advantage in terms of scrubbing, on the one hand has benefited from its high specific surface area so that it can adsorb pollutant efficiently；On the other hand it is owing to itself having higher reactivity, with multiple pollutant generation chemical reaction, and then the effect of scrubbing can be reached.
Along with going deep into of research, find that being used alone nanometer Fe 0 repairs water body and there is oxidizable outstanding problem, can lump with nanometer Fe 0 in course of reaction storing, and the lengthening along with test period, instability in air and water, being oxidized easily, this problem seriously constrains the nanometer Fe 0 effect to water remediation.In order to solve these problems, people improve by modifying the surface of nano material, and achieve certain effect.
This invention is by modifying to Nanoscale Iron composition, and the nanosized iron alloy powder body of preparation not only maintains good water and processes vigor, it is often more important that powder body oxidation resistance is strong, can preserve for a long time and use；It addition, the powder magnetic of present invention design can be higher compared with pure iron powder body, it is easy to remove with magnetic field after processing waste water.
Summary of the invention
It is an object of the invention to for problem above, a kind of ultra-fine magnetic powder water slurry and preparation method thereof is provided, being suspended in pure water make the suspension that can store the long period by the dispersion of a kind of ultra-fine magnetic powder, this suspension can be with heavy-metal ion removal after being proportionally added in effluent containing heavy metal ions stirring a period of time.
The present invention is achieved like this, and a kind of effluent containing heavy metal ions processes with nano-powder water slurry and preparation method thereof, it is characterised in that its preparation method is as follows:
(1) primary raw material prepares: ferrous sulfate (FeSO4), six hydration nickel sulfate (NiSO4), hydrazine hydrate (analytical reagent, content >=80.0%), sodium hydroxide (analytical pure, content >=97.0%), bentonite powder body (MMT, particle diameter≤5 μm, purity >=98.0%)；
(2) (wherein mol ratio x/y meets: 5:5≤x/y≤6:4, it is recommended that x/y=6/4): by NiSO to prepare nanometer Fe xNiy powder body4And FeSO4X/y ratio mixes in pure water in molar ratio, makes the aqueous solution that (Ni2++Fe2+) concentration is about 0.01mol/ml ~ 0.05mol/ml, adds hydrazine hydrate (N2H4), and the mol ratio of hydrazine hydrate/(Ni2++Fe2+) is 2:1 ~ 3:1；The pH value adding sodium hydroxide regulation aqueous solution reaches 13 ~ 14；Heating aqueous temperature reaches 80 DEG C ~ 90 DEG C, and aqueous solution starts reduction reaction, about reacts 20 ~ 40min, generates black FeNi magnetic alloy powder body in water, and powder body forms suspension in water；The 500ml beaker that will be equipped with magnetic alloy powder body water slurry again is placed in Br >=0.1T, cylindric, a diameter of 5cm, it is highly above the Magnet of 1 ~ 10cm, powder in beaker is deposited in rapidly the region near Magnet, is now poured out by the residual water in beaker, the most repeatedly adds clear water and washs ultra-fine magnetic powder, it is separated from the water out ultra-fine magnetic powder, FexNiy powder quality of weighing by the method；
(3) make nanometer Fe xNiy powder body water slurry: the powder body of FexNiy in mass ratio/MMT/ pure water=3/3/100, MMT, FexNiy powder body, water are mixed together, after being sufficiently stirred for, make nanometer Fe xNiy powder body water slurry.
The beneficial effects of the present invention is: (1), by modifying Nanoscale Iron composition, the nanosized iron alloy powder body of preparation not only maintains good water and processes vigor, it is often more important that powder body oxidation resistance is strong, can preserve for a long time and use；(2) powder magnetic of present invention design can be higher compared with pure iron powder body, it is easy to removes with magnetic field after processing waste water.
Detailed description of the invention
Embodiment 1: a kind of heavy metal ion use in waste water treatment nano-powder water slurry and preparation method thereof, it is characterised in that its preparation method is as follows:
(1) primary raw material prepares: ferrous sulfate (FeSO4), six hydration nickel sulfate (NiSO4), hydrazine hydrate (analytical reagent, content >=80.0%), sodium hydroxide (analytical pure, content >=97.0%), bentonite powder body (MMT, particle diameter≤5 μm, purity >=98.0%)；
(2) nanometer Fe xNiy powder body is prepared: wherein mol ratio x/y=5:5, by NiSO4And FeSO45/5 ratio mixes in pure water in molar ratio, and making (Ni2++Fe2+) concentration is the aqueous solution of 0.01mol/ml, adds hydrazine hydrate (N2H4), and the mol ratio of hydrazine hydrate/(Ni2++Fe2+) is 2:1；The pH value adding sodium hydroxide regulation aqueous solution reaches 13；Heating aqueous temperature reaches 80 DEG C, and aqueous solution starts reduction reaction, reacts 20min, generates black FeNi magnetic alloy powder body in water, and powder body forms suspension in water；The 500ml beaker that will be equipped with magnetic alloy powder body water slurry again is placed in Br >=0.1T, cylindric, a diameter of 5cm, it is highly above the Magnet of 1 ~ 10cm, powder in beaker is deposited in rapidly the region near Magnet, is now poured out by the residual water in beaker, the most repeatedly adds clear water and washs ultra-fine magnetic powder, it is separated from the water out ultra-fine magnetic powder, FexNiy powder quality of weighing by the method；
(3) make nanometer Fe xNiy powder body water slurry: the powder body of FexNiy in mass ratio/MMT/ pure water=3/3/100, MMT, FexNiy powder body, water are mixed together, after being sufficiently stirred for, make nanometer Fe xNiy powder body water slurry.
Embodiment 2: a kind of heavy metal ion use in waste water treatment nano-powder water slurry and preparation method thereof, it is characterised in that its preparation method is as follows:
(1) primary raw material prepares: ferrous sulfate (FeSO4), six hydration nickel sulfate (NiSO4), hydrazine hydrate (analytical reagent, content >=80.0%), sodium hydroxide (analytical pure, content >=97.0%), bentonite powder body (MMT, particle diameter≤5 μm, purity >=98.0%)；
(2) nanometer Fe xNiy powder body is prepared: wherein mol ratio x/y=6:4, by NiSO4And FeSO46/4 ratio mixes in pure water in molar ratio, and making (Ni2++Fe2+) concentration is the aqueous solution of 0.05mol/ml, adds hydrazine hydrate (N2H4), and the mol ratio of hydrazine hydrate/(Ni2++Fe2+) is 3:1；The pH value adding sodium hydroxide regulation aqueous solution reaches 14；Heating aqueous temperature reaches 90 DEG C, and aqueous solution starts reduction reaction, reacts 40min, generates black FeNi magnetic alloy powder body in water, and powder body forms suspension in water；The 500ml beaker that will be equipped with magnetic alloy powder body water slurry again is placed in Br >=0.1T, cylindric, a diameter of 5cm, it is highly above the Magnet of 1 ~ 10cm, powder in beaker is deposited in rapidly the region near Magnet, is now poured out by the residual water in beaker, the most repeatedly adds clear water and washs ultra-fine magnetic powder, it is separated from the water out ultra-fine magnetic powder, FexNiy powder quality of weighing by the method；
(3) make nanometer Fe xNiy powder body water slurry: the powder body of FexNiy in mass ratio/MMT/ pure water=3/3/100, MMT, FexNiy powder body, water are mixed together, after being sufficiently stirred for, make nanometer Fe xNiy powder body water slurry.
Embodiment 3: a kind of heavy metal ion use in waste water treatment nano-powder water slurry and preparation method thereof, it is characterised in that its preparation method is as follows:
(1) primary raw material prepares: ferrous sulfate (FeSO4), six hydration nickel sulfate (NiSO4), hydrazine hydrate (analytical reagent, content >=80.0%), sodium hydroxide (analytical pure, content >=97.0%), bentonite powder body (MMT, particle diameter≤5 μm, purity >=98.0%)；
(2) nanometer Fe xNiy powder body is prepared: wherein mol ratio x/y=6:4, by NiSO4And FeSO46/4 ratio mixes in pure water in molar ratio, and making (Ni2++Fe2+) concentration is the aqueous solution of 0.03mol/ml, adds hydrazine hydrate (N2H4), and the mol ratio of hydrazine hydrate/(Ni2++Fe2+) is 2.5:1；The pH value adding sodium hydroxide regulation aqueous solution reaches 13.5；Heating aqueous temperature reaches 85 DEG C, and aqueous solution starts reduction reaction, reacts 30min, generates black FeNi magnetic alloy powder body in water, and powder body forms suspension in water；The 500ml beaker that will be equipped with magnetic alloy powder body water slurry again is placed in Br >=0.1T, cylindric, a diameter of 5cm, it is highly above the Magnet of 1 ~ 10cm, powder in beaker is deposited in rapidly the region near Magnet, is now poured out by the residual water in beaker, the most repeatedly adds clear water and washs ultra-fine magnetic powder, it is separated from the water out ultra-fine magnetic powder, FexNiy powder quality of weighing by the method；
(3) make nanometer Fe xNiy powder body water slurry: the powder body of FexNiy in mass ratio/MMT/ pure water=3/3/100, MMT, FexNiy powder body, water are mixed together, after being sufficiently stirred for, make nanometer Fe xNiy powder body water slurry.
The invention is not restricted to above example, to those of ordinary skill in the art, on the premise of without departing from present inventive concept and principle, it is also possible to make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.

Claims (1)

1. an effluent containing heavy metal ions processes with nano-powder water slurry and preparation method thereof, it is characterised in that its preparation method is as follows:
(1) primary raw material prepares: ferrous sulfate (FeSO4), six hydration nickel sulfate (NiSO4), hydrazine hydrate (analytical reagent, content >=80.0%), sodium hydroxide (analytical pure, content >=97.0%), bentonite powder body (MMT, particle diameter≤5 μm, purity >=98.0%)；
(2) nanometer Fe xNiy powder body is prepared: wherein mol ratio x/y meets: 5:5≤x/y≤6:4, by NiSO4And FeSO4X/y ratio mixes in pure water in molar ratio, and making (Ni2++Fe2+) concentration is the aqueous solution of 0.01mol/ml ~ 0.05mol/ml, adds hydrazine hydrate (N2H4), and the mol ratio of hydrazine hydrate/(Ni2++Fe2+) is 2:1 ~ 3:1；The pH value adding sodium hydroxide regulation aqueous solution reaches 13 ~ 14；Heating aqueous temperature reaches 80 DEG C ~ 90 DEG C, and aqueous solution starts reduction reaction, reacts 20 ~ 40min, generates black FeNi magnetic alloy powder body in water, and powder body forms suspension in water；The 500ml beaker that will be equipped with magnetic alloy powder body water slurry again is placed in Br >=0.1T, cylindric, a diameter of 5cm, it is highly above the Magnet of 1 ~ 10cm, powder in beaker is deposited in rapidly the region near Magnet, is now poured out by the residual water in beaker, the most repeatedly adds clear water and washs ultra-fine magnetic powder, it is separated from the water out ultra-fine magnetic powder, FexNiy powder quality of weighing by the method；
(3) make nanometer Fe xNiy powder body water slurry: the powder body of FexNiy in mass ratio/MMT/ pure water=3/3/100, MMT, FexNiy powder body, water are mixed together, after being sufficiently stirred for, make nanometer Fe xNiy powder body water slurry.
CN201610436803.0A 2016-06-20 2016-06-20 Nano powder aqueous suspension for heavy metal ion wastewater treatment and preparation method thereof Active CN105858853B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110240134A (en) * 2019-06-06 2019-09-17 宜宾海丰和锐有限公司 Remove Fe in ketazine process hydrazine hydrate3+With the method for organic matter
CN114734050A (en) * 2022-04-01 2022-07-12 浙江旭德新材料有限公司 Preparation machine and preparation method of superfine pure copper powder for thermal spraying technology
CN115028253A (en) * 2022-06-23 2022-09-09 南昌大学 Magnetic powder for efficiently degrading Cr (VI) wastewater and preparation method thereof

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CN103586481A (en) * 2013-10-19 2014-02-19 南昌大学 Preparation method for Fe100-xNix nanometer powder
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110240134A (en) * 2019-06-06 2019-09-17 宜宾海丰和锐有限公司 Remove Fe in ketazine process hydrazine hydrate3+With the method for organic matter
CN114734050A (en) * 2022-04-01 2022-07-12 浙江旭德新材料有限公司 Preparation machine and preparation method of superfine pure copper powder for thermal spraying technology
CN115028253A (en) * 2022-06-23 2022-09-09 南昌大学 Magnetic powder for efficiently degrading Cr (VI) wastewater and preparation method thereof
CN115028253B (en) * 2022-06-23 2023-10-31 南昌大学 Magnetic powder for degrading Cr (VI) wastewater and preparation method thereof

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