CN107308922A - A kind of water process is with Ni-based from growth three-dimensional material and preparation method thereof - Google Patents
A kind of water process is with Ni-based from growth three-dimensional material and preparation method thereof Download PDFInfo
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- CN107308922A CN107308922A CN201710748404.2A CN201710748404A CN107308922A CN 107308922 A CN107308922 A CN 107308922A CN 201710748404 A CN201710748404 A CN 201710748404A CN 107308922 A CN107308922 A CN 107308922A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention discloses a kind of water process with Ni-based from growth three-dimensional material and preparation method thereof.This method comprises the following steps：(1) metal substrate is cleaned with surface conditioning agent, obtains metal substrate I；(2) by nickel salt and divalent iron salt dissolving in a solvent, precipitating reagent and protective agent are added, is stirred, mixed solution is obtained；(3) mixed solution obtained in step (2) is poured into the metal substrate I obtained in step (1), reacted under the conditions of 110 DEG C~130 DEG C, then take precipitation, washed, dry, obtain the persursor material of nickel ferrite based magnetic loaded/foam nickel composite；(4) persursor material of the nickel ferrite based magnetic loaded obtained in step (3)/foam nickel composite is calcined, obtains water process with Ni-based from growth three-dimensional material.The inventive method is simple and easy to apply, with low cost and environmental protection, and what is be made is Ni-based big from growth three-dimensional material specific surface area, can effectively remove organic dyestuff and heavy metal ion in sewage.
Description
Technical field
The invention belongs to technical field of sewage, more particularly to a kind of water process with it is Ni-based from growth three-dimensional material and its
Preparation method.
Background technology
In recent years, with the quickening of process of industrialization, problem of environmental pollution turns into the tight of human being's production and life and health
Threaten again.Wherein, water pollution problems is increasingly paid close attention to by people, has become the key of pollution problem.A poisonous huge sum of money
Category ion and organic dyestuff are generally all less likely to occur light degradation and biodegradation, and they easily accumulate and cause tight in the tissue
The actual bodily harm of weight.Therefore, heavy-metal ion removal and organic dyestuff have turned into the important hand that processing environment pollutes from waste water
Section.
So far, developed it is many elimination water pollutants methods, such as adsorb, flocculate, ozonisation, membrane filtration and
Biological treatment.Wherein absorption is considered as a kind of method for extremely having an application prospect, by its convenient operation, low cost and efficiently
Rate comes heavy-metal ion removal and organic dyestuff.However, traditional adsorbent is present, processing speed is slow, adsorption capacity is limited and holds
Easily cause some problems such as secondary pollution.In order to further improve the absorption property of adsorbent, new, cheap, Gao Bibiao is developed
Area, the sorbing material of high adsorption capacity have turned into the focus that sewage disposal is studied.
Application of the people to magnetic material in wastewater treatment in recent years is increasingly taken seriously.Compared with traditional material, magnetic
Property material as sewage-treating agent have speed fast, precision is high, magnetic separation separation, easy to operate, reusable etc. excellent after stripping paint
Point, is separated composite with waste water using magnetic, is improved waste water treatment efficiency, is reduced cost, makes it as high suction of new generation
There are tremendous expansion potentiality in terms of the sewage treating material of attached property.
Among magnetic material, ferrite NiFe2O4Due to its significant saturation magnetization, and aboundresources,
Cost is relatively low, environmentally friendly, is used as magnetic carrier the advantages of physics and chemical stability and low intrinsic toxicity.
NiFe2O4It is considered as a kind of sewage disposal sorbing material of great application prospect.
But NiFe2O4As sewage disposal sorbing material there is also some shortcoming and deficiency, material synthesis processes are multiple
It is miscellaneous, cause production cost high, adsorption efficiency is low, and adsorption effect is undesirable.Therefore, further investigation exploitation novel adsorption agent material,
With low cost, high efficiency removes a large amount of organic dyestuff and heavy metal ion pollutant is most important.
The content of the invention
The primary and foremost purpose of the present invention is to overcome the shortcoming and deficiency of prior art there is provided a kind of water process with Ni-based spontaneous
The preparation method of long three-dimensional material.
Another object of the present invention is to provide water process that methods described prepares with Ni-based from growth three-dimensional material.
The purpose of the present invention is achieved through the following technical solutions：A kind of water process is with Ni-based from the preparation for growing three-dimensional material
Method, comprises the following steps：
(1) metal substrate is cleaned with surface conditioning agent, obtains metal substrate I；
(2) by nickel salt and divalent iron salt dissolving in a solvent, precipitating reagent and protective agent are added, is stirred, is mixed
Close solution；
(3) mixed solution obtained in step (2) is poured into the metal substrate I obtained in step (1), at 110 DEG C
Reacted under the conditions of~130 DEG C, then take precipitation, washed, dried, obtain the presoma material of nickel ferrite based magnetic loaded/foam nickel composite
Material；
(4) persursor material of the nickel ferrite based magnetic loaded obtained in step (3)/foam nickel composite is calcined, obtained at water
Reason is with Ni-based from growth three-dimensional material.
Metal substrate described in step (1) is preferably nickel foam, more preferably 110PPI nickel foams.
The size of described nickel foam is preferably 4 × 6cm, is conducive to nickel ferrite based magnetic loaded to be uniformly deposited in nickel foam,
And the growth of the more suitable nickel ferrite based magnetic loaded in nickel foam space of this specification.
Surface conditioning agent described in step (1) is at least one of acetone, absolute ethyl alcohol and deionized water.
Cleaning described in step (1) is ultrasonic cleaning；Preferably successively with acetone, absolute ethyl alcohol and deionized water ultrasound
Cleaning.
The described ultrasonic time is preferably 30~60min, and ultrasonic power is preferably 180~240w.
Nickel salt described in step (2) is soluble nickel salt, preferably in nickel chloride, nickel nitrate and nickel sulfate at least
It is a kind of；More preferably six water nickel nitrate (Ni (NO3)2·6H2O)。
The concentration of nickel ion is 0.01~0.1mol/L in mixed solution described in step (2)；Preferably 0.04~
0.08mol/L。
Divalent iron salt described in step (2) is soluble divalent iron salt, preferably frerrous chloride, ferrous nitrate and sulphur
At least one of sour ferrous iron.
The concentration of ferrous ion is 0.02~0.2mol/L in mixed solution described in step (2)；Preferably 0.08
~0.16mol/L.
The mol ratio of nickel salt and divalent iron salt described in step (2) is preferably 1：2.
The mol ratio of nickel ion and ferrous ion is preferably 1 in mixed solution described in step (2)：2.
Solvent described in step (2) is water, preferably deionized water.
Precipitating reagent described in step (2) is preferably ammonium fluoride or ammonium chloride.
Protective agent described in step (2) is preferably urea.
The concentration of precipitating reagent is 0.001~0.005mol/L in mixed solution described in step (2)；Protectant concentration
For 0.001~0.01mol/L.
The time of stirring described in step (2) is 0.5~2 hour.
The mass ratio of mixed solution and the metal substrate I described in step (3) is preferably 45~150:1.
The time of reaction described in step (3) is preferably 10~20 hours.
Dirty-green tablet is precipitated as described in step (3).
Washing described in step (3) is to be washed successively with absolute ethyl alcohol and deionized water.
The condition of drying described in step (3) is：50~80 DEG C of dryings 6~12 hours；Preferably at 50~80 DEG C
Dried 6~12 hours in air dry oven.
The condition of calcining described in step (4) is：Under air or oxygen atmosphere, 300~600 DEG C of 2~6h of calcining；It is excellent
Elect as under air or oxygen atmosphere, 400~450 DEG C calcining 2~4h；More preferably under air or oxygen atmosphere, with 2 DEG C/
Min speed is warming up to 400~450 DEG C, then calcines 2~4h.
A kind of water process, from growth three-dimensional material, is prepared with Ni-based by the method described in any of the above-described.
The described Ni-based application from growth three-dimensional material in sewage treatment area.
Described sewage is preferably the sewage containing organic dyestuff or heavy metal ion.
Described organic dyestuff is preferably Congo red.
Described heavy metal ion is preferably chromium ion；More preferably hexavalent chromium.
The principle of the present invention：Common hydro-thermal method is often with trivalent iron salt as reactant, and obtained ferrous acid nickel material is often
Three-dimensional shape structure can not be formed, and after waste water has been handled, the separation with waste water is not thorough enough, so as to cause the secondary of water body
Pollution and, adsorbance relatively low shortcoming poor to organic dyestuff and heavy metal ion adsorbed efficiency.And present invention employs two
Valency molysite and nickel foam prepare three-dimensional flower-shaped ferrous acid nickel material, and ammonium fluoride is received as precipitating reagent, generation nickel ferrite based magnetic loaded presoma
Rice grain simultaneously independently dresses up nanometer sheet in nickel foam, and very thin nanoscale twins are further combined into three-dimensional flower-shaped structure.It is this
Structure largely increases itself and organic dyestuff and the contact area of heavy metal ion, and has nickel foam as substrate, makes
It directly can be separated from waste water, largely simplified waste water processes and reduced processing cost.
The surface of nickel ferrite based magnetic loaded carries positive charge, mainly occurs Anion-adsorption.Congo red surface You Liangge functional groups, respectively
It is sulfonic group and amido, can be completely dissolved or protonate in water and become negatively charged and positive charge group.And amido
It is hydrophilic and luminous group, it is Congo red to be dissolved in water and show red due to the presence of amido.In electrostatic adsorption
Under, negatively charged nickel ferrite based magnetic loaded adsorbs positively charged amido, therefore Congo red absorption is in ferrite surfaces so that containing Congo red
Red solution become clarification.Heavy metal ion Cr (VI) solution configured for potassium bichromate, mainly with HCrO4 -Form is present,
Occur surface ligand with nickel ferrite based magnetic loaded to exchange and surface electrostatic absorption.
The present invention has the following advantages and beneficial effect relative to prior art：
(1) present invention prepares the flower-shaped nickel ferrite based magnetic loaded of nano-sheet self assembly, its is equal using nickel foam as template
Even is distributed on the skeleton of nickel foam.The unique three-dimensional flower-shaped structure of products therefrom shows larger specific surface area, can fill
That divides contacts with organic dyestuff and heavy metal ion.
(2) present invention successfully solves that traditional sorbent treatment speed is slow, adsorption capacity limited and easily causes secondary
The problem of pollution.Adsorption rate to organic dyestuff can reach 81.5% within ten minutes, and absorption reaches adsorbance during balance
For 105.7mg g-1, the adsorption rate of heavy metal ion can reach 89% in ten minutes, and absorption reaches adsorbance during balance
For 49.6mg g-1.It is expected that above-mentioned new NiFe2O4Anode material has the good organic dyestuff and a huge sum of money that remove in water
Belong to the absorption property of ion.
(3) present invention successfully solves the problem of adsorbent is separated with waste water difficulty in the prior art, because of nickel ferrite based magnetic loaded/nickel foam
Good magnetic and nickel foam contribute to separate with waste water as substrate.
(4) preparation method of the invention is simple, with low cost, environmental protection, can make adsorbent in terms of sewage disposal
Application it is wider.
Brief description of the drawings
Fig. 1 is the XRD spectra of nickel ferrite based magnetic loaded/foam nickel composite of the gained of embodiment 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of Flied emission nickel ferrite based magnetic loaded/foam nickel composite of the gained of embodiment 1.
Fig. 3 is absorption property figure of the gained nickel ferrite based magnetic loaded of the embodiment 1/foam nickel composite to organic dyestuff.
Fig. 4 is the absorption property figure of the gained nickel ferrite based magnetic loaded of embodiment 1/foam nickel composite heavy metal ion.
Fig. 5 is absorption property figure of the gained nickel ferrite based magnetic loaded of the embodiment 2/foam nickel composite to organic dyestuff.
Fig. 6 is the absorption property figure of the gained nickel ferrite based magnetic loaded of embodiment 2/foam nickel composite heavy metal ion.
Fig. 7 is absorption property figure of the gained nickel ferrite based magnetic loaded of the embodiment 3/foam nickel composite to organic dyestuff.
Fig. 8 is the absorption property figure of the gained nickel ferrite based magnetic loaded of embodiment 3/foam nickel composite heavy metal ion.
Fig. 9 is preparation method flow chart of the sewerage disposing of the present invention with the Ni-based three-dimensional material of growth certainly.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
(1) nickel foam (110ppi nickel foams) is first cut into 4*6*0.05 centimetres of rectangle (0.690 gram), it is wide with it is anti-
Answer kettle internal diameter close, length is concordant with the page, so that nickel foam during the course of the reaction is kept upright state, be conducive to reacting is more equal
It is even.The nickel foam cut is put into 200mL beakers again, 100mL acetone ultrasound 30min is poured into, ultrasonic power is 240w.
Then acetone is outwelled, with deionized water rinsing, then the same ultrasound 30min of 100mL absolute ethyl alcohols is poured into (power is 240w).Most
Absolute ethyl alcohol is outwelled afterwards, with deionized water rinsing, then with deionized water ultrasound 30min (power is 240w).After the completion of ultrasound,
The nickel foam handled is put into 150mL autoclaves vertically.
(2) 1.163g six water nickel nitrate (Ni (NO are weighed respectively3)2·6H2O), 2.224g ferrous sulfate heptahydrate
(FeSO4·7H2O) mixed dissolution is in the 100mL aqueous solution, wherein, the molar concentration of nickel nitrate is 0.04 mol/L, and nitric acid is sub-
The molar concentration of iron is 0.08 mol/L, and the mol ratio of nickel ion and ferrous ion is 1：2, add until completely dissolved
0.3g urea is as protective agent, and 0.111g ammonium fluorides are stirred 0.5 hour, obtained mixed solution as template.
(3) mixed solution obtained in step (2) is poured into step (1) in 150mL autoclave, taken the photograph 120
Heated 12 hours under family name's degree, obtain the nickel foam with green precipitate.With absolute ethyl alcohol and deionized water rinsing several times after, put
Enter in air dry oven 70 degrees Celsius of dryings 8 hours, obtain the persursor material of nickel ferrite based magnetic loaded/foam nickel composite.
(4) persursor material of obtained nickel ferrite based magnetic loaded/foam nickel composite in step (3) 400 is taken the photograph under oxygen atmosphere
Family name's degree is calcined 2 hours, and heating rate is 2 DEG C/min, obtains water process with Ni-based from growing three-dimensional ferrous acid nickel composite material.
Material for water treatment, test are used as from growth three-dimensional composite material on Ni-based using nickel ferrite based magnetic loaded made from embodiment 1
It is to organic dyestuff and the absorption property of heavy metal ion.125mg/L Congo red standard liquid is prepared first.With electronics day
The flat Congo red powder for weighing 0.0625g, pours into 200mL beakers and adds 100mL deionized water stirring and dissolving.Then will
Solution after well mixed is transferred in 500mL volumetric flask, and beaker and glass bar is washed with deionized, and cleaning solution is fallen
Enter in volumetric flask, add at deionized water to graduation mark and shake up.The Congo red standard liquids of 125mg/L for taking 75mL to configure
In sample bottle, addition 0.3g nickel ferrite based magnetic loadeds/(the above-mentioned water process prepared is with Ni-based from growing three-dimensional ferrous acid for foam nickel material
Nickel composite material) stir, its Congo red concentration is tested with ultra-violet and visible spectrophotometer at regular intervals, so that
Obtain absorption property of the embodiment 1 to organic dyestuff.Likewise, 0.17668g potassium bichromate powder is weighed, with 500mL capacity
Bottle configures 125mg/L heavy metal chromium solions in the same way.Take the 125mg/L heavy metal chromium ions that 75mL has been configured
Standard liquid is in sample bottle, and adding 0.3g nickel ferrite based magnetic loadeds/foam nickel material, (the above-mentioned water process prepared is with Ni-based from growth
Three-dimensional ferrous acid nickel composite material) stir, test its huge sum of money with inductance Coupled Plasma Spectroscopy generator at regular intervals
Belong to the concentration of ion, so as to obtain the absorption property of the heavy metal ion of embodiment 1.
Fig. 1 is the XRD spectrum of nickel ferrite based magnetic loaded/nickel foam.The collection of illustrative plates and nickel ferrite based magnetic loaded and the standard card JCPDSno.10- of nickel
0325th, JCPDSno.04-0850 matches, without NiO, Fe2O3Deng the diffraction maximum of impurity, it is pure nickel ferrite based magnetic loaded/bubble to illustrate product
Foam nickel composite.Fig. 2 is the stereoscan photograph of nickel ferrite based magnetic loaded/nickel foam, it can be seen that three-dimensional flower-shaped nickel ferrite based magnetic loaded is uniformly given birth to
Length is on the skeleton of nickel foam, flower-shaped a length of 2~4 μm of average diameter, and Fig. 3 is nickel ferrite based magnetic loaded/foam nickel composite to organic dyestuff
Absorption property figure.Adsorbance to organic dyestuff can reach 81.8% within ten minutes, and absorption reaches adsorbance during balance
For 105.7mg g-1, Fig. 4 is the absorption property figure of nickel ferrite based magnetic loaded/foam nickel composite heavy metal ion.Heavy metal ion
Adsorbance can reach 89.6% in ten minutes, and absorption reaches that adsorbance during balance is 49.3mg g-1。
Embodiment 2
(1) nickel foam (110ppi nickel foams) is first cut into 4*6*0.05 centimetres of rectangle (0.690 gram), it is wide with it is anti-
Answer kettle internal diameter close, length is concordant with the page, so that nickel foam during the course of the reaction is kept upright state, be conducive to reacting is more equal
It is even.The nickel foam cut is put into 200mL beakers again, 100mL acetone ultrasound 40min is poured into, ultrasonic power is 200w.
Then acetone is outwelled, with deionized water rinsing, then the same ultrasound 40min of 100mL absolute ethyl alcohols is poured into (power is 200w).Most
Absolute ethyl alcohol is outwelled afterwards, with deionized water rinsing, then with deionized water ultrasound 40min (power is 200w).After the completion of ultrasound,
The nickel foam handled is put into 150mL autoclaves vertically.
(2) 2.328g six water nickel nitrate (Ni (NO are weighed respectively3)2·6H2O), 4.896g ferrous sulfate heptahydrate
(FeSO4·7H2O) mixed dissolution is in the 100mL aqueous solution, and wherein the molar concentration of nickel nitrate is 0.08 mol/L, and nitric acid is sub-
The molar concentration of iron is 0.16 mol/L, and the mol ratio of nickel ion and ferrous ion is 1：2, add until completely dissolved
0.06g urea is as protective agent, and 0.037g ammonium fluorides are stirred 2 hours, obtained mixed solution as template.
(3) mixed solution obtained in step (2) is poured into step (1) in 150mL autoclave, taken the photograph 110
Heated 16 hours under family name's degree, obtain the nickel foam with green precipitate.With absolute ethyl alcohol and deionized water rinsing several times after, put
Enter in air dry oven 60 degrees Celsius of dryings 10 hours, obtain the persursor material of nickel ferrite based magnetic loaded/foam nickel composite.
(4) persursor material of obtained nickel ferrite based magnetic loaded/foam nickel composite in step (3) 450 is taken the photograph under oxygen atmosphere
Family name's degree is calcined 3 hours, and heating rate is 2 DEG C/min, obtains water process with Ni-based from growing three-dimensional ferrous acid nickel composite material.
Material for water treatment, test are used as from growth three-dimensional composite material on Ni-based using nickel ferrite based magnetic loaded made from embodiment 2
It is to organic dyestuff and the absorption property of heavy metal ion.125mg/L Congo red standard liquid is prepared first.With electronics day
The flat Congo red powder for weighing 0.0625g, pours into 200mL beakers and adds 100mL deionized water stirring and dissolving.Then will
Solution after well mixed is transferred in 500mL volumetric flask, and beaker and glass bar is washed with deionized, and cleaning solution is fallen
Enter in volumetric flask, add at deionized water to graduation mark and shake up.The Congo red standard liquids of 125mg/L for taking 75mL to configure
In sample bottle, addition 0.3g nickel ferrite based magnetic loadeds/(the above-mentioned water process prepared is with Ni-based from growing three-dimensional ferrous acid for foam nickel material
Nickel composite material) stir, its Congo red concentration is tested with ultra-violet and visible spectrophotometer at regular intervals, so that
Obtain absorption property of the embodiment 2 to organic dyestuff.Likewise, 0.17668g potassium bichromate powder is weighed, with 500mL capacity
Bottle configures 125mg/L heavy metal chromium solions in the same way.Take the 125mg/L heavy metal chromium ions that 75mL has been configured
Standard liquid is in sample bottle, and adding 0.3g nickel ferrite based magnetic loadeds/foam nickel material, (the above-mentioned water process prepared is with Ni-based from growth
Three-dimensional ferrous acid nickel composite material) stir, test its huge sum of money with inductance Coupled Plasma Spectroscopy generator at regular intervals
Belong to the concentration of ion, so as to obtain the absorption property of the heavy metal ion of embodiment 2.
Fig. 5 is absorption property figure of the nickel ferrite based magnetic loaded/foam nickel composite to organic dyestuff.To the adsorption rate of organic dyestuff ten
79.3% is can reach within minute, absorption reaches that adsorbance during balance is 100.2mg g-1, Fig. 6 is that nickel ferrite based magnetic loaded/nickel foam is multiple
The absorption property figure of compound heavy metal ion.The adsorption rate of heavy metal ion can reach 87.2%, absorption in ten minutes
It is 48.6mg g to reach adsorbance during balance-1。
Embodiment 3
(1) nickel foam (110ppi nickel foams) is first cut into 4*6*0.05 centimetres of rectangle (0.690 gram), it is wide with it is anti-
Answer kettle internal diameter close, length is concordant with the page, so that nickel foam during the course of the reaction is kept upright state, be conducive to reacting is more equal
It is even.The nickel foam cut is put into 200mL beakers again, 100mL acetone ultrasound 50min is poured into, ultrasonic power is 180w.
Then acetone is outwelled, with deionized water rinsing, then the same ultrasound 50min of 100mL absolute ethyl alcohols is poured into (ultrasonic power is
180w).Finally absolute ethyl alcohol is outwelled, with deionized water rinsing, then with deionized water ultrasound 50min, (ultrasonic power is
180w).After the completion of ultrasound, the nickel foam handled is put into 150mL autoclaves vertically.
(2) 1.163g six water nickel nitrate (Ni (NO are weighed respectively3)2·6H2O), 2.224g ferrous sulfate heptahydrate
(FeSO4·6H2O) mixed dissolution is in the 100mL aqueous solution, and wherein the molar concentration of nickel nitrate is 0.04 mol/L, and nitric acid is sub-
The molar concentration of iron is 0.08 mol/L, and the mol ratio of nickel ion and ferrous ion is 1：2, add until completely dissolved
0.6g urea is as protective agent, and 0.185g ammonium fluorides are stirred 1 hour, obtained mixed solution as template.
(3) mixed solution obtained in step (2) is poured into step (1) in 150mL autoclave, taken the photograph 130
Heated 10 hours under family name's degree, obtain the nickel foam with green precipitate.With absolute ethyl alcohol and deionized water rinsing several times after, put
Enter in air dry oven 70 degrees Celsius of dryings 8 hours, obtain the persursor material of nickel ferrite based magnetic loaded/foam nickel composite.
(4) persursor material of obtained nickel ferrite based magnetic loaded/foam nickel composite in step (3) 500 is taken the photograph under oxygen atmosphere
Family name's degree is calcined 4 hours, and heating rate is 2 DEG C/min, obtains water process with Ni-based from growing three-dimensional ferrous acid nickel composite material.
Material for water treatment, test are used as from growth three-dimensional composite material on Ni-based using nickel ferrite based magnetic loaded made from embodiment 3
It is to organic dyestuff and the absorption property of heavy metal ion.125mg/L Congo red standard liquid is prepared first.With electronics day
The flat Congo red powder for weighing 0.0625g, pours into 200mL beakers and adds 100mL deionized water stirring and dissolving.Then will
Solution after well mixed is transferred in 500mL volumetric flask, and beaker and glass bar is washed with deionized, and cleaning solution is fallen
Enter in volumetric flask, add at deionized water to graduation mark and shake up.The 125mg/L organic dyestuff standards for taking 75mL to configure are molten
Liquid adds 0.3g nickel ferrite based magnetic loadeds/(the above-mentioned water process prepared is with Ni-based from growing three-dimensional iron for foam nickel material in sample bottle
Sour nickel composite material) stir, its Congo red concentration is tested with ultra-violet and visible spectrophotometer at regular intervals, from
And obtain absorption property of the embodiment 3 to organic dyestuff.Likewise, 0.17668g potassium bichromate powder is weighed, with 500mL appearance
Measuring bottle configures 125mg/L heavy metal chromium solions in the same way.Take the 125mg/L heavy metal chromiums that 75mL has been configured from
Substandard solution is in sample bottle, and adding 0.3g nickel ferrite based magnetic loadeds/foam nickel material, (the above-mentioned water process prepared is with Ni-based spontaneous
Long three-dimensional ferrous acid nickel composite material) stir, it is heavy to test its with inductance Coupled Plasma Spectroscopy generator at regular intervals
The concentration of metal chromium ions, so as to obtain the absorption property of the heavy metal ion of embodiment 3.
Fig. 7 is absorption property figure of the nickel ferrite based magnetic loaded/foam nickel composite to organic dyestuff.To the adsorbance of organic dyestuff ten
83.5% is can reach within minute, absorption reaches that adsorbance during balance is 107.3mg g-1, Fig. 8 is that nickel ferrite based magnetic loaded/nickel foam is multiple
The absorption property figure of compound heavy metal ion.The adsorbance of heavy metal ion can reach 90.2%, absorption in ten minutes
It is 51.1mg g to reach adsorbance during balance-1。
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of water process is with Ni-based from the preparation method for growing three-dimensional material, it is characterised in that comprise the following steps：
(1) metal substrate is cleaned with surface conditioning agent, obtains metal substrate I；
(2) by nickel salt and divalent iron salt dissolving in a solvent, precipitating reagent and protective agent are added, is stirred, mixing is obtained molten
Liquid；
(3) mixed solution obtained in step (2) is poured into the metal substrate I obtained in step (1), 110 DEG C~130
Reacted under the conditions of DEG C, then take precipitation, washed, dried, obtain the persursor material of nickel ferrite based magnetic loaded/foam nickel composite；
(4) persursor material of the nickel ferrite based magnetic loaded obtained in step (3)/foam nickel composite is calcined, obtains water process use
Ni-based growth three-dimensional material certainly.
2. water process according to claim 1 is with Ni-based from the preparation method for growing three-dimensional material, it is characterised in that：
Metal substrate described in step (1) is nickel foam；
Nickel salt described in step (2) is soluble nickel salt；
Divalent iron salt described in step (2) is soluble divalent iron salt；
Precipitating reagent described in step (2) is ammonium fluoride or ammonium chloride；
Protective agent described in step (2) is urea.
3. water process according to claim 2 is with Ni-based from the preparation method for growing three-dimensional material, it is characterised in that：
Metal substrate described in step (1) is 110PPI nickel foams；
Surface conditioning agent described in step (1) is at least one of acetone, absolute ethyl alcohol and deionized water；
Nickel salt described in step (2) is at least one of nickel chloride, nickel nitrate and nickel sulfate；
Divalent iron salt described in step (2) is at least one of frerrous chloride, ferrous nitrate and ferrous sulfate；
Solvent described in step (2) is deionized water.
4. water process according to claim 1 is with Ni-based from the preparation method for growing three-dimensional material, it is characterised in that：
The concentration of nickel ion is 0.01~0.1mol/L in mixed solution described in step (2), and the concentration of ferrous ion is
0.02~0.2mol/L；
The mol ratio of nickel ion and ferrous ion is 1 in mixed solution described in step (2)：2.
5. water process according to claim 1 is with Ni-based from the preparation method for growing three-dimensional material, it is characterised in that：Step
(2) concentration of precipitating reagent is 0.001~0.005mol/L in the mixed solution described in；Protectant concentration be 0.001~
0.01mol/L。
6. water process according to claim 1 is with Ni-based from the preparation method for growing three-dimensional material, it is characterised in that：
Cleaning described in step (1) is successively with acetone, absolute ethyl alcohol and deionized water ultrasonic cleaning；
Washing described in step (3) is to be washed successively with absolute ethyl alcohol and deionized water；
The time of reaction described in step (3) is 10~20 hours；
The condition of drying described in step (3) is：50~80 DEG C of dryings 6~12 hours；
The condition of calcining described in step (4) is：Under air or oxygen atmosphere, 300~600 DEG C of 2~6h of calcining.
7. water process according to claim 1 is with Ni-based from the preparation method for growing three-dimensional material, it is characterised in that：
The condition of calcining described in step (4) is：It is warming up to 400 under air or oxygen atmosphere, with 2 DEG C/min speed~
450 DEG C, then calcine 2~4h.
8. a kind of water process is with Ni-based from growth three-dimensional material, it is characterised in that：By described in any one of claim 1~7
Method is prepared.
9. the Ni-based application from growth three-dimensional material in sewage treatment area described in claim 8.
10. the Ni-based application from growth three-dimensional material in sewage treatment area according to claim 8 is characterized in that：
Described sewage is the sewage containing organic dyestuff or heavy metal ion；Described organic dyestuff is Congo red；A described huge sum of money
Category ion is chromium ion.
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| CN109225123A (en) * | 2018-10-18 | 2019-01-18 | 太原理工大学 | It is a kind of using three-dimensional foam nickel as the preparation method and application of the hierarchical porous structure NiO/Ni of skeleton |
| CN109794247A (en) * | 2019-01-16 | 2019-05-24 | 北京工业大学 | A kind of amorphous iron-doped nickel oxide nano-sheet electrocatalysis material and its preparation and application |
| CN110040789A (en) * | 2019-04-17 | 2019-07-23 | 天津大学 | A kind of preparation method of nickel ferrite based magnetic loaded microballoon electrode material for super capacitor |
| CN112547096A (en) * | 2020-12-10 | 2021-03-26 | 华南师范大学 | Carbon-based sulfide composite photocatalyst, preparation method and application thereof in heavy metal degradation |
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| CN110040789A (en) * | 2019-04-17 | 2019-07-23 | 天津大学 | A kind of preparation method of nickel ferrite based magnetic loaded microballoon electrode material for super capacitor |
| CN110040789B (en) * | 2019-04-17 | 2021-11-02 | 天津大学 | Preparation method of nickel ferrite microsphere supercapacitor electrode material |
| CN112547096A (en) * | 2020-12-10 | 2021-03-26 | 华南师范大学 | Carbon-based sulfide composite photocatalyst, preparation method and application thereof in heavy metal degradation |
| CN113249743A (en) * | 2021-05-18 | 2021-08-13 | 上海大学 | Catalyst for electrocatalytic oxidation of glycerol and preparation method thereof |
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