CN108554367A - A method of preparing magnetic Nano iron oxide particle adsorbent - Google Patents
A method of preparing magnetic Nano iron oxide particle adsorbent Download PDFInfo
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- CN108554367A CN108554367A CN201810496756.8A CN201810496756A CN108554367A CN 108554367 A CN108554367 A CN 108554367A CN 201810496756 A CN201810496756 A CN 201810496756A CN 108554367 A CN108554367 A CN 108554367A
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- iron oxide
- oxide particle
- magnetic nano
- nano iron
- suspension
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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
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
-
- 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
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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
- C02F1/28—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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
- C02F1/488—Treatment of water, waste water, or sewage with magnetic or electric fields for separation of magnetic materials, e.g. magnetic flocculation
-
- 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
- C02F2101/103—Arsenic compounds
-
- 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
Abstract
The invention discloses a kind of method preparing magnetic Nano iron oxide particle adsorbent, step includes：Simultaneously FeCl is conveyed into T-type mixing channel3With FeCl2Mixed solution and NaOH solution；Enter helix tube after being mixed rapidly in T-type mixing channel, forms the suspension of magnetic Nano iron oxide particle crystal in helix tube, and finally flow into recovery system；The magnetic Nano iron oxide particle crystal in suspension is recycled using magnetic field；The granule crystal being recovered to is washed with deionized；Suspension is made in the granule crystal for disperseing to be resuspended after washing with deionized water, and the pH value for adjusting suspension is 4.0, is saved backup under the conditions of being placed in+4 DEG C.The preparation method can serialization, prepare magnetic Nano iron oxide particle adsorbent to homogenization, and the magnetic Nano iron oxide particle adsorbent adsorption capacity being prepared is strong.
Description
Technical field
The invention belongs to environment water treatment field more particularly to a kind of magnetic Nano iron oxide particle adsorbents of preparing
Method.
Background technology
The iron oxide nanoparticles adsorbent with superparamagnetism received a large amount of concerns in recent years, was keeping high
While specific surface area there is magnetics to recycle characteristic, can realize the system of nano adsorber high adsorption capacity and low recycling separation costs
One.But its traditional water phase co-precipitation preparation method has preparation process crystallization time length and crystalline environment otherness big equal intrinsic scarce
Point, the product lack of homogeneity caused, reunion degree is high, is difficult to realize industrial-scale production.
Invention content
Goal of the invention：There is provided a kind of serialization, the method that homogenization prepares magnetic Nano iron oxide particle adsorbent.
Technical solution：A kind of method preparing magnetic Nano iron oxide particle adsorbent of the present invention, including such as
Lower step：
Step 1, it while being conveyed into T-type mixing channel and contains 0.1mol/L FeCl3With 0.05mol/L FeCl2Mixing it is molten
The NaOH solution of liquid and 0.5mol/L；
Step 2, pass through during through spiral Bottomhole pressure into helix tube after being mixed rapidly in T-type mixing channel
" crystallization-dissolution-crystallization " repeatedly forms the suspension of magnetic Nano iron oxide particle crystal, and finally flows into recycling system
System；
Step 3, the magnetic Nano iron oxide particle crystal in suspension is recycled using magnetic field；
Step 4, the magnetic Nano iron oxide particle crystal being recovered to is washed with deionized, removes remained on surface
Object；
Step 5, suspension is made in the magnetic Nano iron oxide particle crystal for disperseing to be resuspended after washing with deionized water, adjusts
The pH value of suspension after section dispersion resuspension is 4.0, is saved backup under the conditions of being placed in+4 DEG C.
Further, in step 1, conveying contains 0.1mol/L FeCl3With 0.05mol/L FeCl2Mixed solution it is defeated
It is 5.0mL/min to send flow velocity；The conveying flow velocity for conveying the NaOH solution of 0.5mol/L is 2.5mL/min.It is uninterrupted using two-way
Synchronous transport FeCl3With FeCl2Mixed solution and NaOH solution, can realize serialization, homogenization chemically react, and
Respective conveying flow velocity is adapted with respective concentration so that the material ratio of reaction, which meets to prepare, to be required.
Further, in step 2, the length of helix tube is 12m and internal diameter is 0.5mm.Using the helix tube energy of the size
Enough ensure to react duration and solution mixed effect.
Further, in step 2, helix tube is located in water bath with thermostatic control.It can ensure coprecipitation reaction using water bath with thermostatic control
When crystallization process temperature it is constant.
Further, it in step 2, between the temperature of water bath with thermostatic control maintains 59-61 DEG C, is tied when ensuring coprecipitation reaction
The temperature of brilliant process is constant.
Further, in step 3, magnetic field is the magnetic field that permanent magnet or electromagnet form 0.6T.Using the magnetic field of 0.6T
MNPs that can be in high efficiente callback suspension.
Further, in step 4, deionized water washing times are 3-4 times.It is washed using 3-4 deionized water, Neng Gouyou
The residue of effect removal magnetic Nano iron oxide particle plane of crystal.
Further, in step 5, it is come the pH value for adjusting the suspension after dispersion is resuspended using 0.1mol/L HCl solutions
4.0.Using 0.1mol/L HCl solutions come adjust pH value be 4.0 so that the adsorbent of preparation is easy to store spare.
Compared with prior art, the present invention advantage is：Preparation method through the invention can serialization, uniformly
Magnetic Nano iron oxide particle adsorbent is prepared with changing, when overcoming the crystallization of traditional water phase co-precipitation preparation method preparation process
Between the long and big inherent defect of crystalline environment otherness, and prepared magnetic Nano iron oxide particle adsorbent adsorption capacity
By force, it is easily recycled.
Description of the drawings
Fig. 1 is the preparation system structural schematic diagram of the present invention；
Fig. 2 is the transmission electron microscope picture (TEM) of the nano-scale magnetic iron oxide particle of the present invention.
Specific implementation mode
Technical solution of the present invention is described in detail below in conjunction with the accompanying drawings, but protection scope of the present invention is not limited to
The embodiment.
As shown in Figure 1, the method disclosed by the invention for preparing magnetic Nano iron oxide particle adsorbent, including walk as follows
Suddenly：
Step 1, from pump a and pump b, into T-type mixing channel, conveying contains 0.1mol/L FeCl simultaneously respectively3With 0.05mol/
L FeCl2Mixed solution and 0.5mol/L NaOH solution；It pumps a conveyings and contains 0.1mol/L FeCl3With 0.05mol/L
FeCl2Mixed solution conveying flow velocity be 5.0mL/min；The conveying flow velocity of NaOH solution of pump b conveyings 0.5mol/L is
2.5mL/min。
Step 2, helix tube is entered after being mixed rapidly in T-type mixing channel, the length of helix tube is 12m and internal diameter is
0.5mm, helix tube are located in water bath with thermostatic control, between the temperature of water bath with thermostatic control maintains 59-61 DEG C, preferably 60 DEG C, and to ensure
The temperature of crystallization process is constant when coprecipitation reaction, the Fe in solution3+With Fe2+Iron is formed under the action of pH mutagens NaOH
Oxysome nucleus forms Magnetic nano iron oxygen during through spiral Bottomhole pressure by " crystallization-dissolution-crystallization " repeatedly
The suspension of compound granule crystal, and finally flow into recovery system；
Step 3, using magnetic field recycle suspension in magnetic Nano iron oxide particle crystal, magnetic field be permanent magnet or
Electromagnet forms the magnetic field of 0.6T；
Step 4, the magnetic Nano iron oxide particle crystal being recovered to is washed with deionized, washing times 3-4
It is secondary, preferably 3 times, remove surface residue；
Step 5, suspension is made in the magnetic Nano iron oxide particle crystal for disperseing to be resuspended after washing with deionized water, profit
The pH value for adjusting the suspension after dispersion is resuspended with 0.1mol/L HCl solutions is 4.0, and the absorption formed after pH is adjusted
Agent saves backup under the conditions of being placed in+4 DEG C.
Embodiment 1：
As shown in Fig. 2, the transmission electron microscope picture (TEM) of the nano-scale magnetic iron oxide particle of gained is prepared for the present invention,
The grain size for the magnetic Nano ferriferous oxide being prepared is about between 8-12nm.
Embodiment 2：
At 25 DEG C, the magnetic Nano iron oxide particle that 0.2g is prepared is dispersed in 100mL deionized waters
In, after using intensity to recycle 5min for the external magnetic field of 0.6T, it can realize that the separation of magnetic nanoparticle and water phase, the rate of recovery reach
To 99.96% or more.
Embodiment 3：
By 0.1g prepare gained magnetic Nano iron oxide particle adsorbent be added 100mL, pH value=7.0, As just
Begin the NaH of a concentration of 50mg/L2AsO3It is molten under the conditions of the temperature of 30 DEG C of maintenance, the concussion of 175rpm after reaction 50min in solution
The removal rate of As (III) is higher than 99.91% in liquid, and residual concentration is less than 0.09mg/L, and meeting the upper limit in national waste water is
The arsenic content discharge standard of 0.5mg/L.
Embodiment 4：
By 0.1g prepare gained magnetic Nano iron oxide particle adsorbent be added 100mL, pH value=3.0, As just
Begin the NaH of a concentration of 50mg/L2AsO4It is molten under the conditions of the temperature of 30 DEG C of maintenance, the concussion of 175rpm after reaction 50min in solution
The residual concentration of As (V) is that removal rate is higher than 99.96% in liquid, and residual concentration is less than 0.04mg/L, meets in national waste water
It is limited to the arsenic content discharge standard of 0.5mg/L.
Embodiment 5：
By 0.2g prepare gained magnetic Nano iron oxide particle adsorbent be added 100mL, pH value=3.0, Cr just
Begin the K of a concentration of 50mg/L2Cr2O7It is molten under the conditions of the temperature of 30 DEG C of maintenance, the concussion of 175rpm after reaction 50min in solution
The residual concentration of Cr (VI) is that removal rate is higher than 99.97% in liquid, and residual concentration is less than 0.03mg/L, meets in national waste water
It is limited to Cr (VI) content discharge standard of 0.5mg/L.
As described above, although the present invention has been indicated and described with reference to specific preferred embodiment, must not explain
For the limitation to invention itself.It without prejudice to the spirit and scope of the invention as defined in the appended claims, can be right
Various changes can be made in the form and details for it.
Claims (8)
1. a kind of method preparing magnetic Nano iron oxide particle adsorbent, which is characterized in that include the following steps：
Step 1, it while being conveyed into T-type mixing channel and contains 0.1mol/L FeCl3With 0.05mol/L FeCl2Mixed solution with
And the NaOH solution of 0.5mol/L；
Step 2, helix tube is entered after being mixed rapidly in T-type mixing channel, during through spiral Bottomhole pressure, by repeatedly
" crystallization-dissolution-crystallization " form the suspension of magnetic Nano iron oxide particle crystal, and finally flow into recovery system；
Step 3, the magnetic Nano iron oxide particle crystal in suspension is recycled using magnetic field；
Step 4, the magnetic Nano iron oxide particle crystal being recovered to is washed with deionized, removes surface residue；
Step 5, suspension is made in the magnetic Nano iron oxide particle crystal for disperseing to be resuspended after washing with deionized water, adjusts and divides
The pH value of suspension after bulk weight is outstanding is 4.0, is saved backup under the conditions of being placed in+4 DEG C.
2. the method according to claim 1 for preparing magnetic Nano iron oxide particle adsorbent, which is characterized in that step
In 1, conveying contains 0.1mol/L FeCl3With 0.05mol/L FeCl2Mixed solution conveying flow velocity be 5.0mL/min；It is defeated
It is 2.5mL/min to send the conveying flow velocity of the NaOH solution of 0.5mol/L.
3. the method according to claim 1 for preparing magnetic Nano iron oxide particle adsorbent, which is characterized in that step
In 2, the length of helix tube is 12m and internal diameter is 0.5mm.
4. the method according to claim 1 for preparing magnetic Nano iron oxide particle adsorbent, which is characterized in that step
In 2, helix tube is located in water bath with thermostatic control.
5. the method according to claim 4 for preparing magnetic Nano iron oxide particle adsorbent, which is characterized in that step
In 2, between the temperature of water bath with thermostatic control maintains 59-61 DEG C, the temperature of crystallization process is constant when ensuring coprecipitation reaction.
6. the method according to claim 1 for preparing magnetic Nano iron oxide particle adsorbent, which is characterized in that step
In 3, magnetic field is the magnetic field that permanent magnet or electromagnet form 0.6T.
7. the method according to claim 1 for preparing magnetic Nano iron oxide particle adsorbent, which is characterized in that step
In 4, deionized water washing times are 3-4 times.
8. the method according to claim 1 for preparing magnetic Nano iron oxide particle adsorbent, which is characterized in that step
In 5, the pH value for adjusting the suspension after dispersion is resuspended using 0.1mol/L HCl solutions is 4.0.
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| CN201810496756.8A CN108554367A (en) | 2018-05-22 | 2018-05-22 | A method of preparing magnetic Nano iron oxide particle adsorbent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111208192A (en) * | 2020-01-15 | 2020-05-29 | 中国科学院生态环境研究中心 | Magnetic Fe in the environment3O4Circulating enrichment device for separating and extracting nano particles and detection method thereof |
| CN112125344A (en) * | 2019-06-25 | 2020-12-25 | 北京化工大学 | Preparation method of monodisperse nano iron oxide dispersoid |
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Application publication date: 20180921 |