CN108554385A - A kind of preparation method of the mesoporous carbosphere of magnetic ferric alginate of adsorbable heavy metal element - Google Patents
A kind of preparation method of the mesoporous carbosphere of magnetic ferric alginate of adsorbable heavy metal element Download PDFInfo
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- CN108554385A CN108554385A CN201810044203.9A CN201810044203A CN108554385A CN 108554385 A CN108554385 A CN 108554385A CN 201810044203 A CN201810044203 A CN 201810044203A CN 108554385 A CN108554385 A CN 108554385A
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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
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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
- B01J20/28014—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 form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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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
- B01J20/28054—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 surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
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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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/103—Arsenic compounds
Abstract
The present invention relates to a kind of preparation methods of the mesoporous carbosphere of magnetic ferric alginate of adsorbable heavy metal element, SAC precursor solutions are prepared by sodium alginate saturated solution and urea (urea), and ferric alginate microballoon has been synthesized by ionic cross-linking, and it is prepared for the mesoporous carbosphere of magnetic ferric alginate (MAMC) that nano-iron oxide is adhered on surface using vacuum refrigeration and high-temperature cracking method;The present invention prepares that simple, highly practical, thermal stability is good, and the material is good to the adsorption effect of water body As (III), As (V);And the microballoon (MAMC) has superparamagnetism, it can realize the separation between the solute and solvent under externally-applied magnetic field intervention, therefore heavy metal ion and material can be removed into water-outlet body after material adsorption saturation, high degree avoids heavy metal secondary pollution.In addition, the MAMC material regeneration abilities are strong, can recycled for multiple times, 90% is being maintained at for the adsorption rate of As (III) by 4 desorptions and regeneration MAMC, is further improving the cyclic utilization rate of sorbing material.
Description
Technical field
The present invention relates to a kind of sorbing material technical field, the magnetic ferric alginate of especially a kind of adsorbable heavy metal is situated between
The preparation method of hole carbosphere.
Background technology
While with economic fast development, many industrial pollution problems are also brought, such as machine-building, chemical industry exist
Many heavy metal wastewater therebies are produced in production process, heavy metal arsenic (Arsenic) is a kind of metalloid element that toxicity is extremely strong, arsenic
And the compound of arsenic is widely present in nature, research finds that the toxicity of inorganic arsenic is much larger than organo-arsenic, and trivalent arsenic toxicity
It is stronger than pentavalent arsenic, at present for arsenic in water body pollution processing method mainly include removal separation and oxidation toxicity reduction, but this two
Kind method is limited by complex process, processing cost high condition, and the heavy metal after adsorption treatment has recycling and is stranded
The problems such as difficult, and the stability of sorbing material is poor.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of magnetic ferric alginate mesoporous carbon of adsorbable heavy metal element
The preparation method of microballoon.
The technical scheme is that:A kind of preparation of the mesoporous carbosphere of magnetic ferric alginate of adsorbable heavy metal element
Method includes the following steps:
S1 the sodium alginate that 2%~4% is configured in deionized water), will be dissolved under the conditions of sodium alginate powder heating bath
Saturated solution, it is for use after cooling;
S2 the urea (urea) of certain mass), is added in sodium alginate saturated solution, it is cold after 10~40min of magnetic agitation
But it is for use that SAC precursor solutions are obtained;
S3), nine water ferric nitrate solid powders are dissolved in deionized water, are configured to 5%~10% iron nitrate solution,
Then SAC precursor solutions are added dropwise in iron nitrate solution with the rate of 20 drops/min under agitation, as SAC forerunner
Solution can form the little particle of drops when encountering iron nitrate solution, the ripples whirlpool that magnetic stirring apparatus is formed can be the small of formation
Particle screws in solution bottom, it is ensured that the particle being subsequently formed does not generate adhesion phenomenon;
S4 it), seals after completion of the reaction, and places and be aged 48h at room temperature, take the particulate matter of formation after ageing
Go out, deionized water collocation ultrasonic cleaner is used in combination to clean 12~15 times, until cleaning oozes middle detection without Fe3+Exudation;
S5), material is put into vacuum freeze dryer after cleaning completely and is freeze-dried 48h, obtains moisture free Huang
Brown solid particle (SA@Fe Particles);
S6), SA@Fe particles are positioned in tube furnace, according to the heating rate of 1 DEG C/min under conditions of being passed through nitrogen
It is warming up to 300 DEG C, and Heat preservation 3h, the mesoporous carbosphere of magnetic ferric alginate (MAMC) is then obtained after natural cooling.
In above-mentioned technical proposal, step S1) in, the pure grade of chemistry of the sodium alginate powder be (viscosity (10g/L) >=
0.02Pa·s)。
In above-mentioned technical proposal, step S2) in, the urea (urea) of addition is 1 with the mass ratio of sodium alginate:1.
Beneficial effects of the present invention are:
1, prepare that simple, highly practical, thermal stability is good, with sodium alginate be forerunner's template by sub- cross-linking method successfully
Porous ferric alginate microballoon has been synthesized, the mesoporous carbosphere of magnetic ferric alginate is prepared for by vacuum refrigeration and high temperature cabonization
(MAMC), the material is good to the adsorption effect of water body As (III), As (V);
2, the mesoporous carbosphere of magnetic ferric alginate (MAMC) prepared has superparamagnetism, can realize externally-applied magnetic field intervention
Under solute and solvent between separation, therefore can after material adsorption saturation by heavy metal ion and material stripping water outlet
Body, high degree avoid heavy metal secondary pollution.
3, the raw material of the mesoporous carbosphere of magnetic ferric alginate (MAMC) synthesized is relatively inexpensive, and wherein Na-alginate is natural
The application of the polysaccharide component extracted in seaweed, nine water ferric nitrates is also more universal, and realization scale can save cost after generating
And material " green, economic feasibility " can be played.
4.MAMC material regeneration abilities are strong, can recycled for multiple times, by 4 times desorption and regeneration MAMC for As
(III) adsorption rate is maintained at 90%, further improves the cyclic utilization rate of sorbing material.
Description of the drawings
Fig. 1 is the SEM figures of MAMC materials prepared by embodiment 1, wherein figure B is the partial enlarged view for scheming A.
Fig. 2 is the adsorption rate figure of MAMC materials prepared by embodiment 1;
Fig. 3 is the influence diagram for the MAMC adsorption capacities of materials that waste water PH prepares embodiment 1;
Fig. 4 is the pore-size distribution and BHJ curve graphs of MAMC materials prepared by embodiment 1;
Fig. 5 is weightlessness (TGA) figure of MAMC material heat prepared by embodiment 1;
Specific implementation mode
The specific implementation mode of the present invention is described further below in conjunction with the accompanying drawings:
Embodiment 1
A kind of preparation method of the mesoporous carbosphere of magnetic ferric alginate of adsorbable heavy metal element, includes the following steps:
S1), pure grade (viscosity (10g/L) >=0.02Pas) sodium alginate powder of 2g chemistry is weighed using position balance very much
Be dissolved under the conditions of heating bath be configured in 98mL deionized waters 2% sodium alginate saturated solution, it is for use after cooling;
S2 the urea of 2g), is added in sodium alginate saturated solution, it is molten that magnetic agitation 30min postcoolings obtain SAC forerunner
Liquid is for use;
S3), nine water ferric nitrate solid powders are dissolved in deionized water, 5% iron nitrate solution is configured to, then exists
SAC precursor solutions are added dropwise in iron nitrate solution with the rate of 20 drops/min under stirring condition, when SAC precursor solutions are met
To the little particle that can form drops when iron nitrate solution, the ripples whirlpool that magnetic stirring apparatus is formed can revolve the little particle of formation
Enter solution bottom, it is ensured that the particle being subsequently formed does not generate adhesion phenomenon;
S4 it), seals after completion of the reaction, and places and be aged 48h at room temperature, take the particulate matter of formation after ageing
Go out, deionized water collocation ultrasonic cleaner is used in combination to clean 12~15 times, until cleaning oozes middle detection without Fe3+Exudation;
S5), material is put into vacuum freeze dryer after cleaning completely and is freeze-dried 48h, obtains moisture free Huang
Brown solid particle (SA@Fe Particles);
S6), SA@Fe particles are positioned in tube furnace, according to the heating rate of 1 DEG C/min under conditions of being passed through nitrogen
It is warming up to 300 DEG C, and Heat preservation 3h, the mesoporous carbosphere of magnetic ferric alginate (MAMC) is then obtained after natural cooling.
Embodiment 2
A kind of preparation method of the mesoporous carbosphere of magnetic ferric alginate of adsorbable heavy metal element, includes the following steps:
S1 the sodium alginate powder of the pure grade (viscosity (10g/L) >=0.02Pas) of 3g chemistry), is weighed using position balance very much
Be dissolved under the conditions of last heating bath be configured in 97mL deionized waters 3% sodium alginate saturated solution, it is for use after cooling;
S2 the urea of 3g), is added in sodium alginate saturated solution, it is molten that magnetic agitation 30min postcoolings obtain SAC forerunner
Liquid is for use;
S3), nine water ferric nitrate solid powders are dissolved in deionized water, 5% iron nitrate solution is configured to, then exists
SAC precursor solutions are added dropwise in iron nitrate solution with the rate of 20 drops/min under stirring condition, when SAC precursor solutions are met
To the little particle that can form drops when iron nitrate solution, the ripples whirlpool that magnetic stirring apparatus is formed can revolve the little particle of formation
Enter solution bottom, it is ensured that the particle being subsequently formed does not generate adhesion phenomenon;
S4 it), seals after completion of the reaction, and places and be aged 48h at room temperature, take the particulate matter of formation after ageing
Go out, deionized water collocation ultrasonic cleaner is used in combination to clean 12~15 times, until cleaning oozes middle detection without Fe3+Exudation;
S5), material is put into vacuum freeze dryer after cleaning completely and is freeze-dried 48h, obtains moisture free Huang
Brown solid particle (SA@Fe Particles);
S6), SA@Fe particles are positioned in tube furnace, according to the heating rate of 1 DEG C/min under conditions of being passed through nitrogen
It is warming up to 300 DEG C, and Heat preservation 3h, the mesoporous carbosphere of magnetic ferric alginate (MAMC) is then obtained after natural cooling.
Embodiment 3
A kind of preparation method of the mesoporous carbosphere of magnetic ferric alginate of adsorbable heavy metal element, includes the following steps:
S1 the sodium alginate powder of the pure grade (viscosity (10g/L) >=0.02Pas) of 3g chemistry), is weighed using position balance very much
Be dissolved under the conditions of last heating bath be configured in 97mL deionized waters 3% sodium alginate saturated solution, it is for use after cooling;
S2 the urea of 3g mass fractions), is added in sodium alginate saturated solution, magnetic agitation 30min postcoolings obtain
SAC precursor solutions are for use;
S3), nine water ferric nitrate solid powders are dissolved in deionized water, are configured to 10% iron nitrate solution, then
SAC precursor solutions are added dropwise in iron nitrate solution with the rate of 20 drops/min under agitation, when SAC precursor solutions
The little particle of drops can be formed when encountering iron nitrate solution, the ripples whirlpool that magnetic stirring apparatus is formed can be the little particle of formation
Screw in solution bottom, it is ensured that the particle being subsequently formed does not generate adhesion phenomenon;
S4 it), seals after completion of the reaction, and places and be aged 48h at room temperature, take the particulate matter of formation after ageing
Go out, deionized water collocation ultrasonic cleaner is used in combination to clean 12~15 times, until cleaning oozes middle detection without Fe3+Exudation;
S5), material is put into vacuum freeze dryer after cleaning completely and is freeze-dried 48h, obtains moisture free Huang
Brown solid particle (SA@Fe Particles);
S6), SA@Fe particles are positioned in tube furnace, according to the heating rate of 1 DEG C/min under conditions of being passed through nitrogen
It is warming up to 300 DEG C, and Heat preservation 3h, the mesoporous carbosphere of magnetic ferric alginate (MAMC) is then obtained after natural cooling.
Embodiment 4
1.1MAMC morphology analysis
Fig. 1 is the SEM figures of the mesoporous carbosphere of magnetic ferric alginate (MAMC) material prepared by the embodiment, can be with from figure
Finding out on microballoon has many irregular holes, and dispersibility is higher, and as can be seen that material surface loads from figure B
A large amount of granular object, it can be seen that iron oxide particle is intensive have been loaded in material interlayer interlayer hole, table
Bright ferric oxide particles have successfully loaded to the surface of alginate presoma, and show material iron member by EDS data
The accounting of element is 52.32% or more.
1.2 adsorption rates are tested
A concentration of 50mg/L of 25mL are added in centrifuge tube A, B, C, D, E, F of 50mL contains As (III) waste liquid, then divides
The mesoporous carbosphere of magnetic ferric alginate (MAMC) for not taking 0.125g, 0.25g, 0.5g, 0.75g, 1g, 1.25g embodiment 1 to prepare
Be added in centrifuge tube A, B, C, D, E, F, be positioned in gas bath isothermal vibration case concussion until adsorption equilibrium, 3200r/min from
It is separated by filtration after the heart, filter liquor dilution is to be measured, and the filtrate after adsorption equilibrium is measured molten using inductive coupling plasma emission spectrum
The concentration of remaining arsenic in liquid, wherein waste liquid is natrium arsenicum (Na3AsO3), sodium arsenite (NaAsO2) prepare mother liquor dilution, from
In Fig. 2 as can be seen that when test waste strength be 50mg/L when, microballoon add for 1g when, adsorption rate reaches as high as 96%
More than.
Influence of the 1.3 waste water pH values to adsorption rate
Waste liquid pH value is adjusted using the NaOH and HCl of 0.1mol/L, wherein liquid waste concentration containing As is 150mg/L, is adjusted
PH value is to 2,3,4,5,6,7,8,9,10,11, according to 1:The MAMC that 25 solid-to-liquid ratio accurately weighs the preparation of embodiment 1 is added to
In the waste water for stating different pH value, 3200rpm is centrifuged after fully shaking 24 hours, and 0.45um filter membrane mistakes are installed using injector for medical purpose
Filter, filter liquor dilution, and adsorption rate female in waste water is detected, as shown in figure 3, absorption of the MAMC materials to As (III) and As (V)
Amount is more close with the pH value relationship of solution, and for containing the waste water of As (V), acid condition is more advantageous to the absorption of material, but pH
When gradually rising, the adsorbance of unit (g) material continuously decreases, and drastically declines in pH=9, this is because the table of adsorbent
Surface charge characteristic and solute form and the pH value of solution have important relationship, when pH value is maintained between 3.0~6.0, As (V)
Ion is mainly with H2AsO4 -Form exist;When pH value is 8.0~10.5, As (V) ion is with HAsO4 2-Form exist, and
AsO4 3-Higher pH value section is appeared in, (the pH when the pH value in solution medium is more than the isoelectric pH value of MAMCPZC 6.3±
0.5) negative charge amount of material surface, can be increased, and then increases the electrostatic repulsion of material and anion, the adsorbance of As (V) can
It can significantly reduce, for containing the waste water of As (III), material is in the adsorption effect of high ph-values and low pH all unobvious;Work as solution
PH value it is relatively low when, the part ferriferous oxide on the surfaces MAMC can dissolve, to reduce the adsorption site of arsenate.With
The pH value of solution gradually rises, and the ligand absorption on metal oxide gradually increases, unionized arsenious acid (H3AsO3 0) more advantageous
In being adsorbed onto on the non-ionic site of MAMC, when pH is much larger than PZC points, hydrolysate Fe occurs for nano-iron oxide
(OH)3Electronics transfer occurs and generates Fe (OH)4 -, increase and denounceed with interionic competitive Adsorption existing for anionic form and coulomb
Power, to inhibit H2AsO3-,HAsO3 2-,AsO3 3-The absorption of the anionic forms such as equal arsenates.
1.4MAMC pore-size distributions and BHJ and thermal stability analysis
The results are shown in Figure 4 by being obtained to the BET of MAMC materials analysis and pore analysis, and the specific surface area of MAMC is about
For 62.583m2The pore analysis result of/g, material are Pore Size=12.96nm, in a nitrogen environment, by changing pressure
And the adsorption and desorption curve of material is depicted using BJH methods, it can obviously observe hysteresis loop at 0.63P/P0Place occurs, compared with
High relative pressure region MAMC does not show any absorption limitation, illustrates that MAMC is that a kind of absorption property is superior, gap and ratio
The more flourishing mesoporous material in surface;
The MAMC materials for taking 3.2mg embodiments to prepare, in a nitrogen environment with the heating rate test material of 10 DEG C/min
Thermal stability, the results are shown in Figure 5, at a temperature of 0 DEG C~300 DEG C be pyrolyzed phenomenon it is more gentle, material still keeps preferable
Thermal stability, but sodium alginate embedding forerunner is volatilized by thermal decomposition when temperature reaches 400 DEG C or more, causes the pyrolysis speed of material
Rate increases.
1.5MAMC material regenerations are analyzed
MAMC materials of the NaOH to absorption As (III) and As (V) of 0.01mol/L, 0.1mol/L, 1mol/L is respectively adopted
It is desorbed and is regenerated, the results showed that use the NaOH of 0.1mol/L ideal as the desorption and actified solution of material, material
Material is maintained to 90% and 60% or more the removal effect of As (III) and As (V) after carrying out four desorptions, it was demonstrated that
MAMC can realize multiple recycling, be preferable green sorbing material.
The above embodiments and description only illustrate the principle of the present invention and most preferred embodiment, is not departing from this
Under the premise of spirit and range, various changes and improvements may be made to the invention, these changes and improvements both fall within requirement and protect
In the scope of the invention of shield.
Claims (3)
1. a kind of preparation method of the mesoporous carbosphere of magnetic ferric alginate of adsorbable heavy metal element, which is characterized in that including
Following steps:
S1 the sodium alginate for being configured to 2%~4% in deionized water), will be dissolved under the conditions of sodium alginate powder heating bath to be saturated
Solution, it is for use after cooling;
S2 the urea (urea) of certain mass), is added in sodium alginate saturated solution, magnetic agitation 10~40min postcoolings obtain
It is for use to SAC precursor solutions;
S3), nine water ferric nitrate solid powders are dissolved in deionized water, are configured to 5%~10% iron nitrate solution, then
SAC precursor solutions are added dropwise in iron nitrate solution with the rate of 20 drops/min under agitation, when SAC precursor solutions
The little particle of drops can be formed when encountering iron nitrate solution, the ripples whirlpool that magnetic stirring apparatus is formed can be the little particle of formation
Screw in solution bottom, it is ensured that the particle being subsequently formed does not generate adhesion phenomenon;
S4 it), seals after completion of the reaction, and places and be aged 48h at room temperature, take out the particulate matter of formation after ageing, and
It is cleaned 12~15 times with deionized water collocation ultrasonic cleaner, until cleaning oozes middle detection without Fe3+Exudation;
S5), material is put into vacuum freeze dryer after cleaning completely and is freeze-dried 48h, obtains moisture free yellowish-brown
Solid particle (SA@Fe Particles);
S6), SA@Fe particles are positioned in tube furnace, are heated up according to the heating rate of 1 DEG C/min under conditions of being passed through nitrogen
To 300 DEG C, and Heat preservation 3h, the mesoporous carbosphere of magnetic ferric alginate (MAMC) is then obtained after natural cooling.
2. a kind of preparation side of the mesoporous carbosphere of magnetic ferric alginate of adsorbable heavy metal element according to claim 1
Method, it is characterised in that:Step S1) in, the pure grade of chemistry of the sodium alginate powder is (viscosity (10g/L) >=0.02Pa
s)。
3. a kind of preparation side of the mesoporous carbosphere of magnetic ferric alginate of adsorbable heavy metal element according to claim 1
Method, it is characterised in that:Step S2) in, the urea (urea) of addition is 1 with the mass ratio of sodium alginate:1.
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