CN106362690A - Magnetic biochar adsorbing material and preparation method thereof - Google Patents
Magnetic biochar adsorbing material and preparation method thereof Download PDFInfo
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- CN106362690A CN106362690A CN201610928550.9A CN201610928550A CN106362690A CN 106362690 A CN106362690 A CN 106362690A CN 201610928550 A CN201610928550 A CN 201610928550A CN 106362690 A CN106362690 A CN 106362690A
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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
- B01J20/20—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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- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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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
- C02F1/48—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
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/485—Plants or land vegetals, e.g. cereals, wheat, corn, rice, sphagnum, peat moss
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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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
- C02F2101/20—Heavy metals or heavy metal 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention discloses a magnetic biochar adsorbing material and a preparation method thereof. The preparation method comprises the following steps: (1) preparation of biochar: by using powder obtained by treating plant biomass as a raw material, roasting under oxygen-free conditions to obtain porous biochar; (2) preparation of ferric iron precursor liquid: by using ethanediol as a dispersing agent, adding a solid-state ferric iron salt, continuing adding sodium acetate and a surfactant into the ethanediol, and stirring to form a disperse system which is the ferric iron precursor liquid; and (3) solvothermal reaction: uniformly mixing the biochar and ferric iron precursor solution to obtain a mixture, putting the mixture into a teflon hydrothermal reaction kettle, and carrying out solvothermal reaction to obtain the magnetic biochar adsorbing material. The pretreatment technique of the key biomass raw material and the specific conditions of solvothermal reaction in the preparation method are improved, thereby effectively solving the problem of poor connection stability between the magnetic biochar material magnetic particles and biomass.
Description
Technical field
The invention belongs to waste process field, more particularly, to a kind of magnetic bio charcoal adsorbing material and its preparation side
Method, is particularly suited for being recycled of plant base waste material (such as plant biomass, such as agriculture and forestry organic waste material), the magnetic preparing
Property charcoal can be applied as adsorbing material.
Background technology
Agriculture and forestry organic waste material mainly includes fruit residue, bark, straw, rice husk etc., is the plant of one of three major types biomass
The important ingredient of biomass (other two big biolobic materials are respectively animal organism matter and microbial biomass).China
Every year produce substantial amounts of agriculture and forestry organic waste material, in vast rural area, these garbages are mainly used in directly burning heat production, also one
Divide as feedstuff, fertilizer and pulping paper industry raw material, but the 50% of shared utilization rate deficiency agriculture and forestry organic waste material, still have big every year
Part agriculture and forestry organic waste material is thrown aside in natural environment or open incineration, causes the very big of resource while causing environmental pollution again
Waste.The fossil resources such as oil, coal are a large amount of to consume caused crisis of resource so that by Renewable resources such as agriculture and forestry organic waste materials
Become a kind of new development trend for commercial production, more and more particularly developed country of country is biological agricultural
The trans-utilization of the Renewable resources such as matter lists the grand strategy of Sustainable Socioeconomic Development in.
By agriculture and forestry organic waste material resource conversion be industrial chemicals or infant industry material has two ways: one kind is by agriculture woods
Garbage is separately converted to industrial products after being separated into cellulose, hemicellulose and lignin, and this method transformation efficiency is high, agriculture
Woods garbage can obtain maximum higher value application, but complex operation, and technique is loaded down with trivial details；Another kind is by agriculture and forestry organic waste material
All components are converted into industrial products, this mode can not only Simplified flowsheet, reduce production cost, and can reduce
The ambient pressure bringing during agriculture and forestry organic waste material Component seperation.Agriculture and forestry organic waste material can be used for removing industry as biological adsorption agent
Greasy dirt, heavy metal ion in waste water, organic pollution and radioactive wastewater can also be processed it might even be possible to for from sea water return
Receive precious metal, application prospect is very wide.Recently as the progress faster of industrial fast development and urban modernization, ring
Border pollution problem is more serious, and the environmental disaster property wherein being caused by heavy metal pollution is severe, has caused each side's concern.Logical
Cross using economical, effectively, the method for environmental protection to administer heavy metal pollution has become the important subject of current water treatment field.
Adsorption capacity is little, stability is poor, be difficult to long-term directly to apply agriculture and forestry organic waste material to exist as heavy-metal adsorption material
The shortcoming preserving, it is a kind of conventional method of modifying that waste biomass carry out activation to be prepared charcoal.But, in order to ensure relatively
Bigger serface, the charcoal of activation preparation mostly is powder, and particle diameter is little, mechanical strength is low, and it is solid in actual application
Liquid separating difficulty is big, recycle high cost, limits the scale application of charcoal adsorbing material.
The magnetic bio charcoal prepared in conjunction with magnetic separation technique can realize biological adsorption agent in the presence of externally-applied magnetic field
Sharp separation, improve sewage disposal efficiency, be a kind of new adsorbing material.Prepared by the magnetic bio carbon adsorbent of report
Method includes infusion process, covalent cross-linking method, cladding process and chemical coprecipitation.Patent cn103480331a and patent
Cn104258823a using infusion process, agriculture and forestry organic waste material is immersed in ferric ion solutions and then roasting obtains under anaerobic
Magnetic carbon material.Patent cn103316636a prepares activated carbon with biomass for raw material, and the activated carbon after pickling is immersed in
In advance in the ferroso-ferric oxide solution of preparation, by adsorption, ferroso-ferric oxide is adsorbed on activated carbon and obtains magnetic charcoal.
Agriculture and forestry organic waste material is loaded by patent cn104028214a with ferric ion ultrasonic mixing, after adding sodium hydroxide pellets, through low
The hot carburizing reagent of warm water obtains the carbon-based magnetic adsorptive material of biomass.Patent cn101314123a is by magnetic nano-particle and yellow spore
Raw wool flat lead fungi mycopowder mixture is added in sodium alginate soln, obtains magnetic bio absorption by embedding the method solidifying
Agent.
All there is different degrees of limitation in these methods above-mentioned: infusion process relies on the thing between magnetic particle and biomass
The connection stability that reason absorption is formed is not good；Covalent cross-linking method operating condition is complicated, and can consume adsorbing material surface sense
Group, reduces material absorption property；Cladding process needs to add the admixtures such as sodium alginate as embedding medium；Chemical coprecipitation should
With extensive but in preparation process, easily blocking biomaterial pore structure reduces specific surface area, and magnetic core less stable.
Content of the invention
Disadvantages described above for prior art or Improvement requirement, it is an object of the invention to provide a kind of magnetic bio charcoal is inhaled
Enclosure material and preparation method thereof, wherein by anti-to the pre-treating technology of crucial biomass material in preparation method, solvent thermal
The actual conditions (including the composition of presoma and proportioning, type of solvent, reaction temperature and time etc.) answered improves, and existing
Technology is compared and be can effectively solve the problem that and couple the not good problem of stability between magnetic bio Carbon Materials magnetic particle and biomass, and
And this magnetic bio charcoal adsorbing material has good absorption property, separating rate is fast.
For achieving the above object, according to one aspect of the present invention, there is provided a kind of system of magnetic bio charcoal adsorbing material
Preparation Method is it is characterised in that comprise the following steps:
(1) preparation of charcoal:
The powder being obtained through dried and break process with plant biomass as raw material, 200 DEG C～1000
DEG C oxygen free condition under roasting 1h～4h, obtain cavernous charcoal；
(2) preparation of ferric iron precursor liquid:
With ethylene glycol as dispersant, in this ethylene glycol add solid-state trivalent iron salt, make described trivalent iron salt with described
The solid masses of ethylene glycol is 1:(20～100 with the ratio of liquid volume) mg/l, then in this ethylene glycol, continuously add acetic acid
Sodium and surfactant, form disperse system after stirring, this disperse system is ferric iron precursor liquid；In this disperse system, described ferric iron
Salt, described Sodium Acetate Trihydrate are 1:12:(3.5～21 with the mass ratio of described surfactant three)；
(3) solvent thermal reaction prepares magnetic bio charcoal adsorbing material:
The described ferric iron precursor liquid that the described charcoal that described step (1) is obtained is obtained with described step (2)
Mix homogeneously obtains mixture, and charcoal described in this mixture is (0.5～10) with the mass ratio of ferrum element: 1；Then, will
Described mixture is placed in politef hydrothermal reaction kettle, and carries out solvent thermal reaction 8h～12h at 200 DEG C, obtains
Solvent hot is magnetic bio charcoal adsorbing material.
As present invention further optimization, in described step (1), described plant biomass is carrying out described dried
Front also have passed through carrying out washing treatment；The mesh number of described powder is not less than 60 mesh；Preferably, described plant biomass is discarded for agricultural
Thing；Preferably, described agriculture and forestry organic waste material is straw, bark, peel, pit, fallen leaves, Pericarppium arachidis hypogaeae, corn cob, sawdust, bagasse
In at least one.
As present invention further optimization, in described step (1), described roasting is carried out at 500 DEG C.
As present invention further optimization, in described step (2), described trivalent iron salt is iron chloride, iron sulfate, nitric acid
At least one in ferrum；Described trivalent iron salt and the solid masses of described ethylene glycol are 1:60mg/l with the ratio of liquid volume.
As present invention further optimization, in described step (2), described surfactant is Polyethylene Glycol, poly- diformazan
At least one in base diallyl ammonium chloride, sodium citrate.
As present invention further optimization, in described step (3), described solvent hot be through separation, washing and
At least 6h is dried at 60 DEG C, thus obtaining described magnetic bio charcoal adsorbing material.
As present invention further optimization, in described step (3), charcoal described in described mixture and ferrum element
Mass ratio is 5.5:1；The time of described solvent thermal reaction is 10h.
As present invention further optimization, in described step (2), the described Sodium Acetate Trihydrate of addition is anhydrous sodium acetate.
It is another aspect of this invention to provide that the invention provides the magnetic bio charcoal being prepared using above-mentioned preparation method
Adsorbing material.
By the contemplated above technical scheme of the present invention, compared with prior art, due to magnetic is prepared using solvent-thermal method
Property biological carbon materials, are the anaerobic calcination process by primitive organism material (i.e. plant biomass) under uniform temperature first
Obtain charcoal, prepare ferric iron precursor liquid simultaneously, and control trivalent iron salt in this ferric iron precursor liquid, Sodium Acetate Trihydrate, surface to live
Property agent and ethylene glycol ratio, then charcoal and this ferric iron precursor liquid are mixed to get solvent thermal reaction by a certain percentage
Presoma, by the overall co-ordination of each step of preparation method so that prepared magnetic bio Carbon Materials have good steady
Qualitative and adsorption effect.Although solvent-thermal method is widely used in magnetic Nano material synthesis, easy and simple to handle, formed material
Can be homogeneous, but yet there are no report using the research that this method prepares magnetic biological adsorption agent；The present invention adopts solvent thermal anti-
Should, by solvent thermal reaction condition (including composition and proportioning, type of solvent, solvent thermal reaction temperature and time etc. of presoma)
Cooperating and other steps such as pre-treating technology of biomass between, can be successfully prepared out magnetic by solvent-thermal method
Biological adsorption agent, has good stability and absorption property, overcomes the limitation of traditional method.
The magnetic bio charcoal adsorbing material that the present invention is obtained includes the charcoal skeleton of three-dimensional porous structure and is attached to life
Nanometer Fe 3 O 4 magnetic particle on thing charcoal skeleton.The present invention is to activate into agriculture and forestry organic waste material to have three-dimensional porous structure
Charcoal, using biological carbon surface enrich functional group absorption, chelating fe3+, and it is translated into fixation under a reducing atmosphere
Nanometer fe on charcoal skeleton3o4Particle, technological operation is simple.Compared to chemical coprecipitation, the nanometer being loaded
fe3o4Magnetic particle is homogeneous with reference to stablizing pattern, and crystalline phase purity is high, excellent magnetic.Rely on the modification of surfactant, magnetic
The stability of core is all improved with the absorption property of adsorbent.
The magnetic bio Carbon Materials that the present invention prepares, combine absorption property and the magnetic ferroferric oxide of charcoal
Magneto separate characteristic, heavy metal ion has the advantages that adsorption efficiency is high and sharp separation, has extensively in heavy metal process field
Wealthy application prospect.
Specifically, the present invention can obtain following beneficial effect:
(1) preparation method of the magnetic bio charcoal adsorbing material that the present invention provides, is prepared for raw material using agriculture and forestry organic waste material
Charcoal mix with the precursor liquid of trivalent iron salt through solvent thermal reaction be obtained, low cost, adsorbing material easy and simple to handle, prepared
Pattern is good, and structure is excellent, and charcoal is combined closely with nano ferriferrous oxide granule, relies on the modification of surfactant to make
With magnetic core stable performance.
(2) the magnetic bio charcoal adsorbing material that the present invention provides, low cost, adsorption efficiency are high, separating rate is fast, have wide
Application prospect, can be used for the removal of heavy metal ions in wastewater, dyestuff, pigment etc..
Brief description
Fig. 1 is the mechanism schematic diagram of solvent structure magnetic bio adsorbing material of the present invention；
Fig. 2 is Folium firmianae charcoal (i.e. using Folium firmianae as the plant biomass raw material of reaction, after anaerobic calcination process
The charcoal obtaining) sem image (amplification of this sem image be 2500 times)；
Fig. 3 is that (amplification of this sem image is the magnetic Folium firmianae biological adsorption material sem image that is obtained of the present invention
10000 times)；
Fig. 4 is the xrd collection of illustrative plates of the Folium firmianae magnetic bio charcoal adsorbing material prepared by embodiment 1；
Fig. 5 is that the magnetic Folium firmianae biological adsorption material Magneto separate process that the present invention is obtained is illustrated.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, below in conjunction with drawings and Examples, right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only in order to explain the present invention, not
For limiting the present invention.As long as additionally, involved technical characteristic in each embodiment of invention described below that
The conflict of not constituting between this just can be mutually combined.
The preparation method of magnetic bio charcoal adsorbing material in the present invention, comprises the following steps:
(1) prepare charcoal: scrubbed, dry, broken, 60 mesh sieves excessively with plant biomass (e.g., agriculture and forestry organic waste material)
Powder is raw material, and under 200-1000 DEG C of oxygen free condition, calcination activation is processed, and roasting time controls in 1-4h, obtains biology
Charcoal.
(2) prepare ferric iron precursor liquid: trivalent iron salt is dissolved in ethylene glycol by magnetic agitation, trivalent iron salt and ethylene glycol
Solid masses and the ratio of liquid volume be 1:(20-100) between (unit mg/l), preferably 1:60, be subsequently added Glacial acetic acid
Sodium and surfactant, the homogeneous ferric iron precursor liquid of continuously stirred formation, trivalent iron salt in described precursor liquid: Glacial acetic acid
Sodium: the mass ratio of surfactant controls between 1:12:3.5-21.
(3) solvent thermal reaction prepares magnetic bio charcoal: charcoal and emulsion fully mix formation mixture, described mixing
In thing, the mass ratio of charcoal and ferrum element is (10-0.5): between 1；
Then, this mixture is poured in politef hydrothermal reaction kettle, solvent thermal reaction 8-12h at 200 DEG C, reaction
After the completion of natural cooling, the separated washing of the product obtaining, be placed in and 6h be dried in 60 DEG C in vacuum drying oven and obtain magnetic bio
Charcoal.
Mainly there is nucleation at high temperature by solvent-thermal method in the magnetic bio adsorbing material that above-mentioned preparation method obtains
Reaction makes fe3o4Particle growth is formed in biological carbon surface, and its mechanism is as shown in Figure 1.Because biological carbon surface contains
There are the functional groups such as a large amount of carboxyls, hydroxyl, the fe that can adsorb, chelate in ferric iron precursor liquid3+.And ethylene glycol is that kind is high boiling
Reproducibility solvent, can adsorb the fe in biological carbon surface under the synergism of anhydrous sodium acetate with partial reduction during high temperature3+And
Form fe on its surface3o4Nano microcrystalline.Additionally, anhydrous sodium acetate is added in reaction system as electrostatic stabilization agent, on surface
The growth course of crystal can be controlled under activating agent synergism, prevent nano microcrystalline in course of reaction from extensive reunion occurring,
Meanwhile, surface modification is carried out to nanoparticle by surfactant, lift its stability.Liter with reaction temperature
Height, nano microcrystalline constantly growth the final good fe of pattern rule, magnetic on charcoal area load3o4Nanoparticle.
It is below specific embodiment
Embodiment 1
The preparation method and applications example of the magnetic bio charcoal adsorbing material in the present embodiment, comprises the following steps:
(1) prepare charcoal: agriculture and forestry organic waste material is the Firmiana platanifolia (Linn. f.) Marsili fallen leaves collected in campus, scrubbed, dry, broken, mistake 60
Powder after mesh is raw material, is placed in Muffle furnace roasting 2h under 500 DEG C of oxygen free conditions, obtains Folium firmianae charcoal, Fig. 2 is
Its sem image.
(2) prepare ferric iron precursor liquid: take 2.7g fecl3·6h2O is dissolved in 80ml ethylene glycol solution, subsequently thereto
Add 7.2g anhydrous sodium acetate and 2g Polyethylene Glycol (molecular weight is 4000), by the continuously stirred 30min of magnetic agitation so as to shape
Become homogeneous emulsion.
(3) solvent thermal reaction prepares magnetic bio charcoal: adds 0.77g Firmiana platanifolia (Linn. f.) Marsili base charcoal toward above-mentioned emulsion, by magnetic
Power stirs 2h, so that charcoal is fully mixed with emulsion.
(4) emulsion after mixing is poured in 100ml politef hydrothermal reaction kettle, at room temperature with 3 DEG C/min
Heating rate make in-furnace temperature after rising to 200 DEG C, react 10h at such a temperature, it is natural that reaction terminates rear equal solvent thermal response kettle
Cooling, by Magneto separate acquisition magnetic bio charcoal and multiple with ethanol and deionized water wash, finally magnetic bio charcoal is placed in
6h is dried in vacuum drying oven and obtains magnetic bio charcoal adsorbing material at 60 DEG C.Due to charcoal and ferrum element matter in solvent thermal reaction
Amount ratio only 1.375, its surface fe3o4Load capacity is higher, and Fig. 3 is its sem image.Analyze the crystalline substance of gained adsorbing material by xrd
Type, result is as shown in figure 4, wherein 6 main peaks are the fe of inverse spinel structure3o4(jcpds 75-1609), sample noise
Larger, show to contain amorphous charcoal composition in sample.
(5) take the magnetic bio charcoal adsorbing material 20mg of preparation in 10ml concentration be 50mg/l cr (vi) solution in,
Static adsorption 24h under room temperature, carries out solid-liquid separation operation by externally-applied magnetic field, as shown in Figure 5.And pass through spectrophotometry
The adsorption rate of cr (vi) in solution during different adsorption time, obtains magnetic bio charcoal adsorbing material and the balance of cr (vi) ion is inhaled
Attached clearance is 87.5%.
Embodiment 2
The preparation method and applications example of the magnetic bio charcoal adsorbing material in the present embodiment, comprises the following steps:
(1) prepare charcoal: agriculture and forestry organic waste material is the Firmiana platanifolia (Linn. f.) Marsili fallen leaves collected in campus, scrubbed, dry, broken, mistake 60
Powder after mesh is raw material, is placed in Muffle furnace roasting 2h under 500 DEG C of oxygen free conditions, obtains Folium firmianae charcoal.
(2) prepare ferric iron precursor liquid: take 2.7g fecl3·6h2O is dissolved in 80ml ethylene glycol solution, subsequently thereto
Add 7.2g anhydrous sodium acetate and 2g Polyethylene Glycol (molecular weight is 4000), by the continuously stirred 30min of magnetic agitation so as to shape
Become homogeneous emulsion.
(3) solvent thermal reaction prepares magnetic bio charcoal: adds 1.54g Firmiana platanifolia (Linn. f.) Marsili base charcoal toward above-mentioned emulsion, by magnetic
Power stirs 2h, so that charcoal is fully mixed with emulsion.
(4) emulsion after mixing is poured in 100ml politef hydrothermal reaction kettle, at room temperature with 3 DEG C/min
Heating rate make in-furnace temperature after rising to 200 DEG C, react 10h at such a temperature, it is natural that reaction terminates rear equal solvent thermal response kettle
Cooling, by Magneto separate acquisition magnetic bio charcoal and multiple with ethanol and deionized water wash, finally magnetic bio charcoal is placed in
6h is dried in vacuum drying oven and obtains magnetic bio charcoal adsorbing material at 60 DEG C.
(5) take the magnetic bio charcoal adsorbing material 20mg of preparation in 10ml concentration be 50mg/l cr (vi) solution in,
Static adsorption 24h under room temperature, carries out solid-liquid separation operation by externally-applied magnetic field.And when relying on the different absorption of spectrophotometry
Between when solution in cr (vi) adsorption rate, obtaining magnetic bio charcoal adsorbing material to the equilibrium adsorption rate of cr (vi) ion is
83.7%.
Embodiment 3
The preparation method and applications example of the magnetic bio charcoal adsorbing material in the present embodiment, comprises the following steps:
(1) prepare charcoal: agriculture and forestry organic waste material is the Semen Ginkgo fallen leaves collected in campus, scrubbed, dry, broken, mistake 60
Powder after mesh sieve is raw material, is placed in Muffle furnace roasting 2h under 500 DEG C of oxygen free conditions, obtains Folium Ginkgo charcoal.
(2) prepare ferric iron precursor liquid: take 2.7g fecl3·6h2O is dissolved in 80ml ethylene glycol solution, subsequently thereto
Add 7.2g anhydrous sodium acetate and 2g Polyethylene Glycol (molecular weight is 4000), by the continuously stirred 30min of magnetic agitation so as to shape
Become homogeneous emulsion.
(3) solvent thermal reaction prepares magnetic bio charcoal: adds 1.54g Firmiana platanifolia (Linn. f.) Marsili base charcoal toward above-mentioned emulsion, by magnetic
Power stirs 2h, so that charcoal is fully mixed with emulsion.
(4) emulsion after mixing is poured in 100ml politef hydrothermal reaction kettle, at room temperature with 3 DEG C/min
Heating rate make in-furnace temperature after rising to 200 DEG C, react 10h at such a temperature, it is natural that reaction terminates rear equal solvent thermal response kettle
Cooling, by Magneto separate acquisition magnetic bio charcoal and multiple with ethanol and deionized water wash, finally magnetic bio charcoal is placed in
6h is dried in vacuum drying oven and obtains magnetic bio charcoal adsorbing material at 60 DEG C, mean diameter is about 570nm.Solvent thermal reaction
Middle charcoal is 2.75 with ferrum element mass ratio, and the nanoparticle of load tails off.
(5) take the magnetic bio charcoal adsorbing material 20mg of preparation in 10ml concentration be 50mg/l cr (vi) solution in,
Static adsorption 24h under room temperature, carries out solid-liquid separation operation by externally-applied magnetic field.And when relying on the different absorption of spectrophotometry
Between when solution in cr (vi) adsorption rate, obtaining magnetic bio charcoal adsorbing material to the equilibrium adsorption rate of cr (vi) ion is
80.4%.
Embodiment 4
The preparation method and applications example of the magnetic bio charcoal adsorbing material in the present embodiment, comprises the following steps:
(1) prepare charcoal: agriculture and forestry organic waste material is the Firmiana platanifolia (Linn. f.) Marsili fallen leaves collected in campus, scrubbed, dry, broken, mistake 60
Powder after mesh is raw material, is placed in Muffle furnace roasting 2h under 500 DEG C of oxygen free conditions, obtains Folium firmianae charcoal.
(2) prepare ferric iron precursor liquid: take 2.7g fecl3·6h2O is dissolved in 160ml ethylene glycol solution, subsequently thereto
Add 7.2g anhydrous sodium acetate and 2g Polyethylene Glycol (molecular weight is 4000), by the continuously stirred 30min of magnetic agitation so as to shape
Become homogeneous emulsion.
(3) solvent thermal reaction prepares magnetic bio charcoal: adds 0.77g Firmiana platanifolia (Linn. f.) Marsili base charcoal toward above-mentioned emulsion, by magnetic
Power stirs 2h, so that charcoal is fully mixed with emulsion.
(4) emulsion after mixing is poured in 100ml politef hydrothermal reaction kettle, at room temperature with 3 DEG C/min
Heating rate make in-furnace temperature after rising to 200 DEG C, react 10h at such a temperature, it is natural that reaction terminates rear equal solvent thermal response kettle
Cooling, by Magneto separate acquisition magnetic bio charcoal and multiple with ethanol and deionized water wash, finally magnetic bio charcoal is placed in
6h is dried in vacuum drying oven and obtains magnetic bio charcoal adsorbing material at 60 DEG C.Compared to embodiment 3, due to fe in solution3+
Molar concentration reduces, and magnetic particle mean diameter is about 370nm.
(5) take the magnetic bio charcoal adsorbing material 20mg of preparation in 10ml concentration be 50mg/l cr (vi) solution in,
Static adsorption 24h under room temperature, carries out solid-liquid separation operation by externally-applied magnetic field.And when relying on the different absorption of spectrophotometry
Between when solution in cr (vi) adsorption rate, obtaining magnetic bio charcoal adsorbing material to the equilibrium adsorption rate of cr (vi) ion is
93.8%.
Table 1 various embodiments of the present invention experiment parameter catalog
Each embodiment result shows the magnetic bio charcoal adsorbing material pattern synthesizing under different condition by solvent thermal reaction
Well, structure is excellent, and charcoal is combined closely with nano ferriferrous oxide granule, stable performance, has excellent suction to cr (vi)
Attached effect.Table 1 is design parameter and the experimental result catalog of various embodiments above, the result table of embodiment 1 and embodiment 2
Bright, charcoal is different with the ratio of ferrum element, magnetic fe of charcoal area load3o4Nanoparticle quantity has differences, suitably
Improve ferrum element ratio and be conducive to the adsorption efficiency to cr (vi) for the adsorbing material；Comparative example 1 and embodiment 3 it is found that
Different biological material surface functional group quantity, property have differences, the suction to cr (vi) for the magnetic adsorptive material thus prepared
There is difference in attached effect；With respect to embodiment 1, the adsorbing material of embodiment 4 is higher to the adsorption efficiency of cr (vi), this be due to
Fe in ferric iron precursor liquid in embodiment 43+Concentration is relatively low, the fe being consequently formed3o4Particle diameter diminishes, lead to adsorbing material integrally than
Surface area becomes big, lifts adsorption efficiency.
In the present invention, the preparation process of charcoal can be mutual with the preparation process order of ferric iron precursor liquid, both permissible
First prepare charcoal, prepare ferric iron precursor liquid again it is also possible to first preparing ferric iron precursor liquid, preparing charcoal again.The present invention
In oxygen free condition can be under vacuum or protective atmosphere (as nitrogen atmosphere or inert gas atmosphere).Used in the present invention
Surfactant can include the Polyethylene Glycol of different molecular weight, PDDA, sodium citrate.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, not in order to
Limit the present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc., all should comprise
Within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of magnetic bio charcoal adsorbing material is it is characterised in that comprise the following steps:
(1) preparation of charcoal:
The powder being obtained through dried and break process with plant biomass as raw material, at 200 DEG C～1000 DEG C
Under oxygen free condition, roasting 1h～4h, obtains cavernous charcoal；
(2) preparation of ferric iron precursor liquid:
To in this ethylene glycol, with ethylene glycol as dispersant, add the trivalent iron salt of solid-state, make described trivalent iron salt and described second two
The ratio of the solid masses of alcohol and liquid volume is 1:(20～100) mg/l, then continuously add in this ethylene glycol Sodium Acetate Trihydrate and
Surfactant, forms disperse system after stirring, this disperse system is ferric iron precursor liquid；In this disperse system, described trivalent iron salt, institute
The mass ratio stating Sodium Acetate Trihydrate with described surfactant three is 1:12:(3.5～21)；
(3) solvent thermal reaction prepares magnetic bio charcoal adsorbing material:
The described charcoal that described step (1) is obtained is mixed with the described ferric iron precursor liquid that described step (2) obtains
Uniformly obtain mixture, charcoal described in this mixture is (0.5～10) with the mass ratio of ferrum element: 1；Then, will be described
Mixture is placed in politef hydrothermal reaction kettle, and carries out solvent thermal reaction 8h～12h, the solvent obtaining at 200 DEG C
Hot is magnetic bio charcoal adsorbing material.
2. the preparation method of magnetic bio charcoal adsorbing material as claimed in claim 1 is it is characterised in that in described step (1), institute
State plant biomass and also have passed through carrying out washing treatment before carrying out described dried；The mesh number of described powder is not less than 60 mesh；Excellent
Choosing, described plant biomass is agriculture and forestry organic waste material；Preferably, described agriculture and forestry organic waste material is straw, bark, peel, pit, falls
At least one in leaf, Pericarppium arachidis hypogaeae, corn cob, sawdust, bagasse.
3. the preparation method of magnetic bio charcoal adsorbing material as claimed in claim 1 is it is characterised in that in described step (1), institute
State roasting to carry out at 500 DEG C.
4. the preparation method of magnetic bio charcoal adsorbing material as claimed in claim 1 is it is characterised in that in described step (2), institute
State trivalent iron salt be iron chloride, iron sulfate, at least one in ferric nitrate；Described trivalent iron salt and the solid matter of described ethylene glycol
Amount is 1:60mg/l with the ratio of liquid volume.
5. the preparation method of magnetic bio charcoal adsorbing material as claimed in claim 1 is it is characterised in that in described step (2), institute
State surfactant be Polyethylene Glycol, PDDA, at least one in sodium citrate.
6. the preparation method of magnetic bio charcoal adsorbing material as claimed in claim 1 is it is characterised in that in described step (3), institute
Stating solvent hot is through separating, washing and at least 6h is dried at 60 DEG C, thus obtaining described magnetic bio charcoal adsorption material
Material.
7. the preparation method of magnetic bio charcoal adsorbing material as claimed in claim 1 is it is characterised in that in described step (3), institute
The mass ratio stating charcoal described in mixture with ferrum element is 5.5:1；The time of described solvent thermal reaction is 10h.
8. the preparation method of magnetic bio charcoal adsorbing material as claimed in claim 1 is it is characterised in that in described step (2), plus
The described Sodium Acetate Trihydrate entering is anhydrous sodium acetate.
9. the magnetic green being prepared using magnetic bio charcoal adsorbing material preparation method as described in claim 1-8 any one
Thing charcoal adsorbing material.
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