CN108404867A - A kind of lignin-base carbon magnetic Nano material and preparation method and the application in adsorbing methyl orange - Google Patents
A kind of lignin-base carbon magnetic Nano material and preparation method and the application in adsorbing methyl orange Download PDFInfo
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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
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
Abstract
The invention belongs to sorbent material technical field, a kind of lignin-base carbon magnetic Nano material and preparation method thereof and the application in adsorbing methyl orange are disclosed.Preparation method of the present invention includes the following steps：Ferrous sulfate and iron chloride is soluble in water, and ammonium hydroxide and hydrogen peroxide, 70~90 DEG C of 1~3h of heat preservation curing are added dropwise in preheating；In lignin liquor, short chain alcohol addition system, 1~3h of insulated and stirred；Separation, it is dry；500~650 DEG C of 3~4h of carbonization, cooling, crushing obtain lignin-base carbon magnetic Nano material under inert atmosphere.The method of the present invention with the lignin of abundance be for carbon source, it is cheap, not only reduce the production cost of magnetic material, and meet Green Sustainable strategy；It is combined by the way that high temperature cabonization is synchronous with high temperature reformation, the quality base carbon magnetic Nano material being prepared has the advantages that uniform particle diameter, the carbon amount of containing are big, strong to Adsorption of Methyl Orange ability, can be used for adsorbing in methyl orange.
Description
Technical field
The invention belongs to sorbent material technical field, more particularly to a kind of lignin-base carbon magnetic Nano material and its system
Preparation Method and the application in adsorbing methyl orange.
Background technology
In recent years, very active about the research of carbon nanomaterial, the carbon nanomaterial of various shapes emerges one after another.Carbon is received
Rice material is widely used in reinforcing fiber, thermal conductivity material, stealth material, hydrogen storage material, electrode material, super capacitor
Device, sorbing material, Water warfare catalytic carrier numerous areas, have excellent hardness, optical characteristics, heat resistance, radiation hardness characteristic,
Chemical-resistant resistance characteristic, electric conductivity, surface and interfacial characteristics etc..
Magnetic material due to excellent magnetic performance, be widely used in magnetic fluid, targeting medical treatment, adsorbing separation,
The fields such as nuclear magnetic resonance, trace detection.Scientific worker has carried out this large amount of research work both at home and abroad at present.
Xuan etc. prepares Fe3O4Then aniline is added in nano particle, cause aniline molecule in nanometer by initiator
Grain surface aggregate, is made Fe3O4/ polyaniline magnetic composite microsphere.This microballoon has the form of blueberry, then coats one on surface
After layer gold nanoparticle, there are special applications in catalytic field.Bhaumik etc. then utilizes pyrrole monomer oxidizable poly- in aqueous solution
It closes, pyrroles is aggregated in Fe3O4Nano grain surface.The magnetic particle of preparation is in Cr (VI) solution of the 200mg/L of pH=2
It may be implemented to adsorb Cr (VI) completely.Zhu etc. to methyl acrylate solution containing nano oxidized iron particle and styrene copolymerized,
Obtain the magnetic Nano microsphere that styrene-acrylic resin contains.Obtained high molecule magnetic microsphere is evenly distributed, the coupling of this magnetic microsphere
Primer strand can be used for detaching the probe of VEGF nucleic acid.
By carbon material with magnetic material by either physically or chemically being combined, will assign simultaneously new material with magnetic properties and
Carbon material characteristic, and the fields such as targeting medical treatment, catalysis, Magneto separate are can be applied to, but at present combined magnetic material with carbon material
The also rare report of research.
Lignin is the biological material that content is second largest on the earth.According to statistics, the whole world is produced by pulp and paper industry every year
Raw industrial lignin is more than 50,000,000 tons.In natural biological material, lignin molecule phosphorus content is high, is a kind of good
Carbon source.Studies have shown that the carbon material prepared by lignin can be used as electrode material, ultracapacitor, device material etc..But mesh
Before until, both at home and abroad using lignin major way be burning, small part it is modified be used as dispersion of industry agent.This mode is only
It is a kind of low value utilization, huge waste is caused to Liginon Resource, it is difficult to alleviates the contradiction of shortage of resources, also be unfavorable for society
Sustainable development.Currently, preparing the research report of carbon magnetic Nano material using lignin as carbon source not yet.
Invention content
The shortcomings that in order to overcome above-mentioned prior art lignin low value to utilize and deficiency, the primary purpose of the present invention is that carrying
For a kind of preparation method of lignin-base carbon magnetic Nano material.The method of the present invention is using lignin as carbon source, with Fe3O4Knot
Lignin-base carbon magnetic Nano material is prepared in conjunction, improves the surcharge of lignin, expands the application range of lignin, real
The recycling of existing lignin, the realization for the strategic objective that promotes sustainable development.
Another object of the present invention is to provide the lignin-base carbon magnetic Nano materials that the above method is prepared.
It is still another object of the present invention to provide above-mentioned lignin-base carbon magnetic Nano material answering in adsorbing methyl orange
With.
The purpose of the present invention is realized by following proposal：
A kind of preparation method of lignin-base carbon magnetic Nano material, includes the following steps：Ferrous sulfate and iron chloride
Soluble in water, ammonium hydroxide and hydrogen peroxide, 70~90 DEG C of 1~3h of heat preservation curing are added dropwise in preheating；Lignin liquor, short chain alcohol are added
Enter in system, 1~3h of insulated and stirred；Separation, it is dry；500~650 DEG C of 3~4h of carbonization, cooling, crushing obtain under inert atmosphere
Lignin-base carbon magnetic Nano material.
In the method for the present invention, the dosage of each component is formulated as follows, mass parts meter：2~5 parts of lignin, short chain alcohol 10~25
Part, 2.5~5 parts of ferrous sulfate, 3~6 parts of iron chloride, 10~20 parts of ammonium hydroxide, 1~5 part of hydrogen peroxide.
The lignin can be industrial lignin, such as alkali lignin, sodium lignin sulfonate, enzymolysis xylogen, lignin
At least one of sulfoacid calcium, sulfonated wheat-strew lignin.
The short chain alcohol can be at least one of methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol；
Preferably ethyl alcohol.
The temperature of the heat preservation curing is more preferably 80 DEG C.
The time of the heat preservation curing is more preferably 3h.
The concentration of ammonium hydroxide used is preferably 25%.
The concentration of hydrogen peroxide used is preferably 35%.
The ammonium hydroxide and hydrogen peroxide preferably sequentially add.
The speed of the dropwise addition is preferably 1 drop/sec.
The concentration of the lignin liquor is preferably 10~30wt%, more preferably 20wt%.
The time of the insulated and stirred is preferably 2h.
The lignin liquor, short chain alcohol are preferably added drop-wise in system.More preferably lignin liquor, short chain alcohol be simultaneously
It is added drop-wise in system.
The separation can carry out isolated magnetic-particle using magnet.
The isolated material can be washed using ethyl alcohol.
The temperature of the drying is preferably 50~70 DEG C, more preferably 60 DEG C.
Material of the present invention with the lignin of abundance be for carbon source, it is cheap, not only reduce the life of magnetic material
Cost is produced, and meets Green Sustainable strategy
The present invention also provides the lignin-base carbon magnetic Nano materials that the above method is prepared.Material of the present invention has grain
Diameter is uniform, the carbon amount of containing is big, the advantage strong to Adsorption of Methyl Orange ability.
The method of the present invention is combined by the way that high temperature cabonization is synchronous with high temperature reformation, and material is improved while obtaining carbon material
Magnetism, the more crucial regulation and control being to magnetic Nano material grain size improve its absorption property to methyl orange, can be used for adsorbing
In methyl orange.
The present invention compared with the existing technology, has the following advantages and advantageous effect：
(1) industrial lignin molecule is spacial framework, contains compared with polyfunctional group in molecular skeleton, is easy in magnetism
Nanoparticle surface forms firm connection, is conducive to the functionalization of nano particle；(2) by adjusting carburizing temperature, lignin carbon
Its surface still retains hydroxyl, carboxyl isoreactivity functional group after change, and its specific surface area is larger, has good absorption property；(3)
The present invention Fe that remaining functional group adsorbs methyl orange, and the precipitation method is utilized to prepare after not being carbonized merely with lignin molecule3O4
The inorganic O contained in particle2-、OH-Strong electrostatic interaction is formed etc. the polar group in highly polar ion, with methyl orange.Lignin
With Fe3O4Particle cooperative acts on, and further improves the absorption property to methyl orange；(4) pole of solution is adjusted by short chain alcohol
Property, using the industrial lignin characteristic that solubility reduces in nonpolar solvent, rationally increase lignin on magnetic-particle surface
The amount of containing, improve lignin-base magnetic Nano material application performance；(5) by high temperature cabonization technique, carbon material is being obtained
While also reformed the lattice structure of magnetic-particle, substantially increase the magnetism of material；(6) industrial lignin abundance,
It is cheap.Carbon magnetic Nano material is prepared using industrial lignin, greatly reduces the production cost of magnetic-particle, effectively profit
With renewable resource, there is environmentally protective advantage.
Description of the drawings
Fig. 1 is the infrared spectrum of the lignin-base carbon magnetic Nano material prepared by embodiment 1.
Fig. 2 is the XRD diagram of the lignin-base carbon magnetic Nano material prepared by embodiment 1.
Fig. 3 is the Raman spectrograms of the lignin-base carbon magnetic Nano material prepared by embodiment 1.
Fig. 4 is the SEM figures of the lignin-base carbon magnetic Nano material prepared by embodiment 1.
Fig. 5 is the hysteresis loop figure of the lignin-base carbon magnetic Nano material prepared by embodiment 1.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Material involved in the following example can be obtained from commercial channel.
Embodiment 1
2.5g ferrous sulfate and 3g iron chloride are dissolved in the water of 100mL, four-hole boiling flask is transferred to, rises under mechanical stirring
Temperature is successively slowly dropped into the 35%H of 25% ammonia spirit and 1g of 10g in order to 80 DEG C2O2, rate of addition is 1 drop/sec.Drop
After adding, 80 DEG C of heat preservation curing 1h.After 2g alkali lignins are dissolved into 10g aqueous solutions, dripped simultaneously together with 10g absolute ethyl alcohols
Enter in above-mentioned reaction system, rate of addition is 1 drop/sec, and rear insulated and stirred 2h is added dropwise.Finally magnetism is isolated with permanent magnet
Particle, ethyl alcohol are washed three times, are dried in vacuo at 60 DEG C.Take dry product in N2Be carbonized in atmosphere at 550 DEG C 3h, cooling
After grind, you can obtain lignin-base carbon magnetic nanoparticle.Prepared lignin-base carbon magnetic nanoparticle average grain diameter
About 140nm, BET specific surface area 252m2/g。
0.1g lignin-base carbon magnetic nanoparticles are taken to be added in the methyl orange solution of a concentration of 0.1g/L of 100mL,
It is placed at 25 DEG C on the fixed shaking table for shaking speed and shakes absorption.After absorption, by nano particle Magneto separate 5min in external magnetic field,
Supernatant liquor is taken, pH=2.0 is measured using ultra-violet absorption spectrum, the saturated extent of adsorption of methyl orange is 63.3mg/g at 20 DEG C.With
Material, the saturated extent of adsorption to the same terms Methyl Orange are only 25.3mg/g to commercially available lignin adsorbent as a comparison case.
Embodiment 2
5g ferrous sulfate and 6g iron chloride are dissolved in the water of 100mL, four-hole boiling flask is transferred to, heats up under mechanical stirring
To 70 DEG C, it is successively slowly dropped into the 35%H of 25% ammonia spirit and 5g of 20g in order2O2, rate of addition is 1 drop/sec.It is added dropwise
After, heat preservation curing 3h.After 5g sodium lignin sulfonates are dissolved into 50g aqueous solutions, instilled simultaneously together with 25g methanol above-mentioned
In reaction system, rate of addition is 1 drop/sec, and rear insulated and stirred 1h is added dropwise.Magnetic-particle finally is isolated with permanent magnet,
Ethyl alcohol washs three times, is dried in vacuo at 50 DEG C.Take dry product in N2Be carbonized in atmosphere at 500 DEG C 4h, is ground after cooling
It is broken, you can to obtain lignin-base carbon magnetic nanoparticle.Prepared lignin-base carbon magnetic nanoparticle average grain diameter is about
160nm, BET specific surface area 231m2/g。
0.1g lignin-base carbon magnetic nanoparticles are taken to be added in the methyl orange solution of a concentration of 0.1g/L of 100mL,
It is placed at 25 DEG C on the fixed shaking table for shaking speed and shakes absorption.After absorption, by nano particle Magneto separate 5min in external magnetic field,
Supernatant liquor is taken, pH=2.0 is measured using ultra-violet absorption spectrum, the saturated extent of adsorption of methyl orange is 59.9mg/g at 20 DEG C.With
Material, the saturated extent of adsorption to the same terms Methyl Orange are only 25.3mg/g to commercially available lignin adsorbent as a comparison case.
Embodiment 3
3g ferrous sulfate and 5g iron chloride are dissolved in the water of 100mL, four-hole boiling flask is transferred to, heats up under mechanical stirring
To 90 DEG C, it is successively slowly dropped into the H of 25% ammonia spirit and 3g of 15g in order2O2, rate of addition is 1 drop/sec.It is added dropwise
Afterwards, heat preservation curing 2h.After 4g enzymolysis xylogens are dissolved into 13g aqueous solutions, above-mentioned reaction is instilled simultaneously together with 20g normal propyl alcohols
In system, rate of addition is 1 drop/sec, and rear insulated and stirred 3h is added dropwise.Finally magnetic-particle, ethyl alcohol are isolated with permanent magnet
Washing three times, is dried in vacuo at 70 DEG C.Take dry product in N2Be carbonized in atmosphere at 650 DEG C 3.5h, is ground after cooling,
It can be obtained lignin-base carbon magnetic nanoparticle.Prepared lignin-base carbon magnetic nanoparticle average grain diameter is about
145nm, BET specific surface area 259m2/g。
0.1g lignin-base carbon magnetic nanoparticles are taken to be added in the methyl orange solution of a concentration of 0.1g/L of 100mL,
It is placed at 25 DEG C on the fixed shaking table for shaking speed and shakes absorption.After absorption, by nano particle Magneto separate 5min in external magnetic field,
Supernatant liquor is taken, pH=2.0 is measured using ultra-violet absorption spectrum, the saturated extent of adsorption of methyl orange is 56.3mg/g at 20 DEG C.With
Material, the saturated extent of adsorption to the same terms Methyl Orange are only 25.3mg/g to commercially available lignin adsorbent as a comparison case.
Embodiment 4
2.5g ferrous sulfate and 5g iron chloride are dissolved in the water of 100mL, four-hole boiling flask is transferred to, rises under mechanical stirring
Temperature is successively slowly dropped into the 35%H of 25% ammonia spirit and 4g of 10g in order to 85 DEG C2O2, rate of addition is 1 drop/sec.Drop
After adding, heat preservation curing 1h.After 3g calcium lignosulfonates are dissolved into 15g aqueous solutions, instilled simultaneously together with 15g isopropanols
In above-mentioned reaction system, rate of addition is 1 drop/sec, and rear insulated and stirred 2h is added dropwise.Finally magnetic is isolated with permanent magnet
Grain, ethyl alcohol are washed three times, are dried in vacuo at 50 DEG C.Take dry product in N2Be carbonized in atmosphere at 600 DEG C 3h, after cooling
It grinds, you can obtain lignin-base carbon magnetic nanoparticle.Prepared lignin-base carbon magnetic nanoparticle average grain diameter is about
For 155nm, BET specific surface area 222m2/g。
0.1g lignin-base carbon magnetic nanoparticles are taken to be added in the methyl orange solution of a concentration of 0.1g/L of 100mL,
It is placed at 25 DEG C on the fixed shaking table for shaking speed and shakes absorption.After absorption, by nano particle Magneto separate 5min in external magnetic field,
Supernatant liquor is taken, pH=2.0 is measured using ultra-violet absorption spectrum, the saturated extent of adsorption of methyl orange is 58.5mg/g at 20 DEG C.With
Material, the saturated extent of adsorption to the same terms Methyl Orange are only 25.3mg/g to commercially available lignin adsorbent as a comparison case.
Embodiment 5
5g ferrous sulfate and 6g iron chloride are dissolved in the water of 100mL, four-hole boiling flask is transferred to, heats up under mechanical stirring
To 75 DEG C, it is slowly dropped into 25% ammonia spirit of 20g and the 35%H of 2g in order2O2, rate of addition is 1 drop/sec.It is added dropwise
Afterwards, heat preservation curing 3h.After 5g sulfonated wheat-strew lignins are dissolved into 50g aqueous solutions, instilled simultaneously together with 25g n-butanols above-mentioned anti-
It answers in system, rate of addition is 1 drop/sec, and rear insulated and stirred 1h is added dropwise.Finally magnetic-particle, second are isolated with permanent magnet
Alcohol washs three times, is dried in vacuo at 70 DEG C.Take dry product in N2Be carbonized in atmosphere at 550 DEG C 3.5h, is ground after cooling
It is broken, you can to obtain lignin-base carbon magnetic nanoparticle.Prepared lignin-base carbon magnetic nanoparticle average grain diameter is about
125nm, BET specific surface area 301m2/g。
0.1g lignin-base carbon magnetic nanoparticles are taken to be added in the methyl orange solution of a concentration of 0.1g/L of 100mL,
It is placed at 25 DEG C on the fixed shaking table for shaking speed and shakes absorption.After absorption, by nano particle Magneto separate 5min in external magnetic field,
Supernatant liquor is taken, pH=2.0 is measured using ultra-violet absorption spectrum, the saturated extent of adsorption of methyl orange is 62.1mg/g at 20 DEG C.With
Material, the saturated extent of adsorption to the same terms Methyl Orange are only 25.3mg/g to commercially available lignin adsorbent as a comparison case.
Embodiment 6
4g ferrous sulfate and 5g iron chloride are dissolved in the water of 100mL, four-hole boiling flask is transferred to, heats up under mechanical stirring
To 70 DEG C, it is successively slowly dropped into the 35%H of 25% ammonia spirit and 1g of 12g in order2O2, rate of addition is 1 drop/sec.It is added dropwise
After, heat preservation curing 1h.After 3g alkali lignins are dissolved into 10g aqueous solutions, instilled simultaneously together with 15g isobutanols above-mentioned anti-
It answers in system, rate of addition is 1 drop/sec, and rear insulated and stirred 3h is added dropwise.Finally magnetic-particle, second are isolated with permanent magnet
Alcohol washs three times, is dried in vacuo at 50 DEG C.Take dry product in N2Be carbonized in atmosphere at 500 DEG C 4h, is ground after cooling,
It can be obtained lignin-base carbon magnetic nanoparticle.Prepared lignin-base carbon magnetic nanoparticle average grain diameter is about
168nm, BET specific surface area 199m2/g。
0.1g lignin-base carbon magnetic nanoparticles are taken to be added in the methyl orange solution of a concentration of 0.1g/L of 100mL,
It is placed at 25 DEG C on the fixed shaking table for shaking speed and shakes absorption.After absorption, by nano particle Magneto separate 5min in external magnetic field,
Supernatant liquor is taken, pH=2.0 is measured using ultra-violet absorption spectrum, the saturated extent of adsorption of methyl orange is 60.1mg/g at 20 DEG C.With
Material, the saturated extent of adsorption to the same terms Methyl Orange are only 25.3mg/g to commercially available lignin adsorbent as a comparison case.
The following table 1 is the elemental analysis of the lignin-base carbon magnetic Nano material prepared by embodiment 1.As shown in Table 1, implement
1 product of example also contains the elements such as N, H, S other than Fe, C element, this explanation is after high temperature cabonization appropriate, nano material
In can retain more active function groups, be conducive to subsequent modification or the absorption to organic matter.
The constituent content (/wt%) of 1 embodiment of table, 1 product
Fig. 1 is the infrared spectrum of 1 product of embodiment.Wherein, 3400cm-1Place is-OH absorption peaks, 2380cm-1The spike at place
For C-O stretching vibration peaks, 1203cm-1Place is C-C stretching vibration peaks, and 1720cm-1Place is the stretching vibration peak of Fe-O, 560cm-1The spike at place is Fe3O4Characteristic absorption peak.Infrared spectrum shows after high-temperature process, Fe3O4Crystal structure more advise
It is whole, and lignin can still retain certain functional group, and carbon material and Fe oxides after proper temperature is carbonized in its molecule
Between there is strong chemical bonds, therefore the carbon magnetic material prepared has stronger structure.
Fig. 2 is the XRD diagram of 1 product of embodiment.Wherein, the spike at 2 θ=30 ° of incidence angle, 37 °, 58 ° and 62 ° is
Fe3O4Diffraction maximum, the absorption peak at 2 θ=12 ° of incidence angle is the diffraction maximum of simple substance carbon.XRD spectra shows by high-temperature process
Afterwards, the more regular Fe of structure can be obtained3O4Crystal.
Fig. 3 is the Raman spectrum of 1 product of embodiment.It can be seen that ID/IG ratios are higher, illustrate after high temperature cabonization,
Carbon graphite degree is higher, is conducive to subsequent application.
Fig. 4 is that the SEM of 1 product of embodiment schemes.By in figure it will be evident that after high temperature, carbon magnetic Nano material shape
More regular, close to spherical shape, and grain diameter is more uniform, and specific surface area is larger, has good absorption property.
The hysteresis loop figure of 1 product of embodiment when Fig. 5 is T=300K.By in figure it is found that in T=300K embodiment 1
Product shows preferable superparamagnetism feature, and saturation magnetization 15.6emu/g has good magnetic responsiveness.This
Important premise is provided for subsequent application.
The properties of product of other embodiment are the same as embodiment 1.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of lignin-base carbon magnetic Nano material, it is characterised in that include the following steps：Ferrous sulfate
Soluble in water with iron chloride, ammonium hydroxide and hydrogen peroxide, 70~90 DEG C of 1~3h of heat preservation curing are added dropwise in preheating；Lignin liquor,
In short chain alcohol addition system, 1~3h of insulated and stirred；Separation, it is dry；500~650 DEG C of 3~4h of carbonization under inert atmosphere, cooling,
It crushes, obtains lignin-base carbon magnetic Nano material.
2. the preparation method of lignin-base carbon magnetic Nano material according to claim 1, it is characterised in that each component
Dosage is formulated as follows, mass parts meter：2~5 parts of lignin, 10~25 parts of short chain alcohol, 2.5~5 parts of ferrous sulfate, iron chloride 3~6
Part, 10~20 parts of ammonium hydroxide, 1~5 part of hydrogen peroxide.
3. the preparation method of lignin-base carbon magnetic Nano material according to claim 1, it is characterised in that：The wood
Quality is industrial lignin, including alkali lignin, sodium lignin sulfonate, enzymolysis xylogen, calcium lignosulfonate, sulfonation alkali are wooden
At least one of element.
4. the preparation method of lignin-base carbon magnetic Nano material according to claim 1, it is characterised in that：Described is short
Chain alcohol is at least one of methanol, ethyl alcohol, normal propyl alcohol, isopropanol, n-butanol, isobutanol.
5. the preparation method of lignin-base carbon magnetic Nano material according to claim 1, it is characterised in that：The heat preservation
The temperature of curing is 80 DEG C；The time of the heat preservation curing is 3h.
6. the preparation method of lignin-base carbon magnetic Nano material according to claim 1, it is characterised in that：Ammonium hydroxide used
A concentration of 25%；A concentration of the 35% of hydrogen peroxide used.
7. the preparation method of lignin-base carbon magnetic Nano material according to claim 1, it is characterised in that：It is described wooden
A concentration of 10~30wt% of plain solution.
8. the preparation method of lignin-base carbon magnetic Nano material according to claim 1, it is characterised in that：The heat preservation
The time of stirring is 2h；The temperature of the drying is 50~70 DEG C.
9. a kind of lignin-base carbon magnetic Nano material, it is characterised in that according to claim 1~8 any one of them preparation side
Method obtains.
10. application of the lignin-base carbon magnetic Nano material in adsorbing methyl orange described in claim 9.
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| CN109012590A (en) * | 2018-08-24 | 2018-12-18 | 华南理工大学 | A kind of lignin-base transition metal-nitrogen-doped carbon material and its preparation and application |
| CN109126746A (en) * | 2018-10-17 | 2019-01-04 | 北京林业大学 | A kind of preparation method of magnetism lignosulfonates adsorbent material |
| CN116618025A (en) * | 2023-05-25 | 2023-08-22 | 南京工业大学 | Novel bio-based adsorbent for selectively adsorbing anionic dye |
| CN117399022A (en) * | 2023-12-15 | 2024-01-16 | 河北唯沃环境工程科技有限公司 | Lignin-based composite catalytic material and preparation method and application thereof |
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| CN109012590A (en) * | 2018-08-24 | 2018-12-18 | 华南理工大学 | A kind of lignin-base transition metal-nitrogen-doped carbon material and its preparation and application |
| CN109012590B (en) * | 2018-08-24 | 2020-04-07 | 华南理工大学 | Lignin-based transition metal-nitrogen-doped carbon material and preparation and application thereof |
| CN109126746A (en) * | 2018-10-17 | 2019-01-04 | 北京林业大学 | A kind of preparation method of magnetism lignosulfonates adsorbent material |
| CN116618025A (en) * | 2023-05-25 | 2023-08-22 | 南京工业大学 | Novel bio-based adsorbent for selectively adsorbing anionic dye |
| CN117399022A (en) * | 2023-12-15 | 2024-01-16 | 河北唯沃环境工程科技有限公司 | Lignin-based composite catalytic material and preparation method and application thereof |
| CN117399022B (en) * | 2023-12-15 | 2024-03-08 | 河北唯沃环境工程科技有限公司 | Lignin-based composite catalytic material and preparation method and application thereof |
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