CN106219517A - A kind of magnetic carbon Nano microsphere with lignin as carbon source and preparation method thereof - Google Patents
A kind of magnetic carbon Nano microsphere with lignin as carbon source and preparation method thereof Download PDFInfo
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- CN106219517A CN106219517A CN201610652178.3A CN201610652178A CN106219517A CN 106219517 A CN106219517 A CN 106219517A CN 201610652178 A CN201610652178 A CN 201610652178A CN 106219517 A CN106219517 A CN 106219517A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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Abstract
The invention belongs to nano composite material technical field, disclose a kind of magnetic carbon Nano microsphere with lignin as carbon source and preparation method thereof.Described preparation method is: lignin and ferric acetyl acetonade are dissolved in N, N dimethylformamide, obtains the lignin electrostatic solution containing ferric acetyl acetonade, then obtains the lignin Nano microsphere containing ferric acetyl acetonade by electrostatic；Gained lignin Nano microsphere is pre-oxidized at a temperature of 250～280 DEG C, at a temperature of 400～900 DEG C, then carries out carbonization treatment, obtain the described magnetic carbon Nano microsphere with lignin as carbon source.The preparation method raw material of the present invention is easy to get, energy-conserving and environment-protective, and products therefrom microscopic appearance, dispersive property and magnetic property are good, have preferable application prospect in the fields such as information, the energy, detection and biology.
Description
Technical field
The invention belongs to nano composite material technical field, be specifically related to a kind of magnetic carbon nanometer with lignin as carbon source
Microsphere and preparation method thereof.
Background technology
In recent years, the most effectively and fully use abundant, the renewable and biomass resource of environmental protection, alleviate the severe energy
With environmental problem, obtain the extensive concern of various circles of society.
One of resource that lignin is widely present most as nature, is that plant kingdom's content is only second to the second largest of cellulose
The polyphenol polymer of unformed shape.It is a kind of renewable, green, the natural macromolecular material of environmental protection.Commercial wood element conduct
The side-product of paper industry, is present in black liquid, is seldom further processed and utilizes, causing the waste of resource,
Even can bring environmental problem.Lignin molecule has abundant carbon content, thus can be processed further being prepared as material with carbon element and enter
Exercise and use.The lignin being widely present by nature causes the attention of various countries' researcher as carbon source, 1975, material scholar
First Johnson proposes to prepare carbon fibre material with lignin for carbon source.The material with carbon element that people use at present is generally petrochemical industry base
, himself there is problem non-renewable, that the feature of environmental protection is poor and cost is high in material with carbon element.Magnetic material is at machinery, electronics, optics, magnetic
Learning, chemistry and biology field has a wide range of applications.At present, rarely have both at home and abroad using simple lignin as carbon source system
Research in terms of standby magnetic carbon Nano microsphere, the problem being primarily present is that lignin is prepared Nano carbon balls and is difficult to keep its microcosmic shape
Looks, cause it restricted in using further.
Summary of the invention
In place of solving the shortcoming and defect of above prior art, the primary and foremost purpose of the present invention is to provide a kind of with wood
Quality is the preparation method of the magnetic carbon Nano microsphere of carbon source.
Another object of the present invention is to provide a kind of magnetic with lignin as carbon source prepared by said method
Property carbon nanometer micro ball.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of the magnetic carbon Nano microsphere with lignin as carbon source, including following preparation process:
(1) lignin and ferric acetyl acetonade are dissolved in DMF, obtain the wood containing ferric acetyl acetonade
Quality electrostatic solution；
(2) the lignin electrostatic solution that step (1) gained contains ferric acetyl acetonade is transferred in the equipment of electrostatic,
The lignin Nano microsphere containing ferric acetyl acetonade is obtained by electrostatic；
(3) the lignin Nano microsphere containing ferric acetyl acetonade is pre-oxidized at a temperature of 250～280 DEG C；
(4) the lignin Nano microsphere containing ferric acetyl acetonade of pre-oxidation is carried out carbonization at a temperature of 400～900 DEG C
Process, obtain the described magnetic carbon Nano microsphere with lignin as carbon source.
Preferably, containing in the lignin electrostatic solution of ferric acetyl acetonade described in step (1), the quality of lignin is divided
Number is 20%～50%, and the content of ferric acetyl acetonade is the 5%～30% of lignin quality.
Preferably, described in step (2), the condition of electrostatic is: electrostatic pressure is 10～30kv, receiving range be 10～
20cm, the fltting speed of electrostatic solution is 1～3ml/h.
Preferably, described in step (3), preoxidation process is carried out in air atmosphere, and preoxidation time is 2～6h, heats up
Speed is 0.2～1 DEG C/min.
Preferably, described in step (4), carbonization treatment process is carried out under nitrogen or argon gas atmosphere, the time of carbonization treatment
Being 0.5～2h, heating rate is 0.5～2 DEG C/min.
A kind of magnetic carbon Nano microsphere with lignin as carbon source, is prepared by said method.
Preparation method and the obtained product of the present invention have the advantage that and beneficial effect:
(1) the be able to lignin of the present invention be the magnetic carbon Nano microsphere of carbon source be with low cost, renewable, degradable
Commercial wood element is as carbon source, compared with conventional carbon nanomaterial, has raw material and is easy to get, has taken into full account energy-conservation and environmental protection is former
Then, this has great importance for the sustainable development of resource and environment；
(2) the be able to lignin of the present invention is that the microscopic appearance of magnetic carbon Nano microsphere of carbon source is good, has good simultaneously
Good dispersive property, can improve the serviceability of lignin material with carbon element；
(3) the be able to lignin of the present invention is that the magnetic carbon Nano microsphere of carbon source has good magnetic property, at information, energy
The fields such as source, detection and biology there is preferable application prospect；
(4) preparation method of the present invention magnetic carbon Nano microsphere with lignin as carbon source is simple, and preparation cost is cheap, tool
There is good actual application value.
Accompanying drawing explanation
Fig. 1 is the microscopic appearance figure of the magnetic carbon Nano microsphere with lignin as carbon source of the embodiment of the present invention 1 preparation
((a) 5000 ×, (b) 10000 ×).
Fig. 2 is the hysteresis curve figure of the magnetic carbon Nano microsphere with lignin as carbon source of the embodiment of the present invention 4 preparation.
Fig. 3 is the hysteresis curve figure of the magnetic carbon Nano microsphere with lignin as carbon source of the embodiment of the present invention 5 preparation.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention do not limit
In this.
Embodiment 1
(1) weighing commercial wood element and ferric acetyl acetonade, use DMF is solvent, is configured to lignin
Mass fraction be 35% the lignin electrostatic solution containing ferric acetyl acetonade (wherein acetylacetone,2,4-pentanedione iron content is lignin
10%, w/w)；
(2) the lignin electrostatic solution containing ferric acetyl acetonade of step (1) is transferred in the equipment of electrostatic, quiet
Voltage is 25kv, and receiving range is 15cm, and the fltting speed of electrostatic solution is to carry out electrostatic under conditions of 3ml/h, obtains
Lignin Nano microsphere containing ferric acetyl acetonade；
(3) lignin Nano microsphere gained being contained ferric acetyl acetonade is positioned among tube furnace, uses 250 DEG C pre-
This lignin Nano microsphere is pre-oxidized by oxidizing temperature, and pre-oxidation is carried out in atmosphere, and its heating rate is 0.2 DEG C/
Min, preoxidation time is 3h；
(4) the lignin Nano microsphere containing ferric acetyl acetonade of above-mentioned pre-oxidation is carried out carbonization treatment, carburizing temperature
Being 400 DEG C, carbonization is carried out in nitrogen, and its heating rate is 2 DEG C/min, and carbonization time is 0.5h, finally gives with lignin
Magnetic carbon Nano microsphere for carbon source.
The scanning electron microscope (SEM) photograph of the magnetic carbon Nano microsphere with lignin as carbon source obtained in the present embodiment as it is shown in figure 1,
As seen from Figure 1: the magnetic carbon Nano microsphere with lignin as carbon source presents good spherical morphology, have preferably simultaneously
Dispersive property.
Embodiment 2
(1) weighing commercial wood element and ferric acetyl acetonade, use DMF is solvent, is configured to lignin
Mass fraction be 45% the lignin electrostatic solution containing ferric acetyl acetonade (wherein acetylacetone,2,4-pentanedione iron content is lignin
30%, w/w)；
(2) the lignin electrostatic solution containing ferric acetyl acetonade of step (1) is transferred in the equipment of electrostatic, quiet
Voltage is 15kv, and receiving range is 15cm, and the fltting speed of electrostatic solution is to carry out electrostatic under conditions of 3ml/h, obtains
Lignin Nano microsphere containing ferric acetyl acetonade；
(3) lignin Nano microsphere gained being contained ferric acetyl acetonade is positioned among tube furnace, uses 280 DEG C pre-
This lignin Nano microsphere is pre-oxidized by oxidizing temperature, and pre-oxidation is carried out in atmosphere, and its heating rate is 0.5 DEG C/
Min, preoxidation time is 6h；
(4) the lignin Nano microsphere containing ferric acetyl acetonade of above-mentioned pre-oxidation is carried out carbonization treatment, carburizing temperature
Being 400 DEG C, carbonization is carried out in nitrogen, and its heating rate is 1 DEG C/min, and carbonization time is 2h, finally gives favorable dispersibility
The magnetic carbon Nano microsphere with lignin as carbon source.
Embodiment 3
(1) weighing commercial wood element and ferric acetyl acetonade, use DMF is solvent, is configured to lignin
Mass fraction be 35% the lignin electrostatic solution containing ferric acetyl acetonade (wherein acetylacetone,2,4-pentanedione iron content is lignin
20%, w/w)；
(2) the lignin electrostatic solution containing ferric acetyl acetonade of step (1) is transferred in the equipment of electrostatic, quiet
Voltage is 15kv, and receiving range is 10cm, and the fltting speed of electrostatic solution is to carry out electrostatic under conditions of 2ml/h, obtains
Lignin Nano microsphere containing ferric acetyl acetonade；
(3) lignin Nano microsphere gained being contained ferric acetyl acetonade is positioned among tube furnace, uses 280 DEG C pre-
This lignin Nano microsphere is pre-oxidized by oxidizing temperature, and pre-oxidation is carried out in atmosphere, and its heating rate is 0.2 DEG C/
Min, preoxidation time is 2h；
(4) the lignin Nano microsphere containing ferric acetyl acetonade of above-mentioned pre-oxidation is carried out carbonization treatment, carburizing temperature
Being 600 DEG C, carbonization is carried out in argon, and its heating rate is 0.5 DEG C/min, and carbonization time is 1h, finally gives dispersibility good
The good magnetic carbon Nano microsphere with lignin as carbon source.
Embodiment 4
(1) weighing commercial wood element and ferric acetyl acetonade, use DMF is solvent, is configured to lignin
Mass fraction be 35% the lignin electrostatic solution containing ferric acetyl acetonade (wherein acetylacetone,2,4-pentanedione iron content is lignin
5%, w/w)；
(2) the lignin electrostatic solution containing ferric acetyl acetonade of step (1) is transferred in the equipment of electrostatic, quiet
Voltage is 15kv, and receiving range is 10cm, and the fltting speed of electrostatic solution is to carry out electrostatic under conditions of 2ml/h, obtains
Lignin Nano microsphere containing ferric acetyl acetonade；
(3) lignin Nano microsphere gained being contained ferric acetyl acetonade is positioned among tube furnace, uses 280 DEG C pre-
This lignin Nano microsphere is pre-oxidized by oxidizing temperature, and pre-oxidation is carried out in atmosphere, and its heating rate is 0.2 DEG C/
Min, preoxidation time is 2h；
(4) the lignin Nano microsphere containing ferric acetyl acetonade of above-mentioned pre-oxidation is carried out carbonization treatment, carburizing temperature
Being 800 DEG C, carbonization is carried out in nitrogen, and its heating rate is 2 DEG C/min, and carbonization time is 2h, finally gives favorable dispersibility
The magnetic carbon Nano microsphere with lignin as carbon source.
The be able to lignin of the present embodiment be the hysteresis curve figure of the magnetic carbon Nano microsphere of carbon source as shown in Figure 2.
Embodiment 5
(1) weighing commercial wood element and ferric acetyl acetonade, use DMF is solvent, is configured to lignin
Mass fraction be 35% the lignin electrostatic solution containing ferric acetyl acetonade (wherein acetylacetone,2,4-pentanedione iron content is lignin
30%, w/w)；
(2) the lignin electrostatic solution containing ferric acetyl acetonade of step (1) is transferred in the equipment of electrostatic, quiet
Voltage is 15kv, and receiving range is 10cm, and the fltting speed of electrostatic solution is to carry out electrostatic under conditions of 2ml/h, obtains
Lignin Nano microsphere containing ferric acetyl acetonade；
(3) lignin Nano microsphere gained being contained ferric acetyl acetonade is positioned among tube furnace, uses 280 DEG C pre-
This lignin Nano microsphere is pre-oxidized by oxidizing temperature, and pre-oxidation is carried out in atmosphere, and its heating rate is 0.2 DEG C/
Min, preoxidation time is 2h；
(4) the lignin Nano microsphere containing ferric acetyl acetonade of above-mentioned pre-oxidation is carried out carbonization treatment, carburizing temperature
Being 900 DEG C, carbonization is carried out in nitrogen, and its heating rate is 1 DEG C/min, and carbonization time is 0.5h, finally gives dispersibility good
The good magnetic carbon Nano microsphere with lignin as carbon source.
The be able to lignin of the present embodiment be the hysteresis curve figure of the magnetic carbon Nano microsphere of carbon source as shown in Figure 3.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (6)
1. the preparation method of the magnetic carbon Nano microsphere with lignin as carbon source, it is characterised in that include preparing as follows step
Rapid:
(1) lignin and ferric acetyl acetonade are dissolved in DMF, obtain the lignin containing ferric acetyl acetonade
Electrostatic solution；
(2) transfer to the lignin electrostatic solution that step (1) gained contains ferric acetyl acetonade, in the equipment of electrostatic, pass through
Electrostatic obtains the lignin Nano microsphere containing ferric acetyl acetonade；
(3) the lignin Nano microsphere containing ferric acetyl acetonade is pre-oxidized at a temperature of 250～280 DEG C；
(4) the lignin Nano microsphere containing ferric acetyl acetonade of pre-oxidation is carried out at carbonization at a temperature of 400～900 DEG C
Reason, obtains the described magnetic carbon Nano microsphere with lignin as carbon source.
The preparation method of a kind of magnetic carbon Nano microsphere with lignin as carbon source the most according to claim 1, its feature
Be: described in step (1) containing ferric acetyl acetonade lignin electrostatic solution in, the mass fraction of lignin be 20%～
50%, the content of ferric acetyl acetonade is the 5%～30% of lignin quality.
The preparation method of a kind of magnetic carbon Nano microsphere with lignin as carbon source the most according to claim 1, its feature
It is that described in step (2), the condition of electrostatic is: electrostatic pressure is 10～30kv, and receiving range is 10～20cm, and electrostatic is molten
The fltting speed of liquid is 1～3ml/h.
The preparation method of a kind of magnetic carbon Nano microsphere with lignin as carbon source the most according to claim 1, its feature
Being: described in step (3), preoxidation process is carried out in air atmosphere, preoxidation time is 2～6h, and heating rate is 0.2
～1 DEG C/min.
The preparation method of a kind of magnetic carbon Nano microsphere with lignin as carbon source the most according to claim 1, its feature
Being: described in step (4), carbonization treatment process is carried out under nitrogen or argon gas atmosphere, the time of carbonization treatment is 0.5～2h,
Heating rate is 0.5～2 DEG C/min.
6. the magnetic carbon Nano microsphere with lignin as carbon source, it is characterised in that: by any one of Claims 1 to 5 institute
The method stated prepares.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107221641A (en) * | 2017-06-26 | 2017-09-29 | 浙江工业大学 | A kind of lignin is the MoS of carbon source2The preparation method of@C combination electrode materials |
| CN107349905A (en) * | 2017-08-30 | 2017-11-17 | 华南理工大学 | The method that a kind of nitrogen co-doped magnetic carbon material of fluorine removes hexavalent chromium in industrial wastewater |
| CN107758640A (en) * | 2017-10-27 | 2018-03-06 | 华中科技大学 | A kind of preparation method and product of the hollow carbon of erythrocyte shape |
| 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 |
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| US20140271443A1 (en) * | 2013-03-15 | 2014-09-18 | University Of Tennessee Research Foundation | High Glass Transition Lignins and Lignin Derivatives for the Manufacture of Carbon and Graphite Fibers |
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Cited By (6)
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| CN107349905A (en) * | 2017-08-30 | 2017-11-17 | 华南理工大学 | The method that a kind of nitrogen co-doped magnetic carbon material of fluorine removes hexavalent chromium in industrial wastewater |
| CN107758640A (en) * | 2017-10-27 | 2018-03-06 | 华中科技大学 | A kind of preparation method and product of the hollow carbon of erythrocyte shape |
| 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 |
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