CN110451485A - A kind of lignin thermogravimetric structure assembling carbon nanomaterial and preparation method thereof - Google Patents
A kind of lignin thermogravimetric structure assembling carbon nanomaterial and preparation method thereof Download PDFInfo
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- CN110451485A CN110451485A CN201910812557.8A CN201910812557A CN110451485A CN 110451485 A CN110451485 A CN 110451485A CN 201910812557 A CN201910812557 A CN 201910812557A CN 110451485 A CN110451485 A CN 110451485A
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Abstract
The invention discloses a kind of lignin thermogravimetric structure assembling carbon nanomaterials and preparation method thereof, the preparation method will cross metal salt and be loaded on lignin by excessive infusion process, after being pyrolyzed and Muffle furnace is calcined, the lignin-base carbon material rich in nano transition metal oxides particle is obtained；The lignin-base carbon material is placed in vertical fixed-bed, gaseous carbon source such as ethylene or methane and nitrogen mixed gas is passed through, is reacted at a certain temperature, final collect obtains carbon nanotube-lignin-base carbon material mixture after thermogravimetric structure.The present invention utilizes renewable resource lignin; the lignin carbon material of low value is converted to the carbon nanomaterial for high value; raw material are simple and easy to get; preparation condition is controllable; have a wide range of application; the renewable resource for successfully having developed and used this low value of lignin, is of great significance to the utilization of resources and environmental protection, has the value of popularization and application.
Description
Technical field
The invention belongs to technical field of energy material, and in particular to relate to a kind of lignin thermogravimetric structure assembling carbon nanomaterial and
Preparation method.
Background technique
Lignin is the solids such as important component (15-35%) and black liquid residue, the hydrolytic residue of biomass
The main component (80% or more) of waste.Therefore, this kind of " low price " renewable resource of lignin, preparation " high price are developed and used
The biomass base class carbon material of value ", is of great significance for comprehensive utilization of resources and environmental protection.Wherein, prepared by lignin
Carbon material is one of important use of lignin, while lignin is preparing carbon as the highest renewable resource of phosphorus content
Material aspect is richly endowed by nature, can not be substituted.But current lignin-base carbon material is mainly with the low-quality charcoal such as active carbon and charcoal
Based on, it is unable to satisfy (such as carbon nanotube, carbon nano-fiber, graphene, the fullerene of the demand to high performance carbon material in the market
Carbon nanomaterial).On the other hand, the carbon material mixture containing carbon nanomaterial is because of the pore structure of its multi-layer, conduction, thermally conductive
And effect of mass transmitting, there is huge application value in terms of catalysis, energy storage and environment.The method prepared at present is mainly by two kinds
Carbon material, i.e. carbon nanomaterial and conventional carbon (active carbon or charcoal etc.), are mixed and are grafted.Although resulting contain
The carbon material mixture of carbon nanomaterial has excellent performance, but this problem of there is also some urgent need to resolve.For example, carbon is received
The nano effect of rice material itself is it is obvious that be difficult to disperse and be difficult to uniform with another carbon material (active carbon or charcoal etc.)
Mixing thereby results in gained carbon material limited performance, and stability is poor, and service life and power of regeneration are also undesirable.It is anxious as a result,
A kind of method of easy lignin thermogravimetric structure assembling carbon nanomaterial need to be proposed, the carbon material containing carbon nanomaterial is realized
Mixture preparation, realize biomass solid wastes to carbon nanomaterial higher value application.
Summary of the invention
Goal of the invention: in view of the problems of the existing technology, the present invention provides a kind of lignin thermogravimetric structure assemble carbon nanometer
Material and preparation method thereof, the present invention can utilize renewable resource lignin, the carbon material of low value are changed into high value
Carbon nanomaterial.Simple lignin thermogravimetric structure proposed by the present invention assembles carbon nanomaterial method, and carbon containing nanometer may be implemented
Prepared by the carbon material mixture of material, uniformity stability is more preferable.
Technical solution: to achieve the goals above, a kind of lignin thermogravimetric structure assembles carbon nanomaterial as described herein
Preparation method, which comprises the following steps: transition metal salt is loaded on lignin by excessive infusion process,
After pyrolysis and calcining, the lignin-base carbon material rich in nano transition metal oxides particle is obtained；By the lignin-base
Carbon material is passed through gaseous carbon source and nitrogen mixed gas, is reacted in high temperature, and final collect obtains the carbon nanometer after thermogravimetric structure
Pipe-lignin-base carbon material mixture, as lignin thermogravimetric structure assemble carbon nanomaterial.
Wherein, the excessive infusion process is that transition metal salt solution is mixed to 60 DEG C of heating water bath 2h with lignin, then
It is put into baking oven and stands 12h.
Wherein, the transition metal salt is chlorate or nitrate.Preferably NiCl2、Ni(NO3)2、FeNO3、FeCl3、
Co(NO3)2Or CoCl2。
Preferably, the lignin includes lignin of black liquid or Kelly Clarkson lignin.
Wherein, it is described transition metal salt is loaded on lignin by excessive infusion process after pyrolysis temperature be 800-900
DEG C, pyrolysis temperature constant temperature handles 2-3h.
Wherein, the calcining is preferably 400 DEG C of calcining 2h of Muffle furnace.
Preferably, the gaseous carbon source is ethylene or methane.
Preferably, described be passed through gaseous carbon source and nitrogen mixed gas, reaction is carried out as at 700 DEG C -900 DEG C in high temperature
Under carry out reaction 1-1.5h.
It is furthermore preferred that the gaseous carbon source being passed through is ethylene, ethene flow 10ml/min, nitrogen flow 100ml/
Min (and whole process is passed through) is arranged 700-900 DEG C of target temperature, and heating rate is 10 DEG C/min.Temperature reaches perseverance after target temperature
Temperature 1 hour, preceding half an hour are passed through ethylene with the rate of 10ml/min, stop logical ethylene after half an hour after.
Wherein, lignin thermogravimetric structure assembling carbon nanomaterial is grown under the catalytic action of transition metal particles
Grown on top.
The lignin thermogravimetric structure assembling of the preparation method preparation of lignin thermogravimetric structure assembling carbon nanomaterial of the present invention
Carbon nanomaterial.
Wherein, lignin thermogravimetric structure assembling carbon nanomaterial is multi-walled carbon nanotube and its caliber is 20nm-
120nm。
The utility model has the advantages that compared with prior art, the present invention has the advantage that
The preparation method of lignin thermogravimetric structure assembling carbon nanomaterial of the present invention, the lignin carbon material of low value is converted
The carbon nanomaterial for becoming high value meets market for the demand of high value carbon material；It is at low cost, application material range
Extensively, for environmental-friendly, the recycling of resource and the saving of the energy are realized.
The present invention introduced in lignin pyrolytic process be blended substance (be blended substance guide into gaseous carbon source, ethylene or
The mixture of person's methane and nitrogen) decomposition of lignin can be deepened, the secondary polycondensation of tar is reduced and promote lignin structure
Deoxidation is conducive to obtain the carbon product of more " pure ".The carbon product of " pure " is under the guidance and specific operating condition of catalyst
It is the good raw material for preparing high performance carbon nano material.
Raw material of the invention are simple and easy to get, and preparation condition is controllable, have a wide range of application, and have successfully developed and used wooden
The renewable resource of this plain low value, is of great significance to the utilization of resources and environmental protection, has the value of popularization and application.
Detailed description of the invention
Fig. 1 is the SEM scanning electron microscope (SEM) photograph of lignin-base carbon material in embodiment 1；
Fig. 2 is the SEM scanning electron microscope (SEM) photograph of gained carbon nanomaterial in embodiment 1；
Fig. 3 is the TEM transmission electron microscope picture of gained carbon nanomaterial in embodiment 1；
Fig. 4 is the TEM transmission electron microscope picture of gained carbon nanomaterial in embodiment 1.
Specific embodiment
Below with reference to embodiment, the present invention will be further explained.
Embodiment 1
A kind of preparation method of lignin thermogravimetric structure assembling carbon nanomaterial, the specific steps are as follows:
Weigh six water nickel chloride (NiCl of 2.377g2·6H2O), it is dissolved in 50mL distilled water；It is wooden to weigh 10g Kelly Clarkson
Element is placed in 100mL beaker, and the Ni solution of middle 50mL is transferred to wherein, is stirred 2 hours for 60 DEG C in water-bath.Stirring terminates, and takes
Out, be transferred in baking oven, 105 DEG C drying 12 hours.The sample of 2g is weighed, setting target pyrolysis temperature is 800 DEG C, constant temperature time
It is 3 hours, heating rate is 10 DEG C/min, with N2As protective gas (flow 100mL/min), lignin-base carbon materials are prepared
Material.0.1g lignin-base carbon material is weighed, target pyrolysis temperature 800 is arranged as protective gas (flow 100mL/min) in N2
DEG C, heating rate is 10 DEG C/min.When constant temperature 1 is small after fixed bed temperature reaches 800 DEG C, first 0.5 hour with 10ml/min's
Rate is passed through ethylene, and stopping in latter 0.5 hour is passed through ethylene, enables carbon nanomaterial growth complete.
Performance test: Electronic Speculum (SEM), X-ray are scanned to obtained lignin-base carbon material and carbon nanomaterial
XPS Analysis (XPS), transmission electron microscope (TEM) phenetic analysis.
The scanning electron microscope (SEM) photograph of lignin-base carbon material and carbon nanomaterial that the present embodiment obtains is as shown in Figure 1 and Figure 2, carbon
The transmission electron microscope picture of nano material is as shown in Figure 3, Figure 4.The carbon nanomaterial of synthesis is hollow multi wall tubular structure, thickness of pipe wall
About 10nm, interfloor distance 0.3-0.4nm, diameter 20-70nm, length 800-1800nm, it may be determined that the carbon nanometer of synthesis
Material is multi-walled carbon nanotube.Discovery has nickel particle attachment on the top of carbon nanometer, therefore the growth course of carbon nanotube meets top
The mechanism of growth is held, i.e. carbon nanotube is precipitated from the lower part of nickel particle, and nickel particle is always positioned at the top of carbon nanotube.Pass through figure
2, Fig. 3 can be seen that carbon nanotube is uniformly mixed with other carbon materials, realize the carbon material mixture containing carbon nanomaterial
Preparation, realize biomass solid wastes to carbon nanomaterial higher value application.
Embodiment 2
A kind of preparation method of lignin thermogravimetric structure assembling carbon nanomaterial, the specific steps are as follows:
Weigh six water nickel chloride (NiCl of 1.189g2·6H2O), it is dissolved in 50mL distilled water；It is wooden to weigh 10g Kelly Clarkson
Element is placed in 100mL beaker, and the Ni solution of middle 50mL is transferred to wherein, is stirred 2 hours for 60 DEG C in water-bath.Stirring terminates, and takes
Out, be transferred in baking oven, 105 DEG C drying 12 hours.The sample of 2g is weighed, and it is 800 DEG C, when constant temperature that target pyrolysis temperature, which is arranged,
Between be 3 hours, heating rate be 10 DEG C/min, with N2As protective gas (flow 100mL/min), lignin-base carbon is prepared
Material.0.1g lignin-base carbon material will be weighed to set, N2 is arranged target and is pyrolyzed as protective gas (flow 100mL/min)
900 DEG C of temperature, heating rate is 10 DEG C/min.When constant temperature 1 is small after fixed bed temperature reaches 900 DEG C, first 0.5 hour with
The rate of 10ml/min is passed through ethylene, and stopping in latter 0.5 hour is passed through ethylene, enables carbon nanomaterial growth complete.
Phenetic analysis is carried out to lignin-base carbon material and carbon nanomaterial is obtained.Gained carbon nanomaterial is that multi wall carbon is received
Mitron, caliber 30-80nm.
Embodiment 3
A kind of preparation method of lignin thermogravimetric structure assembling carbon nanomaterial, the specific steps are as follows:
Weigh six water nickel chloride (NiCl of 1.189g2·6H2O), it is dissolved in 50mL distilled water；It is wooden to weigh 10g Kelly Clarkson
Element is placed in 100mL beaker, and the Ni solution of middle 50mL is transferred to wherein, is stirred 2 hours for 60 DEG C in water-bath.Stirring terminates, and takes
Out, be transferred in baking oven, 105 DEG C drying 12 hours.The sample of 2g is weighed, and it is 800 DEG C, when constant temperature that target pyrolysis temperature, which is arranged,
Between be 3 hours, heating rate is that 10 DEG C/min using N2 as protective gas (flow 100mL/min) is then placed in Muffle furnace
400 DEG C of calcining 2h, prepare lignin-base carbon material.Weigh 0.1g lignin-base carbon material, (flow is N2 as protective gas
100mL/min), it is arranged 900 DEG C of target pyrolysis temperature, heating rate is 10 DEG C/min.It is permanent after fixed bed temperature reaches 900 DEG C
Temperature 1.5 hours, preceding 1 hour rate with 10ml/min is passed through ethylene, and stopping in latter 0.5 hour is passed through ethylene, enables carbon nanomaterial
Growth is complete.
Phenetic analysis is carried out to lignin-base carbon material and carbon nanomaterial is obtained.Gained carbon nanomaterial is that multi wall carbon is received
Mitron, caliber 60-120nm.
Embodiment 4
Embodiment 4 is identical as 1 preparation method of embodiment, the difference is that: transition metal salt is Ni (NO3)2, lignin
For Kelly Clarkson lignin, 900 DEG C of pyrolysis temperature, heating rate is 10 DEG C/min, and pyrolysis constant temperature handles 2h；Gaseous carbon source is first
Alkane is passed through gaseous carbon source, and reaction 1.5h is carried out at 700 DEG C.
Embodiment 5
Embodiment 5 is identical as 1 preparation method of embodiment, the difference is that: transition metal salt FeCl3, lignin is
Lignin of black liquid, 850 DEG C of pyrolysis temperature, heating rate is 10 DEG C/min, and pyrolysis constant temperature handles 2.5h；Gaseous carbon source is that ethylene exists
Reaction 1h is carried out at 900 DEG C.
Claims (10)
1. a kind of preparation method of lignin thermogravimetric structure assembling carbon nanomaterial, which comprises the following steps: by transition
Metal salt is loaded on lignin by excessive infusion process, after pyrolysis and calcining, obtains aoxidizing rich in nano transition metal
The lignin-base carbon material of composition granule；By the lignin-base carbon material, be passed through gaseous carbon source and nitrogen mixed gas, high temperature into
Row reaction, final collect obtain carbon nanotube-lignin-base carbon material mixture after thermogravimetric structure, as lignin thermogravimetric structure group
Fill carbon nanomaterial.
2. the preparation method of lignin thermogravimetric structure assembling carbon nanomaterial according to claim 1, which is characterized in that described
Transition metal salt is chlorate or nitrate.
3. the preparation method of lignin thermogravimetric structure assembling carbon nanomaterial according to claim 1, which is characterized in that described
Chlorate or nitrate are preferably NiCl2、Ni(NO3)2、FeNO3、FeCl3、Co(NO3)2Or CoCl2。
4. the preparation method of lignin thermogravimetric structure assembling carbon nanomaterial according to claim 1, which is characterized in that described
Lignin includes lignin of black liquid or Kelly Clarkson lignin.
5. the preparation method of lignin thermogravimetric structure assembling carbon nanomaterial according to claim 1, which is characterized in that described
Pyrolysis temperature is 800-900 DEG C after transition metal salt is loaded on lignin by excessive infusion process, at pyrolysis temperature constant temperature
Manage 2-3h.
6. the preparation method of lignin thermogravimetric structure assembling carbon nanomaterial according to claim 1, which is characterized in that described
Gaseous carbon source is ethylene or methane.
7. the preparation method of lignin thermogravimetric structure assembling carbon nanomaterial according to claim 1, which is characterized in that described
It is passed through gaseous carbon source and nitrogen mixed gas, carries out reaction in high temperature to be reacted at 700 DEG C -900 DEG C, the reaction time is
1-1.5h。
8. the preparation method of lignin thermogravimetric structure assembling carbon nanomaterial according to claim 1, which is characterized in that described
Being grown to for lignin thermogravimetric structure assembling carbon nanomaterial carbon nanomaterial is raw in the catalytic action next top of transition metal particles
It is long.
9. a kind of lignin thermogravimetric structure assemble carbon nanometer material of the preparation method preparation of lignin thermogravimetric structure assembling carbon nanomaterial
Material.
10. lignin thermogravimetric structure assembling carbon nanomaterial according to claim 8 is multi-walled carbon nanotube and its caliber is
20nm-120nm。
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Cited By (4)
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| CN111170402A (en) * | 2020-02-12 | 2020-05-19 | 东华大学 | Method for removing perfluorooctanoic acid in water body by using lignin-based carbon nano tube |
| CN111634902A (en) * | 2020-06-01 | 2020-09-08 | 南京博岭节能环保研究院有限公司 | Method for preparing carbon nano tube by secondary catalytic reforming of lignin pyrolysis gas |
| CN112265981A (en) * | 2020-10-23 | 2021-01-26 | 中南林业科技大学 | Method for preparing carbon nano tube by lignin nano micelle |
| CN112973625A (en) * | 2021-02-05 | 2021-06-18 | 中南林业科技大学 | Lignin-based carbon nanotube and preparation method and application thereof |
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Cited By (5)
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