CN109704307A - A kind of preparation and its application of the sulfur doping porous carbon based on sterculia seed slag - Google Patents
A kind of preparation and its application of the sulfur doping porous carbon based on sterculia seed slag Download PDFInfo
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- CN109704307A CN109704307A CN201910092250.5A CN201910092250A CN109704307A CN 109704307 A CN109704307 A CN 109704307A CN 201910092250 A CN201910092250 A CN 201910092250A CN 109704307 A CN109704307 A CN 109704307A
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Abstract
The present invention provides the preparations and its application of a kind of sulfur doping porous carbon based on sterculia seed slag, steps are as follows: using the sterculia seed slag after making tea as raw material, high temperature cabonization obtains sulfur doping carbon under an inert atmosphere with sulfur doping agent, after through it is physically activated processing obtain sulfur doping porous carbon.The present invention prepares sulfur doping porous carbon using high temperature cabonization and the physically activated method combined, and method is easy to operate, and process is easily controllable, does not need to wash after activation, reduces production cost, carbon yield is higher, and environmental-friendly；The sulfur doping porous carbon of preparation is flaky nanometer structure, specific surface area and pore-size distribution are controllable, electric conductivity is high, sulfur content is adjustable, particularly suitable for fields such as heavy metal containing wastewater treatment, dyeing waste water absorption, lithium-sulfur cell, lithium ion battery, sodium-ion battery, supercapacitor and catalyst loads.
Description
Technical field
The present invention relates to biomass carbon preparation field more particularly to a kind of systems of the sulfur doping porous carbon based on sterculia seed slag
Standby and its application.
Background technique
From for the first time, after second industrial revolution, with non-renewable resources such as tellurian coal, petroleum, natural gases
The problems such as exploitation and utilization, environmental pollution, lack of energy, also constantly generates.Fundamentally to solve these problems, various countries are ground
The persons of studying carefully are devoted to the new cleaning resource of research and development to substitute the use of coal, petroleum, natural gas, such as: wind energy, geothermal energy,
Solar energy, tide energy and biomass energy etc..Biomass refers to the organic substance formed using green plants photosynthesis, including
Plant, animal and microorganism and its excretion, metabolin in addition to fossil fuel, have reproducibility, and low pollution is widely distributed
The biological natures such as property.Research finds that various countries all gradually utilize the biomass materials such as various agricultural wastes, forestry residue every year
Go biomass energies, material and the chemicals such as production ethyl alcohol, combustion gas, biogas, plastics, amino acid, glucose, starch, biomass
Carbon material belongs to one of numerous biological materials.
The sterculia seed, alias sea, SEMEN STERCULIAE LYCHNOPHORAE etc., the big dry mature seed for sending out the Sterculiaceae plant sterculia seed, originate in Thailand,
The states such as Cambodia, Malaysia.When fruit maturation in 4 ~ June cracks, seed is harvested, use is dried.It is chiefly used in making tea, drop can be played
The effect of blood pressure, throat-moistening resolve phlegm.Residue after the usual sterculia seed is made tea all is dropped, and not only causes the waste of resource, also dirty
Environment is contaminated.Contain a large amount of carbohydrate and fatty acid in the sterculia seed, and it is loose porous, therefore the sterculia seed residue after making tea in
The pyrolysis of inert atmosphere high temperature, can be obtained the biomass carbon material of rich carbon, high stability, Large ratio surface, not only can be sufficiently sharp
With biomass castoff, our ecological environment is also protected.
Currently, being that the method that raw material prepares porous carbon mainly has template and activation method with biomass (waste).Wherein
Template includes soft template method and hard template method.Soft template method is using amphiphilic or copolymer as template, with carbon materials
Material precursor is combined to obtain composite Nano micella by hydrogen bond, and resolidification precursor forms three-dimensional crosslinking structure, last carbon
Change obtains orderly porous carbon materials.Hard template method is first to penetrate into carbon precursor in template gap, is carbonized after crosslinking,
It is cleaned again with strong acid or strong base solution, thus obtains ordered porous carbon.However, template is because its is complicated for operation, corrosive nature
By force, the disadvantages of being difficult to control, limits its large-scale application.Wherein activation method is divided into chemical activation method and physical activation method again
Deng chemical activation is by such as KOH, H3PO4、K2CO3, NaOH and H2SO4A series ofization occurs for equal chemical reagent and carbon material
Reaction is learned, to go the method for createing micropore.Physical activation method is under the high temperature conditions, to utilize the various composition in air
(such as carbon dioxide, water vapour) is reacted with the carbon atom in carbon material, is formed by aperture, reaming etc. various micro-
Pore structure.Physically activated advantage is simple process, cleaning, does not need to wash after activation, is conducive to meet heavy industrialization
Production needs, in recent years by the concern of various countries' researcher.In addition, using miscellaneous element (such as N, P, S, B, F) to carbon bone
Frame is doped, and is remarkably improved the surface nature of carbon material, such as is improved wetability, improved electric conductivity and electrocatalysis characteristic,
The active site of reaction is also used as in electrochemistry.
Summary of the invention
The invention proposes the preparation and its application of a kind of sulfur doping porous carbon based on sterculia seed slag, raw materials are
The sterculia seed make tea after residue, it is from a wealth of sources, it is low in cost, sulfur doping agent be easy obtain, it is cheap, it is easy to accomplish industrialization
Large-scale production.
Realize the technical scheme is that
A kind of preparation of the sulfur doping porous carbon based on sterculia seed slag, steps are as follows:
(1) sterculia seed after making tea removes the peel deseeding, is put into freeze drier and is freeze-dried, and is crushed after dry with plant
Machine crushes, crosses sieve, obtains sterculia seed ground-slag end；
(2) sterculia seed ground-slag end that step (1) obtains and sulfur doping agent are put into nickel crucible, isometric alcohol and water is added
It after being sufficiently mixed uniformly and stands for 24 hours, is put into vacuum oven and is dried, then by dry products therefrom in protective gas
High temperature cabonization is carried out in atmosphere, and carbonized product taking-up is filtered with acid and is washed to neutrality, then gained filter residue is done in vacuum
It is dried in dry case, obtains sulfur doping carbon；
(3) sulfur doping carbon in step (3) is packed into sample cell, be placed in tube furnace, with certain liter under protective gas protection
Warm rate is heated to activation temperature, and stopping is passed through protective gas, and is passed through the oxidizing gas of certain flow, in activation temperature item
Activated under part after a certain period of time, stopping be passed through oxidizing gas, be cooled to room temperature under protective gas atmosphere, take out material and
Drying in oven obtains sulfur doping porous carbon.
The temperature being freeze-dried in the step (1) is -70 ~ -50 DEG C, and vacuum degree is less than 20pa, time 20-24h, is planted
Object pulverizer revolving speed is 1400r/min, and sieve mesh number is 100 mesh.
The mass ratio of sterculia seed ground-slag end and sulfur doping agent is 20:(1-4 in the step (2))；Sulphur in the step (2)
Dopant is selected from one of elemental sulfur, cysteine, cystine, thioacetic acid, mercaptoethanol and mercaptopropionic acid.
Vacuum drying temperature is 100-110 DEG C in the step (2), drying time 10-12h；In the step (2)
The temperature of high temperature cabonization is 700-900 DEG C, and heating rate is 3-7 DEG C/min, and the processing time is 1-4h.
The protective gas is nitrogen, argon gas or the helium that mass fraction is 99.99%, gas flow 100-
300sccm。
Acid is hydrochloric acid, sulfuric acid or the nitric acid of concentration 1-3mol/L in the step (2).
Activation temperature is warming up to the heating rate of 8-10 DEG C/min in the step (3), stopping is passed through protective gas, so
After be passed through oxidizing gas, oxidizing gas is air, carbon dioxide or vapor, gas flow 500-700sccm.
Activation temperature is 800-1000 DEG C in the step (3), activation time 1-4h；Dry temperature in the step (3)
Degree is 120-150 DEG C, drying time 4-6h.
Described is electric in heavy metal containing wastewater treatment, dyeing waste water absorption, lithium sulphur based on the sulfur doping porous carbon of sterculia seed slag
Application in pond, lithium ion battery, sodium-ion battery, supercapacitor and catalyst load.
The beneficial effects of the present invention are: the present invention prepares sulfur doping using high temperature cabonization and the physically activated method combined
Porous carbon, method is easy to operate, and process is easily controllable, does not need to wash after activation, reduces production cost, and carbon yield is higher,
And it is environmental-friendly；The sulfur doping porous carbon of preparation is flaky nanometer structure, and specific surface area and pore-size distribution are controllable, and electric conductivity is high,
Sulfur content is adjustable, particularly suitable for heavy metal containing wastewater treatment, dyeing waste water absorption, lithium-sulfur cell, lithium ion battery, sodium from
The fields such as sub- battery, supercapacitor and catalyst load.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the scanning electron microscope (SEM) photograph for the sulfur doping porous carbon that the embodiment of the present invention 1 obtains；
Fig. 2 is the transmission electron microscope picture for the sulfur doping porous carbon that the embodiment of the present invention 1 obtains；
Fig. 3 is the XRD diagram for the sulfur doping porous carbon that the embodiment of the present invention 1 obtains；
Fig. 4 is the Raman spectrogram for the sulfur doping porous carbon that the embodiment of the present invention 1 obtains.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's every other embodiment obtained under that premise of not paying creative labor, belongs to this hair
The range of bright protection.
Embodiment 1
A kind of preparation of the sulfur doping porous carbon based on sterculia seed slag, steps are as follows:
(1) it takes the sterculia seed after making tea to remove the peel deseeding, is put into freeze drier and is freeze-dried, the temperature of freeze-drying is -60
DEG C, vacuum degree is less than 20pa, time 21h, is crushed afterwards with FZ102 type plant pulverizer, revolving speed 1400r/min, crosses 100 mesh
Sieve obtains sterculia seed ground-slag end；
(2) sterculia seed ground-slag end that mass ratio is 20:2 and cysteine are put into nickel crucible, be added isometric alcohol and
After water is sufficiently mixed uniformly and stand for 24 hours, after be put into 105 DEG C of vacuum ovens and dry 11h, then dry products therefrom is existed
High temperature cabonization, gas flow 150sccm are carried out in the argon atmosphere that mass fraction is 99.99%；High temperature cabonization temperature is 800
DEG C, heating rate is 6 DEG C/min, and the processing time is 2h, and carbonized product taking-up is filtered with the sulfuric acid that concentration is 3mol/L
It washs to neutrality, then gained filter residue is dried into 12h in 100 DEG C of vacuum ovens, obtains sulfur doping carbon；
(3) it takes a certain amount of sulfur doping carbon to be packed into sample cell, is placed in tube furnace, under the argon gas protection that mass fraction is 99.99%
900 DEG C, argon flow 200sccm are heated to 9 DEG C/min heating rate, stopping is passed through argon gas, and is passed through gas flow and is
The carbon dioxide of 600sccm, after activating 2h under the conditions of 900 DEG C, stopping is passed through carbon dioxide, continues under 99.99% argon gas
It is cooled to room temperature, takes out material and dries 5h in 130 DEG C of baking ovens to get sulfur doping porous carbon is arrived.
Fig. 1 and Fig. 2 is the scanning electron microscope (SEM) photograph and transmission electron microscope picture of the sulfur doping porous carbon based on sterculia seed slag of preparation, can
To find out gained sample for typical flaky nanometer structure, and there are many holes on surface, this is because caused by activation.Fig. 3
XRD diagram in it can be seen that no apparent diffraction maximum, illustrate that the sulfur doping porous carbon of preparation is undefined structure.The peak D in Fig. 4
Presence show gained the porous carbon surface of sulfur doping there are some defects, these defects may be hole and the official of carbon material surface
Caused by capable of rolling into a ball；The presence at the peak G shows the good conductivity of gained sulfur doping porous carbon, and the peak value at the peak G is greater than the peak D, shows it
With certain degree of graphitization.Table 1 is the mass fraction of each element in sulfur doping porous carbon, shows that obtained carbon sample is certain
For sulfur doping carbon, wherein S element mass fraction is 1.82%.In conclusion the present invention has been successfully prepared one kind based on the sterculia seed
The sulfur doping porous carbon materials of slag.
The mass fraction of each element in 1 sulfur doping porous carbon of table
Embodiment 2
A kind of preparation of the sulfur doping porous carbon based on sterculia seed slag, steps are as follows:
(1) it takes the sterculia seed after making tea to remove the peel deseeding, is put into freeze drier and is freeze-dried, the temperature of freeze-drying is -70
DEG C, vacuum degree is less than 20pa, time 20h, is crushed afterwards with FZ102 type plant pulverizer, revolving speed 1400r/min, crosses 100 mesh
Sieve obtains sterculia seed ground-slag end；
(2) mass ratio is put into nickel crucible for the sterculia seed ground-slag end of 20:1 and sulphur, it is abundant that isometric alcohol and water is added
After mixing and stand for 24 hours, after be put into 100 DEG C of vacuum ovens and dry 10h, then will dry products therefrom in quality point
High temperature cabonization, gas flow 100sccm are carried out in the nitrogen atmosphere that number is 99.99%；High temperature cabonization temperature is 700 DEG C, heating
Rate is 3 DEG C/min, and the processing time is 1h, and carbonized product taking-up is filtered washing into the hydrochloric acid that concentration is 1mol/L
Property, then gained filter residue is dried to 10h in 110 DEG C of vacuum ovens, obtain sulfur doping carbon；
(3) it takes a certain amount of sulfur doping carbon to be packed into sample cell, is placed in tube furnace, in the case where mass fraction is 99.99% nitrogen protection
800 DEG C, nitrogen flow 100sccm are heated to 8 DEG C/min heating rate, stopping is passed through nitrogen, and is passed through gas flow and is
The air of 500sccm, after activating 1h under the conditions of 800 DEG C, stopping is passed through air, and continuation is cooled to room under 99.99% nitrogen
Temperature takes out material and dries 6h in 120 DEG C of baking ovens to get sulfur doping porous carbon is arrived.
Embodiment 3
A kind of preparation of the sulfur doping porous carbon based on sterculia seed slag, steps are as follows:
(1) it takes the sterculia seed after making tea to remove the peel deseeding, is put into freeze drier and is freeze-dried, the temperature of freeze-drying is -50
DEG C, vacuum degree is less than 20pa, and the time is for 24 hours, to be crushed afterwards with FZ102 type plant pulverizer, revolving speed 1400r/min, crosses 100 mesh
Sieve obtains sterculia seed ground-slag end；
(2) mass ratio is put into nickel crucible for the sterculia seed ground-slag end of 20:3 and cystine, isometric alcohol and water is added
After being sufficiently mixed uniformly and stand for 24 hours, after be put into 110 DEG C of vacuum ovens and dry 12h, then will dry products therefrom in matter
High temperature cabonization, gas flow 300sccm are carried out in the helium atmosphere that amount score is 99.99%；High temperature cabonization temperature is 900 DEG C,
Heating rate is 7 DEG C/min, and the processing time is 4h, and carbonized product taking-up is filtered washing with the nitric acid that concentration is 3mol/L
10h is dried in 110 DEG C of vacuum ovens to neutrality, then by gained filter residue, obtains sulfur doping carbon；
(3) it takes a certain amount of sulfur doping carbon to be packed into sample cell, is placed in tube furnace, under the helium protection that mass fraction is 99.99%
1000 DEG C, helium gas flow 300sccm are heated to 10 DEG C/min heating rate, stopping is passed through helium, and is passed through gas flow
For the vapor of 700sccm, after activating 4h under the conditions of 1000 DEG C, stopping is passed through vapor, continues under 99.99% helium
It is cooled to room temperature, takes out material and dries 4h in 150 DEG C of baking ovens to get sulfur doping porous carbon is arrived.
Embodiment 4
A kind of preparation of the sulfur doping porous carbon based on sterculia seed slag, steps are as follows:
(1) it takes the sterculia seed after making tea to remove the peel deseeding, is put into freeze drier and is freeze-dried, the temperature of freeze-drying is -50
DEG C, vacuum degree is less than 20pa, time 21h, is crushed afterwards with FZ102 type plant pulverizer, revolving speed 1400r/min, crosses 100 mesh
Sieve obtains sterculia seed ground-slag end；
(2) sterculia seed ground-slag end that mass ratio is 20:4 and mercaptoethanol are put into nickel crucible, be added isometric alcohol and
After water is sufficiently mixed uniformly and stand for 24 hours, after be put into 105 DEG C of vacuum ovens and dry 10h, then dry products therefrom is existed
High temperature cabonization, gas flow 200sccm are carried out in the nitrogen atmosphere that mass fraction is 99.99%；High temperature cabonization temperature is 850
DEG C, heating rate is 5 DEG C/min, and the processing time is 2h, and carbonized product taking-up is filtered with the sulfuric acid that concentration is 2mol/L
It washs to neutrality, then gained filter residue is dried into 12h in 100 DEG C of vacuum ovens, obtains sulfur doping carbon；
(3) it takes a certain amount of sulfur doping carbon to be packed into sample cell, is placed in tube furnace, under the argon gas protection that mass fraction is 99.99%
950 DEG C, argon flow 250sccm are heated to 9 DEG C/min heating rate, stopping is passed through argon gas, and is passed through gas flow and is
The carbon dioxide of 550sccm, after activating 2h under the conditions of 950 DEG C, stopping is passed through carbon dioxide, continues under 99.99% argon gas
It is cooled to room temperature, takes out material and dries 5h in 130 DEG C of baking ovens to get sulfur doping porous carbon is arrived.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation of the sulfur doping porous carbon based on sterculia seed slag, it is characterised in that steps are as follows:
(1) sterculia seed after making tea removes the peel deseeding, is put into freeze drier and is freeze-dried, and is crushed after dry with plant
Machine crushes, crosses sieve, obtains sterculia seed ground-slag end；
(2) sterculia seed ground-slag end that step (1) obtains and sulfur doping agent are put into nickel crucible, isometric alcohol and water is added
It after being sufficiently mixed uniformly and stands for 24 hours, is put into vacuum oven and is dried, then by dry products therefrom in protective gas
High temperature cabonization is carried out in atmosphere, and carbonized product taking-up is filtered with acid and is washed to neutrality, then gained filter residue is done in vacuum
It is dried in dry case, obtains sulfur doping carbon；
(3) sulfur doping carbon in step (3) is packed into sample cell, be placed in tube furnace, with certain liter under protective gas protection
Warm rate is heated to activation temperature, and stopping is passed through protective gas, and is passed through the oxidizing gas of certain flow, in activation temperature item
Activated under part after a certain period of time, stopping be passed through oxidizing gas, be cooled to room temperature under protective gas atmosphere, take out material and
Drying in oven obtains sulfur doping porous carbon.
2. the preparation of the sulfur doping porous carbon according to claim 1 based on sterculia seed slag, it is characterised in that: the step
(1) temperature being freeze-dried in is -70 ~ -50 DEG C, and vacuum degree is less than 20pa, time 20-24h, and plant pulverizer revolving speed is
1400r/min, sieve mesh number are 100 mesh.
3. the preparation of the sulfur doping porous carbon according to claim 1 based on sterculia seed slag, it is characterised in that: the step
(2) mass ratio of sterculia seed ground-slag end and sulfur doping agent is 20:(1-4 in)；Sulfur doping agent is selected from simple substance in the step (2)
One of sulphur, cysteine, cystine, thioacetic acid, mercaptoethanol and mercaptopropionic acid.
4. the preparation of the sulfur doping porous carbon according to claim 1 based on sterculia seed slag, it is characterised in that: the step
(2) vacuum drying temperature is 100-110 DEG C in, drying time 10-12h；The temperature of step (2) high temperature carbonization is
700-900 DEG C, heating rate is 3-7 DEG C/min, and the processing time is 1-4h.
5. the preparation of the sulfur doping porous carbon according to claim 1 based on sterculia seed slag, it is characterised in that: the protection
Gas is nitrogen, argon gas or the helium that mass fraction is 99.99%, gas flow 100-300sccm.
6. the preparation of the sulfur doping porous carbon according to claim 1 based on sterculia seed slag, it is characterised in that: the step
(2) acid is hydrochloric acid, sulfuric acid or the nitric acid of concentration 1-3mol/L in.
7. the preparation of the sulfur doping porous carbon according to claim 1 based on sterculia seed slag, it is characterised in that: the step
(3) activation temperature is warming up to the heating rate of 8-10 DEG C/min in, stopping is passed through protective gas, then passes to oxidisability gas
Body, oxidizing gas are air, carbon dioxide or vapor, gas flow 500-700sccm.
8. the preparation of the sulfur doping porous carbon according to claim 1 based on sterculia seed slag, it is characterised in that: the step
(3) activation temperature is 800-1000 DEG C in, activation time 1-4h；Drying temperature is 120-150 DEG C in the step (3), is done
The dry time is 4-6h.
9. claim 1-8 it is described in any item based on the sulfur doping porous carbon of sterculia seed slag heavy metal containing wastewater treatment, printing and dyeing
Application in waste water absorption, lithium-sulfur cell, lithium ion battery, sodium-ion battery, supercapacitor and catalyst load.
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