CN106276909B - A kind of method that carbene material is extracted from plant - Google Patents
A kind of method that carbene material is extracted from plant Download PDFInfo
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- CN106276909B CN106276909B CN201510363368.9A CN201510363368A CN106276909B CN 106276909 B CN106276909 B CN 106276909B CN 201510363368 A CN201510363368 A CN 201510363368A CN 106276909 B CN106276909 B CN 106276909B
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Abstract
The invention discloses a kind of method that carbene material is extracted from plant, comprise the following steps:A. the plant material that can be carbonized is put into the vacuum tank of inflated with nitrogen, 3 6h that are carbonized at 500 1800 DEG C obtain carbon block；B. obtained carbon block is put into high-speed shearing machine, 3800 24000rpm rotating speed down cut is the superfine powder of 200 500nm particle diameters；C. obtained superfine powder is put into the container filled with ammonia and inert gas, the 10h of deoxidation 4 at 300 400 DEG C, it is carried out oozing the 180min of ruthenium modification 30 afterwards；D. the superfine powder for oozing ruthenium modification is put into the 10 50Hz low-frequency vibration separator filled with ammonia and carries out the translucent flaky powder that Separation by vibration obtains.The carbene material extremely similar with graphene property can not only be made by method provided by the invention, and the raw material used is reproducible natural plants.
Description
Technical field
The invention belongs to field of graphene, in particular to a kind of method that carbene material is extracted from plant.
Background technology
Graphene (Graphene) be one kind by carbon atom with sp2Hybridized orbit composition hexangle type is in the plane of honeycomb lattice
Film, the two-dimensional material of only one carbon atom thickness, be single-layer graphene, bilayer graphene and multi-layer graphene general designation.
Graphene is known most thin, most hard nano material, and it is almost fully transparent, only absorbs 2.3%
Light；Thermal conductivity factor is up to 5300W/mK, and higher than CNT and diamond, its electron mobility exceedes under normal temperature
15000cm2/ Vs, but it is higher than CNT or silicon crystal, and about 1 Ω m of resistivity, it is lower than copper or silver, for electricity in the world
The minimum material of resistance rate.Because its resistivity is extremely low, the speed of electron transfer is exceedingly fast, thus be expected to can be used to develop it is thinner, lead
Electric speed electronic component or transistor of new generation faster.Because graphene is substantially a kind of transparent, good conductor, also fit
Share to manufacture transparent touch screen, even tabula rasa, solar cell.
Graphene industry still has micromechanics stripping method, epitaxial growth method, oxygen in volume production stage of fumbling, main preparation method
Graphite reducing process and vapour deposition process, wherein graphite oxide reducing process are main preparation sides due to preparing advantage of lower cost
Method.
Chinese patent 201310617981.X, disclose a kind of answering for the graphene that preparation method of graphene is extremely prepared
With.A kind of preparation method of graphene, is concretely comprised the following steps：(1) graphite, the concentrated sulfuric acid, sodium nitrate, potassium permanganate are mixed in ice bath
Reaction 2h is closed, is then transferred in 35 DEG C of water-bath and continues to react 12h, then mixed liquor dilutes 3 times with deionized water, adds certain
The 30%H of volume2O2Solution stirs 30min, and the then hydrochloric acid solution and distillation water washing with 5%, freeze-drying obtains aoxidizing stone
Ink；(2) the graphite oxide ultrasound 1h of step (1) is dispersed in N, uniform 10mg/mL point is formed in N-dimethylformamide solution
Dispersion liquid, and be reducing agent redox graphene at a certain temperature using hydrazine hydrate, it is dried to obtain graphene by washing.
This programme prepares graphite oxide by two step hybrid reactions, significantly reduces reaction temperature, while utilize hydration
Hydrazine reduces as reducing agent, reduction temperature.This method reaction condition is gentle, simple, convenient effective, significantly reduces industry
Metaplasia produces the cost of graphene, graphene electrochemical performance prepared by this method.
The raw material used in such scheme is mainly graphite, while prepares what is used in the method for graphene in the prior art
Raw material is also mostly mineral matter, and these raw materials are non-renewable resources, can not continue to use for a long time.
The content of the invention
It is an object of the invention to provide a kind of method that carbene is extracted from plant, the raw material used in this method is day
Right growing plants, it is complete regenerated resources, while the carbene material prepared is translucent sheet, and existing graphene performance
Extremely similar, hardness is big, has extremely low earth resistivity and high electron mobility, observes under an electron microscope, its is microcosmic
Structure is identical with existing graphene-structured, the plane mesh structure of individual layer hexagonal.
In order to achieve the above object, concrete scheme is as follows：
A kind of method that carbene material is extracted from plant, comprises the following steps:
A. the plant material that can be carbonized is put into the vacuum tank of inflated with nitrogen, the 3-6h that is carbonized at 500-1800 DEG C obtains carbon
Block；
B. obtained carbon block is put into high-speed shearing machine, is 200-500nm in 3800-24000rpm rotating speed down cut
The superfine powder of particle diameter；
C. obtained superfine powder is put into the container filled with ammonia and inert gas, the deoxidation 4- at 300-400 DEG C
10h, it is continued to ooze ruthenium modification 30-180min afterwards；
D. the superfine powder for oozing ruthenium modification is put into the 10-50Hz low-frequency vibration separator filled with ammonia and carried out
Separation by vibration processing, obtained translucent flaky powder is the carbene material.
The present invention, will by the way that by the vacuum tank of selected plant material input inflated with nitrogen, carbon block is obtained after high temperature cabonization
The carbon block is cut into 200-500nm superfine powder in high-speed shearing machine, then obtained superfine powder is put into ammonia and indifferent gas
It is carried out to ooze ruthenium modification after deoxidation in the container of body mixing atmosphere, put into afterwards in low-frequency vibration separator, from low frequency
The translucent flaky powder that vibratory separator air outlet overflows is required plant carbene material.
The carbene material extremely similar with graphene property can not only be made by method provided by the invention, and is made
Raw material is reproducible natural plants.
Further, in step a, the plant material is pricklyash hull, and wild pepper seed, Acacia is young, any of coconut husk.
Further, in step a, the carbonization is carried out several times, it is preferable that can be carried out in four times.
Carbonisation is divided into four progress, raw material carbonization can not only be ensured, meanwhile, it is capable to remove miscellaneous in raw material
Matter.
Further, in step a, the temperature of carbonization is 1000-1200 DEG C, carbonization time 3-4h.According to different material
Characteristic, its be carbonized temperature and time it is different, preferably the carburizing temperature of pricklyash hull and wild pepper seed be 500-800 DEG C, gold
The young carburizing temperature of silk tree is 1000-1300 DEG C, and the carburizing temperature of coconut husk is 1100-1800 DEG C.
Further, in step c, the volume ratio of ammonia and inert gas is 1:5-1:6.
The inert gas is any one in helium, neon, argon gas, Krypton, xenon, preferably argon gas.
Further, in step c, the pressure of ammonia is 0.1-0.3MPa in the container.
Further, in step d, the pressure of ammonia is normal pressure in the low-frequency vibration separator.
Further, in step d, in the low-frequency vibration separator during separating treatment：
Air inlet is opened, air outlet is provided with pressure switch, and the superfine powder of low-frequency vibration separator bottom is bounced by vibrations, deuterium
Lamp is irradiated above it, and when the pressure in low-frequency vibration separator reaches preset value, pressure switch is opened, and part superfine powder exists
Overflowed under the carrying of the wind entered from air inlet from air outlet, the plant carbene material of recovery required for spilling portion is divided into.
Further, also include being passivated processing to obtained plant carbene material after step d.
The carbene material that spilling is separated from low-frequency vibration separator is easily oxidized, and powdered not easy to maintain, is
It is easy to high-volume to preserve, obtained carbene material can be passivated processing.
Further, the Passivation Treatment is specially：Obtained plant carbene material powder is put into fischer-tropsch reactor
Processing is passivated, the temperature of processing is 500-1600 DEG C, pressure 15-60MPa, time 30-80min.
Preferably, the carbene material handled by fischer-tropsch reactor, can be made into bar-shaped tubing, not only be not easy by oxygen
Change, while be easy to deposit.
Embodiment
The present invention is described in further detail below by specific examples of the implementation.
Embodiment 1:
A kind of method that carbene material is extracted from pricklyash hull and wild pepper seed, comprises the following steps:
A. pricklyash hull and wild pepper seed are put into the vacuum tank of inflated with nitrogen, the 4h that is carbonized at 500 DEG C obtains carbon block, carbonisation
Carry out in four times；
B. obtained carbon block is put into high-speed shearing machine, is the ultra-fine of 500nm particle diameters in 3800rpm rotating speed down cut
Powder；
C. obtained superfine powder is put into the container filled with ammonia and argon gas, the volume ratio of ammonia and argon gas is 1:5, ammonia
The pressure of gas is 0.1MPa, the deoxidation 4h at 300 DEG C, it is continued to ooze ruthenium modification 30min afterwards；
D. the low-frequency vibration filled with ammonia that the superfine powder input vibration frequency for oozing ruthenium modification is 50Hz is separated
Carry out Separation by vibration processing in device, the pressure of ammonia be normal pressure in vibratory separator, and opening air inlet, air outlet is provided with pressure
Switch, the superfine powder of low-frequency vibration separator bottom are bounced by vibrations, and deuterium lamp irradiates above it, when in low-frequency vibration separator
Pressure when reaching preset value, pressure switch is opened, and part superfine powder is under the carrying of the wind entered from air inlet from air outlet
Overflow, it is Chinese prickly ash carbene material that spilling portion, which is divided into translucent flaky powder,；
E. Chinese prickly ash carbene material input fischer-tropsch reactor will be obtained and be passivated processing, the temperature of processing is 500 DEG C, pressure
20MPa, time 40min, obtain the bar-shaped carbene tubing of Chinese prickly ash.
Embodiment 2
A kind of method that carbene material is extracted in son from Acacia, it is characterised in that comprise the following steps:
A. by the young input inflated with nitrogen vacuum tank of Acacia, the 5h that is carbonized at 1000 DEG C obtains carbon block, and carbonization is carried out in four times；
B. obtained carbon block is put into high-speed shearing machine, is the super of 300nm particle diameters in 14000rpm rotating speed down cut
Fine powder；
C. obtained superfine powder is put into the container filled with ammonia and argon gas, the volume ratio of ammonia and argon gas is 1:6,
The pressure of ammonia is 0.2MPa, the deoxidation 6h at 350 DEG C, it is continued to ooze ruthenium modification 100min afterwards；
D. the low-frequency vibration filled with ammonia that the superfine powder input vibration frequency for oozing ruthenium modification is 30Hz is separated
Separation by vibration processing is carried out in device, wherein ammonia pressure is normal pressure, opens air inlet, and air outlet is provided with pressure switch, low frequency
The superfine powder of vibratory separator bottom is bounced by vibrations, and deuterium lamp irradiates above it, when the pressure in low-frequency vibration separator reaches
During to preset value, pressure switch is opened, and part superfine powder is overflowed under the carrying of the wind entered from air inlet from air outlet, is overflowed
Part is Acacia son's carbene material for translucent flaky powder；
E. Acacia son's carbene material input fischer-tropsch reactor will be obtained and be passivated processing, the temperature of processing is 1000
DEG C, pressure 45MPa, time 50min, obtain the young bar-shaped carbene tubing of Acacia.
Embodiment 3
A kind of method that carbene material is extracted from coconut husk, it is characterised in that comprise the following steps:
A. coconut husk is put into the vacuum tank of inflated with nitrogen, the 6h that is carbonized at 1800 DEG C obtains carbon block；
B. obtained carbon block is put into high-speed shearing machine, is the super of 200nm particle diameters in 24000rpm rotating speed down cut
Fine powder；
C. obtained superfine powder is put into the container filled with ammonia and argon gas, the volume ratio of ammonia and argon gas is 1:5, ammonia
The pressure of gas is 0.3MPa, the deoxidation 10h at 400 DEG C, afterwards, it is continued to ooze ruthenium modification 180min；
D. the low-frequency vibration filled with ammonia that the superfine powder input vibration frequency for oozing ruthenium modification is 10Hz is separated
Separation by vibration processing is carried out in device, wherein ammonia pressure is normal pressure, opens air inlet, and air outlet is provided with pressure switch, low frequency
The superfine powder of vibratory separator bottom is bounced by vibrations, and deuterium lamp irradiates above it, when the pressure in low-frequency vibration separator reaches
During to preset value, pressure switch is opened, and part superfine powder is overflowed under the carrying of the wind entered from air inlet from air outlet, is overflowed
Part is coconut husk carbene material for translucent flaky powder；
E. obtained coconut husk carbene material input fischer-tropsch reactor being passivated processing, the temperature of processing is 1600 DEG C,
Pressure 60MPa, time 80min, obtain the bar-shaped carbene tubing of coconut husk.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention type, for this area
For technical staff, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made is any
Modification, equivalent substitution, improvement etc., should be included in the scope of the protection.
Claims (7)
- A kind of 1. method that carbene material is extracted from plant, it is characterised in that comprise the following steps:A. the plant material that can be carbonized is put into the vacuum tank of inflated with nitrogen, the 3-6h that is carbonized at 500-1800 DEG C obtains carbon block； The plant material is pricklyash hull and wild pepper seed；B. obtained carbon block is put into high-speed shearing machine, is 200-500nm particle diameters in 3800-24000rpm rotating speed down cut Superfine powder；C. obtained superfine powder is put into the container filled with ammonia and inert gas, the deoxidation 4-10h at 300-400 DEG C, it It is continued afterwards to ooze ruthenium modification 30-180min；The volume ratio of above-mentioned ammonia and inert gas is 1:5-1:6, it is described The pressure of ammonia is 0.1-0.3MPa in container；D. the superfine powder for oozing ruthenium modification is put into the 10-50Hz low-frequency vibration separator filled with ammonia and vibrated Separating treatment, obtained translucent flaky powder are the carbene material.
- A kind of 2. method that carbene material is extracted from plant according to claim 1, it is characterised in that in step a, institute Carbonization is stated to carry out several times.
- A kind of 3. method that carbene material is extracted from plant according to claim 1, it is characterised in that in step a, carbon The temperature of change is 1000-1200 DEG C, carbonization time 3-4h.
- A kind of 4. method that carbene material is extracted from plant according to claim 1, it is characterised in that in step d, institute The pressure for stating ammonia in low-frequency vibration separator is normal pressure.
- A kind of 5. method that carbene material is extracted from plant according to claim 1, it is characterised in that in step d, In the low-frequency vibration separator during separating treatment：Air inlet is opened, air outlet is provided with pressure switch, and the superfine powder of low-frequency vibration separator bottom is bounced by vibrations, and deuterium lamp exists Its top is irradiated, and when the pressure in low-frequency vibration separator reaches preset value, pressure switch is opened, and part superfine powder is from entering Overflowed under the carrying for the wind that air port enters from air outlet, spilling portion is divided into the plant carbene material of required recovery.
- 6. a kind of method that carbene material is extracted from plant according to claim 1, it is characterised in that after step d Also include being passivated processing to obtained plant carbene material.
- 7. a kind of method that carbene material is extracted from plant according to claim 6, it is characterised in that at the passivation Reason is specially：Obtained plant carbene material powder is put into fischer-tropsch reactor and is passivated processing, the temperature of processing is 500-1600 DEG C, pressure 15-60MPa, time 30-80min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807210A (en) * | 2012-08-20 | 2012-12-05 | 上海交通大学 | Method for preparing graphene by biomass derived carbonaceous mesophase |
| CN103332687A (en) * | 2013-07-11 | 2013-10-02 | 黑龙江大学 | Method for preparing boron and nitrogen codoped graphitized nano carbon by taking biomass as carbon source |
| CN103935986A (en) * | 2014-02-28 | 2014-07-23 | 中国科学院宁波材料技术与工程研究所 | Method for high yield preparation of graphene by using biologic carbon source material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807210A (en) * | 2012-08-20 | 2012-12-05 | 上海交通大学 | Method for preparing graphene by biomass derived carbonaceous mesophase |
| CN103332687A (en) * | 2013-07-11 | 2013-10-02 | 黑龙江大学 | Method for preparing boron and nitrogen codoped graphitized nano carbon by taking biomass as carbon source |
| CN103935986A (en) * | 2014-02-28 | 2014-07-23 | 中国科学院宁波材料技术与工程研究所 | Method for high yield preparation of graphene by using biologic carbon source material |
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