CN106276909A - A kind of method extracting carbene material from plant - Google Patents
A kind of method extracting carbene material from plant Download PDFInfo
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- CN106276909A CN106276909A CN201510363368.9A CN201510363368A CN106276909A CN 106276909 A CN106276909 A CN 106276909A CN 201510363368 A CN201510363368 A CN 201510363368A CN 106276909 A CN106276909 A CN 106276909A
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Abstract
The invention discloses a kind of from plant extract carbene material method, comprise the following steps: a. by can carbonization plant material put into inflated with nitrogen vacuum tank in, at 500 1800 DEG C, carbonization 3 6h obtains carbon block；B. the carbon block obtained being put in high-speed shearing machine, the rotating speed down cut of 3800 24000rpm is the micropowder of 200 500nm particle diameters；C. the micropowder obtained is put in the container being filled with ammonia and noble gas, deoxidation 4 10h at 300 400 DEG C, afterwards it is oozed ruthenium modification 30 180min；D. by ooze the micropowder that ruthenium modification crosses put into 10 50Hz be filled with the low-frequency vibration separator of ammonia in carry out the translucent flaky powder that Separation by vibration obtains.The method provided by the present invention can not only make the carbene material the most similar with Graphene character, and the raw material used is reproducible natural plants.
Description
Technical field
The invention belongs to field of graphene, from plant, extract carbon in particular to one
The method of alkene material.
Background technology
Graphene (Graphene) be a kind of by carbon atom with sp2Hybrid orbital composition six
Angle-style is the flat film of honeycomb lattice, the two-dimensional material of only one of which carbon atom thickness,
It it is the general designation of single-layer graphene, bilayer graphene and multi-layer graphene.
Graphene is the thinnest, the hardest known nano material, and it is the most thoroughly
Bright, only absorb the light of 2.3%；Heat conductivity is up to 5300W/m K, higher than carbon nanometer
Pipe and diamond, under room temperature, its electron mobility is more than 15000cm2/ V s, again than nanometer
Carbon pipe or silicon wafer height, and resistivity only about 1 Ω m are lower than copper or silver, in the world
The material that resistivity is minimum.Because its resistivity is extremely low, the speed of electron transfer is exceedingly fast, because of
This is expected to can be used to develop thinner, conduction speed a new generation's electronic component or crystalline substance faster
Body pipe.Due to a kind of transparent, good conductor of Graphene, also be adapted for for
Manufacture transparent touch screen, tabula rasa, even solaode.
Graphene industry is still in the volume production stage of fumbling, and main preparation method has micromechanics to shell
From method, epitaxial growth method, graphite oxide reducing process and vapour deposition process, wherein aoxidize stone
Ink reducing process is relatively low due to preparation cost, is main preparation methods.
Chinese patent 201310617981.X, discloses the preparation method pole of a kind of Graphene
The application of its Graphene prepared.The preparation method of a kind of Graphene, concretely comprises the following steps:
(1) by graphite, concentrated sulphuric acid, sodium nitrate, potassium permanganate hybrid reaction 2h in ice bath,
Then proceeding to continue reaction 12h in the water-bath of 35 DEG C, then mixed liquor deionized water is dilute
Release 3 times, add the 30%H of certain volume2O2Solution stirring 30min, then with 5% salt
Acid solution and distilled water wash, lyophilization obtains graphite oxide；(2) by step (1)
The ultrasonic 1h of graphite oxide is dispersed in N, is formed uniformly in N-dimethylformamide solution
The dispersion liquid of 10mg/mL, and utilize hydrazine hydrate for reducing agent oxygen reduction at a certain temperature
Functionalized graphene, is dried to obtain Graphene through washing.
This programme prepares graphite oxide by two step hybrid reactions, significantly reduces reaction
Temperature, utilizes hydrazine hydrate to reduce as reducing agent, reduction temperature simultaneously.The method is reacted
Mild condition, simple, convenient effectively, significantly reduce industrialized production Graphene
Cost, Graphene electrochemical performance prepared by the method.
The raw material used in such scheme is mainly graphite, prepares stone in prior art simultaneously
The raw material used in the method for ink alkene is the most also mineral, and these raw materials be can not
Regenerated resources, it is impossible to persistently use for a long time.
Summary of the invention
It is an object of the invention to provide a kind of method extracting carbene from plant, the method
The raw material of middle use is the plant of spontaneous growth, for complete regenerated resources, the carbon prepared simultaneously
Alkene material is translucent lamellar, the most similar with existing Graphene performance, and hardness is big, tool
Having extremely low earth resistivity and high electron mobility, observe under an electron microscope, it is micro-
See structure identical with existing graphene-structured, the plane reticular structure of monolayer hexagonal.
In order to achieve the above object, concrete scheme is as follows:
A kind of method extracting carbene material from plant, comprises the following steps:
A. by can carbonization plant material put into inflated with nitrogen vacuum tank in, 500-1800 DEG C
Lower carbonization 3-6h obtains carbon block；
B. the carbon block obtained is put in high-speed shearing machine, at the rotating speed of 3800-24000rpm
Down cut is the micropowder of 200-500nm particle diameter；
C. the micropowder obtained is put in the container being filled with ammonia and noble gas,
Deoxidation 4-10h at 300-400 DEG C, proceeds to ooze ruthenium modification to it afterwards
30-180min；
D. the low frequency being filled with ammonia of the micropowder input 10-50Hz that ruthenium modification is crossed will be oozed
Carrying out Separation by vibration process in vibratory separator, the translucent flaky powder obtained is described
Carbene material.
The present invention by selected plant material being put in the vacuum tank of inflated with nitrogen, pyrocarbon
Obtain carbon block after change, this carbon block is cut into the ultra-fine of 200-500nm in high-speed shearing machine
Powder, then the micropowder obtained input ammonia is mixed with noble gas deoxidation in the container of atmosphere
Afterwards it is oozed ruthenium modification, put into afterwards in low-frequency vibration separator, from low frequency vibration
The translucent flaky powder that flow separator air outlet overflows is required plant carbene material.
The method provided by the present invention can not only be made the most similar with Graphene character
Carbene material, and the raw material used is reproducible natural plants.
Further, in step a, described plant material is pricklyash hull, Semen Pericarpium Zanthoxyli, and Acacia farnesiana Willd. is young,
Any one in coconut husk.
Further, in step a, described carbonization is carried out several times, it is preferable that can divide four
Secondary carry out.
Carbonisation is divided into four times and carrying out, can not only ensure raw material carbonization, meanwhile,
Impurity in raw material can be removed.
Further, in step a, the temperature of carbonization is 1000-1200 DEG C, and carbonization time is
3-4h.According to the characteristic of different material, the temperature and time of its carbonization is the most different, preferably
The carburizing temperature of pricklyash hull and Semen Pericarpium Zanthoxyli is 500-800 DEG C, and the carburizing temperature of Acacia farnesiana Willd. son is
1000-1300 DEG C, the carburizing temperature of coconut husk is 1100-1800 DEG C.
Further, in step c, the volume ratio of ammonia and noble gas is 1:5-1:6.
Described noble gas is any one in helium, neon, argon, Krypton, xenon,
It is preferably argon.
Further, in step c, in described container, the pressure of ammonia is 0.1-0.3MPa.
Further, in step d, in described low-frequency vibration separator, the pressure of ammonia is normal
Pressure.
Further, in step d, in described low-frequency vibration separator during separating treatment:
Opening air inlet, air outlet is provided with pressure switch, surpassing of low-frequency vibration separator bottom
Fine powder 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 micropowder is taken the wind entered from air inlet
Leukorrhagia overflows from air outlet, overflows the plant carbene material that part is required recovery.
Further, also include after step d that the plant carbene material to obtaining is passivated
Process.
The carbene material separating spilling from low-frequency vibration separator is the most oxidized, and powder
Powder is difficult to preserve, and preserves for the ease of high-volume, can be carried out by the carbene material that obtain
Passivation Treatment.
Further, described Passivation Treatment is particularly as follows: the plant carbene material powder that will obtain
Being passivated in putting into fischer-tropsch reactor processing, the temperature of process is 500-1600 DEG C, pressure
15-60MPa, time 30-80min.
Preferably, through the carbene material that fischer-tropsch reactor processes, can be made into bar-shaped
Tubing, is not only difficult to oxidized, simultaneously facilitates and deposit.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail.
Embodiment 1:
A kind of method extracting carbene material from pricklyash hull and Semen Pericarpium Zanthoxyli, comprises the following steps:
A. pricklyash hull and Semen Pericarpium Zanthoxyli are put in the vacuum tank of inflated with nitrogen, carbonization 4h at 500 DEG C
Obtaining carbon block, carbonisation is carried out in four times；
B. the carbon block obtained is put in high-speed shearing machine, at the rotating speed down cut of 3800rpm
Micropowder for 500nm particle diameter；
C. the micropowder obtained is put in the container being filled with ammonia and argon, ammonia and argon
Volume ratio be 1:5, the pressure of ammonia is 0.1MPa, and at 300 DEG C, deoxidation 4h, the most right
It proceeds to ooze ruthenium modification 30min；
D. by ooze the micropowder that ruthenium modification crosses put into frequency of vibration be 50Hz be filled with ammonia
Separation by vibration process is carried out, the pressure of ammonia in vibratory separator in the low-frequency vibration separator of gas
Power is normal pressure, opens air inlet, and air outlet is provided with pressure switch, low-frequency vibration separator
The micropowder of bottom is 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 micropowder is entering from air inlet
Wind carrying under from air outlet overflow, overflow part be Pericarpium Zanthoxyli for translucent flaky powder
Carbene material；
E. will obtain Pericarpium Zanthoxyli carbene material input fischer-tropsch reactor to be passivated processing, process
Temperature is 500 DEG C, pressure 20MPa, time 40min, obtains Pericarpium Zanthoxyli bar-shaped carbene tubing.
Embodiment 2
A kind of from Acacia farnesiana Willd. son extract carbene material method, it is characterised in that include with
Lower step:
A. putting in inflated with nitrogen vacuum tank by Acacia farnesiana Willd. son, at 1000 DEG C, carbonization 5h obtains carbon
Block, carbonization is carried out in four times；
B. the carbon block obtained is put in high-speed shearing machine, at the rotating speed down cut of 14000rpm
Micropowder for 300nm particle diameter；
C. the micropowder obtained is put in the container being filled with ammonia and argon, ammonia and argon
The volume ratio of gas is 1:6, and the pressure of ammonia is 0.2MPa, deoxidation 6h at 350 DEG C, afterwards
Proceed to ooze ruthenium modification 100min to it；
D. by ooze the micropowder that ruthenium modification crosses put into frequency of vibration be 30Hz be filled with ammonia
Carrying out Separation by vibration process in the low-frequency vibration separator of gas, wherein ammonia pressure is normal pressure, beats
Driving air port into, air outlet is provided with pressure switch, the micropowder of low-frequency vibration separator bottom
Being bounced by vibrations, deuterium lamp irradiates above it, when the pressure in low-frequency vibration separator reaches pre-
If during value, pressure switch is opened, and part micropowder is under the carrying of the wind entered from air inlet
Overflow from air outlet, overflow part and be Acacia farnesiana Willd. son's carbene material for translucent flaky powder；
E. will obtain Acacia farnesiana Willd. son's carbene material input fischer-tropsch reactor to be passivated processing, place
The temperature of reason is 1000 DEG C, pressure 45MPa, time 50min, obtains the young bar-shaped carbon of Acacia farnesiana Willd.
Alkene tubing.
Embodiment 3
A kind of method extracting carbene material from coconut husk, it is characterised in that include following step
Rapid:
A. being put into by coconut husk in the vacuum tank of inflated with nitrogen, at 1800 DEG C, carbonization 6h obtains carbon block；
B. the carbon block obtained is put in high-speed shearing machine, at the rotating speed down cut of 24000rpm
Micropowder for 200nm particle diameter；
C. the micropowder obtained is put in the container being filled with ammonia and argon, ammonia and argon
Volume ratio be 1:5, the pressure of ammonia is 0.3MPa, deoxidation 10h at 400 DEG C, afterwards,
Proceed to ooze ruthenium modification 180min to it；
D. by ooze the micropowder that ruthenium modification crosses put into frequency of vibration be 10Hz be filled with ammonia
Carrying out Separation by vibration process in the low-frequency vibration separator of gas, wherein ammonia pressure is normal pressure,
Opening air inlet, air outlet is provided with pressure switch, low-frequency vibration separator bottom ultra-fine
Powder is bounced by vibrations, and deuterium lamp irradiates above it, when the pressure in low-frequency vibration separator reaches
During preset value, pressure switch is opened, and part micropowder is carried the wind entered from air inlet
Under from air outlet overflow, overflow part be coconut husk carbene material for translucent flaky powder；
E. it is passivated processing by the coconut husk carbene material obtained input fischer-tropsch reactor, processes
Temperature be 1600 DEG C, pressure 60MPa, time 80min, obtain coconut husk bar-shaped carbene tubing.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention
Type, for a person skilled in the art, the present invention can have various modifications and variations.
All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement made
Deng, should be included within the scope of the present invention.
Claims (10)
1. the method extracting carbene material from plant, it is characterised in that include following
Step:
A. by can carbonization plant material put into inflated with nitrogen vacuum tank in, 500-1800 DEG C
Lower carbonization 3-6h obtains carbon block；
B. the carbon block obtained is put in high-speed shearing machine, at the rotating speed of 3800-24000rpm
Down cut is the micropowder of 200-500nm particle diameter；
C. the micropowder obtained is put in the container being filled with ammonia and noble gas,
Deoxidation 4-10h at 300-400 DEG C, proceeds to ooze ruthenium modification to it afterwards
30-180min；
D. the low frequency being filled with ammonia of the micropowder input 10-50Hz that ruthenium modification is crossed will be oozed
Carrying out Separation by vibration process in vibratory separator, the translucent flaky powder obtained is described
Carbene material.
A kind of method extracting carbene material from plant the most according to claim 1,
It is characterized in that, in step a, described plant material is pricklyash hull, Semen Pericarpium Zanthoxyli, and Acacia farnesiana Willd. is young,
Any one in coconut husk.
A kind of method extracting carbene material from plant the most according to claim 1,
It is characterized in that, in step a, described carbonization is carried out several times.
A kind of method extracting carbene material from plant the most according to claim 1,
It is characterized in that, in step a, the temperature of carbonization is 1000-1200 DEG C, and carbonization time is
3-4h。
A kind of method extracting carbene material from plant the most according to claim 1,
It is characterized in that, in step c, the volume ratio of ammonia and noble gas is 1:5-1:6.
A kind of method extracting carbene material from plant the most according to claim 5,
It is characterized in that, in step c, in described container, the pressure of ammonia is 0.1-0.3MPa.
A kind of method extracting carbene material from plant the most according to claim 1,
It is characterized in that, in step d, in described low-frequency vibration separator, the pressure of ammonia is normal pressure.
A kind of method extracting carbene material from plant the most according to claim 1,
It is characterized in that, in step d, in described low-frequency vibration separator during separating treatment:
Opening air inlet, air outlet is provided with pressure switch, surpassing of low-frequency vibration separator bottom
Fine powder 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 micropowder is taken the wind entered from air inlet
Leukorrhagia overflows from air outlet, overflows the plant carbene material that part is required recovery.
A kind of method extracting carbene material from plant the most according to claim 1,
It is characterized in that, also include after step d the plant carbene material obtained is passivated place
Reason.
A kind of method extracting carbene material from plant the most according to claim 9,
It is characterized in that, described Passivation Treatment is particularly as follows: throw the plant carbene material powder obtained
Being passivated in entering fischer-tropsch reactor processing, the temperature of process is 500-1600 DEG C, pressure
15-60MPa, time 30-80min.
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| CN109627907A (en) * | 2018-11-17 | 2019-04-16 | 上海亿尚金属有限公司 | A kind of static conductive thermal dispersant coatings and preparation method thereof |
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| CN102807210B (en) * | 2012-08-20 | 2014-06-25 | 上海交通大学 | Method for preparing graphene by biomass derived carbonaceous mesophase |
| CN103332687B (en) * | 2013-07-11 | 2015-12-02 | 黑龙江大学 | A kind of take biomass as the method that carbon source prepares the nitrogen co-doped graphitization nano carbon of boron |
| CN103935986B (en) * | 2014-02-28 | 2016-03-30 | 中国科学院宁波材料技术与工程研究所 | A kind of method preparing Graphene with biological carbon source material high yield |
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| CN109627907A (en) * | 2018-11-17 | 2019-04-16 | 上海亿尚金属有限公司 | A kind of static conductive thermal dispersant coatings and preparation method thereof |
| CN109627907B (en) * | 2018-11-17 | 2020-09-01 | 上海亿尚金属有限公司 | Static-conducting heat-dissipating coating and preparation method thereof |
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