CN106430171B - A kind of the alcohol prosthetic device and alcohol restorative procedure of graphene - Google Patents

A kind of the alcohol prosthetic device and alcohol restorative procedure of graphene Download PDF

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CN106430171B
CN106430171B CN201610986827.3A CN201610986827A CN106430171B CN 106430171 B CN106430171 B CN 106430171B CN 201610986827 A CN201610986827 A CN 201610986827A CN 106430171 B CN106430171 B CN 106430171B
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alcohol
reaction unit
gas
graphene
material placing
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CN106430171A (en
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郝胐
赵伟
汪国庆
刘元杰
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ENN Science and Technology Development Co Ltd
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ENN Science and Technology Development Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/40Electric properties

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Abstract

The present invention relates to technical field of graphene more particularly to the alcohol prosthetic devices and alcohol restorative procedure of a kind of graphene.It can create conditions for the large-scale production of graphene with reparation in reaction unit without carrying out continuous repair in alcohol steam atmosphere to graphene in the case where cooling.Overcome the defect for being difficult to realize large-scale production and the reparation of graphene in the prior art.The embodiment of the present invention provides a kind of alcohol prosthetic device of graphene, comprising: reaction unit;First material placing device, first material placing device includes that feed inlet, discharge port and first blow gas import, for being passed through graphene powder to be repaired, the discharge port is connected to the feed inlet with the feed inlet of the reaction unit, and described first blows gas import for being passed through inert gas;The alcohol steam generation facility is for generating alcohol steam and the alcohol steam being passed through in the reaction unit;Discharging device, the discharging device are connected to the discharge port of the reaction unit.

Description

A kind of the alcohol prosthetic device and alcohol restorative procedure of graphene
Technical field
The present invention relates to technical field of graphene more particularly to the alcohol prosthetic devices and alcohol restorative procedure of a kind of graphene.
Background technique
Since graphene self-discovery, since it is with big theoretical specific surface area, heating conduction outstanding, excellent mechanics The quantum hall effect of performance, higher electron mobility and perfect quantum tunneling effect, half-integer, and make it in electricity The fields such as son, biological medicine, information and the energy all have wide application prospect.
Oxide-reduction method is the maximally efficient method that current low cost prepares graphene, however, passing through this method institute The graphene of preparation usually has vacancy defect and Heteroatom doping defect (mainly oxygen atom), and vacancy defect refers to graphite In six-membered carbon ring on alkene layer, there is one or more carbon atom missing, to make to form vacancy in graphene. Dopant impurity atoms defect refers to that foreign atom is adsorbed on graphene film and is not easily disconnected from or foreign atom directly replaces graphite Carbon atom in alkene structure.These defects make the performance for preparing graphene obtained have a greatly reduced quality.
In order to reduce disadvantages described above, the quality of graphene is improved, needs to repair the structure of graphene, is mostly used at present Method be to be passed through reducibility gas at high temperature, such as hydrogen, ammonia, or be passed through carbon source methane, ethyl alcohol, ethylene etc. to remove Oxygen either repairs vacancy defect.Research is found: best with the repairing effect of alcohols in these renovation agents.
A certain amount of graphene powder to be repaired is usually placed in reacting furnace by the alcohol reparation of graphene at present, and It is passed through alcohol steam into reacting furnace under conditions of isolation air, is rapidly heated to pass through the alcohol steam to the graphene powder It is repaired, it is limited to repair the amount being added every time, and every reparation once needs equipment to cool down, and takes a long time, limits graphene The extensive reparation of powder.
Summary of the invention
The embodiment of the present invention provides the alcohol prosthetic device and alcohol restorative procedure of a kind of graphene, can reaction unit not Continuous repair is carried out in alcohol steam atmosphere to graphene in the case where being cooled down, is the large-scale production and reparation of graphene It creates conditions.
In order to achieve the above objectives, the embodiment of the present invention adopts the following technical scheme that
On the one hand, the embodiment of the present invention provides a kind of alcohol prosthetic device of graphene, comprising:
Reaction unit, reaction unit include inlet port and outlet port;
First material placing device, the first material placing device include that feed inlet, discharge port and first blow gas import, the first charge dress The feed inlet set connects for being passed through graphene powder to be repaired, the discharge port of the first material placing device and the feed inlet of reaction unit Logical, first blows gas import for being passed through inert gas;
Alcohol steam generation facility, alcohol steam generation facility are connected to the feed inlet of reaction unit, and alcohol steam generation facility is used In generation alcohol steam and alcohol steam is passed through in reaction unit;
Discharging device, discharging device are connected to the discharge port of reaction unit.
Optionally, whirlwind feeding device is provided between the discharge port of the first material placing device and the feed inlet of reaction unit, Whirlwind feeding device includes import, gas vent and solid outlet, and the import of whirlwind feeding device goes out with the first material placing device Material mouth connection, the solid outlet of whirlwind feeding device are connected to the feed inlet of reaction unit.
Preferably, the solid outlet of whirlwind feeding device is connected to the feed inlet of reaction unit by second pipe, and second The position of the solid outlet of whirlwind feeding device is provided with second on pipeline and blows gas import, second, which blows gas import, is used for It is passed through inert gas, auxiliary is carried out to the graphene powder in second pipe and is blowed, to be dredged to second pipe.
Further, alcohol steam generation facility includes the second material placing device and heating device, and the second material placing device is for containing Liquid alcohol is put, for heating device for heating to the liquid alcohol, the second material placing device includes that steam (vapor) outlet and third blow Gas import, third blow gas import for being passed through inert gas, and steam (vapor) outlet is connected to the feed inlet of reaction unit.
Preferably, alcohol steam generation facility is connected to the feed inlet of reaction unit by third pipeline, and the of second pipe One end is connected to the solid outlet of whirlwind feeding device, and the first end of third pipeline and the steam (vapor) outlet of alcohol steam generation facility connect Logical, the second end of third pipeline is connected to the feed inlet of reaction unit, and the second end of second pipe is connected to third pipeline.
Optionally, second pipe and/or third pipeline are coated with electric heating cover.
Preferably, discharging device includes gas-solid separating device and collection device, and gas-solid separating device includes that import, gas go out Mouth and solid outlet, the import of gas-solid separating device are connected to the discharge port of reaction unit, collection device and gas-solid separating device Solid outlet connection.
Further, gas-solid separating device includes cyclone separator, and cyclone separator is back taper funnel structure, gas-solid point Gas vent from device is located at the top of back taper funnel structure, and the solid outlet of gas-solid separating device is located at back taper funnel The bottom of structure.
On the other hand, the embodiment of the present invention provides a kind of alcohol restorative procedure of graphene, repairs applied to alcohol as described above Apparatus for coating, alcohol restorative procedure include:
Step 1) is passed through the graphene powder to be repaired of predetermined amount into the first material placing device, blows gas import by first Inert gas is blowed with the first preset flow rate into the first material placing device, graphene powder to be repaired is conveyed into reaction unit In;
Step 2) generates alcohol steam by alcohol steam generation facility and is passed through in reaction unit, so that alcohol steam is as reparation Agent repairs graphene powder to be repaired under preset temperature;
Step 3) blows gas import by first and blows inert gas into the first material placing device with the second preset flow rate, will Graphene powder after the completion of reparation is blown into discharging device.
Preferably, institute's preset temperature is 800-1000 DEG C;
First preset flow rate is 0.5-4L/min;
Second preset flow rate is 10-20L/min.
Preferably, it when alcohol steam generation facility includes the second material placing device and heating device, is filled by alcohol steam generation It sets to generate alcohol steam and alcohol steam is passed through in reaction unit and specifically include:
Liquid alcohol is added in the second material placing device, liquid alcohol is heated by heating device, and is blown by second Import of supplying gas blows inert gas into the second material placing device with third preset flow rate, and the alcohol steam that liquid alcohol is volatilized is brought into instead It answers in device.
Preferably, gas import being blowed into the first material placing device by described first, indifferent gas is blowed with the first preset flow rate Body, before graphene powder to be repaired is conveyed into reaction unit further include: blow gas import to reaction unit by first In inert gas preset time blowed with the 4th preset flow rate, inert gas replacement is carried out to reaction unit.
Preferably, liquid alcohol is 3- butene-1-ol.
The embodiment of the invention provides a kind of alcohol prosthetic device of graphene and alcohol restorative procedures, are carrying out alcohol to graphene When reparation, graphene powder to be repaired can be blown from reaction unit in the case where completely cutting off air conditions and to the reaction unit In be passed through alcohol steam, graphene to be repaired can be continuously conveyed in alcohol steam atmosphere and it is repaired, also, repaired After multiple completion, by adjusting the flow velocity of inert gas, the graphene powder after reparation is blown into discharging device and is gathered up Come, so as to, without carrying out continuous repair in alcohol steam atmosphere to graphene in the case where cooling, be in reaction unit The large-scale production of graphene creates conditions with reparation.It overcomes and enters every time when carrying out alcohol reparation to graphene in the prior art Amount it is limited, every repaired once needs equipment to cool down, and takes a long time and the large-scale production of graphene and reparation are caused The defect of limitation.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the alcohol prosthetic device of graphene provided in an embodiment of the present invention;
Fig. 2 is the structural schematic diagram of the alcohol prosthetic device of another graphene provided in an embodiment of the present invention;
Fig. 3 is the structural schematic diagram of the alcohol prosthetic device of another graphene provided in an embodiment of the present invention;
Fig. 4 is the structural schematic diagram of the alcohol prosthetic device of another graphene provided in an embodiment of the present invention;
Fig. 5 is the structural schematic diagram of the alcohol prosthetic device of another graphene provided in an embodiment of the present invention;
Fig. 6 is a kind of flow diagram of the alcohol restorative procedure of graphene provided in an embodiment of the present invention.
Specific embodiment
With reference to the accompanying drawing the alcohol prosthetic device to a kind of graphene provided in an embodiment of the present invention and alcohol restorative procedure into Row detailed description.
On the one hand, the embodiment of the present invention provides a kind of alcohol prosthetic device of graphene, referring to Fig. 1, comprising:
Reaction unit 1, reaction unit 1 include inlet port and outlet port;
First material placing device 2, the first material placing device 2 blow gas import, the first charge including feed inlet, discharge port and first The feed inlet of device 2 is for being passed through graphene powder to be repaired, the charging of the discharge port and reaction unit of the first material placing device 2 Mouth connection, first blows gas import for being passed through inert gas;
Alcohol steam generation facility 3, alcohol steam generation facility 3 are connected to the feed inlet of reaction unit 1, alcohol steam generation facility 3 for generating alcohol steam and alcohol steam being passed through in reaction unit 1;
Discharging device 4, discharging device 4 are connected to the discharge port of reaction unit 1.
The embodiment of the invention provides a kind of alcohol prosthetic devices of graphene, to be repaired when carrying out alcohol reparation to graphene Multiple graphene powder can be blown from reaction unit 1 in the case where completely cutting off air conditions, and alcohol steam is passed through into reaction unit 1, Graphene to be repaired can be continuously conveyed in alcohol steam atmosphere and it is repaired, also, after repairing completion, led to The flow velocity for overregulating inert gas blows the graphene powder after reparation into discharging device 4, so as in reaction unit 1 without cooling in the case where continuous repair is carried out in alcohol steam atmosphere to graphene, be graphene large-scale production with Reparation creates conditions.The amount entered every time when overcoming in the prior art to graphene progress alcohol reparation is limited, every to have repaired one It is secondary that equipment is needed to cool down, it takes a long time and the large-scale production of graphene and reparation is made to cause the defect limited.
In one embodiment of the invention, discharging device 4 includes gas-solid separating device 41 and collection device 42, gas solid separation dress Setting 41 includes import, gas vent and solid outlet, and the import of gas-solid separating device 41 is connected to the discharge port of reaction unit 1, Collection device 42 is connected to the solid outlet of gas-solid separating device 41.
Gas can be discharged from the gas vent, be kept inside and outside alcohol prosthetic device by the way that gas-solid separating device 41 is arranged Air pressure balance, reduce the pressure-bearing demand of the alcohol prosthetic device, and the graphene powder separated can also be collected In collection device 42.
In one embodiment of the invention, the first material placing device 2 is three-necked flask, and the mouth in the middle part of three-necked flask is feed inlet, A mouth blows gas import for first in other two mouth, another mouth is discharge port.By the way that graphite to be repaired is added thereto Alkene powder, then inert gas is blowed by the first wind blower import, graphene powder to be repaired can be rolled, and will be to be repaired Graphene powder is brought into reaction unit 1.
Wherein, three-necked flask is glass material, by three-necked flask it can be seen that graphene powder to be repaired is rolled-up simultaneously It is blown from the entire fill process into reaction unit 1, and is controlled by the flow velocity to inert gas, it can be to stone to be repaired The inlet amount of black alkene powder is controlled.
Preferably, reaction unit 1 is tube furnace, and the inlet port and outlet port of reaction unit 1 are relatively arranged on tube furnace Both ends.Tube furnace is conducive to the input of graphene powder to be repaired and the output of graphene powder after the reaction was completed.
It wherein, without limitation to the structure of gas-solid separating device 41, as long as can be by the inert gas blown into and graphite Alkene powder separates.
In one embodiment of the invention, gas-solid separating device 41 is cyclone separator, and cyclone separator is back taper funnel Structure, the gas vent of gas-solid separating device 41 are located at the top of back taper funnel structure, and the solid of gas-solid separating device 41 goes out Mouth is located at the bottom of back taper funnel structure.It, can be by centrifugal force by graphene powder to be repaired using cyclone separator Separated from the inert gas, and graphene powder to be repaired separated after can be settled down to by gravity The solid outlet of gas-solid separating device 41, inert gas is then diffused up to be discharged from the gas vent of gas-solid separating device 41, symbol Collaborate the body characteristics of motion, reduces unnecessary energy loss.
Since the graphene powder is lighter, it is easy to overflow from gas vent in the drive of inert gas, it is preferred that gas-solid Dust filtering bag 5 is connected on the gas vent of separator 41.In such manner, it is possible under graphene powder to be repaired is filtered Come, so that it be made to settle down under the effect of gravity, avoids pollution air.
In another embodiment of the present invention, referring to fig. 2, the import of the discharge port and gas-solid separating device 41 of reaction unit 1 Between be additionally provided with heat exchanger 6.It can exchange heat to graphene powder obtained is reacted.
Wherein, the structure of heat exchanging device 6 is without limitation.
In one embodiment of the invention, the import of the discharge port and gas-solid separating device 41 of reaction unit 1 passes through the first pipe Road a connection, heat exchanger 6 include shell 61 and the heat transferring medium being contained in shell 61, at least part folding of first pipe a Embowment is arranged in heat transferring medium.In this way, it is smaller to transporting resistance of the graphene powder in the first pipe a, and And the transfer path of graphene powder can also be increased, improve heat transfer effect.
Wherein, heat transferring medium can be mixture of ice and water.
In one embodiment of the invention, referring to Fig. 3, the feed inlet of the discharge port of the first material placing device 2 and reaction unit 1 it Between be provided with whirlwind feeding device 7, whirlwind feeding device 7 includes import, gas vent and solid outlet, whirlwind feeding device 7 Import be connected to the discharge port of first material placing device 2, the solid outlet of whirlwind feeding device 7 and reaction unit 1 into Material mouth connection.By the way that whirlwind feeding device 7 is arranged, can by centrifugal force by graphene powder to be repaired from the inert gas In separate, and the graphene powder to be repaired to settle down is conveyed into reaction unit 1 by solid outlet, Neng Goushi Now uniform feeding.
In another embodiment of the present invention, the feed inlet of the solid outlet of whirlwind feeding device 7 and reaction unit 1 passes through the Two pipeline b are connected to, and the position of the solid outlet of whirlwind feeding device 7 is provided with second on second pipe b and blows gas import, Second blows gas import for being passed through inert gas, carries out auxiliary to the graphene powder in second pipe b and blows, to second Pipeline b is dredged.
In one embodiment of the invention, referring to fig. 4, alcohol steam generation facility 3 includes the second material placing device 31 and heating dress 32 are set, the second material placing device 31 is for holding liquid alcohol, and heating device 32 is for heating liquid alcohol, the second material placing device 31 include that steam (vapor) outlet and third blow gas import, and third blows gas import for being passed through inert gas, steam (vapor) outlet with react The feed inlet of device 1 is connected to.By heating to liquid alcohol, alcohol steam is evaporated, then is passed through inert gas, can be by alcohol Steam is brought into reaction unit 1.
Wherein, it should be noted that in order to increase the charging of alcohol steam, liquid alcohol can also be stirred, improve liquid The evaporation rate of state alcohol.
Wherein, the second material placing device 31 can be flask, and magnetic agitation can be used when being stirred to liquid alcohol.
In another embodiment of the present invention, the feed inlet of alcohol steam generation facility 3 and the reaction unit 1 passes through third pipe Road c connection, the first end of second pipe b are connected to the solid outlet of whirlwind feeding device 7, the first end and alcohol of third pipeline c The steam (vapor) outlet of steam generation facility 3 is connected to, and the second end of third pipeline c is connected to the feed inlet of reaction unit 1, second pipe The second end of b is connected to third pipeline c.
It in embodiments of the present invention, can be by second by the way that the second end of second pipe b to be connected to third pipeline c When graphene powder in pipeline b is conveyed into third pipeline c, by the inert gas that is passed through in third pipeline c by uniformly defeated It is sent into reaction unit 1.
In another embodiment of the present invention, referring to Fig. 5, second pipe b and/or third pipeline c are coated with electric heating cover 8.The electric heating cover 8 can steam the graphene powder to be repaired by second pipe b and/or the alcohol by third pipeline c Vapour is kept the temperature.In such manner, it is possible to prevent the condensation of the alcohol steam.
On the other hand, the embodiment of the present invention provides a kind of alcohol restorative procedure of graphene, repairs applied to alcohol as described above Apparatus for coating, referring to Fig. 6, alcohol restorative procedure includes:
Step 1) is passed through the graphene powder to be repaired of predetermined amount into the first material placing device, blows gas import by first Inert gas is blowed with the first preset flow rate into the first material placing device, graphene powder to be repaired is conveyed into reaction unit In;
Step 2) generates alcohol steam by alcohol steam generation facility and is passed through in reaction unit, so that alcohol steam is as reparation Agent repairs graphene powder to be repaired under preset temperature;
Step 3) blows gas import by first and blows inert gas into the first material placing device with the second preset flow rate, will Graphene powder after the completion of reparation is blown into discharging device.
The embodiment of the invention provides a kind of alcohol restorative procedures of graphene, to be repaired when carrying out alcohol reparation to graphene Multiple graphene powder can be blown from reaction unit in the case where completely cutting off air conditions, and alcohol steam, energy are passed through into reaction unit Enough graphene to be repaired is continuously conveyed in alcohol steam atmosphere repairs it, also, after repairing completion, passes through Adjust inert gas flow velocity, the graphene powder after reparation is blowed into discharging device, can reaction unit without Continuous repair is carried out in alcohol steam atmosphere to graphene in the case where cooling, is that the large-scale production of graphene and reparation are created Condition.It is limited to overcome the amount that enters every time when carrying out alcohol reparation to graphene in the prior art, every has repaired primary needs to set Make preparation for dropping temperature, take a long time and the defect that makes the large-scale production of graphene and reparation cause limitation.
In one embodiment of the invention, preset temperature is 800-1000 DEG C.Under the preset temperature, the graphene powder When reacting with alcohol steam generation reparation, the oxygen in graphene powder to be repaired becomes small molecule compound such as carbon dioxide and water, It is overflowed from the piece interlayer of graphene powder, can be improved the quality of the graphene powder.
In another embodiment of the present invention, the first preset flow rate is 0.5-4L/min;Second preset flow rate is 10-20L/ min.Using the flow rates, on the one hand the inert gas provides inert atmosphere as protection gas for alcohol prosthetic device, another Aspect, additionally it is possible to graphene powder to be repaired be blown into institute's reaction unit as power source, the graphite after the completion of reparation Alkene powder is blown into discharging device.
It is described that alcohol steam is generated by alcohol steam generation facility and alcohol steam is passed through reaction in one embodiment of the invention It is specifically included in device:
Liquid alcohol is added in the second material placing device, liquid alcohol is heated by heating device, and is blown by second Import of supplying gas blows inert gas into the second material placing device with third preset flow rate, and the alcohol steam that liquid alcohol is volatilized is brought into instead It answers in device.
In embodiments of the present invention, alcohol steam is blowed using inert gas, can be improved the volatile quantity of liquid alcohol, Also the inlet amount of alcohol steam can be controlled.
Preferably, third preset flow rate is 0.2-1L/min.
In another embodiment of the present invention, gas import is blowed into the first material placing device with the first preset flow rate by first Inert gas is blowed, before the graphene powder to be repaired is conveyed into reaction unit further include: blow gas by first Import blows inert gas preset time into reaction unit with the 4th preset flow rate, carries out inert gas to reaction unit and sets It changes.Inert atmosphere is provided for the alcohol reparation reaction of graphene powder.
Preferably, preset time 30min.
Wherein, without limitation to the type of liquid alcohol, liquid alcohol can be ethyl alcohol, or methanol.
In one embodiment of the invention, liquid alcohol is 3- butene-1-ol.Using 3- butene-1-ol to the Graphene powder Body is repaired compared with being repaired using ethyl alcohol, methanol to graphene powder, the repairing effect under same repairing condition Preferably.It theoretically analyzes, since there are vacancy defects in existing graphene powder, is repaired when carrying out annealing to graphene powder When multiple, the oxygen atom in graphene powder can be made to become small-molecule substance and overflowed from graphene powder, but repairing effect It is poor;When being repaired using ethyl alcohol to graphene powder, part ethyl alcohol decomposes release methane gas at high temperature, or Some carbon atoms replace the oxygen atom in graphene powder, and part ethyl alcohol pyrolytic is in ethylene, with graphene powder Addition reaction occurs for the phenyl ring on vacancy periphery, so as to repair vacancy;When being repaired using methanol to graphene powder, Methanol can only release methane gas at high temperature or be removed the oxygen atom in graphene powder by carbon atom, to sky The effect that position is repaired is weaker;When being repaired using 3- butene-1-ol to graphene powder, 3- butene-1-ol can be It is decomposed into adiene cpd under high temperature, it is anti-that Dies-Alder can occur for the phenyl ring at adiene cpd and vacancy defect edge It answers, generates new hexatomic ring, meanwhile, other substances such as methane after 3- butene-1-ol decomposes at high temperature can be played and be removed The effect of oxygen;So ethyl alcohol, methanol and 3- butene-1-ol to the repairing effect of graphene powder be followed successively by 3- butene-1-ol, Ethyl alcohol and methanol.
In addition, we use ethyl alcohol, methanol and 3- butene-1-ol to stone by (800-1000 DEG C) at a certain temperature Black alkene powder is repaired, and carries out conductivity test and Raman Characterization respectively to graphene powder obtained is repaired, As a result as shown in table 1 below.Wherein, conductivity is a physics concept, refers to that the product of the amount and electric field strength in the medium is equal to Conduction current density.The physical significance of conductivity is to indicate the performance of substance conductance.The more big then electric conductivity of conductivity is stronger, instead It is smaller.In general, the hetero atom oxygen of the conductivity of graphene powder and the graphene powder content and vacancy defect it is more Rare pass, the defects of described graphene powder is fewer, and conductivity is higher.There are two typical Raman spies for single-layer graphene Sign is respectively located at 1582cm-1The neighbouring peak G and it is located at 2700cm-1The peak G' of left and right, and for containing defective graphene Sample or edge in graphene, there is also positioned at 1350cm-1The peak defect D of left and right, and it is located at 1620cm-1It is attached The close peak D';The peak D is to be related to the double resonance Raman Process an of defect scattering, therefore the defect of graphene can be reflected in its Raman On the peak D, quantitatively its defect concentration can be studied by the detection to the peak graphite Raman D;The intensity at the peak D and the peak G Than the important parameter for being often used as defect concentration in characterization graphene, it is assumed that the defects of graphene is that the point of a zero dimension lacks It falls into, the average distance between two o'clock is LD, pass through the intensity ratio I at the peak calculated Raman spectrum D and the peak GD/IGIt can be to LDIt carries out It is quantitative, so as to estimate the defect density in graphene, I is generallyd use in Raman CharacterizationD/IGSize characterize The defect density on graphene powder surface, IG/IDBigger description defect concentration is bigger, ID/IGSmaller, description defect concentration is got over It is small.
Table 1
Renovation agent Conductivity (S/m) Raman characterization (ID/IG)
Nothing 800-1100 1.67
Methanol 1500-1800 1.36
Ethyl alcohol 2300-2600 1.21
3- butene-1-ol 2800-3200 0.75
From upper table 1 it is known that carrying out alcohol reparation to graphene powder compares the electricity that graphene powder carries out annealing reparation Conductance is high, ID/IGValue it is small, illustrate to graphene powder carry out alcohol reparation effect it is more preferable.And it is surveyed using 3- butene-1-ol The conductivity highest of examination, ID/IGValue it is minimum, illustrate that 3- butene-1-ol is best to the repairing effect of the graphene powder, Secondary is ethyl alcohol.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.

Claims (12)

1. a kind of alcohol prosthetic device of graphene characterized by comprising
Reaction unit, the reaction unit include inlet port and outlet port;
First material placing device, first material placing device include that feed inlet, discharge port and first blow gas import, and described first contains For the feed inlet of material device for being passed through graphene powder to be repaired, the discharge port of first material placing device reacts dress with described The feed inlet connection set, described first blows gas import for being passed through inert gas;
Alcohol steam generation facility, the alcohol steam generation facility are connected to the feed inlet of the reaction unit, the alcohol steam hair Generating apparatus is for generating alcohol steam and the alcohol steam being passed through in the reaction unit;The alcohol steam generation facility includes the Two material placing devices and heating device, second material placing device are used for for holding liquid alcohol, the heating device to the liquid State alcohol is heated;
Discharging device, the discharging device are connected to the discharge port of the reaction unit.
2. alcohol prosthetic device according to claim 1, which is characterized in that
Whirlwind feeding device is provided between the discharge port of first material placing device and the feed inlet of the reaction unit, it is described Whirlwind feeding device includes import, gas vent and solid outlet, the import of the whirlwind feeding device and first charge The discharge port of device is connected to, and the solid outlet of the whirlwind feeding device is connected to the feed inlet of the reaction unit.
3. alcohol prosthetic device according to claim 2, which is characterized in that
The solid outlet of the whirlwind feeding device is connected to the feed inlet of the reaction unit by second pipe, and described second The position of the solid outlet of the whirlwind feeding device is provided with second on pipeline and blows gas import, described second blows gas Import carries out auxiliary to the graphene powder in the second pipe and blows for being passed through inert gas, to second pipe Road is dredged.
4. alcohol prosthetic device according to claim 1, which is characterized in that
Second material placing device includes steam (vapor) outlet and third blows gas import, and it is lazy for being passed through that the third blows gas import Property gas, the steam (vapor) outlet are connected to the feed inlet of the reaction unit.
5. alcohol prosthetic device according to claim 4, which is characterized in that
The alcohol steam generation facility is connected to the feed inlet of the reaction unit by third pipeline, and the of the second pipe One end is connected to the solid outlet of the whirlwind feeding device, the first end of the third pipeline and the alcohol steam generation facility Steam (vapor) outlet connection, the second end of the third pipeline is connected to the feed inlet of the reaction unit, the second pipe Second end is connected to the third pipeline.
6. alcohol prosthetic device according to claim 5, which is characterized in that
The second pipe and/or the third pipeline are coated with electric heating cover.
7. alcohol prosthetic device according to claim 1, which is characterized in that
The discharging device includes gas-solid separating device and collection device, and the gas-solid separating device includes import, gas vent And solid outlet, the import of the gas-solid separating device are connected to the discharge port of the reaction unit, the collection device and institute State the solid outlet connection of gas-solid separating device.
8. alcohol prosthetic device according to claim 7, which is characterized in that
The gas-solid separating device includes cyclone separator, and the cyclone separator is back taper funnel structure, the gas-solid point From the top that the gas vent of device is located at the back taper funnel structure, the solid outlet of the gas-solid separating device is located at institute State the bottom of back taper funnel structure.
9. a kind of alcohol restorative procedure of graphene, which is characterized in that be applied to such as the described in any item alcohol reparations of claim 1-8 Device, the alcohol restorative procedure include:
It is passed through the graphene powder to be repaired of predetermined amount in the first material placing device of step 1) Xiang Suoshu, blows gas by described first Import blows inert gas into first material placing device with the first preset flow rate, and the graphene powder to be repaired is conveyed Enter in the reaction unit;
Step 2) generates alcohol steam by the alcohol steam generation facility and is passed through in the reaction unit, so that the alcohol steam The graphene powder to be repaired is repaired under preset temperature as renovation agent;
Step 3) blows gas import into the first material placing device by described first and blows inert gas with the second preset flow rate, will Graphene powder after the completion of reparation is blown into the discharging device;
The preset temperature is 800-1000 DEG C;
First preset flow rate is 0.5-4L/min;
Second preset flow rate is 10-20L/min.
10. alcohol restorative procedure according to claim 9, which is characterized in that
It is described to be filled by the alcohol steam generation when the alcohol steam generation facility includes the second material placing device and heating device It sets to generate alcohol steam and the alcohol steam is passed through in the reaction unit and specifically include:
Liquid alcohol is added in second material placing device, the liquid alcohol is heated by the heating device, and leads to It crosses described second and blows gas import and inert gas is blowed with third preset flow rate into second material placing device, by the liquid The alcohol steam of alcohol volatilization is brought into the reaction unit.
11. alcohol restorative procedure according to claim 9, which is characterized in that
It is described to blow gas import into the first material placing device by described first inert gas is blowed with the first preset flow rate, by institute It states before graphene powder to be repaired is conveyed into the reaction unit further include: blow gas import to described by described first Inert gas preset time is blowed with the 4th preset flow rate in reaction unit, inert gas replacement is carried out to the reaction unit.
12. alcohol restorative procedure according to claim 10, which is characterized in that
The liquid alcohol is 3- butene-1-ol.
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