Utility model content
In view of this, the utility model proposes a kind of grapheme material process units, Graphene material is produced using this device
Material, sticky material shifts simply efficiently between reactor, reduces production difficulty, improves Graphene production efficiency.
This utility model provides a kind of grapheme material process units, including:First reaction component, the second reaction component and
Negative pressure produces assembly;
Described first reaction component includes the first reative cell and the outlet of the first material located at described first reative cell bottom;
Described second reaction component includes the second reative cell and second material entrance;
Connecting path between described first material outlet and described second material entrance is provided with valve;
The aspirating hole that described negative pressure produces assembly is indoor located at the described second reaction.
Preferably, described second material entrance is located at the second reactor top, described first material outlet and described second
The described connecting path of material inlet is set to shortest length.
Preferably, described first reaction component includes the first rabbling mechanism;
Described first rabbling mechanism includes the first agitator of helical-ribbon type, and described first agitator is located at the described first reaction
Chamber interior.
Preferably, described first reaction component also includes temperature-detecting device, and the test side of described temperature-detecting device sets
Inside described first reative cell.
Preferably, the test side of described temperature-detecting device is built in described first agitator.
Preferably, described second reaction component includes the second rabbling mechanism;
Described second rabbling mechanism includes the second agitator of vane type, and described second agitator is indoor located at the second reaction
Portion.
Preferably, described second reative cell includes second material outlet;
Described second material outlet is arranged at side wall or the bottom of described second reative cell.
Preferably, the first reaction component includes ultrasonic disperse assembly;
Described ultrasonic disperse assembly includes ultrasonic bath and ultrasonic generator;
It is outdoor that described ultrasonic bath is set in described first reaction;
Described ultrasonic generator is located at described ultrasonic bath outer surface.
Preferably, described first reaction component includes the first tempering coil and the first heater block, described second reaction group
Part includes the second tempering coil and the second heater block;
Described first tempering coil is sheathed on the periphery of described first reative cell, and described first tempering coil is used for accommodating to be adjusted
Geothermal liquid;Described first heater block is used for heating the indoor material of described first reaction;
Described second tempering coil is sheathed on the periphery of described second reative cell, and described second tempering coil is used for accommodating to be adjusted
Geothermal liquid;Described second heater block is used for heating the indoor material of described second reaction.
This utility model additionally provides a kind of grapheme material production system, is provided with above-mentioned grapheme material and produces dress
Put.
With respect to prior art, of the present utility model have the technical effect that:
A kind of grapheme material process units that this utility model provides, the first reative cell of the first reaction component is used for containing
Put material, after the completion of material implements reaction process in the first reative cell, open valve, by being arranged on the first reative cell bottom
First material exports, and under the influence of gravity, material moves to second material Way in, enters second from second material entrance
Second reative cell of reaction component, carries out the technological process of next step.Now, negative pressure produces assembly and starts, continuous from aspirating hole
Pumping, makes the pressure of the second reative cell be less than the pressure of the first reative cell, the second reative cell is produced to the first reative cell due to pressure reduction
Raw pull of vacuum, material is sucked from the first reative cell and is transferred to the second reative cell, in the common work of gravity and negative pressure-pumping power
With under complete the transfer of material, thus reducing viscous and dense material transfer difficulty.This device is applied widely, for various materials
All there is good transfer effect, especially, oxidation-reduction method prepares its middle reaction mass viscosity of grapheme material greatly, uses
This device is applied and is produced in the technique of grapheme material in oxidation-reduction method, and viscous and dense material can be overcome to be difficult the problem shifting, fall
Low production difficulty, effectively improves the production efficiency of grapheme material.
Specific embodiment
It should be noted that in the case of not conflicting, the embodiment in this utility model and the feature in embodiment can
To be mutually combined.To describe this utility model below with reference to the accompanying drawings and in conjunction with the embodiments in detail.
The technical process that oxidation-reduction method produces grapheme material is using strong oxidizer such as concentrated sulphuric acid, concentrated nitric acid, Gao Meng
Graphite oxidation is become graphite oxide by sour potassium etc., and oxidizing process interts some oxygen-containing functional groups in graphite layers, thus increasing
Graphite layers are away from then so that it may form monolayer or several layers of graphene oxide after sonicated a period of time, then with reducing by force
Graphene oxide is reduced into Graphene by agent such as hydrazine hydrate, sodium borohydride etc..The intermediate product stickiness that above-mentioned reaction produces is big,
In whole Graphene production process, the transfer to this high viscosity material, increases difficulty to continuous production processes.
This utility model provides a kind of grapheme material process units, including:First reaction component 1, the second reaction component 2
Produce assembly 3 with negative pressure;
First reaction component 1 includes the first reative cell 11 and the outlet of the first material located at the first reative cell 11 bottom 12;
Second reaction component 2 includes the second reative cell 21 and second material entrance 22;
Connecting path between first material outlet 12 and second material entrance 22 is provided with valve 4;
Negative pressure produces the aspirating hole of assembly 3 in described second reative cell 21.
This device, in the technical process producing grapheme material, has good transfer effect to material, especially viscous
The material transfer of thick solid-liquid system, is particularly well-suited to based on oxidation-reduction method large-scale continuous production grapheme material.
Refer to Fig. 1, a kind of grapheme material process units of embodiment of this utility model offer is provided
Structure.
First reative cell 11 of the first reaction component 1 is used for holding material, and material implements reaction work in the first reative cell 11
After the completion of skill, open valve 4, export 12 by the first material being arranged on the first reative cell 11 bottom, under the influence of gravity,
Material moves to second material entrance 22 direction, enters the second reative cell 21 of the second reaction component 2 from second material entrance 22,
Carry out the technological process of next step.Now, negative pressure produces assembly 3 and starts, and is constantly evacuated from aspirating hole, makes the second reative cell 21
Pressure is less than the pressure of the first reative cell 11, and the second reative cell 21 produces 21 raw pulls of vacuum due to pressure reduction to the first reative cell, will
Material sucks from the first reative cell 11 and is transferred to the second reative cell 21, completes under the collective effect of gravity and negative pressure-pumping power
The transfer of material, thus reduce viscous and dense material transfer difficulty.This device is applied widely, all has very well for various materials
Transfer effect, especially, it is big, using the application of this device that oxidation-reduction method prepares its middle reaction mass viscosity of grapheme material
Produce in the technique of grapheme material in oxidation-reduction method, viscous and dense material can be overcome to be difficult the problem shifting, reduce production difficulty,
Effectively improve the production efficiency of grapheme material.
First reative cell 11 and the second reative cell 21 can be by metal materials, and such as stainless steel is constituted.For some tools
Mordant material system(As graphite-inorganic strong protonic acid system), or subsequent chemical reaction need add corrosivity former
Material(As KMnO4)Situation, the corrosion resistance of metal material is poor, if from it as reaction vessel, easily causing container
Corrosion, the service life of impact equipment, can be solved using the method increasing corrosion-resistant coating in reaction chamber wall, corrosion-resistant coating
Preferably polytetrafluoroethylene or polypropylene coating.Politef or polypropylene can resist the corrosion of strong acid and strong base, can effectively enough prolong
Long service life of equipment;In addition, because oxidation-reduction method produces grapheme material process, middle product material viscosity is big, each
During material transfer, serious material loss is caused due to glutinous wall phenomenon, thus leading to the decline of graphene product yield.Adopt
It is, coating unusual light to improve material and stick wall phenomenon, reduce material and shifting with another advantage of politef
Loss in journey, increased the yield of grapheme material.
Preferably, located at the second reative cell 21 top, first material outlet 12 is entered second material entrance 22 with second material
The connecting path of mouth 22 is set to shortest length.Specifically, by the first reaction component 1 frame high setting, first material is made to export 12
Position be higher than the second reaction component 2 second material entrance 22 position, then the first reative cell 11 is higher than the second reative cell 21.
First material outlet 12 located at the bottom of the first reative cell 11, second material entrance 22 located at the top of the second reative cell 21, the
One material outlet 12 and second material entrance 22 are connected by pipeline, and pipeline is set to shortest length, and pipeline arranges valve 4,
Form the shortest transport distance, by the opening and closing of the transfering channel of the on-off control material of valve 4.
When needing transfer after material reaction, open valve 4, negative pressure produces assembly 3 and starts, start to be evacuated, the second reaction
Formation pressure reduction between room 21 and the first reative cell 11, produces the suction to material, and one side material can be subject to two reative cells
Between pressure reduction produce pull of vacuum and move;On the other hand, material also can be flowed downward due to the gravity of itself, two power-assisteds
Simultaneously facilitate material transfer, along with path is set to the shortest transport distance between two reaction components, and then reached more
Good transfer effect, reduce further the transfer difficulty of high viscosity material, improves the production efficiency of grapheme material.
Further, the first reaction component 1 includes the first rabbling mechanism 13;
First rabbling mechanism 12 includes the first agitator 131 of helical-ribbon type, and the first agitator 131 is located at the described first reaction
Inside room 11.
Refer to the knot of the grapheme material process units of another embodiment that this utility model shown in Fig. 2 provides
Structure.
It will be understood by those skilled in the art that for chemical reaction, especially liquid phase reactor, being much to need side dispersion to stir
Mix side to carry out, or carry out immediately after dispersion, to prevent the material after disperseing from reuniting again.Therefore, this utility model
The process units that embodiment provides can be not only used for material reaction, can be also used for dispersion stirring, especially can be used as right
Graphite oxide carries out the device disperseing to peel off.For example:It can as the dispersal device of Graphitic pretreatment, graphite oxidation intercalation
Device etc..Therefore the Graphene process units that this utility model provides includes the first rabbling mechanism 13, the first rabbling mechanism 13 can
With the first agitator 131 using helical-ribbon type.First agitator 131 can not only be realized stirring while reacting, and improves liquid
The effect of phase reaction uniformity, the stirring vane of helical-ribbon type is while rotating stirring moreover it is possible to produce boosting materials downward
Thrust.That is, in the present embodiment, when material transitions into the second reative cell 21, receive vacuum draw simultaneously, stir
Mix and promote the effect with gravity to move downward, therefore to high-viscosity material, there is more preferable transfer ability, further increase stone
Black alkene material production efficiency.
Further, chemical method especially oxidation-reduction method produces grapheme material, typically can adopt the tool such as strong acid and strong base
There is the reaction reagent of Strong oxdiative reproducibility, during oxidative deamination process, temperature change is very big, can be timely for the ease of operator
Understand the temperature in the first reative cell 21, the grapheme material process units that the present embodiment provides further preferably includes temperature detection
Device 14, the test side of this temperature-detecting device 14 inside described first reative cell 11, with to the first reative cell 11 intracavity
Material system temperature detected.Said temperature detection means can be thermometer, temperature sensor etc..Setting said temperature
Detection means 14 contributes to the temperature that operator understands dispersion intracavity material in time, is that operator is subsequently adjusted first in time
The operation of reative cell 11 cavity temperature provides foundation, it also avoid the generation of security incident.
Optionally, the test side of temperature-detecting device 14 is built in the first agitator 131, preferably by temperature detection
End, such as thermometer, temperature sensor are built in the shaft of the first agitator 131, have both enabled real-time detection reaction indoor
Temperature of charge, be easy to operator's control material course of reaction;The blade that simultaneously also avoid the first agitator 131 is stirred
In journey, the situation at collision detection end occurs, and further increases the security reliability of Graphene process units.
Known to the skilled person in the art, chemical method production is prepared grapheme material and is generally required through multiple chemical reaction mistakes
Journey, each reaction needs independent operation to react.Therefore, this grapheme material process units includes the second reaction component 2, and material exists
It is transferred to after completing reaction in first reaction component 1 in second reaction component 2 and continue next step reaction.Second reaction component 2
In second reative cell 21, the material in the second reative cell 21 can quickly be stirred by setting vane type the second agitator 23 effectively
Uniformly, help speed up the dispersion of material, improve reaction uniformity.Preferably, the agitator arm of the second agitator 231 can be arranged
Multigroup, increase mixing uniformity, improve stirring efficiency, improve reaction uniformity further.
Another effect of the first agitator 131 and the second agitator 231 is, the uprushing of the amount of localized heat of balancing response material
Or anticlimax, reach the quick effect transmitting temperature, the temperature in reative cell is uniformly distributed, improve grapheme material further and produce
The security reliability of device.
In addition, the second reative cell 21 includes second material outlet, for the ease of the discharging of grapheme material product, the second thing
Material outlet is arranged at side wall or the bottom of the second reative cell 21.When redox reaction completes, grapheme material can be from the second thing
Material exports direct discharging, is easy to operator and collects.
It will be understood by those skilled in the art that after usual redox reaction terminates, grapheme material also needs to through undue
From and be dried, therefore, second material outlet may be connected to the interface separating drying device, continues to complete and produces grapheme material
Subsequent technique.
Prepare grapheme material using oxidation-reduction method in production, because single-layer graphene is very thin, easily reunite, therefore instead
Will be by being stirred continuously dispersion during answering.Therefore further, Graphene process units includes ultrasonic disperse assembly 15, ultrasonic point
Scattered assembly 15 utilizes the superior vibration dispersion ability in liquid medium of ultrasound wave, can complete to Graphene redox reaction
During material dispersion.Refer to the structure of the grapheme material process units of the another embodiment shown in Fig. 3.
Ultrasonic disperse assembly 15 includes ultrasonic bath 151 and ultrasonic generator 152, and it is anti-that ultrasonic bath set 151 is located at first
Answer outside room 11, ultrasonic generator 152 is located at ultrasonic bath 151 outer surface.Ultrasonic bath 151 is used for holding liquid medium, liquid
Medium is used for conduct ultrasound.Ultrasonic generator 152 can be using commercially available conventional Ultrasound agitator in the market.Ultrasonic shake
Swing device by contacting with the outer surface of the first reative cell 11, by sonification medium, ultrasound wave be transmitted in the first reative cell 11,
So that ultrasonic disperse is carried out to the material in the first reative cell 11.Specifically, can be according to the shape of the first reative cell 11 and production
The requirement of condition arranges multiple ultrasonic generators 152, to meet the Production requirement of grapheme material.
Further, for the ease of adding liquid medium into ultrasonic bath 151, can set in ultrasonic bath 151 side wall
It is equipped with import, this import connects with ultrasonic bath 151.Can be entered into by this import by this ultrasound wave conduction liquid medium
In ultrasonic bath 151.Furthermore it is also possible to be provided with drain port, connects in this drain port and ultrasonic bath 151, for by sonification medium
Liquid is discharged, and this drain port can be provided with valve.Certainly, ultrasonic bath 151 is further preferably provided with export, this outlet with ultrasonic
Connection in liquid bath 151;It is arranged on the top of import, the effect of overfall can be played.Or, it is furthermore preferred that liquid level also can be arranged
Detector, when liquid level detector detects liquid level and exceeds highest liquid level, can be automatically stopped the injection of sonification medium, or send report
Alert prompting operator.
Ultrasonic disperse assembly 15 can be used cooperatively by grapheme material process units with the first rabbling mechanism 13, enter simultaneously
Row ultrasonic agitation and mechanical agitation.During dispersed with stirring, ultrasonic generator 152 sends ultrasound wave, and ultrasound wave passes through ultrasonic
Medium is transferred to, inside the material in the first reative cell 11, realize the scattered effect of supersonic vibration;The machinery that agitator applies stirs
The power of mixing helps speed up the flowing of material, to promote the transmission of ultrasound wave, especially for sticky material(As graphite oxide-
Water material), it is favorably improved ultrasound wave and is fully contacted with material, and then improve the uniformity of material dispersion, thus it also avoid
Situations such as runaway reaction that material hot-spot causes.Therefore, the process units range that this utility model embodiment provides
Extensively, for various materials, especially sticky solid-liquid system material also has uniform dispersion effect, safe to use.By its
It is applied to the preparation of grapheme material, be favorably improved solid material scattered uniformity in liquid medium, it helps thing
Material reaction completely, and then improves the homogeneity of product quality.
Further, because grapheme material produces course of reaction, the temperature of material often suddenly height suddenly low, its reason has
Two:On the one hand it is because redox reaction would generally discharge substantial amounts of heat, leads to temperature of charge quickly to raise;Another
Aspect, ultrasound wave and material phase separation can make the temperature of dispersion intracavity material suddenly raise, but for some reactions, ultrasound wave
The temperature producing is often too high or too low, is unfavorable for that reacts is smoothed out.Therefore need to adjust the thing in the first reative cell 11
Material temperature degree, to control response speed.This utility model the first reaction component 1 is provided with the first tempering coil 16 and the first heating
Part 17, the first tempering coil 16 is sheathed on the periphery of the first reative cell 1, and the first heater block 17 is used for heating the first reative cell
Material in 11.Specifically, for realizing preferably thermoregulation effect, the first tempering coil 16 can be close to the side of the first reative cell 11
Wall and/or bottom setting.First tempering coil 16 plays cooling effect, prevents that the temperature rise in ultrasonic procedure is too high to bring bad shadow
Ring;First heater block 17 is then to improve response speed for improving the temperature in ultrasonic procedure.By the first tempering coil
16 and first the using cooperatively of heater block 17, reach the thermoregulator purpose to the first reative cell 11 material reaction.First tune
Winchester disk pipe 16 is used for accommodating temperature regulating liquid, and certainly, the first tempering coil 16 is also equipped with entrance and exit, for temperature regulating liquid
Injection and outflow, take away the heat in the first reative cell 11 by the flowing of temperature regulating liquid.For example, intercalation is being carried out to graphite
During oxidation, oxidation reaction liberated heat and ultrasound wave are too high with the heat of material interaction release, can cause
Reaction rate is too fast, is now passed through cold water into the first tempering coil 16, by controlling the cold water stream in the first tempering coil 16
The dynamic heat taking away material in the first reative cell 11.To reach the purpose of the temperature of adjustment the first reative cell 11 intracavity, Jin Erda
To the effect controlling reaction rate, the quality of further stable prod.
It is again based on adjusting the purpose of the second reative cell 21 intracavity temperature of charge, the second reaction component 2 setting second tune
Winchester disk pipe 25 and the second heater block 26, when in course of reaction blanking easily cause when too fast temperature heat up too high it is therefore desirable to
Lowered the temperature by the second tempering coil 25;And blanking completes after backwash terminates, material needs to be incubated a timing at a certain temperature
Between, therefore need to heat keeping temperature by the second heater block 26.
This utility model additionally provides a kind of grapheme material production system, is provided with above-mentioned grapheme material and produces dress
Put.Specifically, in order to realize the continuous production of grapheme material, this utility model can also include:
Purification devices, for purifying to above-mentioned graphene oxide Solid-liquid mixture, obtain graphene oxide;
Drying device, for being dried graphene oxide material;
Reducing mechanism, for being pulverized dried graphene oxide, obtains graphene oxide powder;
High temperature reduction device, with reducing to by graphene oxide powder, obtains graphene powder.
Specifically, second material outlet can be connected with purification devices material inlet, to realize grapheme material
Continuous production.
Above-mentioned grapheme material production system specifically can be used for preparing Graphene and functionalized graphite's alkene, above-mentioned functionalization
Graphene for example, graphene oxide, amination graphene, carboxylated Graphene, sulfonated Graphene, sulfhydrylation Graphene, cyanogen
Base Graphene, nitro Graphene, boronate Graphene, phosphate Graphene, hydroxylating Graphene, sulfhydrylation Graphene, methyl
Graphite alkene, allylation Graphene, trifluoromethylation Graphene, myristalated Graphene, octadecyl graphite alkene, fluorine
Graphite alkene, bromination Graphene, chlorination Graphene and iodate Graphene etc..
The foregoing is only preferred embodiment of the present utility model, not in order to limit this utility model, all this
Within the spirit of utility model and principle, any modification, equivalent substitution and improvement made etc., should be included in this utility model
Protection domain within.