CN209020386U - A kind of consersion unit being used to prepare graphene - Google Patents

Abstract

The utility model discloses a kind of consersion units for being used to prepare graphene, including reaction kettle, reaction kettle includes being located above, to prepare the reaction kettle barrel of graphene, the inside of reaction kettle barrel be equipped with for when convey liquid charging stock with the fitting of reaction kettle cylinder madial wall with the liquid feeding device that removes the residual powder material of reaction kettle cylinder madial wall and prevent drop from splashing and with the agitating device sufficiently reacted for raw material, it is equipped with positioned at the top of reaction kettle barrel for cleaning reaction kettle barrel when the reaction is finished and reduces graphene viscosity for the spray equipment of its outflow.Above-mentioned consersion unit can solve intercalator and can strut graphite linings, bring it about violent volume expansion, and increase with system viscosity, so that the problem of mobility reduces, so as to improve mass-transfer efficiency of equipment under the conditions of high expansion ratio, high viscosity, and equipment is conducive to highly viscous substance discharging.

Description

A kind of consersion unit being used to prepare graphene

Technical field

The utility model relates to chemical production technical field, in particular to a kind of consersion unit for being used to prepare graphene.

Background technique

With the high speed development of science and technology, demand of the market to new material is consequently increased, as the basis of development, new material Mass, it is standardized preparation be unable to do without corresponding consersion unit.

In recent years, graphene is concerned as the favorite of field of new materials, and the preparation method about graphene is also a variety of Multiplicity, including CVD, epitaxial growth, organic matter high-temperature catalytic graphitization, graphite oxidation reduction method, liquid phase intercalation stripping method.In stone In the preparation method of black alkene, using graphite is maximum as the preparation method yield of raw material, cost is minimum, therefore it is also widely used.Its In, during liquid phase prepares graphene, intercalator can strut graphite linings, violent volume expansion occur, and with body It is that viscosity increases, so that mobility reduces, these mass-transfer efficiencies that will lead to reactant reduce and since heat discharges unevenness Security risk that is even and increasing reaction, and the increase of viscosity will lead to discharging difficulty and increase, and be easy to cause equipment internal residual The problems such as reactant.

Therefore, how to avoid causing the mass-transfer efficiency of reactant to reduce due to high expansion ratio and high viscosity, be ability The current technical issues that need to address of field technique personnel.

Utility model content

The purpose of the utility model is to provide a kind of consersion unit for being used to prepare graphene, which be can solve Intercalator can strut graphite linings, violent volume expansion be brought it about, and increase with system viscosity, so that mobility reduces The problem of, so as to improve the mass-transfer efficiency of reactant under the conditions of high expansion ratio, high viscosity.

To achieve the above object, the utility model provides a kind of consersion unit for being used to prepare graphene, including reaction kettle, The reaction kettle includes the reaction kettle barrel being located above, to prepare graphene, and the inside of the reaction kettle barrel, which is equipped with, to be used In being bonded with the reaction kettle cylinder madial wall when conveying liquid charging stock to remove the residual of the reaction kettle cylinder madial wall Powder material and the liquid feeding device for preventing drop from splashing and with the agitating device sufficiently reacted for raw material, are located at described The top of reaction kettle barrel is equipped with for cleaning the reaction kettle barrel when the reaction is finished and reducing graphene viscosity for it The spray equipment of outflow.

Preferably, the reaction kettle further includes being located at the reaction kettle barrel lower section, the discharge port to export graphene, The inside of the discharge port is equipped with the valve to control the discharge port opening and closing.

Preferably, the inner sidewall of the reaction kettle is equipped with to etch-proof coating.

Preferably, the liquid feeding device include looped pipeline to convey liquid charging stock and several with default Angle is set to the looped pipeline periphery, the outlet to be bonded with the inner sidewall for reacting kettle barrel.

Preferably, the agitating device includes being located in the middle stirring rod, being fixed in the stirring rod and to stir side First mixing component of edge material and below first mixing component and with for lower section material seethe upwards the Two mixing components.

Preferably, the valve includes interconnecting piece to be fixedly connected with the inner sidewall of the discharge port and being capable of edge The axial direction flexible pars contractilis above and below of the interconnecting piece；

The pars contractilis is equipped with positioned at top and for reacting kettle barrel bottom with described when the pars contractilis retracts downwards The flange of portion's closed impaction and positioned at the flange lower section and for when the pars contractilis stretches out upwards open, when described The valve discharge port closed when pars contractilis retracts downwards.

It preferably, further include for guaranteeing leakproofness when the flange is with the reaction kettle cylinder body bottom closed impaction Sealing ring.

Preferably, further include set on the agitating device two sides, to for liquid charging stock be converted to droplet be added it is described anti- Kettle barrel is answered to guarantee the spraying feeding device of reaction uniformity.

It preferably, further include being set to the reaction kettle barrel top, the exhaust gas absorption device to prevent exhaust emission.

It preferably, further include outside the reaction kettle barrel, the driving device to drive the agitating device.

Relative to above-mentioned background technique, the utility model is directed to the different requirements for preparing graphene, devises and is used to prepare The consersion unit of graphene, during liquid phase prepares graphene, intercalator can strut graphite linings, and violent volume occurs Expansion, and with system viscosity increase so that mobility reduce, these will lead to reactant mass-transfer efficiencies reduce and due to Heat release is uneven and increases the security risk of reaction, and the increase of viscosity will lead to discharging difficulty and increase, and be easy to cause The problems such as equipment internal residual reactant, therefore, the special consersion unit of liquid phase intercalation removing exploitation for graphene is ten It is point necessary, and the consersion unit can also be applied to the reaction system of other product viscosities increase.

The above-mentioned consersion unit for being used to prepare graphene includes reaction kettle, and reaction kettle includes the reaction kettle cylinder being located above Body, the raw material for preparing graphene react in reacting kettle barrel with reactant and finally prepare graphene slurry, reaction kettle cylinder The inside of body be equipped with liquid feeding device and agitating device, wherein when conveying liquid charging stock, liquid feeding device with react The fitting of kettle barrel inner sidewall, can be such that liquid charging stock flows down along kettle wall, on the one hand, can remove reaction kettle barrel so in this way On the other hand the residual powder material of inner sidewall is also possible to prevent fluid spills in this way；Agitating device enables to slurries or more It seethes, and when the viscosity of reaction system is higher, agitating device still ensures that raw material mixes and reacts abundant；Specifically, Agitating device, which can be realized, to be rotated forward and rotates backward, and is rotated forward convenient for mixing, is rotated backward convenient for discharging.Above equipment It further include spray equipment, spray equipment is located at the top of reaction kettle barrel, and when the reaction is finished, spray equipment can not only clean Kettle barrel is reacted, and graphene viscosity can be reduced according to actual needs in order to material outflow.So, by anti- Answer setting liquid feeding device, agitating device and spray equipment in kettle barrel that equipment can be improved in high expansion ratio, high viscosity Under the conditions of mass transfer efficiency, and equipment be conducive to highly viscous substance discharging.

Detailed description of the invention

In order to illustrate the embodiment of the utility model or the technical proposal in the existing technology more clearly, below will be to embodiment Or attached drawing needed to be used in the description of the prior art is briefly described, it should be apparent that, the accompanying drawings in the following description is only It is the embodiments of the present invention, for those of ordinary skill in the art, without creative efforts, also Other attached drawings can be obtained according to the attached drawing of offer.

Fig. 1 shows to be used to prepare the structure of the reaction kettle of the consersion unit of graphene provided by the utility model embodiment It is intended to；

Fig. 2 is the vertical view that the reaction kettle of consersion unit of graphene is used to prepare provided by the utility model embodiment Figure；

Fig. 3 is the liquid feeding device that the consersion unit of graphene is used to prepare provided by the utility model embodiment Structural schematic diagram；

Fig. 4 is the valve mechanism signal that the consersion unit of graphene is used to prepare provided by the utility model embodiment Figure.

Wherein:

1- reaction kettle, 11- reaction kettle barrel, 12- discharge port, 2- liquid feeding device, 21- looped pipeline, 22- outlet, 3- agitating device, 31- stirring rod, the first mixing component of 32-, the second mixing component of 33-, 4- spray equipment, 5- valve, 51- connect Socket part, 52- pars contractilis, 53- flange, 54- valve discharge port, 55- sealing ring.

Specific embodiment

The following will be combined with the drawings in the embodiments of the present invention, carries out the technical scheme in the embodiment of the utility model Clearly and completely describe, it is clear that the described embodiments are only a part of the embodiments of the utility model, rather than whole Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are without making creative work Every other embodiment obtained, fall within the protection scope of the utility model.

The core of the utility model is to provide a kind of consersion unit for being used to prepare graphene, which can solve Intercalator can strut graphite linings, violent volume expansion be brought it about, and increase with system viscosity, so that mobility reduces The problem of, to improve the mass-transfer efficiency of high expansion ratio, high viscosity reactant.

In order to make those skilled in the art more fully understand the utility model, with reference to the accompanying drawing and specifically The utility model is described in further detail for embodiment.

It should be noted that the nouns of locality such as " top, lower section " described below are all based on defined in Figure of description.

Please refer to figs. 1 to 4, and Fig. 1 is the consersion unit that graphene is used to prepare provided by the utility model embodiment Reaction kettle structural schematic diagram；Fig. 2 is the consersion unit that graphene is used to prepare provided by the utility model embodiment The top view of reaction kettle；Fig. 3 be the utility model embodiment provided by be used to prepare graphene consersion unit liquid into Expect the structural schematic diagram of device；Fig. 4 is the valve that the consersion unit of graphene is used to prepare provided by the utility model embodiment Door schematic diagram.

The consersion unit of graphene, including reaction kettle 1, reaction kettle 1 are used to prepare provided by the utility model embodiment It is to react to generate graphene and by container derived from graphene for raw material.Reaction kettle 1 includes the reaction kettle barrel 11 being located above, It powder material, liquid charging stock and is used to prepare the reactant of graphene and is reacted in reaction kettle barrel 11 and finally prepare stone Black alkene slurry；Reaction kettle barrel 11 includes columnar structured and positioned at columnar structured lower section the taper knot being located above Structure, the main body reaction chamber of the above-mentioned columnar structured raw material that graphene is as prepared with pyramidal structure.

Further, the inside for reacting kettle barrel 11 is equipped with liquid feeding device 2 and agitating device 3, wherein works as conveying When liquid charging stock, liquid feeding device 2 is bonded with 11 inner sidewall of kettle barrel is reacted, and liquid charging stock can be made along reaction kettle in this way 11 inner sidewall of cylinder flows down, and so, can not only remove the residual powder material of reaction 11 inner sidewall of kettle barrel, Er Qieke Drop is caused to splash to avoid during being directly added into liquid charging stock.

Agitating device 3 can be such that slurries seethe up and down, and when the viscosity of reaction system is higher, agitating device 3 is remained to Guarantee that raw material mixes and reacts abundant；It rotates forward and rotates backward specifically, agitating device 3 can be realized, rotate forward It can be mixed convenient for raw material, rotating backward can discharge convenient for the graphene generated.

In addition, above equipment further includes spray equipment 4, spray equipment 4 is located at the top of reaction kettle barrel 11, when reaction is tied Shu Shi, on the one hand, spray equipment 4 can clean the inner sidewall of reaction kettle barrel 11, on the other hand, and according to actual needs, spray Device 4 can be used for diluting highly viscous material to reduce its viscosity, consequently facilitating material flows out.

In the present embodiment, reaction kettle 1 further includes the discharge port 12 positioned at bottom, wherein discharge port 12 is specifically as follows Columnar structured, the diameter of the columnar structured discharge port can be set as 300 to 400mm range according to the specification for preparing material It is interior；And discharge port 12 is located at 11 lower section of reaction kettle barrel, and effect is to export reacted graphene obtained to lower one of work Sequence.

Specifically, the inside of discharge port 12 is equipped with valve 5, valve 5 is embedded in the inner sidewall of columnar discharge port 12 On, the effect of valve 5 is can to control the opening and closing of discharge port 12, can open and close discharge port 12 in time in this way to guarantee to react The overall stability of kettle 1.

More particularly, which can be set to telescopic valve, the telescopic valve include interconnecting piece 51 and Pars contractilis 52, interconnecting piece 51 with the inner sidewall of discharge port 12 to be fixedly connected, and pars contractilis 52 can be along interconnecting piece 51 Axial upper and lower stretching motion.Pars contractilis 52 is equipped with the flange 53 positioned at top and the valve positioned at the lower section of flange 53 discharges Mouthfuls 54, wherein flange 53 can be set to disk of the diameter greater than 12 diameter of discharge port of reaction kettle 1, valve discharge port 54 with The discharge port 12 of reaction kettle 1 is connected to.When pars contractilis 52 downwards retract when, flange 53 can with react 11 bottom closure pressure of kettle barrel Tightly, at this point, valve 5 is closed；When pars contractilis 52 stretches out upwards, valve discharge port 54 exposes, at this point, valve 5 is opened.

That is, when pars contractilis 52 to reaction kettle barrel 11 inside rise when, valve 5 open, material can be from valve The discharging pipeline that discharge port 54 flows out to 1 lower part of reaction kettle and connect with reaction kettle 1；When pars contractilis 52 is retracted to discharge port 12 When, valve 5 is closed, and valve discharge port 54 is bonded with the inner sidewall of interconnecting piece 51 at this time, and material cannot be defeated from valve discharge port 54 Out.

In order to guarantee leakproofness of the flange 53 in conjunction with reaction 11 bottom of kettle barrel when valve 5 is closed, can combine Place's setting sealing ring 55, the sealing ring 55 can be set to the seal washer of polytetrafluoro rubber, which can guarantee method Orchid 53 is combined closely with 11 bottom of kettle barrel is reacted.

In addition, it should be noted that, the inner sidewall of reaction kettle 1 is equipped with to etch-proof coating, for example, can react The inner sidewall of kettle 1 is coated with the coating or enamel coating of polytetrafluoroethylene (PTFE), reaction kettle 1 can be effectively prevent to prepare in this way Corrosion failure occurs for the process of graphene.Certainly, according to actual needs, agitating device 3, spray equipment 4 and valve 5 can be with The coating of polytetrafluoroethylene (PTFE) is set, so as to prevent from corroding, protects stabilized structure.

Liquid feeding device 2 is fixed on the place suitable for reading of reaction 11 inner sidewall of kettle barrel by the way of coil pipe, specifically, Liquid feeding device 2 includes looped pipeline 21 and several are set to the outlet 22 of 21 periphery of looped pipeline, for example, can go out Erection joint at mouth 22, and the connector and looped pipeline 21 are formed with default angle, according to actual working conditions, preset angle It can be set in the angular range of 30 to 60 degree.

Wherein, looped pipeline 21 is to convey liquid charging stock, the outlet 22 of liquid feeding device 2 can with react kettle barrel 11 inner sidewall fitting；Compared with the structure being vertically arranged, such coil arrangement can be to its inside reaction kettle barrel 11 More spaces are reserved in the setting of his component, and will not be had an impact to the work of other component, outlet 22 and looped pipeline 21 formation inclination angles can wash away the inner sidewall of reaction kettle barrel 11 more in large area, so as to maximumlly remove reaction kettle cylinder Remaining powder material on 11 inner sidewall of body；In addition, the addition of multiple spot can also be such that raw material mixes in advance, stirring can be shortened in this way Time.

Certainly, according to actual needs, delivery pump and flowmeter can also be installed in looped pipeline 21, so as to accurate The liquid charging stock injected to the inside of reaction kettle barrel 11 is controlled, advantageously ensures that the stabilization of reaction 11 inside raw material of kettle barrel reaction Property.

Since reaction late phase reaction system volume acutely expands, viscosity increases simultaneously, can seriously affect mass transfer effect, because This, agitating device 3 can be set to include the first mixing part for being located in the middle stirring rod 31 and being fixed on stirring rod 31 Part 32 and the second mixing component 33, the first mixing component 32 can be set to frame type stirring component, and the second mixing component 33 can be with Double helical-ribbon type mixing components are set as, frame type stirring component can be stirred to react the material at 11 edge of kettle barrel, the second mixing part Part 33 can be set to 32 lower section of the first mixing component, and the second mixing component 33 can seethe upwards lower section material；So, It reacts the available sufficient mixing of material in kettle barrel 11 and reacts, when mixing component reversion, be also convenient for the stone of preparation Black alkene discharging.

Certainly, according to actual needs, above-mentioned consersion unit further includes the driving device for driving agitating device 3 to run, and is considered The exhaust gas of corrosivity and the reaction solution and generation that splash to reaction may corrode driving device, and driving device can be set to It reacts outside kettle barrel 11, can be driven by driving chain between agitating device 3 and driving device, and the driving device has Body is motor.

In order to optimize above-described embodiment, consersion unit further includes spraying feeding device, spraying feeding device can be set in Two side positions of agitating device 3, when conveying corrosivity is low, viscosity is small, is not easy the fluid sample (such as intercalation stripping agent) splashed When, it can be added by spraying feeding device inside reaction kettle barrel 11.Spraying feeding device can be converted to liquid charging stock The droplet of tinyization can guarantee the uniformity of reaction in this way, can also reduce the speed of stirring and shorten the time of reaction；Together When, tiny droplet forms tiny conversion zone, can be too fast to avoid local reaction, heat release excessively acutely caused by part Bumping is overheated, so the requirement of circulating cooling system also can be reduced accordingly, demand can be more easily satisfied in air-cooled and water cooling.

Certainly, according to actual needs, two feed points can be set in spraying feeding device, and are respectively arranged on stirring rod 31 Two sides, for example, two spray points also can be set in spray equipment 4, so, two spray points and two spraying feed points minute It is not placed on the four direction of stirring rod 31, is in this way when can guarantee the uniform cleaning of charging without dead angle.

On the basis of the above, above-mentioned consersion unit further includes the exhaust gas absorption device set on 11 top of reaction kettle barrel, by In the process that reaction system is the great expansion of volume, it can rapidly be released stress using unlimited system, but reacted in order to prevent The exhaust gas of process is discharged into environment, and on 1 top of reaction kettle by the exhaust gas absorption device of negative pressure on cover, exhaust gas absorption device passes through negative The substances such as gas, mist, the cigarette that reaction generates are siphoned away by turbine and are sent in waste gas absorption tower by pressure, and waste gas absorption tower is again Waste liquid concentration after spray-absorption exhaust gas is discharged into wastewater disposal basin, is focused on together with the waste water handled in elution process.

In addition, according to actual needs, can also install mobile blower device additional, blower device provides heat with electric heating Wind, blower device is for the drying after the cleaning of reaction kettle 1, and blower device can be removed after drying, in case it is normal to influence reaction kettle 1 Working condition, disturbing reaction.

It should be noted that in the present specification, such as first and second etc relational terms are used merely to one Entity is distinguished with other several entities, and without necessarily requiring or implying between these entities, there are any this actual Relationship or sequence.

The consersion unit provided by the utility model for being used to prepare graphene is described in detail above.Herein Specific case is applied to be expounded the principles of the present invention and embodiment, the explanation of above example is only intended to Help understands the method and its core concept of the utility model.It should be pointed out that coming for those skilled in the art It says, without departing from the principle of this utility model, several improvements and modifications can be made to this utility model, these change Into in the protection scope for also falling into the utility model claims with modification.

Claims (10)

1. a kind of consersion unit for being used to prepare graphene, including reaction kettle (1), the reaction kettle (1) includes being located above, using To prepare the reaction kettle barrel (11) of graphene, which is characterized in that the inside of reaction kettle barrel (11) is equipped with for when defeated It send and reacts the fitting of kettle barrel (11) inner sidewall with described when liquid charging stock to remove the residual of described reaction kettle barrel (11) inner sidewall Stay powder material and the liquid feeding device (2) that prevents drop from splashing and with the agitating device (3) sufficiently reacted for raw material, Top positioned at reaction kettle barrel (11) is equipped with for cleaning the reaction kettle barrel (11) when the reaction is finished and reducing The spray equipment (4) that graphene viscosity flows out for it.

2. the consersion unit according to claim 1 for being used to prepare graphene, which is characterized in that the reaction kettle (1) is also Including being located at reaction kettle barrel (11) lower section, the discharge port (12) to export graphene, the discharge port (12) it is interior Portion is equipped with the valve (5) to control the discharge port (12) opening and closing.

3. the consersion unit according to claim 2 for being used to prepare graphene, which is characterized in that the reaction kettle (1) Inner sidewall is equipped with to etch-proof coating.

4. the consersion unit according to claim 3 for being used to prepare graphene, which is characterized in that the liquid feeding device It (2) include to convey the looped pipeline of liquid charging stock (21) and several with default angle are set to the looped pipeline (21) Periphery, the outlet (22) to be bonded with the inner sidewall for reacting kettle barrel (11).

5. the consersion unit according to claim 4 for being used to prepare graphene, which is characterized in that the agitating device (3) Including being located in the middle stirring rod (31), being fixed in the stirring rod (31) and the first mixing component to stir edge material (32) it and is set to below first mixing component (32) and with the second mixing component seethed upwards for lower section material (33)。

6. the consersion unit according to claim 5 for being used to prepare graphene, which is characterized in that the valve (5) includes To the interconnecting piece (51) that is fixedly connected with the inner sidewall of the discharge port (12) and can be along the interconnecting piece (51) The axial pars contractilis (52) to stretch above and below；

The pars contractilis (52) be equipped with positioned at top and for when the pars contractilis (52) downwards retract when and the reaction kettle cylinder The flange (53) and be located at the lower section of the flange (53) and be used to work as the pars contractilis (52) that body (11) bottom closure compresses The valve discharge port (54) opened when stretching out upwards, closed when the pars contractilis (52) retracts downwards.

7. the consersion unit according to claim 6 for being used to prepare graphene, which is characterized in that further include for when described Flange (53) with it is described react kettle barrel (11) bottom closure compress when guarantee leakproofness sealing ring (55).

8. the consersion unit according to any one of claims 1 to 7 for being used to prepare graphene, which is characterized in that further include The reaction kettle barrel (11) is added to guarantee set on the agitating device (3) two sides, to be converted to droplet for liquid charging stock React the spraying feeding device of uniformity.

9. the consersion unit according to any one of claims 1 to 7 for being used to prepare graphene, which is characterized in that further include Above the reaction kettle barrel (11), the exhaust gas absorption device to prevent exhaust emission.

10. the consersion unit according to claim 9 for being used to prepare graphene, which is characterized in that further include set on described React kettle barrel (11) outside, the driving device to drive the agitating device (3).