CN204727614U - The device of high-purity carbon nanotube is prepared in automatization - Google Patents
The device of high-purity carbon nanotube is prepared in automatization Download PDFInfo
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- CN204727614U CN204727614U CN201520300339.3U CN201520300339U CN204727614U CN 204727614 U CN204727614 U CN 204727614U CN 201520300339 U CN201520300339 U CN 201520300339U CN 204727614 U CN204727614 U CN 204727614U
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Abstract
The utility model relates to the device that high-purity carbon nanotube is prepared in a kind of automatization, it comprises reactant e Foerderanlage, chemical reaction equipment, collection device, Furnace Temperature Controlling System and vacuum pump apparatus, raw material, catalyzer and reducing gas are transported in chemical reaction equipment by reactant e Foerderanlage, Formed nanotube in chemical reaction equipment, carbon nanotube is pushed in collection device; Chemical reaction equipment comprises the pre-reactor and main reactor that are cascaded, pre-reactor and main reactor control its temperature of reaction by Furnace Temperature Controlling System, raw material, catalyzer and reducing gas be pre-reaction Formed nanotube in pre-reactor, is then blown into by carbon nanotube in main reactor and continues reaction; The tail gas of pre-reactor passes in described main reactor and continues to transform, and passes into catalyzer and raw material to main reactor inside simultaneously.This device can the continuous seepage high-purity carbon nanotube of safety and stability, improves the stability of product and the handiness of operation.
Description
Technical field
The utility model belongs to high-purity field of carbon nanotubes, especially prepares the apparatus and method of high-purity carbon nanotube, is specifically related to the device that high-purity carbon nanotube is prepared in a kind of automatization.
Background technology
Carbon nanotube is a kind of one dimension building material, and it has structure graphene film being rolled into tubular, and have aspect ratio, carbon nanotube has many premium propertiess: outstanding physical strength and flexibility, has semi-conductor or metallic conductivity, stable chemical property.Arc discharge method and CVD pyrolysis method are the methods of two kinds of conventional production carbon nanotubes, within 1991, Japanese physicist Sumio Iijima utilizes arc discharge method Late Cambrian carbon nanotube from carbon fiber, the detailed process of arc discharge method is: Graphite Electrodes is placed in the reaction vessel being full of helium or argon gas, electric arc is excited between the two poles of the earth, temperature reaches about 4000 DEG C, under these conditions, the product that graphite evaporation is produced comprises soccerballene (C
60), agraphitic carbon and single wall or multi-walled carbon nano-tubes, by controlling the hydrogen content in catalyzer and container, the relative content of several product can be regulated.CVD pyrolysis method adopts transition metal as catalyzer, under the condition of 700-1600K, obtains carbon nanotube by the decomposition of hydrocarbon polymer.
Arc discharge method is prepared in carbon nanotube technology fairly simple, but the carbon nanotube generated and C
60mixed in together Deng product, be difficult to obtain the higher carbon nanotube of purity, the method reaction consumed energy is too large in addition.At present, produce the technique of multi-walled carbon nano-tubes by catalysis hydrocarbon cracking and there is business model, but how to ensure the smooth fluidisation of monodimension nanometer material, caking does not appear in reaction bed body, not produce localized hyperthermia and density unevenness and realize continuous prodution be the difficult problem being difficult in carbon nanotube production industry overcome always.
The general preparation process of carbon nanotube and organic synthesis reflect similar, and its side reaction complexity is various, but limit industrial scale due to the reason of equipment.The simple content by controlling hydrogen in container, effectively can not control growth and the output of carbon nanotube.At present, prior art is all only use independent fluidized-bed to carry out reaction to prepare carbon nanotube, really do not realize the production of serialization, and cannot in relative broad range adjusting process condition, be difficult to control the stability that fluidized state and mass transfer wear heat, thus cannot ensure the carbon nanotube continuously producing high-quality.
Utility model content
For solving the problems of the technologies described above, the utility model provides the apparatus and method that high-purity carbon nanotube is prepared in a kind of automatization, and this device can producing Nano carbon tubes continuously, can safety and stability mass-producing produce high-purity carbon nanotube.
Principle of the present utility model is: catalystic pyrolysis is under the effect of the temperature of 600-1000 DEG C and catalyzer, makes carbonaceous gas raw material (as carbon monoxide, methane, ethene, propylene and benzene etc.) decompose a kind of method preparing carbon nanotube.This method makes carbon compound be cracked into carbon atom at relatively high temperatures, and carbon atom, under Transition metal-catalyzed dose of effect, is attached to catalyst particles and is formed as carbon nanotube on the surface.The catalyst activity component used in catalystic pyrolysis mostly is the 8th group 4 transition metal or its alloy, adds the adjustable activity metal energy states such as Cu, Zn, Mg on a small quantity, changes its chemisorption and the ability of decomposing carbonaceous gas.Catalyst precursor has impact, metal oxide, sulfide, carbide and organometallic compound to the activity forming metal simple-substance.
For achieving the above object, the technical solution of the utility model is as follows:
The device of high-purity carbon nanotube is prepared in a kind of automatization, it comprises reactant e Foerderanlage, chemical reaction equipment, collection device, Furnace Temperature Controlling System and vacuum pump apparatus, raw material, catalyzer and reducing gas are transported in described chemical reaction equipment by described reactant e Foerderanlage, Formed nanotube in described chemical reaction equipment, carbon nanotube is pushed in collection device; Described chemical reaction equipment comprises the pre-reactor and main reactor that are cascaded, described pre-reactor and main reactor control its temperature of reaction by described Furnace Temperature Controlling System, raw material, catalyzer and reducing gas be pre-reaction Formed nanotube in described pre-reactor, is then blown into by carbon nanotube in described main reactor and continues reaction; The tail gas of described pre-reactor passes in described main reactor and continues to transform, and passes into catalyzer and raw material to described main reactor inside simultaneously.
In a preferred embodiment of the present utility model, comprise further, described Furnace Temperature Controlling System comprises: heating by electric cooker device, exhaust emission system, an electric heating element system, power control system and temperature controlling system, described heating by electric cooker device is heated chemical reaction equipment by described an electric heating element system, the waste gas of described chemical reaction equipment inside is discharged by described exhaust emission system, described power control system controls described chemical reaction equipment discharging, and described temperature controlling system controls the temperature of described chemical reaction equipment.
In a preferred embodiment of the present utility model, comprise further, described heating by electric cooker device comprises: preheat chamber, main heating chamber and insulation furnace lining, described preheat chamber is set to the heating of described pre-reactor, described main heating chamber is the heating of described main reactor, and described insulation furnace lining is used for preheat chamber and the insulation of main heating chamber.
In a preferred embodiment of the present utility model, comprise further, described temperature controlling system comprises some thermopairs for parameter sampling, and described thermopair is separately positioned on described heating by electric cooker device and chemical reaction equipment is inner.
In a preferred embodiment of the present utility model, comprise further, described reactant e Foerderanlage comprises feedstock storage unit and gas device, and described feedstock storage unit is connected on pre-reactor by pipeline, and described gas device is connected on described pre-reactor by pipeline.
In a preferred embodiment of the present utility model, comprise further, pipeline between described feedstock storage unit and pre-reactor is provided with hot gas flow data control unit, pipeline between described gas device and pre-reactor is also provided with hot gas flow data control unit, controls described feedstock storage unit and the gas device speed by material in pre-reactor respectively by described hot gas flow data control unit.
The beneficial effects of the utility model are:
One, device of the present utility model can the continuous seepage high-purity carbon nanotubes of safety and stability, improve the stability of product and the handiness of operation, this device production high-purity carbon nanotube is used to realize continuous prodution from being fed to discharging, improve flow path efficiency, and the purity of the carbon nanotube product obtained is high.
Two, the utility model catalyzer can the top charging of chemically reaction unit, the hydrogen in split product can be utilized to reduce to catalyzer, reuse, make rational use of resources, save cost.
Three, the utility model utilizes the feature that solids product tap density is larger, realizes selectivity discharging bottom chemical reaction equipment, and empties feed bin when being moved and realized production by base plate with the design of two feed bins simultaneously.
Four, device of the present utility model is provided with exhaust emission system, is provided with fume emission mouth at chemical reaction equipment top, and by after exhaust gas processing device process, safety dumping is to outside workshop, environmentally friendly, and guarantee that device security reliably uses.
Five, temperature controlling system of the present utility model can the temperature of Real-time Collection heating by electric cooker device and chemical reaction equipment inside, and the parameter of collection is supplied to temperature controlling system, according to the temperature conditions timely adjustment of chemical reaction equipment inside, reach best heats.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the utility model embodiment technology, be briefly described to the accompanying drawing used required in the description of embodiment technology below, apparently, accompanying drawing in the following describes is only embodiments more of the present utility model, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
The principle flow chart of the device of Fig. 1 preparation high-purity carbon of the present utility model nanotube.
Embodiment
Below in conjunction with the accompanying drawing in the utility model embodiment, be clearly and completely described the technical scheme in the utility model embodiment, obviously, described embodiment is only the utility model part embodiment, instead of whole embodiments.Based on the embodiment in the utility model, those of ordinary skill in the art are not making the every other embodiment obtained under creative work prerequisite, all belong to the scope of the utility model protection.
Embodiment
As shown in Figure 1, the device that high-purity carbon nanotube is prepared in a kind of automatization is disclosed in the present embodiment, it comprises reactant e Foerderanlage, chemical reaction equipment, collection device, Furnace Temperature Controlling System and vacuum pump apparatus, raw material, catalyzer and reducing gas are transported in above-mentioned chemical reaction equipment by above-mentioned reactant e Foerderanlage, Formed nanotube in above-mentioned chemical reaction equipment, carbon nanotube is pushed in collection device, completes carbon nanotube and produces.
Above-mentioned chemical reaction equipment comprises the pre-reactor and main reactor that are cascaded, above-mentioned pre-reactor and main reactor control its temperature of reaction by above-mentioned Furnace Temperature Controlling System, raw material, catalyzer and reducing gas be pre-reaction Formed nanotube in above-mentioned pre-reactor, is then blown into by carbon nanotube in above-mentioned main reactor and continues reaction; The tail gas of above-mentioned pre-reactor passes in above-mentioned main reactor and continues to transform, and passes into catalyzer and raw material to above-mentioned main reactor inside simultaneously.
Concrete, above-mentioned Furnace Temperature Controlling System comprises: heating by electric cooker device, exhaust emission system, an electric heating element system, power control system and temperature controlling system, above-mentioned heating by electric cooker device is heated chemical reaction equipment by above-mentioned an electric heating element system, the waste gas of above-mentioned chemical reaction equipment inside is discharged by above-mentioned exhaust emission system, above-mentioned power control system controls above-mentioned chemical reaction equipment discharging, and said temperature Controlling System controls the temperature of above-mentioned chemical reaction equipment.
Concrete, above-mentioned exhaust emission system is provided with fume emission mouth at chemical reaction equipment top, and by after exhaust gas processing device process, safety dumping is to outside workshop, environmentally friendly, and guarantee that device security reliably uses.
Above-mentioned heating by electric cooker device comprises: preheat chamber, main heating chamber and insulation furnace lining, and above-mentioned preheat chamber is set to the heating of above-mentioned pre-reactor, and above-mentioned main heating chamber is the heating of above-mentioned main reactor, and above-mentioned insulation furnace lining is used for preheat chamber and the insulation of main heating chamber.
Said temperature Controlling System comprises some thermopairs for parameter sampling, and above-mentioned thermopair is separately positioned on above-mentioned heating by electric cooker device and chemical reaction equipment is inner.In the present embodiment, wherein 5 parameter samplings for 5 temperature control districts of heating by electric cooker device, the parameter of sampling is supplied to the temperature in temperature control system control Lu Neige district automatically.Other 5 parameter samplings for chemical reaction container reaction gases, are supplied to the temperature raising speed situation timely adjustment of operator according to reactor, reach best heats.
Heating unit in above-mentioned an electric heating element system can be silicon controlled rectifier, because silicon controlled rectifier and other electric elements can produce suitable heat when load operation, self is furnished with radiator fan when designing this device at silicon controlled module assembly.
Raw material, catalyzer and reducing gas are transported in above-mentioned chemical reaction equipment by above-mentioned reactant e Foerderanlage, above-mentioned reactant e Foerderanlage comprises feedstock storage unit and gas device, above-mentioned raw materials storing device is connected on pre-reactor by pipeline, and above-mentioned gas device is connected on above-mentioned pre-reactor by pipeline.And, pipeline between above-mentioned raw materials storing device and pre-reactor is provided with hot gas flow data control unit, pipeline between above-mentioned gas device and pre-reactor is also provided with hot gas flow data control unit, controls above-mentioned raw materials storing device and the gas device speed by material in pre-reactor respectively by above-mentioned hot gas flow data control unit.
The effect of above-mentioned vacuum pump apparatus is: in the carburizing reagent preparatory stage, starts vacuum pump apparatus, by emptying for the air in pipeline and pre-reactor and main reactor, and then pass into shielding gas and substantially increases safety and stability in whole preparation process.
In the present embodiment, the device that high-purity carbon nanotube is prepared in above-mentioned automatization forms primarily of five parts: reactant e Foerderanlage, chemical reaction equipment, collection device, Furnace Temperature Controlling System and vacuum pump apparatus, and wherein chemical reaction equipment and Furnace Temperature Controlling System and technological design are the core technologies realizing this apparatus function.
The main body of above-mentioned chemical reaction equipment is formed by 310S Plate Welding, rational in infrastructure, rigid temperature, and chemical reaction equipment main body is provided with the inner vision slit of chemical reaction equipment, the situation of being heated of handled easily personal observations chemical reaction equipment inner workings and chemical reaction equipment, chemical reaction equipment is by above-mentioned Furnace Temperature Controlling System regulating and controlling temperature.
The design of above-mentioned chemical reaction equipment achieves the continuous input and output of Solid raw materials (catalyzer) and solids product, can continually produce, substantially increase flow path efficiency, and the feeding unit charging on catalyzer chemically reaction unit top, the hydrogen in split product can be utilized to reduce to catalyzer, recycle catalyzer, saving resource, reduces costs; Utilize the feature that solids product tap density is larger, bottom chemical reaction equipment, achieve selectivity discharging, and by base plate move with the design of two feed bins can production while empty feed bin; By base plate move with two feed bins and collection device with the use of, well complete the collection of finished product carbon nanotube.
The device that high-purity carbon nanotube is prepared in above-mentioned automatization is adapted to catalystic pyrolysis and prepares high-purity carbon nanotube, catalytic pyrolysis ratio juris is: catalystic pyrolysis is under the effect of the temperature of 600-1000 DEG C and catalyzer, makes carbonaceous gas raw material (as carbon monoxide, methane, ethene, propylene and benzene etc.) decompose a kind of method preparing carbon nanotube.This method makes carbon compound be cracked into carbon atom at relatively high temperatures, and carbon atom, under Transition metal-catalyzed dose of effect, is attached to catalyst particles and is formed as carbon nanotube on the surface.The catalyst activity component used in catalystic pyrolysis mostly is the 8th group 4 transition metal or its alloy, adds the adjustable activity metal energy states such as Cu, Zn, Mg on a small quantity, changes its chemisorption and the ability of decomposing carbonaceous gas.Catalyst precursor has impact, metal oxide, sulfide, carbide and organometallic compound to the activity forming metal simple-substance.
Concrete, the preparation method of high-purity carbon nanotube, comprises the following steps:
The first step: put into by catalyzer in pre-reactor, at 340-950 DEG C, carries out reduction reaction under reducing atmosphere, makes active substance in catalyzer be reduced to elemental metals nano particle.
Second step: catalyzer to 650-950 DEG C, then is transported to pre-reactor from catalytic center by the temperature of pre-reactor, the mixed gas passing into raw material, hydrogen and nitrogen, in pre-reactor, reacts; Wherein raw material comprises carbon-source gas or liquid carbon source, and hydrogen, raw material and nitrogen three volume ratio are 2.5:1:5.5.In this reaction process, the void tower flow velocity of gas is 0.1-4.5m/s.
3rd step: the carbon nanotube generated in pre-reactor expand into whole bed height gradually, is then transported to the carbon nanotube in pre-reactor in main reactor and continues reaction; Then the tail gas of pre-reactor is passed into main reactor to continue to transform, or supplement directly to passing into raw material in main reactor.
In 3rd step by carbon nanotube by the mode be transported in pre-reactor in main reactor comprise following in any one: carbon nanotube is blown in main reactor by the air-flow increased in pre-reactor; Extend the reaction times, thick product density reduces, under normal airflow speed, be entrained with pre-reactor.
4th step: pass into catalyzer and raw material again in main reactor, the inconsistent formation convection current of density of the tail gas passed into from pre-reactor and the catalyzer passed into and raw material, makes fully to react in main reactor
5th step: be pushed in collection device by the pneumavalve be arranged between main reactor and collection device by carbon nanotube, use shielding gas to protect in propelling movement process, then cooling down, finally pack.
The principle of above-mentioned preparation high-purity carbon nanotube is: catalyzer is in pre-reactor, under the comprehensive action of reductive agent and temperature etc., catalyzer carries out reduction reaction, obtain and there is active element metal particle, elemental metals nano particle is as transition metal, then continue on to main reactor, carbon-source gas in main reactor with Formed nanotube under the comprehensive actions such as active element metal particle.
The catalyzer related to of the present utility model can be Fe-series catalyst, also can be other composite catalyst, as long as can realize the catalyzer producing carbon nanotube in this area, is not restricted here.
Device of the present utility model can the continuous seepage high-purity carbon nanotube of safety and stability, improve the stability of product and the handiness of operation, this device production high-purity carbon nanotube is used to realize continuous prodution from being fed to discharging, improve flow path efficiency, and the purity of the carbon nanotube product obtained is high.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the utility model.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein when not departing from spirit or scope of the present utility model, can realize in other embodiments.Therefore, the utility model can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (6)
1. the device of high-purity carbon nanotube is prepared in an automatization, it comprises reactant e Foerderanlage, chemical reaction equipment, collection device, Furnace Temperature Controlling System and vacuum pump apparatus, raw material, catalyzer and reducing gas are transported in described chemical reaction equipment by described reactant e Foerderanlage, Formed nanotube in described chemical reaction equipment, carbon nanotube is pushed in collection device; It is characterized in that, described chemical reaction equipment comprises the pre-reactor and main reactor that are cascaded, described pre-reactor and main reactor control its temperature of reaction by described Furnace Temperature Controlling System, raw material, catalyzer and reducing gas be pre-reaction Formed nanotube in described pre-reactor, is then blown into by carbon nanotube in described main reactor and continues reaction; The tail gas of described pre-reactor passes in described main reactor and continues to transform, and passes into catalyzer and raw material to described main reactor inside simultaneously.
2. the device of high-purity carbon nanotube is prepared in automatization according to claim 1, it is characterized in that, described Furnace Temperature Controlling System comprises: heating by electric cooker device, exhaust emission system, an electric heating element system, power control system and temperature controlling system, described heating by electric cooker device is heated chemical reaction equipment by described an electric heating element system, the waste gas of described chemical reaction equipment inside is discharged by described exhaust emission system, described power control system controls described chemical reaction equipment discharging, described temperature controlling system controls the temperature of described chemical reaction equipment.
3. the device of high-purity carbon nanotube is prepared in automatization according to claim 2, it is characterized in that, described heating by electric cooker device comprises: preheat chamber, main heating chamber and insulation furnace lining, described preheat chamber is set to the heating of described pre-reactor, described main heating chamber is the heating of described main reactor, and described insulation furnace lining is used for preheat chamber and the insulation of main heating chamber.
4. the device of high-purity carbon nanotube is prepared in automatization according to claim 2, it is characterized in that, described temperature controlling system comprises some thermopairs for parameter sampling, and described thermopair is separately positioned on described heating by electric cooker device and chemical reaction equipment is inner.
5. the device of high-purity carbon nanotube is prepared in automatization according to claim 1, it is characterized in that, described reactant e Foerderanlage comprises feedstock storage unit and gas device, described feedstock storage unit is connected on pre-reactor by pipeline, and described gas device is connected on described pre-reactor by pipeline.
6. the device of high-purity carbon nanotube is prepared in automatization according to claim 5, it is characterized in that, pipeline between described feedstock storage unit and pre-reactor is provided with hot gas flow data control unit, pipeline between described gas device and pre-reactor is also provided with hot gas flow data control unit, controls described feedstock storage unit and the gas device speed by material in pre-reactor respectively by described hot gas flow data control unit.
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