CN109809394A - A kind of iodine purifying plant and its method of purification based on carbon nanotube - Google Patents
A kind of iodine purifying plant and its method of purification based on carbon nanotube Download PDFInfo
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- CN109809394A CN109809394A CN201910259304.2A CN201910259304A CN109809394A CN 109809394 A CN109809394 A CN 109809394A CN 201910259304 A CN201910259304 A CN 201910259304A CN 109809394 A CN109809394 A CN 109809394A
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Abstract
The iodine method of purification based on carbon nanotube that the invention discloses a kind of, comprising the following steps: S1: add iodine particle；S2: add carbon nanotube dust；S3: exhaust；S4: heating；S5: reaction；S6: cooling；S7: it collects；S8: filtering；The invention also discloses a kind of iodine purifying plant based on carbon nanotube, including heating response device, quartz tube furnace and water tank, it is connected between the heating response device and quartz tube furnace by the first connecting tube, it is connected between the quartz tube furnace and water tank by the second connecting tube, and the second connecting tube is plugged in water tank far from one end of quartz tube furnace.Advantage is: core purificant iodine used in the present invention is internal in systems to be recycled, and not will cause environmental pollution；Purificant recycles, and reduces cost, and heating temperature is low, reduces energy consumption；Iodine steam can be sublimated at once in air as iodine particle if any leakage, it is ensured that safe operation.
Description
Technical field
The present invention relates to the technical field of purification of carbon nanotube more particularly to a kind of iodine purifying plants based on carbon nanotube
And its method of purification.
Background technique
Lithium ion battery industry is quickly grown in recent years, and the carbon nanotube industry as positive conductive agent quickly emerges.?
Power lithium-ion battery field, it is high to carbon nano pipe purity and conduction needs, usually require that the metal impurities in its powder
Within 100ppm.The common purification process of carbon nanotube has sour purifying, high temperature graphitization, chlorine purifying.Sour purification process is every
200 tons of waste water can be generated by purifying one ton of carbon nanotube, and environmental protection treatment cost is high；High temperature graphitization equipment for purifying is expensive, consumption
A large amount of electric energy, the product resistance after purification rise 50% or more；Chlorine purifying risk is higher, will cause serious people if any leakage
Member's injures and deaths.
In response to the above problems, Chinese Patent Application No. be " 201680004658.7 " disclosed in " fluidized-bed reactor
CNT purification process " and Chinese Patent Application No. be " purification process of carbon nanotube " disclosed in " 201680003101.1 " all
Improved method is proposed to this, but still has many places insufficient in implementation process:
1, fluidized-bed reactor in use violent during continuous flowing due to solid particle and bubble recycle and
Agitation, no matter gas phase or solid phase all there is quite wide residence time destributions, lead to unsuitable product distribution, reduce mesh
Mark the yield of product；
2, reactant passes through bed in the form of bubbles in fluidized-bed reactor, reduces the touch opportunity between vapor solid, reduces
Reaction conversion ratio, meanwhile, complex fluid mechanics, transport phenomenon in bed, under the conditions of so that process is in unsteady, it is difficult to take off
Show its unified rule, it is also difficult to be detached from experience amplification, experiential operating
3, the hard hit due to solid catalyst in flow process and friction make catalyst accelerate dusting, in addition bed top
The explosion of portion's bubble and high-speed motion, a large amount of particulate catalysts are taken out of, cause apparent catalyst loss, catalyst it is a large amount of
Loss causes production cost higher.
For this purpose, it is proposed that a kind of solved the above problems based on the iodine purifying plant of carbon nanotube and its method of purification.
Summary of the invention
The purpose of the present invention is to solve the problems of the prior art, and a kind of iodine based on carbon nanotube proposed mentions
Pure device and its method of purification.
To achieve the goals above, present invention employs following technical solutions:
A kind of iodine method of purification based on carbon nanotube, comprising the following steps:
S1: add iodine particle；It takes a certain amount of iodine particle to be added in heating response device and seals heating response device；
S2: add carbon nanotube dust；A certain amount of carbon nanotube is taken to be added in quartz tube furnace；
S3: exhaust；Quartz tube furnace is connected with heating response device, is passed through nitrogen after connection into heating response device, nitrogen is logical
Enter the air in heating response device is discharged；
S4: heating；The temperature of heating response device is heated to 300~350 DEG C, the iodine particle in heating response device generates iodine and steams
Vapour makees carrier gas with nitrogen and iodine steam is passed into quartz tube furnace together；
S5: reaction；Quartz tube furnace is heated to 800~900 DEG C, iodine steam and carbon nanotube are sufficiently anti-in quartz tube furnace
It answers 1~3 hour, removes the metal impurities in carbon nanotube；
S6: cooling；Quartz tube furnace is closed, the height in quartz tube furnace is collected after quartz tube type in-furnace temperature is reduced to 80 DEG C
Pure nano-carbon tube；
S7: it collects；The tail gas containing metal iodide generated in iodine steam and carbon nanotube reaction process is mixed with iodine steam
Gas is closed to be collected to form iodine particle with ice water；
S8: filtering；Iodine particle is collected after filtering in ice water spare.
In the above-mentioned iodine method of purification based on carbon nanotube, the carbon nanotube of iodine particle and step S2 in step S1
Weight ratio is 1:15~1:25.
A kind of iodine purifying plant based on carbon nanotube, including heating response device, quartz tube furnace and water tank, the heating
It is connected between reactor and quartz tube furnace by the first connecting tube, passes through the second connection between the quartz tube furnace and water tank
Pipe connection, and the second connecting tube is plugged in water tank far from one end of quartz tube furnace.
In the above-mentioned iodine purifying plant based on carbon nanotube, the heating response device includes reacting cabinet and lid,
And lid is rotatably connected on reaction cabinet, the lower end of the reaction cabinet is symmetrically arranged with multiple supporting legs, the reaction chamber
Heating coil is installed, the upper end of the lid is communicated with air inlet pipe and exhaust pipe, and the first connecting tube is logical on the lateral wall of body
Connecting flange is crossed to be mounted on exhaust pipe.
In the above-mentioned iodine purifying plant based on carbon nanotube, the heating response device includes reacting cabinet and lid,
The upper surface of the lid is welded with mounting rack, and the upper surface of the mounting rack is equipped with driving motor, the driving motor
Output shaft is through lid and is welded with blender.
In the above-mentioned iodine purifying plant based on carbon nanotube, the quartz tube furnace includes body, on the body
Level is inserted with quartzy tube body, and cavity is offered in the body, installs having heaters in the cavity, and heater ring is located at
On the tube wall of quartzy tube body, one end of the quartz tube body is equipped with installing mechanism, is inserted on the installing mechanism into tracheae
And escape pipe, and enter tracheae and connect with the first connecting tube, and escape pipe is connect with the second connecting tube.
In the above-mentioned iodine purifying plant based on carbon nanotube, the installing mechanism includes installation pedestal and installation
Seat, the installation pedestal is mounted on the side wall of quartzy tube body, and the nozzle of quartzy tube body through installation pedestal and with installation base
Seat end face be in same plane, the installation stroma is mounted in installation pedestal by lock-screw, it is described enter tracheae with
Escape pipe is plugged on installation stroma and extends in quartz ampoule body.
In the above-mentioned iodine purifying plant based on carbon nanotube, the first valve, institute are installed in first connecting tube
It states and the second valve is installed in the second connecting tube.
In the above-mentioned iodine purifying plant based on carbon nanotube, the quartz tube body is set far from an end plug of installing mechanism
There is heat preservation plug, handle is installed on the heat preservation plug.
In the above-mentioned iodine purifying plant based on carbon nanotube, rubber ring is installed on the end face of the installation stroma,
And rubber ring is divided into mounting portion and extension, the diameter of the mounting portion is equal with the quartzy outer diameter of tube body, and mounting portion and stone
The port of English tube body offsets, and the diameter of the extension is equal with the quartzy internal diameter of tube body, and extension extends to quartzy tube body
It is interior.
In the above-mentioned iodine purifying plant based on carbon nanotube, multiple triangles are symmetrically welded on the side wall of the body
Frame is welded with stiffening plate between corresponding two tripods in position, the upper surface of one of them stiffening plate jointly
It offsets with the lower end of installing mechanism, the upper surface of another stiffening plate and the lower end surface of heat preservation plug offset.
Compared with prior art, the invention has the benefit that
1, for the present invention using the iodine purifying carbon nano-tube recycled, heating temperature is relatively low, and iodine can be collected by ice water and be followed
Ring utilizes, and cost is relatively low, non-environmental-pollution.
2, purification efficiency of the present invention is high, and the single purification period was 5~8 hours, better than at least 48 hours of high temperature graphitization
With 72 hours of acid purifying.
3, refining effect of the present invention is significant, and metal impurities are can be controlled within 100ppm in finished product carbon nanotube dust.
4, quartz tube furnace is used in the present invention to carry out the purifying of carbon nanotube, quartz tube furnace manufacturing process at
Ripe, furnace type structure is simple, easy to operate, convenient for control, can be realized continuous production, and power consumption is few, and the thermal efficiency is high, for
It is higher to produce collection of products rate, reduces production cost to a certain extent.
Core purificant iodine used in the present invention is internal in systems to be recycled, and not will cause environmental pollution；Purificant follows
Ring utilizes, and reduces cost, and heating temperature is low, reduces energy consumption；Iodine steam if any leakage can sublimate at once in air as iodine particle,
Ensure safe operation.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of the iodine purifying plant based on carbon nanotube proposed by the present invention；
Fig. 2 is the structural schematic diagram of heating response device in a kind of iodine purifying plant based on carbon nanotube proposed by the present invention；
Fig. 3 is quartz tube furnace part-structure enlarged drawing in a kind of iodine purifying plant based on carbon nanotube proposed by the present invention.
In figure: 1 heating response device, 2 quartz tube furnaces, 3 stiffening plates, 4 tripods, 5 rubber rings, 6 second valves, 7 first
Valve, 8 first connecting tubes, 9 second connecting tubes, 10 water tanks；
1 heating response device, 101 reaction cabinets, 102 heating coils, 103 supporting legs, 104 lids, 105 exhaust pipes, 106 driving electricity
Machine, 107 mounting racks, 108 air inlet pipe, 109 blenders；
2 quartz tube furnaces, 201 bodies, 202 heaters, 203 quartzy tube bodies, 204 heat preservation plugs, 205 installation pedestals, 206 enter gas
Pipe, 207 escape pipes, 208 installation stromas.
Specific embodiment
Following embodiment only exists in illustrative purpose, limits the scope of the invention without being intended to.
Embodiment one
Referring to Fig.1-3, a kind of iodine purifying plant based on carbon nanotube, including heating response device 1, quartz tube furnace 2 and water tank
10, it is connected between heating response device 1 and quartz tube furnace 2 by the first connecting tube 8, first valve is installed in the first connecting tube 8
Door 7, heating response device 1 includes reaction cabinet 101 and lid 104, and lid 104 is rotatably connected on reaction cabinet 101, reaction
The lower end of cabinet 101 is symmetrically arranged with multiple supporting legs 103, reacts and is equipped with heating coil 102 on the lateral wall of cabinet 101,
The upper end of lid 104 is communicated with air inlet pipe 108 and exhaust pipe 105, and the first connecting tube 8 is mounted on exhaust pipe by connecting flange
On 105；
The upper surface of lid 104 is welded with mounting rack 107, and the upper surface of mounting rack 107 is equipped with driving motor 106, driving electricity
The output shaft of machine 106 is through lid 104 and is welded with blender 109.
It is connected between quartz tube furnace 2 and water tank 10 by the second connecting tube 9, second valve is installed in the second connecting tube 9
Door 6, and the second connecting tube 9 is plugged in water tank 10 far from one end of quartz tube furnace 2.
Quartz tube furnace 2 includes body 201, and level is inserted with quartzy tube body 203 on body 201, is offered in body 201
Cavity, cavity is interior to install having heaters 202, and 202 ring of heater is located on the tube wall of quartzy tube body 203, quartzy tube body 203
One end is equipped with installing mechanism, is inserted on installing mechanism into tracheae 206 and escape pipe 207, and enters tracheae 206 and connect with first
Pipe 8 connects, and escape pipe 207 is connect with the second connecting tube 9, and quartzy tube body 203 is equipped with heat preservation far from an end plug of installing mechanism
Plug 204 keeps the temperature and is equipped with handle on plug 204.
Installing mechanism includes installation pedestal 205 and installation stroma 208, and installation pedestal 205 is mounted on the side of quartzy tube body 203
On wall, and the nozzle of quartzy tube body 203 is in same plane in through installation pedestal 205 and with the end face of installation pedestal 205, is pacified
Dress stroma 208 is mounted in installation pedestal 205 by lock-screw, enters tracheae 206 and escape pipe 207 is plugged in installation stroma
On 208 and extend in quartzy tube body 203.
It installs and rubber ring 5 is installed on the end face of stroma 208, and rubber ring 5 divides for mounting portion and extension, mounting portion
Diameter is equal with the quartzy outer diameter of tube body 203, and the port of mounting portion and quartzy tube body 203 offsets, the diameter and stone of extension
The internal diameter of English tube body 203 is equal, and extension extends in quartzy tube body 203.
It is symmetrically welded with multiple tripods 4 on the side wall of body 201, it is common between corresponding two tripods 4 in position
It is welded with stiffening plate 3, the upper surface of one of stiffening plate 3 and the lower end of installing mechanism offset, the upper end of another stiffening plate 3
Face and the lower end surface of heat preservation plug 204 offset.
S1: weighing 5 kilograms of iodine particle first, rotating cover 104, by iodine particle from lid 104 with react cabinet 101 it
Between gap be added to reaction cabinet 101 in, close lid 104；
S2: weighing 100 kilograms of iron series carbon nanotubes (iron content 10000ppm), will keep the temperature plug 204 from quartz ampoule by handle
It is dismantled at the nozzle of body 203, weighed iron series carbon nanotube is added in quartzy tube body 203, then pacify heat preservation plug 204
At the nozzle of quartzy tube body 203；
S3: opening the first valve 7 and the second valve 6, through external connecting pipe and air inlet pipe 108 into reaction cabinet 101
It is passed through nitrogen, after nitrogen enters reaction cabinet 101, the air inside cabinet 101 is reacted and quartz ampoule is entered by the first connecting tube 8
In body 203, with increasing for nitrogen, quartzy tube body 203 is discharged by the second connecting tube 9 in air；
S4: open heating coil 102, by react cabinet 101 temperature be heated to 350 DEG C, 1 in heating response device in iodine particle
Iodine steam is generated, driving motor 106 is opened simultaneously, but the output shaft of motor 106 drives blender 109 to rotate, to reaction cabinet
Material inside 101 is stirred, and fixture block iodine particle generates the speed of iodine steam, is made carrier gas with nitrogen and is passed through iodine steam together
Into quartzy tube body 203；
S5: opening heater 202, until quartzy tube body 203 is heated to 800 DEG C, iodine steam and iron series carbon nanotube dust exist
It is sufficiently reacted in quartzy tube body 203 2 hours；
S6: closing heater 202, dismantles heat preservation plug 204 by handle after the temperature of quartzy tube body 203 is reduced to 80 DEG C,
Collect the intracorporal high-purity carbon nanotube of quartz ampoule；
S7: the iron iodide and iodine steam mixed gas that can be generated in iodine steam and iron series carbon nanotube reaction process, mixing
Gas is entered in water tank 10 by escape pipe 207, and the ice water held in mixed gas and water tank 10, which reacts, generates the sedimentation of iodine particle
To bottom；
S8: 3.5 kilograms of iodine particles are obtained by the solution in filter device water tank with strainer 10, filtered solution is iron iodide
Aqueous solution.
Being detected wherein iron content to the carbon nanotube after purifying in S6 is 50ppm, reduces 99.5%.
Embodiment two:
S1: weighing 5 kilograms of iodine particle first, rotating cover 104, by iodine particle from lid 104 with react between cabinet 101
Gap is added in reaction cabinet 101, closes lid 104；
S2: weighing 100 kilograms of cobalt system carbon nanotubes (cobalt content 8000ppm), will keep the temperature plug 204 from quartzy tube body by handle
It is dismantled at 203 nozzle, weighed cobalt system carbon nanotube is added in quartzy tube body 203, then heat preservation plug 204 is installed
At the nozzle of quartzy tube body 203；
S3: opening the first valve 7 and the second valve 6, through external connecting pipe and air inlet pipe 108 into reaction cabinet 101
It is passed through nitrogen, after nitrogen enters reaction cabinet 101, the air inside cabinet 101 is reacted and quartz ampoule is entered by the first connecting tube 8
In body 203, with increasing for nitrogen, quartzy tube body 203 is discharged by the second connecting tube 9 in air；
S4: open heating coil 102, by react cabinet 101 temperature be heated to 350 DEG C, 1 in heating response device in iodine particle
Iodine steam is generated, driving motor 106 is opened simultaneously, but the output shaft of motor 106 drives blender 109 to rotate, to reaction cabinet
Material inside 101 is stirred, and fixture block iodine particle generates the speed of iodine steam, is made carrier gas with nitrogen and is passed through iodine steam together
Into quartzy tube body 203；
S5: opening heater 202, until quartzy tube body 203 is heated to 850 DEG C, iodine steam and cobalt system carbon nanotube are in quartz
It is sufficiently reacted in tube body 203 3 hours；
S6: closing heater 202, dismantles heat preservation plug 204 by handle after the temperature of quartzy tube body 203 is reduced to 80 DEG C,
Collect the intracorporal high-purity carbon nanotube of quartz ampoule；
S7: the iodate Asia cobalt and iodine steam mixed gas that can be generated in iodine steam and carbon nanotube dust reaction process, mixing
Gas is entered in water tank 10 by escape pipe 207, and the ice water held in mixed gas and water tank 10, which reacts, generates the sedimentation of iodine particle
To bottom；
S8: 3.3 kilograms of iodine particles are obtained by the solution in filter device water tank with strainer 10, filtered solution is iodate Asia cobalt
Aqueous solution.
Being detected wherein cobalt content to the carbon nanotube after purifying in S6 is 80ppm, reduces 99.2%.
Although heating response device 1, reaction cabinet 101, heating coil 102, supporting leg 103, lid is used more herein
Body 104, exhaust pipe 105, driving motor 106, mounting rack 107, air inlet pipe 108, blender 109, quartz tube furnace 2, body
201, heater 202, quartzy tube body 203, heat preservation plug 204, heater 205, enter tracheae 206, escape pipe 207, installation stroma
208, stiffening plate 3, tripod 4, rubber ring 5, the second valve 6, the first valve 7, the first connecting tube 8, the second connecting tube 9, water tank
10 equal terms, but it does not exclude the possibility of using other terms.The use of these items is only for more easily describing and
Explain essence of the invention；Being construed as any additional limitation is disagreed with spirit of that invention.
Claims (10)
1. a kind of iodine method of purification based on carbon nanotube, it is characterised in that: the following steps are included:
S1: add iodine particle；It takes a certain amount of iodine particle to be added in heating response device and seals heating response device；
S2: add carbon nanotube dust；A certain amount of carbon nanotube is taken to be added in quartz tube furnace；
S3: exhaust；Quartz tube furnace is connected with heating response device, is passed through nitrogen after connection into heating response device, nitrogen is logical
Enter the air in heating response device is discharged；
S4: heating；The temperature of heating response device is heated to 300~350 DEG C, the iodine particle in heating response device generates iodine and steams
Vapour makees carrier gas with nitrogen and iodine steam is passed into quartz tube furnace together；
S5: reaction；Quartz tube furnace is heated to 800~900 DEG C, iodine steam and carbon nanotube are sufficiently anti-in quartz tube furnace
It answers 1~3 hour, removes the metal impurities in carbon nanotube；
S6: cooling；Quartz tube furnace is closed, the height in quartz tube furnace is collected after quartz tube type in-furnace temperature is reduced to 80 DEG C
Pure nano-carbon tube；
S7: it collects；The tail gas containing metal iodide generated in iodine steam and carbon nanotube reaction process is mixed with iodine steam
Gas is closed to be collected to form iodine particle with ice water；
S8: filtering；Iodine particle is collected after filtering in ice water spare.
2. a kind of iodine purifying plant based on carbon nanotube, including heating response device (1), quartz tube furnace (2) and water tank (10),
It is characterized by: being connect between the heating response device (1) and quartz tube furnace (2) by the first connecting tube (8), the quartz
It is connect between tube furnace (2) and water tank (10) by the second connecting tube (9), and the second connecting tube (9) is far from quartz tube furnace (2)
One end be plugged in water tank (10).
3. a kind of iodine purifying plant based on carbon nanotube according to claim 2, it is characterised in that: the heating reaction
Device (1) includes reaction cabinet (101) and lid (104), and lid (104) is rotatably connected in reaction cabinet (101), described anti-
It answers the lower end of cabinet (101) to be symmetrically arranged with multiple supporting legs (103), is equipped on the lateral wall of reaction cabinet (101)
Heating coil (102), the upper end of the lid (104) are communicated with air inlet pipe (108) and exhaust pipe (105), and the first connecting tube
(8) it is mounted on exhaust pipe (105) by connecting flange.
4. a kind of iodine purifying plant based on carbon nanotube according to claim 2, it is characterised in that: the heating reaction
Device (1) includes reaction cabinet (101) and lid (104), and the upper surface of the lid (104) is welded with mounting rack (107), described
The upper surface of mounting rack (107) is equipped with driving motor (106), and the output shaft of the driving motor (106) runs through lid (104)
And it is welded with blender (109).
5. a kind of iodine purifying plant based on carbon nanotube according to claim 2, it is characterised in that: the quartz tube type
Furnace (2) includes body (201), and level is inserted with quartzy tube body (203) on the body (201), is opened up in the body (201)
There is cavity, having heaters (202) be installed in the cavity, and heater (202) ring is located on the tube wall of quartzy tube body (203),
One end of the quartz tube body (203) is equipped with installing mechanism, is inserted on the installing mechanism into tracheae (206) and escape pipe
(207), and enter tracheae (206) and connect with the first connecting tube (8), and escape pipe (207) is connect with the second connecting tube (9).
6. a kind of iodine purifying plant based on carbon nanotube according to claim 5, it is characterised in that: the installing mechanism
Including installation pedestal (205) and installation stroma (208), the installation pedestal (205) is mounted on the side wall of quartzy tube body (203)
On, and the nozzle of quartzy tube body (203) through installation pedestal (205) and is in same plane with the end face of installation pedestal (205)
Interior, the installation stroma (208) is mounted on installation pedestal (205) by lock-screw, it is described enter tracheae (206) and escape pipe
(207) it is plugged in installation stroma (208) and extends in quartzy tube body (203).
7. a kind of iodine purifying plant based on carbon nanotube according to claim 1, it is characterised in that: first connection
It is equipped with the first valve (7) on pipe (8), the second valve (6) is installed on second connecting tube (9).
8. a kind of iodine purifying plant based on carbon nanotube according to claim 5, it is characterised in that: the quartz tube body
(203) end plug far from installing mechanism is equipped with heat preservation plug (204), is equipped with handle on the heat preservation plug (204).
9. a kind of iodine purifying plant based on carbon nanotube according to claim 6, it is characterised in that: the installation stroma
(208) be equipped on end face rubber ring (5), and rubber ring (5) is divided into mounting portion and extension, the diameter of the mounting portion with
The outer diameter of quartzy tube body (203) is equal, and the port of mounting portion and quartzy tube body (203) offsets, the diameter of the extension with
The internal diameter of quartzy tube body (203) is equal, and extension extends in quartzy tube body (203).
10. a kind of iodine purifying plant based on carbon nanotube according to claim 8, it is characterised in that: the body
(201) it is symmetrically welded on side wall multiple tripods (4), is welded jointly between corresponding two tripods (4) in position
Be connected to stiffening plate (3), the upper surface of one of them stiffening plate (3) and the lower end of installing mechanism offset, another it is described plus
The upper surface of strong plate (3) and the lower end surface of heat preservation plug (204) offset.
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| CN2019203777956 | 2019-03-25 | ||
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Cited By (1)
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