WO2016097985A2 - Production of carbon nanotubes in large scale continuously using industrial emission at industrial sites - Google Patents

Production of carbon nanotubes in large scale continuously using industrial emission at industrial sites Download PDF

Info

Publication number
WO2016097985A2
WO2016097985A2 PCT/IB2015/059616 IB2015059616W WO2016097985A2 WO 2016097985 A2 WO2016097985 A2 WO 2016097985A2 IB 2015059616 W IB2015059616 W IB 2015059616W WO 2016097985 A2 WO2016097985 A2 WO 2016097985A2
Authority
WO
WIPO (PCT)
Prior art keywords
reactor
ieg
gas
catalyst
carbon nanotubes
Prior art date
Application number
PCT/IB2015/059616
Other languages
French (fr)
Other versions
WO2016097985A3 (en
Inventor
Venkateswara Rao SODISETTI
Venkatesan K. R.
Venkateswer Rao MANDAPATI
Original Assignee
Sodisetti Venkateswara Rao
K R Venkatesan
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sodisetti Venkateswara Rao, K R Venkatesan filed Critical Sodisetti Venkateswara Rao
Publication of WO2016097985A2 publication Critical patent/WO2016097985A2/en
Publication of WO2016097985A3 publication Critical patent/WO2016097985A3/en

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/16Preparation
    • C01B32/162Preparation characterised by catalysts
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/158Carbon nanotubes
    • C01B32/16Preparation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Definitions

  • the present invention relates to the synthesis of Carbon Nanotubes (CNTs) from industrial emission. More particularly, the invention relates to an apparatus and a novel process thereof for synthesizing CNTs from industrially emitted gas (IEG) and also simultaneously reducing the carbon emissions and helping to reduce greenhouse effect using hybrid reactor, as well as to the method to carry it out.
  • IEG industrially emitted gas
  • Carbon nanomaterials have been discovered in 1991, and since then, it has many exceptional electrical, optical, magnetic and mechanical properties and attractive potential applications. These CNMs can be formed from a wide variety of different materials.
  • Industrially emitted gas IEG can be considered as one of the most basic and inexpensive materials for the production of carbon nanomaterials.
  • the present invention discloses a process of synthesizing carbon nanotubes (CNTs) in large quantities with continuous process and high purity by hybrid reactor using industrially emitted gas (IEG) as a carbon source.
  • IEG industrially emitted gas
  • the present invention employs a novel hybrid CVD rector that employs the industrially emitted gas (IEG) as an input and produces CNTs at significant yields and at very low cost and also simultaneously reducing the carbon emissions and helping to reduce green house effect.
  • an industrially emitted gas (IEG) conversion process in which the industrially emitted gas (IEG) introduced into a reactor, the reaction taking place at temperatures 700° C to allow the formation of CNTs inside the reactor is disclosed.
  • a reactor in which the reactor vessel is connected with a inlet jet for catalyst insertion, the reactor which will convert industrially emitted gas (IEG) to high density carbon and hydrogen at temperature 700°C is disclosed.
  • an apparatus for producing carbon nanotubes (CNT's) using hybrid catalytic chemical vapour decomposition an industrially emitted gas (IEG) comprises of one or more stagedfurnace, which further comprises of one or more temperature controller; and one or more reactor for the production of said CNT's.
  • the reactor at its one end, is configured to receive one or more catalyst by a means of one or more jet sprayer maintained at a controlled temperature, wherein said catalyst is present inside a precursor chamber located outside said furnace; and receive a dried industrially emitted gas (IEG) by a means of a flow element connected to one or more dryer, wherein said dryer is located outside said furnace.
  • the temperature controller is configured to attain a particular temperature and thereby induces production of said CNT's inside said reactor.
  • a method for producing carbon nanotubes (CNT's) using a hybrid catalytic chemical vapour decomposition and an industrially emitted gas (IEG) in an apparatus is disclosed. The method comprises of:
  • a custom designed jet sprayer for sending the catalyst vapour along with its carrier gas and carbon precursor gas separately inside the carbon-cracking zone of the CVD reactor.
  • Figure 1 is a schematic representation of the complete process used in the present invention to produce carbon nanotubes in a continuous way from Industrially Emitted gas (IEG).
  • IEG Industrially Emitted gas
  • Figure 2 is a schematic representation of the volatile separating chamber, process used to separate volatiles continuously from the Industrially Emitted Gas (IEG).
  • IEG Industrially Emitted Gas
  • Figure 3 is a schematic representation of the particle filter, process used to filter the particulate matter from the Industrially Emitted Gas (IEG).
  • Figure 4 is a schematic representation of the mist eliminator, process used to eliminate the moisture presence in the Industrially Emitted Gas (IEG).
  • Figure 5 is a schematic representation of the reactor with furnace, process used in detail of the feeding zone of the catalyst and Industrially Emitted Gas (IEG) through Jet sprayer and the process in which the synthesis of the CNT are made.
  • IEG Industrially Emitted Gas
  • Figure 6 is a schematic representation of the CNT collector with vacuum sucker, process used to collect the produce CNT from the reactor with the help of vacuum sucker.
  • Figure 7 is a schematic representation of the precursor chamber, process used to feed the catalyst into the reactor with help of dozing pump and spray jet.
  • Figure 8 is a representation of photomicrograph of Carbon nanotubes obtained in the example.
  • Figure 9 is a flow chart representation of the method for producing carbon nanotubes (CNT's) using hybrid catalytic chemical vapor decomposition and an industrially emitted gas (IEG) in an apparatus.
  • the present invention is directed to a process of continuous production of carbon nanotubes (CNTs).
  • This apparatus for the CNT synthesis comprises:
  • FIG 1 is a schematic representation for the production of CNTs; the industrially emitted gases (IEG) may enter atar separating chambers 1, where the volatiles that may be present in the industrially emitted gas (IEG)may be separated from bottom of the Tar Separating Chambers.
  • the residual gas includes some solid particles, which are removed with the help of a filter 2.
  • the gas may further enter a mist eliminator 3, which traps the moisture present in the gas.
  • the moisture free gas may then enters a reactor 8 in measured flows with a flow element 4.
  • the reactor 8 is a specially designed rector in which the CNTs are produced continuously.
  • the CNTs are prepared in a vertical stainless steel tube reactor 8 within the furnace 11.
  • a catalyst metalocene may sent into the reactor 8, using in-situ method in the middle of the first stage furnace with the help of jet sprayer 12, of which the temperature is maintained between 300°C to 400°C.
  • the precursor chamber 7 may produce the metalocene required with the help of metering/dosing pump 6 into the reactor 8.
  • a particular flow of dried industrially emitted gas (IEG) is introduced in the reactor 8 with the help of a flow Element 4.
  • the reactor 8 is provided with one or more plate means for distribution of gases in a pre-described flow patterns.
  • the distribution plates comprise one or more pattern of holes to maintain different flow patterns of IEG inside the reactor.
  • the second stage furnace 13 is ramped at a particular heating rate to the desired reaction temperature and is held at a final temperature, between 700°C to 1000°C.for efficient cracking of carbon precursor, and for the formation of the CNT inside reactor.
  • a final temperature between 700°C to 1000°C.for efficient cracking of carbon precursor, and for the formation of the CNT inside reactor.
  • At other end of the reactor 8 is connected to the blower/ vacuum pump 10, to suck the CNTs into the bag fiber filter 9 for the collection of the CNT.
  • Figure 1 also shows the concept of the present invention to demonstrative equipment.
  • a device of any type is used to admix the liquids, is fed with a mixture on an industrially emitted gas (IEG) and a catalyst in the suitable proportion to produce the formation of CNT.
  • IEG industrially emitted gas
  • the jet sprayer 12 may be within the heating zone of the first stage furnace is shown in the figure 5 that is controlled between 300°C to 400°C, to allow the passage of the liquid catalyst in vapour form, where the CNT will form on the catalyst seeds.
  • the furnace 11 is heated continuously, and the positioning is made by means of clamps, in such a way that at the beginning of the process, the furnace 11 is heated till the CNTs synthesis temperature, for example, between 600°C and 1000°C, preferably to 700°C.
  • the reactor 8 may be fixed inside the furnace 11 and may be warmed up to reach the synthesis temperature, simultaneously the inert gas (that may include but not limited to helium, neon, argon, carbon dioxide, and the like) flow may be passed through the reactor 8 with the flow element 5 (being the most preferred, due to lowest cost) to create the inert atmosphere in the reactor 8. It may be understood that other suitable gasses may also be passed through the reactor 8 based on the applicability. After reaching the required temperature of the reactor 8 feed the industrially emitted gas (IEG) and catalyst reagents inside the reactor 8.
  • IEG industrially emitted gas
  • the flow may be adjusted preferably in base to the linear speed of the gas that will between 200 seem to 1000 seem, preferably 400 seem.
  • the reaction time maybe chosen based on the length required by the CNTs.
  • the growth speed is based on the synthesis condition of the synthesis and emissions and catalyst used, as well as on the proportion between these.
  • CNTs formed in the internal surface of the reactor may be cleaned for every 30 min using inert gas under high pressure and sucks into the bag fiber filler chamber 9 for collecting CNTs using vacuum device 10.
  • inert gas under high pressure
  • the vacuum is deactivated. Meanwhile, the reactor 8 is in the synthesis position and once the time of CNT synthesis has been finalized, the industrially emitted gas (IEG) and catalyst feeding maybe suspended preferably for 3 minutes.
  • IEG industrially emitted gas
  • the previously described method may include the following steps: Feeding, a mixture of an industrially emitted gas (IEG) and catalyst, in the suitable proportion, into the reactor for the formation of the CNT. It may be understood that the catalyst and the IEG may be fed separately to the reactor.
  • IEG industrially emitted gas
  • Pre -heating system is controlled between 300°C to 400°C to pass the liquid towards the reactor 8 using jet spray 12.
  • the furnace 11 is positioning is made by means of clamps, the furnace 11 is has the synthesis temperature of the CNT, namely, between 600°C to 1200°C, preferably to 700°C.
  • the reactor 8 inside the furnace may be warmed up to reach the reaction temperature as mentioned above.
  • a flow of inert gas may be passed through the reactor 8 continuously from starting to end of the reaction.
  • the flow of industrially emitted gas (IEG) may be adjusted preferably on the basis of the linear speed of the gas that will be between 200 seem to 1000 seem, preferably 400 seem.
  • the feeding of industrially emitted gas (IEG) and catalyst mixture may begin to allow the formation of the CNTs.
  • the reaction time is chosen based on the length required for the carbon nanotubes.
  • the CNTs formed in the internal surface of the reactor 8 are cleaned for every 30 min using inert gas under high pressure and also sucks into the bag fiber filler chamber 9 for collecting CNTs using vacuum device.
  • the vacuum may be deactivated.
  • the industrially emitted gas (IEG) and catalyst feeding may be suspended preferably 3 minutes.
  • a method of producing carbon nanotubes using industrially emitted gas (IEG) having a production station may comprise of:
  • each chamber contains inlet for gas and water and outlet for tar and water, with a level gauge to show the water level.
  • At least one filter to remove the solid particles from the residual industrially emitted gas (IEG) coming out from the volatile separating chambers connected in line.
  • IEG industrially emitted gas
  • a mist eliminator chamber which traps the moisture present in the industrially emitted gas, having the inlet and outlet for gas.
  • a furnace is maintaining at a predetermined temperature to allow the synthesis of carbon nanotubes inside the reactor chamber, furnace designed in two part, part - 1 heater and part - 2 heater.
  • Part -1 is maintained at predetermined temperature for converting catalyst from liquid phase to vapor phase and part -2 is for converting industrially emitted gas (EIG) to carbon nanotubes with support of vapor phase catalyst.
  • EIG industrially emitted gas
  • a bag fiber filter chamber to collect the carbon nanotubes in bag, which is connected to the outlet of reactor chamber.
  • a control system is mounted on the front frame of the hybrid reactor.
  • the precursor chamber may be connected to the metering pump.
  • the metering pump flows with the predetermined flows of catalyst into the reactor from 0.1 to 10 ml/min.
  • the jet sprayer may be plugged at the inlet of the reactor chamber in the middle of the first state furnace, wherein it consists of inner and outer tube, whereas inner tube supply catalyst and outer tube supply gas into the reactor chamber for the production of carbon nanotubes within the predetermined temperature 300°C to 400°C.
  • the method and apparatus may produce a single walled carbon nanotubes using industrially emitted gas.
  • the method and apparatus may produce a multi walled carbon nanotubes using industrially emitted gas.
  • the catalyst Ferrocene was dissolved in solvent is predetermined 0.5, 1, 1.5 and 2 grms for the production of carbon nanotubes using industrially emitted gas (IEG).
  • the temperatures predetermined may be in the range of 700°C to 900°C for the production of carbon nanotubes using industrially emitted gas (IEG).
  • the carbon nanotubes may show homogeneity or heterogeneity in the sizes of the CNTs, with respect to the catalyst composition and temperature.
  • the catalyst particle size may be in the range of 10- 50 nm.
  • the carbon nanotubes may be homogeneous and/or heterogeneous in size and size may vary in between 10 to 100 nm.
  • FIG 2 is a schematic representation of the volatile separating chamber 1, process used to separate volatiles continuously from the Industrially Emitted Gas (IEG).
  • the separating chamber 1 may comprise of an industrial emission inlet 201, a sequence inlet line to particle eliminator 202, a level gauge of water 203, and a volatile drains outlet 204.
  • water may be supplied to the IEG received in the chamber 1.
  • a pump may be provided to feed water inside the chamber 1.
  • FIG 3 is a schematic representation of the particle filter 2, process used to filter the particulate matter from the Industrially Emitted Gas (IEG).
  • the filter 2 to separate particles in industrial emission receives the volatile free Industrially Emitted Gas (IEG) from the chamber 1.
  • the filter may be provided with a differential pressure gauge 301 to adjust the pressure of the input from the chamber 1.
  • the mist eliminator 3 receives a filtered IEG to a chamber to capture mist form the IEG.
  • the eliminator 3 may include a level gauge 401, a water drain to remove the moisture 402, needle valve to outlet the moisture free gas to rotameter 403.
  • FIG 5 a schematic representation of the reactor with furnace, process used in detail of the feeding zone of the catalyst and Industrially Emitted Gas (IEG) and the position in which the synthesis of the CNT is made and shows the furnace in order to cover the reactor at appropriate temperatures.
  • the reaction chamber is shown.
  • the chamber comprises of a furnace 11 enclosing a reactor 8 inside it.
  • the furnace may include temperature controllers 13 connected to it which are configured to maintain temperature suitable for the reaction inside the reactor.
  • the chamber comprises of an inlet of IEG which may be received from the rotameter and also include a jet sprayer 12 which is configured to provide an inlet to the catalyst from the same end.
  • the other end of the reactor provides an outlet to the CNT's formed inside the reactor and is connected to collection unit shown in figure 6.
  • FIG 6 a schematic representation of the CNT collector with vacuum sucker 10, process used to collect the produce CNT from the reactor 8 with the help of vacuum sucker 10 is shown.
  • the collection unit comprises of bag filler 9, a collection chamber 601, a collecting outlet 602 and a Vacuum sucker 10 attached to it.
  • the precursor tank 7 may include a precursor feeder 701, a ball valve 702, an air remover 703, a storage tank 704, a level gauge 705, a pulsation dampener706 outlet connected to a dosing pump 6.
  • the task of precursor chamber / tank 7 is to store the catalyst which may be present along with a solvent inside the tank 704 and to provide the same to the reactor 8 during the initiation of the reaction.
  • FIG 8 a method for producing carbon nanotubes (CNT's) using hybrid catalytic chemical vapor decomposition and industrially emitted gas (IEG) in an apparatus is shown.
  • a method for producing carbon nanotubes (CNT's) using hybrid catalytic chemical vapour decomposition an industrially emitted gas (IEG) in an apparatus comprises of:
  • an apparatus for producing carbon nanotubes (CNT's) using hybrid catalytic chemical vapour decomposition an industrially emitted gas (IEG) comprises of one or more furnace which further comprises of one or more temperature controller; and one or more reactor for the production of said CNT's.
  • the reactor at its one end, is configured to receive one or more catalyst by a means of one or more jet sprayer maintained at a controlled temperature, wherein said catalyst is present inside a precursor chamber located outside said furnace; and receive a dried industrially emitted gas (IEG) by a means of a flow element connected to one or more dryer, wherein said dryer is located outside said furnace.
  • the temperature controller is configured to attain a particular temperature and thereby induces production of said CNT's inside said reactor.
  • said rector is a vertical stainless steel tube reactor.
  • said catalyst is an organometallic compound and preferably ferrocene. In one implementation, said catalyst is dissolved in a solvent.
  • said catalyst is in a particulate form with a particle size in a range of 5 - 50 nm.
  • said precursor chamber is configured to feed said catalyst into said reactor by a means of a metering pump.
  • said precursor chamber is configured to feed said catalyst into said reactor by means of an inlet means covered by said jet sprayer.
  • said jet sprayer is maintained at said controlled temperature, preferably, in a range of 300 °C to 400 °C.
  • dried industrially emitted gas is a moisture free gas, which obtained from: said dryer coupled to one or more mist eliminator which is further coupled to one or more filter which is further coupled to one or more tar separating chamber, wherein: said tar separating chamber is configured to receive an industrially emitted gases (IEG) and separate volatiles present in said industrially emitted gas (IEG) from bottom of said tar separating chamber thereby forming residual gas; said filter is configured to remove solid particles, if any, from said residual gas; and said mist eliminator is configured to trap the moisture present in said residual gas, and thereby feed said residual gas to said dryer wherein said residual gas is dried to form said dried industrially emitted gas (IEG).
  • said particular temperature is in a range, of 600 °C to 1200 °C, and preferably of 700 °C.
  • said reactor at other end, is connected to blower configured to suck said CNT's into bag fiber filter for the collection of said CNT's.
  • an inert gas is passed through said reactor, before inducing said production of CNT's, to create an inert atmosphere in said reactor.
  • an inert gas is passed with a flow in a range, of 200 seem to 1000 seem, and preferably of 400 seem.
  • the blower is configured to suck CNT's using inert gas under high pressure.
  • said dried industrially emitted gas (IEG) from said dryer is feed to the reactor using rotameter.
  • CNT's are of size between 10 to 100 nm.
  • IEG industrially emitted gas
  • IEG Industrially emitted gas
  • ferrocene as a catalyst.
  • the ferrocene concentration was 0.5g/50 ml methanol using in-situ method in the middle of the first stage furnace 8 at 400°C with the help of jet sprayer 12.
  • the temperature in the second stage furnace 8 was set at 800°C.
  • the mixture feeding of IEG and catalyst for each one of the tubes will form, so that the formation of the CNT inside of reactor 8 is produced continuously.
  • Simultaneously removal of the CNTs CNTs formed in the internal surface of the reactor.
  • the production of carbon nanotubes was of 5 grams at efficiency rate of 70%, being the average diameter of 10 to 50 nm and length up to 150 ⁇ .
  • Fig 8 shows the produced carbon nanotubes in these conditions.

Abstract

The present invention discloses a hybrid apparatus for continuous production Carbon nanotubes (CNTs) using Industrial emitted gases (IEG) at industrial sites economically, as well as the method to carry it out. The apparatus for the CNT synthesis is includes: A pair of volatile separating tanks; particle filter; moisture trapper, connected in line to flow meter; simultaneously also connected to the reactor separately; a furnace is maintained suitable temperature to allow the formation of CNTs inside the reactor; a vacuum system is connected end of the reactor to collect CNTs in bag fibre filter.

Description

PRODUCTION OF CARBON NANOTUBES IN LARGE SCALE CONTINUOUSLY USING
INDUSTRIAL EMISSION AT INDUSTRIAL SITES FIELD OF INVENTION
The present invention relates to the synthesis of Carbon Nanotubes (CNTs) from industrial emission. More particularly, the invention relates to an apparatus and a novel process thereof for synthesizing CNTs from industrially emitted gas (IEG) and also simultaneously reducing the carbon emissions and helping to reduce greenhouse effect using hybrid reactor, as well as to the method to carry it out.
BACKGROUND OF INVENTION Carbon nanomaterials (CNMs) have been discovered in 1991, and since then, it has many exceptional electrical, optical, magnetic and mechanical properties and attractive potential applications. These CNMs can be formed from a wide variety of different materials. Industrially emitted gas (IEG) can be considered as one of the most basic and inexpensive materials for the production of carbon nanomaterials.
Till date, a number of methods for the synthesis of CNMs have been reported, which can be grouped into three types: arc discharge (R.H. Baughman, 2002), laser ablation (C. Journet, 1997, Z. Shi, 2000) and catalytic chemical vapor deposition (CCVD) (M. Zhang, 2001, J. Kong, 1998, D.E. Resasco, 2002). Of these methods, the CCVD method has drawn more attention due to its potential for inexpensive and continuous production of CNMs in large amounts.
Carbon nanomaterials production increases with the addition of metal catalyst to the industrially emitted gas (IEG). Even CNMs synthesis takes place at respective temperatures, reaction time and complete decomposition of the catalytic precursor is expected which acts as a nucleation agent to enhance growth of the CNMs.
There are no complete studies about the synthesis of CNMs with industrially emitted gas (IEG) as a carbon source in the literature. The results obtained by the present invention demonstrate that industrially emitted gas (IEG) may be a good carbon sourcefor the production of CNMs by the hybrid CCVD method, for which one of the reasons might be due to the mixture of the components such as CH4, CO and ¾ in industrial emissions that are involved, in one way or another, in the formation process of CNMs.
SUMMARY OF INVENTION
This summary is provided to introduce concepts related to a production of carbon nanotubes in large scale continuously using industrial emission at industrial sites and the concepts are further described below in the detailed description. This summary is not intended to identify essential features of the claimed subject matter nor is it intended for use in determining or limiting the scope of the claimed subject matter.
The present invention discloses a process of synthesizing carbon nanotubes (CNTs) in large quantities with continuous process and high purity by hybrid reactor using industrially emitted gas (IEG) as a carbon source.
In one implementation, the present invention employs a novel hybrid CVD rector that employs the industrially emitted gas (IEG) as an input and produces CNTs at significant yields and at very low cost and also simultaneously reducing the carbon emissions and helping to reduce green house effect. In one implementation, an industrially emitted gas (IEG) conversion process in which the industrially emitted gas (IEG) introduced into a reactor, the reaction taking place at temperatures 700° C to allow the formation of CNTs inside the reactor is disclosed. In one implementation, a reactor in which the reactor vessel is connected with a inlet jet for catalyst insertion, the reactor which will convert industrially emitted gas (IEG) to high density carbon and hydrogen at temperature 700°C is disclosed.
In one implementation, an apparatus for producing carbon nanotubes (CNT's) using hybrid catalytic chemical vapour decomposition an industrially emitted gas (IEG) is disclosed. The apparatus comprises of one or more stagedfurnace, which further comprises of one or more temperature controller; and one or more reactor for the production of said CNT's. The reactor, at its one end, is configured to receive one or more catalyst by a means of one or more jet sprayer maintained at a controlled temperature, wherein said catalyst is present inside a precursor chamber located outside said furnace; and receive a dried industrially emitted gas (IEG) by a means of a flow element connected to one or more dryer, wherein said dryer is located outside said furnace. The temperature controller is configured to attain a particular temperature and thereby induces production of said CNT's inside said reactor. In one implementation, a method for producing carbon nanotubes (CNT's) using a hybrid catalytic chemical vapour decomposition and an industrially emitted gas (IEG) in an apparatus is disclosed. The method comprises of:
• receiving one or more catalyst by a means of one or more jet sprayer maintained at a controlled temperature of first stage furnace, preferably, in a range of 300 °C to 400 °C, wherein said catalyst is metalocene and is present inside a precursor chamber located outside said furnace; and
• receiving a industrially emitted gas (IEG) by means of a one or more volatile separating chambers connected to a dryer, wherein said volatile separation chamber located outside said furnace; and • receiving a dried industrially emitted gas (IEG) by a means of a flow element connected to one or more dryer, wherein said dryer is located outside said furnace and connected to a mist eliminator; and
• use of gas distribution plate with custom designed pattern of holes that has effect on the flow pattern of gas inside the reactor, ultimately influencing the cracking of sent gas and the yield of CNTs formation.
• A custom designed jet sprayer for sending the catalyst vapour along with its carrier gas and carbon precursor gas separately inside the carbon-cracking zone of the CVD reactor.
• attaining a particular temperature in second stage furnace, preferably of 700 °C, using temperature controller, thereby inducing production of said CNT's inside said reactor.
BRIEF DISCRIPTION OF THE ACCOMPANYING DRAWING
These and other features, aspects, and advantages of the present invention will become better understood, when the following detailed description is read with reference to the accompanying drawing in which like reference numerals represent like parts throughout the several drawings, wherein:
Figure 1 is a schematic representation of the complete process used in the present invention to produce carbon nanotubes in a continuous way from Industrially Emitted gas (IEG).
Figure 2 is a schematic representation of the volatile separating chamber, process used to separate volatiles continuously from the Industrially Emitted Gas (IEG).
Figure 3 is a schematic representation of the particle filter, process used to filter the particulate matter from the Industrially Emitted Gas (IEG). Figure 4 is a schematic representation of the mist eliminator, process used to eliminate the moisture presence in the Industrially Emitted Gas (IEG).
Figure 5 is a schematic representation of the reactor with furnace, process used in detail of the feeding zone of the catalyst and Industrially Emitted Gas (IEG) through Jet sprayer and the process in which the synthesis of the CNT are made.
Figure 6 is a schematic representation of the CNT collector with vacuum sucker, process used to collect the produce CNT from the reactor with the help of vacuum sucker.
Figure 7 is a schematic representation of the precursor chamber, process used to feed the catalyst into the reactor with help of dozing pump and spray jet.
Figure 8 is a representation of photomicrograph of Carbon nanotubes obtained in the example.
Figure 9 is a flow chart representation of the method for producing carbon nanotubes (CNT's) using hybrid catalytic chemical vapor decomposition and an industrially emitted gas (IEG) in an apparatus.
DETAILED DESCRIPTION OF THE PRESENT INVENTION
The present invention is directed to a process of continuous production of carbon nanotubes (CNTs).
While aspects of described a production of carbon nanotubes in large scale continuously using industrial emission at industrial sites may be implemented in any number of different environments, and/or configurations, the embodiments are described in the context of the following exemplary apparatus. This apparatus for the CNT synthesis comprises:
Referring to figure 1 is a schematic representation for the production of CNTs; the industrially emitted gases (IEG) may enter atar separating chambers 1, where the volatiles that may be present in the industrially emitted gas (IEG)may be separated from bottom of the Tar Separating Chambers. The residual gas includes some solid particles, which are removed with the help of a filter 2. The gas may further enter a mist eliminator 3, which traps the moisture present in the gas. The moisture free gas may then enters a reactor 8 in measured flows with a flow element 4.
The reactor 8 is a specially designed rector in which the CNTs are produced continuously. The CNTs are prepared in a vertical stainless steel tube reactor 8 within the furnace 11.
It may have two stage furnace systems. A catalyst metalocene may sent into the reactor 8, using in-situ method in the middle of the first stage furnace with the help of jet sprayer 12, of which the temperature is maintained between 300°C to 400°C. The precursor chamber 7 may produce the metalocene required with the help of metering/dosing pump 6 into the reactor 8. A particular flow of dried industrially emitted gas (IEG) is introduced in the reactor 8 with the help of a flow Element 4. The reactor 8 is provided with one or more plate means for distribution of gases in a pre-described flow patterns. The distribution plates comprise one or more pattern of holes to maintain different flow patterns of IEG inside the reactor. The second stage furnace 13 is ramped at a particular heating rate to the desired reaction temperature and is held at a final temperature, between 700°C to 1000°C.for efficient cracking of carbon precursor, and for the formation of the CNT inside reactor. At other end of the reactor 8 is connected to the blower/ vacuum pump 10, to suck the CNTs into the bag fiber filter 9 for the collection of the CNT.
Figure 1 also shows the concept of the present invention to demonstrative equipment. For the CNT production, a device of any type is used to admix the liquids, is fed with a mixture on an industrially emitted gas (IEG) and a catalyst in the suitable proportion to produce the formation of CNT.
The jet sprayer 12 may be within the heating zone of the first stage furnace is shown in the figure 5 that is controlled between 300°C to 400°C, to allow the passage of the liquid catalyst in vapour form, where the CNT will form on the catalyst seeds.
The furnace 11 is heated continuously, and the positioning is made by means of clamps, in such a way that at the beginning of the process, the furnace 11 is heated till the CNTs synthesis temperature, for example, between 600°C and 1000°C, preferably to 700°C.
As in the first step, the reactor 8 may be fixed inside the furnace 11 and may be warmed up to reach the synthesis temperature, simultaneously the inert gas (that may include but not limited to helium, neon, argon, carbon dioxide, and the like) flow may be passed through the reactor 8 with the flow element 5 (being the most preferred, due to lowest cost) to create the inert atmosphere in the reactor 8. It may be understood that other suitable gasses may also be passed through the reactor 8 based on the applicability. After reaching the required temperature of the reactor 8 feed the industrially emitted gas (IEG) and catalyst reagents inside the reactor 8.
As there is no restriction in the diameter and length of the reactor 8, the flow may be adjusted preferably in base to the linear speed of the gas that will between 200 seem to 1000 seem, preferably 400 seem. The reaction time maybe chosen based on the length required by the CNTs. The growth speed is based on the synthesis condition of the synthesis and emissions and catalyst used, as well as on the proportion between these.
Simultaneously for the removal of the CNTs, CNTs formed in the internal surface of the reactor, it may be cleaned for every 30 min using inert gas under high pressure and sucks into the bag fiber filler chamber 9 for collecting CNTs using vacuum device 10. Without this being limitative, since we have all the time in which the CNT in the reactor 8 are in the synthesized position inside the furnace 11 to carry out the cleaning of the reactor 8. Once the reactor cleaning has concluded, the vacuum is deactivated. Meanwhile, the reactor 8 is in the synthesis position and once the time of CNT synthesis has been finalized, the industrially emitted gas (IEG) and catalyst feeding maybe suspended preferably for 3 minutes.
The previously described method may include the following steps: Feeding, a mixture of an industrially emitted gas (IEG) and catalyst, in the suitable proportion, into the reactor for the formation of the CNT. It may be understood that the catalyst and the IEG may be fed separately to the reactor.
Pre -heating system is controlled between 300°C to 400°C to pass the liquid towards the reactor 8 using jet spray 12.
The furnace 11 is positioning is made by means of clamps, the furnace 11 is has the synthesis temperature of the CNT, namely, between 600°C to 1200°C, preferably to 700°C. The reactor 8 inside the furnace may be warmed up to reach the reaction temperature as mentioned above.
A flow of inert gas may be passed through the reactor 8 continuously from starting to end of the reaction. The flow of industrially emitted gas (IEG) may be adjusted preferably on the basis of the linear speed of the gas that will be between 200 seem to 1000 seem, preferably 400 seem.
Once the synthesis temperature is reached, the feeding of industrially emitted gas (IEG) and catalyst mixture may begin to allow the formation of the CNTs. The reaction time is chosen based on the length required for the carbon nanotubes.
Simultaneously, the CNTs formed in the internal surface of the reactor 8 are cleaned for every 30 min using inert gas under high pressure and also sucks into the bag fiber filler chamber 9 for collecting CNTs using vacuum device.
Once the reactor cleaning has concluded, the vacuum may be deactivated.
Once the time of CNT synthesis has been finalized, the industrially emitted gas (IEG) and catalyst feeding may be suspended preferably 3 minutes.
In one implementation, a method of producing carbon nanotubes using industrially emitted gas (IEG) having a production station may comprise of:
a) A tapping connection from the industrial emitting source from industry.
b) At least a pair of volatile separating chambers to separate tar from the industrially emitted gas (IEG), each chamber contains inlet for gas and water and outlet for tar and water, with a level gauge to show the water level.
c) At least one filter to remove the solid particles from the residual industrially emitted gas (IEG) coming out from the volatile separating chambers connected in line.
d) A mist eliminator chamber, which traps the moisture present in the industrially emitted gas, having the inlet and outlet for gas.
e) A furnace is maintaining at a predetermined temperature to allow the synthesis of carbon nanotubes inside the reactor chamber, furnace designed in two part, part - 1 heater and part - 2 heater. Part -1 is maintained at predetermined temperature for converting catalyst from liquid phase to vapor phase and part -2 is for converting industrially emitted gas (EIG) to carbon nanotubes with support of vapor phase catalyst.
f) A bag fiber filter chamber to collect the carbon nanotubes in bag, which is connected to the outlet of reactor chamber.
g) A suction device connected to the extraction pipe, wherein the suction comprises for the collection of carbon nanotubes in bag fiber filter.
h) a control system is mounted on the front frame of the hybrid reactor.
In one implementation, the precursor chamber may be connected to the metering pump.
In one implementation, the metering pump flows with the predetermined flows of catalyst into the reactor from 0.1 to 10 ml/min.
In one implementation, the jet sprayer may be plugged at the inlet of the reactor chamber in the middle of the first state furnace, wherein it consists of inner and outer tube, whereas inner tube supply catalyst and outer tube supply gas into the reactor chamber for the production of carbon nanotubes within the predetermined temperature 300°C to 400°C.
In one implementation, the method and apparatus may produce a single walled carbon nanotubes using industrially emitted gas.
In one implementation, the method and apparatus may produce a multi walled carbon nanotubes using industrially emitted gas.
In one implementation, the catalyst Ferrocene was dissolved in solvent is predetermined 0.5, 1, 1.5 and 2 grms for the production of carbon nanotubes using industrially emitted gas (IEG). In one implementation, the temperatures predetermined may be in the range of 700°C to 900°C for the production of carbon nanotubes using industrially emitted gas (IEG). In one implementation, the carbon nanotubes may show homogeneity or heterogeneity in the sizes of the CNTs, with respect to the catalyst composition and temperature.
In one implementation, the catalyst particle size may be in the range of 10- 50 nm. In one implementation, the carbon nanotubes may be homogeneous and/or heterogeneous in size and size may vary in between 10 to 100 nm.
Referring now to figure 2 is a schematic representation of the volatile separating chamber 1, process used to separate volatiles continuously from the Industrially Emitted Gas (IEG). As shown in the figure 2, the separating chamber 1 may comprise of an industrial emission inlet 201, a sequence inlet line to particle eliminator 202, a level gauge of water 203, and a volatile drains outlet 204. In one implementation, water may be supplied to the IEG received in the chamber 1. A pump may be provided to feed water inside the chamber 1. Referring now to figure 3 is a schematic representation of the particle filter 2, process used to filter the particulate matter from the Industrially Emitted Gas (IEG). As shown in figure 3 the filter 2 to separate particles in industrial emission receives the volatile free Industrially Emitted Gas (IEG) from the chamber 1. The filter may be provided with a differential pressure gauge 301 to adjust the pressure of the input from the chamber 1.
Referring now to figure 4 a schematic representation of the mist eliminator 3, process used to eliminate the moisture presence in the Industrially Emitted Gas (IEG) is shown. As shown in figure 4, the mist eliminator 3 receives a filtered IEG to a chamber to capture mist form the IEG. The eliminator 3 may include a level gauge 401, a water drain to remove the moisture 402, needle valve to outlet the moisture free gas to rotameter 403.
Referring now to figure 5 a schematic representation of the reactor with furnace, process used in detail of the feeding zone of the catalyst and Industrially Emitted Gas (IEG) and the position in which the synthesis of the CNT is made and shows the furnace in order to cover the reactor at appropriate temperatures. As shown in figure 5, the reaction chamber is shown. The chamber comprises of a furnace 11 enclosing a reactor 8 inside it. The furnace may include temperature controllers 13 connected to it which are configured to maintain temperature suitable for the reaction inside the reactor.
As shown in figure 5, the chamber comprises of an inlet of IEG which may be received from the rotameter and also include a jet sprayer 12 which is configured to provide an inlet to the catalyst from the same end. The other end of the reactor provides an outlet to the CNT's formed inside the reactor and is connected to collection unit shown in figure 6.
Referring now to figure 6 a schematic representation of the CNT collector with vacuum sucker 10, process used to collect the produce CNT from the reactor 8 with the help of vacuum sucker 10 is shown. As shown in the figure 6, the collection unit comprises of bag filler 9, a collection chamber 601, a collecting outlet 602 and a Vacuum sucker 10 attached to it.
The uses and working of the collecting unit is explained above. Referring now to figure 7 a schematic representation of the precursor chamber 7, process used to feed the catalyst into the reactor 8 with help of dozing pump 6 and jet sprayer is shown. As shown in the figure 7, the precursor tank 7 may include a precursor feeder 701, a ball valve 702, an air remover 703, a storage tank 704, a level gauge 705, a pulsation dampener706 outlet connected to a dosing pump 6. The task of precursor chamber / tank 7 is to store the catalyst which may be present along with a solvent inside the tank 704 and to provide the same to the reactor 8 during the initiation of the reaction.
Referring now to figure 8 a method for producing carbon nanotubes (CNT's) using hybrid catalytic chemical vapor decomposition and industrially emitted gas (IEG) in an apparatus is shown.
In one implementation, a method for producing carbon nanotubes (CNT's) using hybrid catalytic chemical vapour decomposition an industrially emitted gas (IEG) in an apparatus is disclosed. The method comprises of:
• receiving (802) one or more catalyst by a means of one or more jet sprayer maintained at a controlled temperature, preferably, in a range of 300 °C to 400 °C, wherein said catalyst is ferrocene and is present inside a precursor chamber located outside said furnace; and
• receiving (804) a dried industrially emitted gas (IEG) by a means of a flow element connected to one or more dryer, wherein said dryer is located outside said furnace and connected to a mist eliminator 3; and
• attaining (806) a particular temperature, preferably of 700 °C, using temperature controller, thereby inducing production of said CNT's inside said reactor.
In one implementation, an apparatus for producing carbon nanotubes (CNT's) using hybrid catalytic chemical vapour decomposition an industrially emitted gas (IEG) is disclosed. The apparatus comprises of one or more furnace which further comprises of one or more temperature controller; and one or more reactor for the production of said CNT's. The reactor, at its one end, is configured to receive one or more catalyst by a means of one or more jet sprayer maintained at a controlled temperature, wherein said catalyst is present inside a precursor chamber located outside said furnace; and receive a dried industrially emitted gas (IEG) by a means of a flow element connected to one or more dryer, wherein said dryer is located outside said furnace. The temperature controller is configured to attain a particular temperature and thereby induces production of said CNT's inside said reactor. In one implementation, said rector is a vertical stainless steel tube reactor.
In one implementation, said catalyst is an organometallic compound and preferably ferrocene. In one implementation, said catalyst is dissolved in a solvent.
In one implementation, said catalyst is in a particulate form with a particle size in a range of 5 - 50 nm. In one implementation, said precursor chamber is configured to feed said catalyst into said reactor by a means of a metering pump.
In one implementation, said precursor chamber is configured to feed said catalyst into said reactor by means of an inlet means covered by said jet sprayer.
In one implementation, said jet sprayer is maintained at said controlled temperature, preferably, in a range of 300 °C to 400 °C.
In one implementation, dried industrially emitted gas (IEG) is a moisture free gas, which obtained from: said dryer coupled to one or more mist eliminator which is further coupled to one or more filter which is further coupled to one or more tar separating chamber, wherein: said tar separating chamber is configured to receive an industrially emitted gases (IEG) and separate volatiles present in said industrially emitted gas (IEG) from bottom of said tar separating chamber thereby forming residual gas; said filter is configured to remove solid particles, if any, from said residual gas; and said mist eliminator is configured to trap the moisture present in said residual gas, and thereby feed said residual gas to said dryer wherein said residual gas is dried to form said dried industrially emitted gas (IEG). In one implementation, said particular temperature is in a range, of 600 °C to 1200 °C, and preferably of 700 °C.
In one implementation, said reactor, at other end, is connected to blower configured to suck said CNT's into bag fiber filter for the collection of said CNT's.
In one implementation, an inert gas is passed through said reactor, before inducing said production of CNT's, to create an inert atmosphere in said reactor.
In one implementation, an inert gas is passed with a flow in a range, of 200 seem to 1000 seem, and preferably of 400 seem.
In one implementation, the blower is configured to suck CNT's using inert gas under high pressure. In one implementation, said dried industrially emitted gas (IEG) from said dryer is feed to the reactor using rotameter.
In one implementation, CNT's are of size between 10 to 100 nm. In one implementation, an apparatus for producing carbon nanotubes (CNT's) using a hybrid catalytic chemical vapor decomposition and industrially emitted gas (IEG), said apparatus comprising: a pair of volatile separating tanks, a particle filter, a moisture trapper, connected in line to a flow meter, and simultaneously connected to a reactor separately; a furnace enclosing the reactor is maintained at a suitable temperature to allow formation of CNTs inside the reactor; a vacuum system is connected end of the reactor to collect CNT's in a bag fiber filter.
Examples:
Industrially emitted gas (IEG) was used as hydrocarbon source at 400 seem and ferrocene as a catalyst. The ferrocene concentration was 0.5g/50 ml methanol using in-situ method in the middle of the first stage furnace 8 at 400°C with the help of jet sprayer 12. The temperature in the second stage furnace 8 was set at 800°C. In the mean time, the mixture feeding of IEG and catalyst for each one of the tubes will form, so that the formation of the CNT inside of reactor 8 is produced continuously. Simultaneously removal of the CNTs, CNTs formed in the internal surface of the reactor. Thus the cleaned for every 30 min using inert gas under high pressure and sucks into the bag fibre filter chamber 9 for collecting CNTs using vacuum device 10. In these conditions the production of carbon nanotubes was of 5 grams at efficiency rate of 70%, being the average diameter of 10 to 50 nm and length up to 150 μπι. Fig 8 shows the produced carbon nanotubes in these conditions.
Although implementations for a production of carbon nanotubes in large scale continuously using industrial emission at industrial sites have been described in language specific to structural features and/or methods, it is to be understood that the appended claims are not necessarily limited to the specific features or methods described. Rather, the specific features and methods are disclosed as examples of implementations for a production of carbon nanotubes in large scale continuously using industrial emission at industrial sites.

Claims

1. An apparatus for producing carbon nanotubes (CNT's) using a hybrid catalytic chemical vapor decomposition and an industrially emitted gas (IEG), said apparatus comprising:
one or more furnace comprising:
one or more temperature controller; and
one or more reactor for the production of said CNT's, WHEREIN:
said reactor, at its one end, is configured to:
receive one or more catalyst by a means of one or more jet sprayer maintained at a controlled temperature, wherein said catalyst is present inside a precursor chamber located outside said furnace; and
receive a dried industrially emitted gas (IEG) by a means of a flow element connected to one or more dryer, wherein said dryer is located outside said furnace; and said temperature controller is configured to attain a particular temperature and thereby induces production of said CNT's inside said reactor.
2. The apparatus as claimed in claim 1, wherein said reactor is a vertical stainless steel tube reactor.
3. The apparatus as claimed in claims 1 and 2, wherein said reactor comprises gas distribution plates having one or more holes to maintain uniform flow of IEG inside the reactor.
4. The apparatus as claimed in any of the preceding claims wherein said catalyst is an organometallic compound and preferably metalocene.
5. The apparatus as claimed in any of the preceding claims wherein said catalyst is dissolved in a solvent.
6. The apparatus as claimed in any of the preceding claims wherein said catalyst is in a particulate form with a particle size in a range of 5- 50 nm.
7. The apparatus as claimed in any of the preceding claims wherein said precursor chamber is configured to feed said catalyst into said reactor by a means of a dozing pump.
8. The apparatus as claimed in any of the preceding claims wherein said precursor chamber is configured to feed said catalyst into said reactor by means of an inlet means covered by said jet sprayer.
9. The apparatus as claimed in any of the preceding claims wherein said jet sprayer is maintained at said controlled temperature, preferably, in a range of 300 °C to 400 °C.
10. The apparatus as claimed in any of the preceding claims wherein said dried industrially emitted gas (IEG) is a moisture free gas, which obtained from:
said dryer coupled to one or more mist eliminator which is further coupled to one or more filter which is further coupled to one or more tar separating chamber, wherein:
said tar separating chamber is configured to receive an industrially emitted gases (IEG) and separate volatiles present in said industrially emitted gas (IEG) from bottom of said tar separating chamber thereby forming residual gas;
said filter is configured to remove solid particles, if any, from said residual gas; and said mist eliminator is configured to trap the moisture present in said residual gas, and thereby feed said residual gas to said dryer wherein said residual gas is dried to form said dried industrially emitted gas (IEG).
11. The apparatus as claimed in any of the preceding claims wherein said particular temperature is in a range, of 600 °C to 1200 °C, and preferably of 700 °C.
12. The apparatus as claimed in any of the preceding claims wherein said reactor, at other end, is connected to one or more blower configured to suck said CNT's into one or more bag fiber filter for the collection of said CNT's.
13. The apparatus as claimed in any of the preceding claims wherein an inert gas is passed through said reactor, before inducing said production of CNT's, to create an inert atmosphere in said reactor.
14. The apparatus as claimed in any of the preceding claims wherein an inert gas is passed with a flow in a range, of 200sccm to lOOOsccm, and preferably of 400 seem.
15. The apparatus as claimed in any of the preceding claims wherein blower is configured to suck CNT's using inert gas under high pressure.
16. The apparatus as claimed in any of the preceding claims wherein said dried industrially emitted gas (IEG) from said dryer is feed to said reactor using rotameter.
17. The apparatus as claimed in any of the preceding claims wherein CNT's are of size between 10 to 100 nm.
18. The apparatus as claimed in any of the preceding claims comprises one or more separating chambers configured to provide an industrially emitted gas (IEG) to said dryer, wherein said separation chamber is located outside said furnace.
19. An apparatus for producing carbon nanotubes (CNT's) using a hybrid catalytic chemical vapor decomposition and an industrially emitted gas (IEG), said apparatus comprising:
a pair of volatile separating tanks, a particle filter, a moisture trapper, connected in line to a flowmeter, and simultaneously connected to a reactor separately; a furnace enclosing the reactor is maintained at a suitable temperature to allow formation of CNTs inside the reactor;
a vacuum system is connected end of the reactor to collect CNT's in a bag fiber filter.
20. A method for producing carbon nanotubes (CNT's) using a hybrid catalytic chemical vapor decomposition and an industrially emitted gas (IEG) in an apparatus, said method comprising:
receiving one or more catalyst by a means of one or more jet sprayer maintained at a controlled temperature, preferably, in a range of 300 °C to 400 °C, wherein said catalyst is ferrocene and is present inside a precursor chamber located outside said furnace; and receiving a dried industrially emitted gas (IEG) by a means of a flow element connected to one or more dryer, wherein said dryer is located outside said furnace and connected to a mist eliminator; and
attaining a particular temperature, preferably of 700°C, using temperature controller, thereby inducing production of said CNT's inside said reactor.
21. The method as claimed in claim 20, wherein said dried industrially emitted gas (IEG) is a moisture free gas, which is obtained by:
receiving, by a tar separating chamber, an industrially emitted gases (IEG) and separating volatiles present in said industrially emitted gas (IEG) from bottom of said tar separating chamber thereby forming residual gas;
removing, by a filter, solid particles, if any, from said residual gas; and
trapping, using a mist eliminator, moisture present in said residual gas, and thereby feeding said residual gas to said dryer wherein said residual gas is dried to form said dried industrially emitted gas (IEG).
22. The method as claimed in any of the preceding claims comprises sucking, using one or more blower, said CNT's produced inside said reactor into one or more bag fiber filter.
23. The method as claimed in any of the preceding claims comprises one or more separating chambers configured to provide an industrially emitted gas (IEG) to said dryer, wherein said separation chamber is located outside said furnace.
24. A method of producing carbon nanotubes using Industrially Emitted gas (IEG) having a production station comprising.
a) A tapping connection from the industrial emitting source from industry. b) At least a pair of volatile separating chambers to separate tar from the
Industrially Emitted gas (IEG), each chamber contains inlet for gas and water and outlet for tar and water, with a level gauge to show the water level. c) At least one filter to remove the solid particles from the residual Industrially Emitted gas (IEG) coming out from the volatile separating chambers connected in line.
d) A mist eliminator chamber, which traps the moisture present in the Industrial Emitted gas, having the inlet and outlet for gas. e) A furnace is maintaining at a predetermined temperature to allow the synthesis of carbon nanotubes inside the reactor chamber, furnace designed in two part, part -1 heater and part - 2 heater. Part -1 is maintained at predetermined temperature for converting catalyst from liquid phase to vapor phase and part -2 is for converting industrially emitted gas (EIG) to carbon nanotubes with support of vapor phase catalyst.
f) A bag fiber filter chamber to collect the carbon nanotubes in bag, which is connected to the outlet of reactor chamber.
g) A suction device connected to the extraction pipe, wherein the suction comprises for the collection of carbon nanotubes in bag fiber filter, h) A control system is mounted on the front frame of the hybrid reactor.
25. The method as claimed in claim 24, wherein the temperatures isin the range of 400°C to 700°C.
26. The method as claimed in claim 24, wherein the precursor chamber is connected to the metering pump.
27. The method as claimed in claim 24, wherein the metering pump flows the predetermined flows of catalyst into the reactor from 0.1 to 10 ml/min.
28. The method as claimed in claim 24, wherein the jet sprayer is plugged at the inlet of the reactor chamber in the middle of the first state furnace, wherein it consists of inner and outer tube, whereas inner tube supply catalyst and outer tube supply gas into the reactor chamber for the production of carbon nanotubes within the predetermined temperature 300°C to 400°C.
29. The method as claimed in claim 24, producing single walled carbon nanotubes using industrially emitted gas.
30. The method as claimed in claim 24, producing multi walled carbon nanotubes using industrially emitted gas.
31. The method as claimed in claim 24, wherein the catalyst Ferrocene was dissolved in solvent is predetermined 0.5, 1, 1.5 and 2grams for the production of carbon nanotubes using industrially emitted gas (IEG).
32. The method as claimed in claim 24, wherein the carbon nanotubes shows homogeneity or heterogeneity in the sizes of the CNTs, with respect to the catalyst composition and temperature.
33. The method as claimed in claim 24, wherein the catalyst particle size is in the range of 10- 50nm.
34. The method as claimed in claim 24, wherein the carbon nanotubes homogeneous and heterogeneous in size between 10 to lOOnm.
35. The method as claimed in any preceding claims is adapted to all smoke emitting industries.
36. The method as claimed in any preceding claims wherein unnecessary gases which are not needed for the CNT production are separated out.
PCT/IB2015/059616 2014-12-15 2015-12-15 Production of carbon nanotubes in large scale continuously using industrial emission at industrial sites WO2016097985A2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IN3106/CHE/2014 2014-12-15
IN3106CH2014 IN2014CH03106A (en) 2014-12-15 2015-12-15

Publications (2)

Publication Number Publication Date
WO2016097985A2 true WO2016097985A2 (en) 2016-06-23
WO2016097985A3 WO2016097985A3 (en) 2016-12-08

Family

ID=54397168

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IB2015/059616 WO2016097985A2 (en) 2014-12-15 2015-12-15 Production of carbon nanotubes in large scale continuously using industrial emission at industrial sites

Country Status (2)

Country Link
IN (1) IN2014CH03106A (en)
WO (1) WO2016097985A2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11110049B2 (en) 2017-06-23 2021-09-07 The Procter & Gamble Company Composition and method for improving the appearance of skin

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7138100B2 (en) * 2001-11-21 2006-11-21 William Marsh Rice Univesity Process for making single-wall carbon nanotubes utilizing refractory particles
US8753602B2 (en) * 2006-10-19 2014-06-17 University Of Cincinnati Composite catalyst and method for manufacturing carbon nanostructured materials
JP5301793B2 (en) * 2007-05-07 2013-09-25 国立大学法人北海道大学 Fine carbon fiber aggregate for redispersion and method for producing the same
TW201341609A (en) * 2011-12-12 2013-10-16 Exxonmobil Upstream Res Co Methods and system for forming carbon nanotubes
KR101821113B1 (en) * 2011-12-12 2018-01-23 엑손모빌 업스트림 리서치 캄파니 Method and systems for forming carbon nanotubes
TWI627130B (en) * 2012-04-18 2018-06-21 美商艾克頌美孚上游研究公司 Removing carbon nanotubes from a continuous reactor effluent

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
None

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11110049B2 (en) 2017-06-23 2021-09-07 The Procter & Gamble Company Composition and method for improving the appearance of skin

Also Published As

Publication number Publication date
IN2014CH03106A (en) 2015-05-22
WO2016097985A3 (en) 2016-12-08

Similar Documents

Publication Publication Date Title
CN100586846C (en) Method for mass preparing hollow nano carbon cages with high quality
ES2716085T3 (en) Production procedure of carbon nanotube structures
CN1545486A (en) Production of carbon nanotubes
RU2540618C2 (en) Method and device to produce trisilylamine
CN1268414C (en) Method and installation for treating flue gas containing hydrocarbons
US6887291B2 (en) Filter devices and methods for carbon nanomaterial collection
Ding et al. Highly conductive and transparent single-walled carbon nanotube thin films from ethanol by floating catalyst chemical vapor deposition
KR20100092927A (en) Carbon nanotube or carbon nanofiber production apparatus and recovery apparatus
JP5860547B2 (en) Manufacturing method and manufacturing apparatus for long carbon nanotube
CN1757595A (en) Method for preparing orientation micron tube by original self-assembling of multi-wall carbon nanometer tubes
JP2018108588A (en) Multi reactor system in which pressure is adjusted
WO2016097985A2 (en) Production of carbon nanotubes in large scale continuously using industrial emission at industrial sites
US20230405510A1 (en) Methods and systems for adsorbing organometallic vapor
JP2005097014A (en) Carbon nanotube production apparatus, production method, and gas decomposer used therein
WO2014194181A1 (en) Method of preparing nanoparticle composition and nanoparticle composition formed thereby
US8119074B2 (en) Method and apparatus for the continuous production of carbon nanotubes
CN208545248U (en) A kind of efficiently purifying water installations
CN107001044A (en) The method that carbon structure is separated from seed crystal structure
RU2537487C2 (en) Production of material based on carbon nanotubes
CN106457406A (en) Apparatus for preparing synthesizing nano-particles using laser
RU2365674C2 (en) Device of carbon nanotubes growth by method of ethanol pyrolysis
CN217526913U (en) Purifier for rectifying column
CN212799643U (en) Nitrogen purification device
RU2567283C2 (en) Method and device for producing of carbon nanotubes
CN214749242U (en) Device for extracting soot particulate matters of engine oil

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 15828375

Country of ref document: EP

Kind code of ref document: A2

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 15828375

Country of ref document: EP

Kind code of ref document: A2