WO2016097985A2 - Fabrication en série et en continu de nanotubes de carbone au moyen d'une émission industrielle sur des sites industriels - Google Patents

Fabrication en série et en continu de nanotubes de carbone au moyen d'une émission industrielle sur des sites industriels Download PDF

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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
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WO
WIPO (PCT)
Prior art keywords
reactor
ieg
gas
catalyst
carbon nanotubes
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Application number
PCT/IB2015/059616
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English (en)
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WO2016097985A3 (fr
Inventor
Venkateswara Rao SODISETTI
Venkatesan K. R.
Venkateswer Rao MANDAPATI
Original Assignee
Sodisetti Venkateswara Rao
K R Venkatesan
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Publication date
Application filed by Sodisetti Venkateswara Rao, K R Venkatesan filed Critical Sodisetti Venkateswara Rao
Publication of WO2016097985A2 publication Critical patent/WO2016097985A2/fr
Publication of WO2016097985A3 publication Critical patent/WO2016097985A3/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • C01B32/162—Preparation characterised by catalysts
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture 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

La présente invention a trait à un appareil hybride qui sert à fabriquer en continu et de façon économique des nanotubes de carbone (CNT) à l'aide de gaz émis industriels (IEG) sur des sites industriels, ainsi qu'à un procédé pour la réalisation de cette fabrication. L'appareil pour la synthèse de CNT comprend : une paire de réservoirs de séparation volatils ; un filtre à particules ; un piège à humidité qui est relié en ligne à un débitmètre, et qui est aussi relié simultanément et séparément à un réacteur ; un four qui est maintenu à une température appropriée pour permettre la formation de CNT à l'intérieur du réacteur ; un système à vide qui est relié à une extrémité du réacteur pour collecter des CNT dans un filtre fibreux à sac.
PCT/IB2015/059616 2014-12-15 2015-12-15 Fabrication en série et en continu de nanotubes de carbone au moyen d'une émission industrielle sur des sites industriels WO2016097985A2 (fr)

Applications Claiming Priority (2)

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

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WO2016097985A2 true WO2016097985A2 (fr) 2016-06-23
WO2016097985A3 WO2016097985A3 (fr) 2016-12-08

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US11110049B2 (en) 2017-06-23 2021-09-07 The Procter & Gamble Company Composition and method for improving the appearance of skin

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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 (ja) * 2007-05-07 2013-09-25 国立大学法人北海道大学 再分散用微細炭素繊維集合塊およびその製造方法
TW201341609A (zh) * 2011-12-12 2013-10-16 Exxonmobil Upstream Res Co 用於形成碳奈米管之方法及系統
WO2013090444A1 (fr) * 2011-12-12 2013-06-20 Exxonmobil Upstream Research Company Procédé et systèmes pour former des nanotubes de carbone
TWI627130B (zh) * 2012-04-18 2018-06-21 美商艾克頌美孚上游研究公司 由連續反應器流出物移出碳奈米管之方法

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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

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WO2016097985A3 (fr) 2016-12-08

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