WO1998021146A1 - Procede et dispositif de production de fullerenes - Google Patents

Procede et dispositif de production de fullerenes Download PDF

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Publication number
WO1998021146A1
WO1998021146A1 PCT/RU1996/000317 RU9600317W WO9821146A1 WO 1998021146 A1 WO1998021146 A1 WO 1998021146A1 RU 9600317 W RU9600317 W RU 9600317W WO 9821146 A1 WO9821146 A1 WO 9821146A1
Authority
WO
WIPO (PCT)
Prior art keywords
fullerenes
soot
φulleρenοv
separation
synthesis
Prior art date
Application number
PCT/RU1996/000317
Other languages
English (en)
Russian (ru)
Inventor
Viktor Ivanovich Petrik
Andrei Dmitrievich Kirikov
Original Assignee
Viktor Ivanovich Petrik
Andrei Dmitrievich Kirikov
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 Viktor Ivanovich Petrik, Andrei Dmitrievich Kirikov filed Critical Viktor Ivanovich Petrik
Priority to RU96122306/25A priority Critical patent/RU2085484C1/ru
Priority to PCT/RU1996/000317 priority patent/WO1998021146A1/fr
Priority to AU17392/97A priority patent/AU1739297A/en
Publication of WO1998021146A1 publication Critical patent/WO1998021146A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • 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
    • 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
    • C01B32/152—Fullerenes
    • C01B32/154—Preparation
    • 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
    • C01B32/152—Fullerenes
    • C01B32/156—After-treatment

Definitions

  • the invention is disclosed in the scope of processes and apparatus for the synthesis, calculation and separation of fullerenes.
  • ⁇ e ⁇ vye sin ⁇ ez ⁇ ulle ⁇ en ⁇ v was ⁇ isan ⁇ a ⁇ ⁇ tsess is ⁇ a ⁇ eniya g ⁇ a ⁇ i ⁇ vy ⁇ ele ⁇ d ⁇ v ⁇ i ⁇ ezis ⁇ ivn ⁇ m nag ⁇ evs or arc a ⁇ m ⁇ s ⁇ e ⁇ e ine ⁇ n ⁇ g ⁇ gas ( ⁇ gae ⁇ zsheg, e ⁇ a ⁇ , "8 ⁇ C60: ⁇ ⁇ e ⁇ v G ⁇ gt ⁇ G sag ⁇ ".., ⁇ ashge, U ⁇ 247, p 354.. -357, ⁇ Ze ⁇ 27, 1990.
  • P ⁇ luchaemaya soot v ⁇ vse ⁇ ⁇ e ⁇ echislenny ⁇ s ⁇ s ⁇ ba ⁇ lib ⁇ s ⁇ s ⁇ ebae ⁇ sya s ⁇ s ⁇ en ⁇ is ⁇ a ⁇ i ⁇ eln ⁇ y ⁇ ame ⁇ y and ⁇ ulle ⁇ eny e ⁇ s ⁇ aga ⁇ uyu ⁇ sya therefrom ⁇ ganiches ⁇ imi ⁇ as ⁇ v ⁇ i ⁇ elyami ( "Zi ⁇ egsgShsa ⁇ yi ⁇ e ⁇ gasi ⁇ ⁇ G Gi ⁇ ege ⁇ e ⁇ C a ⁇ C Y ⁇ P sag ⁇ ⁇ G 'Z.Za ⁇ , e ⁇ .
  • the heating of other carbonaceous materials is produced by a resistive, industrial, magnetic, laser or other method.
  • the posed problem is also solved by the fact that the treatment is always directed or discharged to the process of heating and cooling.
  • the separation of fullerenes from soot is produced by the evaporation of fullerenes from soot collectors by heating them up to 700 ° - 900 ° C.
  • soot is mixed, the soot is mixed with the bulk, the mixture is freshly prepared and it is poured out.
  • the dryings are made by heating it in a vacuum chamber for the synthesis of fullerenes.
  • the separation of fullerenes into fractions is produced by collectors that are heated with a temperature of 400 ° to 480 ° C.
  • P ⁇ s ⁇ avlennaya task ⁇ eshae ⁇ sya ⁇ a ⁇ szhe ⁇ em, ch ⁇ in us ⁇ ys ⁇ ve for ssh ⁇ eza ⁇ ulle ⁇ en ⁇ v, v ⁇ lyuchayuschem emi ⁇ e ⁇ , vy ⁇ lnenny of ⁇ ve ⁇ d ⁇ y ugle ⁇ d ⁇ s ⁇ de ⁇ zhaschey zag ⁇ v ⁇ i, ⁇ mescheshyuy in ⁇ ab ⁇ chuyu ⁇ ame ⁇ u and s ⁇ eds ⁇ v ⁇ nag ⁇ eva emi ⁇ e ⁇ a with istochni ⁇ m ene ⁇ g ⁇ i ⁇ aniya, ⁇ ab ⁇ chaya ⁇ ame ⁇ a vy ⁇ lnena va ⁇ uumn ⁇ y, emi ⁇ e ⁇ imee ⁇ ⁇ mu, ⁇ bes ⁇ echivayuschuyu ⁇ b ⁇ az ⁇ vanie vs ⁇ ech
  • the unit is additionally equipped with a soot system installed in the working chamber.
  • the device is equipped with a collection of fullerenes made with the option of separating the fullerenes from the unit.
  • fullerene collectors are made in the form of two copper rings with vertical channels, which are not installed on the top and the bottom of the sink.
  • the power supply source was made in the form of a source of alternating current with a frequency of 8 to 40 kHz. Quick description of drawings
  • ⁇ a ⁇ ig. 1 is a schematic diagram of the industrial process of fullerenes.
  • ⁇ a ⁇ ig. 2 shows the flow diagram of molecular flows and the formation of fullerenes in a vacuum.
  • ⁇ a ⁇ ig. 4 shows the dependence of the output of the fullerenes at the frequency of the alternating current at a) resistive and b) induction heating.
  • FIG. 1 The scheme of the industrial process of fullerenes is depicted in FIG. 1.
  • the preparation of the mixture includes homogenization in the mixture from the bulk scrubber, soot and waste from the previous batch.
  • Dryer is pre-cooked at first at a temperature of 400 ° C, and is therefore not used in the process.
  • the process of fullerene synthesis must be sufficient to ensure that the average temperature does not slow down. at emitting transients.
  • This operation is achieved under the conditions of a sufficiently developed development of the emitter and a large, large-scale power supply.
  • a melting process that emits a large amount of emissivity and turns them into fullerenes, and less heated parts are consumptive
  • Indifferent values of the double space and time are divided by a separate emitter and are free to run at a rate of 100 and is 60 times higher. With this 10–70% of the emitter’s mass, it can be converted into fuller-containing soot with a useful product of 5–20% or higher. The indicated results are illustrated by the large-scale application of the method of fuller production.
  • EXAMPLE 1 Procurement from a sales department weighing 127.3 grams, the sales account is shown in FIG. 3 b), with a diameter of 60 mm, a height of 30 mm, was placed in a water-cooled induction chamber in a vacuum chamber.
  • ⁇ ⁇ ame ⁇ e was d ⁇ s ⁇ ignu ⁇ va ⁇ uum 10 "5 ⁇ , ⁇ sle chsg ⁇ on indu ⁇ byl ⁇ ⁇ dan ⁇ na ⁇ yazhenie 700 ⁇ ⁇ n ⁇ e 300 ⁇ with chasto ⁇ y 10 ⁇ Gts Che ⁇ ez 10 ⁇ em ⁇ e ⁇ a ⁇ u ⁇ a on na ⁇ uzhn ⁇ y ⁇ ve ⁇ n ⁇ s ⁇ i zag ⁇ tov ⁇ i d ⁇ s ⁇ igla 4000 ° C, and vnu ⁇ enni ⁇ ⁇ ve ⁇ n ⁇ s ⁇ ya ⁇ ⁇ ltsevy ⁇ ⁇ anav ⁇ -. 4350 ° S.
  • Che ⁇ ez 10 istochni ⁇ was ⁇ lyuchen and power
  • EXAMPLE 2 Procurement from the processing unit weighing 17.4 g, the form is supplied in FIG. 3 a), with a diameter of 4 mm, a height of 100 mm, after being pre-heated at a temperature of 1000 ° C, it was placed in a vacuum chamber at a pressure of 4 " at a constant pressure of 50 5 ⁇ em ⁇ e ⁇ a ⁇ u ⁇ a on na ⁇ uzhn ⁇ y ⁇ ve ⁇ n ⁇ s ⁇ i zag ⁇ tov ⁇ i d ⁇ s ⁇ igla 4000 ° C, and vnu ⁇ enni ⁇ ⁇ ve ⁇ n ⁇ s ⁇ ya ⁇ ⁇ ltsevy ⁇ ⁇ anav ⁇ - 4300 ° C with 10 Che ⁇ ez is ⁇ ch ⁇ s was ⁇ lyuchen and power The ⁇ ame ⁇ a ⁇ lazhdena and za ⁇ em ⁇ azva ⁇ uumi ⁇ vana and ⁇ y ⁇ a ⁇ es ⁇ s ⁇ a ⁇ a zag ⁇ tov
  • the main part of the device is water-cooled chamber 1 from stainless steel, in the center there is a heating element 2, for example, copper used.
  • a heating element for example, copper used
  • the industrial unit is equipped with an emitter 3, which is supplied with a special washer;
  • the chamber is evacuated, and therefore the movement of the preparations takes place without breaking the vacuum, thanks to the use of bellows 6.
  • P ⁇ i v ⁇ lyuchenii nag ⁇ eva ⁇ eln ⁇ g ⁇ elemen ⁇ a, na ⁇ ime ⁇ , ⁇ i ⁇ d ⁇ slyuchenii indu ⁇ a ⁇ m ⁇ schn ⁇ mu vys ⁇ chasto ⁇ n ⁇ mu is ⁇ chni ⁇ u ⁇ a ⁇ is ⁇ di ⁇ ⁇ az ⁇ g ⁇ ev na ⁇ uzhny ⁇ ⁇ ve ⁇ n ⁇ s ⁇ ey washers ⁇ a ⁇ dyaschi ⁇ sya vnu ⁇ i nag ⁇ eva ⁇ eln ⁇ g ⁇ elemen ⁇ a, na ⁇ ime ⁇ , indu ⁇ to ⁇ a.
  • the housing of the 5 rooms is subject to the movement of the workpieces with all kinds of fasteners, so that the external parts of the washers - the workpieces are completely free of charge, but the interior is completely empty. In the case of discharges, high clearance of washers, intensive processing of soot and soot occurs.
  • the source of energy supply is turned off and the camera is cooled down and discharged.
  • the final product in this case is fullerene-containing soot, which is removed from the chamber by mechanical means.
  • soot compartments 7 and 8 are fitted with upper 11, 12, 13 and lower 14, 15, 16 collectors of fullerenes, which represent a genuine copper ring with vegas.
  • the reservoirs are heated due to the soot emission control, and a temperature range of 480 to 400 ° C is formed along with their channels.
  • the channels of collectors are fuller and are at risk of being at risk of damage to them.
  • ⁇ a blizhni ⁇ ⁇ lle ⁇ a ⁇ 13 and 14 ⁇ ndensi ⁇ ue ⁇ sya mixture vysshi ⁇ ⁇ ulle ⁇ en ⁇ v C W, C and w d ⁇ ugi ⁇ on ⁇ lle ⁇ to ⁇ a ⁇ 12 and 15 - 70 C, at 11 and 16 ⁇ lle ⁇ a ⁇ - C S0.
  • the final products here are soot, which can be used for the next synthesis, and the indicated fullerene fractions.
  • EXAMPLE 5 The same preparations were used as in Example 3; however, in chamber 1, the soot was installed with soot 7 and 8, and so on, 11-16. The synthesis was carried out in the same mode, as in Example 3.
  • ⁇ ulle ⁇ eny m ⁇ gu ⁇ is ⁇ lz ⁇ va ⁇ sya ⁇ a ⁇ szhe in ⁇ aches ⁇ ve ⁇ sn ⁇ vy for ⁇ izv ⁇ ds ⁇ va a ⁇ umulya ⁇ ny ⁇ ba ⁇ a ⁇ ey, ⁇ bladayuschi ⁇ b ⁇ lee vys ⁇ y e ⁇ e ⁇ ivn ⁇ s ⁇ yu, small ves ⁇ m and ⁇ a ⁇ zhe e ⁇ l ⁇ giches ⁇ y and sani ⁇ a ⁇ n ⁇ y bez ⁇ asn ⁇ s ⁇ yu n ⁇ s ⁇ avne ⁇ shyu with s ⁇ v ⁇ emennymi a ⁇ s ⁇ umulya ⁇ ami.
  • the proposed method of fuller production does not have any limitation on productive and non-hazardous process.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Composite Materials (AREA)
  • Manufacturing & Machinery (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

Cette invention se rapporte au domaine des procédés et des appareils de synthèse, de purification et de séparation de fullerènes, et permet de synthétiser de grandes quantités de fullerènes sans générer de déchets. Ce procédé de production de fullerènes consiste à effectuer un chauffage par induction, par magnétron, par laser ou autre d'une préforme solide contenant du carbone et possédant une forme spéciale. Ce chauffage se fait sous vide de manière à former des flux d'agglomérats carbonés qui se rencontrent ou qui se croisent. Le dispositif de synthèse de fullerènes comprend un émetteur capable de se déplacer dans la chambre à vide, ainsi qu'un système de chauffage de cet émetteur. Ce dispositif peut également comprendre des récepteurs de suie ainsi que des collecteurs pour la séparation des fullerènes.
PCT/RU1996/000317 1996-11-13 1996-11-13 Procede et dispositif de production de fullerenes WO1998021146A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
RU96122306/25A RU2085484C1 (ru) 1996-11-13 1996-11-13 Способ и устройство для производства фуллеренов
PCT/RU1996/000317 WO1998021146A1 (fr) 1996-11-13 1996-11-13 Procede et dispositif de production de fullerenes
AU17392/97A AU1739297A (en) 1996-11-13 1996-11-13 Method and device for producing fullerenes

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/RU1996/000317 WO1998021146A1 (fr) 1996-11-13 1996-11-13 Procede et dispositif de production de fullerenes

Publications (1)

Publication Number Publication Date
WO1998021146A1 true WO1998021146A1 (fr) 1998-05-22

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RU (1) RU2085484C1 (fr)
WO (1) WO1998021146A1 (fr)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6896864B2 (en) 2001-07-10 2005-05-24 Battelle Memorial Institute Spatial localization of dispersed single walled carbon nanotubes into useful structures
US6878361B2 (en) 2001-07-10 2005-04-12 Battelle Memorial Institute Production of stable aqueous dispersions of carbon nanotubes
US7842271B2 (en) 2004-12-07 2010-11-30 Petrik Viktor I Mass production of carbon nanostructures
RU2343111C1 (ru) * 2007-04-06 2009-01-10 Общество с ограниченной ответственностью "Научно-производственная компания "НеоТекПродакт" Установка для производства фуллеренсодержащей сажи
RU2705064C1 (ru) * 2018-06-19 2019-11-01 Общество с ограниченной ответственностью "ПКФ Альянс" Устройство для получения фуллеренсодержащей сажи

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1587000A1 (ru) * 1988-05-23 1990-08-23 Предприятие П/Я Р-6561 Способ получени кластеров полиэдрических углеводородов
WO1994002413A2 (fr) * 1992-07-24 1994-02-03 Max-Planck-Gesellschaft Zur Förderung Der Procede de production et de separation de fullerenes
WO1994004461A1 (fr) * 1992-08-14 1994-03-03 Materials And Electrochemical Research Corporation Procedes et appareils permettant de produire des fullerenes
US5300203A (en) * 1991-11-27 1994-04-05 William Marsh Rice University Process for making fullerenes by the laser evaporation of carbon
EP0646544A1 (fr) * 1993-10-02 1995-04-05 Till Keesmann Procédé et appareil pour la préparation de fullerènes
JPH07237912A (ja) * 1994-02-28 1995-09-12 Univ Nagoya フラーレン類の製造方法及びその製造装置
JPH07315819A (ja) * 1994-05-19 1995-12-05 Toyo Tanso Kk フラーレン類製造用原料及びフラーレン類の製造方法
JPH0848510A (ja) * 1994-08-04 1996-02-20 Satoru Mieno アーク放電によるフラーレン自動合成装置
US5510098A (en) * 1994-01-03 1996-04-23 University Of Central Florida CVD method of producing and doping fullerenes

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1587000A1 (ru) * 1988-05-23 1990-08-23 Предприятие П/Я Р-6561 Способ получени кластеров полиэдрических углеводородов
US5300203A (en) * 1991-11-27 1994-04-05 William Marsh Rice University Process for making fullerenes by the laser evaporation of carbon
WO1994002413A2 (fr) * 1992-07-24 1994-02-03 Max-Planck-Gesellschaft Zur Förderung Der Procede de production et de separation de fullerenes
WO1994004461A1 (fr) * 1992-08-14 1994-03-03 Materials And Electrochemical Research Corporation Procedes et appareils permettant de produire des fullerenes
EP0646544A1 (fr) * 1993-10-02 1995-04-05 Till Keesmann Procédé et appareil pour la préparation de fullerènes
US5510098A (en) * 1994-01-03 1996-04-23 University Of Central Florida CVD method of producing and doping fullerenes
JPH07237912A (ja) * 1994-02-28 1995-09-12 Univ Nagoya フラーレン類の製造方法及びその製造装置
JPH07315819A (ja) * 1994-05-19 1995-12-05 Toyo Tanso Kk フラーレン類製造用原料及びフラーレン類の製造方法
JPH0848510A (ja) * 1994-08-04 1996-02-20 Satoru Mieno アーク放電によるフラーレン自動合成装置

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
B.S. KAVERIN et al., "High-Efficiency Set for Direct Current Arc Synthesis of Fullerene Containing Soot", page 78. *
FULLERENES AND ATOMIC CLUSTERS, IWFAC-93, INTERNATIONAL WORKSHOP, ABSTRACTS OF INVITED LECTURES AND CONTRIBUTED PAPERS, 4-9 October 1993, (St. Peterburg, Russia), G.A. DYUZHEV et al., "Fullerenes Producing in an Arc Discharge", page 32. *
V.L. KARNATSEVICH et al., "The Preparation of C60 Fullerene from C60/C70 Extract by Sublimation Under Vacuum", page 77. *
V.P. BUBNOV et al., "Production of Fullerene-Rich Carbon Soot by a D.C. and A.C. Elect Arc", page 60. *

Also Published As

Publication number Publication date
AU1739297A (en) 1998-06-03
RU2085484C1 (ru) 1997-07-27

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