• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    An apparatus for the production of Graphene and similar atomic scale laminar materials by the delamination of a bulklaminar material, such as graphite; the apparatus comprising a main pump for pumping a fluid comprising a solid suspension of particles of the bulk laminar material, at a pressure of greater than 1MPa, towards core components (10) comprising a fluid conduit(12),wherein the fluid conduit directs fluid against an impact head(16); the impact head and the conduit being arranged so that an annular gap(202)of between 500μm and 1μm results between an end of the conduit and the impact head, and an impact head surround (26) which extends the region in which the fluid is constrained before exiting the core components. The present invention describes an apparatus for the production of Graphene and similar atomic scale laminar materials by the delamination of a bulk laminar material, such as graphite. The apparatus comprises a pump which directs fluid against an impact head and through an annular gap of between 500μm and 1μm. This causes differential shear forces, causing the bulk material to split into laminar sheets.
    公开号:ES2681960A2
    申请号:ES201890023
    申请日:2016-10-13
    公开日:2018-09-17
    发明作者:Paul Ladislaus；Lee GLASGOW；Ronan McHale
    申请人:Thomas Swan and Co Ltd；
    IPC主号:
    专利说明:

    image 1
    image2
    image3
    image4
    image5
    nucleus.
    Preferably, the solid particles are graphite particles, hexagonal boron nitride or molybdenum disulfide. More preferably, the solid particles are graphite.
    The fluid can be a suspension of particles in the particle size range of 1 µm to 1000 µm.
    It has been found that this apparatus allows the delamination of graphite and similar sheet materials at pressures and energy levels below those required by a microfluor. This has the additional advantage that it reduces heat accumulation in the process.
    In a (substantially) perpendicular arrangement and within a narrow band of pneumatically assisted movement, annular separation is highly beneficial in providing a consistent product. Therefore, substantially perpendicular encompasses at least a 10 ° deviation, preferably not more than 1 °, more preferably not more than 0.1 °. Such deviation or displacement can be achieved by a cone to provide a symmetrical impact face of the impact head.
    In delamination processes, high temperature is beneficial as well as, for example, additional kinetic energy, to separate (exfoliate) a sheet of material, such as graphene is reduced.
    Surprisingly it has been found that production efficiency is inversely proportional to temperature. The apparatus of the present invention, as described above, therefore preferably comprises:
    a cooler / cooler in fluid communication with the fluid conduit and the pump, the cooler / cooler being configured to reduce the temperature of the fluid, preferably at a temperature below 10 ° C. This is particularly advantageous when a head impact brittle material is used, such as diamond, silicon nitride, silicon carbide, or cubic boron nitride as cracking and fragmentation can be reduced.
    image6
    image7
    image8
    a suspension of sheet material in a liquid.
    In the process of the present invention, the sheet material is preferably graphite and the atomic scale sheet material is graphene.
    The liquid in which the sheet material is suspended is preferably water. Water is preferable due to its high specific thermal capacity, which allows the process to be better maintained in the temperature range of 30 ° C to 80 ° C. In addition, the localized head temperature, which, as mentioned above, is preferably below room temperature and is more easily maintained with water as a liquid. Other suitable liquids are liquid hydrocarbons.
    The process of the present invention is preferably performed at a temperature of 30 ° C to 80 ° C.
    The graphite is preferably in the particle size range of 1 µm to 1000 µm, more preferably in the particle size range of 3 µm to 50 µm, more preferably in the size range of 15 to 25 µm. The size can be determined using a Mastersizer Malvern particle size measurement using measure D4.
    The sheet material, preferably graphite, charged in the liquid phase is preferably in the range of up to 500 grams per liter (g / l), more preferably the sheet material load is 10 to 125 g / l, more preferably 125 g / l.
    The fluid of the present invention is impacted on the impact head at a pressure greater than 1 MPa, more preferably at a pressure in the range of 10 MPa to 150 MPa, still more preferably in the range of 40 MPa to 100 MPa, with greater preference at a pressure in the range of 50 to 70 MPa. Pressure selection provides optimized quantity, performance and energy consumption.
    It has surprisingly been determined that simply the case of a higher pressure is better, this potentially produces greater impact forces on the impact head, but that an optimum pressure range is found. This optimal range provides higher quality in laminated sheets, particularly graphene and
    image9
    surfactant of the sheet of material (which during this process can be precipitated) to produce a composition consisting of sheet sheets of material in the liquid.
    The process of the present invention preferably comprises a filtration stage in which the particulate material is removed by means of the filtration stage (using any mechanism). The filtration stage may preferably take place after the neutralization stage.
    The present invention also encompasses a further aspect of the use of a high pressure homogenizer, such as that of the type described with respect to the drawings, for the production of graphene from graphite in aqueous suspension.
    The conditions and parameters relevant to the process of the present invention are also applicable to the configuration of the apparatus of the present invention. Unless otherwise indicated herein, temperatures are 25 ° C and atmospheric pressure is 1 atm.
    An impact head material is a material that comprises the impact head and does not need to cover the entire head, but comprises at least part, preferably the entire impact face of the impact head. Brief description of the figures
    The apparatus of the present invention will be illustrated below by means of the following drawings in which:
    Figure 1 shows a schematic view of the fluid path through the apparatus of the present invention and illustrates core components.
    Figure 2 shows a schematic cross-sectional view of a first arrangement of core components of the apparatus of the present invention.
    Figure 3 shows a schematic cross-sectional view of a second arrangement of core components of the apparatus of the present invention.
    Figure 4 shows a schematic cross-sectional view of a second arrangement of core components of the apparatus of the present invention.
    Figure 5 shows a schematic view of a system or apparatus of the present invention comprising the core components together with auxiliary components to provide an optimal processing system for performing the process of the present invention.
    The following characteristics are provided in the drawings:
    10 Core component set. 12 Duct / volume of fluid. 14 Entrance to the fluid conduit at a distal point of the impact head. 16 Impact head assembly. 18 Face (optional) of the impact head assembly (optional. 20 Annulus (ring). 202 Trunk ring. 204 Outer ring. 22 Support structure. 24 Fluid conduit outlet near the impact head / proximal end of the conduit. 242 Proximal end of the duct, alternatively 26 Flange for the impact head 28 Face of the impact head 32 Duct / pipe 100 System or apparatus (expanded) of the present invention 110 Container of starting material 112 Pump high pressure 114 Valve 124 Pressure drop valve 116 Container of finished product.
    image10
    The width of the annular space is between 500 µm and 200 µm at its widest end, and between 200 µm and 1 µm at its narrowest end.
    In Figure 4, the proximal end of the duct does not abut a flange for the
    5 impact head and provides an outer annular zone 204 in which turbulent flow can occur for improved processing. Specifically, greater delamination can be achieved when that area is used. The area also seems to reduce fluid cavitation that increases the wear speed of the components. The area of the outer ring 204 is shown in Figure 3 together with the face
    10 beveled internally, but Figure 3 can be provided without zone 204.
    With reference to Figure 5, a processing system of the present invention comprises core components 10 as described above. The system is configured so that the raw material is provided in the
    15 container 110 and is pumped through the high pressure pump 112 into the duct 12/32 in the core components 10 and in particular the impact head 16 before exiting the optional pressure drop valve 124 to provide back pressure to core components for improved processing.
    20 Specifically, maintaining a back pressure, such as 10 to 100 kPa, reduces fluid cavitation in the impact head and prolongs the life of the device. The system is further configured in such a way that the fluid then passes through the directional control valve 114, either as a finished product to the product container 116 or is recirculated through the cooler / cooler 118
    25 before entering high pressure pump 112 for optional recirculation.
    权利要求:
    Claims (1)
    [1]
    image 1
    image2
    image3
    类似技术:
    公开号 | 公开日 | 专利标题
    ES2681960A2|2018-09-17|Apparatus and method for bulk production of atomically thin 2-dimensional materials including graphene
    ES2600458T3|2017-02-09|Aerosol generator device and system with improved air flow
    ES2555552T3|2016-01-04|Intervertebral implant
    CO7230341A2|2015-03-31|Propping agent discharge system and a container for use in said pointing agent discharge system
    CN105112578B|2017-08-25|A kind of slag cooling device
    ES2533829T3|2015-04-15|Axially and radially cooled brake disc with cover
    ES2290638T3|2008-02-16|METHOD AND APPARATUS TO COOL A HEAT GENERATION STRUCTURE.
    ES2864198T3|2021-10-13|Exfoliation of Layered Materials Using Wet Jet Grinding Techniques
    US9533277B2|2017-01-03|Device for producing gas hydrate
    AR096087A1|2015-12-02|REDUCTION OF THE SIZE OF THE PARTICLE OF AN ANTIMUSCARINIC COMPOUND, MICRONIZED CRYSTALLINE PARTICLES, FORMULATION AND INHALER FOR DRY POWDER
    AR088015A1|2014-04-30|MIXING CANILLA WITH FILTER
    BR112015025318A2|2017-07-18|adapter, set of an adapter and a sachet, system, and method for preparing at least a portion of a single beverage serving with an adapter
    CO2018001611A2|2018-07-10|Sustaining agent particles formed from slurry droplets and methods of use
    CL2013002966A1|2014-05-16|Stable mixture comprising surface modified particles; process to produce said particle; and use of said particles.
    ES2525574T3|2014-12-26|Jet regulator
    EP2008721A3|2012-01-18|Center-feed nozzle in a cylindrical feed-inlet tube for improved grinding efficiency in a fluid-energy mill
    CN205690082U|2016-11-16|A kind of drainage arrangement of thinning machine vacuum line
    ES2829632T3|2021-06-01|Multi-stage compression system and procedure of a gas using a liquid
    ES2859149T3|2021-10-01|Apparatus and procedure for the bulk production of atomically thin two-dimensional materials, including graphene
    ES2553589T3|2015-12-10|Bioreactor comprising a mixing chamber
    MX2018001197A|2018-04-24|Methods of pneumatically conveying solid particulates.
    AR100266A1|2016-09-21|FLAT HYDRAULIC CYLINDER, HYDRAULIC LIFTING PAD, USE OF ONE OF THESE AND PROCEDURE TO ALIGN A GENERATOR
    ES2666137T3|2018-05-03|Heat exchanger with collector channel for the extraction of a liquid phase
    CN105792997A|2016-07-20|Conveyance device
    CHEN et al.2016|Process Research of Lapping Efficiently and Super Smooth Polishing on the Al_ | O_3 Ceramics Substrate
    同族专利:
    公开号 | 公开日
    GB2543486A|2017-04-26|
    GB201617395D0|2016-11-30|
    CN108137328A|2018-06-08|
    ES2681960R1|2018-10-09|
    US10822238B2|2020-11-03|
    US20200255293A1|2020-08-13|
    GB2545060B|2018-05-23|
    WO2017064496A1|2017-04-20|
    CN108137328B|2022-01-25|
    ES2681960B1|2019-04-22|
    GB2545060A|2017-06-07|
    GB201518105D0|2015-11-25|
    GB2543486B|2018-07-18|
    KR20180066153A|2018-06-18|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US4352573A|1980-01-29|1982-10-05|Gaulin Corporation|Homogenizing method|
    US6318649B1|1999-10-06|2001-11-20|Cornerstone Technologies, Llc|Method of creating ultra-fine particles of materials using a high-pressure mill|
    WO2004052567A2|2002-12-06|2004-06-24|Cornerstone Technologies, L.L.C.|High g mill in a blending and drying system|
    ITPR20070080A1|2007-10-23|2009-04-24|Niro Soavi Spa|HOMOGENIZING VALVE|
    US9199841B2|2009-01-26|2015-12-01|Advanced Fiber Technologies, Inc.|Method for disentanglement of carbon nanotube bundles|
    CN101671015B|2009-10-13|2011-07-20|南昌航空大学|Method of producing graphene|
    GB2483288A|2010-09-03|2012-03-07|Trinity College Dublin|Exfoliation process for forming semiconducting nanoflakes|
    GB201103499D0|2011-03-01|2011-04-13|Univ Ulster|Process|
    AU2012286515C1|2011-07-19|2016-10-27|Flex-G Pty Ltd|Exfoliating laminar material by ultrasonication in surfactant|
    BR102012000855A2|2012-01-13|2013-11-19|Evolucoes En Ltda|PERPETUAL GENERATION SYSTEM BY SELF-GENERATION CYCLE|
    CN103570003B|2012-07-25|2016-03-16|中国科学院大连化学物理研究所|A kind of method of macroscopic preparation of graphene and two-dimentional boron nitride crystal material|
    GB201304770D0|2013-03-15|2013-05-01|Provost Fellows Foundation Scholars And The Other Members Of Board Of|A scalable process for producing exfoliated defect-free, non-oxidised 2-dimens ional materials in large quantities|
    WO2015099457A1|2013-12-26|2015-07-02|주식회사 엘지화학|Production method for graphene|
    WO2015099378A1|2013-12-26|2015-07-02|주식회사 엘지화학|Graphene production method, and graphene dispersion composition|
    KR101753294B1|2015-01-13|2017-07-20|에스엠에스주식회사|Manufacturing Method of Graphene|
    CN106455603B|2015-04-30|2021-03-16|Gea机械设备意大利股份公司|Method for making yoghurt or another fermented milk-based product|GB201613012D0|2016-07-27|2016-09-07|Price Richard J|Improvements relating to graphene nanomaterials|
    EP3525935A1|2016-10-13|2019-08-21|Thomas Swan & Co. Ltd|Apparatus and method for bulk production of atomically thin 2-dimensional materials including graphene|
    GB2550985B|2016-10-13|2020-03-25|Swan Thomas & Co Ltd|Apparatus and method for bulk production of atomically thin 2-dimensional materials including graphene|
    GB2555097B|2016-10-13|2020-04-08|Swan Thomas & Co Ltd|Apparatus and method for bulk production of atomically thin 2-dimensional materials including graphene|
    CN108059152B|2018-01-26|2021-06-15|黑龙江科技大学|Method for preparing graphene nanosheet through micro-friction and abrasion|
    GB201801590D0|2018-01-31|2018-03-14|Swan Thomas & Co Ltd|Improvements Relating to Nanomaterials|
    IT201800010845A1|2018-12-05|2020-06-05|Gea Mech Equipment Italia S P A|HIGH PRESSURE HOMOGENIZING VALVE AND PRODUCTION PROCESS OF CARBON-BASED NANOSTRUCTURED MATERIALS, IN PARTICULAR GRAPHENE AND CARBON NANOTUBES|
    US20210158995A1|2019-11-26|2021-05-27|Trimtabs Ltd|Cables and methods thereof|
    GB202018325D0|2020-11-20|2021-01-06|First Graphene Uk Ltd|Improvements relating to carbon materials|
    GB202116753D0|2021-11-19|2022-01-05|First Graphene Uk Ltd|Improvements relating to graphene nanomaterial suspensions|
    法律状态:
    2018-09-17| BA2A| Patent application published|Ref document number: 2681960 Country of ref document: ES Kind code of ref document: A2 Effective date: 20180917 |
    2018-10-09| EC2A| Search report published|Ref document number: 2681960 Country of ref document: ES Kind code of ref document: R1 Effective date: 20181002 |
    2019-04-22| FG2A| Definitive protection|Ref document number: 2681960 Country of ref document: ES Kind code of ref document: B1 Effective date: 20190422 |
    优先权:
    申请号 | 申请日 | 专利标题
    GB1518105.0A|GB2543486B|2015-10-13|2015-10-13|Apparatus and method of using the apparatus for bulk production of atomically thin 2-dimensional materials including graphene|
    GB1518105|2015-10-13|
    PCT/GB2016/053177|WO2017064496A1|2015-10-13|2016-10-13|Apparatus and method for bulk production of atomically thin 2-dimensional materials including graphene|
    [返回顶部]