CN108654828A - Liquid-based method and apparatus for graphite purification - Google Patents

Liquid-based method and apparatus for graphite purification Download PDF

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Publication number
CN108654828A
CN108654828A CN201711071753.1A CN201711071753A CN108654828A CN 108654828 A CN108654828 A CN 108654828A CN 201711071753 A CN201711071753 A CN 201711071753A CN 108654828 A CN108654828 A CN 108654828A
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CN
China
Prior art keywords
graphite
present
graphite flake
water
flake
Prior art date
Legal status (The legal status 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 status listed.)
Pending
Application number
CN201711071753.1A
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Chinese (zh)
Inventor
谢尔盖·阿列克谢耶夫
鲍里斯·戈德斯坦
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Nano Graphene Ltd By Share Ltd
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Nano Graphene Ltd By Share Ltd
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Publication of CN108654828A publication Critical patent/CN108654828A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03BSEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B7/00Combinations of wet processes or apparatus with other processes or apparatus, e.g. for dressing ores or garbage
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/20Graphite
    • C01B32/21After-treatment
    • C01B32/215Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B04CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04BCENTRIFUGES
    • B04B5/00Other centrifuges
    • B04B5/10Centrifuges combined with other apparatus, e.g. electrostatic separators; Sets or systems of several centrifuges

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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

The present invention relates to the device and method for purifying natural graphite, by removing rock material to increase the concentration of the carbon in graphite flake.The gist of the invention is that centrifugal acceleration is applied to the mixture of water and graphite flake.The acceleration of application so that graphite flake is impinging one another;Therefore, triggering rock material is detached and is rinsed from graphite flake.The method provided is simple, because it does not need complex equipment, and can implement near graphite deposit, and This further reduces transport and overall manufacturing costs.

Description

Liquid-based method and apparatus for graphite purification
Technical field
The present invention relates to the technical fields of carbon material, graphite material and natural graphite ore dressing.Specifically, the present invention describes From the device and method of graphite flake removal of impurity by for being subjected to centrifugal acceleration by making the mixture of graphite flake and water.
Background technology
Graphite, as the most common polymorph of naturally occurring crystalline carbon, many different products (such as accumulator, Refractory material, electric product, etc.) production in be widely used.Graphite is a kind of unique material, because as covalent object Matter does not answer conduction, however it is really conductive.Graphite is pure carbonizable substance, three covalently bondeds wherein in its valence electron to three A other carbon atoms.However, the 4th valence electron is unfettered, and therefore can move freely.Such valence electron allows electric current to exist Certain party flows upwardly through graphite mass.
Rock material and the other impurity being present in graphite are natural insulator, and electric conductivity is good unlike graphite It is good.Therefore, as concentration of carbon increases and rock material concentration reduces, the electric conductivity of graphite crystal also increases, this is because graphite Better than the excellent conductivity of rock material.
Pure graphite is attributed to low-surface-energy and has natural hydrophobicity on fracture plane.Therefore, conventional, mostly The common commercial graphites purification process of number is to pass through flotation.However, although graphite has natural floatability, from such as feldspar, stone English, mica and carbonate gangue mineral separation usually require use chemical interface activating agent and inhibitor, this make processing compared with It is expensive and have an impact to ecology.In addition, graphite is only capable of being purified to by flotation the degree of the carbon no more than 95%, and flotation it Afterwards, some impurity distribution returns in graphite flakes.Other methods of purification of graphite are related to acid leaching and basic roasting, not only Costliness, but also environmental pollution may be caused.
Therefore, the demand that high-grade graphite is produced by energy-efficient and environmentally friendly technology is very big.In recent years, it is selected in graphite It is increasing to the interest of microwave heating in mine.Microwave irradiation has many advantages, because it allows quick and selective add Heat, at the same it is still environmentally friendly.However, the method needs highly complex equipment, thus it is with high costs.Other isolation technics include Gravity Separation, the separation of two liquid and film flotation.Although these technologies quite have foreground, additional numerous studies and phase are needed really When big investment.With the development of graphene, the demand to graphite constantly increases.This fact has been pushed to new graphite ore recently The exploration of bed.Due to these graphite deposits usually it is low than the graphite grade currently produced, strongly need using new method come Graphite products quality is kept, while containing ore-dressing technique cost.
Invention content
Method and apparatus described in the present invention can produce high purity graphite, while keep at low cost and almost to ring Border is without influence.The main difference of the present invention and related art is that any chemicals or excipient is not present.In addition, of the invention The middle sole component used is water, can repeatedly using and reuse, without recycling.Reactor design it is simple Property with the combination of its reduction process temperature also contributed to effectiveness of the invention described herein.
The present invention be directed to for by centrifugal acceleration to be applied to the mixture of graphite flake and water from natural graphite The device and method of piece removal of impurity.
Method described here includes:A) water and the working solution of natural graphite flakes are prepared;B) working solution is set In flow reactor;C) working solution is made to be circulated in the flow reactor;Therefore, cause the solution The follow-up collision of the graphite flake contained in centrifugal flow and the solution;D) via leaching and rinse out rock material with Purification of graphite piece;And e) from the isolated high purity graphite piece of the working solution.
A kind of equipment for purifying natural graphite, including:
Flow reactor;And
At least two impellers.
Method and apparatus described herein can significantly increase the carbon content in natural graphite.It is true by multiple tests It accepts effectiveness of the invention, the test observes that conductivity averagely increases 30% to 40%.
Description of the drawings
This can be more readily understood by the detailed description to various aspects of the present invention carried out below in conjunction with attached drawing These and other feature of invention.
Fig. 1 show for by comprising graphite flake and water mixture apply centrifugal acceleration by from the graphite flake move Deimpurity equipment.
Specific implementation mode
It is the specific implementation mode for being provided to auxiliary those skilled in the art and putting into practice the present invention below.Fields Technical staff can be described herein embodiment in make many modifications and variations, without departing from the present invention spirit Or range.Unless otherwise defined, otherwise all technical and scientific terms used herein have and fields of the present invention The identical meaning of the normally understood meaning of those of ordinary skill.The term used in the description of this invention herein is only used In description specific embodiment, and it is not intended to the limitation present invention.All publication mentioned in this article, patent application, patent, figure and Other bibliography are clearly incorporated in entirety by reference.
The present invention be directed to for by centrifugal acceleration to be applied to the mixture of graphite flake and water from natural graphite The device and method of piece removal of impurity.
The main idea of the method and apparatus proposed is that centrifugal force is applied to the flowing reactive being placed in equipped with rotary blade The mixture of water and graphite flake in device.In the case where being moved with higher linear velocity, graphite flake is impinging one another;Therefore, make Rock material is obtained from graphite flake leaching to go out.In addition, the centrifugal acceleration of high speed causes graphite flake to be vortexed in the reactor, to Lead to the friction level higher of graphite-water, and then enhances removal of the rock material from graphite flake.
With reference to figure 1, rotary blade 1 and 4, which generates, is applied to the centrifugal acceleration of working solution, working solution or substantially exist It is collided at the point of impingement 2.Internal diameter of the diameter of impeller 1 and 4 generally similar to reactor 3;In this way, providing no more than between 0.8mm Gap.
In an exemplary embodiment, by mixing 15kg in 100L water and there is the natural graphite of 98% carbon content Preparation work solution.Then make the working solution with the speed of about 20 meter per seconds at a temperature in the range of in 40 to 50 DEG C Pass through flow reactor.Aforementioned processing persistently carries out about 15 minutes, hereafter, working solution is divided into two using general purpose centrifuge Point:Relatively small portion and relatively most of.Once complete solution of processing, i.e., be dehydrated the watery slurry of gained, and from The pulp separation obtains the graphite flake with high-carbon content (up to 99.8%).Compared with original graphite, gained graphite is led Electrically increase 30% to 35%.
In other exemplary embodiments, working solution can be made of 100 parts of water and 10 to 20 parts of graphite, and be applied high Up to the linear velocity of the centrifugal acceleration and up to 40 meter per seconds of 20g, reach the speed within the scope of 30 to 50 meter per seconds.
In other exemplary embodiments, aforementioned processing is in the pressure of 5 to 15 bars (bar) and within the scope of 40 to 65 DEG C At a temperature of carry out.
Based on foregoing teachings, the present invention provides ecologically clean and cheap graphite purification method, the carbon content of the graphite Up to 99.8% and have high conductivity and thermal conductivity.A kind of component, i.e. water is used only in method and apparatus described herein, It can be reused repeatedly without recycling.Further, since the present invention does not need a large amount of energy, complicated dress is not needed yet It is standby, therefore it can be implemented in the place near graphite mineral reserve, which in turn reduces transportation cost and overall manufacturing cost.
The description of the embodiment of the present invention is presented for purposes of illustration, but it does not mean that all or limits the invention to Disclosed form.It will be apparent to those skilled in the art that many modifications and variations are made on ground.
Those skilled in the art will understand that element depicted herein can change depending on embodiment. Discribed example is not meant to imply the framework limitation for the present invention.
Above or in the dependent claims, term " comprising " is synonymous with "comprising".Such as " X includes A, B and C " The use of term is not intended to imply that A, B and C must be only component or the most important components of X.
Unless understanding and clearly stating, otherwise the appended claims are not intended to imply that any specific action sequence.Power If the stem portion of sharp claim include such as a), b), c) or 1), 2), 3) label itself do not imply that any particular order, and Actually it is intended only to facilitate the reference to the part.
Reaffirm, it is the principle of the present invention, practical application, and so that institute in order to most preferably explain to select and describe all embodiments The those of ordinary skill in category field is it will be appreciated that the present invention.Various other embodiments with various modifications may be suitable for being contained The specific use of lid, is also within the scope of the present invention.

Claims (2)

1. a kind of method of purifying natural graphite, which is characterized in that including:
Solution is prepared by mixing multiple natural graphite particles in water;
The solution is placed in the flow reactor equipped at least two impellers;
So that the solution circulates in the flow reactor by rotating the impeller;And
The separating obtained high purity graphite particle from the solution.
2. a kind of equipment for purifying natural graphite, which is characterized in that including:
Flow reactor;And
At least two impellers.
CN201711071753.1A 2017-03-28 2017-11-03 Liquid-based method and apparatus for graphite purification Pending CN108654828A (en)

Applications Claiming Priority (2)

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US201762477742P 2017-03-28 2017-03-28
US62/477,742 2017-03-28

Publications (1)

Publication Number Publication Date
CN108654828A true CN108654828A (en) 2018-10-16

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WO (1) WO2018183521A1 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2615349B (en) * 2022-02-07 2024-02-07 Graphene Star Ltd Improvements in or relating to graphite processing

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1112357A (en) * 1993-08-03 1995-11-22 印德莱斯科股份有限公司 Beneficiation of flake graphite
CN1557704A (en) * 2004-01-21 2004-12-29 敏 岳 Method for purifying natural crystalline flake graphite of high purity
US20060062716A1 (en) * 2002-03-01 2006-03-23 Hydro-Quebec Method for the surface purification of a graphite containing impurities using a dilute aqueous solution of nh4f and h2so4
CN103213972A (en) * 2013-03-22 2013-07-24 中国科学院山西煤炭化学研究所 Method for rapid continuous separation and purification of graphite oxide
CN103221338A (en) * 2010-09-21 2013-07-24 高温物理有限责任公司 Process for the production of carbon graphenes and other nanomaterials
CN205495102U (en) * 2016-04-13 2016-08-24 深圳粤网节能技术服务有限公司 Purification device and graphite alkene production system

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2787528A (en) * 1953-09-18 1957-04-02 Southwestern Graphite Company Process for purifying graphite
US5560892A (en) * 1994-09-26 1996-10-01 Indresco Inc. Apparatus system for beneficiation of kish graphite
US7168641B2 (en) * 2004-08-31 2007-01-30 Spx Corporation Attrition scrubber apparatus and method
CN101367517B (en) * 2008-09-24 2011-08-10 青岛恒胜石墨有限公司 Method for preparing high pure graphite with steam heating

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1112357A (en) * 1993-08-03 1995-11-22 印德莱斯科股份有限公司 Beneficiation of flake graphite
US20060062716A1 (en) * 2002-03-01 2006-03-23 Hydro-Quebec Method for the surface purification of a graphite containing impurities using a dilute aqueous solution of nh4f and h2so4
CN1557704A (en) * 2004-01-21 2004-12-29 敏 岳 Method for purifying natural crystalline flake graphite of high purity
CN103221338A (en) * 2010-09-21 2013-07-24 高温物理有限责任公司 Process for the production of carbon graphenes and other nanomaterials
CN103213972A (en) * 2013-03-22 2013-07-24 中国科学院山西煤炭化学研究所 Method for rapid continuous separation and purification of graphite oxide
CN205495102U (en) * 2016-04-13 2016-08-24 深圳粤网节能技术服务有限公司 Purification device and graphite alkene production system

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