CN104495810B - Prepare the green method of Graphene on a large scale - Google Patents

Prepare the green method of Graphene on a large scale Download PDF

Info

Publication number
CN104495810B
CN104495810B CN201410756521.XA CN201410756521A CN104495810B CN 104495810 B CN104495810 B CN 104495810B CN 201410756521 A CN201410756521 A CN 201410756521A CN 104495810 B CN104495810 B CN 104495810B
Authority
CN
China
Prior art keywords
organic substance
graphene
graphite
water soluble
soluble organic
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.)
Active
Application number
CN201410756521.XA
Other languages
Chinese (zh)
Other versions
CN104495810A (en
Inventor
陈国华
林少芬
赵立平
洪江彬
黄卫明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
XIAMEN KNANO GRAPHENE TECHNOLOGY Corp Ltd
Huaqiao University
Original Assignee
XIAMEN KNANO GRAPHENE TECHNOLOGY Corp Ltd
Huaqiao University
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 XIAMEN KNANO GRAPHENE TECHNOLOGY Corp Ltd, Huaqiao University filed Critical XIAMEN KNANO GRAPHENE TECHNOLOGY Corp Ltd
Priority to CN201410756521.XA priority Critical patent/CN104495810B/en
Publication of CN104495810A publication Critical patent/CN104495810A/en
Application granted granted Critical
Publication of CN104495810B publication Critical patent/CN104495810B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The present invention provides a kind of green method preparing Graphene on a large scale, it utilizes water soluble organic substance melt to assist three roller strippings to prepare Graphene, specifically includes following steps: (1) weighs water soluble organic substance that mass ratio is 5:1~500:1 and graphite is standby;(2) water soluble organic substance is positioned on three-roll grinder roller, the softening point of heating roller to water soluble organic substance, prepares adhesive, run three-roll grinder, treat that adhesive is laid on the roller of three-roll grinder, be slow added into graphite, be ground peeling off to the graphite added;(3) product that step (2) obtains is immersed in distilled water, washing, to remove water soluble organic substance, i.e. obtains Graphene.The present invention uses physical method to prepare Graphene, preparation technology environmental protection, nontoxic, can apply to the biomedical sector of ground floor safety, and the method has simple, for equipment without particular/special requirement, low cost, efficiency is high, can carry out the advantages such as large-scale production.

Description

Prepare the green method of Graphene on a large scale
Technical field
The present invention relates to technical field of graphene, particularly relate to one and prepare Graphene on a large scale Green method.
Background technology
Graphene as a kind of novel Two-dimensional Carbon material, has the architectural feature of uniqueness and excellent Different electricity, mechanics, optics and thermal property, nano electron device, energy storage material, The fields such as catalysis, sensor, pharmaceutical carrier and functional material have a wide range of applications Prospect.Research shows, Graphene is at biomedical sector, including targeted drug conveying, cell The aspects such as imaging, biological detection, oncotherapy have huge application prospect.But, graphite Alkene also needs to consider biological effect and safety in the application of biomedical sector.If preparation technology Environmental protection, nontoxic, its application of biomedical sector ground floor safety just To ensure that, Graphene and living things system interaction mechanism only need to be considered.
Currently, the preparation method of Graphene mainly has electronation graphene oxide method, chemistry gas As the sedimentation method, crystal epitaxy method, mechanical stripping method etc..Wherein electronation graphite oxide Alkene method is fully to be peeled off in water by graphite oxide, then it is carried out electronation or heat Reduction obtains Graphene, and the method is considered as that one most possibly realizes Graphene industrialization system For obtaining important method.But due to the process through Strong oxdiative-reduction, the electricity of graphene sheet layer Sub-conjugated structure is destroyed, and reduces its physical and chemical performance.And in the oxidizing process of graphite Need high-temperature process, or use the chemical substance that hydrazine hydrate, sodium borohydride etc. are poisonous, not only Power consumption is big, efficiency is low, cost is high, and pollutes environment.
The chemical vapor sedimentation method mainly utilize gaseous carbon source at high temperature to decompose after at matrix surface On catalytic growth prepare Graphene, the method is to prepare high-quality and large area monolayer stone The important method of ink alkene.But its working condition is the harshest, power consumption is big, and cost is high.
Silicon carbide epitaxial growth method is by heating monocrystalline silicon carbide, under the high temperature conditions, by table The Si in face etches away so that carbon atom separates out and reconfigures formation Graphene, prepared by the method The Graphene mass ratio gone out is higher.But its Graphene obtained is the mixed of monolayer and multilamellar mostly Compound, and there is stronger effect with matrix and be difficult to transfer so that the method is difficult to scale Produce.
Mechanical stripping method is by the limellar stripping of Graphene by certain mechanical force, thus prepares The less Graphene of defect.The mechanical stripping method occurred at present mainly has following 4 kinds:
(1) " tear tape " method: Gao Ding peels off the most repeatedly by adhesive tape in Geim seminar To pyrolytic graphite, then the sample obtained is transferred on silicon chip, finally fall glue with acetone solution Band, is prepared into single-layer graphene first.But the method productivity is low, it is difficult to realize extensive system Standby.
(2) liquid phase stripping method: i.e. under liquid-phase system directly by ultrasonic or ball milling to graphite Lamella is peeled off.Coleman seminar in METHYLPYRROLIDONE solvent or Add and graphite is carried out the most ultrasonic by the aqueous solution of surfactant, prepare monolayer With minority layer graphene.Chen Guohua seminar utilizes wet ball grinding to be 30 45 in surface tension The organic solvent of mNm-1 carries out ball milling to graphite powder and prepares Graphene.But ultrasonic and ball The solvent and the surfactant that use in mill method are difficult to thoroughly remove, and not only affect Graphene Actual application, and the cost removing organic solvent and surfactant is high.
(3) three roller methods: Chen Guohua seminar utilizes industrial common processing technique three roller to peel off Method, prepares adhesive by macromolecule dissolution in organic solvent, by three-roller tool power and grinding thereof Dispersion effect, uses for reference the original preparation method " adhesive tape method " of Graphene, is peeled off layer by layer by graphite Prepare Graphene.Concrete operations for PVC is dissolved in o-phthalic acid dibutyl ester, magnetic force Adhesive is prepared, by macromolecular adhesive and graphite flake after 250 DEG C of heated and stirred 30min of constant temperature Adding from the charging aperture of three-roller tool successively, the not stall along with three rollers is moved, and will constantly peel off Graphite flake, is finally prepared into that defect is few, monolayer and the Graphene of minority layer.But owing to obtaining Graphene need to utilize a large amount of organic solvent such as acetone, oxolane, Ketohexamethylene etc. or high Temperature adds heat abstraction macromolecular adhesive, and cost is high and pollutes environment, limits it big in industrialization Large-scale production is applied.
(4) solid particle Aided Machine stripping method: Wang Lidong, Fei Weidong [Wang Lidong, Fei Wei , high-efficiency and low-cost mechanical stripping prepares the method [P] of Graphene or graphene oxide, in State's patent: CN101817516A, 2010-09-01] invent high-efficiency and low-cost mechanical stripping The method preparing Graphene or graphene oxide, the party's bright use automation, with the most small Solid particle up-stripping process, by solid particle to the shearing of carbon materials and clash into make With, increase the contact area in stripping process and peel off number of times.But the preparation that this invention provides Method work system is complicated, can use organic solvent etc., pollutes environment, limits it in industry On large-scale production.
Therefore, a kind of simple in the urgent need to exploitation, low cost, productivity be high, pollution-free, The environmental protection novel preparation method easily promoted the use of.
Summary of the invention
The invention aims to solve high cost present in existing graphene preparation technology, Inefficient, pollution environment, it is impossible to the problem that industrial scale produces, it is provided that a kind of extensive Prepare the green method of Graphene.
To achieve these goals, the present invention adopts the following technical scheme that
Prepare the green method of Graphene on a large scale, comprise the following steps:
(1) it is 5:1~500:1 according to the mass ratio of water soluble organic substance Yu graphite, weighs water-soluble Property Organic substance and graphite are standby;This water soluble organic substance, for reaching its softening point when temperature, to obtain final product To the water soluble organic substance melt with gumminess;
(2) water soluble organic substance is positioned on three-roll grinder roller, heats three-roll grinder Roller, the softening point of water soluble organic substance to be achieved, prepare and have as the water solublity of adhesive Machine thing melt, bring into operation three-roll grinder, treats that water soluble organic substance melt is laid in three rollers and grinds On the roller of grinding machine, being slow added into graphite, three-roll grinder continues to run with the graphite added It is ground peeling off, obtains Graphene and water soluble organic substance melt blend;
(3) Graphene step (2) obtained and water soluble organic substance melt blend submergence In distilled water, wash 3-5 time, to remove water soluble organic substance, i.e. obtain Graphene.
Described water soluble organic substance use the one in water solublity monosaccharide, disaccharide, oligosaccharide or Multiple mixture, any two kinds and mixed above time be any proportioning.
Described water solublity monosaccharide use glucose, fructose, galactose, sorbose, Tagatose, Inositol or mannose;Described water solublity disaccharide uses sucrose, lactose or maltose;Described Water soluble oligosaccharide uses cottonseed sugar, xylose, trehalose, stachyose, cyclodextrin, Fructus Hordei Germinatus Oligosaccharide, fructose oligosaccharides or soybean oligo saccharide.
Described graphite is in native graphite, expanded graphite, highly oriented graphite and thermal cracking graphite The mixture of one or more, any two kinds and mixed above time be any proportioning.
In described step (2), the time of three-roll grinder stripping graphite is 0.5~72h.
Compared with prior art, present invention have an advantage that
(1) present invention is to utilize water soluble organic substance melt auxiliary three-roll grinder to peel off graphite, Obtain Graphene and water soluble organic substance melt blend, then remove water solublity with distilled water wash Organic substance melt, thus obtain Graphene.The present invention is using water soluble organic substance melt as gluing Agent, imitate " tear tape " method prepare Graphene, improve Chen Guohua seminar by PVC It is dissolved in o-phthalic acid dibutyl ester, prepares after 250 DEG C of heated and stirred 30min of magnetic force constant temperature Adhesive, then adds from the charging aperture of three-roller tool successively by macromolecular adhesive and graphite flake Enter, utilize three rollers to peel off graphite, finally remove height with organic solvent such as acetone or high-temperature heating The preparation method of molecule adhesive.There is low cost, and environmental protection, industrialization can be carried out Large-scale production.And whole preparation technology environmental protection, nontoxic, it is determined that it is being given birth to The ground floor safety of thing field of medical applications.
(2) Wang Lidong, the high-efficiency and low-cost mechanical stripping of expense dimension invention prepare Graphene Or the method for graphene oxide [Wang Lidong, Fei Weidong, prepared by high-efficiency and low-cost mechanical stripping The method [P] of Graphene or graphene oxide, Chinese patent: CN101817516A, 2010-09-01], the party's bright use automation, with the most small solid particle up-stripping Process, by solid particle to the shearing of carbon materials and effect of impact, increases in stripping process Contact area and peel off number of times, relative to this invention, the principle of the present invention be utilize with water-soluble Property Organic substance melt as adhesive, use for reference " adhesive tape method " and prepare Graphene, rather than with greatly Amount minute solid particles carries out mechanical stripping as auxiliary.Have simple for process, there is ring Border friendly, easily promotes the use of, it is adaptable to industrial scale produces.
Detailed description of the invention
In order to be better understood from the present invention, it is further elucidated with in the present invention below in conjunction with embodiment Hold, but present disclosure is not limited solely to below example.
Embodiment 1:
Prepare the green method of Graphene on a large scale, comprise the steps:
(1) quality of expanded graphite 4g, glucose 20g, glucose and expanded graphite is weighed Ratio is 5:1;
(2) glucose is positioned on three-roll grinder roller, the roller of heating three-roll grinder Cylinder, the softening point of glucose to be achieved 130 DEG C, prepare the glucose melt as adhesive, Bring into operation three-roll grinder, treats that glucose melt is laid on the roller of three-roll grinder, then Being slowly added to expanded graphite, the expanded graphite that three-roll grinder continues to run with adding is ground Peel off 30min, obtain Graphene and glucose melt blend;
(3) Graphene and glucose melt blend step (2) obtained is immersed in distillation In water, first with after 100 DEG C of distilled water washs 3 times, then wash 2 times with normal-temperature distilled water, remove Remove adhesive glucose melt, vacuum filtration, finally the product after sucking filtration is done in electric heating air blast In dry case, 100 DEG C of dry 12h, obtain Graphene.
Embodiment 2:
Prepare the green method of Graphene on a large scale, comprise the steps:
(1) matter of native graphite 4g, maltose 200g, maltose and native graphite is weighed Amount ratio is 50:1;
(2) maltose is positioned on three-roll grinder roller, the roller of heating three-roll grinder Cylinder, the softening point of maltose to be achieved 95 DEG C, prepare the maltose melt as adhesive, Bring into operation three-roll grinder, treats that maltose melt is laid on the roller of three-roll grinder, then Being slowly added to native graphite, the native graphite that three-roll grinder continues to run with adding is ground Peel off 2h, obtain Graphene and maltose melt blend;
(3) Graphene and maltose melt blend step (2) obtained is immersed in distillation In water, first with after 100 DEG C of distilled water washs 3 times, then wash 2 times with normal-temperature distilled water, remove Remove adhesive maltose melt, vacuum filtration, finally the product after sucking filtration is done in electric heating air blast In dry case, 100 DEG C of dry 12h, obtain Graphene.
Embodiment 3:
Prepare the green method of Graphene on a large scale, comprise the steps:
(1) thermal cracking graphite 2g, cottonseed sugar 500g, cottonseed sugar and thermal cracking graphite are weighed Mass ratio be 250:1;
(2) cottonseed sugar is positioned on three-roll grinder roller, the roller of heating three-roll grinder Cylinder, the softening point of cottonseed sugar to be achieved 65 DEG C, prepare the cottonseed sugar melt as adhesive, Bring into operation three-roll grinder, treats that cottonseed sugar melt is laid on the roller of three-roll grinder, then Being slowly added to thermal cracking graphite, the thermal cracking graphite that three-roll grinder continues to run with adding is carried out Grind and peel off 24h, obtain Graphene and cottonseed sugar melt blend;
(3) Graphene and cottonseed sugar melt blend step (2) obtained is immersed in distillation In water, first with after 100 DEG C of distilled water washs 3 times, then wash 2 times with normal-temperature distilled water, remove Remove adhesive cottonseed sugar melt, vacuum filtration, finally the product after sucking filtration is done in electric heating air blast In dry case, 100 DEG C of dry 12h, obtain Graphene.
Embodiment 4:
Prepare the green method of Graphene on a large scale, comprise the steps:
(1) highly oriented graphite 3g is weighed, sucrose 90g, sucrose and the matter of highly oriented graphite Amount ratio is 30:1;
(2) sucrose is positioned on three-roll grinder roller, the roller of heating three-roll grinder, The softening point of sucrose to be achieved 165 DEG C, prepares the sucrose melt as adhesive, brings into operation Three-roll grinder, treats that sucrose melt is laid on the roller of three-roll grinder, is slow added into height Orientation graphite, three-roll grinder continues to run with and is ground peeling off to the highly oriented graphite added 48h, obtains Graphene and sucrose melt blend;
(3) Graphene and sucrose melt blend step (2) obtained is immersed in distilled water In, first with after 100 DEG C of distilled water washs 3 times, then wash 2 times with normal-temperature distilled water, remove Adhesive sucrose melt, vacuum filtration, finally by the product after sucking filtration at electric drying oven with forced convection In 100 DEG C of dry 12h, obtain Graphene.
Embodiment 5:
Prepare the green method of Graphene on a large scale, comprise the steps:
(1) expanded graphite 2g, native graphite 1g, xylose 1200g, xylose and stone are weighed The mass ratio of ink is 400:1;
(2) xylose is positioned on three-roll grinder roller, the roller of heating three-roll grinder, The softening point of xylose to be achieved 75 DEG C, prepares the xylose melt as adhesive, brings into operation Three-roll grinder, treats that xylose melt is laid on the roller of three-roll grinder, is slow added into swollen Swollen graphite and native graphite, three-roll grinder continues to run with the expanded graphite added and natural stone Ink is ground peeling off 60h, obtains Graphene and xylose melt blend;
(3) Graphene and xylose melt blend step (2) obtained is immersed in distilled water In, first with after 100 DEG C of distilled water washs 3 times, then wash 2 times with normal-temperature distilled water, remove Adhesive xylose melt, vacuum filtration, finally by the product after sucking filtration at electric drying oven with forced convection In 100 DEG C of dry 12h, obtain Graphene.
Embodiment 6:
Prepare the green method of Graphene on a large scale, comprise the steps:
(1) thermal cracking graphite 2g, fructose 1000g, fructose and thermal cracking graphite are weighed Mass ratio is 500:1;
(2) fructose is positioned on three-roll grinder roller, the roller of heating three-roll grinder, The softening point of fructose to be achieved 80 DEG C, prepares the fructose melt as adhesive, brings into operation Three-roll grinder, treats that fructose melt is laid on the roller of three-roll grinder, is slow added into heat Cracking graphite, three-roll grinder continues to run with and is ground peeling off to the thermal cracking graphite added 72h, obtains Graphene and fructose melt blend;
(3) Graphene and fructose melt blend step (2) obtained is immersed in distilled water In, first with after 100 DEG C of distilled water washs 3 times, then wash 2 times with normal-temperature distilled water, remove Adhesive fructose melt, vacuum filtration, finally by the product after sucking filtration at electric drying oven with forced convection In 100 DEG C of dry 12h, obtain Graphene.
Embodiment 7:
Prepare the green method of Graphene on a large scale, comprise the steps:
(1) matter of expanded graphite 2g, galactose 400g, galactose and expanded graphite is weighed Amount ratio is 200:1;
(2) galactose is positioned on three-roll grinder roller, the roller of heating three-roll grinder Cylinder, the softening point of galactose to be achieved 140 DEG C, prepare the galactose melt as adhesive, Bring into operation three-roll grinder, treats that galactose melt is laid on the roller of three-roll grinder, then Being slowly added to expanded graphite, the expanded graphite that three-roll grinder continues to run with adding is ground Peel off 8h, obtain Graphene and galactose melt blend;
(3) Graphene and galactose melt blend step (2) obtained is immersed in distillation In water, first with after 100 DEG C of distilled water washs 3 times, then wash 2 times with normal-temperature distilled water, remove Remove adhesive galactose melt, vacuum filtration, finally the product after sucking filtration is done in electric heating air blast In dry case, 100 DEG C of dry 12h, obtain Graphene.
Embodiment 8:
Prepare the green method of Graphene on a large scale, comprise the steps:
(1) expanded graphite 4g, glucose 25g, maltose 25g, sucrose 30g are weighed, Organic substance is 20:1 with the mass ratio of graphite;
(2) glucose, maltose and sucrose are positioned on three-roll grinder roller, heating The roller of three-roll grinder, the softening point of sucrose to be achieved 165 DEG C, prepare as adhesive By the mixing Organic substance melt of glucose melt, maltose melt and sucrose melt mixed, Bring into operation three-roll grinder, treats that this mixing Organic substance melt is laid in the roller of three-roll grinder On, it being slow added into expanded graphite, the expanded graphite that three-roll grinder continues to run with adding enters Row grinds peels off 30h, obtains Graphene and mixing Organic substance melt blend;
(3) Graphene step (2) obtained and mixing Organic substance melt blend are immersed in In distilled water, first with after 100 DEG C of distilled water washs 3 times, then wash 2 times with normal-temperature distilled water, Removing adhesive mixing Organic substance melt, vacuum filtration, finally by the product after sucking filtration at electric heating In air dry oven, 100 DEG C of dry 12h, obtain Graphene.
Embodiment 9:
Prepare the green method of Graphene on a large scale, comprise the steps:
(1) expanded graphite 2.5g, thermal cracking graphite 2.5g, sucrose 25g, fructose are weighed 25g, Organic substance is 10:1 with the mass ratio of graphite;
(2) sucrose and fructose are positioned on three-roll grinder roller, heat three-roll grinder Roller, the softening point of sucrose to be achieved 165 DEG C, prepare as adhesive by sucrose melt With the mixing Organic substance melt of fructose melt mixed, bring into operation three-roll grinder, treats this Mixing Organic substance melt be laid on the roller of three-roll grinder, be slow added into expanded graphite and Thermal cracking graphite, three-roll grinder continues to run with and enters the expanded graphite added and thermal cracking graphite Row grinds peels off 4h, obtains Graphene and mixing Organic substance melt blend;
(3) Graphene step (2) obtained and mixing Organic substance melt blend are immersed in In distilled water, first with after 100 DEG C of distilled water washs 3 times, then wash 2 times with normal-temperature distilled water, Removing adhesive mixing Organic substance melt, vacuum filtration, finally by the product after sucking filtration at electric heating In air dry oven, 100 DEG C of dry 12h, obtain Graphene.
In the present invention, it is by as follows that water soluble organic substance is heated into water soluble organic substance melt Mode realizes: between adjusting in the usual way before, during and after three-roll grinder between roller Gap, then part aqueous Organic substance is respectively placed on three rollers, heating roller makes water-soluble Property Organic substance is melted into the melt with gumminess, more remaining water soluble organic substance is poured on tool Having on the melt of gumminess, water soluble organic substance is stuck, and will not drop to outside roller, continues Heating makes whole water soluble organic substances all be melted into the melt with gumminess.

Claims (4)

  1. Prepare the green method of Graphene the most on a large scale, it is characterised in that comprise the following steps:
    (1) it is 5:1~500:1 according to the mass ratio of water soluble organic substance Yu graphite, weighs water-soluble Property Organic substance and graphite are standby;This water soluble organic substance reaches its softening point when temperature, i.e. obtains There is the water soluble organic substance melt of gumminess;
    (2) water soluble organic substance is positioned on three-roll grinder roller, heats three-roll grinder Roller, the softening point of water soluble organic substance to be achieved, prepare and have as the water solublity of adhesive Machine thing melt, bring into operation three-roll grinder, treats that water soluble organic substance melt is laid in three rollers and grinds On the roller of grinding machine, being slow added into graphite, three-roll grinder continues to run with the graphite added It is ground peeling off, obtains Graphene and water soluble organic substance melt blend;
    (3) Graphene step (2) obtained and water soluble organic substance melt blend submergence In distilled water, wash 3-5 time, to remove water soluble organic substance, i.e. obtain Graphene;
    Described water soluble organic substance uses one or more in water solublity monosaccharide, oligosaccharide Mixture, any two kinds and mixed above time be any proportioning.
  2. The green method preparing Graphene on a large scale the most according to claim 1, it is special Levying and be, described water solublity monosaccharide uses glucose, fructose, galactose, sorbose, tower Lattice sugar, inositol or mannose;Described water soluble oligosaccharide use sucrose, lactose, cottonseed sugar, Trehalose, stachyose, cyclodextrin, Fructus Hordei Germinatus oligose, fructose oligosaccharides or soybean oligo saccharide.
  3. The green method preparing Graphene on a large scale the most according to claim 1, it is special Levying and be, described graphite is native graphite, expanded graphite, highly oriented graphite and thermal cracking stone The mixture of one or more in ink, any two kinds and mixed above time be any proportioning.
  4. The green method preparing Graphene on a large scale the most according to claim 1, it is special Levying and be, in described step (2), the time of three-roll grinder stripping graphite is 0.5~72h.
CN201410756521.XA 2014-12-10 2014-12-10 Prepare the green method of Graphene on a large scale Active CN104495810B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410756521.XA CN104495810B (en) 2014-12-10 2014-12-10 Prepare the green method of Graphene on a large scale

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410756521.XA CN104495810B (en) 2014-12-10 2014-12-10 Prepare the green method of Graphene on a large scale

Publications (2)

Publication Number Publication Date
CN104495810A CN104495810A (en) 2015-04-08
CN104495810B true CN104495810B (en) 2016-10-05

Family

ID=52937291

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410756521.XA Active CN104495810B (en) 2014-12-10 2014-12-10 Prepare the green method of Graphene on a large scale

Country Status (1)

Country Link
CN (1) CN104495810B (en)

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106554010A (en) 2015-09-25 2017-04-05 苏州烯时代石墨烯科技有限公司 The method of preparation of industrialization big size graphene
CN106365156B (en) * 2016-08-28 2018-07-06 桂林新艺制冷设备有限责任公司 A kind of method for preparing graphene
CN107055519A (en) * 2016-12-28 2017-08-18 成都新柯力化工科技有限公司 A kind of method peeled off and prepare graphene microchip that rubbed using three-roll grinder in the same direction
CN106564884A (en) * 2017-01-19 2017-04-19 成都新柯力化工科技有限公司 Method for preparing graphene through mechanical stretching
CN108328603B (en) * 2017-01-20 2021-10-12 清华大学 Method for transferring sugar-based nanomaterials
CN107140628B (en) * 2017-07-03 2020-02-14 北京旭碳新材料科技有限公司 Modified graphene slurry and preparation method thereof
CN108163847B (en) * 2018-01-12 2020-04-17 昂星新型碳材料常州有限公司 Preparation method of large-sheet-diameter graphene and large-sheet-diameter graphene
CN108675288A (en) * 2018-07-25 2018-10-19 恒力(厦门)石墨烯科技产业集团有限公司 A kind of method that Mechanical Method prepares high purity graphite alkene microplate
CN109019577A (en) * 2018-09-29 2018-12-18 深圳市通产丽星股份有限公司 A kind of graphene and preparation method thereof
CN108996495A (en) * 2018-09-29 2018-12-14 深圳市通产丽星股份有限公司 A kind of nano-graphene microplate and preparation method thereof
CN110143586B (en) * 2019-03-26 2021-04-02 中科悦达(上海)材料科技有限公司 Preparation method of single-layer or few-layer graphene
CN110040727B (en) * 2019-05-15 2022-07-29 华侨大学 Continuous stripping preparation method of graphene sheet
CN111847433A (en) * 2020-06-29 2020-10-30 深圳石墨烯创新中心有限公司 Method for preparing graphene by using three-roller grinding machine
CN115611271B (en) * 2022-10-28 2024-02-23 中国科学院福建物质结构研究所 Preparation method of graphene

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101817516A (en) * 2010-05-21 2010-09-01 哈尔滨工业大学 Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101817516A (en) * 2010-05-21 2010-09-01 哈尔滨工业大学 Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Continuous mechanical exfoliation of graphene sheets via three-roll mill;jinfeng Chen et al.;《Journal of Materials Chemistry》;20120803;第22卷;第19625-19628页 *

Also Published As

Publication number Publication date
CN104495810A (en) 2015-04-08

Similar Documents

Publication Publication Date Title
CN104495810B (en) Prepare the green method of Graphene on a large scale
CN104772064B (en) Method for preparing grapheme dispersion liquid
CN105253878B (en) A kind of method that expanded graphite or graphene are directly prepared under normal temperature and pressure
CN105217612B (en) A kind of ultrasonic assistant sand mill stripping prepares the method for graphene and peels off the device of graphene processed
US10472243B2 (en) Industrial method for preparing large-sized graphene
CN103435705B (en) Method for preparing starch nanocrystal
CN110143586A (en) A kind of preparation method of the graphene of single layer or few layer
CN108163894B (en) Ultrahigh-concentration stripping method for transition metal sulfide
CN103979505B (en) A kind of preparation method of minority layer bismuth selenide nanometer sheet
CN107792848A (en) The method that synchronizing ultrasound chemistry prepares functionalization graphene with mechanochemical reaction
CN113077921B (en) Biological micro-fluidic chip 3D printing electrode material, 3D printing electrode and preparation method thereof
CN106564885B (en) A kind of continuous fluidic device and its method for preparing graphene
CN108163847B (en) Preparation method of large-sheet-diameter graphene and large-sheet-diameter graphene
CN103553030A (en) Preparation method of few-layer graphene
CN105645366A (en) Liquid-phase stripping preparation method of single-layer or few-layer phosphaalkene
CN104878197B (en) Ultrasonic-assisted method for leaching potassium at low temperature under normal pressure
CN103626162A (en) Preparation method of graphene
CN113416334B (en) Hydroxyethyl cellulose/boron nitride nano composite film and preparation method thereof
CN105776193A (en) Method for preparing graphene nanoplatelets with pulsed high pressure water jet mill
CN104891485A (en) Method for preparing nano graphite sheet
CN106672951A (en) Environment-friendly, high-efficiency and large-scale graphene preparation method
CN105776190A (en) Method for preparing graphene micro-sheets through foaming expansion and stretching of screw machine
CN103738949A (en) Preparation method for single-layer graphene isopropanol solution
CN106986960A (en) It is a kind of to prepare graphene three-dimensional construction method of the powder body material containing carbon polymer
CN214829040U (en) Three-dimensional graphite alkene industrial production device

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
CB02 Change of applicant information

Address after: Fengze District of Quanzhou city of Fujian Province east of Huaqiao University, 362000

Applicant after: Huaqiao University

Applicant after: XIAMEN KNANO GRAPHENE TECHNOLOGY CORPORATION LIMITED

Address before: Fengze District of Quanzhou city of Fujian Province east of Huaqiao University, 362000

Applicant before: Huaqiao University

Applicant before: Xiamen Knano Graphene Technology Corporation Limited

COR Change of bibliographic data
C14 Grant of patent or utility model
GR01 Patent grant