CN104891485A - Method for preparing nano graphite sheet - Google Patents
Method for preparing nano graphite sheet Download PDFInfo
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- CN104891485A CN104891485A CN201510307618.7A CN201510307618A CN104891485A CN 104891485 A CN104891485 A CN 104891485A CN 201510307618 A CN201510307618 A CN 201510307618A CN 104891485 A CN104891485 A CN 104891485A
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Abstract
The invention relates to a method for preparing a nano graphite sheet, which is prepared by taking expanded graphite powder as a raw material, adding the expanded graphite powder in a dispersive solution according to the ratio of 0.5-10g/L, circularly adding the mixed solution into an ultrasonic pulverizer through a centrifuge pump, starting the ultrasonic pulverizer for carrying out ultrasonic peeling nano-crystallization operation on the mixed solution for 40-72h to obtain a nano graphite sheet solution, wherein the dispersive solution is an ethanol solution, and the nano graphite sheet solution obtained through ultrasonic peeling nano-crystallization operation is subjected to standing, filtering and drying to obtain the nano graphite sheet powder with the thickness of 20-50nm. The method disclosed by the invention is simple in preparation process, free of complex equipment, capable of continuous operation, high in production efficiency, and applicable to industrialized continuous production in a large scale.
Description
Technical field
The present invention relates to a kind of preparation technology of graphite material, specifically a kind of preparation method of nano graphite flakes.
Background technology
Nano graphite flakes is formed by monolayer carbon atomic plane structure graphite alkene stacking, and thickness is the bidimensional nano-graphite material of nanoscale.Due between graphite flake layer be by faint Van der Waals force combine, so its limellar stripping can be obtained nano-graphite material.Nano graphite flakes not only has high erosion resistance and chemical stability, also has good conduction and thermal conductivity.
The preparation method of nano graphite flakes is more, and conventional physical method is mechanical attrition method and ultrasonic grinding method.Mechanical attrition method be utilize graphite layers reactive force to be less than the bonding force of graphite linings carbon atom and the principle be easily stripped to prepare nano graphite flakes.Such as, CN104505512A discloses a kind of method that ball milling prepares micro crystal graphite alkene, and its preparation time grows (80-120 hour) and the abrading-ball loss of ball milling use is higher.
Ultrasonic grinding method produces under utilizing ultrasonication to suppress the field of force, is liquid generation cavitation, fragmentation or explosion, thus expanded graphite interlayer is come off, thus obtain nano graphite flakes.CN203794630U discloses a kind of continuous prodution graphene powder full scale plant, and it adopts ultrasonic disintegrator and microwave oven combined utilization to prepare Graphene, and the equipment requirements of needs is higher, needs to be equipped with microwave device, spray drying unit etc.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art, and provide a kind of technique simple, reasonable, processing ease, preparation efficiency is high, is applicable to industrialization, the mass-produced nano-graphite piece preparation method of serialization.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of nano-graphite piece preparation method, and it, is characterized in that for raw material with expanded graphite powder: first add in dispersion solvent by expanded graphite powder, composition mixed solution; Then by impeller pump, mixed solution circulation is joined in ultrasonic grinder; Start ultrasonic grinder and ultrasonic stripping comminution process is carried out 40 minutes to 72 hours to mixed solution, obtain nano graphite flakes solution.
Described dispersion solvent is spirituous solution, the interpolation concentration range 0.5 ~ 10g/L of expanded graphite powder in this dispersion solvent, ultrasonic stripping comminution process obtains nano graphite flakes spirituous solution, after described nano graphite flakes spirituous solution leaves standstill, filtration, drying obtain the graphite nano plate powder of thickness 20-50 nanometer.
Described spirituous solution is water and the ethanol mass ratio ethanolic soln lower than 1:2.
Described dispersion solvent is the aqueous solution containing tensio-active agent, the interpolation concentration 0.5 ~ 1.5g/L of expanded graphite powder in this dispersion solvent.
The described aqueous solution contains Xylo-Mucine (CMC) tensio-active agent of 0.1-2%, and solution ph is 11.
The described aqueous solution contains the Sodium dodecylbenzene sulfonate dispersion agent that mass content is 0.5%.
Ultrasonic generator ultrasonic power in described ultrasonic grinder be 1.2-2.2 kilowatt adjustable, ultrasonic frequency 20KHz.
Preparation process of the present invention is simple, and ultrasonic wave nanometer produces under utilizing ultrasonication to suppress the field of force, is liquid generation cavitation, fragmentation or explosion, thus expanded graphite interlayer is come off, thus obtain nano graphite flakes.Only need simple, common, the easy-operating equipment such as ultrasonic generator.The cavity of ultrasonic grinder effect, adopts impeller pump continuous feeding, installs cooling circulating water additional outside cavity.The nano graphite flakes solution obtained may be used for producing or scientific experimentation, or uses method acquisition nano graphite flakes powders such as filtering, centrifugal, dry.The present invention only need be equipped with the simple corollary apparatus such as impeller pump, and drying process uses simple usual means or natural drying to complete.
Specific embodiments
Below in conjunction with specific embodiment, the present invention will be further described.
A kind of nano-graphite piece preparation method, be that the expanded graphite that raw material obtains adds ethanol by 0.5 ~ 10g/L or contains in the aqueous solution of tensio-active agent by 80 order crystalline flake graphites, solution centrifugal pumping is entered in the cavity of ultrasonic cell disruptor effect, continuous action, after 40 minutes to 72 hours, can obtain the dispersion soln of nano graphite flakes.
The medium that the present invention uses in the nanometer process of expanded graphite is ethanolic soln.The present invention can also use other solvents, such as add proper amount of surfactant in aqueous, if Xylo-Mucine, Sodium dodecylbenzene sulfonate etc. are as dispersion agent, weaken the reunion of expanded graphite, and expanded graphite is evenly distributed in the solution, nanometer degree is higher.Ultrasonic power controls more than 2 kilowatts, and powder and spirituous solution concentration are about 10g/L, and ultrasonic time can obtain the good Nano graphite lamella of uniformity coefficient at 40 minutes, 5 ~ 50 microns, sheet footpath, thickness 20 ~ 50 nanometer.
Described solution can be the mixed solution of water and tensio-active agent, but difference and the feature of spirituous solution are that in water solvent, expanded graphite material concentration is in the dilute solution of 0.5 ~ 1.5g/L, and what obtain is the dispersion liquid of graphite nano plate, leaves standstill and does not produce precipitation in 2 months.
Ultrasonic generator ultrasonic power in described ultrasonic grinder be 1.2-2.2 kilowatt adjustable, ultrasonic frequency 20KHz.
Embodiment 1: a kind of preparation method of graphite nano plate, it carries out as follows: first take 200 order expanded graphite 3g, add the dehydrated alcohol of 6L, in ultrasonic grinder working cavity, continuous ultrasound nanometer, after carrying out 72h, dry solution, gained powder is nano graphite flakes, 5 ~ 10 microns, sheet footpath, thickness 30 nanometer.
Example 2: by 80 order expanded graphite 80g, add massfraction 90% industrial spirit of 8L, use impeller pump to be sent into continuously by mixing liquid in ultrasonic grinder Work container, with the continuous nanometer of ultrasonic grinder, after carrying out 40 minutes, release liquid, leave standstill 2 hours, pour out supernatant liquid, suction filtration, oven dry, gained powder is nano graphite flakes, 20 ~ 50 microns, sheet footpath, thickness 30 nanometer.
Example 3: take expanded graphite 12g, add deionized water and massfraction 0.1% Xylo-Mucine (CMC) mixed solution of 8L, be 11 by ammoniacal liquor regulator solution pH value, use impeller pump continuous feeding, Ultrasonic cell smash carries out nanometer to mixing liquid, after carrying out 24h, gained solution is the nano graphite flakes aqueous solution, leaves standstill and does not produce precipitation in 2 months.
Example 4: take expanded graphite 8g, add deionized water and the massfraction 0.5% Sodium dodecylbenzene sulfonate mixed solution of 8L, be 11 by ammoniacal liquor regulator solution pH value, use impeller pump continuous feeding, Ultrasonic cell smash carries out nanometer to mixing liquid, after carrying out 72h, gained solution is the nano graphite flakes aqueous solution, leaves standstill and does not produce precipitation in 2 months.
Claims (7)
1. a nano-graphite piece preparation method, its with expanded graphite powder for raw material, it is characterized in that: first expanded graphite powder is added in dispersion solvent; Then by impeller pump, mixing solutions circulation is joined in ultrasonic grinder; Start ultrasonic grinder and ultrasonic stripping nano equalization is carried out 40 minutes to 72 hours to mixing solutions, obtain nano graphite flakes solution.
2. nano-graphite piece preparation method according to claim 1, it is characterized in that: described dispersion solvent is ethanolic soln, the interpolation concentration 0.5 ~ 10g/L of expanded graphite powder in this dispersion solvent, ultrasonic nano equalization obtains nano graphite flakes ethanolic soln, after described nano graphite flakes ethanolic soln leaves standstill, filtration, drying obtain the graphite nano plate powder of thickness 20-50 nanometer.
3. nano-graphite piece preparation method according to claim 2, is characterized in that described spirituous solution is the ethanolic soln that water and ethanol mass ratio are less than 1:2.
4. nano-graphite piece preparation method according to claim 1, is characterized in that: described dispersion solvent is the aqueous solution containing tensio-active agent, the interpolation concentration 0.5 ~ 1.5g/L of expanded graphite powder in this dispersion solvent.
5. nano-graphite piece preparation method according to claim 4, is characterized in that: the described aqueous solution contains the Xylo-Mucine tensio-active agent of 0.1-0.5%, and solution ph is 11.
6. nano-graphite piece preparation method according to claim 4, is characterized in that: the described aqueous solution contains 0.5% Sodium dodecylbenzene sulfonate dispersion agent.
7. nano-graphite piece preparation method according to claim 1, is characterized in that: the ultrasonic generator ultrasonic power in described ultrasonic grinder be 1.2-2.2 kilowatt adjustable, ultrasonic frequency 20KHz.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500285A (en) * | 2017-09-30 | 2017-12-22 | 湖南国盛石墨科技有限公司 | The preparation method of superfine graphite |
| CN109384219A (en) * | 2018-11-16 | 2019-02-26 | 新奥石墨烯技术有限公司 | Nano-fluid towards high efficient heat exchanging working medium and preparation method thereof and heat exchange equipment |
| CN110467178A (en) * | 2019-09-29 | 2019-11-19 | 威海云山科技有限公司 | A method of preparing graphene |
| WO2019223756A1 (en) * | 2018-05-24 | 2019-11-28 | 深圳三匚科技有限公司 | Graphite material and preparation method and application thereof |
| CN112919457A (en) * | 2021-02-26 | 2021-06-08 | 中科雷舜智能科技(宁波)有限公司 | Nano material and preparation method thereof |
| CN114709506A (en) * | 2022-05-20 | 2022-07-05 | 中南大学 | Modification method of retired lithium ion battery negative electrode material |
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| US20120219719A1 (en) * | 2009-11-03 | 2012-08-30 | Jong-Sam Yu | Method of manufacturing composite carbon sheet using expanded graphite sheet and mixed dispersion solution |
| EP2537801A1 (en) * | 2010-02-19 | 2012-12-26 | Incubation Alliance Inc. | Carbon material and method for producing same |
| CN103435033A (en) * | 2013-08-12 | 2013-12-11 | 上海理工大学 | Simple and convenient method for preparing graphene-zinc oxide nanorod composite material in ultrasonic wave |
| CN103693636A (en) * | 2013-11-11 | 2014-04-02 | 中国科学院深圳先进技术研究院 | Graphene preparation method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20120219719A1 (en) * | 2009-11-03 | 2012-08-30 | Jong-Sam Yu | Method of manufacturing composite carbon sheet using expanded graphite sheet and mixed dispersion solution |
| EP2537801A1 (en) * | 2010-02-19 | 2012-12-26 | Incubation Alliance Inc. | Carbon material and method for producing same |
| CN103435033A (en) * | 2013-08-12 | 2013-12-11 | 上海理工大学 | Simple and convenient method for preparing graphene-zinc oxide nanorod composite material in ultrasonic wave |
| CN103693636A (en) * | 2013-11-11 | 2014-04-02 | 中国科学院深圳先进技术研究院 | Graphene preparation method |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107500285A (en) * | 2017-09-30 | 2017-12-22 | 湖南国盛石墨科技有限公司 | The preparation method of superfine graphite |
| WO2019223756A1 (en) * | 2018-05-24 | 2019-11-28 | 深圳三匚科技有限公司 | Graphite material and preparation method and application thereof |
| CN112188994A (en) * | 2018-05-24 | 2021-01-05 | 深圳三匚科技有限公司 | Graphite material and preparation method and application thereof |
| CN109384219A (en) * | 2018-11-16 | 2019-02-26 | 新奥石墨烯技术有限公司 | Nano-fluid towards high efficient heat exchanging working medium and preparation method thereof and heat exchange equipment |
| CN110467178A (en) * | 2019-09-29 | 2019-11-19 | 威海云山科技有限公司 | A method of preparing graphene |
| CN110467178B (en) * | 2019-09-29 | 2022-07-22 | 威海云山科技有限公司 | Method for preparing graphene |
| CN112919457A (en) * | 2021-02-26 | 2021-06-08 | 中科雷舜智能科技(宁波)有限公司 | Nano material and preparation method thereof |
| CN114709506A (en) * | 2022-05-20 | 2022-07-05 | 中南大学 | Modification method of retired lithium ion battery negative electrode material |
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Application publication date: 20150909 |