CN108083265A - A kind of dry type of graphene nano powder removes production technology - Google Patents
A kind of dry type of graphene nano powder removes production technology Download PDFInfo
- Publication number
- CN108083265A CN108083265A CN201710107333.8A CN201710107333A CN108083265A CN 108083265 A CN108083265 A CN 108083265A CN 201710107333 A CN201710107333 A CN 201710107333A CN 108083265 A CN108083265 A CN 108083265A
- Authority
- CN
- China
- Prior art keywords
- graphite
- nano powder
- graphene nano
- production technology
- dry type
- 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
Links
Abstract
The present invention relates to the production method technical fields of graphene, and in particular to a kind of dry type of graphene nano powder removes production technology.Specifically include following steps：(1) using the expansible graphite of high expansioning multiple as raw material, graphite worm is obtained after heating expansion under inertia or reducing gas atmosphere；(2) collect obtained graphite worm becomes graphite microchip in crusher chamber by ultrahigh speed rotational shear；(3) graphite microchip importing is placed in processing (4) in the high-pressure bottle in shock platforms will continuously be removed from the graphite microchip importing high pressure ultrasonic wave stripping chamber that high-pressure bottle flows out, obtains graphene nano powder.Obtained graphene single-layer sheet footpath is big, and the number of plies is few, and versatility is good；Highly conductive, low resistance, high-specific surface area；And it manufactures at low cost.
Description
Technical field
The present invention relates to the production method technical fields of graphene, and in particular to a kind of dry type stripping of graphene nano powder
From production technology.
Background technology
Graphene (Graphene) is a kind of two-dimensional material being made of single layer of carbon atom, be found since 2004 with
Come, constantly show its excellent performance to common people.For graphene because of its outstanding light transmittance, huge thermal conductivity factor is extremely low
Resistivity and receive pro-gaze, be known as trigger Industrial Revolution next-generation material.At present, the main method for preparing graphene has：
Mechanical stripping method, solvent stripping method, chemical vapour deposition technique, crystal epitaxy method, oxidation-reduction method etc..Wherein, preceding two
Kind stripping method low production efficiency；Chemical vapour deposition technique and crystal epitaxy method are of high cost, complicated for operation and can not produce big
Area graphite alkene；Though and it is oxidation-reduction method cost bottom, simple for process, the graphene-structured defect prepared is larger and impurity contains
It measures more.Since the above method all has cost, and the basic reason of the large-scale application of graphene is hindered to be exactly into
This, on the premise of cost is higher, the application of graphene is only high tip, and great demand is because price reasons are kept outside of the door,
Such as magnesia carbon brick of anticorrosive coating, rubber, plastics, heat proof material etc., each annual demand are above ten thousand tons or even 100,000
Ton, price endurance is relatively low, and multi-layer graphene can meet these demands, therefore, develops a kind of new, ultralow
The graphene production technology of cost is imperative.
The content of the invention
The purpose of the present invention is to solve the above problem, the dry type for providing a kind of graphene nano powder removes production work
Skill.
In order to reach foregoing invention purpose, the present invention uses following technical scheme：
A kind of dry type of graphene nano powder removes production technology, specifically includes following steps：
(1) using the expansible graphite of high expansioning multiple as raw material, the heat expandable under inertia or reducing gas atmosphere
Graphite powder to temperature is 800 DEG C -1400 DEG C, makes that it prepares high expansioning multiple after expanding completely and the graphite of high-specific surface area is compacted
Worm；
(2) collect obtained graphite worm becomes graphite microchip in crusher chamber by ultrahigh speed rotational shear；
(3) graphite microchip importing is placed in the high-pressure bottle in shock platforms, after filling of the container using compressed gas
Supercharging makes pressure be more than or equal to 1MPa；By controlling powder from high-pressure bottle bottom pipe to the adjustment of vibration frequency and amplitude
Discharge；
(4) it will import from the graphite microchip that high-pressure bottle flows out in high pressure ultrasonic wave stripping chamber and continuously be removed, then
It is graphene nano powder to be reduced to by pressure loading valve and recycle powder by cyclopneumatic separator after normal pressure.
As further preferred embodiment, the expansion multiple of graphite worm is more than 300 times in the step (1), specific surface
Product is more than 30m2/g。
As further preferred embodiment, the expansion multiple of graphite worm is more than 500 times in the step (1), specific surface
Product is more than 60m2/g。
As further preferred embodiment, the expansion multiple of graphite worm is more than 800 times in the step (1), specific surface
Product is more than 70m2/g。
As further preferred embodiment, expansible graphite is for low-sulphur expanded graphite or without sulphur heavy metal free in step (1)
The expanded graphite of oxide intercalation.
It is raw after being cleaned multiple times of hydrochloric acid, nitric acid or organic acid that low-sulphur expanded graphite is that the expanded graphite after sulfuric acid intercalation passes through
Into graphite, it using hydrogen peroxide and nitric acid as oxidant, organic acid is slotting that the expanded graphite of no sulphur heavy metal free oxide intercalation, which is,
The expanded graphite without sulphur heavy metal free of layer agent.
As further preferred embodiment, heat expandable graphite powder heating expansion furnace used is microwave heating expansion furnace,
Expansion temperature is more than 800 DEG C.
As further preferred embodiment, expansion temperature is 1200 DEG C -1400 DEG C.
As further preferred embodiment, in step (2), the graphite microchip after ultrahigh speed rotational shear is 10-100 μm
Fluffy graphite flake, bulk density be more than 0.1g/cm3.
As further preferred embodiment, in crusher chamber crusher used be multigroup high-speed rotating blade, crusher knife
The rotating speed of piece is more than 1000rpm.
As further preferred embodiment, the gas pressure of ultrasonic wave stripping cavity is more than 1MPa in step (4), and gas is
Inertia or reducibility gas are specially nitrogen, argon gas or carbon dioxide.
As further preferred embodiment, step (4) mesohigh ultrasonic wave removes the work of the supersonic generator used in chamber
Make head to design using multigroup work head, be specially 3 groups or more, and the power of every group of work head is more than 1kW.
As further preferred embodiment, audio impedance matching shape may be employed in the work head of supersonic generator, surpasses
The work head of sonic generator is multisectional multilayer material structure, and the audio impedance of layers of material is from gradual close to supersonic generator
It is reduced to close to gas, multisectional multilayer material is the combination of titanium alloy, aluminium alloy, graphite and epoxy resin.
Compared with prior art, the present invention advantageous effect is：Draw ratio is big, and cost is extremely low.
Specific embodiment
Explanation is further described to technical scheme below by specific embodiment.
If without specified otherwise, the raw material employed in the embodiment of the present invention is raw material commonly used in the art, is implemented
Method employed in example is the conventional method of this field.
Overall technical solution is：
A kind of dry type of graphene nano powder removes production technology, specifically includes following steps：
(1) using the expansible graphite of high expansioning multiple as raw material, the heat expandable under inertia or reducing gas atmosphere
Graphite powder to temperature is 800 DEG C -1400 DEG C, makes that it prepares high expansioning multiple after expanding completely and the graphite of high-specific surface area is compacted
Worm；The expansion multiple of graphite worm is more than 300 times, and specific surface area is more than 30m2The expansion multiple of/g, preferably graphite worm are more than
500 times, specific surface area is more than 60m2/g；The expansion multiple of more preferable graphite worm is more than 800 times, and specific surface area is more than 70m2/
g.Expansible graphite is low-sulphur expanded graphite or the expanded graphite without sulphur heavy metal free oxide intercalation；Heat expandable graphite powder
Heating expansion furnace used is microwave heating expansion furnace, and expansion temperature is more than 800 DEG C, it is preferred that expansion temperature is 1200 DEG C -1400
℃。
(2) collect obtained graphite worm becomes graphite microchip in crusher chamber by ultrahigh speed rotational shear；Through superelevation
The fluffy graphite flake that graphite microchip after fast rotational shear is 10-100 μm, bulk density are more than 0.1g/cm3；In crusher chamber
Crusher used is multigroup high-speed rotating blade, and the rotating speed of breaker bar is more than 1000rpm.
(3) graphite microchip importing is placed in the high-pressure bottle in shock platforms, after filling of the container using compressed gas
Supercharging makes pressure be more than or equal to 1MPa；By controlling powder from high-pressure bottle bottom pipe to the adjustment of vibration frequency and amplitude
Discharge；
(4) it will import from the graphite microchip that high-pressure bottle flows out in high pressure ultrasonic wave stripping chamber and continuously be removed, then
It is graphene nano powder to be reduced to by pressure loading valve and recycle powder by cyclopneumatic separator after normal pressure；Ultrasonic wave removes cavity
Gas pressure be more than 1MPa, gas be inertia or reducibility gas, be specially nitrogen, argon gas or carbon dioxide；High pressure ultrasound
The work head that ripple removes the supersonic generator used in chamber is designed using multigroup work head, is specially 3 groups or more, and every group of work
The power of head is more than 1kW；Audio impedance matching shape, the work of supersonic generator may be employed in the work head of supersonic generator
Make head as multisectional multilayer material structure, the audio impedance of layers of material is gradually decreased as from close to supersonic generator close to gas
Body, multisectional multilayer material are the combination of titanium alloy, aluminium alloy, graphite and epoxy resin.
Embodiment 1：
A kind of dry type of graphene nano powder removes production technology, specifically includes following steps：
(1) using the expansible graphite of high expansioning multiple as raw material, added under inertia or reducing gas atmosphere using microwave
Thermal expansion stove；Heat expandable graphite powder makes it prepare high expansioning multiple and high-ratio surface after expanding completely to temperature for 1200 DEG C
Long-pending graphite worm；The expansion multiple of graphite worm is more than 300 times, and specific surface area is more than 30m2/ g is specifically chosen graphite worm
Expansion multiple be more than 500 times, specific surface area be more than 60m2/g；Expansible graphite is low-sulphur expanded graphite；Heat expandable stone
Heating expansion furnace is used in ink powder
(2) collect obtained graphite worm becomes graphite microchip in crusher chamber by ultrahigh speed rotational shear；Through superelevation
The fluffy graphite flake that graphite microchip after fast rotational shear is 10-20 μm, bulk density are more than 0.1g/cm3；Institute in crusher chamber
It is multigroup high-speed rotating blade with crusher, the rotating speed of breaker bar is more than 1000rpm；It is 3000rm herein；
(3) graphite microchip importing is placed in the high-pressure bottle in shock platforms, after filling of the container using compressed gas
Supercharging makes pressure be more than or equal to 1MPa；Control pressure is 2MPa herein；By controlling powder to the adjustment of vibration frequency and amplitude
From the discharge of high-pressure bottle bottom pipe；
(4) it will import from the graphite microchip that high-pressure bottle flows out in high pressure ultrasonic wave stripping chamber and continuously be removed, then
It is graphene nano powder to be reduced to by pressure loading valve and recycle powder by cyclopneumatic separator after normal pressure；Ultrasonic wave removes cavity
Gas pressure for 1.5MPa, gas is inertia or reducibility gas.
Embodiment 2：
A kind of dry type of graphene nano powder removes production technology, specifically includes following steps：
(1) using the expansible graphite of high expansioning multiple as raw material, added under inertia or reducing gas atmosphere using microwave
Thermal expansion stove；Heat expandable graphite powder makes it prepare high expansioning multiple and high-ratio surface after expanding completely to temperature for 1400 DEG C
Long-pending graphite worm；The expansion multiple of graphite worm is more than 300 times, and specific surface area is more than 30m2/ g is specifically chosen graphite worm
Expansion multiple be more than 700 times, specific surface area be more than 70m2/g；Expansible graphite is low-sulphur expanded graphite；Heat expandable stone
Heating expansion furnace is used in ink powder
(2) collect obtained graphite worm becomes graphite microchip in crusher chamber by ultrahigh speed rotational shear；Through superelevation
The fluffy graphite flake that graphite microchip after fast rotational shear is 50-70 μm, bulk density are more than 0.1g/cm3；Institute in crusher chamber
It is multigroup high-speed rotating blade with crusher, the rotating speed of breaker bar is more than 1000rpm；It is 5000rm herein；
(3) graphite microchip importing is placed in the high-pressure bottle in shock platforms, after filling of the container using compressed gas
Supercharging makes pressure be more than or equal to 1MPa；Control pressure is 1.5MPa herein；By controlling powder to the adjustment of vibration frequency and amplitude
Body is from the discharge of high-pressure bottle bottom pipe；
(4) it will import from the graphite microchip that high-pressure bottle flows out in high pressure ultrasonic wave stripping chamber and continuously be removed, then
It is graphene nano powder to be reduced to by pressure loading valve and recycle powder by cyclopneumatic separator after normal pressure；Ultrasonic wave removes cavity
Gas pressure for 1.5MPa, gas is inertia or reducibility gas.
Claims (10)
1. a kind of dry type of graphene nano powder removes production technology, which is characterized in that specifically includes following steps：
(1) using the expansible graphite of high expansioning multiple as raw material, the heat expandable graphite under inertia or reducing gas atmosphere
Powder to temperature is 800 DEG C -1400 DEG C, it is made to prepare the graphite worm of high expansioning multiple and high-specific surface area after expanding completely；
(2) collect obtained graphite worm becomes graphite microchip in crusher chamber by ultrahigh speed rotational shear；
(3) graphite microchip importing is placed in the high-pressure bottle in shock platforms, is pressurized after filling of the container using compressed gas
Pressure is made to be more than or equal to 1MPa；Pass through adjustment control outflow of the powder from high-pressure bottle bottom pipe to vibration frequency and amplitude
Amount；
(4) it will import from the graphite microchip that high-pressure bottle flows out in high pressure ultrasonic wave stripping chamber and continuously be removed, then be passed through
It is graphene nano powder that pressure loading valve, which is reduced to after normal pressure by cyclopneumatic separator recycling powder,.
2. a kind of dry type of graphene nano powder according to claim 1 removes production technology, which is characterized in that described
The expansion multiple of graphite worm is more than 300 times in step (1), and specific surface area is more than 30m2/g。
3. a kind of dry type of graphene nano powder according to claim 1 removes production technology, which is characterized in that described
Expansible graphite is low-sulphur expanded graphite or the expanded graphite without sulphur heavy metal free oxide intercalation in step (1).
4. a kind of dry type of graphene nano powder according to claim 1 removes production technology, which is characterized in that step
(1) heat expandable graphite powder heating expansion furnace used is microwave heating expansion furnace in, and expansion temperature is more than 800 DEG C.
5. a kind of dry type of graphene nano powder according to claim 4 removes production technology, which is characterized in that step
(1) expansion temperature is 1200 DEG C -1400 DEG C in.
6. a kind of dry type of graphene nano powder according to claim 1 removes production technology, which is characterized in that step
(2) in, the graphite microchip after ultrahigh speed rotational shear is 10-100 μm of fluffy graphite flake, and bulk density is more than 0.1g/
cm3。
7. a kind of dry type of graphene nano powder according to claim 1 removes production technology, which is characterized in that step
(2) in, crusher used is multigroup high-speed rotating blade in crusher chamber, and the rotating speed of breaker bar is more than 1000rpm.
8. a kind of dry type of graphene nano powder according to claim 1 removes production technology, which is characterized in that step
(4) gas pressure of ultrasonic wave stripping cavity is more than 1MPa in, and gas is inertia or reducibility gas, is specially nitrogen, argon gas
Or carbon dioxide.
9. a kind of dry type of graphene nano powder according to claim 1 removes production technology, which is characterized in that step
(4) mesohigh ultrasonic wave remove chamber used in supersonic generator work head using multigroup work head design, specially 3 groups with
On, and the power of every group of work head is more than 1kW.
10. a kind of dry type of graphene nano powder according to claim 9 removes production technology, which is characterized in that super
The work head of sonic generator uses audio impedance matching shape, and the work head of supersonic generator is multisectional multilayer material knot
Structure, the audio impedance of layers of material are gradually decreased as from close to supersonic generator close to gas, and multisectional multilayer material closes for titanium
The combination of gold, aluminium alloy, graphite and epoxy resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710107333.8A CN108083265A (en) | 2017-02-27 | 2017-02-27 | A kind of dry type of graphene nano powder removes production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710107333.8A CN108083265A (en) | 2017-02-27 | 2017-02-27 | A kind of dry type of graphene nano powder removes production technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108083265A true CN108083265A (en) | 2018-05-29 |
Family
ID=62171660
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710107333.8A Pending CN108083265A (en) | 2017-02-27 | 2017-02-27 | A kind of dry type of graphene nano powder removes production technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108083265A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108545728A (en) * | 2018-07-17 | 2018-09-18 | 北京化工大学 | A kind of bulking type graphene preparation facilities and method |
| CN108675667A (en) * | 2018-06-05 | 2018-10-19 | 苏州鼎烯聚材纳米科技有限公司 | A kind of device and method preparing concrete graphene nano aqueous slurry |
| CN108862259A (en) * | 2018-08-13 | 2018-11-23 | 深圳天元羲王材料科技有限公司 | A kind of graphene production method and device |
| CN108910869A (en) * | 2018-09-04 | 2018-11-30 | 宜昌新成石墨有限责任公司 | The preparation method of graphene slurry |
| CN110104639A (en) * | 2019-05-13 | 2019-08-09 | 四川欧迅能源工程科技有限公司 | A kind of extensive, controllable, inexpensive graphene preparation method |
| CN114575038A (en) * | 2022-03-11 | 2022-06-03 | 湖北瑞康医用耗材有限公司 | Preparation method of graphene non-woven fabric with microorganism inactivation performance |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060148966A1 (en) * | 2002-09-12 | 2006-07-06 | Board Of Trustees Operating Michigan State University | Expanded graphite and products produced therefrom |
| CN102583326A (en) * | 2012-01-11 | 2012-07-18 | 上海交通大学 | Method for preparing graphite by compressing CO2 fluid under ultrasonic assistance |
| CN103922330A (en) * | 2014-04-28 | 2014-07-16 | 南京新月材料科技有限公司 | Method for preparing graphene powder by using dry process |
| CN104555995A (en) * | 2013-10-22 | 2015-04-29 | 现代自动车株式会社 | Method of preparing graphene nanoplate, prepared graphene nanoplate, graphene nanoplate paste, and conductive layer including the graphene nanoplate |
| CN105417523A (en) * | 2015-07-14 | 2016-03-23 | 张亚妮 | Low-cost and large-scale production process of graphene nano powders and device used for same |
-
2017
- 2017-02-27 CN CN201710107333.8A patent/CN108083265A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060148966A1 (en) * | 2002-09-12 | 2006-07-06 | Board Of Trustees Operating Michigan State University | Expanded graphite and products produced therefrom |
| CN102583326A (en) * | 2012-01-11 | 2012-07-18 | 上海交通大学 | Method for preparing graphite by compressing CO2 fluid under ultrasonic assistance |
| CN104555995A (en) * | 2013-10-22 | 2015-04-29 | 现代自动车株式会社 | Method of preparing graphene nanoplate, prepared graphene nanoplate, graphene nanoplate paste, and conductive layer including the graphene nanoplate |
| CN103922330A (en) * | 2014-04-28 | 2014-07-16 | 南京新月材料科技有限公司 | Method for preparing graphene powder by using dry process |
| CN105417523A (en) * | 2015-07-14 | 2016-03-23 | 张亚妮 | Low-cost and large-scale production process of graphene nano powders and device used for same |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675667A (en) * | 2018-06-05 | 2018-10-19 | 苏州鼎烯聚材纳米科技有限公司 | A kind of device and method preparing concrete graphene nano aqueous slurry |
| CN108545728A (en) * | 2018-07-17 | 2018-09-18 | 北京化工大学 | A kind of bulking type graphene preparation facilities and method |
| CN108545728B (en) * | 2018-07-17 | 2023-04-21 | 北京化工大学 | Puffed graphene preparation device and method |
| CN108862259A (en) * | 2018-08-13 | 2018-11-23 | 深圳天元羲王材料科技有限公司 | A kind of graphene production method and device |
| CN108862259B (en) * | 2018-08-13 | 2022-04-01 | 深圳天元羲王材料科技有限公司 | Graphene production method and device |
| CN108910869A (en) * | 2018-09-04 | 2018-11-30 | 宜昌新成石墨有限责任公司 | The preparation method of graphene slurry |
| CN110104639A (en) * | 2019-05-13 | 2019-08-09 | 四川欧迅能源工程科技有限公司 | A kind of extensive, controllable, inexpensive graphene preparation method |
| CN114575038A (en) * | 2022-03-11 | 2022-06-03 | 湖北瑞康医用耗材有限公司 | Preparation method of graphene non-woven fabric with microorganism inactivation performance |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108083265A (en) | A kind of dry type of graphene nano powder removes production technology | |
| Dong et al. | Synthesis and reduction of large sized graphene oxide sheets | |
| Kairi et al. | Toward high production of graphene flakes–a review on recent developments in their synthesis methods and scalability | |
| CN106115666B (en) | A kind of ultrasonic wave, supercritical CO2And the microwave method that stripping prepares graphene three times | |
| Zhang et al. | 3D printing of graphene aerogels | |
| CN106882795B (en) | A kind of scale ultrasound stripping prepares the method for graphene and the application of graphene | |
| CN104310375B (en) | A kind of method of removing carbon impurity in SWCN | |
| JP6283508B2 (en) | Exfoliated graphite dispersion and method for producing exfoliated graphite | |
| CN107298440B (en) | A kind of method for continuously preparing graphene in screw machine using supercritical fluid | |
| CN105668554A (en) | Method of preparing graphene nanoplatelets through air flow stripping classification | |
| CN105858641B (en) | Graphene production method | |
| Wang et al. | Microstructure and properties of carbon nanosheet/copper composites processed by particle-assisted shear exfoliation | |
| CN106744881A (en) | A kind of method that utilization ultrasonic continuous prepare Graphene | |
| CN103663439A (en) | Method and device for preparing graphene through processing dry ice by shock waves | |
| Sari et al. | Facile preparation of carbon nanofiber from banana peel waste | |
| CN105905889A (en) | Method for producing graphene through high pressure hydrothermal expansion method | |
| Suslova et al. | Carbon nanotube frameworks by spark plasma sintering | |
| CN106335925B (en) | A kind of method for preparing individual layer 2H phases molybdenum disulfide/graphene composite material | |
| CN111908452A (en) | Graphene carbon nanotube composite high-thermal-conductivity film and preparation method thereof | |
| CN111349905A (en) | Preparation method of enhanced copper-based composite wire | |
| CN106006621B (en) | Preparation method of multilayer graphene | |
| KR20180074102A (en) | High purity reduced graphene oxide and manufacturing method thereof | |
| CN104402450A (en) | Method for quickly preparing Ti2AlN ceramic powder on the basis of thermal explosion reaction at low temperature | |
| CN110386597B (en) | Equipment and method for large-scale production of thin-layer graphene | |
| CN105521752A (en) | Graphite chemical substance intercalation reaction vessel and technological method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180529 |