CN105776193A - Method for preparing graphene nanoplatelets with pulsed high pressure water jet mill - Google Patents
Method for preparing graphene nanoplatelets with pulsed high pressure water jet mill Download PDFInfo
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- CN105776193A CN105776193A CN201610110956.6A CN201610110956A CN105776193A CN 105776193 A CN105776193 A CN 105776193A CN 201610110956 A CN201610110956 A CN 201610110956A CN 105776193 A CN105776193 A CN 105776193A
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- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
Abstract
The invention relates to the field of graphene materials, in particular to a method for preparing graphene nanoplatelets with a pulsed high pressure water jet mill.According to the method, a plugging layer is pressurized, Van der Waals' force among graphite powder layers is reduced, so that the graphite layers are easy to strip, then graphite powder is crushed and stripped under the action of water jet and turbulent flow and cavitation through pulsed high pressure water jet of the pulsed high pressure water jet mill, the evenly-dispersed graphene nanoplatelets with the number of layers ranging from 100 to 200 are obtained.Continuous and large-scale production of the graphene nanoplatelets with the number of layers being even is achieved, the yield is high, the cost is low, no pollution is caused, the layer thickness meets the use requirements in the fields of rubber enhancement, plastic enhancement, coating corrosion prevention, lubrication and sewage treatment, and it is convenient to promote large-scale application of graphene.
Description
Technical field
The present invention relates to grapheme material field, be specifically related to a kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip.
Background technology
Graphene is the another Novel Carbon Nanomaterials being found after CNT, due to the structure that it is special so that Graphene presents physics, chemistry and the mechanical property of uniqueness, presents wide application prospect, receives unprecedented concern and attention.Although the prospect of Graphene is the most tempting, but still have many extremely challenging problems, wherein the preparation of Graphene is exactly the most basic in all problems, if cannot the Graphene that high-quality and high yield be prepared of high-efficient simple, then will be very limited about the otherwise research of Graphene and application.
Chinese invention patent application 201210248634.X discloses the preparation method of a kind of Graphene, comprise the following steps: glucide is mixed with graphite oxide in mass ratio 0.01～0.2:1, add deionized water, ultrasonic 30～60 minutes, obtain the mixed solution of glucide and graphene oxide；Mixed solution is filtered, after the filter residue obtained is dried 12 ~ 24 hours at 60 ~ 80 DEG C, is placed in reacting furnace；Heating reaction furnace, to 300～600 DEG C, is incubated and reacts for 10～30 minutes, after question response terminates, be cooled to room temperature, opens reacting furnace, collects solid product, and this solid product is Graphene.The graphene preparation method that the present invention provides, preparation technology is simple, and the Graphene obtained has loose structure, and crystal structure is complete, functional, but the preparation method of this invention is with high costs, is difficult to industrialized production.
Chinese invention patent application number 201510174415.5 discloses a kind of method that Graphene is prepared in rotational shear under electric field environment, and step is: cathode anode is connected dc source, stirs electrolyte with agitator；Under constant voltage, high purity graphite is peeled off in cathodic polarization, and electrolyte is under agitator effect simultaneously, is stirred by certain speed, makes the multi-layer graphene that cathodic disbonding is got off again by a shearing force, prepares the solution containing Graphene；Solution containing Graphene is cleaned at least 5 times, ultrasonic disperse, low-speed centrifugal；Then the supernatant liquor high speed centrifugation of product that will obtain；Last drying to obtain Graphene.The preparation method of the present invention is simple and efficient, safe green, cost are relatively low and can directly peel off native graphite, but the preparation method complex process of this invention, it is difficult to industrialized production.
Chinese invention patent application number 201310151062.8 discloses a kind of method that in using, air pressure jet flow plasma prepares graphene oxide/silver antibacterial composite material, and this invention is by immersion silver presoma, at surface of graphene oxide load silver ion；In the most at room temperature using, air pressure hydrogen cold-plasma jet processes, and silver ion reduction is become Nano silver grain, obtains graphene oxide/silver composite material.This invention utilizes the method for plasma deoxidization predecessor, it is to avoid use the chemical reagent having pollution to environment, owing to reducing under dry state, greatly reduce the loss of noble metal, can efficiently prepare graphene oxide/silver composite material, but the preparation method productivity of this invention is low, yield is little.
Transformation for modern industry is upgraded, and Graphene will be likely to become one of power-assisted, but existing graphene preparation method is due to defects such as cost height, complex process, environmental pollution are big, hardly results in actual application and popularization.Therefore, a kind of preparation technology is simple in invention, production safety environmental protection, and production cost is low, and yield is high, the graphene preparation method of constant product quality, the application to promotion grapheme material, promotes that the development of Graphene industry is significant.
Summary of the invention
High for current Graphene production cost, environmental pollution is big, and the shortcoming of complicated process of preparation, the present invention proposes a kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip.The method utilizes high voltage pulse water jet mill to prepare the number of plies graphene microchip being evenly distributed at 100-200 layer, the graphene microchip of preparation can be applicable in the composites such as rubber, plastics, coating, lubricating oil, sewage disposal, or as preparing the raw material of Graphene further, the preparation cost of current Graphene can be greatly reduced.
For solve the problems referred to above, the present invention by the following technical solutions:
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip, it is characterized in that: first graphite powder is uniformly divided and spread in aqueous, then pressurization intercalated graphite powder, weaken Van der Waals force between graphite linings, graphite powder is made to pulverize stripping under the effect of water jet, turbulent flow and cavitation by the high voltage pulse water jet of high voltage pulse water jet mill again, obtaining the number of plies finely dispersed graphene microchip at 100-200 layer, concrete grammar is as follows:
(1) by graphite powder heat pre-treatment 20min-40min at heating-up temperature is 180 DEG C-220 DEG C that weight portion is 90-98, then it is the ethanol of 0.5-2.0 by graphite powder and weight portion, in the high-speed mixer that weight portion is the PTPP of 0.4-1.5 and water that weight portion is 500-1000 adds, adition process stirs with rotating speed 360rpm-480rpm simultaneously, mixing time 3min, obtains the graphite powder aqueous solution；
(2) graphite powder aqueous solution step (1) obtained is sent in closed reactor, and under pressure is 10MPa-25MPa, pressurize intercalation embrittlement 4h-10h by graphite powder, weakens graphite powder interlayer Van der Waals force, obtains pretreating graphite amidin；
(3) pretreating graphite amidin step (2) obtained is sent in high voltage pulse water jet mill, the rotated joint of high voltage pulse water jet, by nozzle directive graphite powder, under buoyancy of water effect, graphite powder is hit by high voltage pulse water jet, simultaneously under the effect of turbulent flow and cavitation so that graphite powder is pulverized and peeled off, through filtering, drying, obtain the number of plies finely dispersed graphene microchip at 100-300 layer.
Described graphite powder is any one in expanded graphite, thermal cracking graphite, and particle diameter is between 0.5 millimeter and 5 millimeters.
Described high pressurewater cleaning machine work water pressure is 10-60MPa, and pulse frequency is 20-50Hz.
Described nozzle is round mouth nozzle, and nozzle diameter is between 8mm and 20mm, and the work angle of nozzle is between 30 ° and 60 °.
Further, described nozzle at least one, when having two and with top nozzle, both can work between nozzle, it is also possible to alternation simultaneously.
First being uniformly dispersed in the aqueous solution by graphite powder, the environment in pressurization carries out intercalation processing, makes graphite powder interlayer brittle, weakens Van der Waals force between graphite linings, make graphite linings be more easy to crushed stripping；Then in high voltage pulse water jet mill, the rotated joint of high voltage pulse water jet, by nozzle directive graphite powder, graphite powder is under buoyancy of water effect, constantly hit by high voltage pulse water jet, in the process, the water hammer hitting power that graphite powder is formed by high voltage pulse water jet, it it is tens times of common high-pressure water jet so that the pulverizing that graphite powder can be more efficient is peeled off；Simultaneously, when pulse water jet is in floodage, turbulent flow and cavitation can be produced around high voltage pulse water jet, turbulent flow not only causes the collision between graphite powder, so that grinding voluntarily between graphite powder, but also can will be located in again bearing jet in the particle volume outside main hitting region is drawn onto Da Ji district and hit；Cavitation produces bubble, the hyperpressure that bubble washes away when crumbling and fall acts on graphite powder so that being in the graphite powder beyond power stream hitting region and receive additional pulverization, it is the most that bubble produces, the intensity of pressure produced is the biggest, the best to the pulverizing peeling effect of graphite powder.Under the effect of the water hammer, turbulent flow and the cavitation that are produced by high voltage pulse water jet, make graphite powder constantly peel off, thus obtain the uniform graphene microchip of the number of plies.
In order to promote the extensive application of grapheme material, the present invention proposes a kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip, the method can the acquisition number of plies of volume production in the graphene microchip of 100-200 layer, stable production process, and it is pollution-free, without dust, low cost, the graphene microchip not only number of plies of preparation is uniform, and have the mechanical strength of excellence concurrently, conduction, heat conductivility, and good lubrication, high temperature resistant and anticorrosion properties, but also there is the specific surface area of super large, thus graphene microchip can be applied to rubber, plastics, coating, in the composites such as lubricating oil；The preparation cost of current Graphene can also can be greatly reduced as preparing the raw material of Graphene further.
A kind of graphene microchip utilizing high voltage pulse water jet mill to prepare of the present invention, not only the number of plies is uniformly dispersed, and pollution-free, low cost, meet the requirement in fields such as rubber reinforcement, plastics enhancing, anticorrosion with coat, lubrication, sewage disposals, be conducive to promoting the large-scale application of Graphene.
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip of the present invention, compared with prior art, its prominent feature and excellent effect are:
1, utilize pressurization intercalation pretreating graphite powder, make graphite layers brittle, reduce Van der Waals force between graphite linings so that graphite linings is more easily peeled.
2, high pressurewater cleaning machine is utilized, the common effect of water hammer, turbulent flow and cavitation graphite powder caused by high voltage pulse water jet, allow graphite constantly pulverize stripping, it is thus achieved that the number of plies is controlled, the graphene microchip that is evenly distributed.
3, preparation method of the present invention is easily controllable, can realize the closed production of serialization, puts into little, low cost, non-environmental-pollution, yield height, has significant market using value.
Accompanying drawing explanation
For further illustrating the method utilizing high voltage pulse water jet mill to prepare graphene microchip, illustrated by accompanying drawing.
Accompanying drawing 1: for high voltage pulse water jet mill schematic diagram.1-swivel joint；2-nozzle.
Detailed description of the invention
Below by way of detailed description of the invention, the present invention is described in further detail, but this should not being interpreted as, the scope of the present invention is only limitted to Examples below.In the case of without departing from said method thought of the present invention, the various replacements made according to ordinary skill knowledge and customary means or change, should be included in the scope of the present invention.
Embodiment 1
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip:
(1) by graphite powder heat pre-treatment 20min at heating-up temperature is 180 DEG C that weight portion is 90, then it is the ethanol of 0.5 by graphite powder and weight portion, weight portion be 0.4 PTPP and the high-speed mixer that adds of water that weight portion is 500 in, adition process stirs with rotating speed 360rpm simultaneously, mixing time 3min, obtains the graphite powder aqueous solution；
(2) graphite powder aqueous solution step (1) obtained is sent in closed reactor, and under pressure is 10MPa, pressurize intercalation embrittlement 4h by graphite powder, weakens graphite powder interlayer Van der Waals force, obtains pretreating graphite amidin；
(3) pretreating graphite amidin step (2) obtained is sent in high voltage pulse water jet mill, the rotated joint of high voltage pulse water jet, by nozzle directive graphite powder, under buoyancy of water effect, graphite powder is hit by high voltage pulse water jet, simultaneously under the effect of turbulent flow and cavitation so that graphite powder is pulverized and peeled off, through filtering, drying, obtain the number of plies finely dispersed graphene microchip at 100-300 layer.
Embodiment 2
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip:
(1) by graphite powder heat pre-treatment 40min at heating-up temperature is 220 DEG C that weight portion is 98, then it is the ethanol of 2.0 by graphite powder and weight portion, weight portion be 1.5 PTPP and the high-speed mixer that adds of water that weight portion is 1000 in, adition process stirs with rotating speed 480rpm simultaneously, mixing time 3min, obtains the graphite powder aqueous solution；
(2) graphite powder aqueous solution step (1) obtained is sent in closed reactor, and under pressure is 25MPa, pressurize intercalation embrittlement 10h by graphite powder, weakens graphite powder interlayer Van der Waals force, obtains pretreating graphite amidin；
(3) pretreating graphite amidin step (2) obtained is sent in high voltage pulse water jet mill, the rotated joint of high voltage pulse water jet, by nozzle directive graphite powder, under buoyancy of water effect, graphite powder is hit by high voltage pulse water jet, simultaneously under the effect of turbulent flow and cavitation so that graphite powder is pulverized and peeled off, through filtering, drying, obtain the number of plies finely dispersed graphene microchip at 100-300 layer.
Embodiment 3
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip:
(1) by graphite powder heat pre-treatment 30min at heating-up temperature is 200 DEG C that weight portion is 93, then it is the ethanol of 1.6 by graphite powder and weight portion, weight portion be 1.1 PTPP and the high-speed mixer that adds of water that weight portion is 8000 in, adition process stirs with rotating speed 400rpm simultaneously, mixing time 3min, obtains the graphite powder aqueous solution；
(2) graphite powder aqueous solution step (1) obtained is sent in closed reactor, and under pressure is 16MPa, pressurize intercalation embrittlement 6h by graphite powder, weakens graphite powder interlayer Van der Waals force, obtains pretreating graphite amidin；
(3) pretreating graphite amidin step (2) obtained is sent in high voltage pulse water jet mill, the rotated joint of high voltage pulse water jet, by nozzle directive graphite powder, under buoyancy of water effect, graphite powder is hit by high voltage pulse water jet, simultaneously under the effect of turbulent flow and cavitation so that graphite powder is pulverized and peeled off, through filtering, drying, obtain the number of plies finely dispersed graphene microchip at 100-300 layer.
Embodiment 4
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip:
(1) by graphite powder heat pre-treatment 25min at heating-up temperature is 190 DEG C that weight portion is 94, then it is the ethanol of 1.4 by graphite powder and weight portion, weight portion be 0.9 PTPP and the high-speed mixer that adds of water that weight portion is 600 in, adition process stirs with rotating speed 420rpm simultaneously, mixing time 3min, obtains the graphite powder aqueous solution；
(2) graphite powder aqueous solution step (1) obtained is sent in closed reactor, and under pressure is 18MPa, pressurize intercalation embrittlement 5h by graphite powder, weakens graphite powder interlayer Van der Waals force, obtains pretreating graphite amidin；
(3) pretreating graphite amidin step (2) obtained is sent in high voltage pulse water jet mill, the rotated joint of high voltage pulse water jet, by nozzle directive graphite powder, under buoyancy of water effect, graphite powder is hit by high voltage pulse water jet, simultaneously under the effect of turbulent flow and cavitation so that graphite powder is pulverized and peeled off, through filtering, drying, obtain the number of plies finely dispersed graphene microchip at 100-300 layer.
Embodiment 5
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip:
(1) by graphite powder heat pre-treatment 30min at heating-up temperature is 200 DEG C that weight portion is 92, then it is the ethanol of 1.8 by graphite powder and weight portion, weight portion be 1.3 PTPP and the high-speed mixer that adds of water that weight portion is 800 in, adition process stirs with rotating speed 450rpm simultaneously, mixing time 3min, obtains the graphite powder aqueous solution；
(2) graphite powder aqueous solution step (1) obtained is sent in closed reactor, and under pressure is 20MPa, pressurize intercalation embrittlement 8h by graphite powder, weakens graphite powder interlayer Van der Waals force, obtains pretreating graphite amidin；
(3) pretreating graphite amidin step (2) obtained is sent in high voltage pulse water jet mill, the rotated joint of high voltage pulse water jet, by nozzle directive graphite powder, under buoyancy of water effect, graphite powder is hit by high voltage pulse water jet, simultaneously under the effect of turbulent flow and cavitation so that graphite powder is pulverized and peeled off, through filtering, drying, obtain the number of plies finely dispersed graphene microchip at 100-300 layer.
Claims (5)
1. one kind utilizes the method that high voltage pulse water jet mill prepares graphene microchip, it is characterized in that: by pressurization intercalation, weaken graphite powder interlayer Van der Waals force, then the leap high high voltage pulse water jet of pressure water jet pulverizer of passages through which vital energy circulates makes graphite powder pulverize stripping under the effect of water jet, turbulent flow and cavitation, obtaining the number of plies finely dispersed graphene microchip at 100-200 layer, concrete grammar is as follows:
(1) by graphite powder heat pre-treatment 20min-40min at heating-up temperature is 180 DEG C-220 DEG C that weight portion is 90-98, then it is the ethanol of 0.5-2.0 by graphite powder and weight portion, in the high-speed mixer that weight portion is the PTPP of 0.4-1.5 and water that weight portion is 500-1000 adds, adition process stirs with rotating speed 360rpm-480rpm simultaneously, mixing time 3min, obtains the graphite powder aqueous solution；
(2) graphite powder aqueous solution step (1) obtained is sent in closed reactor, and under pressure is 10MPa-25MPa, pressurize intercalation embrittlement 4h-10h by graphite powder, weakens graphite powder interlayer Van der Waals force, obtains pretreating graphite amidin；
(3) pretreating graphite amidin step (2) obtained is sent in high voltage pulse water jet mill, the rotated joint of high voltage pulse water jet, by nozzle directive graphite powder, under buoyancy of water effect, graphite powder is hit by high voltage pulse water jet, simultaneously under the effect of turbulent flow and cavitation so that graphite powder is pulverized and peeled off, through filtering, drying, obtain the number of plies finely dispersed graphene microchip at 100-300 layer.
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip, it is characterised in that: described graphite powder is any one in expanded graphite, thermal cracking graphite, and particle diameter is between 0.5mm and 5mm.
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip, it is characterised in that: described high voltage pulse water jet mill work water pressure is 10-60MPa, and pulse frequency is 20-50Hz.
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip, it is characterized in that: described nozzle is round mouth nozzle, nozzle diameter is between 8mm and 20mm, the work angle of nozzle is between 30 ° and 60 °, nozzle quantity at least one, when having two and with top nozzle, both can work between nozzle, it is also possible to alternation simultaneously.
A kind of method utilizing high voltage pulse water jet mill to prepare graphene microchip, it is characterised in that: graphene microchip prepared by described method meets in rubber reinforcement, plastics enhancing, anticorrosion with coat, lubrication, the application of sewage treatment area.
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Cited By (7)
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| CN106448926A (en) * | 2016-10-26 | 2017-02-22 | 成都新柯力化工科技有限公司 | Preparation method of graphene conductive paste special for lithium battery |
| CN107698772A (en) * | 2017-10-17 | 2018-02-16 | 成都新柯力化工科技有限公司 | A kind of method of the branched enhancing regenerated plastics in original position |
| CN107915218A (en) * | 2016-10-09 | 2018-04-17 | 汪又翔 | Hybrid nappe flip length graphite produces graphene |
| CN107973292A (en) * | 2016-10-24 | 2018-05-01 | 林逸樵 | A kind of devices and methods therefor for producing graphene |
| TWI625299B (en) * | 2017-01-24 | 2018-06-01 | Apparatus for producing graphene and method thereof | |
| CN108126808A (en) * | 2017-11-21 | 2018-06-08 | 包头稀土研究院 | High pressure liquid stream fuel pulverizing plant and its milling method |
| CN114832928A (en) * | 2022-07-02 | 2022-08-02 | 江苏秦烯新材料有限公司 | Pulsed intelligent breaker of high-purity phosphorus |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107915218A (en) * | 2016-10-09 | 2018-04-17 | 汪又翔 | Hybrid nappe flip length graphite produces graphene |
| CN107973292A (en) * | 2016-10-24 | 2018-05-01 | 林逸樵 | A kind of devices and methods therefor for producing graphene |
| CN106448926A (en) * | 2016-10-26 | 2017-02-22 | 成都新柯力化工科技有限公司 | Preparation method of graphene conductive paste special for lithium battery |
| CN106448926B (en) * | 2016-10-26 | 2018-01-23 | 广州天镒研磨材料有限公司 | A kind of preparation method of lithium battery special graphite alkene electrocondution slurry |
| TWI625299B (en) * | 2017-01-24 | 2018-06-01 | Apparatus for producing graphene and method thereof | |
| CN107698772A (en) * | 2017-10-17 | 2018-02-16 | 成都新柯力化工科技有限公司 | A kind of method of the branched enhancing regenerated plastics in original position |
| CN107698772B (en) * | 2017-10-17 | 2018-10-09 | 浙江中邦塑胶股份有限公司 | A kind of method of the branched enhancing regenerated plastics in original position |
| CN108126808A (en) * | 2017-11-21 | 2018-06-08 | 包头稀土研究院 | High pressure liquid stream fuel pulverizing plant and its milling method |
| CN114832928A (en) * | 2022-07-02 | 2022-08-02 | 江苏秦烯新材料有限公司 | Pulsed intelligent breaker of high-purity phosphorus |
| CN114832928B (en) * | 2022-07-02 | 2022-12-09 | 江苏秦烯新材料有限公司 | Pulsed intelligent breaker of high-purity phosphorus |
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