CN109553094A - A kind of grapheme platelet liquid phase ultrasonic dispersing method - Google Patents
A kind of grapheme platelet liquid phase ultrasonic dispersing method Download PDFInfo
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- CN109553094A CN109553094A CN201910003784.6A CN201910003784A CN109553094A CN 109553094 A CN109553094 A CN 109553094A CN 201910003784 A CN201910003784 A CN 201910003784A CN 109553094 A CN109553094 A CN 109553094A
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- ultrasonic
- grapheme platelet
- grapheme
- ultrasonic wave
- platelet
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- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000007791 liquid phase Substances 0.000 title claims abstract description 24
- 239000006185 dispersion Substances 0.000 claims abstract description 41
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 239000003054 catalyst Substances 0.000 claims abstract description 29
- 238000006213 oxygenation reaction Methods 0.000 claims abstract description 29
- 239000002002 slurry Substances 0.000 claims abstract description 25
- 239000007900 aqueous suspension Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 19
- 238000004806 packaging method and process Methods 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 5
- 238000002604 ultrasonography Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 238000005057 refrigeration Methods 0.000 claims description 2
- 239000006228 supernatant Substances 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 4
- 239000004575 stone Substances 0.000 claims 2
- 238000004108 freeze drying Methods 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 2
- 229910021389 graphene Inorganic materials 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000013019 agitation Methods 0.000 description 3
- 239000007770 graphite material Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- -1 graphite alkene Chemical class 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
Abstract
The invention discloses a kind of grapheme platelet liquid phase ultrasonic dispersing methods, comprising the following steps: S1, grapheme platelet slurry and deionized water are mixed in liquid stirrers, obtain diluted grapheme platelet aqueous suspension liquid；S2, grapheme platelet aqueous suspension liquid is sent into ultrasonic wave dispersion bottle, and carries out surface with the oxygenation catalyst in ultrasonic wave dispersion bottle and contacts；S3, starting ultrasonic wave stick and refrigerator, grapheme platelet aqueous suspension liquid carry out ultrasonic disperse, and refrigerator controls the temperature in ultrasonic wave dispersion bottle；Grapheme platelet aqueous suspension liquid discharge after S4, ultrasonic disperse, send into vacuum freeze drier vacuum freeze drying, packaging facilities is escaped and enter after vacuum freeze drying, i.e. the dispersion of completion grapheme platelet liquid phase ultrasonic.Dispersing method proposed by the present invention increases the chance at grapheme platelet edge and carboxyl group combination, improves dispersion effect, reduce energy consumption, shortens jitter time.
Description
Technical field
The present invention relates to graphene production technical field more particularly to a kind of grapheme platelet liquid phase ultrasonic dispersion sides
Method.
Background technique
Graphene is the two dimension crystalline substance for the only one layer atomic thickness for being stripped out from graphite material, being made of carbon atom
Body, application are paid close attention to by the whole world, however at present for the research of graphene, also in the starting stage.Graphite material is by stripping
Grapheme platelet is prepared into from after, the grapheme platelet after removing can not directly carry out the processing in downstream, it usually needs pass through again
Dispersion step is crossed, to improve the dispersion performance of grapheme platelet, the grapheme platelet appearance after a period of time stores is avoided to roll into a ball again
Poly- phenomenon loses the function of graphene.Currently used graphene dispersion method is mainly to utilize surpassing for ultrasonic device generation
The bubble that sound wave generates inside liquid energy caused by closure moment comes dispersed graphite alkene small pieces, most of ultrasound wavelength-division
Scattered process is required using multiple ultrasonic wave bottles, and each ultrasonic wave bottle is required with ultrasonic waves more than 15000 watts of power
Stick is run more than 20 hours, therefore energy consumption and time are longer, so that the production cycle of grapheme platelet extends, production
Cost improves, and is not suitable for the industrialized production of graphene.Based on this, the present invention proposes that one kind is easy to operate, production cost is low
Grapheme platelet liquid phase ultrasonic dispersing method.
Summary of the invention
The purpose of the present invention is to solve disadvantages existing in the prior art, and a kind of grapheme platelet liquid phase proposed
Ultrasonic scattering method.
A kind of grapheme platelet liquid phase ultrasonic dispersing method, comprising the following steps:
S1, mixing: grapheme platelet slurry and deionized water being added in liquid stirrers, and are mixed,
Obtain diluted grapheme platelet aqueous suspension liquid；
S2, the contact of oxygenation catalyst: the grapheme platelet aqueous suspension liquid that step S1 is mixed to get is sent into ultrasonic wave dispersion
In bottle, and surface is carried out with the oxygenation catalyst in ultrasonic wave dispersion bottle and is contacted；
S3, ultrasonic disperse: starting ultrasonic wave stick and refrigerator, the grapheme platelet aqueous suspension liquid after oxygenation catalyst
Ultrasonic disperse is carried out under the action of ultrasonic wave stick again, the temperature in ultrasonic procedure in refrigerator control ultrasonic wave dispersion bottle is 55
~65 DEG C；
S4, vacuum freeze drying: the grapheme platelet aqueous suspension liquid discharge after ultrasonic disperse, and it is sent to vacuum refrigeration
In drying machine, vacuum freeze drying is carried out, escapes and enter packaging facilities after vacuum freeze drying, is i.e. completion graphene is small
The dispersion of piece liquid phase ultrasonic.
Preferably, the number of plies of the grapheme platelet slurry is 10 layers or less.
Preferably, the volume ratio of the grapheme platelet slurry and deionized water is 1~2000:10000.
Preferably, the time of the mixing is stirred according to every 10kg object to be mixed with the liquid stirrers of 1.5KW power
30~90s is mixed, the object to be mixed is the summation of grapheme platelet slurry and deionized water.
Preferably, the upper surface diameter of the oxygenation catalyst and ultrasonic wave dispersion bottle intake port ratio be 2~
4:1, the distance of the oxygenation catalyst to ultrasonic wave dispersion bottle feed inlet and the ratio of ultrasonic wave dispersion bottle intake port are
0.75~1.5:1.
Preferably, the time of the ultrasonic disperse waits for ultrasonic wave stick (6) ultrasound point of ultrasonic object 2W power according to 10kg
Dissipate 1~2h, it is described to ultrasonic object be grapheme platelet slurry and deionized water summation.
Preferably, the negative pressure of vacuum of the vacuum freeze drying is -20~-150Pa, and cryogenic temperature is -30~-60 DEG C.
Compared with prior art, the invention has the benefit that
1, the equipment that the present invention increases oxygenation catalyst in ultrasonic wave dispersion bottle makes ultrasound to enhance the effect of ultrasonic wave
Wavelength-division dissipates the boundary for reaching optimal ultrasonic wave dispersion；
2, by oxygenation catalyst and high-temperature process ultrasonic wave process match in the way of, more oxygen are dissolved in graphene
In small pieces aqueous suspension liquid, the chance at grapheme platelet edge and carboxyl group combination is considerably increased, compared to traditional ultrasound
Method, it is more energy efficient, faster；
3, dispersing method proposed by the present invention greatly subtracts compared to the energy needed for traditional ultrasonic wave dispersion and time
It is few, and the effect dispersed than other it is more longlasting more have legs, 2/3 can be reduced by measuring energy consumption through test, and shorten dispersion
Time.
Detailed description of the invention
Fig. 1 is a kind of flow chart of grapheme platelet liquid phase ultrasonic dispersing method proposed by the present invention.
In figure, 1, deionized water, 2, grapheme platelet slurry, 3, grapheme platelet aqueous suspension liquid, 4, ultrasonic wave dispersion
Bottle, 5, oxygenation catalyst, 6, ultrasonic wave stick, 7, refrigerator, 8, vacuum freeze drier, 9, packaging facilities.
Specific embodiment
Referring to Fig.1, combined with specific embodiments below the present invention is made further to explain.
Embodiment one
A kind of grapheme platelet liquid phase ultrasonic dispersing method proposed by the present invention, comprising the following steps:
S1, mixing: grapheme platelet slurry 2 and deionized water 1 are added to liquid according to volume ratio for 1500:10000
In blender, and be mixed, time of mixing according to every 10kg object to be mixed 1.5KW power liquid agitation
Machine stirs 60s, and the object to be mixed is the summation of grapheme platelet slurry 2 and deionized water 1, obtains diluted grapheme platelet
Aqueous suspension liquid 3；
S2, the contact of oxygenation catalyst: the grapheme platelet aqueous suspension liquid 3 that step S1 is mixed to get is sent into ultrasonic wave dispersion
In bottle 4, and surface is carried out with the oxygenation catalyst 5 in ultrasonic wave dispersion bottle 4 and is contacted；
S3, ultrasonic disperse: starting ultrasonic wave stick 6 and refrigerator 7, the grapheme platelet aqueous suspension after oxygenation catalyst 5
Liquid 3 carries out ultrasonic disperse under the action of ultrasonic wave stick 6 again, and the time of ultrasonic disperse waits for ultrasonic object 2W power according to 10kg
Ultrasonic wave stick 6 ultrasonic disperse 1.5h, described is the summation of grapheme platelet slurry 2 and deionized water 1 to ultrasonic object, in ultrasonic mistake
The temperature that refrigerator 7 controls in ultrasonic wave dispersion bottle 4 in journey is 60 DEG C；
S4, vacuum freeze drying: the grapheme platelet aqueous suspension liquid 3 after ultrasonic disperse is discharged, and it is cold to be sent to vacuum
In lyophilizer 8, vacuum freeze drying is carried out, the negative pressure of vacuum of vacuum freeze drying is -70Pa, and cryogenic temperature is -50 DEG C, very
Packaging facilities 9 is escaped and enter after vacuum freecing-dry, i.e. the dispersion of completion grapheme platelet liquid phase ultrasonic.
In the present invention, the number of plies of grapheme platelet slurry 2 is 9 layers；The upper surface diameter and ultrasonic wave of oxygenation catalyst 5 disperse
The ratio of the intake port of bottle 4 is 3:1, the distance and ultrasonic wavelength-division of the oxygenation catalyst 5 to ultrasonic wave dispersion 4 feed inlet of bottle
The ratio for dissipating 4 intake port of bottle is 1:1.
Embodiment two
A kind of grapheme platelet liquid phase ultrasonic dispersing method proposed by the present invention, comprising the following steps:
S1, mixing: grapheme platelet slurry 2 and deionized water 1 are added to liquid according to volume ratio for 2000:10000
In blender, and be mixed, time of mixing according to every 10kg object to be mixed 1.5KW power liquid agitation
Machine stirs 90s, and the object to be mixed is the summation of grapheme platelet slurry 2 and deionized water 1, obtains diluted grapheme platelet
Aqueous suspension liquid 3；
S2, the contact of oxygenation catalyst: the grapheme platelet aqueous suspension liquid 3 that step S1 is mixed to get is sent into ultrasonic wave dispersion
In bottle 4, and surface is carried out with the oxygenation catalyst 5 in ultrasonic wave dispersion bottle 4 and is contacted；
S3, ultrasonic disperse: starting ultrasonic wave stick 6 and refrigerator 7, the grapheme platelet aqueous suspension after oxygenation catalyst 5
Liquid 3 carries out ultrasonic disperse under the action of ultrasonic wave stick 6 again, and the time of ultrasonic disperse waits for ultrasonic object 2W power according to 10kg
Ultrasonic wave stick 6 ultrasonic disperse 1h, described is the summation of grapheme platelet slurry 2 and deionized water 1 to ultrasonic object, in ultrasonic procedure
The temperature that middle refrigerator 7 controls in ultrasonic wave dispersion bottle 4 is 60 DEG C；
S4, vacuum freeze drying: the grapheme platelet aqueous suspension liquid 3 after ultrasonic disperse is discharged, and it is cold to be sent to vacuum
In lyophilizer 8, vacuum freeze drying is carried out, the negative pressure of vacuum of vacuum freeze drying is -150Pa, and cryogenic temperature is -60 DEG C,
Packaging facilities 9 is escaped and enter after vacuum freeze drying, i.e. the dispersion of completion grapheme platelet liquid phase ultrasonic.
In the present invention, the number of plies of grapheme platelet slurry 2 is 6 layers；The upper surface diameter and ultrasonic wave of oxygenation catalyst 5 disperse
The ratio of the intake port of bottle 4 is 4:1, the distance and ultrasonic wavelength-division of the oxygenation catalyst 5 to ultrasonic wave dispersion 4 feed inlet of bottle
The ratio for dissipating 4 intake port of bottle is 0.75:1.
Embodiment three
A kind of grapheme platelet liquid phase ultrasonic dispersing method proposed by the present invention, comprising the following steps:
S1, mixing: grapheme platelet slurry 2 and deionized water 1 are added to liquid agitation according to volume ratio for 1:10000
It in machine, and is mixed, the time of mixing is stirred according to every 10kg object to be mixed with the liquid stirrers of 1.5KW power
30s is mixed, the object to be mixed is the summation of grapheme platelet slurry 2 and deionized water 1, and it is outstanding to obtain diluted grapheme platelet water
Supernatant liquid body 3；
S2, the contact of oxygenation catalyst: the grapheme platelet aqueous suspension liquid 3 that step S1 is mixed to get is sent into ultrasonic wave dispersion
In bottle 4, and surface is carried out with the oxygenation catalyst 5 in ultrasonic wave dispersion bottle 4 and is contacted；
S3, ultrasonic disperse: starting ultrasonic wave stick 6 and refrigerator 7, the grapheme platelet aqueous suspension after oxygenation catalyst 5
Liquid 3 carries out ultrasonic disperse under the action of ultrasonic wave stick 6 again, and the time of ultrasonic disperse waits for ultrasonic object 2W power according to 10kg
Ultrasonic wave stick 6 ultrasonic disperse 2h, described is the summation of grapheme platelet slurry 2 and deionized water 1 to ultrasonic object, in ultrasonic procedure
The temperature that middle refrigerator 7 controls in ultrasonic wave dispersion bottle 4 is 55 DEG C；
S4, vacuum freeze drying: the grapheme platelet aqueous suspension liquid 3 after ultrasonic disperse is discharged, and it is cold to be sent to vacuum
In lyophilizer 8, vacuum freeze drying is carried out, the negative pressure of vacuum of vacuum freeze drying is -20Pa, and cryogenic temperature is -30 DEG C, very
Packaging facilities 9 is escaped and enter after vacuum freecing-dry, i.e. the dispersion of completion grapheme platelet liquid phase ultrasonic.
In the present invention, the number of plies of grapheme platelet slurry 2 is 8 layers；The upper surface diameter and ultrasonic wave of oxygenation catalyst 5 disperse
The ratio of the intake port of bottle 4 is 2:1, the distance and ultrasonic wavelength-division of the oxygenation catalyst 5 to ultrasonic wave dispersion 4 feed inlet of bottle
The ratio for dissipating 4 intake port of bottle is 1.5:1.
Same batch grapheme platelet slurry is taken, above-described embodiment one, embodiment two, embodiment three are utilized respectively and is passed
The ultra-sonic dispersion method of system carries out decentralized processing, calculates energy consumption, and by the energy consumption of embodiment one, embodiment two and embodiment three with
The energy consumption of traditional ultra-sonic dispersion method is compared, as a result as follows:
| Embodiment one | Embodiment two | Embodiment three | |
| Energy consumption variation | - 71.8% | - 68.1% | - 70.6% |
In table, "-" indicates to reduce compared to traditional ultra-sonic dispersion method energy consumption.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of grapheme platelet liquid phase ultrasonic dispersing method, which comprises the following steps:
S1, mixing: grapheme platelet slurry (2) and deionized water (1) are added in liquid stirrers, and are carried out mixing and stirred
It mixes, obtains diluted grapheme platelet aqueous suspension liquid (3)；
S2, the contact of oxygenation catalyst: the grapheme platelet aqueous suspension liquid (3) that step S1 is mixed to get is sent into ultrasonic wave dispersion bottle
(4) in, and surface contact is carried out with the oxygenation catalyst (5) in ultrasonic wave dispersion bottle (4)；
S3, ultrasonic disperse: starting ultrasonic wave stick (6) and refrigerator (7), the grapheme platelet water after oxygenation catalyst (5) are outstanding
Supernatant liquid body (3) carries out ultrasonic disperse under the action of ultrasonic wave stick (6) again, and refrigerator (7) controls ultrasonic wavelength-division in ultrasonic procedure
Dissipating the temperature in bottle (4) is 55~65 DEG C；
S4, vacuum freeze drying: grapheme platelet aqueous suspension liquid (3) discharge after ultrasonic disperse, and it is sent to vacuum refrigeration
In drying machine (8), vacuum freeze drying is carried out, escapes and enter packaging facilities (9) after vacuum freeze drying, is i.e. completion stone
Black alkene small pieces liquid phase ultrasonic dispersion.
2. a kind of grapheme platelet liquid phase ultrasonic dispersing method according to claim 1, which is characterized in that the graphite
The number of plies of alkene small pieces slurry (2) is 10 layers or less.
3. a kind of grapheme platelet liquid phase ultrasonic dispersing method according to claim 1, which is characterized in that the graphite
The volume ratio of alkene small pieces slurry (2) and deionized water (1) is 1~2000:10000.
4. a kind of grapheme platelet liquid phase ultrasonic dispersing method according to claim 1, which is characterized in that the mixing
The time of stirring stirs 30~90s according to the liquid stirrers of every 10kg object to be mixed 1.5KW power, and the object to be mixed is
The summation of grapheme platelet slurry (2) and deionized water (1).
5. a kind of grapheme platelet liquid phase ultrasonic dispersing method according to claim 1, which is characterized in that the oxygenation
The ratio of the intake port of upper surface diameter and the ultrasonic wave dispersion bottle (4) of catalyst (5) is 2~4:1, the oxygenation catalyst
(5) it is 0.75~1.5 to the ratio of the distance of ultrasonic wave dispersion bottle (4) feed inlet and ultrasonic wave dispersion bottle (4) intake port:
1。
6. a kind of grapheme platelet liquid phase ultrasonic dispersing method according to claim 1, which is characterized in that the ultrasound
The time of dispersion waits for ultrasonic wave stick (6) 1~2h of ultrasonic disperse of ultrasonic object 2W power according to 10kg, and described to ultrasonic object is stone
The summation of black alkene small pieces slurry (2) and deionized water (1).
7. a kind of grapheme platelet liquid phase ultrasonic dispersing method according to claim 1, which is characterized in that the vacuum
The negative pressure of vacuum of freeze-drying is -20~-150Pa, and cryogenic temperature is -30~-60 DEG C.
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| US20180261402A1 (en) * | 2015-09-18 | 2018-09-13 | Toray Industries, Inc. | Graphene dispersion, process for producing same, process for producing particles of graphene/active material composite, and process for producing electrode paste |
| CN109107528A (en) * | 2018-08-23 | 2019-01-01 | 中国船舶重工集团公司第七二五研究所 | A kind of preparation method of graphene-supported nickel magnetic composite |
-
2019
- 2019-01-03 CN CN201910003784.6A patent/CN109553094A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170050854A1 (en) * | 2014-05-01 | 2017-02-23 | Rmit University | Graphene production process |
| CN104387446A (en) * | 2014-10-11 | 2015-03-04 | 中国石油大学(华东) | Preparation methods of graphene dispersant and graphene dispersion liquid |
| CN104843688A (en) * | 2015-04-20 | 2015-08-19 | 德阳烯碳科技有限公司 | Graphene preparation method |
| US20180261402A1 (en) * | 2015-09-18 | 2018-09-13 | Toray Industries, Inc. | Graphene dispersion, process for producing same, process for producing particles of graphene/active material composite, and process for producing electrode paste |
| CN106276874A (en) * | 2016-08-10 | 2017-01-04 | 安徽省宁国天成电工有限公司 | A kind of preparation method of heater Graphene |
| CN107857257A (en) * | 2017-11-23 | 2018-03-30 | 深圳市大族元亨光电股份有限公司 | The preparation method of single-layer graphene dispersion liquid |
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