CN108117069B - Concentration method and device for large graphene oxide solution - Google Patents
Concentration method and device for large graphene oxide solution Download PDFInfo
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- CN108117069B CN108117069B CN201810061945.2A CN201810061945A CN108117069B CN 108117069 B CN108117069 B CN 108117069B CN 201810061945 A CN201810061945 A CN 201810061945A CN 108117069 B CN108117069 B CN 108117069B
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- C01—INORGANIC CHEMISTRY
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The invention discloses a method and a system for concentrating a large graphene oxide solution. According to the invention, a large graphene oxide solution flows through a limited space and is rapidly sheared, so that the graphene oxide is coagulated. The final concentration of the precipitated graphene oxide was 60-100mg/mL after collection by filtration. The coagulated graphene oxide is stretched and recovered to a uniform morphological structure under slow shearing, and is well dispersed in a solution. The method can be used for rapid and continuous concentration of the graphene oxide solution.
Description
Technical Field
The invention relates to a concentration method of a two-dimensional material, in particular to a concentration method and a concentration device of a large graphene oxide solution.
Background
In 2010, the stable graphene was first isolated by professor Andre Geim. The graphene has excellent electrical properties (the electron mobility can reach 2 multiplied by 10 at room temperature)5cM2Vs), outstanding thermal conductivity (5000W/(MK), extraordinary specific surface area (2630M)2In g), its Young's modulus (1100GPa) and breaking strength (125 GPa). The excellent electric and heat conducting performance of the graphene completely exceeds that of metal, meanwhile, the graphene has the advantages of high temperature resistance and corrosion resistance, and the good mechanical property and the low density of the graphene enable the graphene to have the potential of being applied in various fields.
Graphene oxide is the most important precursor of graphene, and has excellent physicochemical properties. However, graphene oxide is generally present in the form of a low concentration dispersion, and the concentration process thereof remains a challenge. Generally, high-concentration graphene oxide is obtained by high-speed centrifugation of a graphene oxide solution, and the method needs a high-speed centrifuge, has long centrifugation time and poor centrifugation effect (centrifugation is carried out for 1 hour, and the concentration is 20-40 mg/mL). The limited shear reported to date requires the addition of metal salts, which have changed the original purpose of concentration. Therefore, a limited shearing method is invented, so that the graphene oxide is subjected to coagulation, and the graphene oxide concentrated solution is obtained after simple centrifugation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method and a device for concentrating a large graphene oxide solution.
The purpose of the invention is realized by the following technical scheme: a concentration method of a large graphene oxide solution is provided, wherein the size of graphene oxide is larger than 3um, and the concentration method comprises the following steps: enabling the graphene oxide solution to flow through a slit at a speed of 20-100m/s for shearing, wherein the flow time is 1-2 minutes, and the graphene oxide is subjected to coagulation; then dehydrating by a cloth bag centrifuge to obtain precipitated graphene oxide, and finishing concentration; one dimension of the cross section of the slit is smaller than 10 um.
Further, the centrifugal force of the cloth bag centrifuge is 6000-.
Further, one dimension of the cross section of the slit is not more than 1 um.
A concentration system of a large graphene oxide solution comprises a shearing device and a dehydration device, wherein the shearing device is a mold provided with a slit with the size smaller than 10um, and graphene oxide is subjected to coagulation after the graphene oxide solution to be concentrated flows through the slit at the speed of 20-100 m/s; and dehydrating by a dehydrating device to obtain the precipitated graphene oxide, and finishing concentration.
Further, the device also comprises a flow rate controller for controlling the flow rate of the graphene oxide solution.
The invention has the beneficial effects that: according to the invention, the high-concentration graphene oxide dispersion liquid is obtained by a mode of limited shearing and bag centrifugation combination. The limited shearing can lead the graphene oxide to be gathered, precipitated and separated out at a lower shearing rate in a shorter time, and the separated graphene oxide is agglomerated together to form a large granular object which is not easy to block holes. And then dewatering by a cloth bag centrifuge to obtain the graphene oxide concentrated solution. The graphene oxide particles have relatively large diameters, have certain rigidity, are not easy to block holes, and are beneficial to the centrifugation of a cloth bag centrifuge.
Drawings
Fig. 1 is the state of graphene oxide before and after limited shear.
Fig. 2 is a schematic view of a shearing apparatus of the present invention.
Detailed Description
The invention is further described with reference to the following figures and examples. The present invention is further illustrated by the following examples, which are not to be construed as limiting the scope of the invention, and the non-essential changes and modifications thereof by those skilled in the art can be made without departing from the spirit and scope of the invention.
Example 1:
(1) a4 mg/mL large-size graphene oxide aqueous solution was injected into the slit of the shearing apparatus shown in FIG. 2 at 20m/s, the height of the slit was 1um, and the shearing was performed for 2 min. After shearing, the graphene oxide is coagulated, as shown in fig. 1b, and it can be seen that the graphene oxide aggregates have a diameter of millimeter.
(2) Then dehydrating by using a cloth bag centrifuge (centrifugal force 6000XG) to obtain a graphene oxide concentrated solution with the concentration of 60mg/mL, as shown in figure 1 c;
after the graphene oxide concentrate is redispersed in water, the original highly dispersed state of graphene oxide is maintained, as shown in fig. 1 d.
Example 2:
(1) a large-size graphene oxide aqueous solution of 3mg/mL was injected into the slit of the shearing apparatus shown in FIG. 2 at 100m/s, the height of the slit was 10um, and the shearing was performed for 2 min. After shearing, the graphene oxide is coagulated, and the graphene oxide aggregate has a millimeter-sized diameter.
(2) Then dehydrating by using a cloth bag centrifuge (centrifugal force 17000XG) to obtain a graphene oxide concentrated solution with the concentration of 100 mg/mL;
and re-dispersing the graphene oxide concentrated solution in water, and keeping the original highly dispersed state of the graphene oxide.
Example 3:
(1) a large-size graphene oxide aqueous solution of 5mg/mL was injected at 40m/s into the slit of the shearing apparatus shown in FIG. 2, the height of the slit was 4um, and the shearing was performed for 1.5 min. After shearing, the graphene oxide is coagulated, and the graphene oxide aggregate has a millimeter-sized diameter.
(2) Then dehydrating by using a cloth bag centrifuge (centrifugal force 12000XG) to obtain an oxidized graphene concentrated solution with the concentration of 80 mg/mL;
and re-dispersing the graphene oxide concentrated solution in water, and keeping the original highly dispersed state of the graphene oxide.
Example 4:
(1) a large-size graphene oxide aqueous solution of 6mg/mL was injected at 70m/s into the slit of the shearing apparatus shown in FIG. 2, the height of the slit was 1um, and the shearing was performed for 1 min. After shearing, the graphene oxide is coagulated, and the graphene oxide aggregate has a millimeter-sized diameter.
(2) Then dehydrating by using a cloth bag centrifuge (centrifugal force 10000xG) to obtain a graphene oxide concentrated solution with the concentration of 90 mg/mL;
and re-dispersing the graphene oxide concentrated solution in water, and keeping the original highly dispersed state of the graphene oxide.
Example 5:
(1) 4mg/mL of a large-size graphene oxide aqueous solution was injected into the slit of the shearing apparatus shown in FIG. 2 at 40m/s, the height of the slit was 6um, and shearing was performed for 1 min. After shearing, the graphene oxide is coagulated, and the graphene oxide aggregate has a millimeter-sized diameter.
(2) Then dehydrating by using a cloth bag centrifuge (centrifugal force 9000xG) to obtain a graphene oxide concentrated solution with the concentration of 60 mg/mL;
and re-dispersing the graphene oxide concentrated solution in water, and keeping the original highly dispersed state of the graphene oxide.
Claims (4)
1. A concentration method of a large graphene oxide solution, wherein the size of graphene oxide is larger than 3 μm, is characterized in that the concentration method comprises the following steps: enabling the graphene oxide solution to flow through a slit at a speed of 20-100m/s for shearing, wherein the flow time is 1-2 minutes, the graphene oxide is subjected to coagulation, and a graphene oxide aggregate formed after the coagulation has a millimeter-scale diameter; then dehydrating by a cloth bag centrifuge to obtain precipitated graphene oxide, and finishing concentration; one dimension of the cross section of the slit is not more than 10 μm.
2. The method of claim 1, wherein the cross-section of the slit has one dimension no greater than 1 μm.
3. The concentration system of the large graphene oxide solution is characterized by comprising a shearing device and a dehydration device, wherein the shearing device is a die provided with a slit, and one dimension of the cross section of the slit is not more than 10 microns; after the graphene oxide solution to be concentrated flows through the slit at the speed of 20-100m/s, the graphene oxide is subjected to coagulation; then dehydrating by a dehydrating device to obtain precipitated graphene oxide, and finishing concentration; wherein the size of the graphene oxide is larger than 3 μm.
4. The concentration system of claim 3, further comprising a flow rate controller for controlling a flow rate of the graphene oxide solution.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017035193A1 (en) * | 2015-08-24 | 2017-03-02 | Northwestern University | Methods for preparation of concentrated graphene ink compositions and related composite materials |
| WO2017167941A1 (en) * | 2016-03-31 | 2017-10-05 | Total Research & Technology Feluy | Process for the preparation of carbon fibers precursor or carbon slit tapes precursor |
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| KR101910976B1 (en) * | 2012-07-16 | 2018-10-23 | 삼성전자주식회사 | Field effect transistor using graphene |
| CN105293476B (en) * | 2015-11-16 | 2018-07-10 | 复旦大学 | A kind of preparation method of large scale graphene oxide or graphene |
| CN106185895A (en) * | 2016-07-06 | 2016-12-07 | 青岛华高墨烯科技股份有限公司 | A kind of graphene dispersion liquid and preparation method thereof |
| CN106587027A (en) * | 2017-01-05 | 2017-04-26 | 苏州高通新材料科技有限公司 | Method for rapidly preparing small-dimensional graphene |
| CN106915741A (en) * | 2017-04-11 | 2017-07-04 | 深圳市佩成科技有限责任公司 | The preparation method of improved graphene oxide |
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| WO2017035193A1 (en) * | 2015-08-24 | 2017-03-02 | Northwestern University | Methods for preparation of concentrated graphene ink compositions and related composite materials |
| WO2017167941A1 (en) * | 2016-03-31 | 2017-10-05 | Total Research & Technology Feluy | Process for the preparation of carbon fibers precursor or carbon slit tapes precursor |
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