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CN113274763A - Method and device for concentrating graphene oxide dispersion liquid - Google Patents

Method and device for concentrating graphene oxide dispersion liquid Download PDF

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Publication number
CN113274763A
CN113274763A CN202110652115.9A CN202110652115A CN113274763A CN 113274763 A CN113274763 A CN 113274763A CN 202110652115 A CN202110652115 A CN 202110652115A CN 113274763 A CN113274763 A CN 113274763A
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CN
China
Prior art keywords
graphene oxide
oxide dispersion
dispersion liquid
concentration
water
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CN202110652115.9A
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Chinese (zh)
Inventor
杜鸿达
陈威
褚晓东
康飞宇
李宝华
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Shenzhen International Graduate School of Tsinghua University
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Shenzhen International Graduate School of Tsinghua University
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Priority to CN202110652115.9A priority Critical patent/CN113274763A/en
Publication of CN113274763A publication Critical patent/CN113274763A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D15/00Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08Selective adsorption, e.g. chromatography

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Carbon And Carbon Compounds (AREA)

Abstract

A method for concentrating a graphene oxide dispersion, comprising: providing a graphene oxide dispersion liquid and water-absorbent resin before concentration; mixing the graphene oxide dispersion liquid before concentration with water-absorbent resin to obtain a mixed liquid, wherein the water-absorbent resin is used for absorbing water in the graphene oxide dispersion liquid; and separating the graphene oxide dispersion liquid from the water-absorbent resin after absorbing water in the mixed liquid to obtain a concentrated graphene oxide dispersion liquid, wherein the concentration of the concentrated graphene oxide dispersion liquid is 2.5-600 times of that of the graphene oxide dispersion liquid before concentration. The invention also provides a concentration device of the graphene oxide dispersion liquid. The method for concentrating the graphene oxide dispersion liquid has a good concentration effect.

Description

Method and device for concentrating graphene oxide dispersion liquid
Technical Field
The present invention relates to a method for concentrating a graphene oxide dispersion liquid, and a device for concentrating a graphene oxide dispersion liquid.
Background
The concentration of the graphene oxide dispersion is mostly less than 2g/L, which greatly limits the transportation, storage, and downstream applications of graphene oxide. The graphene oxide dispersion liquid can be concentrated by adopting modes such as suction filtration, filter pressing, film filtration and the like to obtain the graphene oxide dispersion liquid with higher concentration. The graphene oxide dispersion liquid with high concentration is convenient to transport and store. Moreover, with the increase of the concentration of the graphene oxide dispersion liquid, the arrangement mode of the graphene oxide sheet layers tends to be ordered to form a colloidal liquid crystal phase, so that the prepared macroscopic assembly material can furthest keep the excellent performance of the graphene sheet layers. However, the above-mentioned concentration method has a disadvantage of poor concentration effect.
Disclosure of Invention
In view of the above, it is necessary to provide a method for concentrating a graphene oxide dispersion to solve the problem of poor concentration effect of the graphene oxide dispersion.
A method for concentrating a graphene oxide dispersion liquid comprises the following steps:
providing a graphene oxide dispersion liquid and water-absorbent resin before concentration;
mixing the graphene oxide dispersion liquid before concentration with water-absorbent resin to obtain a mixed liquid, wherein the water-absorbent resin is used for absorbing water in the graphene oxide dispersion liquid; and
and separating the graphene oxide dispersion liquid from the water-absorbent resin after absorbing water in the mixed liquid to obtain a concentrated graphene oxide dispersion liquid, wherein the concentration of the concentrated graphene oxide dispersion liquid is 2.5-600 times of that of the graphene oxide dispersion liquid before concentration.
Further, after the mixing of the graphene oxide dispersion liquid before concentration and the water-absorbent resin, and before the separation of the graphene oxide dispersion liquid in the mixed liquid and the water-absorbent resin after water absorption, the method for concentrating the graphene oxide dispersion liquid further includes the steps of:
standing the mixed solution for 3-10 hours; or
Stirring the mixed solution for 20-40 min.
Further, the mass ratio of the graphene oxide dispersion liquid before concentration to the water-absorbent resin is 1-10: 1; and/or
The concentration of the graphene oxide dispersion liquid before concentration is 0.05-2 g/L; and/or
The concentration of the concentrated graphene oxide dispersion liquid is 5-30 g/L; and/or
The water-absorbent resin is granular, and the particle size of the granular water-absorbent resin is 0.3-10 mm; and/or
The water-absorbing resin is at least one of polyacrylate resin, polyacrylonitrile resin, polyvinyl alcohol resin, vinyl acetate and starch-acrylonitrile graft copolymer.
The utility model provides a enrichment facility of oxidation graphite alkene dispersion, includes concentrated cauldron, is used for storing the first storage tank of oxidation graphite alkene dispersion, is used for storing absorbent resin's second storage tank, and separation sieve, first storage tank, second storage tank, and separation sieve all with concentrated cauldron intercommunication.
Further, the separating screen is communicated with one end of the concentrating kettle, which is far away from the first storage tank; and/or
The diameter of the holes of the separating screen is 0.3-10 mm.
Further, the graphene oxide dispersion liquid concentration device further comprises a driver for driving the concentration kettle to rotate, and the driver is connected with the concentration kettle; or
The device for concentrating the graphene oxide dispersion liquid further comprises a stirrer extending into the concentrating kettle.
Further, the concentration device of the graphene oxide dispersion liquid also comprises a third storage tank communicated with the separation sieve, and the third storage tank is used for storing the concentrated graphene oxide dispersion liquid.
Further, the graphene oxide dispersion liquid concentration device further comprises a regulating pump connected between the first storage tank and the concentration kettle; and/or
The device for concentrating the graphene oxide dispersion liquid further comprises a regulating valve connected between the second storage tank and the concentrating kettle.
Further, the device for concentrating the graphene oxide dispersion liquid further comprises a flushing chamber communicated with the separation screen.
Further, the device for concentrating the graphene oxide dispersion liquid further comprises a drying chamber communicated with the flushing chamber and the second storage tank.
In the method for concentrating the graphene oxide dispersion liquid, the graphene oxide dispersion liquid before concentration is mixed with the water-absorbing resin, and the water-absorbing resin absorbs water in the graphene oxide dispersion liquid, so that the purpose of concentrating the graphene oxide dispersion liquid is achieved. The concentration of the concentrated graphene oxide dispersion liquid is 2.5-600 times of that of the graphene oxide dispersion liquid before concentration, and the concentration method of the graphene oxide dispersion liquid has a good concentration effect.
Drawings
Fig. 1 is a schematic structural diagram of a graphene oxide dispersion liquid concentrating device according to a first embodiment of the present invention.
Fig. 2 is a schematic structural diagram of a graphene oxide dispersion liquid concentrating device according to a second embodiment of the present invention.
Description of the main elements
Enrichment facility of graphite oxide dispersion 100,100’ Regulating valve 31
Concentration kettle 10,10’ Separating screen 40
Stirrer 11 Flushing chamber 50
The first storage tank 20,20’ Drying chamber 60
First regulating pump 21 Third storage tank 70,70’
Second storage tank 30,30’ Second regulating pump 71
The following detailed description will further illustrate the invention in conjunction with the above-described figures.
Detailed Description
So that the manner in which the above recited objects, features and advantages of the present invention can be understood in detail, a more particular description of the invention, briefly summarized above, may be had by reference to the embodiments thereof which are illustrated in the appended drawings. In addition, the embodiments and features of the embodiments of the present application may be combined with each other without conflict. In the following description, numerous specific details are set forth to provide a thorough understanding of the present invention, and the described embodiments are merely a subset of the embodiments of the present invention, rather than a complete embodiment. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes all and any combination of one or more of the associated listed items.
In various embodiments of the present invention, for convenience in description and not in limitation, the term "coupled" as used in the specification and claims of the present application is not limited to physical or mechanical couplings, either direct or indirect. "upper", "lower", "left", "right", and the like are used merely to indicate relative positional relationships, and when the absolute position of the object being described is changed, the relative positional relationships are changed accordingly.
The embodiment of the invention provides a method for concentrating a graphene oxide dispersion liquid.
The method for concentrating the graphene oxide dispersion comprises the following steps:
step S1: providing a graphene oxide dispersion liquid and water-absorbent resin before concentration;
step S2: mixing the graphene oxide dispersion liquid before concentration with water-absorbent resin to obtain a mixed liquid, wherein the water-absorbent resin is used for absorbing water in the graphene oxide dispersion liquid; and
step S3: and separating the graphene oxide dispersion liquid from the water-absorbent resin after absorbing water in the mixed liquid to obtain a concentrated graphene oxide dispersion liquid, wherein the concentration of the concentrated graphene oxide dispersion liquid is 2.5-600 times of that of the graphene oxide dispersion liquid before concentration.
In one embodiment, the mass ratio of the graphene oxide dispersion liquid before concentration to the water-absorbent resin is 1-10: 1. for example, 1: 1. 3: 1. 4: 1. 5: 1. 7: 1. 9: 1. or 10: 1.
in one embodiment, the concentration of the graphene oxide dispersion liquid before concentration is 0.05-2 g/L. For example, 0.05g/L, 0.1g/L, 0.5g/L, 1g/L, 1.5g/L, or 2 g/L.
In one embodiment, the concentration of the concentrated graphene oxide dispersion liquid is 5-30 g/L. For example, 5g/L, 10g/L, 15g/L, 20g/L, 25g/L, or 30 g/L.
In one embodiment, the water absorbent resin is in a granular shape, and the particle size of the granular water absorbent resin is 0.3-10 mm. For example, 0.3mm, 0.5mm, 1mm, 3mm, 5mm, 7mm, 9mm, or 10 mm.
In one embodiment, the water absorbent resin is spherical, polyhedral, or irregularly shaped.
In one embodiment, the water-absorbent resin is at least one of polyacrylate resin, polyacrylonitrile resin, polyvinyl alcohol resin, vinyl acetate, and starch-acrylonitrile graft copolymer.
In the method for concentrating the graphene oxide dispersion liquid, the graphene oxide dispersion liquid before concentration is mixed with the water-absorbing resin, and the water-absorbing resin absorbs water in the graphene oxide dispersion liquid, so that the purpose of concentrating the graphene oxide dispersion liquid is achieved. The concentration of the concentrated graphene oxide dispersion liquid is 2.5-600 times of that of the graphene oxide dispersion liquid before concentration, and the concentration method of the graphene oxide dispersion liquid has a good concentration effect.
After the graphene oxide dispersion liquid before concentration and the water-absorbent resin are mixed, and before the graphene oxide dispersion liquid in the mixed liquid is separated from the water-absorbent resin after water absorption, the method for concentrating the graphene oxide dispersion liquid further comprises the following steps:
standing the mixed solution for 3-10 hours; or
Stirring the mixed solution for 20-40 min.
In the technical scheme of the invention, the mixed solution is kept stand for 3-10 hours or stirred for 20-40 min, so that the water-absorbent resin can fully absorb water in the graphene oxide dispersion liquid, and the aim of concentrating the graphene oxide dispersion liquid is fulfilled. Compared with the mode of concentrating the graphene oxide dispersion liquid by suction filtration, filter pressing, membrane filtration and the like in the prior art, the method for concentrating the graphene oxide dispersion liquid has the advantages of simple and convenient operation and high concentration efficiency.
A first embodiment of the present invention provides a graphene oxide dispersion liquid concentration apparatus 100.
The graphene oxide dispersion liquid concentration device 100 comprises a concentration kettle 10, a first storage tank 20 for storing graphene oxide dispersion liquid, a second storage tank 30 for storing water-absorbent resin, and a separation sieve 40, wherein the first storage tank 20, the second storage tank 30, and the separation sieve 40 are all communicated with the concentration kettle 10.
In one embodiment, the separating screen 40 is in communication with an end of the concentrating tank 10 remote from the first storage tank 20. Preferably, the separating screen 40 is communicated with the bottom end of the concentrating still 10 far away from the first storage tank 20.
In one embodiment, the diameter of the holes of the separating screen 40 is 0.3-10 mm. For example, 0.3mm, 0.5mm, 1mm, 3mm, 5mm, 7mm, 9mm, or 10 mm.
In one embodiment, the concentrating tank 10 is vertically disposed, and the first storage tank 20 and the second storage tank 30 are located above the concentrating tank 10.
In the graphene oxide dispersion liquid concentration device 100 provided by the invention, the first storage tank 20 and the second storage tank 30 are both communicated with the concentration kettle 10, and after the graphene oxide dispersion liquid in the first storage tank 10 and the water-absorbent resin in the second storage tank 30 enter the concentration kettle 10, the water-absorbent resin can absorb the water in the graphene oxide dispersion liquid, so that the purpose of concentrating the graphene oxide dispersion liquid is achieved. The concentrated graphene dispersion and the water-absorbent resin after water absorption may be separated by a separation sieve 40. The concentration of the concentrated graphene oxide dispersion liquid is 2.5-600 times that of the concentrated graphene oxide dispersion liquid before concentration, and the concentration device 100 for the graphene oxide dispersion liquid has a good concentration effect.
The graphene oxide dispersion liquid concentration apparatus 100 further includes a stirrer 11 extending into the concentration kettle 10.
In the technical scheme of the present invention, the graphene oxide dispersion concentration apparatus 100 further includes a stirrer 11 extending into the concentration kettle 10, so that the graphene oxide dispersion and the water-absorbent resin can be sufficiently mixed, and the graphene oxide in the graphene oxide dispersion can be prevented from being adsorbed on the surface of the water-absorbent resin.
The graphene oxide dispersion liquid concentration apparatus 100 further includes a third storage tank 70 communicated with the separation screen 40, and the third storage tank 70 is configured to store the concentrated graphene oxide dispersion liquid.
In the technical scheme of the present invention, the graphene oxide dispersion concentration apparatus 100 further includes a third storage tank 70 communicated with the separation screen 40, and the concentrated graphene oxide dispersion may be stored in the third storage tank 70.
The graphene oxide dispersion concentration apparatus 100 further includes a first regulating pump 21 connected between the first storage tank 20 and the concentration tank 10.
In the technical scheme of the present invention, the graphene oxide dispersion concentration apparatus 100 further includes a first adjusting pump 21 connected between the first storage tank 20 and the concentration kettle 10, and the first adjusting pump 21 can adjust a feeding speed of the graphene oxide dispersion before concentration, so that a mass ratio of the graphene oxide dispersion before concentration to the water absorbent resin can reach 1-10: 1, thereby obtaining better concentration effect.
The graphene oxide dispersion concentration apparatus 100 further includes a control valve 31 connected between the second storage tank 30 and the concentration tank 10.
In the technical scheme of the present invention, the graphene oxide dispersion concentration apparatus 100 further includes an adjusting valve 31 connected between the second storage tank 30 and the concentration kettle 10, and the adjusting valve 31 can adjust the feeding speed of the water absorbent resin.
The graphene oxide dispersion concentration apparatus 100 further includes a second adjusting pump 71 connected between the separation screen 40 and the concentration tank 10.
In the technical scheme of the present invention, the graphene oxide dispersion concentration device 100 further includes a second adjusting pump 71 connected between the separation screen 40 and the concentration kettle 10, and the second adjusting pump 71 can adjust an outflow speed of a mixed solution of the graphene oxide dispersion and a water-absorbent resin to control a filling degree of the concentration kettle to be between 50% and 90%.
The graphene oxide dispersion concentration apparatus 100 further includes a rinsing chamber 50 in communication with the separation screen 40.
In the technical scheme of the present invention, the graphene oxide dispersion concentration apparatus 100 further includes a washing chamber 50 communicated with the separation screen 40, and the washing chamber 50 may be used to wash the water-absorbent resin after water absorption.
The graphene oxide dispersion concentration apparatus 100 further includes a drying chamber 60 communicating with the rinsing chamber 50 and the second storage tank 30.
In the technical scheme of the present invention, the graphene oxide dispersion concentration apparatus 100 further includes a drying chamber 60 communicated with the flushing chamber 50 and the second storage tank 30, the washed water-absorbent resin can be dried in the drying chamber 60, and the dried water-absorbent resin can be conveyed to the second storage tank 30 for reuse.
The concentration apparatus 100' for graphene oxide dispersion provided in the second embodiment of the present invention differs from the concentration apparatus 100 for graphene oxide dispersion provided in the first embodiment at least in: the concentration kettle 10 ' is horizontally arranged, the first storage tank 20 ' and the second storage tank 30 ' are positioned at one side of the concentration kettle 10 ', and the separating screen 40 ' and the third storage tank 70 ' are positioned at the other side of the concentration kettle 10 '.
In one embodiment, the thickening tank 10' may be a hollow rod, preferably a hollow screw. In the process of flowing the hollow rod, the graphene oxide dispersion liquid and the water absorbent resin in the first storage tank 20 'and the second storage tank 30' are uniformly mixed, and the water absorbent resin absorbs water in the graphene oxide dispersion liquid.
In an embodiment, the graphene oxide dispersion concentration apparatus 100 ' further includes a driver (not shown) connected to the concentration kettle 10 ' to drive the concentration kettle 10 ' to rotate.
In an embodiment, the apparatus 100 ' for concentrating graphene oxide dispersion further includes a bracket (not shown) supporting the concentrating still 10 ' so that a driver drives the concentrating still 10 ' to rotate.
The present invention will be specifically described below with reference to specific examples.
Example one
Providing a graphene oxide dispersion liquid with the concentration of 0.05g/L and a water-absorbing resin with the particle size of 5mm, wherein the mass ratio of the graphene oxide dispersion liquid to the water-absorbing resin is 5: 1;
mixing the graphene oxide dispersion liquid and water-absorbent resin to obtain a mixed liquid, and stirring for 30min, wherein the water-absorbent resin is used for absorbing water in the graphene oxide dispersion liquid; and
and separating the graphene oxide dispersion liquid from the water-absorbent resin after absorbing water in the mixed liquid to obtain a concentrated graphene oxide dispersion liquid, wherein the concentration of the concentrated graphene oxide dispersion liquid is 20g/L, and the concentration of the concentrated graphene oxide dispersion liquid is 400 times that of the graphene oxide dispersion liquid before concentration.
Example two
Providing a graphene oxide dispersion liquid with the concentration of 0.1g/L and a water-absorbing resin with the particle size of 6mm, wherein the mass ratio of the graphene oxide dispersion liquid to the water-absorbing resin is 4: 1;
mixing the graphene oxide dispersion liquid and water-absorbent resin to obtain a mixed liquid, and stirring for 30min, wherein the water-absorbent resin is used for absorbing water in the graphene oxide dispersion liquid; and
and separating the graphene oxide dispersion liquid from the water-absorbent resin after absorbing water in the mixed liquid to obtain a concentrated graphene oxide dispersion liquid, wherein the concentration of the concentrated graphene oxide dispersion liquid is 22g/L, and the concentration of the concentrated graphene oxide dispersion liquid is 220 times that of the graphene oxide dispersion liquid before concentration.
EXAMPLE III
Providing a graphene oxide dispersion liquid with the concentration of 1g/L and a water-absorbing resin with the particle size of 6mm, wherein the mass ratio of the graphene oxide dispersion liquid to the water-absorbing resin is 3: 1;
mixing the graphene oxide dispersion liquid and water-absorbent resin to obtain a mixed liquid, and stirring for 30min, wherein the water-absorbent resin is used for absorbing water in the graphene oxide dispersion liquid; and
and separating the graphene oxide dispersion liquid from the water-absorbent resin after absorbing water in the mixed liquid to obtain a concentrated graphene oxide dispersion liquid, wherein the concentration of the concentrated graphene oxide dispersion liquid is 25g/L, and the concentration of the concentrated graphene oxide dispersion liquid is 25 times that of the graphene oxide dispersion liquid before concentration.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention.

Claims (10)

1. A method for concentrating a graphene oxide dispersion liquid is characterized by comprising the following steps:
providing a graphene oxide dispersion liquid and water-absorbent resin before concentration;
mixing the graphene oxide dispersion liquid before concentration with water-absorbent resin to obtain a mixed liquid, wherein the water-absorbent resin is used for absorbing water in the graphene oxide dispersion liquid; and
and separating the graphene oxide dispersion liquid from the water-absorbent resin after absorbing water in the mixed liquid to obtain a concentrated graphene oxide dispersion liquid, wherein the concentration of the concentrated graphene oxide dispersion liquid is 2.5-600 times of that of the graphene oxide dispersion liquid before concentration.
2. The method of concentrating a graphene oxide dispersion liquid according to claim 1, wherein the method of concentrating a graphene oxide dispersion liquid further comprises, after the mixing of the graphene oxide dispersion liquid before the concentration and the water-absorbent resin, before the separation of the graphene oxide dispersion liquid in the mixed liquid and the water-absorbent resin after the absorption of water, the steps of:
standing the mixed solution for 3-10 hours; or
Stirring the mixed solution for 20-40 min.
3. The method for concentrating the graphene oxide dispersion liquid according to claim 1, wherein the mass ratio of the graphene oxide dispersion liquid before concentration to the water-absorbent resin is 1-10: 1; and/or
The concentration of the graphene oxide dispersion liquid before concentration is 0.05-2 g/L; and/or
The concentration of the concentrated graphene oxide dispersion liquid is 5-30 g/L; and/or
The water-absorbent resin is granular, and the particle size of the granular water-absorbent resin is 0.3-10 mm; and/or
The water-absorbing resin is at least one of polyacrylate resin, polyacrylonitrile resin, polyvinyl alcohol resin, vinyl acetate and starch-acrylonitrile graft copolymer.
4. The utility model provides a enrichment facility of oxidation graphite alkene dispersion, its characterized in that, the enrichment facility of oxidation graphite alkene dispersion includes concentrated cauldron, is used for storing the first storage tank of oxidation graphite alkene dispersion, is used for storing absorbent resin's second storage tank, and separation sieve, first storage tank, second storage tank, and separation sieve all with concentrated cauldron intercommunication.
5. The graphene oxide dispersion liquid concentration device according to claim 4, wherein the separation sieve is communicated with one end of the concentration kettle far away from the first storage tank; and/or
The diameter of the holes of the separating screen is 0.3-10 mm.
6. The graphene oxide dispersion liquid concentration device according to claim 4, further comprising a driver for driving the concentration kettle to rotate, wherein the driver is connected with the concentration kettle; or
The device for concentrating the graphene oxide dispersion liquid further comprises a stirrer extending into the concentrating kettle.
7. The apparatus for concentrating a graphene oxide dispersion according to claim 4, further comprising a third storage tank in communication with the separation sieve, wherein the third storage tank is configured to store the concentrated graphene oxide dispersion.
8. The apparatus for concentrating a graphene oxide dispersion according to claim 4, further comprising a conditioning pump connected between the first storage tank and the concentration tank; and/or
The device for concentrating the graphene oxide dispersion liquid further comprises a regulating valve connected between the second storage tank and the concentrating kettle.
9. The apparatus for concentrating a graphene oxide dispersion according to claim 4, further comprising a rinsing chamber in communication with the separation screen.
10. The apparatus of claim 9, further comprising a drying chamber in communication with the rinsing chamber and the second reservoir.
CN202110652115.9A 2021-06-08 2021-06-08 Method and device for concentrating graphene oxide dispersion liquid Pending CN113274763A (en)

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