CN109231197B - Low-impurity and low-layer-number graphene oxide preparation system - Google Patents
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Abstract
The invention provides a low-impurity and low-layer graphene oxide preparation system, which comprises a graphene oxide purification device and a low-layer graphene oxide preparation device, wherein the graphene oxide purification device comprises a first feeding hole, a tank body, a first partition plate, a second partition plate, an ultrasonic generation unit and a first discharging hole; the graphene oxide preparation device with the low layer number comprises a hydrogel forming unit, a low-temperature drying unit and a conveying mechanism, and can receive the graphene oxide purified by the graphene oxide purifying device and freeze-dry the graphene oxide. The system can effectively separate the graphene oxide from impurity ions, can improve the thoroughness of graphene oxide purification, and has high purification efficiency and low cost; the structure of the graphite oxide sheet layer can not be damaged in the freeze drying process, functional groups can be well preserved, and the graphite oxide subjected to freeze drying is not easy to agglomerate.
Description
Technical Field
The invention relates to the technical field of graphene oxide production, in particular to a graphene oxide preparation system with low impurities and a low number of layers.
Background
The scientific community appeared the graphite nanoplatelets as a material in the beginning of the 21 st century. In 2006, two scientists in The University of Manchester, UK skillfully prepared a single layer by mechanical peelingGraphite, thereby formally uncovering a veil of graphene, a material, and both consequently acquired the 2010 prize for nobel physics. The ideal graphene material is composed of a single layer of graphite with sp passing between carbon atoms2The hybrid orbitals are linked to form a stable six-membered ring structure. Researches find that the graphene material has good various physicochemical properties. For example: better electron conductivity than metal gold, better mechanical strength than steel, super-large specific surface area, good optical performance, superconductivity and the like. In view of these special properties, graphene materials have great application potential in military, transportation, mobile devices and the like.
In industrial production, the graphene oxide powder can be prepared on a large scale by applying an oxidation intercalation method. The graphene oxide slurry produced by the oxidation intercalation method contains a large amount of impurity ions. The existing equipment has the problems of low efficiency, poor washing effect and the like in the washing process, so that the produced graphene oxide product has low purity and reduced quality. Moreover, because the thermal stability of the graphite oxide is poor, the thermal decomposition phenomenon often occurs in the drying process, and the heated and dried graphite oxide is easy to agglomerate into hard blocks, which is not beneficial to subsequent dispersion.
Disclosure of Invention
In view of the deficiencies in the prior art, it is an object of the present invention to address one or more of the problems in the prior art as set forth above. For example, it is an object of the present invention to provide a system that can produce graphene oxide with a low impurity content and a low number of layers.
In order to achieve the above objects, the present invention provides a low-impurity and low-layer graphene oxide preparation system, which may include a graphene oxide purification apparatus and a low-layer graphene oxide preparation apparatus, wherein,
the graphene oxide purification device comprises a first feed inlet, a tank body, a first partition plate, a second partition plate, an ultrasonic generation unit and a first discharge outlet, wherein the first partition plate and the second partition plate are arranged in the tank body along the cross section of the tank body so as to divide the tank body into a reaction area, a filtering area and a collecting area which are sequentially distributed from top to bottom; the first feed port is arranged at the upper part of the tank body and communicated with the reaction zone, so that a purification object, a complexing agent and an acidic solution enter the reaction zone through the feed port, and the purification object comprises graphene oxide with a first layer number and impurity ions combined on functional groups; the first discharge hole is formed in the side wall of the tank body and located above the second partition plate so as to discharge purified graphene oxide deposited on the filtering component; the ultrasonic generating unit is arranged in the reaction zone to provide an ultrasonic environment for the reaction zone so as to fully perform the complex reaction;
the graphene oxide preparation device with the low layer number comprises a hydrogel forming unit, a low-temperature drying unit and a conveying mechanism, wherein the hydrogel forming unit is provided with a dispersing groove, the dispersing groove can receive water and purified graphene oxide discharged from the first discharge hole and disperse the purified graphene oxide in the water to form graphene oxide hydrogel; the low-temperature drying unit is provided with a temperature control unit, a pressure control unit and a cold drying cavity, wherein the cold drying cavity is formed by a shell and is provided with a second feeding hole, a second discharging hole and a cavity body, the temperature control unit is used for controlling the temperature in the cavity body to be not higher than-50 ℃ and controlling the temperature change in the whole cavity body to be not more than +/-4 ℃, and the pressure control unit is used for controlling the pressure in the cavity body to be lower than 1 atmosphere and controlling the pressure change in the whole cavity body to be not more than +/-100 Pa; the conveying mechanism is provided with a conveying part penetrating through the cold dry cavity and a speed regulating mechanism capable of regulating the advancing speed of the conveying part, the conveying part is used for receiving the graphene oxide hydrogel formed by the hydrogel forming unit and enabling the graphene oxide hydrogel to pass through the whole cold dry cavity, so that graphene oxide with a second layer number is obtained from the second discharging hole, and the second layer number is smaller than the first layer number.
Compared with the prior art, the invention has the beneficial effects that:
(1) the system can effectively separate the graphene oxide from impurity ions, and can improve the thoroughness of graphene oxide purification; the purification efficiency is high and the cost is low; the structure is simple and convenient, the use and the transportation are convenient, and the occupied area is small;
(2) the system provided by the invention is used for treating graphene oxide, the structure of a graphite oxide sheet layer cannot be damaged in the freeze drying process, functional groups are well preserved, and the graphite oxide subjected to freeze drying is not easy to agglomerate;
(3) the graphene oxide product after freeze drying has more excellent dispersion performance, fewer layers and larger specific surface area, and the layer-to-layer distance of the graphene oxide sheets is larger than that of the graphene oxide product after being dried by other drying methods.
Drawings
The above and other objects and features of the present invention will become more apparent from the following description taken in conjunction with the accompanying drawings, in which:
fig. 1 shows a schematic diagram of a graphene oxide purification apparatus in a low-impurity and low-layer-number graphene oxide preparation system according to an exemplary embodiment of the present invention.
Illustration of the drawings:
10-a first feed port, 11-a first sub-feed port, 12-a second sub-feed port; 20-a reaction zone, 21-an ultrasonic generator, 22-a first partition plate; 30-a filtering area, 31-a second clapboard, 32-a first discharge hole, 33-an ICP ion concentration detector, 34-a buffer layer, 40-a collecting area, 41-a liquid discharge hole and 42-a vacuum pump.
Detailed Description
Hereinafter, a low-impurity and low-layer-number graphene oxide production system according to the present invention will be described in detail with reference to the accompanying drawings and exemplary embodiments.
Fig. 1 shows a schematic diagram of a graphene oxide purification apparatus in a low-impurity and low-layer-number graphene oxide preparation system according to an exemplary embodiment of the present invention.
In an exemplary embodiment of the low-impurity and low-layer graphene oxide preparation system of the present invention, the preparation system may include a graphene oxide purification apparatus and a low-layer graphene oxide preparation apparatus.
In an exemplary embodiment of the present invention, as shown in fig. 1, the graphene oxide purification apparatus may be an integrated apparatus. The purification device comprises a tank body, wherein a first feeding hole 10 is formed in the top of the tank body, and the first feeding hole 10 comprises a first sub-feeding hole 11 and a second sub-feeding hole 12; the tank body is divided into a reaction zone 20, a filtering zone 30 and a collecting zone 40 by a first partition plate 22 and a second partition plate 31 which are arranged transversely from top to bottom in sequence. An ultrasonic generator 21 is provided in the reaction zone 20. The first partition 22 is provided with an openable member, and a metal coarse filter screen (not shown) is provided at an opening of the openable member. The second separator 31 may include a filter member (not shown). The bottom of the filtering zone 30 is provided with a first discharge port 32, and the first discharge port 32 is provided with an ICP ion concentration detector 33. Also included in the filtration zone 30 is a buffer layer 34 disposed over the second separator plate. The collection area 40 is provided at the bottom thereof with a liquid discharge port 41 and a vacuum pump 42. The openable and closable member of the first partition 22 connects the reaction zone 20 to the filtration zone 30, and the filter member of the second partition 31 connects the filtration zone 30 to the collection zone 40.
The graphene oxide containing impurities and having a first layer number can enter from a first sub-feed opening 11, and the complexing agent and the dilute hydrochloric acid can enter from a second sub-feed opening 12; complexing agent and impurity heavy metal ions contained in the graphene oxide under acidic condition, and then allowing the complex, the graphene oxide with smaller size and the impurity ions to enter the filtering area 20 through the openable component on the first partition plate 22; buffer protection layer 34 can slow down the impact of ultrasonic wave to the membrane structure in the second baffle 31 filtering component, because the effect of vacuum filtration system (the annular shape of falling U cavity in vacuum pump 42 and collection region), the complex is filtered to collection region 30 with impurity ion under the negative pressure effect, the less oxidized graphene of size can purify, can flow out from first discharge gate 32, the oxidized graphene residual ion concentration that has the first number of layers after accessible ICP ion concentration detector 33 detects the purification, and the waste liquid that contains complex and impurity acid radical ion can flow out from liquid discharge gate 41.
The purified graphene oxide with the first layer number is obtained at the first discharge hole of the purification device, and is detected by the ICP ion concentration detector 33, and the detection result shows that the weight percentage of impurity ions on the purified graphene oxide with the first layer number is below 0.005%, and the impurity ion removal rate is above 99%.
In this exemplary embodiment, the low-layer graphene oxide preparation device can receive the graphene oxide purified by the graphene oxide purification device and perform a freeze-drying process on the graphene oxide. The preparation device of the graphene oxide with the low layer number can be composed of a hydrogel forming unit, a low-temperature drying unit and a conveying mechanism.
The hydrogel-forming unit has dispersion grooves. The dispersion tank can receive the purified graphene oxide with the first layer number and water discharged from the first discharge hole in the graphene oxide purification device, and disperse the purified graphene oxide with the first layer number in water to form graphene oxide hydrogel. For example, the dispersion tank may have a tank body, a second feed port disposed above the tank body, and a second discharge port disposed at a side or bottom of the tank body. The second charging opening is used for adding the purified graphene oxide with the first layer number and water as raw materials. Here, the first layer number may be ten to several tens of layers, for example, 20 to 30 layers. And the second discharge hole is used for discharging the graphene oxide hydrogel. In addition, the hydrogel-forming unit may further have an ultrasound generating mechanism. The ultrasonic generating mechanism can transmit ultrasonic waves to the dispersion tank to form ultrasonic oscillation on the graphene oxide in the water of the dispersion tank, so that the dispersion effect is enhanced.
The purified graphene oxide having the first layer number can be dispersed in water by the dispersion tank, and a graphene oxide hydrogel can be formed. The graphene oxide as a raw material contains an oxygen-containing functional group. For example, the graphene oxide having the first layer number may be prepared by intercalating graphite with protonic acid. In the dispersing process, the dispersing effect is preferably further enhanced by ultrasonic dispersion, so that water molecules fully enter a lamellar structure or folds of the graphene oxide, or are combined with functional groups on the surface of the graphene oxide to form hydrated ions, thereby forming the graphene oxide hydrogel. The graphene oxide hydrogel has a structure in which water molecules are bonded in its own sheet or wrinkle of graphene oxide. The solid content of the graphene oxide hydrogel can be 0.1-50 wt%.
The low-temperature drying unit is provided with a temperature control unit, a pressure control unit and a cold drying cavity. Wherein, the cold dry chamber is enclosed by the casing and has feed inlet, discharge gate and the cavity of determining length. The cavity of the cold dry cavity can be in a U shape or a ring shape with a gap so as to save space. However, the present exemplary embodiment is not limited thereto, and the cavity of the cold dry chamber may also be S-shaped or linear. The feeding hole and the discharging hole are respectively arranged at the front end and the rear end of the cavity along the advancing direction of the materials, and are respectively provided with a valve capable of opening and closing so as to separate the cavity from the outside. The temperature control unit can be a refrigerator which is connected with the cold dry cavity and has a constant temperature control function, and the refrigerator can control the temperature in the cavity of the cold dry cavity to be not higher than-50 ℃ and control the temperature change in the cavity of the whole cold dry cavity to be not more than +/-4 ℃. And the pressure control unit can be a vacuum pump which is connected with the cold dry cavity and has a constant pressure control function, and the vacuum pump can control the pressure in the cavity of the cold dry cavity to be lower than 1 atmosphere and control the pressure variation in the whole cavity to be not more than +/-100 Pa.
Further, the temperature control unit can control the temperature in the cavity within a range of-55 to-65 ℃ and control the temperature change in the whole cavity to be not more than +/-2 ℃, and the pressure control unit can control the pressure in the cavity to be 10 to 100Pa and control the pressure change in the whole cavity to be not more than +/-10 Pa, so that the atmospheric environment with relatively stable low temperature and relatively stable vacuum degree can be obtained.
The water molecules can be changed into ice molecules through the coordination of the temperature control unit and the pressure control unit, and the lamellar structure of the graphite is further widened through volume expansion; and the ice can be desublimated and volatilized at low temperature and low pressure, the temperature is low, the entropy value is low, the strutted structure of the graphene oxide can be maintained, and the prepared graphene oxide material has good dispersibility and large specific surface area. Moreover, the relatively constant low temperature (for example, not higher than-50 ℃ and the temperature variation in the cavity of the whole cold dry cavity is controlled not to exceed +/-4 ℃) and the relatively constant vacuum degree (for example, lower than 1 atmosphere and the pressure variation in the whole cavity is controlled not to exceed +/-100 Pa) are beneficial to relatively stabilizing the condensation speed and degree of water molecules, so that the 'opening' effect on the graphene oxide layer is stable; but also the ice molecule desublimation speed and degree are relatively stable, thus being beneficial to avoiding local defects caused by the local stress of the graphene oxide layer to a certain degree. Furthermore, the temperature control unit and the pressure control unit are used for controlling the atmosphere of the cold drying cavity to be within the range of-55 to-65 ℃, the temperature change in the whole cavity is controlled not to exceed +/-2 ℃, the pressure is controlled to be 10 to 100Pa, the pressure change in the whole cavity is controlled not to exceed +/-10 Pa, the condensation speed and the degree of water molecules are further stabilized, and the opening effect of the graphene oxide layer is stabilized; but also the ice molecule desublimation speed and degree are further stabilized, thereby further avoiding local defects caused by the local stress of the graphene oxide layer.
The conveying structure is provided with a conveying member penetrating through the cold dry cavity and a speed regulating mechanism capable of regulating the traveling speed of the conveying member. The conveyor is capable of receiving the graphene oxide hydrogel formed by the hydrogel-forming unit and advancing the graphene oxide hydrogel through the entire cold dry cavity to finally obtain a second number of layers of graphene oxide from the discharge outlet of the cold dry cavity. The conveyor may be a conveyor belt. The speed regulating mechanism can control the conveyor belt to pass through the cold drying cavity at a preset speed at a uniform speed. The second number of layers is less than the first number of layers. The second number of layers may have a significant reduction compared to the first number of layers. Here, the second number of layers may be 1/3-1/6 of the first number of layers. For example, the second number of layers may be 5 to 7.
In another exemplary embodiment of the present invention, the apparatus for preparing graphene oxide with a low number of layers may further include a buffer region on the basis of the structure of the above exemplary embodiment. Specifically, the buffer region may be connected to the second discharge port, so as to appropriately raise the temperature of the graphene oxide entering the buffer region from the second discharge port, thereby enabling the graphene oxide as a product to be suitable for a room temperature environment or a subsequent treatment process. For example, the length of the buffer area may be 1.5 to 4 meters, but the present exemplary embodiment is not limited thereto.
In another exemplary embodiment of the present invention, the preparation apparatus of graphene oxide with a low number of layers may further include a pretreatment region on the basis of the structure of the above exemplary embodiment. In particular, the pretreatment zone may be connected to said second inlet and itself crossed by said conveyor. The pretreatment area is provided with a cooling component, so that the graphene oxide hydrogel entering the pretreatment area through the conveying member can be subjected to appropriate cooling treatment, and the temperature of the graphene oxide hydrogel is reduced. For example, the temperature within the pretreatment zone can be stably maintained between 1/6 and 3/5 of the temperature within the cavity. Through the setting in preliminary treatment district, can carry out first cooling to oxidation graphite alkene, be convenient for control cooling process, and do benefit to the operation. For example, the length of the pre-treatment region may be 1.5 to 4 meters, but the present exemplary embodiment is not limited thereto.
In an exemplary embodiment of the invention, the apparatus for preparing graphene oxide with a low number of layers may obtain the completely dried graphene oxide with a second number of layers by coordinately controlling the length of the cavity of the cold dry chamber, the temperature and pressure in the cold dry chamber, and the speed of the conveying member. Specifically, when the preparation device of the present invention is designed, the temperature and pressure in the freeze-drying chamber can be determined according to the above-mentioned relevant requirements, and then the length of the chamber and the operation speed of the conveying member can be determined according to the requirements of the field, etc., so as to ensure that the graphene oxide hydrogel conveyed and operated by the conveying member through the freeze-drying chamber can fully complete the processes of low-temperature freezing and desublimation drying. For example, the cavity length of the cold dry cavity may be 10-20 meters, but the present exemplary embodiment is not limited thereto.
In conclusion, the system can effectively separate the graphene oxide from impurity ions, and can improve the thoroughness of the purification of the graphene oxide; high purification efficiency, low cost, simple structure, convenient use and transportation and small occupied area. By using the system provided by the invention to treat graphene oxide, the structure of a graphite oxide sheet layer cannot be damaged in the freeze drying process, functional groups are well preserved, and the graphite oxide after freeze drying is not easy to agglomerate. The graphene oxide product dried by the freeze-dried method has more excellent dispersion performance, fewer layers and larger specific surface area, and the layer-to-layer distance of the graphene oxide sheets is larger than that of the graphene oxide product dried by other drying methods.
Although the present invention has been described above in connection with exemplary embodiments, it will be apparent to those skilled in the art that various modifications and changes may be made to the exemplary embodiments of the present invention without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A low-impurity and low-layer graphene oxide preparation system is characterized by comprising a graphene oxide purification device and a low-layer graphene oxide preparation device, wherein,
the graphene oxide purification device comprises a first feeding hole, a tank body, a first clapboard, a second clapboard, an ultrasonic generation unit and a first discharging hole, wherein,
the first clapboard and the second clapboard are arranged in the tank body along the cross section of the tank body so as to divide the tank body into a reaction area, a filtering area and a collecting area which are sequentially distributed from top to bottom, the first clapboard is provided with an openable component which can communicate the reaction area with the filtering area, and the second clapboard is provided with a filtering component which can realize solid-liquid separation;
the first feed port is arranged at the upper part of the tank body and communicated with the reaction zone, so that a purification object, a complexing agent and an acidic solution enter the reaction zone through the feed port, and the purification object comprises graphene oxide with a first layer number and impurity ions combined on functional groups;
the first discharge hole is formed in the side wall of the tank body and located above the second partition plate so as to discharge purified graphene oxide deposited on the filtering component, and the purified graphene oxide is graphene oxide with a first layer number;
the ultrasonic generating unit is arranged in the reaction zone to provide an ultrasonic environment for the reaction zone so as to fully perform the complex reaction;
the graphene oxide preparation device with the low layer number comprises a hydrogel forming unit, a low-temperature drying unit and a conveying mechanism, wherein,
the hydrogel forming unit is provided with a dispersion tank, and the dispersion tank is used for receiving water and the purified graphene oxide discharged from the first discharge hole and dispersing the purified graphene oxide in the water to form graphene oxide hydrogel;
the low-temperature drying unit is provided with a temperature control unit, a pressure control unit and a cold drying cavity, wherein the cold drying cavity is formed by a shell and is provided with a second feeding hole, a second discharging hole and a cavity body, the temperature control unit is used for controlling the temperature in the cavity body to be not higher than-50 ℃ and controlling the temperature change in the whole cavity body to be not more than +/-4 ℃, and the pressure control unit is used for controlling the pressure in the cavity body to be lower than 1 atmosphere and controlling the pressure change in the whole cavity body to be not more than +/-100 Pa;
the conveying mechanism is provided with a conveying part penetrating through the cold dry cavity and a speed regulating mechanism capable of regulating the advancing speed of the conveying part, the conveying part is used for receiving the graphene oxide hydrogel formed by the hydrogel forming unit and enabling the graphene oxide hydrogel to pass through the whole cold dry cavity, so that graphene oxide with a second layer number is obtained from the second discharging hole, and the second layer number is smaller than the first layer number.
2. The system for preparing graphene oxide with low impurity and number of layers according to claim 1, wherein the graphene oxide purification device further comprises an ion concentration detection unit disposed at the first discharge port to detect the concentration of impurity ions in the purified graphene oxide.
3. The system according to claim 2, wherein the graphene oxide purification apparatus further comprises a material returning unit having a controller and a material conveying member, the controller is connected to the ion concentration detection unit and determines whether to start the material conveying member according to a detection result of the ion concentration detection unit, and the material conveying member is capable of supplying the purified graphene oxide discharged from the first discharge port to the first feed port.
4. The system for preparing graphene oxide with low impurity and number of layers according to claim 1, wherein the graphene oxide purification device further comprises a reduced-pressure suction filtration unit, and the reduced-pressure suction filtration unit is arranged in the collection region and enables the collection region to form an inverted U-shaped cavity.
5. The system for preparing graphene oxide with low impurity and number of layers according to claim 1, wherein the graphene oxide purification device further comprises a buffer protection layer disposed between the first partition plate and the filtering member, and the buffer protection layer can absorb and buffer the ultrasonic waves generated by the ultrasonic generation unit to protect the filtering member.
6. The system for preparing graphene oxide with low impurity content and number of layers according to claim 1, wherein the device for preparing graphene oxide with low number of layers further comprises a buffer zone connected with the second discharge port, and the buffer zone can heat graphene oxide entering the buffer zone from the second discharge port.
7. The system for preparing graphene oxide with low impurity content and a low number of layers according to claim 1, wherein the device for preparing graphene oxide with a low number of layers further comprises a pretreatment region connected with the second feeding hole and penetrated by the conveying member, wherein the pretreatment region can perform cooling treatment on the graphene oxide hydrogel entering the pretreatment region, so that the temperature of the graphene oxide hydrogel is lowered and kept at 1/6-3/5 in the cavity.
8. The system for preparing graphene oxide with low impurity content and number of layers according to claim 1, wherein the graphene oxide with number of layers is completely dried by means of coordinately controlling the length of the cavity of the cold dry chamber, the temperature and pressure in the cold dry chamber, and the speed of the conveying member.
9. The graphene oxide preparation system with low impurities and number of layers according to claim 1, wherein the temperature control unit controls the temperature in the cavity to be within a range of-55 ℃ to-65 ℃ and controls the temperature variation in the whole cavity to be not more than +/-2 ℃.
10. The system for preparing graphene oxide with low impurity and low layer number according to claim 1, wherein the pressure control unit controls the pressure in the cavity to be 10-100 Pa and controls the pressure variation in the whole cavity to be not more than +/-10 Pa.
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| US9844762B2 (en) * | 2014-09-12 | 2017-12-19 | Lawrence Livermore National Security, Llc | Nanoporous metal-carbon composite |
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| CN103058179A (en) * | 2013-01-21 | 2013-04-24 | 张家港市东大工业技术研究院 | Method for preparing spongy graphene oxide by using freeze-drying method |
| CN205252914U (en) * | 2015-12-30 | 2016-05-25 | 安徽易能新材料科技有限公司 | A filter equipment for graphite alkene is hierarchical |
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