CN113104844A - Preparation method of carboxylated graphene - Google Patents
Preparation method of carboxylated graphene Download PDFInfo
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- CN113104844A CN113104844A CN202110393250.6A CN202110393250A CN113104844A CN 113104844 A CN113104844 A CN 113104844A CN 202110393250 A CN202110393250 A CN 202110393250A CN 113104844 A CN113104844 A CN 113104844A
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Abstract
The invention discloses a preparation method of carboxylated graphene, which comprises the following steps: preparing a graphene oxide solution; and secondly, adding lg chloroacetic acid and 1.2g sodium hydroxide into 100mL graphene oxide solution with the mass concentration of 2mg/mL, putting the solution into a water bath, performing ultrasonic treatment for 1h, stirring the solution for reaction for 24h, performing vacuum filtration on the mixed solution by using a vacuum filter device, washing the solution with deionized water for multiple times to obtain carboxylated graphene oxide solution, and drying the solution in a vacuum drying oven at the temperature of 60 ℃ to obtain the carboxylated graphene oxide. Compared with the prior art, the carboxylated graphene oxide is prepared by performing ultrasonic treatment on a graphene oxide solution and reacting the graphene oxide with a vacuum filtering device.
Description
Technical Field
The invention relates to the technical field of preparation of carboxylated graphene, and particularly relates to a preparation method of carboxylated graphene.
Background
Graphene Oxide (GO) is very similar in structure to graphene and is often used as a precursor for making graphene. Because a large number of functional groups such as carboxyl and epoxy groups exist on the surface of graphene oxide, the existence of the functional groups provides a large number of chemical reaction active points for the surface functional modification of the graphene oxide, and because the activity of the carboxyl is relatively high, a large number of grafting reactions can be carried out on the graphene oxide. At present, carboxyl groups are mostly adopted to carry out modification research on the surface of graphene oxide, and the modification of the surface often needs to firstly activate the carboxyl groups so as to improve the reactivity of the graphene oxide.
The existing carboxylated graphene is generally prepared by vacuum filtration. In the using process, the amount of the first suction filtration is found to be small, and solution is usually required to be continuously added in one-time experiment or production, so that unnecessary labor and time are wasted, and the experiment efficiency is low.
In view of the above, the applicant has made an intensive study on the above-mentioned defects in the prior art, and has made this invention.
Disclosure of Invention
The main object of the present invention is to provide a method for producing carboxylated graphene, which can efficiently produce carboxylated graphene.
In order to achieve the above purpose, the solution of the invention is:
a preparation method of carboxylated graphene comprises the following steps:
preparing a graphene oxide solution;
and secondly, adding lg chloroacetic acid and 1.2g sodium hydroxide into 100mL graphene oxide solution with the mass concentration of 2mg/mL, putting the solution into a water bath, performing ultrasonic treatment for 1h, stirring the solution for reaction for 24h, performing vacuum filtration on the mixed solution by using a vacuum filter device, washing the solution with deionized water for multiple times to obtain carboxylated graphene oxide solution, and drying the solution in a vacuum drying oven at the temperature of 60 ℃ to obtain the carboxylated graphene oxide.
Further, the preparation of the graphene oxide solution in the step (i) comprises the following steps:
1) slowly adding 100ml of concentrated sulfuric acid (95%), 1g of expandable graphite and 3g of potassium permanganate in sequence in an ice water bath, and continuously stirring for 30 min;
2) heating to 35 deg.C, and stirring for 30 min; then, slowly adding deionized water dropwise until no bubbles are discharged, wherein the generation of purple smoke is observed;
3) heating the reaction system to 95 ℃, continuing stirring for 15min, adding 300ml of deionized water to stop the reaction, and adding 10ml of hydrogen peroxide (30%) into the obtained tan mixture to change the color into golden yellow; naturally cooling the golden yellow mixture, filtering and washing, firstly washing with 10% hydrochloric acid, finally washing with deionized water until the pH value is 7, and vacuum-drying the obtained red brown colloidal substance at 35 ℃ to obtain graphite oxide;
4) weighing a certain amount of graphite oxide, and ultrasonically stripping in deionized water with a certain volume to prepare a graphene oxide solution.
Further, the vacuum filtering device comprises a suction filtering base, a first filtering body, a second filtering body, a cross rod, a lifting mechanism, a rotating mechanism, a fixed base and a collecting device, wherein a supporting net is formed on the suction filtering base, a vacuum cavity is formed at the lower part of the supporting net, and the vacuum cavity is connected with a negative pressure pump; the fixed base is arranged between the suction filter base and the collecting device, the middle part of the cross rod is connected with the upper part of the lifting mechanism, the lower part of the lifting mechanism is rotationally connected on the fixed base, and the fixed base is also provided with a rotating mechanism for driving the lifting mechanism and the cross rod to rotate horizontally;
the first filter body and the second filter body are respectively provided with filter paper, and the first filter body and the second filter body are respectively arranged at two ends of the cross rod; when suction filtration is carried out, the lifting mechanism is positioned at a low position, the filter paper of the first filter body is attached to the support net of the suction filtration base, and liquid to be filtered is added into the filtration space of the first filter body; after the suction filter is completed, the lifting mechanism rises to a high position, the first filter body is separated from the suction filter base, the rotating mechanism rotates to move the first filter body to the position right above the collecting device, the second filter body is moved to the position right above the suction filter base, and then the lifting mechanism descends to a low position from the high position.
Furthermore, the lifting mechanism is a double-guide-rod electric lifting cylinder.
Furthermore, the rotating mechanism comprises a driven gear fixedly connected with the lower end of the lifting mechanism and a rotating motor fixedly arranged on the fixed base, and a driving gear meshed with the driven gear is fixedly arranged on an output shaft of the rotating motor.
After the structure is adopted, the preparation method of the carboxylated graphene has at least the following beneficial effects:
firstly, the content of carboxyl groups on a graphene oxide sheet layer is improved by performing ultrasonic treatment on chloroacetic acid, sodium hydroxide and a graphene oxide solution, so that carboxylated graphene oxide is obtained.
And secondly, the improved vacuum filtering device is adopted for filtering operation, and the first filtering body and the second filtering body are arranged, when one filtering body is used for filtering, the other filtering body slides on the fixed pipe through the adjusting ring, so that the side, provided with the solid matters, of the filter paper can be turned outwards, and the solid matters can be conveniently collected into the collecting device.
Compared with the prior art, the carboxylated graphene oxide is prepared by performing ultrasonic treatment on a graphene oxide solution and reacting the graphene oxide with a vacuum filtering device.
Drawings
Fig. 1 is a process flow diagram of a preparation method of carboxylated graphene according to the present invention.
Fig. 2 is a schematic structural view of a vacuum filtration apparatus.
Fig. 3 is a schematic view of the vacuum filtration apparatus in filtering and removing solid matter.
Fig. 4 is a partially enlarged structural view of a portion a in fig. 3.
Fig. 5 is a schematic structural view of the first filter body.
Fig. 6 is an enlarged schematic view of a portion B in fig. 4.
In the figure:
a suction filter base 1; a support net 11; a vacuum chamber 12; a water-retaining cover 121; a negative pressure pump 13; a drain pipe 14; an annular seal rubber ring 15; a collecting device 2;
a cross bar 31; a lifting mechanism 32; a rotation mechanism 33; the driven gear 331; a drive gear 332; a rotating motor 333; a fixed base 34;
a first filter body 41; a second filter 42; a fixed tube 43; a first liquid passing chamber 431; a second liquid passing chamber 432; a funnel 433;
a filter paper 44; a filtering space 441; a fixing member 442; an adjustment ring 45; a connecting rod 46; a mounting ring 47; a liquid storage bottle 5; a liquid outlet pipe 51; controlling the switch 52.
Detailed Description
In order to further explain the technical solution of the present invention, the present invention is explained in detail by the following specific examples.
As shown in fig. 1 to fig. 6, the preparation method of carboxylated graphene according to the present invention includes the following steps: preparing a graphene oxide solution; preferably, the preparation of the graphene oxide solution in the step (i) comprises the following steps: 1) slowly adding 100ml of concentrated sulfuric acid (95%), 1g of expandable graphite and 3g of potassium permanganate in sequence in an ice water bath, and continuously stirring for 30 min; 2) heating to 35 deg.C, and stirring for 30 min; then, slowly adding deionized water dropwise until no bubbles are discharged, wherein the generation of purple smoke is observed; 3) heating the reaction system to 95 ℃, continuing stirring for 15min, adding 300ml of deionized water to stop the reaction, and adding 10ml of hydrogen peroxide (30%) into the obtained tan mixture to change the color into golden yellow; naturally cooling the golden yellow mixture, filtering and washing, firstly washing with 10% hydrochloric acid, finally washing with deionized water until the pH value is 7, and vacuum-drying the obtained red brown colloidal substance at 35 ℃ to obtain graphite oxide; 4) weighing a certain amount of graphite oxide, and ultrasonically stripping in deionized water with a certain volume to prepare a graphene oxide solution. During ultrasonic stripping, 30 percent (about 200W) of the maximum power of an ultrasonic cell crusher is adopted for ultrasonic treatment for 2 hours; and centrifuging the graphene oxide dispersion liquid obtained by ultrasonic treatment in a high-speed centrifuge at the rotating speed of 8000r/min for 10min, and taking the supernatant, namely the graphene oxide solution for later use.
And secondly, adding lg chloroacetic acid and 1.2g sodium hydroxide into 100mL graphene oxide solution with the mass concentration of 2mg/mL, putting the solution into a water bath, performing ultrasonic treatment for 1h, stirring the solution for reaction for 24h, performing vacuum filtration on the mixed solution by using a vacuum filter device, washing the solution with deionized water for multiple times to obtain carboxylated graphene oxide solution, and drying the solution in a vacuum drying oven at the temperature of 60 ℃ to obtain the carboxylated graphene oxide.
In this way, according to the preparation method of carboxylated graphene, chloroacetic acid, sodium hydroxide and graphene oxide solution are subjected to ultrasonic treatment, so that the content of carboxyl groups on graphene oxide lamella is increased, and the carboxylated graphene oxide is obtained.
Preferably, the vacuum filter device comprises a suction filter base 1, a first filter body 41, a second filter body 42, a cross bar 31, a lifting mechanism 32, a rotating mechanism 33, a fixed base 34 and a collecting device 2, wherein a supporting net 11 is formed on the suction filter base 1, a vacuum cavity 12 is formed at the lower part of the supporting net 11, and the vacuum cavity 12 is connected with a negative pressure pump 13; the fixed base 34 is arranged between the suction filter base 1 and the collecting device 2, the middle part of the cross rod 31 is connected with the upper part of the lifting mechanism 32, the lower part of the lifting mechanism 32 is rotatably connected on the fixed base 34, and the fixed base 34 is also provided with a rotating mechanism 33 for driving the lifting mechanism 32 and the cross rod 31 to rotate horizontally; the first filter body 41 and the second filter body 42 are both provided with filter paper 44, and the first filter body 41 and the second filter body 42 are respectively arranged at two ends of the cross bar 31; when the suction filtration is performed, the lifting mechanism 32 is located at the low position, the filter paper 44 of the first filter body 41 is attached to the support net 11 of the suction filtration base 1, and the liquid to be filtered is added into the filtering space 441 of the first filter body 41; after the suction filtration is completed, the lifting mechanism 32 is lifted to the high position, the first filter body 41 is separated from the suction filtration base 1, the rotating mechanism 33 rotates to move the first filter body 41 to the position right above the collecting device 2, and move the second filter body 42 to the position right above the suction filtration base 1, and then the lifting mechanism 32 is lowered from the high position to the low position.
The support net 11 provides a supporting force for the filter paper 44, and the water through holes on the support net 11 facilitate the liquid penetrating through the filter paper 44 to flow into the vacuum cavity 12. The pressure in the vacuum chamber 12 is lower than the ambient atmospheric pressure, not to absolute vacuum; preferably, the vacuum chamber 12 is connected to a negative pressure pump 13 through a pipe, and a water blocking cover 121 transversely extending from an upper end of a nozzle of the pipe connected to the negative pressure pump 13 is formed on an inner wall of the vacuum chamber 12 to reduce the filtered water from being sucked into the vacuum pump. A drain pipe 14 is arranged at the bottom of the vacuum cavity 12, and a valve for controlling the opening and closing of the drain pipe 14 is arranged on the drain pipe 14.
The improved vacuum filter device is adopted to carry out filtering operation, and by arranging the first filter body 41 and the second filter body 42, when one filter body carries out filtering, the other filter body slides on the fixed pipe 43 through the adjusting ring 45, so that the side, provided with the solid matters, of the filter paper 44 can be turned outwards, and the solid matters can be conveniently collected into the collecting device 2. Preferably, an annular sealing rubber ring 15 is formed on the upper edge of the suction filter base 1, and when the filter paper 4444 is used for filtering, the lower surface of the edge of the filter paper 44 abuts against and seals the annular sealing rubber ring 15.
Preferably, the lifting mechanism 32 is a double-guide-rod electric lifting cylinder; the double-guide-rod electric lifting cylinder ensures that the cross rod 31 rotates along with the rotation of the lifting mechanism 32, the part structure is reduced, and the arrangement structure is more reasonable and efficient. The rotating mechanism 33 comprises a driven gear 331 fixedly connected with the lower end of the lifting mechanism 32, and further comprises a rotating motor 333 fixedly arranged on the fixed base 34, and an output shaft of the rotating motor 333 is fixedly provided with a driving gear 332 engaged with the driven gear 331.
Preferably, each of the first filter body 41 and the second filter body 42 further includes a fixing tube 43, an adjusting ring 45, a plurality of connecting rods 46 and a mounting ring 47; the filter paper 44 is bowl-shaped and has a filter space 441 with an upward opening, and the center of the bottom of the filter paper 44 is detachably mounted at the lower end of the fixed pipe 43 through a fixing member 442; the mounting ring 47 is fixedly connected to the upper edge of the filter paper 44, the adjusting ring 45 is sleeved on the fixed tube 43 and adjusts the position of the adjusting ring 45 on the fixed tube 43, and two ends of the connecting rods 46 are respectively and rotatably connected to the adjusting ring 45 and the mounting ring 47; the position of the adjusting ring 45 is driven to descend, the upper edge of the filter paper 44 of the first filter body 41 moves downward to a level lower than the lower end surface of the fixed pipe 43, the inner wall of the filtering space 441 of the filter paper 44 is turned outwards, and then the solid matter on the filter paper 44 is collected into the collecting device 2 by using a tool.
During the use, one of first filter 41 and second filter 42 filters the body and uses with inhaling the cooperation of straining base 1, and another filter is located collection device 2 top, and two filters the body and filters and take off the effect of solid matter in turn, have improved the filter effect.
Further, a mechanism for automatically or manually scraping or shaking off the solid matter on the filter paper 44, such as an automatic or manual scraper mechanism, is provided above the collecting device 2. The filter paper 44 on the first filter 41 and the second filter 42 can be replaced at a proper time according to the usage, and when the filter is replaced, the fixing member 442 at the lower end of the fixing tube 43 is removed, a new filter paper 44 is installed, and the upper edge of the filter paper 44 is fixed to the installation ring 47, for example, by bonding. The fixing member 442 is a screw and is screwed to the lower end surface of the fixing tube 43.
Preferably, the second filter body 42 performs a filtering operation on the suction filter base 1 while collecting the solid matters on the filter paper 44 in the first filter body 41. Furthermore, the position of the adjusting ring 45 on the fixing tube 43 is adjusted manually or by an electric mechanism.
Preferably, a first liquid passing cavity 431 is formed in the fixed tube 43 along the length direction of the fixed tube 43, a plurality of second liquid passing cavities 432 are formed on the outer wall of the fixed tube 43 corresponding to the filtering space 441 of the filter paper 44, and the second liquid passing cavities 432 are communicated with the first liquid passing cavity 431; the first liquid passing cavity 431 is provided with an upper opening, a funnel 433 is arranged on the upper opening, and the solution to be filtered enters the first liquid passing cavity 431 through the funnel 433. By arranging the first liquid passing cavity 431 and the second liquid passing cavity 432, the liquid to be filtered can conveniently enter the filtering space 441 of the filter paper 44 through the first liquid passing cavity 431 and the second liquid passing cavity 432.
Preferably, the vacuum filter device further comprises a liquid storage bottle 5, a liquid outlet pipe 51 is formed on the liquid storage bottle 5, a control switch 52 is arranged on the liquid outlet pipe 51, and the tail end of the liquid outlet pipe 51 is positioned above a funnel 433 of the filter body above the suction filter base 1. The liquid storage bottle 5 conveys the liquid to be filtered into the funnel 433 under the control of the control switch 52, so that the automatic addition of the solution to be filtered is realized.
Compared with the prior art, the carboxylated graphene oxide is prepared by performing ultrasonic treatment on a graphene oxide solution and reacting the graphene oxide with a vacuum filtering device.
The above embodiments and drawings are not intended to limit the form and style of the present invention, and any suitable changes or modifications thereof by those skilled in the art should be considered as not departing from the scope of the present invention.
Claims (5)
1. A preparation method of carboxylated graphene is characterized by comprising the following steps:
preparing a graphene oxide solution;
and secondly, adding lg chloroacetic acid and 1.2g sodium hydroxide into 100mL graphene oxide solution with the mass concentration of 2mg/mL, putting the solution into a water bath, performing ultrasonic treatment for 1h, stirring the solution for reaction for 24h, performing vacuum filtration on the mixed solution by using a vacuum filter device, washing the solution with deionized water for multiple times to obtain carboxylated graphene oxide solution, and drying the solution in a vacuum drying oven at the temperature of 60 ℃ to obtain the carboxylated graphene oxide.
2. The method for preparing carboxylated graphene according to claim 1, wherein the step (i) of preparing the graphene oxide solution comprises the following steps:
1) slowly adding 100ml of concentrated sulfuric acid (95%), 1g of expandable graphite and 3g of potassium permanganate in sequence in an ice water bath, and continuously stirring for 30 min;
2) heating to 35 deg.C, and stirring for 30 min; then, slowly adding deionized water dropwise until no bubbles are discharged, wherein the generation of purple smoke is observed;
3) heating the reaction system to 95 ℃, continuing stirring for 15min, adding 300ml of deionized water to stop the reaction, and adding 10ml of hydrogen peroxide (30%) into the obtained tan mixture to change the color into golden yellow; naturally cooling the golden yellow mixture, filtering and washing, firstly washing with 10% hydrochloric acid, finally washing with deionized water until the pH value is 7, and vacuum-drying the obtained red brown colloidal substance at 35 ℃ to obtain graphite oxide;
4) weighing a certain amount of graphite oxide, and ultrasonically stripping in deionized water with a certain volume to prepare a graphene oxide solution.
3. The method according to claim 1, wherein the vacuum filtration device comprises a suction filter base, a first filter, a second filter, a cross bar, a lifting mechanism, a rotating mechanism, a fixed base and a collecting device, wherein a support net is formed on the suction filter base, a vacuum cavity is formed at the lower part of the support net, and the vacuum cavity is connected with a negative pressure pump; the fixed base is arranged between the suction filter base and the collecting device, the middle part of the cross rod is connected with the upper part of the lifting mechanism, the lower part of the lifting mechanism is rotationally connected on the fixed base, and the fixed base is also provided with a rotating mechanism for driving the lifting mechanism and the cross rod to rotate horizontally;
the first filter body and the second filter body are respectively provided with filter paper, and the first filter body and the second filter body are respectively arranged at two ends of the cross rod; when suction filtration is carried out, the lifting mechanism is positioned at a low position, the filter paper of the first filter body is attached to the support net of the suction filtration base, and liquid to be filtered is added into the filtration space of the first filter body; after the suction filter is completed, the lifting mechanism rises to a high position, the first filter body is separated from the suction filter base, the rotating mechanism rotates to move the first filter body to the position right above the collecting device, the second filter body is moved to the position right above the suction filter base, and then the lifting mechanism descends to a low position from the high position.
4. The method of claim 3, wherein the lifting mechanism is a double-guide-rod electric lifting cylinder.
5. The method according to claim 3, wherein the rotating mechanism comprises a driven gear fixedly connected to the lower end of the lifting mechanism, and further comprises a rotating motor fixedly disposed on the fixed base, and an output shaft of the rotating motor is fixedly provided with a driving gear engaged with the driven gear.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110393250.6A CN113104844A (en) | 2021-04-13 | 2021-04-13 | Preparation method of carboxylated graphene |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110393250.6A CN113104844A (en) | 2021-04-13 | 2021-04-13 | Preparation method of carboxylated graphene |
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| CN113104844A true CN113104844A (en) | 2021-07-13 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114314576A (en) * | 2021-11-30 | 2022-04-12 | 西安近代化学研究所 | Method for modifying carboxyl functionalization of graphene oxide |
| CN117089217A (en) * | 2021-09-04 | 2023-11-21 | 高祥 | Preparation method of heat-conducting engineering plastic |
-
2021
- 2021-04-13 CN CN202110393250.6A patent/CN113104844A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117089217A (en) * | 2021-09-04 | 2023-11-21 | 高祥 | Preparation method of heat-conducting engineering plastic |
| CN114314576A (en) * | 2021-11-30 | 2022-04-12 | 西安近代化学研究所 | Method for modifying carboxyl functionalization of graphene oxide |
| CN114314576B (en) * | 2021-11-30 | 2024-03-29 | 西安近代化学研究所 | Graphene oxide carboxyl functional modification method |
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Application publication date: 20210713 |