CN220559175U - Graphite oxidation reaction device with automatic feeding control function - Google Patents
Graphite oxidation reaction device with automatic feeding control function Download PDFInfo
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- CN220559175U CN220559175U CN202322126415.0U CN202322126415U CN220559175U CN 220559175 U CN220559175 U CN 220559175U CN 202322126415 U CN202322126415 U CN 202322126415U CN 220559175 U CN220559175 U CN 220559175U
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- kettle body
- reaction kettle
- feeding port
- valve
- jacket
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 23
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 20
- 239000010439 graphite Substances 0.000 title claims abstract description 20
- 238000006243 chemical reaction Methods 0.000 claims abstract description 58
- 239000002994 raw material Substances 0.000 claims abstract description 17
- 238000007599 discharging Methods 0.000 claims abstract description 4
- 230000002572 peristaltic effect Effects 0.000 claims description 14
- 239000011344 liquid material Substances 0.000 claims description 9
- 239000011343 solid material Substances 0.000 claims description 8
- 238000003860 storage Methods 0.000 claims description 8
- 238000012544 monitoring process Methods 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 230000000007 visual effect Effects 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 21
- 230000003647 oxidation Effects 0.000 abstract description 9
- 239000000376 reactant Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 229910021389 graphene Inorganic materials 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000003321 amplification Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000010327 methods by industry Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The utility model provides an automatic feeding control graphite oxidation reaction device, which relates to the technical field of reaction kettles and comprises a reaction kettle body, wherein a motor is arranged at the top end of the reaction kettle body, a first feeding port, a second feeding port and a third feeding port are sequentially arranged at the top end of the reaction kettle body from right to left, a discharging hole is formed in the bottom of the reaction kettle body, a jacket is arranged at the periphery of the bottom of the reaction kettle body, and a temperature control device is arranged on the right side of the jacket; the first feed inlet is connected with the raw materials charging means, be provided with first valve between first feed inlet and the raw materials charging means, the setting of different feed inlets to the control of a plurality of valves, thereby the order of adding of reactant, time and the interpolation volume are controlled, and the oxidation process of guarantee graphite is more abundant, makes the control accuracy of reaction process higher, cooperates temperature control device to improve reaction efficiency, reduces the influence of external environmental factor.
Description
Technical Field
The utility model relates to the technical field of reaction kettles, in particular to an automatic feeding control graphite oxidation reaction device.
Background
The graphene serving as a novel two-dimensional carbon nanomaterial has the characteristics of good thermal conductivity, electrical conductivity, high mechanical strength and the like, and can be widely applied to various high and new technical fields such as energy storage devices, heat conducting materials, anticorrosive coatings, medical detection and the like. The current preparation method of graphene mainly comprises a mechanical stripping method, a chemical vapor deposition method, an epitaxial growth method and a redox method. However, in the existing preparation method, the preparation of graphene by using natural graphite or small-molecular hydrocarbon gases such as methane and ethylene as a carbon source through oxidation-reduction and chemical vapor deposition is limited by factors such as high raw material cost, harsh process conditions and the like, and breakthrough is difficult to realize in the aspect of large-scale production, so that the development of graphene application technology and market expansion are restricted. Therefore, from the perspective of product engineering and process engineering optimization, the development of a key technology with cost and engineering advantages is the basis for developing graphene related industries.
The current method for preparing graphene oxide by using graphite as a raw material through a chemical oxidation method is a method with large-scale amplification prospect, the addition sequence, time and addition amount of reactants are required to be effectively controlled in the process of preparing the graphene oxide by using the chemical oxidation method, the oxidation process of the graphite can be ensured to be more sufficient, the yield of the graphene oxide is closely related to the control of the reaction process, the control accuracy and the reaction efficiency in the preparation process are low, and in order to reduce the influence of considered control factors, an automatic feeding control graphite oxidation reaction device is provided.
Disclosure of Invention
The utility model aims to solve the defects in the prior art, and the method for preparing graphene oxide by using graphite as a raw material through a chemical oxidation method is a method with a large-scale amplification prospect, and the addition sequence, time and addition amount of reactants are required to be effectively controlled in the process of preparing the graphene oxide by using the chemical oxidation method so as to ensure that the oxidation process of the graphite is more sufficient, the yield of the graphene oxide is closely related to the control of the reaction process, the control accuracy and the reaction efficiency in the preparation process are lower, and the influence of considered control factors is reduced.
In order to achieve the above purpose, the present utility model adopts the following technical scheme:
the graphite oxidation reaction device comprises a reaction kettle body, wherein a motor is arranged at the top end of the reaction kettle body, a first feed inlet, a second feed inlet and a third feed inlet are sequentially formed in the top end of the reaction kettle body from right to left, a discharge hole is formed in the bottom of the reaction kettle body, a jacket is arranged on the periphery of the bottom of the reaction kettle body, and a temperature control device is arranged on the right side of the jacket;
the first feeding port is connected with a raw material feeder, and a first valve is arranged between the first feeding port and the raw material feeder;
the second feeding port is connected with a solid material feeding port, and a screw feeder and a second valve are sequentially arranged between the solid material feeding port and the second feeding port;
the third feeding port is connected with two liquid material storage tanks, a third total valve is arranged near the joint of the third feeding port, and a third valve and a first peristaltic pump are sequentially arranged between the two liquid material storage tanks and the third total valve.
As a preferable scheme of the utility model, the reaction kettle body is made of 316L stainless steel, and a polytetrafluoroethylene coating lining is arranged on the inner wall of the reaction kettle body.
As a preferable scheme of the utility model, the output end of the motor is provided with a stirrer extending to the inside of the reaction kettle body.
As a preferable scheme of the utility model, a sensor monitoring port and a visual window are sequentially arranged on the right side of the first feeding port.
As a preferable scheme of the utility model, the lower end of the discharging hole is sequentially connected with an automatic control valve and a manual safety valve.
As a preferable scheme of the utility model, the temperature control device comprises a temperature controller C-H1, wherein the temperature controller C-H1 is circularly communicated with a jacket through a pipeline, cold and hot oil liquid is injected into the jacket, and a second peristaltic pump is arranged between the jacket and the temperature controller C-H1.
The technical effect of adopting the further scheme is as follows: .
Compared with the prior art, the utility model has the beneficial effects that:
according to the utility model, in the process of preparing graphene oxide by a chemical oxidation method, different feed inlets are arranged, and a plurality of valves are controlled, so that the adding sequence, time and adding amount of reactants are controlled, the oxidation process of graphite is ensured to be more sufficient, the control accuracy of the reaction process is higher, the reaction efficiency is improved by matching with a temperature control device, and the influence of external environmental factors is reduced.
Drawings
FIG. 1 is a schematic diagram of an automatic feed control graphite oxidation reaction apparatus according to the present utility model.
Legend description: 1. a reaction kettle body; 2. a motor; 21. a stirrer; 3. a first feed port; 31. a raw material feeder; 32. a first valve; 4. a second feed inlet; 41. a solid material feed inlet; 42. a screw feeder; 43. a second valve; 5. a third feed inlet; 51. a liquid material storage tank; 52. a third main valve; 53. a third valve; 54. a first peristaltic pump; 6. a discharge hole; 7. a jacket; 8. a temperature control device; 81. a temperature controller C-H1; 82. a second peristaltic pump; 9. a sensor monitoring port; 10. a visual window; 11. automatically controlling the valve; 12. a manual safety valve.
Detailed Description
The technical solutions of the embodiments of the present utility model will be clearly and completely described below in conjunction with the embodiments of the present utility model, and it is apparent that the described embodiments are only some embodiments of the present utility model, but not all embodiments, and all other embodiments obtained by those skilled in the art without making any inventive effort based on the embodiments of the present utility model are within the scope of protection of the present utility model.
In order that the utility model may be readily understood, a more particular description of the utility model will be rendered by reference to specific embodiments thereof which are, however, not limited to the embodiments described herein, but are to be provided for the purpose of making the disclosure of the utility model more thorough.
It will be understood that when an element is referred to as being "mounted" on another element, it can be directly on the other element or intervening elements may also be present, and when an element is referred to as being "connected" to the other element, it may be directly connected to the other element or intervening elements may also be present, the terms "vertical", "horizontal", "left", "right" and the like are used herein for the purpose of illustration only.
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 utility model belongs, and the terms used herein in this description of the utility model are for the purpose of describing particular embodiments only and are not intended to be limiting of the utility model, with the term "and/or" as used herein including any and all combinations of one or more of the associated listed items.
Examples
As shown in fig. 1, the present utility model provides a technical solution: the graphite oxidation reaction device with automatic feed control comprises a reaction kettle body 1, wherein a motor 2 is arranged at the top end of the reaction kettle body 1, a first feed inlet 3, a second feed inlet 4 and a third feed inlet 5 are sequentially arranged at the top end of the reaction kettle body 1 from right to left, a discharge hole 6 is formed in the bottom of the reaction kettle body 1, a jacket 7 is arranged on the periphery of the bottom of the reaction kettle body 1, and a temperature control device 8 is arranged on the right side of the jacket 7;
the first feed inlet 3 is connected with a raw material feeder 31, the raw material feeder 31 is preferably of a funnel-shaped structure, and a first valve 32 is arranged between the first feed inlet 3 and the raw material feeder 31; the first valve 32 of the raw material feeder 31 is connected, and the reaction raw material, which does not need to control the feeding amount, can be fed through the raw material feeder 31.
The second feeding port 4 is connected with a solid material feeding port 41, and a screw feeder 42 and a second valve 43 are sequentially arranged between the solid material feeding port 41 and the second feeding port 4; the solid material feed port 41 is connected with the valve 4, the material with the feed amount to be controlled is fed by the screw feeder 42, and the material enters the reaction kettle body 1 after passing through the second valve 43.
The third feed inlet 5 is connected with two liquid material storage tanks 51, a third total valve 52 is arranged near the joint of the third feed inlet 5, and a third valve 53 and a first peristaltic pump 54 are sequentially arranged between the two liquid material storage tanks 51 and the third total valve 52; the third feeding port 5 is connected with a third total valve 52, liquid materials required by the reaction can be stored through two liquid material storage tanks 51, the feeding quantity is controlled through two groups of first peristaltic pumps 54 corresponding to feeding, and the third total valve 52 and a third valve 53 can control liquid feeding switches.
Further, the reaction kettle body 1 is made of 316L stainless steel, and a polytetrafluoroethylene coating lining is arranged on the inner wall of the reaction kettle body 1.
Further, the output end of the motor 2 is provided with a stirrer 21 extending to the inside of the reaction kettle body 1.
Further, a sensor monitoring port 9 and a visual window 10 are sequentially arranged on the right side of the first feed port 3; the sensor monitoring port 9 includes a temperature and pressure sensor.
Further, the lower end of the discharging hole 6 is sequentially connected with an automatic control valve 11 and a manual safety valve 12, wherein the manual safety valve 12 is in a normally open state.
Further, the temperature control device 8 comprises a temperature controller C-H181, the temperature controller C-H181 is circularly communicated with the jacket 7 through a pipeline, cold and hot oil liquid is injected into the jacket 7, and a second peristaltic pump 82 is arranged between the jacket 7 and the temperature controller C-H181; the jacket 7 can control the temperature of the reaction kettle body 1 through cold and hot oil, the temperature of the cold and hot oil in the jacket 7 is controlled by a temperature controller C-H181, and the circulation of the cold and hot oil in the jacket 7 is realized by the temperature controller C-H181.
The working flow is as follows:
(1) Setting the temperature of the high-low temperature controller C-H1 to be minus 10 ℃, and checking the reaction temperature of the reactor to be between 0 ℃ and 5 ℃ through a sensor monitoring port 9 of the body 1 of the reaction kettle body 1;
(2) Opening a first valve 32 of the reaction kettle body 1 from the top of the reaction kettle body 1, sequentially adding a certain amount of sodium nitrate and concentrated sulfuric acid into the cavity through a raw material feeder 31, and closing the first valve 32;
(3) Controlling the stirrer 21 driven by the motor 2 to rotate at 200r/min, then opening a second valve 43, slowly adding graphite powder by using the screw feeder 42, controlling the feeding amount to be 3g/min, and closing the second valve 43 after the feeding is finished;
(4) Stirring for 30min at the temperature of less than 5 ℃ in the reaction kettle body 1, continuously adding 150g of potassium permanganate into the reaction kettle body 1 through the screw feeder 42, controlling the feeding time for 30min and the feeding rate for 5g/min;
(5) Closing the screw feeder 42;
(6) Heating the reaction temperature of the system from 5 ℃ to 35 ℃ through a temperature controller C-H181, and controlling the heating time to be 30min;
(7) The reaction system is kept at a constant temperature of 35 ℃ for 240min; opening a third main valve 52 and one of the third valves 53, opening a first peristaltic pump 54 communicated with the third valve 53, adding 1500mL of deionized water into the reaction kettle body 1, and feeding water for 30min according to the flow rate of 12 revolutions per minute; after the water inlet is finished, the third valve 53 and the first peristaltic pump 54 are closed;
(8) Heating the reaction temperature of the system to 98 ℃ through a temperature controller C-H1, and controlling the heating time to be 30min;
(9) Setting the temperature to 98 ℃ by an external controller, and keeping the temperature constant; simultaneously opening another group of third valve 53 and first peristaltic pump 54, adding hydrogen peroxide into the reaction kettle body 1, and setting the rotating speed of the first peristaltic pump 54 to be 6 revolutions per minute; after the hydrogen peroxide is fed, the third main valve 52 and the third valve 53 are closed, and the first peristaltic pump 54 is closed; after 30min of reaction, the reaction process was ended.
Although embodiments of the present utility model have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the utility model, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. The utility model provides an automatic graphite oxidation reaction unit of feeding control, includes reation kettle body (1), its characterized in that: the novel reaction kettle comprises a reaction kettle body (1), wherein a motor (2) is arranged at the top end of the reaction kettle body (1), a first feed inlet (3), a second feed inlet (4) and a third feed inlet (5) are sequentially formed in the top end of the reaction kettle body (1) from right to left, a discharge hole (6) is formed in the bottom of the reaction kettle body (1), a jacket (7) is arranged on the periphery of the bottom of the reaction kettle body (1), and a temperature control device (8) is arranged on the right side of the jacket (7);
the first feeding port (3) is connected with a raw material feeder (31), and a first valve (32) is arranged between the first feeding port (3) and the raw material feeder (31);
the second feeding port (4) is connected with a solid material feeding port (41), and a screw feeder (42) and a second valve (43) are sequentially arranged between the solid material feeding port (41) and the second feeding port (4);
the third feeding port (5) is connected with two liquid material storage tanks (51), a third total valve (52) is arranged near the joint of the third feeding port (5), and a third valve (53) and a first peristaltic pump (54) are sequentially arranged between the two liquid material storage tanks (51) and the third total valve (52).
2. An automatic feed controlled graphite oxidation reaction apparatus according to claim 1, wherein: the reaction kettle body (1) is made of 316L stainless steel, and a polytetrafluoroethylene coating lining is arranged on the inner wall of the reaction kettle body (1).
3. An automatic feed controlled graphite oxidation reaction apparatus according to claim 1, wherein: the output end of the motor (2) is provided with a stirrer (21) extending to the inside of the reaction kettle body (1).
4. An automatic feed controlled graphite oxidation reaction apparatus according to claim 1, wherein: the right side of the first feeding hole (3) is provided with a sensor monitoring hole (9) and a visual window (10) in sequence.
5. An automatic feed controlled graphite oxidation reaction apparatus according to claim 1, wherein: the lower end of the discharging hole (6) is sequentially connected with an automatic control valve (11) and a manual safety valve (12).
6. An automatic feed controlled graphite oxidation reaction apparatus according to claim 1, wherein: the temperature control device (8) comprises a temperature controller C-H1 (81), the temperature controller C-H1 (81) is circularly communicated with the jacket (7) through a pipeline, cold and hot oil liquid is injected into the jacket (7), and a second peristaltic pump (82) is further arranged between the jacket (7) and the temperature controller C-H1 (81).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322126415.0U CN220559175U (en) | 2023-08-08 | 2023-08-08 | Graphite oxidation reaction device with automatic feeding control function |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202322126415.0U CN220559175U (en) | 2023-08-08 | 2023-08-08 | Graphite oxidation reaction device with automatic feeding control function |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN220559175U true CN220559175U (en) | 2024-03-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202322126415.0U Active CN220559175U (en) | 2023-08-08 | 2023-08-08 | Graphite oxidation reaction device with automatic feeding control function |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN220559175U (en) |
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2023
- 2023-08-08 CN CN202322126415.0U patent/CN220559175U/en active Active
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