CN114307933B - Equipment for preparing graphene oxide and production method - Google Patents
Equipment for preparing graphene oxide and production method Download PDFInfo
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- CN114307933B CN114307933B CN202210146533.5A CN202210146533A CN114307933B CN 114307933 B CN114307933 B CN 114307933B CN 202210146533 A CN202210146533 A CN 202210146533A CN 114307933 B CN114307933 B CN 114307933B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 42
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 191
- 238000002347 injection Methods 0.000 claims abstract description 179
- 239000007924 injection Substances 0.000 claims abstract description 179
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 64
- 239000007800 oxidant agent Substances 0.000 claims abstract description 56
- 239000000203 mixture Substances 0.000 claims abstract description 55
- 230000001590 oxidative effect Effects 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 52
- 238000004806 packaging method and process Methods 0.000 claims description 33
- 239000000047 product Substances 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 26
- 238000004891 communication Methods 0.000 claims description 23
- 238000000967 suction filtration Methods 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 16
- 239000010439 graphite Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- 238000007789 sealing Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 13
- 239000002351 wastewater Substances 0.000 claims description 13
- 239000007795 chemical reaction product Substances 0.000 claims description 12
- 238000003860 storage Methods 0.000 claims description 12
- 239000011148 porous material Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 6
- 230000002159 abnormal effect Effects 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000007726 management method Methods 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 238000010667 large scale reaction 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
- 230000003647 oxidation Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
Abstract
The invention discloses a device for preparing graphene oxide, which comprises: the reaction device is provided with a reaction kettle, and can move to the reaction finished product area from the mixture injection area to the reaction finished product area through the oxidant injection area and the reducing agent injection area in sequence, wherein metering injection openings are respectively arranged in the mixture injection area, the oxidant injection area and the reducing agent injection area; the invention also discloses a production method for preparing the graphene oxide, and the equipment for preparing the graphene oxide has the characteristic of capability of sequentially processing in small batches and multiple batches.
Description
Technical Field
The invention relates to the technical field of preparation of carbon nano materials, in particular to equipment for preparing graphene oxide and a production method thereof.
Background
The graphene oxide is an oxide of graphene, has more oxygen-containing functional groups on the surface, can be modified, and can be better mixed and modified with other materials compared with the graphene, so that the graphene oxide has wider application and wide chemical modification research prospect.
At present, the preparation mode of graphene oxide is a traditional chemical reaction industry design, and a production line is fixed through a fixed reaction kettle, and the process has the following defects:
The productivity limitation can only be determined according to the size of the reaction kettle, and the increase of the productivity can only be solved by increasing the production line;
Reagent waste, and industrial production often requires excessive strong oxidant to achieve a certain effect;
In addition, the existing technology requires a reaction time longer than 6 hours, the size of the obtained product is reduced due to long-time oxidation reaction and mechanical stirring, and the surface defects of the graphene are excessive, so that the subsequent use is seriously affected;
Poor production environment, frequent shutdown cleaning, and difficult production environment and equipment cleaning;
potential safety hazards, a large amount of strong oxidants are added at a time, the reaction temperature is rapidly increased, and production safety problems such as pipeline and reaction kettle breakage are easily caused.
Disclosure of Invention
The invention aims to provide equipment and a production method for preparing graphene oxide, which can be used for sequentially processing small batches and multiple batches.
In order to achieve the above object, the present invention adopts the following technical scheme.
An apparatus for preparing graphene oxide, comprising: the reaction device is provided with a reaction kettle, and can move to the reaction finished product area from the mixture injection area through the oxidant injection area and the reducing agent injection area in sequence, wherein the mixture injection area, the oxidant injection area and the reducing agent injection area are respectively provided with a metering injection port.
The equipment for preparing the graphene oxide further comprises a control system, the control system is arranged on the reaction device, the mixed material injection area is provided with a resonance sound mixing device, the reaction device is further provided with a bar code area, the mixed material injection area, the oxidant injection area and the reducing agent injection area are respectively provided with a code scanning sensor, the bar code area and the code scanning sensors are all in communication connection with the control system, and the code scanning sensors can identify the code scanning area.
The top of reation kettle is formed with the feed inlet, reation kettle's bottom is equipped with agitating unit, agitating unit drives by the motor and rotates, agitating unit's inside is provided with the discharge gate, the discharge gate passes through the discharging pipe and communicates to a suction filtration device, suction filtration device is equipped with the bung hole that can supply the packing bucket activity business turn over, reaction unit still has measurement conveyer, be equipped with the baffle that two intervals set up on the measurement conveyer, the packing bucket can block between the baffle, control system and equal communication connection of agitating unit, motor, suction filtration device and measurement conveyer.
The packaging barrel is provided with a barrel bar code, the reaction device is further provided with a packaging barrel groove extending from top to bottom, the reaction device is provided with a code scanner, the code scanner is positioned at the bottom of the packaging barrel groove, the packaging barrel can move downwards from the top of the packaging barrel groove until the packaging barrel falls between two baffles of the metering and conveying device, and the control system is in communication connection with the code scanner and the barrel bar code of the packaging barrel.
The reaction device is further provided with a storage barrel for storing the reducing agent, an inlet is formed in the top of the storage barrel, the storage barrel is communicated to a feed inlet of the reaction kettle through a first pipeline, and a first flow control valve is arranged on the first pipeline.
The reaction kettle is internally provided with a viscometer device and a temperature PH device, and the viscometer device and the temperature PH device are both in communication connection with a control system.
The bottom of reaction unit is equipped with water inlet and outlet, the bottom of reaction product district is equipped with water inlet and delivery port, reaction unit's water inlet selectivity and reaction product district's water inlet intercommunication, reaction unit's outlet selectivity and reaction product district's delivery port intercommunication, reaction unit's water inlet communicates to the reation kettle through the inlet tube in, be equipped with a second flow control valve on the inlet tube, the inlet tube communicates in the top of second flow control valve has a downward drain pipe of slope, suction filtration device's bottom communicates to the drain pipe, the top of drain pipe is equipped with a third flow control valve, the drain pipe selectivity communicates to reaction unit's outlet, second flow control valve and third flow control valve all are connected with control system communication, the second flow control valve is located under the drain pipe.
A waste water collecting tank is further arranged between the bottom of the drain pipe and the water outlet of the reaction device, a fourth flow control valve is arranged at the position, between the waste water collecting tank and the suction filtration device, of the drain pipe, a fifth flow control valve is arranged between the waste water collecting tank and the water outlet of the reaction device, a limiting PH sensor is arranged in the waste water collecting tank, and the control system is in communication connection with the fourth flow control valve, the fifth flow control valve and the limiting PH sensor.
The production method for preparing the graphene oxide, which is applied to the equipment for preparing the graphene oxide, comprises the following steps of: the mixture injection area is provided with a mixture of concentrated sulfuric acid and graphite; the reaction device moves to a mixture injection area, and a metering injection port of the mixture injection area injects a mixture of concentrated sulfuric acid and graphite into a reaction kettle of the reaction device; then the reaction device moves to an oxidant injection area, and a metering injection port of the oxidant injection area injects oxidant into a reaction kettle of the reaction device; then the reaction device moves to a reducing agent injection area, and a metering injection port of the reducing agent injection area injects reducing agent into a reaction kettle of the reaction device; then the reaction device moves to a reaction finished product area, and graphene oxide finished products in the reaction kettle are output through the reaction finished product area; and finally, the reaction device moves to a mixture injection area for the next round of circular production.
The equipment for preparing the graphene oxide further comprises a control system, wherein the control system is arranged on the reaction device, the mixed material injection area is provided with a resonance sound mixing device, the reaction device is further provided with a bar code area, the mixed material injection area, the oxidant injection area and the reducing agent injection area are respectively provided with a code scanning sensor, the bar code area and the code scanning sensors are in communication connection with the control system, and the code scanning sensors can identify and scan the bar code area; the control system can receive the proportioning input of the concentrated sulfuric acid and the graphite, calculate the injection quantity of the mixture, the injection quantity of the oxidant and the injection quantity of the reducing agent, and enable the bar code area of the reaction device to correspondingly form a specific bar code; when the code scanning sensor of the mixture injection area recognizes the code scanning area, the mixture injection area can obtain the injection quantity of the mixture calculated by the control system, and the injection quantity of the mixture calculated by the control system is injected into the reaction kettle of the reaction device through the metering injection port of the mixture injection area; when the scanning bar code area is identified by the bar code scanning sensor of the oxidant injection area, the oxidant injection area can obtain the injection amount of the oxidant calculated by the control system, and the injection amount of the oxidant calculated by the control system is injected into a reaction kettle of the reaction device through a metering injection port of the oxidant injection area; when the scanning bar code area is identified by the scanning sensor of the reducing agent injection area, the reducing agent injection area can obtain the injection amount of the reducing agent calculated by the control system, and the injection amount of the reducing agent calculated by the control system is injected into the reaction kettle of the reaction device through the metering injection port of the reducing agent injection area.
After the technical scheme is adopted, the reaction device, the mixture injection area, the oxidant injection area, the reducing agent injection area and the reaction finished product area are matched, and the reaction device can be movably moved to the reaction finished product area from the mixture injection area to the reaction finished product area in sequence through the oxidant injection area and the reducing agent injection area, so that the mixture, the oxidant and the reducing agent can be sequentially added into a reaction kettle of the reaction device, and the small-batch and multi-batch sequential treatment is realized.
Drawings
Fig. 1 is a schematic view of an apparatus for preparing graphene oxide according to the present invention.
FIG. 2 is a schematic view of the reaction apparatus of the present invention.
FIG. 3 is a schematic view of the stirring device of the present invention.
[ Symbolic description ]
Reaction apparatus 1
Bar code area 12 of reaction kettle 11
Sealing plate 1111
Feed inlet 13 stirring device 14
First filter screen 142 of dispersing blade 141
Second screen 143 third screen 144
Fourth screen 145 sealing plate 146
Air hole 147
Discharge hole 16 of motor 15
Suction filtration device 18 of discharging pipe 17
Bung 181 drain pipe 182
Third flow control valve 183 fourth flow control valve 184
Metering conveyor 19
Baffle 191
Packaging barrel 101 packaging barrel groove 102
Storage barrel 104 of code scanner 103
Inlet 1041 first conduit 1042
First flow control valve 1043
Viscometer apparatus 105 temperature PH 106
Water inlet 107 and outlet 108
Fifth flow control valve 1081
Second flow control valve 1072 of water inlet pipe 1071
Waste water collecting tank 109
Limit PH sensor 1091
Transfer wheel 111 stabilizing block 112
Alarm 114 of circulating water chiller 113
Mixture injection zone 2
Resonant acoustic mixing device 21
Oxidant injection zone 3
Reducing agent injection zone 4
Reaction product zone 5
Water inlet 51 and water outlet 52
Conveyor 53
And a control system 6.
Detailed Description
The invention will be described in further detail with reference to the drawings and the specific examples.
Referring to fig. 1 to 3, the present invention discloses an apparatus for preparing graphene oxide, comprising: the reaction device 1 and the mixture injection area 2, the oxidant injection area 3, the reducing agent injection area 4 and the reaction finished product area 5 which are sequentially arranged, wherein the reaction device 1 is provided with a reaction kettle 11, the reaction device 1 can be movably and sequentially moved from the mixture injection area 2 to the reaction finished product area 5 through the oxidant injection area 3 and the reducing agent injection area 4, and the mixture injection area 2, the oxidant injection area 3 and the reducing agent injection area 4 are respectively provided with metering injection openings.
In order to facilitate the realization of automatic control and intelligent automatic production, the equipment for preparing graphene oxide further comprises a control system 6, wherein the control system 6 is arranged on the reaction device 1, the mixed material injection region 2 is provided with a resonance sound mixing device 21, the reaction device 1 is further provided with a bar code region 12, the mixed material injection region 2, the oxidant injection region 3 and the reducing agent injection region 4 are respectively provided with a code scanning sensor, the bar code region 12 and the code scanning sensor are in communication connection with the control system 6, the code scanning sensor can identify the scanning bar code region 12, graphite and concentrated sulfuric acid can be pre-intercalated in advance through the arrangement of the resonance sound mixing device 21, the intercalation time is reduced, and meanwhile, the time for separating graphite sheets into subsequent oxidation reactions to the greatest extent by resonance sound mixing can be greatly reduced; wherein the resonance sound mixing device 21 is required to be at an ultralow temperature, and the ultralow temperature is in the range of-35-0 ℃.
Then, the reaction device 1 may further be provided with a circulation water chiller 113, a cold water pipe of the circulation water chiller 113 is communicated to a kettle wall cavity of the reaction kettle 11, the control system 6 is in communication connection with the circulation water chiller 113, the reaction kettle 11 can be kept at a proper reaction temperature by using the arrangement of the circulation water chiller 113, and the circulation water chiller 113 is controlled to be started by the control system 6.
In order to facilitate accelerating the reaction, a feed inlet 13 is formed at the top of the reaction kettle 11, a stirring device 14 is arranged at the bottom of the reaction kettle 11, the stirring device 14 is driven to rotate by a motor 15, and a discharge outlet 16 is arranged in the stirring device 14; wherein the stirring device 14 performs low-speed stirring, and the stirring speed is more than 1000r/min.
Referring to fig. 3, the stirring device 14 includes dispersing blades 141, a first filter screen 142, a second filter screen 143, a third filter screen 144, a fourth filter screen 145, a sealing plate 146, and an air hole 147, wherein the first filter screen 142, the second filter screen 143, the third filter screen 144, the fourth filter screen 145, the sealing plate 146, and the air hole 147 define a cylindrical barrel; wherein, the pore size of the first filter screen 142 is larger than the pore size of the second filter screen 143, the pore size of the third filter screen 144 is larger than the pore size of the fourth filter screen 145; in practice, the fourth screen 145 is 10-30 microns in size, the third screen 144 is 30-60 microns in size, the second screen 143 is 60-100 microns in size, and the first screen 142 is greater than 100 microns in size; the first filter screen 142, the second filter screen 143, and the third filter screen 144 are respectively used for collecting products with different sizes, and the filter screens can be added or reduced according to the actual required product sizes, when the fourth filter screen 145 is used for washing, the sealing plate 146 is used for reaction, and when the air hole 147 is used for cleaning reaction; the discharge port 16 is selectively opposite to the first filter screen 142, the second filter screen 143, the third filter screen 144, the fourth filter screen 145, the sealing plate 146 or the hollow 147, and the discharge port 16 is selectively communicated with the first filter screen 142, the second filter screen 143, the third filter screen 144, the fourth filter screen 145 or the hollow 147. Wherein, the discharge port 16 is communicated to a suction filtration device 18 through a discharge pipe 17, the suction filtration device 18 is provided with a barrel port 181 for the movable in-out of the packaging barrel 101, and most of water can be removed by suction filtration by the arrangement of the suction filtration device 18, so as to form a filter cake.
Further, in order to facilitate conveying the packaging barrel 101, the reaction device 1 is further provided with a metering and conveying device 19, two baffles 191 are arranged on the metering and conveying device 19 at intervals, the packaging barrel 101 can be clamped between the baffles 191, and the control system 6 is in communication connection with the stirring device 14, the motor 15, the suction filtration device 18 and the metering and conveying device 19; when the invention is in the cleaning state, the baffle 191 moves to the bung 181 of the suction filtration device 18 and seals the bung 181 of the suction filtration device 18.
The packaging barrel 101 can be provided with a barrel bar code, the reaction device 1 is also provided with a packaging barrel groove 102 extending from top to bottom, the reaction device 1 is provided with a code scanner 103, the code scanner 103 is positioned at the bottom of the packaging barrel groove 102, the packaging barrel 101 can move downwards from the top of the packaging barrel groove 102 until falling between two baffles 191 of the metering and conveying device 19, and the control system 6 is in communication connection with the code scanner 103 and the barrel bar code of the packaging barrel 101, so that the management control of the packaging barrel 101 is realized; the control system 6 may perform information characterization by scanning the barrel bar code of the packaging barrel 101 to control different packaging barrels 101 to hold different sized products.
Further, a storage tank 104 for storing the reducing agent is further provided on the reaction device 1, an inlet 1041 is provided at the top of the storage tank 104, the storage tank 104 is connected to the feed inlet 13 of the reaction kettle 11 through a first pipeline 1042, and a first flow control valve 1043 is provided on the first pipeline 1042, so that the reducing agent can be slowly introduced to remove the remaining oxidizing agent, thereby preventing the introduction of new impurities due to the quantitative addition of the reducing agent.
The reaction device 1 may further be provided with an alarm device 114, and the alarm device 114 may alarm an abnormal injection, abnormal temperature, abnormal barcode scanning, abnormal water inflow, etc.
In order to facilitate the control of viscosity, temperature and PH value, a viscometer device 105 and a temperature PH device 106 are arranged in the reaction kettle 11, and the viscometer device 105 and the temperature PH device 106 are both in communication connection with the control system 6, so that the invention can more visually present the degree of graphite oxidation reaction through the viscosity, temperature and PH value feedback curve, thereby controlling the reaction time, reducing the reduction of the diameter of graphite sheets and the increase of edge abnormal defects caused by excessive oxidation, reducing the rotating speed of mechanical stirring of subsequent reaction after pre-intercalation treatment, and preparing large-diameter graphene oxide, wherein the particle diameter of finished graphene oxide is more than 50um, even if the particle diameter of large-diameter graphene oxide is large.
Furthermore, the bottom of the reaction device 1 may be provided with a water inlet 107 and a water outlet 108, the bottom of the reaction product area 5 is provided with a water inlet 51 and a water outlet 52, the water inlet 107 of the reaction device 1 is selectively communicated with the water inlet 51 of the reaction product area 5, the water outlet 108 of the reaction device 1 is selectively communicated with the water outlet 52 of the reaction product area 5, the water inlet 107 of the reaction device 1 is communicated into the reaction kettle 11 through a water inlet pipe 1071, the water inlet pipe 1071 is provided with a second flow control valve 1072, the water inlet pipe 1071 is communicated with a drain pipe 182 which is inclined downwards above the second flow control valve 1072, the bottom of the suction filtration device 18 is communicated with the drain pipe 182, the top of the drain pipe 182 is provided with a third flow control valve 183, the drain pipe 182 is selectively communicated with the water outlet 108 of the reaction device 1, the second flow control valve 1072 and the third flow control valve 183 are all connected with the control system 6 in a communication manner, and the second flow control valve 1072 is positioned below the drain pipe 182.
In order to collect the waste water conveniently, a waste water collecting tank 109 may be further disposed between the bottom of the drain pipe 182 and the drain port 108 of the reaction device 1, a fourth flow control valve 184 is disposed at a position between the drain pipe 182 and the suction filtration device 18, a fifth flow control valve 1081 is disposed between the drain pipe 109 and the drain port 108 of the reaction device 1, a limiting PH sensor 1091 is disposed in the drain pipe 109, and the control system 6 is in communication connection with the fourth flow control valve 184, the fifth flow control valve 1081 and the limiting PH sensor 1091.
Wherein, the reaction product area 5 is also provided with a conveying device 53, and the conveying device 53 of the reaction product area 5 is in butt joint with the metering conveying device 19.
Further, a transfer wheel 111 is further disposed at the bottom of the reaction device 1, the transfer wheel 111 may be a lifting wheel, and the control system 6 is communicatively connected to the transfer wheel 111.
The resonance sound mixing device 21 can be provided with a liquid nitrogen cooling device, wherein the temperature of the liquid nitrogen cooling device is-35-0 ℃, the frequency is 80-200Hz, the amplitude is 1-2.5mm, and the treatment time can be 15-60 minutes.
In addition, a stabilizing block 112 is provided at the bottom of the reaction apparatus 1.
Further, a sealing plate 1111 is disposed in the middle of the reaction kettle 11, the temperature PH device 106 and the viscometer device 105 are disposed on the sealing plate 1111, the stirring device 14 is disposed below the sealing plate 1111, the temperature probe and the PH probe of the temperature PH device 106 extend below the sealing plate 1111, the viscosity probe of the viscometer device 105 extends below the sealing plate 1111, the feed inlet 13 is communicated to the below of the sealing plate 1111, and the control system 6 is in communication connection with the temperature PH device 106 and the viscometer device 105.
From the above, the control of each flow control valve of the reaction device 1 can reduce the use of water, increase the utilization rate, reduce the production cost, and simultaneously upload real-time production data to provide simple management and calculation for producers; the movable computer-controlled reaction device can reduce labor cost and potential safety hazards, and graphene oxide with different sheet diameter sizes can be automatically classified through the cooperation of the first filter screen 142, the second filter screen 143 and the third filter screen 144, so that convenience is provided for subsequent downstream application and sales; the factory can plan a large-scale reaction finished product area and can continuously produce and increase the productivity.
The invention also discloses a production method for preparing graphene oxide, which applies the equipment for preparing graphene oxide and comprises the following steps: the mixture injection area 2 is used for storing a mixture of concentrated sulfuric acid and graphite; the reaction device 1 moves to a mixture injection area 2, and a metering injection port of the mixture injection area 2 injects a mixture of concentrated sulfuric acid and graphite into a reaction kettle 11 of the reaction device 1; then the reaction device 1 moves to an oxidant injection area 3, and a metering injection port of the oxidant injection area 3 injects oxidant into a reaction kettle 11 of the reaction device 1; then the reaction device 1 moves to a reducing agent injection area 4, and a metering injection port of the reducing agent injection area 4 injects reducing agent into a reaction kettle 11 of the reaction device 1; then the reaction device 1 moves to a reaction finished product area 5, and graphene oxide finished products in the reaction kettle 11 are output through the reaction finished product area 5; finally, the reaction device 1 moves to a mixture injection area 2 for the next round of circular production; wherein, the weight ratio of graphite to concentrated sulfuric acid is 1:10 to 60.
The equipment for preparing the graphene oxide further comprises a control system 6, wherein the control system 6 is arranged on the reaction device 1, the mixed material injection region 2 is provided with a resonance sound mixing device 21, the reaction device 1 is further provided with a bar code region 12, the mixed material injection region 2, the oxidant injection region 3 and the reducing agent injection region 4 are respectively provided with a code scanning sensor, the bar code region 12 and the code scanning sensors are in communication connection with the control system 6, and the code scanning sensors can identify the code scanning region 12; the control system 6 can receive the proportioning input of the concentrated sulfuric acid and the graphite, calculate the injection quantity of the mixture, the injection quantity of the oxidant and the injection quantity of the reducing agent, and enable the bar code area 12 of the reaction device 1 to correspondingly form a specific bar code; when the code scanning sensor of the mixture injection area 2 recognizes the scanning bar code area 12, the mixture injection area 2 can acquire the injection quantity of the mixture calculated by the control system 6, and the injection quantity of the mixture calculated by the control system 6 is injected into the reaction kettle 11 of the reaction device 1 through the metering injection port of the mixture injection area 2; when the scanning bar code area 12 is identified by the bar code scanning sensor of the oxidant injection area 3, the oxidant injection area 3 can acquire the injection amount of the oxidant calculated by the control system 6, and the injection amount of the oxidant calculated by the control system 6 is injected into the reaction kettle 11 of the reaction device 1 through the metering injection port of the oxidant injection area 3; when the scanning bar code area 12 is identified by the scanning bar code sensor of the reducing agent injection area 4, the reducing agent injection area 4 can know the injection amount of the reducing agent calculated by the control system 6, and the injection amount of the reducing agent calculated by the control system 6 is injected into the reaction kettle 11 of the reaction device 1 through the metering injection port of the reducing agent injection area 4.
The invention judges whether the reaction is finished or not through the change of the viscosity of the system after the reaction, wherein the viscosity of the reaction system is the curve change, the judgment is carried out through the measurement of the slope of the curve, and when the curve is gradually gentle, the reaction is finished after the slope is lower than a set value (PH curve is the same); in practice, when the tangential slope of the viscosity curve is in the range of 0-0.05, the reaction is nearly gentle and ended; wherein the water inlet 107 of the reaction apparatus 1 is fed into the reaction vessel 11 through the water inlet pipe 1071 by controlling the second flow control valve 1072 to be opened, and the reaction vessel 11 is cleaned to terminate the reaction.
Therefore, according to the invention, through the cooperation design of the reaction device 1, the mixture injection area 2, the oxidant injection area 3, the reducing agent injection area 4 and the reaction finished product area 5, as the reaction device 1 can move from the mixture injection area 2 to the reaction finished product area 5 in sequence through the oxidant injection area 3 and the reducing agent injection area 4, the mixture, the oxidant and the reducing agent can be sequentially added into the reaction kettle 11 of the reaction device 1, and the small-batch and multi-batch sequential treatment can be realized.
The invention can sequentially process small batches and multiple batches, can directly increase the productivity according to actual needs, reduces the reaction time through pre-intercalation treatment, simultaneously reduces the labor cost by adopting a modern design full-automatic process, reduces the waste of chemical reagents in small batches, ensures the quality of products, improves the environment of automatic production, improves the safety performance, changes the traditional chemical production process technology, and improves the production productivity and the product quality by adopting modern equipment and processes.
In actual production, the production method for preparing graphene oxide of the invention comprises the following steps: adding concentrated sulfuric acid and graphite in a certain proportion into the resonance sound mixing device 21, and mixing for 15-60 minutes at a low temperature for standby; the control system 6 receives the proportioning input of the concentrated sulfuric acid and the graphite, calculates the injection quantity of the mixture, the injection quantity of the oxidant and the injection quantity of the reducing agent, and enables the bar code area 12 of the reaction device to correspondingly form a specific bar code; the reaction device 1 starts the circulating water chiller 113 to keep the reaction temperature; driving a conveying wheel 111 of the reaction device 1 to enter a mixture injection area 2, and scanning a bar code scanning sensor of the mixture injection area 2 to set a bar code area 12 for automatic injection according to a formula; Starting a stirring device 14 to stir at a low speed, and entering an oxidant injection area 3, wherein a code scanning sensor of the oxidant injection area 3 scans a bar code area 12 to automatically inject materials according to a formula; entering a reducing agent injection area 4, wherein a code scanning sensor of the reducing agent injection area 4 scans a bar code area 12 to automatically inject materials according to a formula, and the reducing agent is injected into a storage vat; the method comprises the steps that a conveying wheel 111 enters a designated place of a reaction finished product area 5, the conveying wheel 111 is lifted to enable a water inlet 107 and a water outlet 108 of a reaction device 1 to be communicated with a water inlet 51 and a water outlet 52 of the reaction finished product area 5, when a viscosity curve is close to gentle, a tangential slope of the viscosity curve reaches a set value, a first flow control valve 1043 is started to slowly introduce a reducing agent to remove residual reducing agent and slowly introduce the reducing agent to remove residual oxidizing agent, when a temperature and PH curve is stable, the addition of the reducing agent is finished, meanwhile, the consumption of an actual reducing agent is fed back, stirring is stopped, and the temperature and PH curve are measured by a temperature PH meter; Opening the second flow control valve 1072 to feed water, simultaneously controlling the motor 15 to rotate anticlockwise until the fourth filter screen 145 of the stirring device 14 is out, stirring clockwise to clean, and opening the fourth flow control valve 184 to inject washing water into the waste water collecting tank 109; after the set PH value is reached, the fourth flow control valve 183 is closed, stirring is stopped, meanwhile, the code scanner 103 scans the barrel bar code of the packaging barrel 101, and the packaging barrel 101 enters the metering and conveying device 19 to be weighed and conveyed into the suction filtration device 18; the motor 15 is controlled to rotate anticlockwise to the third filter screen 144 of the stirring device 14 and then stir clockwise, the third flow control valve 183 is opened, the flow of the second flow control valve 1072 is reduced or closed, suction filtration is started, at the moment, the fourth flow control valve 184 is closed, filtrate returns to the reaction kettle 11 through the third flow control valve 183, the product size is not influenced by the recycling of the filtrate, and after the suction filtration is finished, the packaging barrel 101 enters the metering and conveying device 19 to be weighed and conveyed to the conveying device 53 of the reaction finished product area 5; Repeating the operation of the storage vat 104 and the operation of the motor 15 until the stirring device 14 rotates from the second filter screen 143 to the first filter screen 142 to the empty port 147, then closing the third flow control valve 183, increasing the flow of the second flow control valve 1072, opening the fourth flow control valve 184, stirring and cleaning the reaction kettle 11 for 2-3 times, recording the capacity and PH after the water level of the wastewater collection tank 109 reaches the limit PH sensor 1091, feeding back to the control system 6 to the terminal, and simultaneously opening the fifth flow control valve 1081 for water drainage; after draining, the transfer wheel 111 is lowered to perform the next cycle.
The above description is only of the preferred embodiments of the present invention, and should not be taken as limiting the technical scope of the present invention, but all changes and modifications that come within the scope of the invention as defined by the claims and the specification are to be embraced by the invention.
Claims (8)
1. An apparatus for preparing graphene oxide, comprising: the reaction device is provided with a reaction kettle, and can move to the reaction finished product area from the mixture injection area to the reaction finished product area through the oxidant injection area and the reducing agent injection area in sequence, wherein metering injection openings are respectively arranged in the mixture injection area, the oxidant injection area and the reducing agent injection area; the device comprises a reaction device, a mixed material injection area, a reducing agent injection area, a bar code area, a control system and a control system, wherein the control system is arranged on the reaction device, the mixed material injection area is provided with a resonance sound mixing device, the reaction device is also provided with a bar code area, the mixed material injection area, the oxidizing agent injection area and the reducing agent injection area are respectively provided with a code scanning sensor, the bar code area and the code scanning sensors are all in communication connection with the control system, and the code scanning sensors can identify and scan the bar code area; the top of the reaction kettle is provided with a feed inlet, the bottom of the reaction kettle is provided with a stirring device, the stirring device is driven by a motor to rotate, a discharge port is arranged in the stirring device, the discharge port is communicated to a suction filtration device through a discharge pipe, the suction filtration device is provided with a barrel opening for a packaging barrel to move in and out, the reaction device is also provided with a metering and conveying device, the metering and conveying device is provided with two baffles arranged at intervals, the packaging barrel can be clamped between the baffles, and the control system is in communication connection with the stirring device, the motor, the suction filtration device and the metering and conveying device; the stirring device is provided with dispersing blades, a first filter screen, a second filter screen, a third filter screen, a fourth filter screen, a sealing plate and an air hole, and the first filter screen, the second filter screen, the third filter screen, the fourth filter screen, the sealing plate and the air hole are enclosed into a cylindrical barrel; wherein, the pore diameter of the first filter screen is larger than the pore diameter of the second filter screen, the pore diameter of the third filter screen is larger than the pore diameter of the fourth filter screen; the first filter screen, the second filter screen and the third filter screen are respectively used for collecting products with different sizes, and the filter screens can be added or reduced according to the actual required product sizes; the discharge port is selectively communicated with the first filter screen, the second filter screen, the third filter screen, the fourth filter screen or the air port.
2. The apparatus for preparing graphene oxide according to claim 1, wherein: the packaging barrel is provided with a barrel bar code, the reaction device is further provided with a packaging barrel groove extending from top to bottom, the reaction device is provided with a code scanner, the code scanner is positioned at the bottom of the packaging barrel groove, the packaging barrel can move downwards from the top of the packaging barrel groove until the packaging barrel falls between two baffles of the metering and conveying device, and the control system is in communication connection with the code scanner and the barrel bar code of the packaging barrel.
3. The apparatus for preparing graphene oxide according to claim 1, wherein: the reaction device is further provided with a storage barrel for storing the reducing agent, an inlet is formed in the top of the storage barrel, the storage barrel is communicated to a feed inlet of the reaction kettle through a first pipeline, and a first flow control valve is arranged on the first pipeline.
4. An apparatus for preparing graphene oxide according to claim 2 or 3, wherein: the reaction kettle is internally provided with a viscometer device and a temperature PH device, and the viscometer device and the temperature PH device are both in communication connection with a control system.
5. An apparatus for preparing graphene oxide according to claim 2 or 3, wherein: the bottom of reaction unit is equipped with water inlet and outlet, the bottom of reaction product district is equipped with water inlet and delivery port, reaction unit's water inlet selectivity and reaction product district's water inlet intercommunication, reaction unit's outlet selectivity and reaction product district's delivery port intercommunication, reaction unit's water inlet communicates to the reation kettle through the inlet tube in, be equipped with a second flow control valve on the inlet tube, the inlet tube communicates in the top of second flow control valve has a downward drain pipe of slope, suction filtration device's bottom communicates to the drain pipe, the top of drain pipe is equipped with a third flow control valve, the drain pipe selectivity communicates to reaction unit's outlet, second flow control valve and third flow control valve all are connected with control system communication, the second flow control valve is located under the drain pipe.
6. The apparatus for preparing graphene oxide according to claim 5, wherein: a waste water collecting tank is further arranged between the bottom of the drain pipe and the water outlet of the reaction device, a fourth flow control valve is arranged at the position, between the waste water collecting tank and the suction filtration device, of the drain pipe, a fifth flow control valve is arranged between the waste water collecting tank and the water outlet of the reaction device, a limiting PH sensor is arranged in the waste water collecting tank, and the control system is in communication connection with the fourth flow control valve, the fifth flow control valve and the limiting PH sensor.
7. A production method for preparing graphene oxide, characterized in that the apparatus for preparing graphene oxide according to claim 1 is applied, comprising the steps of:
the mixture injection area is provided with a mixture of concentrated sulfuric acid and graphite; the reaction device moves to a mixture injection area, and a metering injection port of the mixture injection area injects a mixture of concentrated sulfuric acid and graphite into a reaction kettle of the reaction device; then the reaction device moves to an oxidant injection area, and a metering injection port of the oxidant injection area injects oxidant into a reaction kettle of the reaction device; then the reaction device moves to a reducing agent injection area, and a metering injection port of the reducing agent injection area injects reducing agent into a reaction kettle of the reaction device; then the reaction device moves to a reaction finished product area, and graphene oxide finished products in the reaction kettle are output through the reaction finished product area; and finally, the reaction device moves to a mixture injection area for the next round of circular production.
8. The production method for preparing graphene oxide according to claim 7, wherein: the equipment for preparing the graphene oxide further comprises a control system, wherein the control system is arranged on the reaction device, the mixed material injection area is provided with a resonance sound mixing device, the reaction device is further provided with a bar code area, the mixed material injection area, the oxidant injection area and the reducing agent injection area are respectively provided with a code scanning sensor, the bar code area and the code scanning sensors are in communication connection with the control system, and the code scanning sensors can identify and scan the bar code area;
The control system receives the proportioning input of the concentrated sulfuric acid and the graphite, calculates the injection quantity of the mixture, the injection quantity of the oxidant and the injection quantity of the reducing agent, and enables the bar code area of the reaction device to correspondingly form a specific bar code;
When the code scanning sensor of the mixture injection area recognizes the code scanning area, the mixture injection area obtains the injection quantity of the mixture calculated by the control system, and the injection quantity of the mixture calculated by the control system is injected into the reaction kettle of the reaction device through the metering injection port of the mixture injection area;
When the scanning sensor of the oxidant injection area recognizes the scanning bar code area, the oxidant injection area acquires the injection amount of the oxidant calculated by the control system, and the injection amount of the oxidant calculated by the control system is injected into the reaction kettle of the reaction device through the metering injection port of the oxidant injection area;
When the scanning bar code area is identified by the scanning bar code sensor of the reducing agent injection area, the reducing agent injection area acquires the injection amount of the reducing agent calculated by the control system, and the injection amount of the reducing agent calculated by the control system is injected into the reaction kettle of the reaction device through the metering injection port of the reducing agent injection area.
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| CN202210146533.5A CN114307933B (en) | 2022-02-17 | Equipment for preparing graphene oxide and production method |
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| CN202210146533.5A CN114307933B (en) | 2022-02-17 | Equipment for preparing graphene oxide and production method |
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| CN108499397A (en) * | 2018-04-10 | 2018-09-07 | 广东金宝力化工科技装备股份有限公司 | A kind of multiple batches of small lot ink automatic production line |
| CN215087091U (en) * | 2021-04-10 | 2021-12-10 | 哈尔滨市顺科达精密机械研究院(有限合伙) | Low-temperature reaction device for preparing graphene oxide |
| CN216987658U (en) * | 2022-02-17 | 2022-07-19 | 恒力盛泰（厦门）石墨烯科技有限公司 | Equipment for preparing graphene oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108499397A (en) * | 2018-04-10 | 2018-09-07 | 广东金宝力化工科技装备股份有限公司 | A kind of multiple batches of small lot ink automatic production line |
| CN215087091U (en) * | 2021-04-10 | 2021-12-10 | 哈尔滨市顺科达精密机械研究院(有限合伙) | Low-temperature reaction device for preparing graphene oxide |
| CN216987658U (en) * | 2022-02-17 | 2022-07-19 | 恒力盛泰（厦门）石墨烯科技有限公司 | Equipment for preparing graphene oxide |
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