CN114307933A - Equipment and production method for preparing graphene oxide - Google Patents
Equipment and production method for preparing graphene oxide Download PDFInfo
- Publication number
- CN114307933A CN114307933A CN202210146533.5A CN202210146533A CN114307933A CN 114307933 A CN114307933 A CN 114307933A CN 202210146533 A CN202210146533 A CN 202210146533A CN 114307933 A CN114307933 A CN 114307933A
- Authority
- CN
- China
- Prior art keywords
- reaction
- area
- injection
- control system
- mixture
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 40
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 196
- 238000002347 injection Methods 0.000 claims abstract description 162
- 239000007924 injection Substances 0.000 claims abstract description 162
- 239000000203 mixture Substances 0.000 claims abstract description 70
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 69
- 239000007800 oxidant agent Substances 0.000 claims abstract description 59
- 230000001590 oxidative effect Effects 0.000 claims abstract description 57
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 68
- 239000000463 material Substances 0.000 claims description 36
- 239000000047 product Substances 0.000 claims description 32
- 238000000967 suction filtration Methods 0.000 claims description 27
- 238000004891 communication Methods 0.000 claims description 24
- 229910002804 graphite Inorganic materials 0.000 claims description 17
- 239000010439 graphite Substances 0.000 claims description 17
- 239000002351 wastewater Substances 0.000 claims description 16
- 239000007795 chemical reaction product Substances 0.000 claims description 15
- 238000003860 storage Methods 0.000 claims description 13
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 9
- 238000012856 packing Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 abstract description 5
- 238000003756 stirring Methods 0.000 description 20
- 238000004806 packaging method and process Methods 0.000 description 18
- 238000007789 sealing Methods 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 7
- 230000002159 abnormal effect Effects 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- -1 graphite alkene Chemical class 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 230000002687 intercalation Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000010667 large scale reaction Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Images
Abstract
The invention discloses equipment for preparing graphene oxide, which comprises: the reaction device comprises a reaction device and a mixture injection area, an oxidant injection area, a reductant injection area and a reaction finished product area which are sequentially arranged, wherein the reaction device is provided with a reaction kettle and can movably and sequentially move from the mixture injection area to the reaction finished product area through the oxidant injection area and the reductant injection area, and the mixture injection area, the oxidant injection area and the reductant injection area are respectively provided with a metering injection port; the invention also discloses a production method for preparing the graphene oxide, and the equipment for preparing the graphene oxide has the characteristic of being capable of sequentially processing in small batches and multiple batches.
Description
Technical Field
The invention relates to the technical field of carbon nanomaterial preparation, in particular to equipment and a production method for preparing graphene oxide.
Background
Compared with graphene, the graphene oxide can be better mixed with other materials for modification, is wider in application and has a wide chemical modification research prospect.
The preparation mode of present oxidation graphite alkene is traditional chemical industry reaction industrial design, produces the line through the fixed production of fixed reation kettle, and the shortcoming of this technology has:
the capacity limitation can be determined only according to the size of the reaction kettle, and the capacity increase can be solved only by increasing a production line;
reagents are wasted, and the industrial production usually needs excessive strong oxidant to achieve certain effect;
the product quality difference is caused by incomplete oxidation among graphite layers due to mass production, the existing process needs more than 6 hours of reaction time, the size of the obtained product is reduced due to long-time oxidation reaction and mechanical stirring, the surface defects of graphene are too many, and the subsequent use is seriously influenced;
the production environment is poor, and the production environment and equipment are difficult to clean due to frequent shutdown cleaning;
potential safety hazard, a large amount of strong oxidant is added at one 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 processing in small batches and multiple batches sequentially.
In order to achieve the above purpose, the present invention adopts the following technical scheme.
An apparatus for preparing graphene oxide, comprising: the reaction device comprises a reaction device, and a mixture injection area, an oxidant injection area, a reductant injection area and a reaction finished product area which are sequentially arranged, wherein the reaction device is provided with a reaction kettle, the reaction device can movably and sequentially move to the reaction finished product area from the mixture injection area through the oxidant injection area and the reductant injection area, and the mixture injection area, the oxidant injection area and the reductant injection area are respectively provided with a metering injection port.
The utility model provides an equipment of preparation oxidation graphite alkene, still includes control system, control system sets up on reaction unit, the mixture is annotated the material district and is had resonance sound and mix the device, reaction unit still has the bar code district, the mixture is annotated material district, oxidant and is annotated material district and reductant and annotate the material district and divide equally and do not be provided with and sweep a yard inductor, the bar code district reaches to sweep a yard inductor and all with control system communication connection, sweep a yard inductor distinguishable scanning bar code district.
The utility model discloses a reactor, including reation kettle, agitating unit, suction filtration device, metering conveyer, control system, motor, suction filtration device and control system, reation kettle's top is formed with the feed inlet, reation kettle's bottom is equipped with agitating unit, agitating unit is driven by the motor and rotates, agitating unit's inside is provided with the discharge gate, the discharge gate communicates to a suction filtration device through the discharging pipe, suction filtration device is equipped with the bung hole that can supply the activity of pail pack to pass in and out, reaction unit still has metering conveyer, the last baffle that is equipped with two intervals and sets up of metering conveyer, the pail pack can block between the baffle, control system and agitating unit, motor, suction filtration device and the equal communication connection of metering conveyer.
The pail pack is provided with the bucket bar code, reaction unit still has a packing barrel groove from top to bottom extending, reaction unit is last to be provided with a bar code scanner, the bar code scanner is to the bottom that is located the packing barrel groove, the pail pack can be by the top downstream in packing barrel groove, until falling between two baffles of measurement conveyer, control system and bar code scanner, the equal communication connection of bucket bar code of pail pack.
The reaction device is also provided with a storage barrel for storing the reducing agent, the top of the storage barrel is provided with an inlet, the storage barrel is communicated to a feed inlet of the reaction kettle through a first pipeline, and the first pipeline is provided with a first flow control valve.
Be equipped with viscosimeter device and temperature PH ware in the reation kettle, viscosimeter device and temperature PH ware all with control system communication connection.
The bottom of the reaction device is provided with a water inlet and a water outlet, the bottom of the reaction product area is provided with a water inlet and a water outlet, the water inlet of the reaction device is selectively communicated with the water inlet of the reaction finished product area, the water outlet of the reaction device is selectively communicated with the water outlet of the reaction finished product area, the water inlet of the reaction device is communicated to the inside of the reaction kettle through a water inlet pipe, a second flow control valve is arranged on the water inlet pipe, the water inlet pipe is communicated with a drain pipe which is inclined downwards above the second flow control valve, the bottom of the suction filtration device is communicated with the drain pipe, the top of the drain pipe is provided with a third flow control valve, the drain pipe is selectively communicated with a drain outlet of the reaction device, the second flow control valve and the third flow control valve are both in communication connection with the control system, and the second flow control valve is located below the drain pipe.
Still be equipped with a wastewater collection groove between the bottom of drain pipe and reaction unit's outlet, the position department that the drain pipe is located between wastewater collection groove and the suction filtration device is equipped with a fourth flow control valve, be equipped with a fifth flow control valve between wastewater collection groove and reaction unit's outlet, be equipped with spacing PH inductor in the wastewater collection groove, control system all with fourth flow control valve, fifth flow control valve and spacing PH inductor communication connection.
A production method for preparing graphene oxide by using the equipment for preparing graphene oxide comprises the following steps: the mixture injection area is stored 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 an oxidant into a reaction kettle of the reaction device; then the reaction device is moved to a reducing agent injection area, and a metering injection port of the reducing agent injection area injects a reducing agent into a reaction kettle of the reaction device; then the reaction device moves to a reaction finished product area, and the graphene oxide finished product in the reaction kettle is output through the reaction finished product area; and finally, moving the reaction device to a mixture injection area for next cycle production.
The equipment for preparing the graphene oxide further comprises a control system, the control system is arranged on a reaction device, the mixture injection region is provided with a resonance sound mixing device, the reaction device is further provided with a bar code region, the mixture injection region, the oxidant injection region and the reducing agent injection region are respectively provided with a code scanning sensor, the bar code region and the code scanning sensor are in communication connection with the control system, and the code scanning sensor can identify a scanning bar code region; the control system can receive the proportioning input of concentrated sulfuric acid and graphite, and calculate the material injection amount of the mixture, the material injection amount of the oxidant and the material injection amount of the reducing agent, so that the bar code area of the reaction device can correspondingly form a specific bar code; when the code scanning sensor of the mixture injection area identifies and scans the bar code area, the mixture injection area can acquire the injection amount of the mixture calculated by the control system, and the injection amount of the mixture calculated by the control system is injected into a reaction kettle of the reaction device through a metering injection port of the mixture injection area; when the barcode scanning sensor of the oxidant injection area identifies and scans the barcode area, the oxidant injection area can acquire 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 code scanning sensor of the reducing agent injection area identifies and scans the bar code area, the reducing agent injection area can acquire 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 a reaction kettle of the reaction device through a 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 reductant injection area and the reaction finished product area are matched, and the reaction device can move to the reaction finished product area from the mixture injection area, the oxidant injection area and the reductant injection area in sequence, so that the mixture, the oxidant and the reductant can be added into a reaction kettle of the reaction device in sequence, and the small-batch and multi-batch sequential treatment is realized.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for preparing graphene oxide according to the present invention;
FIG. 2 is a schematic view of the structure of a reaction apparatus of the present invention;
FIG. 3 is a schematic view of the stirring apparatus of the present invention.
[ notation ] to show
Reaction apparatus 1
11 bar code zone 12 of reaction kettle
Dispersing blade 141 first strainer 142
Discharge pipe 17 suction filtration device 18
Drain pipe 182 of bung 181
Third flow control valve 183 fourth flow control valve 184
Metering conveyor 19
Baffle 191
Inlet 1041 first conduit 1042
First flow control valve 1043
Fifth flow control valve 1081
Mixture injection zone 2
Resonant acoustic mixing device 21
Oxidant injection zone 3
Reducing agent injection zone 4
Reaction product zone 5
A control system 6.
Detailed Description
The invention is described in further detail below with reference to the figures and specific examples.
Referring to fig. 1 to 3, the present invention discloses an apparatus for preparing graphene oxide, including: reaction unit 1 and the mixture that sets gradually annotate material district 2, oxidant and annotate material district 3, reductant and annotate material district 4, reaction product district 5, reaction unit 1 has reation kettle 11, reaction unit 1 movably removes to reaction product district 5 from mixture notes material district 2 via oxidant notes material district 3, reductant notes material district 4 in proper order, mixture notes material district 2, oxidant notes material district 3 and reductant notes material district 4 are equallyd divide and are provided with the measurement sprue respectively.
In order to realize 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 mixture injection region 2 is provided with a resonant acoustic mixing device 21, the reaction device 1 is also provided with a bar code region 12, the mixture 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, and the code scanning sensor can identify the bar code region 12; wherein the resonant sound mixing device 21 is at an ultralow temperature, and the temperature range of the ultralow temperature is-35-0 ℃.
Then, the reaction apparatus 1 may further be provided with a circulating water cooler 113, a water cooling pipe of the circulating water cooler 113 is communicated to the cavity of the reactor wall of the reaction kettle 11, the control system 6 is in communication connection with the circulating water cooler 113, the reaction kettle 11 may be kept at a suitable reaction temperature by the arrangement of the circulating water cooler 113, and the circulating water cooler 113 is controlled by the control system 6 to be started.
In order to facilitate the reaction to be accelerated, a feeding hole 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 by a motor 15 to rotate, and a discharging hole 16 is formed inside the stirring device 14; wherein, the stirring device 14 is used for stirring at a low speed, and the stirring speed is more than 1000 r/min.
Referring to fig. 3, the stirring device 14 has a dispersing blade 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 opening 147, and 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 opening 147 form a cylindrical cylinder; in practice, the specification of the fourth filter screen 145 is 10-30 micrometers, the specification of the third filter screen 144 is 30-60 micrometers, the specification of the second filter screen 143 is 60-100, and the specification of the first filter screen 142 is more than 100 micrometers; 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 filter screens can be added or reduced according to the actual required product size, when the fourth filter screen 145 is used for washing, the sealing plate 146 is used for reaction, and the air openings 147 are used for cleaning reaction; the discharge port 16 is selectively aligned with the first filter screen 142, the second filter screen 143, the third filter screen 144, the fourth filter screen 145, the closing plate 146 or the air opening 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 air opening 147. 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 opening 181 through which the packaging barrel 101 can move in and out, and most of water can be removed by suction filtration by means of the suction filtration device 18 to form a filter cake.
Furthermore, in order to facilitate the transportation of the packaging barrel 101, the reaction device 1 is further provided with a metering and conveying device 19, two baffles 191 arranged at intervals are arranged on the metering and conveying device 19, 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 present invention is in a 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 further has a packaging barrel slot 102 extending from top to bottom, a code scanner 103 is arranged on the reaction device 1, the code scanner 103 is located at the bottom of the packaging barrel slot 102, the packaging barrel 101 can move downwards from the top of the packaging barrel slot 102 until the packaging barrel falls 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 as to realize management and control of the packaging barrel 101; the control system 6 can perform information representation by scanning the barrel bar code of the packaging barrel 101 so as to control different packaging barrels 101 to contain products with different sizes.
Further, the reaction device 1 is further provided with a storage barrel 104 for storing a reducing agent, the top of the storage barrel 104 is provided with an inlet 1041, the storage barrel 104 is communicated to the feed inlet 13 of the reaction kettle 11 through a first pipeline 1042, the first pipeline 1042 is provided with a first flow control valve 1043, so that the reducing agent can be slowly introduced to remove the residual oxidizing agent, and new impurities are prevented from being introduced due to the quantitative addition of the reducing agent, and the reducing agent can be added into the storage barrel 104 in advance, so that the subsequent reaction device 1 is not required, and the reducing agent is added from the reaction product zone 5 to the reducing agent injection zone 4 and then returned.
The reaction device 1 may further include an alarm device 114, and the alarm device 114 may give an alarm for abnormal injection, abnormal temperature, abnormal barcode scanning, and/or abnormal water inflow.
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 in communication connection with the control system 6, so that the degree of graphite oxidation reaction can be more visually presented through the feedback curve of viscosity, temperature and pH value, the reaction time is controlled, the reduction of the graphite sheet diameter and the increase of edge abnormal defects caused by excessive oxidation are reduced, the rotating speed of mechanical stirring of subsequent reaction is reduced after pre-intercalation treatment, the large-sheet-diameter graphene oxide can be prepared, the particle size of the finished product graphene oxide is larger than 50 mu m, and the large-sheet-diameter graphene oxide is calculated.
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 with the inside of 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 downward inclined water discharge pipe 182 above the second flow control valve 1072, the bottom of the suction filtration device 18 is communicated with a water discharge pipe 182, the top of the water discharge pipe 182 is provided with a third flow control valve 183, the water discharge pipe 182 is selectively communicated with the water outlet 108 of the reaction device 1, and both the second flow control valve 1072 and the third flow control valve 183 are in communication connection with the control system 6, the second flow control valve 1072 is located below the drain pipe 182.
In order to collect wastewater conveniently, a wastewater collection tank 109 may be further disposed between the bottom of the drainage pipe 182 and the drainage port 108 of the reaction device 1, a fourth flow control valve 184 is disposed at a position of the drainage pipe 182 between the wastewater collection tank 109 and the suction filtration device 18, a fifth flow control valve 1081 is disposed between the wastewater collection tank 109 and the drainage port 108 of the reaction device 1, a limit PH sensor 1091 is disposed in the wastewater collection tank 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 limit 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 butted with the metering conveying device 19.
Further, the bottom of the reaction device 1 is further provided with a transmission wheel 111, the transmission wheel 111 may be a lifting wheel, and the control system 6 is in communication connection with the transmission wheel 111.
The resonance acoustic mixing device 21 can be externally 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 processing time can be 15-60 minutes.
In addition, the bottom of the reaction device 1 is provided with a stabilizing block 112.
Further, middle part is equipped with a sealing plate 1111 in reation kettle 11, temperature PH ware 106 and viscometer device 105 all locate on sealing plate 1111, agitating unit 14 locates the below of sealing plate 1111, the temperature probe and the PH probe of temperature PH ware 106 all extend to the below of sealing plate 1111, the viscosity probe of viscometer device 105 extends to the below of sealing plate 1111, feed inlet 13 communicates to the below of sealing plate 1111, control system 6 all with temperature PH ware 106, viscometer device 105 communication connection.
From the above, the invention can reduce the use of water and increase the utilization rate of the control of each flow control valve of the reaction device 1, reduce the production cost, and simultaneously upload the real-time production data to be convenient for the management and calculation of a producer; the movable computer-controlled reaction device can reduce labor cost reduction and potential safety hazards, and graphene oxide with different sheet diameter sizes is automatically classified through the matching 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 sale; the reaction device is produced and moved circularly without stopping, and a factory can plan a large-scale reaction product area and can continuously produce to increase the capacity.
The invention also discloses a production method for preparing graphene oxide, and the equipment for preparing graphene oxide comprises the following steps: the mixture injection area 2 stores a mixture of concentrated sulfuric acid and graphite; the reaction device 1 moves to the 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 an 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 a 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 the graphene oxide finished product in the reaction kettle 11 is output through the reaction finished product area 5; finally, the reaction device 1 moves to the mixture injection area 2 again to carry out 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 mixture 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 mixture injection region 2, the oxidant injection region 3 and the reducing agent injection region 4 are respectively provided with a bar code scanning sensor, the bar code region 12 and the bar code scanning sensor are in communication connection with the control system 6, and the bar code scanning sensor can identify the bar code scanning region 12; the control system 6 can receive the input of the ratio of concentrated sulfuric acid to graphite, and calculate the material injection amount of the mixture, the material injection amount of the oxidant and the material injection amount of the reducing agent, so that the bar code area 12 of the reaction device 1 can correspondingly form a specific bar code; when the code scanning sensor of the mixture injection area 2 identifies the scanning bar code area 12, the mixture injection area 2 can acquire the injection amount of the mixture calculated by the control system 6, and the injection amount 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 code scanning sensor of the oxidant feeding area 3 identifies the scanning bar code area 12, the oxidant feeding area 3 can acquire the feeding amount of the oxidant calculated by the control system 6, and the feeding 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 feeding port of the oxidant feeding area 3; when the code scanning sensor of the reducing agent injection region 4 identifies the scanning bar code region 12, the reducing agent injection region 4 can acquire 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 region 4.
The method judges whether the reaction is finished or not by the change of the viscosity of the system after the reaction, the viscosity of the reaction system is the change of a curve, and the reaction is finished after the slope of the curve is lower than a set value when the curve is smooth and the slope of the curve is lower than the set value (the PH curve is the same); in practice, when the tangential slope of the viscosity curve is in the range of 0-0.05, the curve is nearly flat, and the reaction is finished; wherein, the second flow control valve 1072 is controlled to open, so that water enters the water inlet 107 of the reaction device 1 and enters the reaction kettle 11 through the water inlet pipe 1071, and the reaction kettle 11 is cleaned to finish the reaction.
Therefore, the invention can achieve the effect of increasing the productivity by automatically increasing the batches, the small-batch processing can easily achieve the oxidation condition, and the quality of the prepared product can be improved because the reaction device 1 can movably move to the reaction finished product area 5 from the mixture injection area 2 through the oxidant injection area 3 and the reductant injection area 4 in sequence by the matching design of the reaction device 1, the mixture injection area 2, the oxidant injection area 3, the reductant injection area 4 and the reaction finished product area 5, so that the reaction device 1 can sequentially add the mixture, the oxidant and the reductant into the reaction kettle 11 of the reaction device 1, and the small-batch and multi-batch processing can be realized.
The invention can be processed in small batch and multiple batches in sequence, can directly increase the productivity according to the actual requirement, reduce the reaction time through the pre-intercalation treatment, simultaneously reduce the labor cost by the modern design full-automatic process, reduce the waste of chemical reagents in small batch, ensure the product quality, improve the production environment and the safety performance by the automation, change the traditional chemical production process technology, and improve the production productivity and the product quality by the modern equipment and process.
The production method for preparing graphene oxide is characterized in that in actual production: adding concentrated sulfuric acid and graphite in a certain ratio into a resonant acoustic mixing device 21, and keeping low-temperature mixing for 15-60 minutes for later use; the control system 6 receives the proportioning input of concentrated sulfuric acid and graphite, and calculates the material injection amount of the mixture, the material injection amount of the oxidant and the material injection amount of the reducing agent, so that the bar code area 12 of the reaction device can correspondingly form a specific bar code; the reaction device 1 starts the circulating water cooler 113 to keep at the reaction temperature; driving a transmission wheel 111 of the reaction device 1 to enter the mixed material injection area 2, and automatically injecting materials according to the formula by scanning a bar code area 12 arranged in a code scanning sensor of the mixed material injection area 2; starting a stirring device 14 to stir at a low speed, entering an oxidant injection area 3, and automatically injecting materials according to a formula in a code scanning sensor scanning bar code area 12 of the oxidant injection area 3; entering a reducing agent injection area 4, automatically injecting a material according to a formula in a code scanning sensor scanning bar code area 12 of the reducing agent injection area 4, and injecting a reducing agent into a storage barrel; the reaction product enters a designated place of the reaction product area 5 through the conveying wheel 111, the conveying wheel 111 is lifted to enable the water inlet 107 and the water outlet 108 of the reaction device 1 to be communicated with the water inlet 51 and the water outlet 52 of the reaction product area 5, when the viscosity curve is nearly smooth and the tangent slope of the viscosity curve reaches a set value, the first flow control valve 1043 is started to slowly introduce the reducing agent to remove the residual reducing agent and slowly introduce the reducing agent to remove the residual oxidizing agent, when the temperature and the pH curve are stable, the addition of the reducing agent is finished, meanwhile, the actual amount of the reducing agent is fed back, stirring is suspended, and the temperature and the pH curve are measured by a temperature and pH device; opening a second flow control valve 1072 to feed water, simultaneously controlling the motor 15 to rotate anticlockwise until a fourth filter screen 145 of the stirring device 14 comes out, stirring clockwise to clean, and opening a fourth flow control valve 184 to inject washing water into the wastewater collection 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 to the suction filtration device 18; controlling the motor 15 to rotate anticlockwise to the third filter screen 144 of the stirring device 14, then stirring clockwise, opening the third flow control valve 83, reducing or closing the flow of the second flow control valve 1072, starting suction filtration, at the moment, closing the fourth flow control valve 184, returning filtrate to the reaction kettle 11 through the third flow control valve 183, recycling the filtrate without influencing the product size, and after suction filtration, weighing and transmitting the packaging barrel 101 into the metering and transmitting device 19 and the transmitting device 53 in the reaction finished product area 5; repeating the operation of the material storage barrel 104 and the operation of the motor 15 until the stirring device 14 rotates to the air hole 147 from the second filter screen 143 and the first filter screen 142, 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, cleaning for 2-3 times, recording the volume and the pH after the water level of the wastewater collection tank 109 reaches the limit pH sensor 1091, feeding the volume and the pH back to the control system 6, and transmitting the volume and the pH to the terminal, and simultaneously opening the fifth flow control valve 1081 for draining; after the water is drained, the conveying wheel 111 is lowered for the next cycle of production.
The above-mentioned embodiments are only preferred embodiments of the present invention, and do not limit the technical scope of the present invention, so that the changes and modifications made by the claims and the specification of the present invention should fall within the scope of the present invention.
Claims (10)
1. An apparatus for preparing graphene oxide, comprising: the reaction device comprises a reaction device, and a mixture injection area, an oxidant injection area, a reductant injection area and a reaction finished product area which are sequentially arranged, wherein the reaction device is provided with a reaction kettle, the reaction device can movably and sequentially move to the reaction finished product area from the mixture injection area through the oxidant injection area and the reductant injection area, and the mixture injection area, the oxidant injection area and the reductant injection area are respectively provided with a metering injection port.
2. The apparatus for preparing graphene oxide according to claim 1, wherein: still include control system, control system sets up on reaction unit, the mixture is annotated the material district and is had resonance sound and mix the device, reaction unit still has the bar code district, the mixture is annotated the material district, the oxidant is annotated the material district and the reductant is annotated the material district and is equallyd divide and do not be provided with and sweep a yard inductor, the bar code district reaches and sweeps a yard inductor and all is connected with control system communication, sweep a yard inductor distinguishable scanning bar code district.
3. The apparatus for preparing graphene oxide according to claim 2, wherein: the utility model discloses a reactor, including reation kettle, agitating unit, suction filtration device, metering conveyer, control system, motor, suction filtration device and control system, reation kettle's top is formed with the feed inlet, reation kettle's bottom is equipped with agitating unit, agitating unit is driven by the motor and rotates, agitating unit's inside is provided with the discharge gate, the discharge gate communicates to a suction filtration device through the discharging pipe, suction filtration device is equipped with the bung hole that can supply the activity of pail pack to pass in and out, reaction unit still has metering conveyer, the last baffle that is equipped with two intervals and sets up of metering conveyer, the pail pack can block between the baffle, control system and agitating unit, motor, suction filtration device and the equal communication connection of metering conveyer.
4. The apparatus for preparing graphene oxide according to claim 3, wherein: the pail pack is provided with the bucket bar code, reaction unit still has a packing barrel groove from top to bottom extending, reaction unit is last to be provided with a bar code scanner, the bar code scanner is to the bottom that is located the packing barrel groove, the pail pack can be by the top downstream in packing barrel groove, until falling between two baffles of measurement conveyer, control system and bar code scanner, the equal communication connection of bucket bar code of pail pack.
5. The apparatus for preparing graphene oxide according to claim 3, wherein: the reaction device is also provided with a storage barrel for storing the reducing agent, the top of the storage barrel is provided with an inlet, the storage barrel is communicated to a feed inlet of the reaction kettle through a first pipeline, and the first pipeline is provided with a first flow control valve.
6. The apparatus for preparing graphene oxide according to any one of claims 3 to 5, wherein: be equipped with viscosimeter device and temperature PH ware in the reation kettle, viscosimeter device and temperature PH ware all with control system communication connection.
7. The apparatus for preparing graphene oxide according to any one of claims 3 to 5, wherein: the bottom of the reaction device is provided with a water inlet and a water outlet, the bottom of the reaction product area is provided with a water inlet and a water outlet, the water inlet of the reaction device is selectively communicated with the water inlet of the reaction finished product area, the water outlet of the reaction device is selectively communicated with the water outlet of the reaction finished product area, the water inlet of the reaction device is communicated to the inside of the reaction kettle through a water inlet pipe, a second flow control valve is arranged on the water inlet pipe, the water inlet pipe is communicated with a drain pipe which is inclined downwards above the second flow control valve, the bottom of the suction filtration device is communicated with the drain pipe, the top of the drain pipe is provided with a third flow control valve, the drain pipe is selectively communicated with a drain outlet of the reaction device, the second flow control valve and the third flow control valve are both in communication connection with the control system, and the second flow control valve is located below the drain pipe.
8. The apparatus for preparing graphene oxide according to claim 7, wherein: still be equipped with a wastewater collection groove between the bottom of drain pipe and reaction unit's outlet, the position department that the drain pipe is located between wastewater collection groove and the suction filtration device is equipped with a fourth flow control valve, be equipped with a fifth flow control valve between wastewater collection groove and reaction unit's outlet, be equipped with spacing PH inductor in the wastewater collection groove, control system all with fourth flow control valve, fifth flow control valve and spacing PH inductor communication connection.
9. A production method for preparing graphene oxide, which is characterized by applying the apparatus for preparing graphene oxide according to claim 1, comprising the steps of:
the mixture injection area is stored 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 an oxidant into a reaction kettle of the reaction device; then the reaction device is moved to a reducing agent injection area, and a metering injection port of the reducing agent injection area injects a reducing agent into a reaction kettle of the reaction device; then the reaction device moves to a reaction finished product area, and the graphene oxide finished product in the reaction kettle is output through the reaction finished product area; and finally, moving the reaction device to a mixture injection area for next cycle production.
10. The production method for preparing graphene oxide according to claim 9, wherein: the equipment for preparing the graphene oxide further comprises a control system, the control system is arranged on a reaction device, the mixture injection region is provided with a resonance sound mixing device, the reaction device is further provided with a bar code region, the mixture injection region, the oxidant injection region and the reducing agent injection region are respectively provided with a code scanning sensor, the bar code region and the code scanning sensor are in communication connection with the control system, and the code scanning sensor can identify a scanning bar code region;
the control system can receive the proportioning input of concentrated sulfuric acid and graphite, and calculate the material injection amount of the mixture, the material injection amount of the oxidant and the material injection amount of the reducing agent, so that the bar code area of the reaction device can correspondingly form a specific bar code;
when the code scanning sensor of the mixture injection area identifies and scans the bar code area, the mixture injection area can acquire the injection amount of the mixture calculated by the control system, and the injection amount of the mixture calculated by the control system is injected into a reaction kettle of the reaction device through a metering injection port of the mixture injection area;
when the barcode scanning sensor of the oxidant injection area identifies and scans the barcode area, the oxidant injection area can acquire 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 code scanning sensor of the reducing agent injection area identifies and scans the bar code area, the reducing agent injection area can acquire 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 a reaction kettle of the reaction device through a metering injection port of the reducing agent injection area.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210146533.5A CN114307933A (en) | 2022-02-17 | 2022-02-17 | Equipment and production method for preparing graphene oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210146533.5A CN114307933A (en) | 2022-02-17 | 2022-02-17 | Equipment and production method for preparing graphene oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114307933A true CN114307933A (en) | 2022-04-12 |
Family
ID=81030754
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210146533.5A Pending CN114307933A (en) | 2022-02-17 | 2022-02-17 | Equipment and production method for preparing graphene oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114307933A (en) |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0531353A (en) * | 1991-07-31 | 1993-02-09 | Asahi Eng Co Ltd | Manufacturing apparatus with moving tank |
| US20060269468A1 (en) * | 2005-05-26 | 2006-11-30 | Sang-Moon Chung | Apparatus and method for mass production of carbon nanotubes |
| RU2396120C1 (en) * | 2009-02-03 | 2010-08-10 | Государственное научное учреждение Всероссийский научно-исследовательский институт механизации животноводства (ГНУ ВНИИМЖ) | Device for grinding and separation of feed grains |
| US20120151877A1 (en) * | 2010-12-16 | 2012-06-21 | Inversiones Hiki6, S.L. | Mobile dosing, mixing and packaging plant |
| CN207591975U (en) * | 2017-11-20 | 2018-07-10 | 辽宁科技学院 | A kind of novel energy-saving mechanical ball mill |
| 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 |
| CN207856415U (en) * | 2017-12-27 | 2018-09-14 | 福建省福灿环保科技有限公司 | Polymeric aluminium reaction residues recycle filter device |
| CN209271003U (en) * | 2018-12-12 | 2019-08-20 | 广州浦连化工科技有限公司 | A kind of chemical industry equipment for separating liquid from solid |
| CN110371965A (en) * | 2019-08-13 | 2019-10-25 | 常州华科聚合物股份有限公司 | A kind of technical grade graphene oxide process units |
| CN214214843U (en) * | 2020-08-14 | 2021-09-17 | 刘海艳 | Traditional chinese medical science internal medicine filters residual waste residue collection device with traditional chinese medicine |
| CN214637627U (en) * | 2020-12-31 | 2021-11-09 | 昆山新正隆机械科技有限公司 | Spraying powder recovery unit with filtering mechanism |
| CN214810683U (en) * | 2021-06-18 | 2021-11-23 | 四川晟锟电子材料有限公司 | Discharging device of reaction kettle for chemical material production and processing |
| 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 |
-
2022
- 2022-02-17 CN CN202210146533.5A patent/CN114307933A/en active Pending
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0531353A (en) * | 1991-07-31 | 1993-02-09 | Asahi Eng Co Ltd | Manufacturing apparatus with moving tank |
| US20060269468A1 (en) * | 2005-05-26 | 2006-11-30 | Sang-Moon Chung | Apparatus and method for mass production of carbon nanotubes |
| RU2396120C1 (en) * | 2009-02-03 | 2010-08-10 | Государственное научное учреждение Всероссийский научно-исследовательский институт механизации животноводства (ГНУ ВНИИМЖ) | Device for grinding and separation of feed grains |
| US20120151877A1 (en) * | 2010-12-16 | 2012-06-21 | Inversiones Hiki6, S.L. | Mobile dosing, mixing and packaging plant |
| CN207591975U (en) * | 2017-11-20 | 2018-07-10 | 辽宁科技学院 | A kind of novel energy-saving mechanical ball mill |
| CN207856415U (en) * | 2017-12-27 | 2018-09-14 | 福建省福灿环保科技有限公司 | Polymeric aluminium reaction residues recycle filter device |
| 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 |
| CN209271003U (en) * | 2018-12-12 | 2019-08-20 | 广州浦连化工科技有限公司 | A kind of chemical industry equipment for separating liquid from solid |
| CN110371965A (en) * | 2019-08-13 | 2019-10-25 | 常州华科聚合物股份有限公司 | A kind of technical grade graphene oxide process units |
| CN214214843U (en) * | 2020-08-14 | 2021-09-17 | 刘海艳 | Traditional chinese medical science internal medicine filters residual waste residue collection device with traditional chinese medicine |
| CN214637627U (en) * | 2020-12-31 | 2021-11-09 | 昆山新正隆机械科技有限公司 | Spraying powder recovery unit with filtering mechanism |
| 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 |
| CN214810683U (en) * | 2021-06-18 | 2021-11-23 | 四川晟锟电子材料有限公司 | Discharging device of reaction kettle for chemical material production and processing |
| 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 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN216987658U (en) | Equipment for preparing graphene oxide | |
| CN206008688U (en) | A kind of circular response kettle | |
| CN113019252A (en) | Liquid automatic measurement batching system | |
| CN114307933A (en) | Equipment and production method for preparing graphene oxide | |
| CN113201798A (en) | Cleaning device for melt-blowing die head and cleaning method thereof | |
| CN207204090U (en) | A kind of polycarboxylate water-reducer synthesizer with automated sensor | |
| CN211971959U (en) | Lactic acid waste liquid treatment retrieval and utilization device | |
| CN110898782B (en) | Automatic preparation facilities of ternary precursor | |
| CN214636141U (en) | Liquid automatic measurement batching system | |
| CN209735586U (en) | Device for extracting short-chain fatty acid by in-situ synthesis of LDH in fermentation liquor | |
| CN209974581U (en) | Sediment dehydration mummification control facility | |
| CN219942820U (en) | Esterification raw material conveying system | |
| CN213172311U (en) | Be used for bacillus licheniformis fermentation cylinder | |
| CN213913768U (en) | Production line for preparing nano material | |
| CN215657830U (en) | Superfine palladium powder preparation device | |
| CN219621183U (en) | Bacteria cultivation storage container | |
| CN215087081U (en) | Automatic add reation kettle of alkali regulation pH value | |
| CN219232346U (en) | Differential polyester production device | |
| CN211255950U (en) | Continuous production and enzyme recovery device of phenylglycine | |
| CN205055989U (en) | Industrial cleaning agent preparation system | |
| CN220126108U (en) | Chemical industry dosing unit | |
| CN109052761A (en) | It is a kind of that electroplating sewerage equipment is handled by DC electric field | |
| CN220665022U (en) | Sewage tempering and desliming system | |
| CN203469959U (en) | System for automatically adding coal washing medium | |
| CN211462974U (en) | Biological reagent agitator tank |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |