阅读说明：本技术 超声辅助超临界流体制备石墨烯复合材料的自动化装置 (Automatic device for preparing graphene composite material by ultrasonic-assisted supercritical fluid ) 是由 喻学锋 赵海涛 康翼鸿 黄逸凡 于 2020-11-20 设计创作，主要内容包括：本发明涉及一种超声辅助超临界流体制备石墨烯复合材料的自动化装置,包括二氧化碳存储装置、输送装置、反应装置、废气处理回收设备；所述反应装置包括自动送样室、自动取样室、控温室；所述反应装置还包括反应釜,反应釜在自动送样室、自动取样室和控温室内可以移动；所述反应装置还包括超声处理器、自锁通气设备,控温室、反应釜上均设有密封口,自锁通气设备和超声处理器穿过密封口与不锈钢反应釜连接；二氧化碳存储装置、输送装置、自锁通气设备和废气处理回收设备间依次通过管道连接。本发明解决了现有石墨烯复合材料制备装置复杂难操作,自动化程度低,制备成本高,产量少,难以满足石墨烯复合材料的高质量、产业化制备的问题。(The invention relates to an automatic device for preparing a graphene composite material by ultrasonic-assisted supercritical fluid, which comprises a carbon dioxide storage device, a conveying device, a reaction device and waste gas treatment and recovery equipment; the reaction device comprises an automatic sample feeding chamber, an automatic sampling chamber and a temperature control chamber; the reaction device also comprises a reaction kettle which can move in the automatic sample feeding chamber, the automatic sampling chamber and the temperature control chamber; the reaction device also comprises an ultrasonic processor and a self-locking ventilation device, wherein sealing ports are formed in the temperature control chamber and the reaction kettle, and the self-locking ventilation device and the ultrasonic processor penetrate through the sealing ports to be connected with the stainless steel reaction kettle; the carbon dioxide storage device, the conveying device, the self-locking ventilation equipment and the waste gas treatment and recovery equipment are connected in sequence through pipelines. The invention solves the problems that the existing graphene composite material preparation device is complex and difficult to operate, has low automation degree, high preparation cost and low yield, and is difficult to meet the requirements of high-quality and industrialized preparation of graphene composite materials.)

1. An automation equipment of graphite alkene combined material is prepared to supplementary supercritical fluid of supersound which characterized in that:

comprises a carbon dioxide storage device, a conveying device, a reaction device and waste gas treatment and recovery equipment (9);

the reaction device comprises a plurality of independent spaces, adjacent spaces are connected through a control door (20),

the space at the two ends of the reaction device is an automatic sample feeding chamber (31), an automatic sampling chamber (32) and a plurality of independent temperature control chambers, and the space between the automatic sample feeding chamber (31) and the automatic sampling chamber (32) is the temperature control chamber; the temperature control chamber is provided with a temperature adjusting device and a temperature sensor;

the reaction device also comprises a reaction kettle (4), and the reaction kettle (4) can move in the automatic sample feeding chamber (31), the automatic sampling chamber (32) and the plurality of independent temperature control chambers; the reaction kettle (4) is provided with a pressure sensor (12) and a temperature sensor,

the reaction device also comprises an ultrasonic processor (8) and a self-locking ventilation device, sealing ports are arranged on the temperature control chamber and the reaction kettle (4), and the self-locking ventilation device and the ultrasonic processor (8) penetrate through the sealing ports to be connected with the stainless steel reaction kettle (4);

the carbon dioxide storage device, the conveying device, the self-locking ventilation equipment and the waste gas treatment and recovery equipment (9) are connected in sequence through pipelines.

2. The automatic device for preparing the graphene composite material by the ultrasonic-assisted supercritical fluid according to claim 1, wherein:

the intelligent control system is characterized by further comprising an intelligent control center (6), wherein the intelligent control center (6) is used for controlling the opening and closing of the conveying device and the control door (20), and the intelligent control center (6) collects data of the pressure sensor (12) and the temperature sensor and controls the temperature adjusting device.

3. The automatic device for preparing the graphene composite material by the ultrasonic-assisted supercritical fluid according to claim 2, wherein:

the reaction device further comprises a top base (17), a lifting device (16) is arranged on the lower portion of the top base (17), and the self-locking ventilation equipment and the ultrasonic processor (8) are fixed on the lifting device (16).

4. The automatic device for preparing the graphene composite material by the ultrasonic-assisted supercritical fluid according to claim 3, wherein:

and the automatic sample feeding chamber (31) and the automatic sampling chamber (32) are internally provided with a mechanical arm (14), the mechanical arm (14) in the automatic sample feeding chamber (31) is used for putting the raw materials into the reaction kettle (4), and the mechanical arm (14) in the automatic sampling chamber (32) is used for taking out the sample from the reaction kettle (4).

5. The automatic device for preparing graphene composite material by using ultrasonic-assisted supercritical fluid according to claim 4, is characterized in that:

the temperature control chambers comprise a first temperature control chamber (51), a second temperature control chamber (52) and a third temperature control chamber (53);

the self-locking ventilation equipment is divided into self-locking gas injection equipment (71) and self-locking gas outlet equipment (72) which are respectively positioned above the first temperature control chamber (51) and the third temperature control chamber (53), the self-locking gas injection equipment (71) is connected with the conveying device through a pipeline, and the self-locking gas outlet equipment (72) is connected with the waste gas treatment and recovery equipment (9) through a pipeline.

6. The automatic device for preparing the graphene composite material by the ultrasonic-assisted supercritical fluid according to claim 5, wherein:

and the bottom of the stainless steel reaction kettle (4) is provided with a roller (15).

7. The automatic device for preparing the graphene composite material by the ultrasonic-assisted supercritical fluid according to claim 6, wherein:

a one-way valve (11) and a safety valve are arranged between the self-locking air release equipment and the waste gas treatment and recovery equipment (9).

8. The automatic device for preparing the graphene composite material by the ultrasonic-assisted supercritical fluid according to claim 7, wherein:

the carbon dioxide storage device and the conveying device are respectively CO₂A gas cylinder (1) and an electric pump (2).

9. The automatic device for preparing graphene composite material by using ultrasonic-assisted supercritical fluid according to claim 8, wherein:

and the inlet and the outlet of the carbon dioxide storage device are respectively connected with the waste gas treatment and recovery equipment (9) and the self-locking gas injection equipment (71) through safety valves.

Technical Field

The invention belongs to the field of research and development and preparation of graphene composite materials, and relates to an automatic device for preparing a graphene composite material by using an ultrasonic-assisted supercritical fluid.

Background

Due to the unique structure and excellent performance of graphene, the graphene serving as a filling phase of the composite material to enhance the performance of the composite material is a very important research direction in the application field of graphene, shows excellent performance in the fields of energy storage, electronic devices, biomedicine, sensing materials and the like, and has wide application prospects.

The large-scale production of graphene composite materials is always limited by preparation methods and preparation devices, and the conventional preparation methods such as micro-mechanical separation, chemical vapor deposition, oxidation-reduction, epitaxial growth and the like have complex and difficult-to-operate preparation processes and devices, low automation degree, high preparation cost and low yield, and are difficult to meet the requirements of high-quality and industrialized preparation of the graphene composite materials.

Disclosure of Invention

The invention provides an automatic device for preparing a graphene composite material by using an ultrasonic-assisted supercritical fluid, which solves the problems that the existing graphene composite material preparation device is complex and difficult to operate, low in automation degree, high in preparation cost and low in yield, and cannot meet the requirements of high-quality and industrial preparation of the graphene composite material.

The technical scheme for solving the problems is as follows: an automatic device for preparing graphene composite material by ultrasonic-assisted supercritical fluid is characterized in that:

comprises a carbon dioxide storage device, a conveying device, a reaction device and waste gas treatment and recovery equipment;

the reaction device comprises a plurality of independent spaces, adjacent spaces are connected through a control door,

the space at the two ends of the reaction device is an automatic sample feeding chamber and an automatic sampling chamber, and the space between the automatic sample feeding chamber and the automatic sampling chamber is a temperature control chamber; the temperature control chamber is provided with a temperature adjusting device and a temperature sensor;

the reaction device also comprises a reaction kettle which can move in the automatic sample feeding chamber, the automatic sampling chamber and the plurality of independent temperature control chambers; the reaction kettle is provided with a pressure sensor and a temperature sensor,

the reaction device also comprises an ultrasonic processor and a self-locking ventilation device, wherein sealing ports are formed in the temperature control chamber and the reaction kettle, and the self-locking ventilation device and the ultrasonic processor penetrate through the sealing ports to be connected with the stainless steel reaction kettle;

the carbon dioxide storage device, the conveying device, the self-locking ventilation equipment and the waste gas treatment and recovery equipment are connected in sequence through pipelines.

And the intelligent control center is used for controlling the opening and closing of the conveying device and the control door, acquiring data of the pressure sensor and the temperature sensor and controlling the temperature adjusting device.

Furthermore, the reaction device also comprises a top base, a lifting device is arranged at the lower part of the top base, and the self-locking ventilation equipment and the ultrasonic processor are fixed on the lifting device.

Furthermore, all be equipped with the manipulator in automatic sample room, the automatic sample room of sending, the indoor manipulator of automatic sample is used for putting into reation kettle with the raw materials, and the indoor manipulator of automatic sample is arranged in taking out the sample from reation kettle.

Further, the temperature control chambers comprise a first temperature control chamber, a second temperature control chamber and a third temperature control chamber;

the self-locking ventilation equipment is divided into self-locking gas injection equipment and self-locking gas outlet equipment which are respectively positioned above the first temperature control chamber and the third temperature control chamber, the self-locking gas injection equipment is connected with the conveying device through a pipeline, and the self-locking gas outlet equipment is connected with the waste gas treatment and recovery equipment through a pipeline.

Further, the bottom of the stainless steel reaction kettle is provided with rollers.

Furthermore, a one-way valve and a safety valve are arranged between the self-locking air outlet equipment and the waste gas treatment and recovery equipment.

Further, the carbon dioxide storage device and the delivery device are a carbon dioxide gas cylinder and an electric pump respectively.

Further, an inlet and an outlet of the carbon dioxide storage device are respectively connected with the waste gas treatment and recovery device and the self-locking gas injection device through safety valves.

The invention has the advantages that:

1) the invention provides a device for preparing a graphene composite material based on ultrasonic-assisted supercritical fluid, which is characterized in that CO is arranged₂The gas cylinder, the electric pump, the automatic feeding/sampling equipment, the temperature control chamber, the stainless steel reaction kettle with the roller, the liftable self-locking ventilation equipment, the ultrasonic processing equipment and the intelligent control center are matched for use, so that the automation and the accuracy of the preparation process can be realized; CO 2₂The gas cylinder, the electric pump, the self-locking gas injection equipment and the stainless steel reaction kettle can enable the supercritical fluid to be used as a solvent for stripping graphene, and meanwhile, an independent temperature control room can provide an accurate and stable temperature environment for each reaction step; the ultrasonic processor can go deep into the stainless steel reaction kettle to carry out ultrasonic treatment on the reaction, and the ultrasonic cavitation brought by the ultrasonic wave can assist the stripping of the graphene sheet layer; the device adopts streamlined operation, and after the current reaction step was accomplished, reation kettle will get into next step automatically, vacates the operation device of the last reaction step and supplies another reation kettle to use, can operate 5 reation kettles simultaneously, has powerfully guaranteed the volume production preparation of graphite alkene combined material.

2) According to the invention, the macroscopic preparation of the graphene composite material is realized by an ultrasonic-assisted supercritical fluid method, the device is simple and safe to prepare and operate, the automation degree is high, and the precise control and the accurate recording of the preparation process are realized by adopting an intelligent control mode.

Drawings

FIG. 1 is a schematic structural view of the present invention;

FIG. 2 is an enlarged view of a portion of the self-locking gas injection apparatus of FIG. 1 according to the present invention.

In the figure: 1-CO₂The system comprises a gas cylinder, a 2-electric pump, a 3-automatic feeding/sampling device, a 31-automatic feeding chamber, a 32-automatic sampling chamber, a 4-reaction kettle, a 5-temperature control chamber, a 51-first temperature control chamber, a 52-second temperature control chamber, a 53-third temperature control chamber, a 6-intelligent control center, a 71-self-locking gas injection device, a 72-self-locking gas outlet device, an 8-ultrasonic processor, a 9-waste gas treatment and recovery device, a 11-one-way valve, a 121-first pressure sensor, a 122-third pressure sensor, aTwo pressure sensors, 131-a first temperature sensor, 132-a second temperature sensor, 14-a manipulator, 15-a roller, 16-a lifting device, 17-a top base, 18-a heating device, 19-a temperature control device, 20-a control door, 21-an ultrasonic probe, 22-a lock catch and 23-a vent pipe.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention.

An automatic device for preparing graphene composite materials by ultrasonic-assisted supercritical fluid comprises a carbon dioxide storage device, a conveying device, a reaction device and a waste gas treatment and recovery device 9.

The reaction device is divided into a plurality of independent spaces by a plurality of control doors 20, the spaces at two ends of the reaction device are an automatic sample feeding chamber 31 and an automatic sampling chamber 32, and the space between the automatic sample feeding chamber 31 and the automatic sampling chamber 32 is a temperature control chamber. The temperature control chamber is provided with a temperature adjusting device and a temperature sensor; the reaction device also comprises a reaction kettle 4, and the reaction kettle 4 can move in the automatic sample feeding chamber 31, the automatic sampling chamber 32 and the plurality of independent temperature control chambers; the reaction kettle 4 is provided with a pressure sensor 12 and a temperature sensor, the reaction device also comprises an ultrasonic processor 8 and a self-locking ventilation device, sealing ports are arranged on the temperature control chamber and the reaction kettle 4, and the self-locking ventilation device and the ultrasonic processor 8 are connected with the stainless steel reaction kettle 4 after penetrating through the sealing ports; the carbon dioxide storage device, the conveying device, the self-locking ventilation equipment and the waste gas treatment and recovery equipment 9 are connected in sequence through pipelines.

The intelligent control center 6 is used for controlling the opening and closing of the conveying device and the control door 20, and the intelligent control center 6 collects data of the pressure sensor 12 and the temperature sensor and controls the temperature adjusting device.

As an embodiment of the invention, the reaction device also comprises a top base 17, a lifting device 16 is fixed on the lower part of the top base 17, and the self-locking aeration equipment and the ultrasonic processor 8 are fixed on the lifting device 16. The lifting device 16 drives the self-locking ventilation equipment and the ultrasonic processor 8 to pass through the temperature control chamber and the sealing port on the reaction kettle 4 to be connected with the stainless steel reaction kettle 4. The intelligent control center 6 controls the lifting device 16 to act. The lifting device 16 can adopt an air cylinder, and the self-locking ventilation equipment and the ultrasonic processor 8 are respectively fixed on a piston rod of the air cylinder.

In one embodiment of the present invention, the manipulators 14 are disposed in both the automatic sample feeding chamber 31 and the automatic sampling chamber 32, the manipulator 14 in the automatic sample feeding chamber 31 is used for feeding the raw material into the reaction vessel 4, and the manipulator 14 in the automatic sampling chamber 32 is used for taking out the sample from the reaction vessel 4. The intelligent control center 6 controls the robot 14 to operate.

As one embodiment of the present invention, the temperature-controlled chambers include a first temperature-controlled chamber 51, a second temperature-controlled chamber 52, and a third temperature-controlled chamber 53.

The self-locking ventilation equipment is divided into self-locking gas injection equipment 71 and self-locking gas outlet equipment 72, the self-locking gas injection equipment 71 and the self-locking gas outlet equipment 72 are respectively positioned above the first temperature control chamber 51 and the third temperature control chamber 53, the self-locking gas injection equipment 71 is connected with the conveying device through a pipeline, and the self-locking gas outlet equipment 72 is connected with the waste gas treatment and recovery equipment 9 through a pipeline.

As an embodiment of the invention, the bottom of the stainless steel reaction kettle 4 is provided with the roller 15, so that the reaction kettle 4 can move between the temperature control room, the automatic sample feeding room 31 and the automatic sampling room 32 conveniently.

As an embodiment of the invention, a one-way valve 11 and a safety valve are arranged between the self-locking air bleeding device and the waste gas treatment and recovery device 9. The one-way valve 11 ensures that the gas flows from the self-locking gas outlet device 72 to the waste gas treatment and recovery device 9 in one way.

In the present invention, the carbon dioxide storage device and the transport device are respectively CO₂A gas cylinder 1 and an electric pump 2. The inlet and the outlet of the carbon dioxide storage device are respectively connected with the waste gas treatment and recovery device 9 and the self-locking gas injection device 71 through safety valves. CO 2₂The gas cylinder 1 is provided with a first pressure sensor 121.

Example (b):

referring to fig. 1 and 2, an automatic device for preparing a graphene composite material by using an ultrasonic-assisted supercritical fluid: comprising CO₂The device comprises a gas cylinder 1, an electric pump 2, an automatic feeding/sampling device 3, a stainless steel reaction kettle 4, a temperature control room 5, an ultrasonic processor 8, a self-locking ventilation device, a waste gas treatment and recovery device 9 and an intelligent control center 6. Wherein CO is₂The gas cylinder 1 is provided with a first pressure sensor 121, the inlet and the outlet of the cylinder opening are respectively provided with a safety valve, and the safety valve at the outlet is connected with the electric pump 2 through a pipeline; the outlet of the electric pump 2 is provided with a safety valve which is connected with a self-locking gas injection device 71 through a pipeline; the automatic feeding/sampling device 3 is connected to a temperature-controlled chamber 5, in which two manipulators 14 are installed.

The temperature control room 5 is divided into three independent first temperature control rooms 51, second temperature control rooms 52 and third temperature control rooms 53 by a control door 20, each independent temperature control room is provided with a heating device 18, a temperature control device 19 and a first temperature sensor 131, the tops of the first temperature control room 51 and the third temperature control room 53 are provided with sealing ports corresponding to self-locking ventilation devices, the top of the second temperature control room 52 is provided with a sealing port corresponding to the ultrasonic processing device 8, three independent temperature control room shells and the control door 20 are made of heat insulation materials, the opening and closing of the control door 20 are controlled by an intelligent control center, and each temperature control room can independently accommodate the stainless steel reaction kettle 4 for reaction without interference.

The second pressure sensor 122 and the second temperature sensor 132 are mounted on the reaction vessel 4, and the outer shell thereof is made of steel. The upper part of the reaction kettle 4 is provided with a connector which can be matched with a component vent pipe 23 of the self-locking ventilation device. The upper part of the reaction kettle 4 is also provided with a sealing port, so that the ultrasonic probe 21 of the ultrasonic processor 8 can be extended into the stainless steel reaction kettle 4.

The top end of the self-locking ventilation equipment is fixed by a lifting device 16The top base 17 can be divided into a self-locking gas injection device 71 and a self-locking gas injection device 72 which are respectively positioned at the upper parts of the first temperature control chamber 51 and the third temperature control chamber 53, the lower ends of the self-locking gas injection device 71 and the self-locking gas injection device 72 are composed of a lock catch 22 and a vent pipe 23, the self-locking gas injection device 71 is connected with the electric pump 2 through a pipeline, and the self-locking gas injection device 72 is connected with a waste gas treatment and recovery device through a pipeline; the ultrasonic processor 8 is fixed on the top base by the lifting device 16 and is positioned at the upper part of the second temperature control chamber 52, the ultrasonic probe 21 can go deep into the reaction kettle through the second temperature control chamber 52 and the sealing ports on the stainless steel reaction kettle 4, and the ultrasonic frequency and time of the ultrasonic probe are controlled by the intelligent control center 6; waste gas treatment and recovery equipment 9, self-locking gas injection equipment 72 and CO₂The gas cylinder 1 is connected through a pipeline, and a safety valve and a one-way valve 11 are assembled on the pipeline between the waste gas treatment and recovery device 9 and the self-locking gas injection device 72; the intelligent control center 6 integrates various control operations of the electric pump 2, the automatic feeding/sampling device 3, the temperature control chamber 5, the self-locking ventilation device, the ultrasonic processor 8 and the stainless steel reaction kettle 4, and can realize integrated control of temperature, pressure and time in the preparation process.

The specific use method of the invention is as follows:

1) the raw materials were put into the stainless steel reaction vessel 4 by the robot arm 14 of the automatic sample-feeding chamber 31.

2) The intelligent control center 6 detects the signal that the placement of the raw materials is finished, and issues an instruction to open the control door 20 between the automatic sample feeding chamber 31 and the first temperature control chamber 51, and the stainless steel reaction kettle 4 is driven by the bottom roller 15 to move to a preset position in the first temperature control chamber 51; after the intelligent control center 6 detects a signal that the stainless steel reaction kettle 4 reaches a preset position, the control door 20 is closed to form a closed space. Starting a temperature control device of the first temperature control chamber 51, and maintaining the temperature in the first temperature control chamber 51 to be unchanged at a set temperature; then the lifting device 16 descends to connect the self-locking gas injection equipment 71 with the stainless steel reaction kettle 4, at the moment, the lock catch 22 is closed, and the two vent pipes are connected together; then the intelligent control center 6 controls CO₂Opening the safety valve behind the gas cylinder and the electric pump, starting the electric pump at the same time, and introducing CO₂Gas is injected into the stainless steel reaction kettle 4 through a pipeline and a self-locking gas injection device 71; when in useWhen the pressure value in the stainless steel reaction kettle 4 reaches the preset pressure, the intelligent control center 6 controls the lock catch 22 of the self-locking gas injection equipment 71 to be opened, the vent pipe 23 is disconnected, and CO is discharged₂The safety valve is closed after the gas cylinder 1 and the electric pump 2 are closed, the electric pump 2 is closed, the stainless steel reaction kettle 4 stands in the first temperature control chamber 51, the temperature in the first temperature control chamber 51 is kept at the preset temperature, the pressure in the stainless steel pressure kettle is kept constant at the preset pressure, and the next step is carried out after the standing time reaches the preset value.

3) The intelligent control center 6 controls the heating device 18 and the temperature control device 19 of the second temperature control room 52 to work, after the temperature is raised to be the same as that of the first temperature control room 51, the control door 20 between the first temperature control room 51 and the second temperature control room 52 is opened, the stainless steel reaction kettle 4 is driven by the bottom roller 15 to move to the preset position in the second temperature control room 52, and then the control door 20 between the first temperature control room 51 and the second temperature control room 52 is closed; the second temperature control chamber 52 starts the operation of the heating device 18 and the temperature control device 19 to raise the temperature to a preset temperature, and the CO in the stainless steel reaction kettle 4 is maintained at the preset temperature₂Will reach and be maintained in a supercritical state; the intelligent control center 6 controls the lifting device 8 to descend, the ultrasonic probe 21 of the ultrasonic processor 8 is inserted into the stainless steel reaction kettle 4 from the second temperature control room 52 and the sealing port on the stainless steel reaction kettle 4 for ultrasonic processing, and the ultrasonic frequency and the ultrasonic time are set and controlled in the intelligent control center 6; and after the ultrasonic treatment is finished, the next step is carried out.

4) The intelligent control center 6 controls the heating device 18 and the temperature control device 19 of the third temperature control room 53 to work, the temperature is raised to be the same as that of the second temperature control room 52 and is kept unchanged, the control door 20 between the second temperature control room 52 and the third temperature control room 53 is opened, and the stainless steel reaction kettle 4 is driven by the bottom roller 15 to move to a preset position in the third temperature control room 53; then the control door 20 between the second temperature control room 52 and the third temperature control room 53 is closed, the lifting device 16 descends to connect the self-locking gas injection equipment 52 with the stainless steel reaction kettle 4, at this time, the lock catch 22 is closed, the vent pipe 23 of the two is connected together, at the same time, the safety valve in front of the waste gas treatment and recovery equipment 9 is opened to open the CO in the stainless steel reaction kettle 4₂Slowly releasing the gas until the pressure in the stainless steel reaction kettle 4 reaches the preset valueValue of CO evolved during which the preset temperature is maintained constant₂The gas enters a waste gas treatment and recovery device 9 for recovery treatment and then is stored in CO₂The gas cylinder is arranged inside; after the air release is finished, the lock catch 22 of the automatic air outlet device 52 is opened to disconnect the automatic air outlet device 72 from the stainless steel reaction kettle 4, the lifting device 16 is lifted to drive the automatic air outlet device 52 to move upwards to reach the original position, the preparation process is finished, and the temperature in the third temperature control chamber 53 is waited to be reduced to be the same as the room temperature.

5) And a control door 20 between the third temperature control room 53 and the automatic sampling room 32 is opened, the stainless steel reaction kettle 4 is driven by the bottom roller 15 to move to a preset position in the automatic sampling room 32, the intelligent control center 6 controls the manipulator 14 to take out the sample prepared in the reaction kettle 4, and the whole process is finished.

The supercritical fluid has gas-liquid dual characteristics, has density and solubility similar to those of liquid, viscosity and diffusion coefficient similar to those of gas, and has extremely high permeability and diffusivity. When the supercritical fluid is used for stripping graphene, the supercritical fluid can easily enter graphite layers, so that van der Waals force between the graphite layers is weakened, meanwhile, the supercritical fluid can adjust gas dissolving capacity and eliminate special physicochemical properties such as surface tension and the like, and the possibility of reducing transverse fracture of the graphene in the intercalation-stripping process from graphite to the graphene can be realized. Ultrasonic wave is a kind of mechanical vibration wave, which can efficiently transmit energy in fluid, so that after fluid molecules absorb the energy of sound field, a series of processes of activation, oscillation, stretching, shrinking, bursting collapse and the like can be completed instantly, and this phenomenon is called as "ultrasonic cavitation". When bubbles of ultrasonic cavitation are broken, high-speed liquid micro-jet can be generated to be used as a solvent micro-pump to force the supercritical fluid to enter the graphite layers. The high-pressure shock wave carried by the microjet can also provide shearing force locally to assist the stripping of the graphene sheet layer.

In summary, the device for preparing the graphene composite material based on the ultrasound-assisted supercritical fluid is provided with CO₂The gas cylinder, the electric pump, the automatic feeding/sampling equipment, the temperature control chamber, the stainless steel reaction kettle with the roller, the liftable self-locking ventilation equipment, the ultrasonic processing equipment and the intelligent control center are matched for use, so that the production is realizedThe preparation process is automated and precise; CO 2₂The gas cylinder, the electric pump, the self-locking gas injection equipment and the stainless steel reaction kettle can enable the supercritical fluid to be used as a solvent for stripping graphene, and meanwhile, an independent temperature control room can provide an accurate and stable temperature environment for each reaction step; the ultrasonic processor can go deep into the stainless steel reaction kettle to carry out ultrasonic treatment on the reaction, and the ultrasonic cavitation brought by the ultrasonic wave can assist the stripping of the graphene sheet layer; the device adopts streamlined operation, after the current reaction step is finished, the reaction kettle automatically enters the next step, and the operation device in the previous reaction step is vacated for another reaction kettle; of course, 5 reaction kettles can be operated simultaneously, and the mass production preparation of the graphene composite material is powerfully guaranteed.

The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent structures or equivalent flow transformations made by using the contents of the specification and the drawings, or applied directly or indirectly to other related systems, are included in the scope of the present invention.