TWI720868B - Process method and device for industrialized mass production of high-purity porous graphene powder - Google Patents

Abstract

The present invention provides a process method for industrialized mass production of high-purity porous graphene powder; the process method includes: (1) taking liquid polyimide in an ultrasonic sprayer for ultrasonic oscillation to make it atomized into mist (2) Make the polyimide mist particles enter a preparation tube, and perform carbon dioxide laser irradiation in the preparation tube; (3) The polyimide mist particles are irradiated by carbon dioxide laser Then, high-purity porous graphene powder is formed and falls on the bottom of the preparation cylinder; thereby, a new mass production method of high-purity porous graphene powder can be provided, and excellent production economic efficiency can be achieved.

Description

Process method and device for industrialized mass production of high-purity porous graphene powder

The present invention relates to a mass production technology of graphene, in particular to a process method and device for mass production of high-purity porous graphene powder by spraying, ultrasonic irradiation, and carbon dioxide laser irradiation.

Graphite is a crystalline structure composed of multiple layers of graphene, while graphene is a single-layer graphite structure. Each carbon atom forms a bond with three adjacent carbon atoms in an sp2 crystalline structure and extends into The honeycomb hexagonal two-dimensional structure, graphene has been widely used in semiconductors, touch panels or solar cells and other fields, and is expected to be widely used in photovoltaics, green energy power generation, environmental biomedical sensing, composite Development of functional materials and many other industrial fields.

Conventional graphene manufacturing methods include mechanical exfoliation, epitaxial growth, chemical vapor deposition (CVD), chemical exfoliation, and electrochemistry. Methods such as electrochemical exfoliation. Although some of these conventional graphene manufacturing methods can produce graphene powder, they are still not a fast and ideal graphene powder efficient mass production and production, and it is not easy to produce high-purity porous graphene, so it is not ideal. The manufacturing method of the product.

For this reason, in view of the fact that the conventional manufacturing method of graphene is not ideal, the inventors set out to develop and conceive its solution, hoping to develop a manufacturing method for energy-producing high-purity porous graphene powder to promote The development of this industry resulted in the creation of the present invention after many years of thinking.

The purpose of the present invention is to provide an industrialized mass production of high-purity porous graphene The powder manufacturing method and its device have the feasibility of mass production, and facilitate the collection and use of graphene, thereby achieving excellent economic efficiency in the production of high-purity porous graphene powder.

In order to achieve the above object, the technical method adopted by the present invention includes: Step 1: Take liquid polyimide in an ultrasonic sprayer and perform ultrasonic oscillation to atomize it into mist-like particles; Step 2: Make The polyimide mist particles enter a preparation tube, and carbon dioxide laser irradiation is performed in the preparation tube; Step 3: After the polyimide mist particles are irradiated with carbon dioxide laser, high-purity porous graphite is formed Alkene powder, and fall on the bottom of the preparation cylinder.

In the foregoing method embodiment, the liquid polyimide is a liquefied Katpon®.

In the foregoing method embodiment, the step 1 is to further introduce a hot air flow into the ultrasonic sprayer, the ultrasonic sprayer is connected to the preparation cylinder, and the hot air flow enters the preparation cylinder for drying. Program operation.

In the foregoing method embodiment, the step 2 is to further introduce a hot air flow into the preparation cylinder to perform the drying process.

In the foregoing method embodiment, the porous graphene powder in the step 3 refers to a few layers of porous graphene with 2-5 layers.

In the foregoing method embodiment, the lower half of the preparation cylinder is a bucket-shaped groove with a wide top and a narrow bottom, and a heating element is arranged around the bucket-shaped groove to provide heating to the preparation cylinder and maintain the preparation. The temperature in the cylinder.

In the foregoing method embodiment, wherein the bottom of the preparation cylinder is provided with a filter, and the bottom is connected with a discharge pipe to communicate with a separator; the separator is connected with a hot gas exhaust pipe, and the heat exhaust pipe is connected with a motor so that The heat exhaust pipe removes hot air, and the separator is equipped with a bag filter, so that the fine porous graphene powder falling on the bottom of the preparation cylinder passes through the filter screen, and is separated from the air through the exhaust pipe, and is It is transported to the separator, passes through the bag filter, and then falls into a collection tank.

The technical means of the present invention also includes: a device for industrial mass production of high-purity porous graphene powder, which includes: a preparation cylinder, the inner and upper periphery of which is provided with a plurality of dioxins Carbonized laser irradiator; an ultrasonic sprayer connected to the top of the preparation tube; a storage tank connected to the ultrasonic sprayer; the aforementioned structure, the storage tank is used to set the liquid polyimide, the liquid The polyimide is transported to the ultrasonic sprayer and atomized into mist-like particles, and the liquid polyimide of the mist-like particles is input into the preparation cylinder and irradiated by the carbon dioxide laser of the carbon dioxide laser irradiators to form high-purity porous The graphene powder falls on the bottom of the preparation cylinder.

In the foregoing embodiment, it further includes an air heater, the air heater is connected to a heating pipe, and the heating pipe is connected to the preparation cylinder.

In the foregoing embodiment, the heating pipeline is first connected to the preparation cylinder via the ultrasonic sprayer.

In the foregoing embodiment, the storage tank is connected to the ultrasonic sprayer via a product pipeline, and a first motor is provided on the product pipeline.

In the foregoing embodiment, the lower half of the preparation cylinder is a bucket-shaped groove with a wide top and a narrow bottom, a heating element is arranged around the bucket-shaped groove, and a filter screen is provided at the bottom of the preparation cylinder. The bottom of the preparation cylinder is connected with a discharge pipe to communicate with a separator. The upper part of the separator is connected with a heat exhaust pipe. The heat exhaust pipe is connected with a second motor. The separator is also provided with a bag filter to make it fall in the preparation. The porous graphene powder at the bottom of the cylinder passes through the filter screen, is separated from the air through the discharge pipe, and is transported to the separator, passes through the bag filter, and falls into a collection tank.

In order to enable your reviewer to have a better understanding and understanding of the technology, method features and achieved effects of the present invention, a preferred embodiment diagram and detailed description are provided. The description is as follows:

11: Polyimide

201: Step 1

202: Step 2

203: Step 3

221: product pipeline

24: storage tank

25: 1st motor

26: Ultrasonic sprayer

31: Preparation cylinder

311: Bucket Slot

312: bottom

313: Filter

314: discharge pipe

316: CO2 laser irradiator

318: heating element

32: Air heater

321: Heating line

33: 2nd motor

331: Heat exhaust pipe

34: Separator

341: Bag filter

35: Collection tank

Figure 1 is a three-dimensional schematic diagram of an embodiment of the device of the present invention.

Figure 2 is a top sectional view of an embodiment of the device of the present invention.

Figure 3 is a schematic flow diagram of the manufacturing method of the present invention.

Please refer to Figures 1, 2 and 3, which show the industrialized mass production of high-purity porous graphite according to the present invention. The preferred embodiments of the process method of olefin powder and the device thereof, these drawings are schematic diagrams for convenience of description, they are only schematically illustrating the basic structure of the present invention, and the drawing of the displayed composition is not limited to the same The shape and size ratio in actual implementation, and the shape and size ratio in actual implementation is an optional design.

As shown in the figure, the present invention provides a process method and device for industrial mass production of high-purity porous graphene powder; the process method and device include:

Step 1 (201): Take liquid polyimide in an ultrasonic sprayer and perform ultrasonic oscillation to make it atomized into mist-like particles; to be more specific, take liquid polyimide 11 (Polyimide, PI for short) ) And placed in a storage tank 24, the storage tank 24 is connected to a product pipeline 221, the product pipeline 221 is connected to an ultrasonic sprayer 26, the liquid polyimide 11 is transported through the product pipeline 221 To the ultrasonic sprayer 26.

Step 2 (202): Make the polyimide mist particles enter a preparation tube, and perform carbon dioxide laser irradiation in the preparation tube; in detail, the ultrasonic sprayer 26 is set in a preparation tube 31 (center ) Above and in communication with a preparation cylinder 31, the preparation cylinder 31 is provided with a plurality of carbon dioxide laser irradiators 316 at the upper periphery of the interior, and the carbon dioxide laser irradiation system of the carbon dioxide laser irradiators 316 is directed to the preparation cylinder The center of 31; the product pipeline 221 is connected to one end of the ultrasonic sprayer 26, and the preparation tube 31 is connected to the other end of the ultrasonic sprayer 26;

Step 3 (203): After the polyimide mist particles are irradiated with carbon dioxide laser, high-purity porous graphene powder is formed and falls on the bottom of the preparation cylinder; in detail, the polyimide 11 The atomized tiny particles (mist-like particles) are irradiated by the carbon dioxide laser to form high-purity porous graphene powder and fall on the bottom 312 of the preparation cylinder 31.

In the foregoing configuration and implementation method, the liquid polyimide 11 first flows through the ultrasonic sprayer 26, and then is sprayed by the ultrasonic sprayer 26 and then enters atomized fine particles (ie, mist-like particles) into the preparation tube 31 , The ultrasonic sprayer 26 uses the principle of electronic oscillation and uses a piezoelectric crystal oscillator (piezoelectric oscillator/oscillator) to generate high-frequency shock waves (ultrasonic waves) to act on the liquid polyimide 11 to transform the liquid The polyimide 11 is shattered into extremely small mist particles. In this embodiment, a fan (that is, a wind flow is generated) can be further used to send out the mist particles of the polyimide 11. at this time The carbon dioxide laser irradiators 316 located in the preparation cylinder 31 also simultaneously activate the carbon dioxide laser to irradiate the atomized fine particles (mist-like particles);

Thereby, a new mass production method of high-purity porous graphene powder can be provided, and excellent production economic efficiency can be achieved.

Among them, the liquid polyimide 11 is a liquefied Katpon®. Katpon® is the trade name of the polyimide (PI) film material produced by DuPont in the United States. It is available on the market and can be used by applying this product. Get polyimide quickly and at low cost.

In addition, the following steps can be added to step 1 (201): adding an air heater 32 and a heating pipe 321, the heating pipe 321 is connected to the air heater 32 and the ultrasonic sprayer 26, the air heating The device 32 is used to generate a hot air flow in the ultrasonic sprayer 26 to provide hot air for spraying and drying the liquid polyimide 11, that is, the air heater 32 passes the hot air through the The heating pipe 321 is conveyed to the ultrasonic sprayer 26, so that the ultrasonic sprayer 26 uses the hot air to accelerate the spraying and granulation of the liquid polyimide 11, and make the polyimide 11 into the preparation cylinder 31 The atomized micro particles (mist-like particles) are still heated by the hot air in the preparation cylinder 31 for the drying process. The atomized polyimide 11 fine particles are irradiated by a carbon dioxide laser to cause the atomic lattice of the polyimide 11 mist particles to vibrate, breaking the C=O and NC bonds in the molecule, making it The atoms rearrange the aromatic compounds (Aromatic compounds) to form porous graphene, and it is also dried by the hot air to be granulated; because polyimine contains aromatic and imide, so Polyimide can eventually form porous graphene powder. In addition, the heating pipe 321 can also be directly connected to the preparation cylinder 31 to operate the hot air flow with a drying effect in the preparation cylinder 31 for the drying process. Furthermore, a first motor 25 can be provided on the product pipeline 221 of step 2 (202) to provide the function of extracting and outputting the liquid polyimide 11.

Among them, the ultrasonic vibration atomization operation of the ultrasonic sprayer 26 in the step 1 (201) and the carbon dioxide laser irradiation of the carbon dioxide laser irradiator 316 in the step 2 (202), when the ultrasonic sprayer 26 is supersonic The sonic oscillating atomization operation and the stronger the intensity of the carbon dioxide laser irradiation of these carbon dioxide laser irradiators 316, or the longer the oscillation and irradiation time, the more the formation The more porous graphene powder is produced, on the contrary, when the ultrasonic vibration atomization operation of the ultrasonic sprayer 26 and the carbon dioxide laser irradiation intensity of the carbon dioxide laser irradiators 316 are weaker, or the vibration and irradiation time is longer Shorter, the less porous graphene powder is formed, so that the powder rate and the number of layers can be adjusted. The aforementioned porous graphene powder refers to 2-5 layers of porous graphene. This is because the more energy the laser irradiates, the more energy is provided for the porous graphene to be reacted into a single layer, so the number of single-layer porous graphene powders produced is also greater.

In addition, optionally, the lower half of the preparation cylinder 31 is a bucket-shaped groove 311 with a wide upper part and a narrow lower part, so that the porous graphene finally falls on the bottom 312 of the preparation cylinder, and its area is larger than that of the preparation cylinder 31. The upper part is small to facilitate the collection of porous graphene.

In addition, optionally, a heating element 318 is arranged around the bucket-shaped groove 311 to provide heating in the preparation cylinder 31 and maintain the temperature in the preparation cylinder 31 to accelerate the accumulation of liquid in the preparation cylinder 31. The reaction of the imine 11 to form porous graphene powder.

In addition, the bottom 312 of the preparation cylinder 31 is provided with a filter 313, and the bottom 312 is connected to a discharge pipe 314 to communicate with a separator 34; the separator 34 can be like a cyclone separator with a hot gas exhaust pipe 331 connected above it. The heat exhaust pipe 331 is connected to a second motor 33 to remove the hot air from the heat exhaust pipe 331. The separator 34 is also provided with a bag filter 341 to allow the porous graphene powder falling on the bottom 312 of the preparation cylinder to pass through After passing through the filter screen 313, it is separated from the air through the discharge pipe 314, and is transported to the separator 34, passes through the bag filter 341, and falls into a collection tank 35. The porous graphite is taken out from the collection tank 35. The olefin powder can be used in industry.

The process method and device for the industrial mass production of high-purity porous graphene powder of the present invention are designed with the aforementioned structure, which can make high-purity porous graphene feasible for mass production, and facilitate the collection and collection of high-purity porous graphene. It can be used to achieve the excellent economic efficiency of the production of high-purity porous graphene powder.

In summary, the present invention is indeed an excellent creative idea, and an invention patent application was filed in accordance with the law; however, the content of the above description is only a preferred embodiment of the present invention, and everything extended by the technical means of the present invention Changes should fall within the scope of the patent application of the present invention.

11: Polyimide

221: product pipeline

24: storage tank

25: 1st motor

26: Ultrasonic sprayer

31: Preparation cylinder

311: Bucket Slot

312: bottom

313: Filter

314: discharge pipe

316: CO2 laser irradiator

318: heating element

32: Air heater

321: Heating line

33: 2nd motor

331: Heat exhaust pipe

34: Separator

341: Bag filter

35: Collection tank

Claims (10)

A process method for industrial mass production of high-purity porous graphene powder, which includes: Step 1: Take the liquid polyimide in an ultrasonic sprayer and perform ultrasonic oscillation to make it atomized into mist-like particles; Step 2: Make the polyimide mist particles enter a preparation tube, and perform carbon dioxide laser irradiation in the preparation tube; Step 3: After the polyimide mist particles are irradiated with carbon dioxide laser, high-purity porous graphene powder is formed and falls on the bottom of the preparation cylinder. As described in item 1 of the scope of patent application, a process method for the industrial mass production of high-purity porous graphene powder, wherein the liquid polyimide is a liquefied Katpon®. An industrialized mass production process method for high-purity porous graphene powder as described in item 1 of the scope of patent application, wherein step 1 further introduces a hot air flow into the ultrasonic sprayer, and the ultrasonic sprayer is connected to the preparation The hot air flow enters the preparation barrel for the drying process; the step 2 is to further introduce a hot air flow into the preparation barrel for the drying process. As described in item 1 of the scope of the patent application, a process method for the industrial mass production of high-purity porous graphene powder, wherein the porous graphene powder in step 3 refers to 2-5 layers of porous graphene with few layers. An industrialized mass production of high-purity porous graphene powder as described in item 1 of the scope of patent application, wherein the bottom half of the preparation cylinder is a bucket-shaped groove with a wide top and a narrow bottom, and the periphery of the bucket-shaped groove A heating element is provided around the preparation cylinder to heat the preparation cylinder and maintain the temperature in the preparation cylinder. The bottom of the preparation cylinder is provided with a filter screen, and the bottom is connected with a discharge pipe to communicate with a separator; the separator There is a hot exhaust pipe connected to the top, the exhaust pipe is connected to a motor to allow the exhaust pipe to remove hot air, and the separator is equipped with a bag filter to allow the porous graphene fine powder falling on the bottom of the preparation cylinder to pass through The filter is separated from the air through the discharge pipe, and is transported to the separator, passes through the bag filter, and falls into a collection tank. An industrialized mass production device for high-purity porous graphene powder, which includes: A preparation tube, with a plurality of carbon dioxide laser irradiators on the upper periphery of the inside; An ultrasonic sprayer connected to the top of the preparation cylinder; A storage tank connected to the ultrasonic sprayer; In the foregoing structure, the storage tank is used to set liquid polyimide, the liquid polyimide is delivered to the ultrasonic sprayer and atomized into mist particles, and the liquid polyimide of the mist particles is input into the preparation cylinder, and The high-purity porous graphene powder is formed by the carbon dioxide laser irradiated by the carbon dioxide laser irradiators and falls on the bottom of the preparation cylinder. As described in item 6 of the scope of patent application, a device for the industrialized mass production of high-purity porous graphene powder further includes an air heater connected to a heating pipe, and the heating pipe is connected to the preparation cylinder. As described in item 7 of the scope of patent application, an industrialized mass production device for high-purity porous graphene powder, wherein the heating pipe is connected to the preparation cylinder through the ultrasonic sprayer. As described in item 8 of the scope of patent application, an industrialized mass production device for high-purity porous graphene powder, wherein the storage tank is connected to the ultrasonic sprayer by a product pipeline, and a first motor is provided on the product pipeline. As described in item 8 of the scope of patent application, an industrialized mass production device for high-purity porous graphene powder, wherein the lower half of the preparation cylinder is a bucket-shaped groove with a wide upper and a narrow bottom, and the circumference of the bucket-shaped groove is A heating element is wound around, the bottom of the preparation cylinder is provided with a filter, the bottom of the preparation cylinder is connected with a discharge pipe to communicate with a separator, and a hot gas exhaust pipe is connected above the separator, and the heat exhaust pipe is connected with a The second motor, the separator is equipped with a bag filter, so that the porous graphene powder falling on the bottom of the preparation cylinder passes through the filter, and is separated from the air through the discharge pipe, and is transported to the separator and passed through After passing through the bag filter, it falls into a collection tank.

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