Preparation method of novel high-grade alkyne nano-graphite
The novel method for preparing high-grade acetylene nanographite solves the problems of high energy consumption, environmental pollution, and low product purity in existing technologies. It enables efficient resource utilization of high-grade acetylene tail gas to produce high-purity nanographite, which has the stability and economics for industrial application.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-01-19
- Publication Date
- 2026-04-10
AI Technical Summary
Existing nanographite preparation technologies suffer from high energy consumption, environmental pollution, high cost, and low product purity. In particular, they lack the resource utilization of high-grade alkyne tail gas and lack standardized catalytic media and product separation processes.
A novel method for preparing advanced acetylene nanographite is employed, comprising steps such as feed gas pretreatment, mixing and pressure stabilization, catalytic medium loading and reactor preheating, feed gas catalytic reaction, preliminary gas-solid separation, and nanographite cooling and secondary purification. The method utilizes molten medium catalysis and multi-stage temperature control, combined with cyclone separation and multi-layer filtration units, to achieve efficient separation and purification.
It realizes the resource utilization of high alkyne tail gas, producing sheet-like nanographite with a purity of ≥99% and a particle size concentrated in 50-200nm, reducing energy consumption and environmental pollution, improving the purity and stability of the product, and making it suitable for industrial applications.
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Figure CN121823563A_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the technical field of nanographite preparation apparatus, specifically, it relates to a novel method for preparing advanced acetylene nanographite. Background Technology
[0002] With the urgent global need for carbon emission reduction, the resource utilization of industrial waste gas has become one of the core directions in the field of green chemical industry.
[0003] As an important basic chemical process, natural gas to acetylene produces approximately 16% high-grade alkyne tail gas (containing multiple components such as acetylene, butyryl, and benzene) for every ton of acetylene produced. Currently, the industry mainly treats this tail gas by direct combustion or flare emission, which not only wastes high-quality carbon sources but also generates additional CO2 emissions, failing to meet the "dual carbon" target.
[0004] Meanwhile, due to its excellent electrical conductivity, thermal conductivity, and mechanical properties, nano-graphite is widely used in lithium battery anodes, thermal conductive films, supercapacitors, and other fields, with an average annual growth rate of over 15% in market demand. Among the existing nano-graphite preparation technologies, mechanical exfoliation requires high-pressure grinding (energy consumption > 500 kWh / t) and the product particle size is uneven; chemical intercalation requires the use of strong acids and bases (such as concentrated sulfuric acid and hydrofluoric acid), which easily causes environmental pollution and the product purity is < 95%; although the vapor deposition method has higher purity, it relies on high-purity methane / acetylene as raw materials (cost > 8000 yuan / ton), making it difficult to achieve low-cost large-scale production.
[0005] As a novel carbon material preparation technology, melt media catalysis technology aims to promote the directional cracking and rearrangement of carbon sources through the catalytic action of metal / metal oxide media. However, existing melt media catalysis technologies mostly use pure acetylene or methane as raw materials, without involving the complex components of advanced alkyne tail gas. Furthermore, the reaction system design lacks a raw material pretreatment unit specifically for the polymerization characteristics of advanced alkynes, resulting in poor raw material transport stability. At the same time, the separation process between the catalytic medium and the product has not been standardized, making it difficult to meet the purity requirements of high-end applications. Summary of the Invention
[0006] The technical problem to be solved by the present invention is to overcome the shortcomings of the prior art and provide a nano-graphite preparation device that can overcome or at least partially solve the above problems.
[0007] To solve the above-mentioned technical problems, the basic concept of the technical solution adopted by the present invention is: a novel method for preparing advanced acetylene nanographite, mainly including the following operation steps: Step 1: Pretreatment of raw gas conveying system Check the sealing of the heat tracing pipeline (DN50 carbon steel with PTFE coating on the inner wall) and the 200L 304 stainless steel mixing tank to ensure there are no leaks; Turn on the electric heat tracing device, set the temperature control range to 55-60℃, monitor the temperature of the pipeline and mixing tank in real time through the temperature probe, keep it warm for 30 minutes until the temperature stabilizes in the set range, and avoid the self-polymerization of advanced alkynes.
[0008] Step 2: Introducing, mixing, and stabilizing the raw material gas Open the high-grade alkyne inlet valve and introduce the high-grade alkyne tail gas, a byproduct of acetylene production from natural gas, into the mixing tank. Control the initial flow rate to 200 mL / min using a flow sensor. Turn on the booster controller and argon gas inlet valve to introduce high-purity argon gas with a purity of ≥99.9%, and use the spiral airflow distributor in the mixing tank to mix the two gases evenly. The pressure inside the tank is monitored in real time by a pressure gauge, and the argon gas intake is automatically adjusted by a pressure booster controller: argon gas is added when the pressure is <80kPa, and the pressure relief valve is opened when the pressure is >120kPa, so that the pressure inside the tank is finally stabilized at 80-120kPa, and the mixing time lasts for 10 minutes.
[0009] Step 3: Catalytic medium loading and reactor preheating Fill the detachable porous medium basket (pore size 50-100μm) of the molten medium catalytic reaction unit with the selected catalytic medium (copper-bismuth alloy Cu-Bi90:10 or Fe2O3-based composite medium Fe2O3-Al2O385:15) and install the medium basket into the catalytic medium chamber at the bottom of the 5L Inconel 625 high-temperature alloy reactor. Turn on the temperature control system and electric heater, and raise the temperature according to the multi-stage heating program: from room temperature to 800℃, the heating rate is 5℃ / min; from 800 to 1100℃, the heating rate is 2℃ / min. After reaching the target reaction temperature, keep it at that temperature for 1 hour to ensure that the catalyst medium is completely melted.
[0010] Step 4: Catalytic reaction and parameter control of feed gas Open the gas outlet valve of the mixing tank and introduce the pretreated mixed raw material gas into the reactor. The gas is then evenly dispersed onto the surface of the molten catalyst medium by the gas distributor at the top of the reactor. The central controller dynamically adjusts the feed gas flow rate (100-500 mL / min) based on the concentration of higher alkynes in the feed gas (e.g., butadiyne content 6.45%, benzene content 4.995%): it is adjusted to 100-200 mL / min when the concentration is high and to 400-500 mL / min when the concentration is low. The pressure inside the reactor is maintained at 0.1-0.15 MPa by a pressure monitoring module. Under the action of the molten catalytic medium, the C≡C bond breaks (directional cracking) of higher alkynes, and carbon atoms rearrange in an orderly manner on the surface of the medium to generate nano-graphite. The reaction lasts for 2-4 hours.
[0011] Step 5: Preliminary gas-solid separation (cyclone separation) The nano-graphite generated by the reaction, along with the gaseous products (hydrogen, argon, and unreacted light hydrocarbons), enters a cyclone separator. The airflow speed is set to 15-20 m / s, and centrifugal force is used to throw the nano-graphite with a particle size of 50-200 nm toward the inner wall of the separator. Nanographite falls along the wall of the separator into a 10L carbon product collection tank below. The anti-vortex baffle installed at the top of the separator reduces the risk of gas entrainment of solid particles and ensures that the initial separation efficiency is ≥99%.
[0012] Step Six: Cooling and Secondary Purification of Nano-Graphite Cooling water at 25-30℃ is introduced into the cooling jacket of the carbon product collection tank to cool the nano-graphite inside the tank to room temperature for 30 minutes. By utilizing a detachable filter with a 20μm pore size at the bottom of the carbon product collection tank, trace impurities remaining in the nano-graphite are filtered out, further improving the purity of the product.
[0013] Step 7: Exhaust gas filtration and emission compliance The gaseous products after initial separation by the cyclone separator are cooled and then enter a gas filter equipped with a ceramic membrane filter element (pore size 0.1μm) to remove tiny carbon particles with a particle size <50nm entrained in the gas. The oxygen content of the gas is monitored by an oxygen content sensor at the filter outlet to ensure that the oxygen content is ≤2%. Once the standard is met, the gas is discharged through the exhaust outlet. If the oxygen content is >2%, the alarm module is triggered and the emission is suspended.
[0014] Step 8: Product Detection and Parameter Optimization Remove the bottom filter of the carbon product collection tank, collect the nano-graphite product, and use X-ray diffraction (XRD) to detect the purity (≥99%). Observe the morphology and particle size (50-200nm) by scanning electron microscopy (SEM). Change the reaction parameters (reaction temperature 800-1100℃, catalyst medium type, feed gas flow rate 100-500mL / min), repeat steps one to seven, and take the average value for each set of parameters in three experiments; Record the curing rate of higher alkynes under different parameters (curing rate = carbon mass of generated nano-graphite / carbon mass of higher alkynes in feed gas × 100%), and screen out the optimal process parameters with a curing rate ≥ 40% and purity ≥ 99%.
[0015] Step Nine: System Stability Verification Under optimal process parameters, the system was started and ran continuously for 72 hours. During this period, samples were taken every 12 hours according to the detection method in step eight to test the purity of the nano-graphite, ensuring that the purity fluctuation range was ≤0.5%. The system monitors the operating parameters of each unit in real time (pipeline temperature, reactor pressure, gas flow rate, etc.), and records the operating data by the data acquisition and control unit to verify the stability and reliability of the system for industrial application.
[0016] Furthermore, the gas filter is equipped with an air inlet, an air outlet, and a pressure detection device, and internally, from bottom to top, are filter unit one and filter unit two.
[0017] Furthermore, the filter unit includes multiple sets of mounting brackets and multiple sets of filter canisters. The filter canisters are located on the mounting brackets, and a canister cover is detachably connected to the top of the filter canister. Filter holes are provided on both the filter canister and the canister cover. A cross-shaped partition plate is installed inside the filter canister, which divides the filter canister into four chambers. The partition plate is lower than the canister cover. Activated carbon is filled inside the filter canister, and the top of the activated carbon is lower than the partition plate. The second filtration unit includes a ceramic filter element.
[0018] Furthermore, multiple sets of telescopic rods are installed inside the filter tank. An inclined push plate is fixedly connected to the telescopic end of each telescopic rod. The two ends of the push plate abut against the tank cover and the filter tank, respectively. By moving the push plate, the activated carbon inside the chamber can be moved. The inclined push plate pushes the activated carbon up and into other chambers, preventing the bottom activated carbon from adsorbing too many particles while the top is unadsorbed. This ensures that the activated carbon flows continuously, promoting uniform adsorption. It is important to note that the push plates in the multiple filter units should not be pushed synchronously, ensuring that one or two filter units continuously adsorb particles in the gas.
[0019] Furthermore, two sets of arc-shaped telescopic cylinders are fixedly connected to the mounting frame, and a top plate is fixedly connected to the bottom of the filter tank. The telescopic ends of the arc-shaped telescopic cylinders abut against the top plate. By extending the telescopic ends of the telescopic cylinders, the filter tank can be intermittently rotated on the mounting frame, thereby generating vibration, which makes the activated carbon in the chamber more uniform under the vibration state.
[0020] Furthermore, the mounting bracket is rotatably connected to multiple sets of ball bearings, which abut against the filter canister to facilitate its rotation.
[0021] After adopting the above technical solution, the present invention has the following beneficial effects compared with the prior art: The present invention realizes the resource utilization of the high alkyne tail gas by-product of natural gas to acetylene, solves the problem of tail gas waste and emission pollution, and produces high-quality sheet-like nano-graphite with a purity ≥99% and a particle size concentrated in 50-200nm through molten medium catalysis, multi-stage temperature control and secondary purification. Attached Figure Description
[0022] In the attached diagram: Figure 1 This is a schematic diagram of the structure of a novel method for preparing advanced acetylene nanographite proposed in this invention; Figure 2 This is a cross-sectional view of a novel method for preparing advanced acetylene nanographite proposed in this invention. Figure 1 ; Figure 3 This is a cross-sectional view of a novel method for preparing advanced acetylene nanographite proposed in this invention. Figure 2 ; Figure 4 This is a schematic diagram of the mounting frame, filter tank, and tank lid in a novel method for preparing advanced acetylene nanographite proposed in this invention. Figure 5 This is a cross-sectional schematic diagram of the filter unit one in the novel advanced acetylene nanographite preparation method proposed in this invention. Figure 6 This invention proposes a novel method for preparing advanced acetylene nanographite. Figure 5 A schematic diagram of the structure of part A; Figure 7 This is a bottom view of the filter unit one in the novel advanced acetylene nanographite preparation method proposed in this invention.
[0023] In the diagram: 1. Gas filter; 101. Air inlet; 102. Air outlet; 103. Pressure detection device; 201. Mounting bracket; 202. Ball bearing; 301. Filter canister; 302. Divider plate; 303. Canister cover; 304. Top plate; 401. Telescopic rod; 402. Push plate; 5. Telescopic cylinder; 6. Ceramic filter element. Detailed Implementation
[0024] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the accompanying drawings. The following embodiments are used to illustrate the present invention, but are not intended to limit the scope of the present invention.
[0025] Example: Refer to Figure 1-7 A novel method for preparing advanced acetylene nanographite mainly includes the following steps: Step 1: Pretreatment of raw gas conveying system Inspect the flange connections of the heat tracing pipeline (DN50 carbon steel with PTFE coating on the inner wall) and the inlet and outlet valves of the 200L304 stainless steel mixing tank. Apply soapy water to the sealing surface and let it stand for 5 minutes. If no bubbles are generated, the sealing performance is confirmed to be qualified. Turn on the electric heat tracing device, set the temperature control range to 55-60℃, and monitor the temperature in real time through temperature probes on the pipeline and the outer wall of the mixing tank. After 30 minutes of heat preservation, the temperature stabilizes at 58℃, which meets the requirements for preventing polymerization of high-grade alkynes.
[0026] Step 2: Introducing, mixing, and stabilizing the raw material gas Open the high-grade alkyne inlet valve, set the initial exhaust gas flow rate to 200 mL / min using the flow sensor, and introduce it into the mixing tank. Turn on the booster controller and argon inlet valve to introduce high-purity argon gas with a purity of 99.95%, and mix the gas using the spiral airflow distributor in the mixing tank. The pressure is monitored in real time by the pressure gauge on the top of the mixing tank: when the pressure drops to 78 kPa, argon gas is added; when it rises to 122 kPa, the pressure relief valve is opened; after continuous adjustment for 10 minutes, the pressure inside the tank stabilizes at 100 kPa.
[0027] Step 3: Catalytic medium loading and reactor preheating Select a copper-bismuth alloy catalyst medium (Cu:Bi=90:10), fill it into a detachable porous medium basket (pore size 50μm), and install the medium basket into the catalyst medium chamber at the bottom of a 5L Inconel 625 high-temperature alloy reactor; Turn on the temperature control system and electric heater, and start multi-stage heating: Room temperature (25℃) → 800℃: heating rate 5℃ / min, time 155min; 800℃→1050℃ (target reaction temperature): heating rate 2℃ / min, time 125min;
[0028] After heating to 1050℃, hold the temperature for 1 hour to confirm that the catalytic medium is completely melted.
[0029] Step 4: Catalytic reaction and parameter control of feed gas Open the gas outlet valve of the mixing tank and introduce the pretreated mixed raw material gas into the reactor. The gas is then evenly dispersed onto the surface of the molten catalyst medium by the gas distributor at the top of the reactor. The pressure inside the reactor was maintained at 0.12 MPa by a pressure monitoring module. Under the action of the molten medium, the C≡C bonds of the higher alkynes underwent directional cracking, and the carbon atoms rearranged in an orderly manner to generate nano-graphite. The reaction continued for 3 hours.
[0030] Step 5: Preliminary gas-solid separation The nano-graphite produced by the reaction, along with the gaseous products (hydrogen, argon, and unreacted methane), enters a cyclone separator with a set airflow velocity of 18 m / s. Under centrifugal force, the nano-graphite is thrown towards the inner wall of the separator and falls into the 10L carbon product collection tank below. The anti-vortex baffle at the top of the separator effectively reduces the proportion of solid particles entrained in the gas, and the initial separation efficiency reaches 99.2%.
[0031] Step Six: Cooling and Secondary Purification of Nano-Graphite Cooling water at 28°C was introduced into the cooling jacket of the carbon product collection tank to cool the nano-graphite inside the tank to room temperature for 30 minutes. The 20μm pore size filter screen at the bottom of the collection tank was removed to filter out residual trace impurities (such as unreacted light hydrocarbon residues) and obtain preliminarily purified nano-graphite products.
[0032] Step 7: Exhaust gas filtration and emission compliance The gaseous products separated by the cyclone separator are passed into the cooler and cooled to 70°C. Then, they enter the equipment through the inlet 101 of the gas filter 1. Pre-treatment of filter unit 1 (adjustment of activated carbon distribution): The mounting bracket 201 of the first filter unit is equipped with four sets of filter canisters 301. Each filter canister 301 is divided into four chambers by a cross-shaped partition plate 302. The chambers are pre-filled with activated carbon to a height lower than the partition plate 302, and then covered with a canister cover 303 with filter holes and sealed. Activate the telescopic rod 401 inside the chamber. Its telescopic end pushes the inclined push plate 402 to move (both ends of the push plate press against the inner wall of the can cover 303 and the filter can 301), pushing the activated carbon up and transferring it to the adjacent chamber. Repeat twice to make the activated carbon evenly distributed in the four chambers. Start the arc-shaped telescopic cylinder 5 on the mounting frame 201. Its telescopic end lifts the top plate 304 at the bottom of the filter tank 301, causing the filter tank 301 to rotate and shake once every 10 seconds under the support of the ball bearing 202 for 1 minute, thus leveling the surface of the activated carbon. Filter Unit 1: Gas Filtration After cooling, the exhaust gas passes through the bottom filter holes of the filter canister 301 from bottom to top, enters the chamber and comes into full contact with the evenly distributed activated carbon, adsorbing organic impurities (unreacted light hydrocarbons and alkyne residues) in the exhaust gas. Then the gas is discharged from the filter canister 301 through the filter holes of the canister cover 303. Filter Unit Two: Fine Gas Filtration The gas purified by the first filter unit continues to pass from bottom to top through the ceramic filter element 6 (pore size 0.1μm) of the second filter unit, trapping tiny carbon particles with a particle size of <50nm carried in the exhaust gas. After the exhaust gas is purified, the pressure inside the filter is monitored by the pressure detection device 103 and found to be 65 kPa. Before being discharged through the outlet 102, the oxygen content sensor detects that the oxygen content is 1.5% (≤2%), which meets the emission standard. If the oxygen content is >2%, the alarm module is triggered and the emission is suspended.
[0033] Step 8: Product Detection and Parameter Optimization The nano-graphite in the carbon product collection container was tested by X-ray diffraction (XRD) and found to have a purity of 99.2%, which meets the requirement of ≥99%. Scanning electron microscopy (SEM) revealed that the product particles were concentrated in the range of 80-180 nm and had a morphology of sheet-like nanographite. This method processes 1 m³ of high-grade alkyne tail gas to obtain 0.9 kg of nano-graphite, with a high-grade alkyne solidification rate of 42%. The application of the filtration unit ensures that the residual impurities in the tail gas are ≤0.01 mg / m³, and the filtration efficiency decay rate is only 4% after 72 hours of continuous operation, which greatly improves the process stability.
[0034] In step seven, the gas filter 1 is equipped with an air inlet 101, an air outlet 102, and a pressure detection device 103. Inside, from bottom to top, are filter unit one and filter unit two.
[0035] The filter unit includes multiple mounting brackets 201 and multiple filter canisters 301. The filter canisters 301 are located on the mounting brackets 201. A canister cover 303 is detachably connected to the top of the filter canisters 301. Filter holes are provided on both the filter canisters 301 and the canister cover 303. A cross-shaped partition plate 302 is installed inside the filter canisters 301. The partition plate 302 divides the filter canisters 301 into four chambers. The partition plate 302 is lower than the canister cover 303. Activated carbon is filled inside the filter canisters 301. The top of the activated carbon is lower than the partition plate 302. Filter unit two includes ceramic filter element 6.
[0036] Multiple sets of telescopic rods 401 are installed in the chamber of the filter tank 301. An inclined push plate 402 is fixedly connected to the telescopic end of the telescopic rod 401. The two ends of the push plate 402 abut against the tank cover 303 and the filter tank 301 respectively. By moving the push plate 402, the activated carbon in the chamber can be moved. The activated carbon is pushed up by the inclined push plate 402 and then enters other chambers.
[0037] Two sets of arc-shaped telescopic cylinders 5 are fixedly connected to the mounting frame 201. A top plate 304 is fixedly connected to the bottom of the filter tank 301. The telescopic ends of the arc-shaped telescopic cylinders 5 abut against the top plate 304. By extending the telescopic ends of the telescopic cylinders 5, the filter tank 301 can be rotated intermittently on the mounting frame 201, thereby generating vibration and making the activated carbon in the chamber relatively level.
[0038] Multiple sets of ball bearings 202 are rotatably connected to the mounting bracket 201, and the ball bearings 202 abut against the filter tank 301.
[0039] This invention achieves synergistic benefits in terms of environmental protection, quality, stability, and economy: it not only utilizes the high-grade alkyne tail gas produced as a byproduct of acetylene production from natural gas, solving the problems of tail gas waste and emission pollution (reducing CO2 emissions by 0.5-0.6 kg per m³ of tail gas treated), but also produces high-quality flake-shaped nano-graphite with a purity ≥99% and a particle size concentrated in the 50-200 nm range through molten medium catalysis, multi-stage temperature control, and secondary purification, achieving a high-grade alkyne solidification rate of 42%. Simultaneously, the heat-traced coated pipeline ensures stable raw material transport without polymerization blockage for 72 hours, while the dual-layer filtration unit with uniformly distributed activated carbon in multiple chambers and a ceramic filter element reduces residual impurities in the tail gas. This not only improves process continuity but also, due to its high degree of automation and convenient maintenance, is adaptable to direct scaling-up to industrial production lines, combining the dual economic value of tail gas treatment cost savings and nano-graphite product benefits.
[0040] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-described technical content to create equivalent embodiments without departing from the scope of the present invention. Any simple modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.
Claims
1. A novel method for preparing advanced acetylene nanographite, characterized in that, The main operating steps are as follows: Step 1: Pretreatment of raw gas conveying system Check the sealing of the heat tracing pipeline and the stainless steel mixing tank to ensure there are no leaks; Turn on the electric heat tracing device, set the temperature control range to 55-60℃, monitor the temperature of the pipeline and mixing tank in real time through the temperature probe, keep the temperature for 30 minutes until the temperature stabilizes within the set range. Step 2: Introducing, mixing, and stabilizing the raw material gas Open the high-grade alkyne inlet valve and introduce the high-grade alkyne tail gas, a byproduct of natural gas-to-acetylene production, into the mixing tank. Turn on the booster controller and argon gas inlet valve to introduce high-purity argon gas with a purity of ≥99.9%, and use the spiral airflow distributor in the mixing tank to mix the two gases evenly. Step 3: Catalytic medium loading and reactor preheating The selected catalytic medium is filled into the detachable porous media basket of the high-temperature alloy reactor; Turn on the temperature control system and electric heater, and raise the temperature according to the multi-stage heating program: from room temperature to 800℃, the heating rate is 5℃ / min; from 800 to 1100℃, the heating rate is 2℃ / min. After reaching the target reaction temperature, keep it at the temperature for 1 hour to ensure that the catalyst medium is completely melted. Step 4: Catalytic reaction and parameter control of feed gas Open the gas outlet valve of the mixing tank and introduce the pretreated mixed raw material gas into the reactor. The gas is then evenly dispersed onto the surface of the molten catalyst medium by the gas distributor at the top of the reactor. The pressure inside the reactor is maintained at 0.1-0.15 MPa by a pressure monitoring module. Higher alkynes undergo directional cracking under the action of molten catalytic medium, and carbon atoms rearrange in an orderly manner on the surface of the medium to generate nano-graphite. The reaction lasts for 2-4 hours. Step 5: Preliminary gas-solid separation The nano-graphite generated by the reaction enters the cyclone separator along with the gaseous products. The airflow speed is set to 15-20 m / s, and the nano-graphite with a particle size of 50-200 nm is thrown towards the inner wall of the separator by centrifugal force. Nanographite falls along the wall of the separator into the carbon product collection tank below, and the anti-vortex baffle installed at the top of the separator reduces the risk of gas entrainment of solid particles. Step Six: Cooling and Secondary Purification of Nano-Graphite Cooling water at 25-30℃ is introduced into the cooling jacket of the carbon product collection tank to cool the nano-graphite inside the tank to room temperature for 30 minutes. By using a detachable filter with a 20μm pore size at the bottom of the carbon product collection tank, trace impurities remaining in the nano-graphite are filtered out, further improving the purity of the product. Step 7: Exhaust gas filtration and emission compliance The gaseous products after initial separation by the cyclone separator are cooled until the temperature drops to 60-80℃, and then enter the gas filter (1). The oxygen content of the gas is monitored by an oxygen content sensor at the filter outlet to ensure that the oxygen content is ≤2%. Once the standard is met, the gas is discharged through the exhaust outlet. If the oxygen content is >2%, the alarm module is triggered and the emission is suspended. Step 8: Product Detection and Parameter Optimization Disassemble the bottom filter screen of the carbon product collection tank, collect the nano-graphite product, and use X-ray diffraction to detect the purity, which must be ≥99%. Observe the morphology and particle size using scanning electron microscopy, which must be 50-200 nm.
2. The novel method for preparing advanced ytylene nanographite according to claim 1, characterized in that, The heat tracing pipeline in step one is made of DN50 carbon steel with a polytetrafluoroethylene coating on the inner wall.
3. The method for preparing novel advanced ytylene nanographite according to claim 1, characterized in that, In step two, the initial flow rate of the high alkyne tail gas entering the mixing tank is 200 mL / min, and the pressure inside the tank is monitored in real time by a pressure gauge. The pressure booster controller automatically adjusts the argon gas intake: when the pressure is <80kPa, argon gas is added; when the pressure is >120kPa, the pressure relief valve is opened, and the pressure inside the tank is finally stabilized at 80-120kPa. The mixing time lasts for 10 minutes.
4. The novel method for preparing advanced acetylene nanographite according to claim 1, characterized in that, The porous media basket in step three has a pore size of 50-100μm and is installed in the catalytic media chamber at the bottom of the high-temperature alloy reactor. Furthermore, the catalytic medium in step three is a mixture of copper-bismuth alloy and Cu-Bi at a ratio of 90:10, or a mixture of Fe2O3 and the basic composite medium Fe2O3-Al2O3 at a ratio of 85:
15.
5. The novel method for preparing advanced ytylene nanographite according to claim 1, characterized in that, The gaseous products generated in step five are hydrogen, argon, and unreacted light hydrocarbons.
6. The novel method for preparing advanced acetylene nanographite according to claim 1, characterized in that, The gas filter (1) in step seven is equipped with an air inlet (101), an air outlet (102), and a pressure detection device (103). Inside, from bottom to top, are filter unit one and filter unit two.
7. The method for preparing novel advanced acetylene nanographite according to claim 6, characterized in that, The filter unit includes multiple sets of mounting brackets (201) and multiple sets of filter canisters (301). The filter canisters (301) are located on the mounting brackets (201). A canister cover (303) is detachably connected to the top of the filter canisters (301). Filter holes are provided on both the filter canisters (301) and the canister cover (303). A cross-shaped partition plate (302) is installed inside the filter canisters (301). The partition plate (302) divides the filter canisters (301) into four chambers, and the partition plate (302) is lower than the canister cover (303). The filter canisters (301) are filled with activated carbon, and the top of the activated carbon is lower than the partition plate (302). The second filtration unit includes a ceramic filter element (6).
8. A novel method for preparing advanced acetylene nanographite according to claim 7, characterized in that, Multiple sets of telescopic rods (401) are installed in the chamber of the filter tank (301). An inclined push plate (402) is fixedly connected to the telescopic end of the telescopic rod (401). The two ends of the push plate (402) abut against the tank cover (303) and the filter tank (301) respectively. The activated carbon in the chamber can be moved by the movement of the push plate (402). The activated carbon is pushed up by the inclined push plate (402) and then enters other chambers.
9. A novel method for preparing advanced acetylene nanographite according to claim 8, characterized in that, Two sets of arc-shaped telescopic cylinders (5) are fixedly connected to the mounting frame (201). A top plate (304) is fixedly connected to the bottom of the filter tank (301). The telescopic end of the arc-shaped telescopic cylinder (5) abuts against the top plate (304). By extending the telescopic end of the telescopic cylinder (5), the filter tank (301) can be rotated intermittently on the mounting frame (201), thereby generating vibration and making the activated carbon in the chamber relatively level.
10. A novel method for preparing advanced acetylene nanographite according to claim 9, characterized in that, Multiple sets of ball bearings (202) are rotatably connected to the mounting bracket (201), and the ball bearings (202) abut against the filter tank (301).