Device and method for preparing graphite samples by multiple systems by means of mixed combustion of biomass and coal
By integrating a multi-system biomass and coal-combusted graphite sample device, the complex and time-consuming problem of graphite preparation in the prior art is solved, and an efficient and convenient graphite preparation process is achieved, which promotes high-precision detection of biomass blending ratio measurement.
Patent Information
- Application Number
- PCT/CN2025/084728
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-05-31
- Filing Date
- 2025-03-25
- Publication Date
- 2025-08-21
AI Technical Summary
The existing graphite preparation system can only be prepared by biomass or coal alone, or the gas mixed with biomass and coal is collected and converted into SrCO3 samples before preparation. The process is complex and time-consuming and labor-intensive, and cannot meet the requirements of high-precision biomass blending ratio measurement.
A multi-system biomass and coal mixed combustion device is designed to make graphite samples, including adapter components, flue gas filters, miscellaneous gas suction components, transfer components and as-is oxidation components. Through the integration of these components, graphite carbon preparation can be carried out for three different sources of raw material samples, simplifying the operation process.
It realizes the convenience and speed of graphite preparation process, improves the preparation efficiency and purity, promotes the application of AMS-based 14C detection method in biomass blending ratio determination, and meets the wide application of biomass and coal mixing technology in power generation power plants.
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Figure CN2025084728_21082025_PF_FP_ABST
Abstract
Description
Device and method for producing graphite samples by co-firing multi-system biomass and coal Technical Field
[0001] The present invention relates to the technical field of coupled combustion of coal and biomass, in particular to a device and method for producing graphite samples by mixed combustion of multi-system biomass and coal. Background Art
[0002] Co-combustion of biomass and coal not only improves biomass resource utilization but also mitigates the environmental impact of coal combustion, achieving emission reductions that meet carbon trading market requirements. However, the widespread application of biomass-coal co-combustion technology in power plants requires high-precision measurement of the biomass blending ratio. To avoid the potential for biased weighing during input-side measurement, the 14C content in the flue gas from the co-combustion output is typically measured to determine the biomass-to-coal ratio in the input feedstock. Carbon exists in nature in three isotopes: 13C, 12C, and 14C. 14C is a radioactive carbon isotope with an abundance of approximately 1.18×10-10% and a half-life of approximately 5730±40 years. Fossil fuels decay over hundreds of millions of years, and their 14C content approaches zero. Biomass, however, undergoes a continuous carbon cycle with the atmosphere, and its 14C content remains essentially the same. Therefore, given the difference in 14C content between biomass fuels and fossil fuels, the 14C content of flue gas emitted by power plants can be used to analyze the biomass fuel blending ratio. Currently, the output-side measurement method mainly uses the 14C detection method. Among them, the 14C detection method based on accelerator mass spectrometry (AMS) can more accurately and quickly determine the 14C content to obtain the biomass blending ratio. However, detection using an AMS instrument requires the original sample to be converted into graphite carbon. Current graphite preparation systems can only produce CO2 from biomass or coal alone, or collect and convert the gas from the co-combustion of biomass and coal into SrCO3 samples before using the graphite preparation system to produce graphite. The experimental process is complex and time-consuming and labor-intensive. Therefore, a multi-system device for producing graphite samples by co-firing biomass and coal is designed. Using this device and the corresponding method, corresponding graphite carbon preparation operations can be performed on raw material samples from three different sources, making the graphite preparation process more convenient and faster, promoting the AMS-based 14C detection method to be more widely used in biomass blending ratio determination, and making biomass and coal co-firing technology more widely used in power plants to adjust the energy utilization structure and meet the "dual carbon" development concept. Summary of the Invention
[0003] In view of the problems existing in the above-mentioned multi-system biomass and coal co-combustion graphite sample device and method, the present invention is proposed.
[0004] Therefore, the problem to be solved by the present invention is how to integrate multiple systems to prepare graphite carbon and improve the preparation purity.
[0005] To solve the above technical problems, the present invention provides the following technical solutions: a multi-system biomass and coal co-combustion device for producing graphite samples, comprising a switching assembly for cooling the high-temperature combustion flue gas;
[0006] a flue gas filter, connected to the adapter assembly, for filtering particulate impurities in the combustion flue gas;
[0007] A miscellaneous gas removal component is connected to the flue gas filter through a glass tube and is used to remove miscellaneous gases in the combustion flue gas;
[0008] a transfer assembly, connected to both ends of the glass tube, for removing water vapor and impurities from the combustion flue gas;
[0009] The original oxidation component is connected to the glass tube and is used for the separate reaction of biomass or coal to produce carbon dioxide.
[0010] As a preferred embodiment of the multi-system biomass and coal co-combustion device for producing graphite samples of the present invention, the device comprises: an oxygen cylinder;
[0011] a tubular furnace, used to provide heat for the combustion reaction, wherein the low temperature zone of the tubular furnace is in communication with the oxygen cylinder;
[0012] a vacuum pump in communication with the transfer assembly;
[0013] The adapter assembly includes an adapter connected to the high-temperature zone of the tube furnace and a conical flask sleeved on the adapter, and the conical flask is placed in the water tank.
[0014] As a preferred solution of the multi-system biomass and coal co-combustion device for producing graphite samples according to the present invention, the impurity gas removal component includes a first serpentine tube connected to the flue gas filter through the glass tube and a gas washing bottle.
[0015] As a preferred embodiment of the multi-system biomass and coal co-combustion device for producing graphite samples described in the present invention, the transfer assembly includes a second serpentine tube connected to the glass tube, a vacuum gauge connected to the second serpentine tube, and a graphitization part connected to the vacuum gauge. The graphitization part includes a reaction tube connected to the glass tube, and the reaction tube is also provided with an outer tube. The interface in the transfer assembly and the interface in the first serpentine tube all adopt vertically connected ball milling mouths, and the ball milling ball mouths are also provided with a spherical interface clamp for fixing the connection end.
[0016] As a preferred solution of the multi-system biomass and coal co-combustion device for producing graphite samples described in the present invention, the original oxidation component includes a vacuum baffle valve connected to the glass tube, a first bellows and a quartz tube, and the vacuum baffle valve, the first bellows and the quartz tube are connected in sequence.
[0017] As a preferred embodiment of the multi-system device for producing graphite samples by co-firing biomass and coal according to the present invention, a first valve is provided at the connection between the other end of the flue gas filter and the glass tube, a second valve and a third valve are provided at the input end of the glass tube, a fourth valve and a fifth valve are provided at the output end of the glass tube, a sixth valve and a seventh valve are provided at the connection between the two sides of the vacuum gauge and the pipeline respectively, an eighth valve is provided at the connection between the glass tube and the vacuum baffle valve, and a ninth valve is provided at the connection between the graphitized part and the second bellows.
[0018] Another object of the present invention is to provide a method for producing graphite samples by co-firing multi-system biomass and coal, which is applied to the above-mentioned portable current transformer polarity and ratio test device, and the method comprises:
[0019] Producing carbon dioxide from biomass or coal alone to make graphite carbon through a first subsystem;
[0020] Co-combustion of biomass and coal to produce carbon dioxide to make graphite carbon through the second subsystem;
[0021] The biological clock is mixed with coal through the third subsystem to produce carbon monoxide to make graphite carbon.
[0022] As a preferred embodiment of the multi-system method for producing graphite samples by co-firing biomass and coal according to the present invention, the first subsystem is composed of an original sample oxidation component, a transfer component, and a vacuum pump, and the three components are connected in sequence;
[0023] The second subsystem is composed of an oxygen cylinder, a tubular furnace, a transfer assembly, a flue gas filter, the transfer assembly, and the vacuum pump, and all of them are connected in sequence;
[0024] The third subsystem is composed of the oxygen cylinder, the tubular furnace, the adapter assembly, the flue gas filter, the impurity suction assembly, the transfer assembly and the vacuum pump, and all of them are connected in sequence.
[0025] As a preferred embodiment of the multi-system method for producing graphite samples by co-combustion of biomass and coal according to the present invention, the preparation method of the first subsystem includes: closing the third valve and the fourth valve, mixing the biomass or coal raw material with copper oxide and placing it in a quartz tube, opening the remaining valves and starting the vacuum pump, and then sealing the quartz tube with a torch. After reacting the quartz tube at different temperatures in a muffle furnace, the generated carbon dioxide is then connected to the transfer assembly;
[0026] After placing zinc and titanium hydride in the outer tube and iron in the interior of the reaction tube, evacuating the reaction tube by the vacuum pump, closing the sixth valve, and releasing the carbon dioxide in the quartz tube;
[0027] Controlling the transfer of carbon dioxide into the interior of the reaction tube, placing the reaction tube in a muffle furnace for reaction, and finally producing a graphite carbon sample;
[0028] The preparation method using the second subsystem includes: closing the eighth valve, the second valve, and the fifth valve, placing zinc and titanium hydride in the outer tube, placing iron in the interior of the reaction tube, placing a mixed raw material of biomass and coal in the low-temperature zone of the tube furnace, evacuating the tube furnace using the vacuum pump, starting to increase the temperature of the tube furnace, introducing oxygen and closing the sixth valve, then continuing to increase the temperature, cooling the combustion flue gas through the adapter assembly and then passing it through a flue gas filter to remove particles;
[0029] After the combustion is completed, the third valve and the seventh valve are closed, and the sixth valve is opened. After the transfer of carbon dioxide to the interior of the reaction tube is controlled by a liquid nitrogen cold trap, the reaction tube is reacted in a muffle furnace to finally obtain a graphite carbon sample.
[0030] As a preferred embodiment of the multi-system method for producing graphite samples by co-combustion of biomass and coal according to the present invention, the preparation method using the third subsystem includes: closing the third valve and the fifth valve, placing zinc and titanium hydride in the outer tube, placing iron inside the reaction tube, placing the biomass and coal mixed raw material into the low-temperature zone of the tubular furnace, evacuating the mixture using the vacuum pump, starting to increase the temperature of the vacuum pump, introducing oxygen, and closing the ninth valve, and cooling the flue gas generated by the combustion through the transfer device and then passing it through the flue gas filter to remove particles;
[0031] Then, the mixture was passed into a gas washing bottle containing sodium hydroxide and pyrogallic acid solution respectively to remove impurities, and the carbon dioxide was transferred to the reaction tube and placed in a muffle furnace for reaction, thereby finally obtaining a graphite carbon sample.
[0032] The beneficial effects of the present invention are: through the coordination of various components, the three subsystems can be integrated and assembled, which can greatly reduce the preparation cost and preparation efficiency. At the same time, corresponding graphite carbon preparation operations can be performed for raw material samples from three different sources, making graphite preparation more convenient and faster. BRIEF DESCRIPTION OF THE DRAWINGS
[0033] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be derived from these drawings without inventive effort. Among them:
[0034] FIG1 is a structural diagram of a device and method for producing graphite samples by co-firing multi-system biomass and coal.
[0035] FIG2 is a diagram showing valve positions of a multi-system apparatus and method for producing graphite samples by co-firing biomass and coal. DETAILED DESCRIPTION
[0036] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below with reference to the accompanying drawings.
[0037] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.
[0038] Secondly, the term "one embodiment" or "embodiment" herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The phrase "in one embodiment" appearing in various places throughout this specification does not necessarily refer to the same embodiment, nor does it individually or selectively refer to an embodiment that is mutually exclusive of other embodiments.
[0039] Example 1
[0040] 1 and 2 , which are the first embodiment of the present invention, provide a device and method for producing graphite samples by co-firing multi-system biomass and coal. The device and method for producing graphite samples by co-firing multi-system biomass and coal include a transfer assembly 300, a flue gas filter 400, a foreign gas removal assembly 500, a transfer assembly 600, and an original oxidation assembly 700.
[0041] Specifically, the oxygen cylinder 100 is used to provide oxygen for the combustion reaction.
[0042] Preferably, the tubular furnace 200 is used to provide heat for the combustion reaction, and the low temperature zone of the tubular furnace 200 is connected to the oxygen cylinder 100. The tubular furnace 200 can adopt the MHY-29908 model, and the oxygen cylinder 100 and the tubular furnace 200 are connected through a copper tube.
[0043] Preferably, the adapter assembly 300 is connected to the high-temperature zone of the tube furnace 200 and is used to cool the combustion flue gas to avoid damage to subsequent components. The adapter assembly 300 includes an adapter 301 connected to the tube furnace 200 and a conical flask 302 sleeved on the adapter 301. The conical flask 302 is placed in a water tank 303, and cooling water is stored in the water tank 303.
[0044] Preferably, the flue gas filter 400 is connected to the adapter assembly 300 and is used to filter particulate impurities in the combustion flue gas to improve the purity of CO2 / CO transferred to the reaction tube 603a. The flue gas filter 400 can be a RUNSHENG304 model.
[0045] Preferably, the impurity gas removal component 500 is connected to the flue gas filter 400 through a glass tube 501, and is used to remove impurities in the combustion flue gas and improve the purity of CO transferred to the reaction tube 603a. The impurity gas removal component 500 includes a first serpentine tube 502 connected to the flue gas filter 400 through a glass tube 501 and a washing bottle 503. There are two washing bottles 503, each of which is filled with sodium hydroxide solution and pyrogallic acid solution for the reaction of the third subsystem, and is used to remove NO2, SO2, CO2, and O2 gases.
[0046] Preferably, the transfer assembly 600 is connected to both ends of the glass tube 501 and is used to remove water vapor and impurities in the combustion flue gas to obtain pure CO2 and transfer it to the reaction tube. The transfer assembly 600 includes a second serpentine tube 601 connected to the glass tube 501, a vacuum gauge 602 connected to the second serpentine tube 601, and a graphitized component 603 connected to the vacuum gauge 602. The graphitized component 603 includes a reaction tube 603a connected to the glass tube 501, and the reaction tube 603a is also provided with an outer tube 603. 03b. The interfaces within the transfer assembly 600 and the interfaces within the first serpentine tube 502 all utilize vertically connected ball mill ports A, and a spherical interface clamp H is also provided on the ball mill port A to fix the connection end. The second serpentine tube 601 is divided into two sections, one for removing water vapor and the other for storing fixed carbon dioxide. The connection between the vacuum gauge 602 and the flow pipe is a vacuum gauge tube and a clamp. The ball mill port A utilizes gravity to press the interfaces tightly together, avoiding the leakage that is prone to occur with the original horizontal connection.
[0047] Preferably, the original oxidation component 700 is connected to the glass tube 501 and is used for the biomass or coal to react separately to produce carbon dioxide. The original oxidation component 700 includes a vacuum baffle valve 701, a first bellows 702 and a quartz tube 703 connected to the glass tube 501. The vacuum baffle valve 701, the first bellows 702 and the quartz tube 703 are connected in sequence.
[0048] Preferably, the vacuum pump 800 is connected to the transfer assembly 600 and is used to evacuate the closed system to avoid the influence of carbon dioxide in the air.
[0049] A first valve 401 is provided at the connection between the other end of the flue gas filter 400 and the glass tube 501, a second and sixth valve 602a01a and a third valve 501b are provided at the input end of the glass tube 501, a fourth and sixth valve 602a01c and a fifth and sixth valve 602a01d are provided at the output end of the glass tube 501, a sixth valve 602a and a seventh valve 602b are provided at the connection between the two sides of the vacuum gauge 602 and the pipeline respectively, an eighth valve 701a is provided at the connection between the glass tube 501 and the vacuum baffle valve 701, and a ninth valve 801a is provided at the connection between the graphitized part 603 and the second bellows 801.
[0050] Example 2
[0051] 1 and 2 , a second embodiment of the present invention is shown, which is based on the previous embodiment.
[0052] Specifically, it also includes: In the above embodiment, the multi-system method for producing graphite samples by co-firing biomass and coal includes using a first subsystem to produce carbon dioxide from biomass or coal alone to produce graphite carbon;
[0053] The second subsystem is used to produce graphite carbon by co-combusting biomass and coal to produce carbon dioxide;
[0054] The biological clock is mixed with coal through the third subsystem to produce carbon monoxide and make graphite carbon.
[0055] First, for the first subsystem, carbon dioxide is produced from biomass or coal alone to produce graphite carbon. Close the third valve 501b and the fourth valve 501c. Mix 2-3 mg of carbon-containing biomass or coal with 70-80 mg of CuO and place them in the quartz tube 703 of the original oxidation assembly 700. Open the remaining valves and start the vacuum pump 800 to evacuate the system to 10-2 Pa. Then, seal the quartz tube 703 with a flame gun. The sealed quartz tube 703 section is then placed in a muffle furnace for reaction at 500°C for 1 hour and 900°C for 4 hours before being reconnected to the original oxidation assembly 700. 30-35 mg of Zn and 10-15 mg of TiH2 are placed in the outer tube 603b, and 3-5 mg of Fe is placed in the reaction tube 603a. Since the entire device will be exposed to air when the quartz tube 703 is reconnected, the system must be evacuated to 10-2 Pa using the vacuum pump 800 again. Close the sixth valve 602a, break the quartz tube 703 from the first bellows 702 to release the CO2, and place a liquid nitrogen cold trap on the second section of the coiled tube 601 to secure the CO2 there. Close the eighth and seventh valves 701a and 602b, then open the sixth valve 602a. Place a liquid nitrogen cold trap on the tube between the sixth and seventh valves 602a and 602b to transfer the CO2 there. Place a -76°C alcohol cold trap on the second coiled tube 601 to remove moisture. After one minute, wait for the vacuum gauge 602 to read zero, then open and quickly close the seventh valve 602b to remove any impurities. Close the sixth valve 602a, remove the liquid nitrogen cold trap, and quantify the CO2 using a vacuum gauge. Close the ninth valve 801a, open the seventh valve 602b, and place a liquid nitrogen cold trap on the graphitized part 603 to fix CO2 into the reaction tube 603a. Then, seal the reaction tube 603a with a flame gun and place it in a muffle furnace to react at 500°C for 3 hours and 600°C for 4 hours to obtain a graphite carbon sample.
[0056] For the second subsystem: implementing the CO2 production and graphite production operation by co-combusting biomass and coal, close the eighth valve 701a, the second valve 501a, and the fourth valve 501c. Place 30-35 mg of Zn and 10-15 mg of TiH2 in the outer tube 603b of the graphitization device, and 3-5 mg of Fe in the reaction tube 603a. Place a crucible containing 1 gram of the biomass and coal mixture in the low-temperature zone of the two-stage tubular furnace 200. Use vacuum pump 800 to evacuate the system to 10-2 Pa, and begin the tubular furnace program. The low-temperature zone and the high-temperature zone were first raised to 120°C and 250°C respectively at the same time. At this time, 50 mL·min-1 of O2 was introduced. The low-temperature zone and the high-temperature zone were then raised to 250°C and 400°C respectively at the same time. Then, they were raised to 400°C and 650°C respectively at the same time. Finally, the low-temperature zone was raised to 850°C in 35 minutes and maintained for 30 minutes. The high-temperature zone was raised to 850°C in 20 minutes and maintained for 45 minutes. When O2 is initially introduced, the sixth valve 602a is closed. The flue gas generated by the combustion is cooled by the transfer device and first passes through the flue gas filter 400 to remove particulates. It then passes through the first section of the second serpentine tube 601, which is fitted with a -76°C alcohol cold trap, to remove moisture. The flue gas is then secured to the second section of the second serpentine tube 601, which is fitted with a liquid nitrogen cold trap. After the combustion is complete, the third valve 501b and the seventh valve 602b are closed. The sixth valve 602a is opened, and a liquid nitrogen cold trap is placed on the tube between the sixth and seventh valves 602a, 602b, to transfer the CO2 there. After one minute, when the vacuum gauge reading drops to 0, the seventh valve 602b is opened and quickly closed to remove impurities. The sixth valve 602a is closed, the liquid nitrogen cold trap is removed, and the CO2 is qualitatively measured using a vacuum gauge. Close the ninth valve 801a, open the seventh valve 602b and put a liquid nitrogen cold trap on the graphitized part 603 to fix CO2 into the reaction tube, then seal the reaction tube with a flame gun and place it in a muffle furnace to react at 500℃ for 3h and 600℃ for 4h to obtain a graphite carbon sample.
[0057] It is worth noting that in common operations, the CO2 generated by combustion in a tubular furnace needs to be collected with an air bag first, and then passed into a washing bottle filled with NaOH for absorption, and then NH4Cl solution is added to adjust the pH value to about 10, and then a saturated SrCl2 solution is poured in. After filtration, it is dried for 10 hours to obtain a SrCO3 sample. SrCO3 and HCl can react in a liquid CO2 production device that replaces the original oxidation component 700 to release CO2, and the graphite is finally obtained by operating according to the steps of the above-mentioned CO2 transfer graphitization device.
[0058] The use of subsystem 2 can eliminate the above-mentioned complex CO2 conversion and release steps, saving at least 12 hours of time and greatly improving efficiency. At the same time, since external gases are easily mixed when adjusting the pH value, the quality of the final generated samples is uneven. We do not need these steps. All of them are sealed by flame guns and the overall process is integrated, so the overall sealing is well guaranteed.
[0059] For the third subsystem: To implement the CO production and graphite production operation of biomass and coal co-combustion, close third valve 501b and fifth valve 501d. Place 30-35 mg of Zn and 10-15 mg of TiH2 in the outer tube of the reaction tube group in the graphitization device, and 3-5 mg of Fe in reaction tube 603a. Place a crucible containing 1 g of the biomass and coal mixture in the low-temperature zone of the two-stage tubular furnace 200. Use a vacuum pump to evacuate the system to 10-2 Pa, and begin the tubular furnace program. This program is identical to the tubular furnace program in the second subsystem. When O2 begins to be introduced, the ninth valve 801a is closed. The flue gas generated by the combustion is cooled by the adapter and first passes through a flue gas filter to remove particles. Then, water vapor is removed by passing through a serpentine tube covered with a -76°C alcohol cold trap. Then, NO2, SO2, CO2, and O2 gases are removed by passing through a gas washing bottle 503 containing 0.7L of 1.25mol·L-1 NaOH and 0.30L of 1.25mol·L-1 pyrogallic acid solution, respectively. CO is transferred to the reaction tube 603a. After the combustion is completed, the tube is sealed and placed in a muffle furnace for reaction at 600°C for 4 hours to produce a graphite carbon sample.
[0060] By adding the third subsystem, high-precision 14C sampling of the gaseous carbon source that has not been completely burned in the flue gas can be performed, and a corresponding calculation model can be established to reduce the error in the blending ratio calculation and improve the accuracy of the biomass blending ratio determination.
[0061] It is worth noting that all the above weights are experimental data and are not limited to this data. The time saved mentioned by us is also variable, but compared with the existing technology, the time can be greatly saved.
[0062] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention may be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, which should all be included in the scope of the claims of the present invention.
Claims
1. A multi-system biomass and coal co-combustion device for producing graphite samples, characterized by: include, The adapter assembly (300) is used to cool the high-temperature combustion flue gas; a flue gas filter (400), connected to the adapter assembly (300), for filtering particulate impurities in the combustion flue gas; A stray gas removal component (500) is connected to the flue gas filter (400) through a glass tube (501) and is used to remove stray gases in the combustion flue gas; A transfer assembly (600) is connected to both ends of the glass tube (501) and is used to remove water vapor and impurities in the combustion flue gas; The original oxidation assembly (700) is connected to the glass tube (501) and is used for the biomass or coal to react alone to produce carbon dioxide.
2. The multi-system biomass and coal co-combustion device for producing graphite samples according to claim 1, characterized in that: including an oxygen cylinder (100); The adapter assembly (300) includes an adapter (301) connected to the high-temperature zone of the tube furnace (200), and a conical flask (302) sleeved on the adapter (301). The conical flask (302) is placed in a water tank (303). The low-temperature zone of the tube furnace (200) is connected to the oxygen cylinder (100).
3. The multi-system biomass and coal co-combustion graphite sample production device according to claim 2, characterized in that: The impurity gas removal component (500) comprises a first serpentine tube (502) connected to the smoke filter (400) through the glass tube (501) and a gas washing bottle (503).
4. The multi-system biomass and coal co-combustion device for producing graphite samples as claimed in claim 3, characterized in that: The transfer assembly (600) includes a second serpentine tube (601) connected to the glass tube (501), a vacuum gauge (602) connected to the second serpentine tube (601), and a graphitized component (603) connected to the vacuum gauge (602). The graphitized component (603) includes a reaction tube (603a) connected to the glass tube (501). The reaction tube (603a) is further provided with an outer tube (603b). The interface in the transfer assembly (600) and the interface in the first serpentine tube (502) all adopt vertically connected ball milling ports (A), and the ball milling port (A) is further provided with a spherical interface clamp (H) for fixing the connection end. The reaction tube (603a) is finally connected to a vacuum pump (800).
5. The multi-system biomass and coal co-combustion device for producing graphite samples according to claim 4, characterized in that: The original oxidation assembly (700) includes a vacuum baffle valve (701) connected to the glass tube (501), a first bellows (702) and a quartz tube (703), and the vacuum baffle valve (701), the first bellows (702) and the quartz tube (703) are connected in sequence.
6. The multi-system biomass and coal co-combustion device for producing graphite samples according to claim 5, characterized in that: A first valve (401) is provided at the connection point between the other end of the flue gas filter (400) and the glass tube (501); a second valve (501a) and a third valve (501b) are provided at the input end of the glass tube (501); a fourth valve (501c) and a fifth valve (501d) are provided at the output end of the glass tube (501); a sixth valve (602a) and a seventh valve (602b) are provided at the connection points between the two sides of the vacuum gauge (602) and the pipeline respectively; an eighth valve (701a) is provided at the connection point between the glass tube (501) and the vacuum baffle valve (701); a ninth valve (801a) is provided at the connection point between the graphitized part (603) and the second bellows (801); and the second bellows (801) is connected to the vacuum pump (800) and the reaction tube (603a).
7. A method for producing graphite samples by co-firing biomass and coal in multiple systems, characterized by: The method is applied to the device for producing graphite samples by co-firing multi-system biomass and coal as claimed in any one of claims 1 to 6, wherein the method comprises: Producing carbon dioxide from biomass or coal alone to make graphite carbon through a first subsystem; Co-combustion of biomass and coal to produce carbon dioxide to make graphite carbon through the second subsystem; The biological clock is mixed with coal through the third subsystem to produce carbon monoxide to make graphite carbon.
8. The method for producing graphite samples by co-firing multi-system biomass and coal as claimed in claim 7, characterized in that: The first subsystem is composed of an original oxidation component (700), a transfer component (600) and a vacuum pump (800), and the three are connected in sequence; The second subsystem is composed of an oxygen cylinder (100), a tubular furnace (200), a switching assembly (300), a flue gas filter (400), the transfer assembly (600), and the vacuum pump (800), and all of them are connected in sequence; The third subsystem is composed of the oxygen cylinder (100), the tubular furnace (200), the adapter assembly (300), the fume filter (400), the impurity suction assembly (500), the transfer assembly (600) and the vacuum pump (800), and all of them are connected in sequence.
9. The method for producing graphite samples by co-firing multi-system biomass and coal as claimed in claim 8, characterized in that: The preparation method of the first subsystem includes: closing the third valve (501b) and the fourth valve (501c), taking biomass or coal raw materials and copper oxide and mixing them into a quartz tube (703), opening the remaining valves and starting the vacuum pump (800), and then sealing the quartz tube (703) with a torch, and reacting the quartz tube (703) at different temperatures in a muffle furnace to generate carbon dioxide, which is then connected to the transfer component (600); After zinc and titanium hydride are placed in the outer tube (603b) and iron is placed inside the reaction tube (603a), vacuum is evacuated by the vacuum pump (800), the sixth valve (602a) is closed, and the carbon dioxide in the quartz tube (703) is released; Controlling the transfer of carbon dioxide into the interior of the reaction tube (603a), placing the reaction tube (603a) in a muffle furnace for reaction, and finally obtaining a graphite carbon sample; The preparation method through the second subsystem includes: closing the eighth valve (701a), the second valve (501a) and the fifth valve (501d), placing zinc and titanium hydride in the outer tube (603b), placing iron inside the reaction tube (603a), placing the biomass and coal mixed raw material into the low temperature zone of the tube furnace (200), performing vacuuming by the vacuum pump (800), starting to increase the temperature of the tube furnace (200), introducing oxygen and closing the sixth valve (602a), then continuing to increase the temperature, and the combustion flue gas passes through the adapter component (300) to cool down and then passes through the flue gas filter (400) to remove particles; After the combustion is completed, the third valve (501b) and the seventh valve (602b) are closed, and the sixth valve (602a) is opened. After the transfer of carbon dioxide to the interior of the reaction tube (603a) is controlled by a liquid nitrogen cold trap, the reaction tube (603a) reacts in a muffle furnace to finally obtain a graphite carbon sample.
10. The method for producing graphite samples by co-firing multi-system biomass and coal as claimed in claim 9, characterized in that: The preparation method through the third subsystem includes: closing the third valve (501b) and the fifth valve (501d), placing zinc and titanium hydride in the outer tube (603b), placing iron inside the reaction tube (603a), placing the biomass and coal mixed raw material into the low temperature zone of the tube furnace (200), performing vacuuming by the vacuum pump (800), starting to increase the temperature of the vacuum pump (800), introducing oxygen and closing the ninth valve (801a), and cooling the flue gas generated by the combustion through the transfer device and then passing through the flue gas filter (400) to remove particles; Then, the mixture is passed into a gas washing bottle containing sodium hydroxide and pyrogallic acid solution respectively to remove impurities, and the carbon dioxide is transferred to the reaction tube (603a) and placed in a muffle furnace for reaction, and finally a graphite carbon sample is obtained.
Citation Information
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