Device and method for preparing graphite sample by co-combustion of multi-system biomass and coal

By designing a multi-system biomass and coal mixed combustion device to make graphite samples, and using multiple subsystems to carry out separate reactions and mixing reactions of biomass or coal, the complex and time-consuming problems of the existing graphite preparation system are solved, and high-purity graphite sample preparation and convenient and rapid preparation process are realized.

CN118624330BActive Publication Date: 2025-05-13CHANGZHOU UNIV
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Patent Information

Application Number
CN202410701916.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-05-31
Publication Date
2025-05-13
Estimated Expiration
2044-05-31

AI Technical Summary

Technical Problem

The existing graphite preparation system can only perform graphite production by biomass or coal alone, or collect and convert the gas mixed with biomass and coal into SrCO3 samples and then use the graphite preparation system to perform graphite production. The process is complex and time-consuming.

Method used

A multi-system biomass and coal mixed combustion to make graphite samples is designed, including adapter components, flue gas filters, miscellaneous gas suction components, transfer components and as-is oxidation components. Through three subsystems, a separate reaction of biomass or coal and a mixed combustion reaction of biomass and coal is carried out to prepare high-purity graphite samples.

Benefits of technology

It has achieved convenient and rapid preparation of samples from three different sources, significantly reduced the preparation cost and time, promoted the application of AMS-based 14C detection method, and promoted the wide application of biomass and coal mixed combustion technology in power plants.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a device and method for preparing graphite samples by co-combustion of multi-system biomass and coal, and relates to the field of coupled combustion of coal and biomass. The device and method for preparing graphite samples by co-combustion of multi-system biomass and coal include an oxygen cylinder, a tubular furnace, a switching assembly, a flue gas filter, a foreign gas absorption assembly, a transfer assembly, an original oxidation assembly and a vacuum pump. The oxygen cylinder is used to provide oxygen for the combustion reaction; the tubular furnace is used to provide heat for the combustion reaction; the switching assembly is used to cool the combustion flue gas; the flue gas filter is used to filter particulate impurities in the combustion flue gas; the foreign gas absorption assembly is used to remove foreign gas in the combustion flue gas; and the transfer assembly is used to remove water vapor and foreign gas in the combustion flue gas. The invention performs corresponding graphite sample preparation operations on raw material samples from three different sources, so that the graphite preparation process is more convenient and faster, and promotes the AMS-based 14C detection method to be more widely used in biomass blending ratio determination.
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Description

Technical Field

[0001] The invention relates to the technical field of coupled combustion of coal and biomass, in particular to a device and method for preparing graphite samples by mixed combustion of multi-system biomass and coal. Background Art

[0002] The coupled combustion of biomass and coal can not only improve the utilization rate of biomass resources, but also alleviate the environmental pollution caused by coal burning, achieving emission reduction effects to meet the market requirements of carbon trading. The widespread application of biomass and coal co-combustion technology in power plants requires high-precision measurement of the biomass blending ratio. In order to avoid the lack of fairness caused by artificial weighing factors in input-side detection, it is generally adopted to detect the coupled combustion flue gas from the output side. 14 The method of calculating the C content is used to obtain the ratio of biomass to coal in the input raw materials. Carbon exists in three isotopes in nature, namely 13 C, 12 C, 14 C, where 14 C is a radioactive carbon isotope with an abundance of about 1.18×10 -10 %, and a half-life of about 5730±40 years. Fossil fuels decay over hundreds of millions of years. 14 C content tends to zero; biomass continuously cycles carbon with the atmosphere. 14 The 14C content of biomass fuels is basically the same as that of the atmosphere. Therefore, given the difference in 14C content between biomass fuels and fossil fuels, the 14 C content to analyze the blending ratio of biomass fuel. 14 C detection method, including accelerator mass spectrometry (AMS) based 14 C detection method can be carried out more accurately and rapidly 14 The C content is determined to obtain the blending ratio of biomass, and the AMS instrument needs to make the original sample into a graphite sample before testing. The current graphite preparation system can only produce CO2 from biomass or coal alone to make graphite, or collect the gas from the co-combustion of biomass and coal and convert it into SrCO3 samples before using the graphite preparation system to make graphite. The experimental process is complicated and time-consuming and labor-intensive. Therefore, a multi-system device for preparing graphite samples by co-combustion of biomass and coal is designed. Using this device and the corresponding method, corresponding graphite sample preparation operations can be performed for raw material samples from three different sources, making the graphite preparation process more convenient and rapid, and promoting AMS-based 14 The C detection method is more widely used in the determination of biomass blending ratio, making the biomass and coal co-combustion technology more widely used in power plants to adjust the energy usage 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 samples and improve the preparation purity.

[0005] In order to solve the above technical problems, the present invention provides the following technical solutions: a device for producing graphite samples by co-combustion of multi-system biomass and coal, comprising a transfer 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 foreign gas absorption component, connected to the flue gas filter through a glass tube, for removing foreign gases from 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 assembly is connected to the glass tube and is used for the biomass or coal to react alone 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 oxygen cylinder;

[0011] A tubular furnace, used to provide heat for the combustion reaction, and the low temperature zone of the tubular furnace is connected to the oxygen cylinder;

[0012] a vacuum pump in communication with the transfer assembly;

[0013] The adapter assembly comprises an adapter connected to the high temperature zone of the tubular 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 component includes a second serpentine tube connected to the glass tube, a vacuum gauge connected to the second serpentine tube and a graphitized component connected to the vacuum gauge, the graphitized component includes a reaction tube connected to the glass tube, the reaction tube is also provided with an outer tube, the interface in the transfer component 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 embodiment 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 biomass and coal co-combustion device for producing graphite samples described in 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 preparing 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 samples through a first subsystem;

[0020] The second subsystem is used to produce carbon dioxide by co-combusting biomass and coal to make graphite samples;

[0021] The biological clock is mixed with coal through the third subsystem to produce carbon monoxide to make graphite samples.

[0022] As a preferred embodiment of the multi-system method for preparing graphite samples by co-combustion of biomass and coal of the present invention, the first subsystem is composed of an original 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 fume 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 method for preparing graphite samples by co-combustion of biomass and coal in a multi-system according to the present invention, the preparation method through the first subsystem includes: closing the third valve and the fourth valve, mixing the biomass or coal raw material with copper oxide and placing them in a quartz tube, opening the remaining valves and starting the vacuum pump, and then sealing the quartz tube with a blast gun, and generating carbon dioxide after reacting in the quartz tube at different temperatures in the muffle furnace and then connecting it to the transfer component;

[0026] After placing zinc and titanium hydride in the outer tube and iron in the reaction tube, evacuating the 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 obtaining a graphite sample;

[0028] The preparation method through 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 inside the reaction tube, placing the biomass and coal mixed raw material into the low temperature zone of the tube furnace, evacuating the vacuum pump, starting to increase the temperature of the tube furnace, introducing oxygen and closing the sixth valve, and then continuing to increase the temperature, and the combustion flue gas is cooled by the adapter component and then removed particles by the flue gas filter;

[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 inside 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 sample.

[0030] As a preferred embodiment of the method for preparing graphite samples by co-combustion of biomass and coal in multiple systems of the present invention, the preparation method through 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 materials into the low temperature zone of the tubular furnace, evacuating the air through the vacuum pump, starting to increase the temperature of the vacuum pump, introducing oxygen and closing the ninth valve, and removing particles from the flue gas generated by the combustion after cooling through the transfer device;

[0031] Then, the mixture is passed into a gas washing bottle respectively filled with sodium hydroxide and pyrogallic acid solution to remove impurities, and the carbon dioxide is transferred to the reaction tube and placed in a muffle furnace for reaction, and finally a graphite sample is obtained.

[0032] The beneficial effects of the present invention are as follows: the three subsystems can be integrated and assembled through the cooperation of the various components, which can greatly reduce the preparation cost and preparation efficiency. At the same time, corresponding graphite sample 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 ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work. Among them:

[0034] Figure 1 The present invention is a structural diagram of a device and method for producing graphite samples by co-combustion of multi-system biomass and coal.

[0035] Figure 2 The present invention is a valve position diagram for a device and method for producing graphite samples by co-firing biomass and coal in multiple systems. 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 in conjunction with the accompanying drawings.

[0037] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein, and 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" as used herein refers to a specific feature, structure or characteristic that may be included in at least one implementation of the present invention. The term "in one embodiment" that appears in different places in this specification does not necessarily refer to the same embodiment, nor is it an embodiment that is mutually exclusive with other embodiments, either individually or selectively.

[0039] Example 1

[0040] Reference Figure 1 and Figure 2 , which is the first embodiment of the present invention, and provides 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 switching component 300, a flue gas filter 400, a foreign gas removal component 500, a transfer component 600 and an original oxidation component 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 adopt the RUNSHENG304 model.

[0045] Preferably, the impurity 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 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, which are respectively filled with sodium hydroxide solution and pyrogallic acid solution for the reaction of the third subsystem, and are 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, 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 graphitization member 603 connected to the vacuum gauge 602. The graphitization member 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 interface in the transfer component 600 and the interface in the first serpentine tube 502 all use vertically connected ball mill mouths A, and the ball mill mouth A is also provided with a spherical interface clamp H for fixing the connection end. The second serpentine tube 601 is divided into two sections, which are respectively used to remove water vapor and store fixed carbon dioxide. The connection part between the vacuum gauge 602 and the circulation pipeline is a vacuum gauge and a clamp. The ball mill mouth A uses gravity to press the interface tightly to avoid the leakage that is easy to occur in 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 alone 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 smoke 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] Reference Figure 1 and Figure 2 , which is the second embodiment of the present invention, and this embodiment is based on the previous embodiment.

[0052] Specifically, it also includes: In the previous embodiment, the method for preparing graphite samples by co-combustion of biomass and coal in multiple systems includes preparing graphite samples by producing carbon dioxide from biomass or coal alone through a first subsystem;

[0053] The second subsystem is used to produce graphite samples 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 to make graphite samples.

[0055] First, for the first subsystem, the carbon dioxide produced by biomass or coal alone is used to make a graphite sample, and the third valve 501b and the fourth valve 501c are closed. A biomass or coal raw material containing 2-3 mg carbon and 70-80 mg CuO are mixed and placed in the quartz tube 703 of the original oxidation component 700, and the remaining valves are opened and the vacuum pump 800 is turned on to evacuate the system to 10 -2After Pa, the quartz tube 703 is sealed with a flame gun, and then the sealed quartz tube 703 is placed in a muffle furnace for reaction at 500℃ for 1h, and then at 900℃ for 4h before being connected to the original oxidation assembly 700 again. 30-35mg Zn and 10-15mg TiH2 are stored in the outer tube 603b, and 3-5mg Fe is stored in the reaction tube 603a. Since the entire device will be in contact with air when the quartz tube 703 is connected again, the vacuum pump 800 needs to be used again to evacuate the system to 10 -2 Pa. Close the sixth valve 602a, break the quartz tube 703 with the first bellows 702 to release CO2, and put a liquid nitrogen cold trap on the second serpentine tube 601 to fix CO2 here. Close the eighth valve 701a and the seventh valve 602b, open the sixth valve 602a, put the liquid nitrogen cold trap on the tube between the sixth valve 602a and the seventh valve 602b to transfer CO2 to this place, put a -76℃ alcohol cold trap on the second serpentine tube 601 to remove water vapor, and after 1 minute, wait for the vacuum gauge 602 to drop to 0, open the seventh valve 602b and quickly close it to remove impurities. Close the sixth valve 602a, remove the liquid nitrogen cold trap and quantify CO2 through the 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 603a, then seal the reaction tube 603a with a flame gun and place it in a muffle furnace for reaction at 500°C for 3h and 600°C for 4h to obtain a graphite sample;

[0056] For the second subsystem: realize the operation of producing CO2 and graphite by co-combustion of biomass and coal, close the eighth valve 701a, the second valve 501a and the fourth valve 501c. Store 30-35 mg Zn and 10-15 mg TiH2 in the outer tube 603b of the graphitization device, store 3-5 mg Fe in the reaction tube 603a, and put the crucible containing 1 g of the biomass and coal mixed raw material into the low temperature zone of the two-stage tubular furnace 200, and use the vacuum pump 800 to evacuate the system to 10 -2 Pa, start running the tube furnace program. The low temperature zone and high temperature zone are first raised to 120℃ and 250℃ respectively, at this time, 50mL·min -1O2, the low temperature zone and the high temperature zone are respectively raised to 250℃ and 400℃ at the same time, then to 400℃ and 650℃ at the same time, finally the low temperature zone is raised to 850℃ in 35min and maintained for 30min, and the high temperature zone is raised to 850℃ in 20min and maintained for 45min. When O2 is introduced, the sixth valve 602a is closed, the flue gas generated by combustion is cooled by the transfer device, and then passes through the flue gas filter 400 to remove particles, and then passes through the first section of the second serpentine tube 601 with a -76℃ alcohol cold trap to remove water vapor and is fixed in the second section of the second serpentine tube 601 with a liquid nitrogen cold trap. After the combustion is completed, the third valve 501b and the seventh valve 602b are closed, the sixth valve 602a is opened, and the liquid nitrogen cold trap is placed on the pipe between the sixth valve 602a and the seventh valve 602b to transfer CO2 to this place. After 1 minute, when the vacuum gauge reading drops to 0, the seventh valve 602b is opened and quickly closed to remove impurities. Close the sixth valve 602a, remove the liquid nitrogen cold trap and determine the CO2 by vacuum gauge. Close the ninth valve 801a, open the seventh valve 602b and put the liquid nitrogen cold trap on the graphitized part 603 to fix the CO2 in 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 sample.

[0057] It is worth mentioning that in common operations, the CO2 generated by combustion in a tubular furnace needs to be collected by an air bag first, and then passed into a gas 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 CO2 transfer graphitization device is operated according to the steps of the above-mentioned device to finally obtain graphite.

[0058] The use of subsystem 2 can omit 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: realize the operation of producing graphite by co-combustion of biomass and coal, close the third valve 501b and the fifth valve 501d. Place 30-35 mg Zn and 10-15 mg TiH2 in the outer tube of the reaction tube group of the graphitization device, and place 3-5 mg Fe in the reaction tube 603a. Place a crucible containing 1 g of the mixed raw material of biomass and coal in the low temperature zone of the two-stage tubular furnace 200, and use a vacuum pump to evacuate the system to 10 -2Pa, start running the tube furnace program, the program is the same as the tube furnace program in the second subsystem. When O2 is introduced, the ninth valve 801a is closed. The flue gas generated by combustion is cooled by the transfer device and first passes through the flue gas filter to remove particles, then passes through the serpentine tube with a -76℃ alcohol cold trap to remove water vapor, and then passes through 0.7L of 1.25mol·L -1 NaOH and 0.30 L of 1.25 mol·L -1 The washing bottle 503 of the pyrogallic acid solution removes NO2, SO2, CO2, and O2 gases, and transfers CO to the reaction tube 603a. After the combustion is completed, it is sealed and placed in a muffle furnace at 600°C for 4 hours to obtain a graphite sample.

[0060] By adding the third subsystem, it is possible to accurately determine the gas phase carbon source for the incompletely burned gas phase carbon in the flue gas. 14 C sample preparation, establish corresponding calculation model, reduce the calculation error of blending ratio, and improve the accuracy of 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 rather than to limit it. 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 device for producing graphite samples by mixing biomass and coal, characterized in that: include, including an oxygen cylinder (100); The adapter assembly (300) is used to cool down the high-temperature combustion flue gas; A smoke filter (400), connected to the adapter assembly (300), for filtering particulate impurities in the combustion smoke; A foreign gas removal component (500) is connected to the fume filter (400) via a glass tube (501) and is used to remove foreign gases in the combustion fume; 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; The adapter assembly (300) comprises an adapter (301) connected to a high temperature zone of a tube furnace (200), and a conical flask (302) sleeved on the adapter (301), wherein the conical flask (302) is placed in a water tank (303), and the low temperature zone of the tube furnace (200) is connected to the oxygen cylinder (100); The device comprises producing carbon dioxide from biomass or coal alone through a first subsystem to make a graphite sample; The second subsystem is used to produce carbon dioxide by co-combusting biomass and coal to make graphite samples; The third subsystem is used to produce carbon monoxide by co-combusting biomass and coal to make graphite samples; The first subsystem is composed of the original oxidation component (700), the transfer component (600) and the vacuum pump (800), and the three are connected in sequence; The second subsystem is composed of the oxygen cylinder (100), the tubular furnace (200), the adapter assembly (300), the 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.

2. The device for producing graphite samples by mixing biomass and coal according to claim 1, 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).

3. The device for producing graphite samples by co-combustion of multi-system biomass and coal as claimed in claim 2, characterized in that: The transfer assembly (600) comprises 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) comprises a reaction tube (603a) connected to the glass tube (501); an outer tube (603b) is further provided on the reaction tube (603a); the interface in the transfer assembly (600) and the interface in the first serpentine tube (502) all adopt a vertically connected ball milling port (A); and a spherical interface clamp (H) for fixing the connection end is further provided on the ball milling port (A); the reaction tube (603a) is finally connected to a vacuum pump (800).

4. The device for producing graphite samples by co-combustion of multi-system biomass and coal as claimed in claim 3, characterized in that: The original oxidation component (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.

5. The device for producing graphite samples by co-combustion of multi-system biomass and coal as claimed in claim 4, characterized in that: A first valve (401) is provided at the connection point between the other end of the smoke 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).

6. A method for preparing graphite samples by co-combustion of multi-system biomass and coal, characterized in that: The method applied to the multi-system biomass and coal mixed combustion graphite sample device as claimed in claim 5 comprises: the preparation method through the first subsystem comprises: closing the third valve (501b) and the fourth valve (501c), taking the biomass or coal raw material and the copper oxide mixed and putting them into the quartz tube (703), opening the remaining valves and starting the vacuum pump (800), and then sealing the quartz tube (703) with a blast gun, and generating carbon dioxide after the quartz tube (703) reacts at different temperatures in the muffle furnace and then connects 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), the 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 reaction tube (603a), placing the reaction tube (603a) in a muffle furnace for reaction, and finally obtaining a graphite 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), evacuating the vacuum pump (800), starting to increase the temperature of the tube furnace (200), introducing oxygen and closing the sixth valve (602a), and then continuing to increase the temperature, and the combustion flue gas is cooled through the adapter component (300) and then removed particles through the flue gas filter (400); 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 inside 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 sample.

7. The method for preparing graphite samples by co-firing multi-system biomass and coal as claimed in claim 6, 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), evacuating the vacuum pump (800), starting to increase the temperature of the tube furnace (200), introducing oxygen and closing the ninth valve (801a), and the flue gas generated by the combustion is cooled by the adapter component (300) and then passed through the flue gas filter (400) to remove particles; Then, the mixture is introduced into a gas washing bottle respectively filled with sodium hydroxide and pyrogallic acid solution 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 sample is obtained.

Citation Information

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