Carbonaceous component separation device and quantitative method
By designing a carbonaceous component separation device including a heating reactor, a hydrogen gas supply, an oxygen gas supply, a cold trap collection device and a carbon dioxide quantitative detection device, the problems of error interference and cumbersome operation in the prior art are solved, and efficient and accurate separation and quantification of carbonaceous component are achieved.
Patent Information
- Application Number
- CN202411915927.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-24
- Publication Date
- 2025-05-13
AI Technical Summary
The existing carbonaceous component separation methods have error interference, complicated operation, misjudgment or repetition, making it difficult to achieve efficient and accurate separation.
A carbonaceous component separation device is designed, including a heating reactor, a hydrogen gas supply member, an oxygen gas supply member, a cold trap collection device and a carbon dioxide quantitative detection device. By adjusting the temperature of the hydrogen and oxygen supply and the heating reactor, the separation and quantification of organic carbon in the sample is achieved.
It realizes efficient separation and quantification of carbonaceous components, and has the advantages of simplicity, efficiency and high accuracy, avoiding errors and operation complexity in the prior art.
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Figure CN119971902A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of carbonaceous component separation and quantitative technology, and specifically relates to a carbonaceous component separation device and a quantitative method. Background Art
[0002] Carbon component separation refers to the process of effectively separating the organic carbon and inorganic carbon components in carbonaceous materials. This process is involved in many fields, mainly including coal processing, atmospheric aerosol analysis, soil organic carbon analysis, etc.
[0003] In the prior art, the methods for separating carbonaceous components are mainly the following:
[0004] (1) Stirring and aerating method: Coal, agglomerated oil and water are mixed and stirred to form agglomerates with the carbonaceous components in the coal, the oil and the air trapped in the agglomerates. The air trapped in the agglomerates gives the agglomerates buoyancy, so the agglomerates gather on the water surface, while the inorganic residual solids gather on the bottom of the water. This method uses the buoyancy characteristics of the agglomerates to separate the carbonaceous components.
[0005] (2) Density grouping method: Soil is centrifuged in heavy liquid to separate organic carbon and inorganic carbon based on density differences. The component floating on the surface of the liquid is light organic carbon, and the precipitated part is heavy organic carbon. Light organic carbon mainly comes from plant debris, plant roots and charcoal, while heavy organic carbon is mainly humus.
[0006] (3) Particle grouping method: Separate particulate organic carbon and mineral-bound organic carbon based on the difference in particle size. Soil particles are dispersed by sodium hexametaphosphate or ultrasound. Particles > 0.053 mm are particulate organic carbon, and particles < 0.053 mm are mineral-bound organic carbon. Particulate organic carbon is mainly produced by plant activities, while mineral-bound organic carbon is produced by microbial activities.
[0007] Based on the above methods, the stirring and aeration method mainly uses the buoyancy characteristics of agglomerates to separate carbonaceous components, so there is a large error interference; the density grouping method mainly achieves stratification through centrifugation, and then further separates the light component organic carbon and the heavy component organic carbon. This method has the problem of cumbersome and complicated operation; the particle grouping method mainly separates organic carbon and inorganic carbon based on density differences, and the particle separation is mainly between 0.053mm particles. Therefore, it is inevitable that there will be misjudgments or duplications on the intermediate value particles. Therefore, there is still room for improvement. Summary of the invention
[0008] In order to overcome the deficiencies of the prior art, the object of the present invention is to provide a carbonaceous component separation device and a quantitative method, which can effectively separate carbonaceous components and have the advantages of simple operation, high efficiency and high precision.
[0009] The purpose of the present invention is achieved through the following technical solutions:
[0010] A carbonaceous component separation device comprises a heating reaction furnace, a hydrogen gas supply component, an oxygen gas supply component, a cold trap collection device, and a carbon dioxide quantitative detection device; the heating reaction furnace is connected to a normally open three-way valve and an electrically controlled three-way valve; the hydrogen gas supply component and the oxygen gas supply component are respectively connected to the two ends of the normally open three-way valve; the cold trap collection device and the carbon dioxide quantitative detection device are respectively connected to the electrically controlled three-way valve.
[0011] Furthermore, the hydrogen supply component includes a valved hydrogen tank, a filter, a gas mass flow meter, and a first one-way valve. The valved hydrogen tank is connected to the inlet of the filter through a pipeline, the outlet of the filter is connected to the inlet of the gas mass flow meter through a pipeline, the outlet of the gas mass flow meter is connected to the inlet of the first one-way valve through a pipeline, and the outlet of the first one-way valve is connected to the normally open three-way valve.
[0012] Furthermore, the oxygen supply component includes a valved oxygen tank, an electrically controlled stop valve, and a second one-way valve. The valved oxygen tank is connected to the electrically controlled stop valve through a pipeline, the electrically controlled stop valve is connected to the inlet of the second one-way valve through a pipeline, and the outlet of the second one-way valve is connected to the normally open three-way valve through a pipeline.
[0013] Furthermore, a pressure gauge is connected between the heating reaction furnace and the normally open three-way valve.
[0014] Furthermore, the cold trap collection device includes a refrigeration cylinder, a reaction adsorption tube, adsorption silica gel, and a manual back pressure valve. The reaction adsorption tube is placed in the refrigeration cylinder, the top of the reaction adsorption tube is connected to the electric three-way valve through a pipeline, the bottom tube pipeline of the reaction adsorption tube is connected to the manual back pressure valve, and the adsorption silica gel is arranged at the inner bottom of the reaction adsorption tube.
[0015] Furthermore, it also includes a carbon dioxide collection device, which is connected to the emission outlet of the carbon dioxide quantitative detection device through a pipeline.
[0016] Furthermore, the heating reaction furnace includes a heating rod, an insulation layer, and a reaction column tube. The insulation layer is arranged on the outer circumference of the heating rod, the reaction column tube is embedded in the heating rod, and the tube mouth of the reaction column tube is exposed at the end of the heating rod.
[0017] Furthermore, the thermal insulation layer includes a thermal insulation layer and a high temperature resistant layer, the thermal insulation layer is placed in the high temperature resistant layer, and the high temperature resistant layer is made of 310S stainless steel material.
[0018] A carbonaceous component quantification method, using the carbonaceous component separation device, comprises the following steps:
[0019] S10: taking a sample to be tested, and determining the total carbon content TC of the sample to be tested, adding it to a quartz sample tube after weighing, and plugging the end of the quartz sample tube with quartz wool; then adding activated adsorption silica gel to the reaction adsorption tube, and plugging both ends of the reaction adsorption tube with quartz wool; then putting the quartz sample tube into a heating reaction furnace, and connecting the carbonaceous component separation device in sequence; adjusting the electric-controlled three-way valve, and connecting the heating reaction furnace and the cold trap collection device, so as to use a manual back pressure valve to perform a gas leakage check;
[0020] S20: After the leakage check is passed, the whole system of the carbonaceous component separation device is maintained at a pressure of 5±0.5MPa; then the valved hydrogen tank is opened, and the valved oxygen tank is closed, and then the manual back pressure valve is adjusted to adjust the flow rate of hydrogen H2 in the valved hydrogen tank into the heating reactor to 2L / min; then the temperature of the heating reactor is adjusted, starting from room temperature, at a rate of 5℃ / min, to 550℃, and finally kept at a constant temperature for 60min; at this time, the sample to be tested is under the reduction environment of high-temperature hydrogen, and the organic carbon is separated into the reaction adsorption tube and adsorbed on the adsorption silica gel;
[0021] S30: adjusting the temperature of the heating reaction furnace to 100°C at a rate of 5°C / min; then adjusting the electrically controlled three-way valve to connect the heating reaction furnace with the carbon dioxide quantitative detection device, then closing the valved hydrogen tank and opening the valved oxygen tank to connect the valved oxygen tank with the heating reaction furnace;
[0022] S40: Then adjust the temperature of the heating reaction furnace to 800°C at a rate of 10°C / min, and finally keep the temperature constant for 6 minutes; at this time, the carbon dioxide generated by the reaction of oxygen with the sample to be tested in the heat reaction furnace is measured by the carbon dioxide quantitative detection device as the black carbon content BC;
[0023] S50: The amount of organic carbon adsorbed in the reaction adsorption tube OC is obtained by subtracting the amount of black carbon BC from the total carbon content TC of the sample to be tested.
[0024] Further, in S10, a catalyst is mixed evenly in the sample to be tested, and the catalyst is (NH4)2MoO2S2.
[0025] The present invention has the following beneficial effects:
[0026] 1. The present invention is provided with a heating reaction furnace, a hydrogen gas supply component, an oxygen gas supply component, a cold trap collection device, and a carbon dioxide quantitative detection device. By adjusting the hydrogen gas supply component, the oxygen gas supply component and the electrically controlled three-way valve, only the hydrogen of the hydrogen gas supply component is communicated with the heating reaction furnace, and the heating reaction furnace is communicated with the cold trap collection device. By adjusting the exhaust speed of the cold trap collection device, the speed at which the oxygen gas supply component discharges into the heating reaction furnace is adjusted. At the same time, the heating reaction furnace is used to gradually increase the temperature in the furnace to 550°C and then keep the temperature constant for a period of time. In this process, the sample in the heating reaction furnace will separate the organic carbon in the sample under the reducing atmosphere of high-temperature hydrogen and discharge it to the cold trap collection device for absorption. After the reduction process is completed, the temperature in the furnace is lowered to 100°C by the heating reaction furnace, and then the hydrogen supply part, oxygen supply part and the electrically controlled three-way valve are adjusted to make only the oxygen of the oxygen supply part communicate with the heating reaction furnace, and the heating reaction furnace is communicated with the carbon dioxide quantitative detection device. At the same time, the temperature in the furnace is raised to 800°C by the heating reaction furnace, and the temperature is kept constant for a period of time to utilize oxygen and the sample separated by reduction to fully burn, thereby generating carbon dioxide, and finally obtaining the amount of black carbon BC in the sample through the carbon dioxide quantitative detection device. Therefore, the amount of organic carbon adsorbed in the cold trap collection device OC can be obtained by subtracting the amount of black carbon BC from the total carbon content TC of the sample. Therefore, compared with the prior art, the carbonaceous component separation device of the present invention can effectively separate carbonaceous components (i.e., organic carbon), and has the advantages of simple operation, high efficiency and high precision.
[0027] 2. The carbonaceous component quantitative method of the present invention is mainly implemented based on the carbonaceous component separation device. Through step S10, the total carbon content TC in the sample can be measured in advance, and the prerequisite preparation for the subsequent sample reaction can be made; through step S20, the organic matter (containing organic carbon) and water vapor in the sample can be separated and adsorbed in the cold trap under the reducing atmosphere of high-temperature hydrogen. Therefore, by setting steps S30 and S40, oxygen and the sample are fully burned at high temperature to completely form carbon dioxide from the carbon in the sample, and the carbon content in the carbon dioxide can be further determined by the carbon dioxide quantitative detection device, thereby obtaining the black carbon content BC of the sample. Therefore, the total carbon content TC minus the black carbon content BC is the organic carbon content OC in the sample adsorbed in the cold trap collection device. Therefore, by adopting the carbonaceous component quantitative method of the present invention, it has the advantages of simple operation, high efficiency and high precision. BRIEF DESCRIPTION OF THE DRAWINGS
[0028] Figure 1 It is a structural principle diagram of the carbonaceous component separation device of the present invention.
[0029] Figure 2 It is a cross-sectional view of the heating reaction furnace of the present invention.
[0030] In the figure: 01, heating reaction furnace; 011, heating rod; 012, insulation layer; 013, reaction column; 02, hydrogen tank with valve; 03, filter; 04, gas mass flow meter; 05, first one-way valve; 06, oxygen tank with valve; 07, electric control stop valve; 08, second one-way valve; 09, normally open three-way valve; 10, pressure gauge; 11, electric control three-way valve connection; 12, cold trap collection device; 121, refrigeration cylinder; 122, reaction adsorption tube; 13, manual back pressure valve; 14, carbon dioxide quantitative detection device; 15, carbon dioxide collection device. DETAILED DESCRIPTION
[0031] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. The terms such as "upper", "inner", "middle", "left", "right" and "one" cited in this specification are only for the convenience of description, and are not used to limit the scope of the present invention. The change or adjustment of their relative relationship shall also be regarded as the scope of the present invention without substantially changing the technical content.
[0032] Example 1
[0033] A carbonaceous component separation device, such as Figure 1 and Figure 2 As shown, it includes a heating reaction furnace 01, a hydrogen gas supply component, an oxygen gas supply component, a cold trap collection device 12, a carbon dioxide quantitative detection device 14, and a carbon dioxide collection device 15; the upper and lower ends of the heating reaction furnace 01 are respectively connected with a normally open three-way valve 09 and an electric-controlled three-way valve through pipelines; the hydrogen gas supply component and the oxygen gas supply component are respectively connected to the two ends of the normally open three-way valve 09; the cold trap collection device 12 and the carbon dioxide quantitative detection device 14 are respectively connected to the electric-controlled three-way valve 11; the carbon dioxide collection device 15 is connected to the discharge outlet of the carbon dioxide quantitative detection device 14 through a pipeline.
[0034] Based on this, the present invention sets a heating reaction furnace 01, a hydrogen gas supply component, an oxygen gas supply component, a cold trap collecting device 12, and a carbon dioxide quantitative detection device 14. By adjusting the hydrogen gas supply component, the oxygen gas supply component and the electrically controlled three-way valve, only the hydrogen of the hydrogen gas supply component is connected to the heating reaction furnace 01, and the heating reaction furnace 01 is connected to the cold trap collecting device 12. By adjusting the exhaust speed of the cold trap collecting device 12, the speed at which the oxygen gas supply component is discharged into the heating reaction furnace 01 can be adjusted. At the same time, the heating reaction furnace 01 is used to gradually increase the temperature in the furnace to 550°C and then keep the temperature constant for a period of time. During this process, the sample in the heating reaction furnace 01 will separate the organic carbon in the sample under the reducing atmosphere of high-temperature hydrogen and discharge it into the cold trap collecting device 12 for absorption. After the reduction process is completed, the temperature in the furnace is lowered to 100°C by heating the reaction furnace 01, and then by adjusting the hydrogen supply component, the oxygen supply component and the electrically controlled three-way valve, only the oxygen of the oxygen supply component is connected to the heating reaction furnace 01, and the heating reaction furnace 01 is connected to the carbon dioxide quantitative detection device 14. At the same time, the temperature in the furnace is raised to 800°C by the heating reaction furnace 01, and the temperature is kept constant for a period of time, so that the oxygen and the sample separated by reduction are fully burned, thereby generating carbon dioxide, and finally the black carbon amount BC in the sample is obtained by the carbon dioxide quantitative detection device 14. Therefore, the amount of organic carbon OC adsorbed in the cold trap collection device 12 can be obtained by subtracting the black carbon amount BC from the total carbon content TC of the sample. Therefore, compared with the prior art, the carbonaceous component separation device of the present invention can effectively separate carbonaceous components (i.e., organic carbon), and has the advantages of simple operation, high efficiency and high precision.
[0035] In this embodiment, the hydrogen supply component includes a valved hydrogen tank 02, a filter 03, a gas mass flowmeter 04, and a first one-way valve 05; the valved hydrogen tank 02 is connected to the inlet of the filter 03 through a pipeline, so that the filter 03 can be used to filter impurities in the hydrogen, and the outlet of the filter 03 is connected to the inlet of the gas mass flowmeter 04 through a pipeline. The gas mass flowmeter 04 is used to measure the flow rate of the hydrogen gas flow in the current pipeline. The outlet of the gas mass flowmeter 04 is connected to the inlet of the first one-way valve 05 through a pipeline. The first one-way valve 05 is used to prevent the backflow of hydrogen in the pipeline. The outlet of the first one-way valve 05 is connected to the normally open three-way valve 09.
[0036] Among them, the relevant specifications of the gas mass flow meter 04 are as follows: material is SS316L; flow range is 0-2000mL / min; error value is ±0.5%Rd plus±0.1%FS; input pressure (P1): 10MPa; output pressure (P2): 0.5...9.5MPa.
[0037] In this embodiment, the oxygen supply component includes a valved oxygen tank 06, an electrically controlled stop valve 07, and a second one-way valve 08; the valved oxygen tank 06 is connected to the electrically controlled stop valve 07 through a pipeline, the electrically controlled stop valve 07 is used to remotely shut off the function of supplying oxygen to the heating reactor 01, the electrically controlled stop valve 07 is connected to the inlet of the second one-way valve 08 through a pipeline, the second one-way valve 08 is used to prevent the backflow of oxygen in the pipeline, and the outlet of the second one-way valve 08 is connected to the normally open three-way valve 09 through a pipeline.
[0038] At the same time, a pressure gauge 10 is connected between the heating reaction furnace 01 and the normally open three-way valve 09 through a pipeline. The pressure gauge 10 is used to measure whether the gas pressure flowing into the heating reaction furnace 01 is within an appropriate range, so as to reduce the working failure of the heating furnace or excessive pressure, and play a beneficial role in effective pressure monitoring and improving safety of use.
[0039] In this embodiment, the cold trap collection device 12 includes a refrigeration cylinder 121, a reaction adsorption tube 122, adsorption silica gel, and a manual back pressure valve 13; the refrigeration cylinder 121 of this embodiment is a device for condensation refrigeration in the cold trap structure, which can achieve refrigeration by holding circulating condensate or by air cooling; the reaction adsorption tube 122 is arranged in the refrigeration cylinder 121, and the reaction adsorption tube 122 is refrigerated by the refrigeration cylinder 121. The top of the reaction adsorption tube 122 is connected to the electric three-way valve 11 through a pipeline, and the bottom tube pipeline of the reaction adsorption tube 122 is connected to the manual back pressure valve 13, the manual back pressure valve 13 is arranged outside the refrigeration cylinder 121, and the adsorption silica gel is arranged at the inner bottom of the reaction adsorption tube 122. Therefore, when the sample in the heating reaction furnace 01 is in a reducing environment of high-temperature hydrogen, the carbonaceous components in the sample to be tested can be separated and discharged to the reaction adsorption tube 122 with the airflow. In a low-temperature environment, the water vapor and organic solvent (including organic carbon) in the airflow can be efficiently attached to the adsorption silica gel, thereby achieving the separation of carbonaceous components.
[0040] In this embodiment, Figure 2 As shown, the heating reaction furnace 01 includes a shell with a sealed door, a heating rod 011, a heat preservation layer 012, and a reaction column tube 013. The heating rod 011 is arranged in the shell, and the heat preservation layer 012 is arranged on the outer peripheral surface of the heating rod 011. The heat preservation layer 012 includes a heat preservation and heat insulation layer and a high temperature resistant layer. The heat preservation and heat insulation layer is arranged in the high temperature resistant layer. The high temperature resistant layer is made of 310S stainless steel material and has the advantage of not being easily deformed at high temperature. The reaction column tube 013 is embedded in the heating rod 011, and the nozzle of the reaction column tube 013 is exposed at the end of the heating rod 011.
[0041] It should be noted that the present invention mainly remotely observes the flow rate of the gas mass flowmeter 04, the pressure value of the pressure gauge 10, the opening and closing of the electric control stop valve 07, the steering and opening and closing of the electric control three-way valve, and the temperature inside the heating reactor 01 through the system control software, so as to facilitate the judgment of the working condition and operation progress of the carbon component separation device at this time, and then facilitate the remote control of the cylinder to adjust the gas pressure in the system, the temperature of the heating reactor 01, and the steering condition of the electric control three-way valve, so as to realize the role of timely following up the internal operation progress and remote regulation, and has the advantages of simple operation, high efficiency and high precision.
[0042] Regarding the system control software, a conventional monitoring system of the prior art can be adopted, which has a visual interactive operation mode, and the real-time data in the system device can be displayed through a curve, which is convenient for analyzing and viewing the long-term operation stability, and different gas flow coefficients will be automatically switched and set.
[0043] Example 2
[0044] A carbonaceous component quantification method, using the carbonaceous component separation device of Example 1, comprises the following steps:
[0045] S10: Take a mixed (NH4)2MoO2S2 catalyst sample to be tested, and determine the total carbon content TC of the sample to be tested by the existing technology, wherein the total carbon content can be determined by infrared absorption method, gas chromatography, elemental analysis, spectrophotometry, etc.; then, weigh the sample to be tested and add it to the quartz sample tube, and then plug the end of the quartz sample tube with quartz wool; then add activated adsorption silica gel to the inner bottom of the reaction adsorption tube 122, and then plug the two ends of the reaction adsorption tube 122 with quartz wool; then put the quartz sample tube into the reaction column tube 013 of the heating reaction furnace 01, and connect the carbonaceous component separation device in sequence; then adjust the electric three-way valve, and make the heating reaction furnace 01 and the cold trap collection device 12 communicate, so as to use the manual back pressure valve 13 to perform a leak check;
[0046] S20: After the leakage check is passed, the entire system of the carbonaceous component separation device is maintained at a pressure of 5±0.5MPa; then the valved hydrogen tank 02 is opened, and the valved oxygen tank 06 is closed, and then the manual back pressure valve 13 is used to adjust the flow rate of the hydrogen H2 in the valved hydrogen tank 02 flowing into the heating reaction furnace 01 to 2L / min; then the temperature of the heating reaction furnace 01 is adjusted, starting from room temperature, at a rate of 5℃ / min, to 550℃, and finally kept at a constant temperature for 60min; at this time, the sample to be tested is under the reducing environment of high-temperature hydrogen, and the organic carbon is separated and enters the reaction adsorption tube 122, and the organic carbon is absorbed by the adsorption silica gel together with the water vapor and organic matter in the cold trap collection device 12, thereby realizing the separation of organic matter and water vapor in the sample;
[0047] S30: Adjust the temperature of the heating reaction furnace 01 to 100°C at a rate of 5°C / min; then adjust the electronically controlled three-way valve to connect the heating reaction furnace 01 with the carbon dioxide quantitative detection device 14, then close the valved hydrogen tank 02, open the valved oxygen tank 06, connect the valved oxygen tank 06 with the heating reaction furnace 01, and discharge oxygen into the heating reaction furnace 01;
[0048] S40: Then adjust the temperature of the heating reaction furnace 01 to 800°C at a rate of 10°C / min, and finally keep the temperature constant for 6 minutes; at this time, the oxygen in the heat reaction furnace fully burns and reacts with the reduced sample to react all the carbon in the sample and produce carbon dioxide, and the carbon dioxide in the reaction furnace is further measured by the carbon dioxide quantitative detection device 14 as the carbon black amount BC;
[0049] S50: The amount of organic carbon OC adsorbed in the reaction adsorption tube 122 is obtained by subtracting the black carbon content BC from the total carbon content TC of the sample to be tested.
[0050] Based on the above method, further exemplify that when the weight of the selected sample to be tested is 98.5 mg and the carbon content of the sample is 150.7 ug / mg, the total carbon content TC can be calculated to be 14843.95 ug. After further going through the above steps S10 to S40, the carbon content is measured by the carbon dioxide through the carbon dioxide quantitative detection device 14 to be 4435.41 ug, that is, the black carbon content BC in the sample is 4435.41 ug. Therefore, the total carbon content TC minus the black carbon content BC is the organic carbon content OC in the sample adsorbed in the cold trap collection device 12. That is, OC=TC-BC=14843.95 ug-4435.41 ug=10408.54 ug.
[0051] In summary, the carbonaceous component quantitative method of the present invention is mainly implemented based on the carbonaceous component separation device. Through step S10, the total carbon content TC in the sample can be measured in advance, and the prerequisite preparation for the subsequent sample reaction can be made; through step S20, the organic matter (containing organic carbon) and water vapor in the sample can be separated and adsorbed in the cold trap under the reducing atmosphere of high-temperature hydrogen. Therefore, by setting steps S30 and S40, oxygen and the sample are fully burned at high temperature to completely convert the carbon in the sample into carbon dioxide, and the carbon dioxide quantitative detection device 14 can be used to determine the carbon content in the carbon dioxide, thereby obtaining the black carbon content BC of the sample. Therefore, the total carbon content TC minus the black carbon content BC is the organic carbon content OC in the sample adsorbed in the cold trap collection device 12. Therefore, by adopting the carbonaceous component quantitative method of the present invention, it has the advantages of simple operation, high efficiency and high precision.
[0052] The implementation methods of the present invention are not limited to this. According to the above content of the present invention, using common technical knowledge and customary means in the field, without departing from the above basic technical ideas of the present invention, the present invention can also make other various forms of modification, replacement or combination, all of which fall within the scope of protection of the present invention.
Claims
1. A carbonaceous component separation device, characterized in that: It includes a heating reaction furnace, a hydrogen gas supply component, an oxygen gas supply component, a cold trap collection device, and a carbon dioxide quantitative detection device; the heating reaction furnace is connected to a normally open three-way valve and an electrically controlled three-way valve; the hydrogen gas supply component and the oxygen gas supply component are respectively connected to the two ends of the normally open three-way valve; the cold trap collection device and the carbon dioxide quantitative detection device are respectively connected to the electrically controlled three-way valve.
2. The carbonaceous component separation device according to claim 1, characterized in that: The hydrogen supply component includes a valved hydrogen tank, a filter, a gas mass flow meter, and a first one-way valve. The valved hydrogen tank is connected to the inlet of the filter through a pipeline, the outlet of the filter is connected to the inlet of the gas mass flow meter through a pipeline, the outlet of the gas mass flow meter is connected to the inlet of the first one-way valve through a pipeline, and the outlet of the first one-way valve is connected to the normally open three-way valve.
3. The carbonaceous component separation device according to claim 1, characterized in that: The oxygen supply component includes a valved oxygen tank, an electrically controlled stop valve, and a second one-way valve. The valved oxygen tank is connected to the electrically controlled stop valve through a pipeline, the electrically controlled stop valve is connected to the inlet of the second one-way valve through a pipeline, and the outlet of the second one-way valve is connected to the normally open three-way valve through a pipeline.
4. The carbonaceous component separation device according to claim 2 or 3, characterized in that: A pressure gauge is connected between the heating reaction furnace and the normally open three-way valve.
5. The carbonaceous component separation device according to claim 1, characterized in that: The cold trap collection device includes a refrigeration cylinder, a reaction adsorption tube, adsorption silica gel, and a manual back pressure valve. The reaction adsorption tube is placed in the refrigeration cylinder. The top end of the reaction adsorption tube is connected to the electric three-way valve through a pipeline. The bottom end of the reaction adsorption tube is connected to the manual back pressure valve through a pipeline. The adsorption silica gel is arranged at the inner bottom of the reaction adsorption tube.
6. The carbonaceous component separation device according to claim 1, characterized in that: It also includes a carbon dioxide collection device, which is connected to the emission outlet of the carbon dioxide quantitative detection device through a pipeline.
7. The carbonaceous component separation device according to claim 1, characterized in that: The heating reaction furnace comprises a heating rod, a heat preservation layer and a reaction column tube. The heat preservation layer is arranged on the outer peripheral surface of the heating rod. The reaction column tube is embedded in the heating rod, and the tube mouth of the reaction column tube is exposed at the end of the heating rod.
8. The carbonaceous component separation device according to claim 7, characterized in that: The thermal insulation layer comprises a thermal insulation layer and a high temperature resistant layer. The thermal insulation layer is arranged in the high temperature resistant layer. The high temperature resistant layer is made of 310S stainless steel material.
9. A carbonaceous component quantitative method, using the carbonaceous component separation device according to any one of claims 1 to 8, characterized in that: The following steps are involved: S10: taking a sample to be tested, and determining the total carbon content TC of the sample to be tested, adding it to a quartz sample tube after weighing, and plugging the end of the quartz sample tube with quartz wool; then adding activated adsorption silica gel to the reaction adsorption tube, and plugging both ends of the reaction adsorption tube with quartz wool; then putting the quartz sample tube into a heating reaction furnace, and sequentially connecting the carbonaceous component separation device; Adjust the electric three-way valve and connect the heating reaction furnace and the cold trap collection device to check for leaks using a manual back pressure valve; S20: After the leakage check is passed, the whole system of the carbonaceous component separation device is maintained at a pressure of 5±0.5MPa; then the valved hydrogen tank is opened, and the valved oxygen tank is closed, and then the manual back pressure valve is adjusted to adjust the flow rate of hydrogen H2 in the valved hydrogen tank into the heating reactor to 2L / min; then the temperature of the heating reactor is adjusted, starting from room temperature, at a rate of 5℃ / min, to 550℃, and finally kept at a constant temperature for 60min; at this time, the sample to be tested is under the reduction environment of high-temperature hydrogen, and the organic carbon is separated into the reaction adsorption tube and adsorbed on the adsorption silica gel; S30: adjusting the temperature of the heating reaction furnace to 100°C at a rate of 5°C / min; then adjusting the electrically controlled three-way valve to connect the heating reaction furnace with the carbon dioxide quantitative detection device, then closing the valved hydrogen tank and opening the valved oxygen tank to connect the valved oxygen tank with the heating reaction furnace; S40: Then adjust the temperature of the heating reaction furnace to 800°C at a rate of 10°C / min, and finally keep the temperature constant for 6 minutes; at this time, the carbon dioxide generated by the reaction of oxygen with the sample to be tested in the heat reaction furnace is measured by the carbon dioxide quantitative detection device as the black carbon content BC; S50: The amount of organic carbon adsorbed in the reaction adsorption tube OC is obtained by subtracting the amount of black carbon BC from the total carbon content TC of the sample to be tested.
10. The carbonaceous component quantification method according to claim 1, characterized in that: In S10, a catalyst is mixed evenly in a sample to be tested, wherein the catalyst is (NH4)2MoO2S2.