CN115326910A - Analysis system for pyrolysis ternary products - Google Patents
Analysis system for pyrolysis ternary products Download PDFInfo
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- CN115326910A CN115326910A CN202210793883.0A CN202210793883A CN115326910A CN 115326910 A CN115326910 A CN 115326910A CN 202210793883 A CN202210793883 A CN 202210793883A CN 115326910 A CN115326910 A CN 115326910A
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- 238000004458 analytical method Methods 0.000 title claims abstract description 20
- 239000007789 gas Substances 0.000 claims abstract description 123
- 238000010438 heat treatment Methods 0.000 claims abstract description 92
- 238000009833 condensation Methods 0.000 claims abstract description 57
- 230000005494 condensation Effects 0.000 claims abstract description 57
- 239000000203 mixture Substances 0.000 claims abstract description 43
- 238000001816 cooling Methods 0.000 claims abstract description 38
- 239000011261 inert gas Substances 0.000 claims abstract description 28
- 239000002910 solid waste Substances 0.000 claims abstract description 19
- 239000000571 coke Substances 0.000 claims abstract description 13
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 238000001819 mass spectrum Methods 0.000 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 229910002804 graphite Inorganic materials 0.000 claims description 15
- 239000010439 graphite Substances 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000001179 sorption measurement Methods 0.000 claims description 12
- 238000004949 mass spectrometry Methods 0.000 claims description 11
- 238000010517 secondary reaction Methods 0.000 claims description 10
- 239000003507 refrigerant Substances 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 6
- 239000011358 absorbing material Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 description 22
- 238000000034 method Methods 0.000 description 11
- 238000013461 design Methods 0.000 description 10
- 238000005057 refrigeration Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 4
- 230000007246 mechanism Effects 0.000 description 4
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/02—Investigating or analyzing materials by the use of thermal means by investigating changes of state or changes of phase; by investigating sintering
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
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Abstract
The specification relates to the technical field of pyrolysis, in particular to an analysis system for pyrolysis ternary products. The system comprises a tabletting device, an infrared heating device, an air inlet device, a cooling pipe, a condensation pipe group, a weighing device, a gas heating device and a mass spectrum analysis device, wherein the tabletting device is used for tabletting solid waste to be pyrolyzed to obtain tabletting to be pyrolyzed, and the infrared heating device is used for heating the tabletting to be pyrolyzed by utilizing infrared rays to obtain an oil-gas mixture and pyrolytic coke; the gas inlet device provides inert gas for the infrared heating device; the cooling pipe cools the temperature of the oil-gas mixture; the condensing tube group comprises a plurality of groups of condensing tubes, and the condensing tubes condense the cooled oil-gas mixture to obtain first pyrolysis gas and pyrolysis oil; weighing the mass of the pyrolysis oil by a weighing device; the gas heating device heats the inert gas to heat and volatilize the pyrolysis oil to form second pyrolysis gas; the mass spectrometer analyzes the composition and mass of the first pyrolysis gas and the composition of the second pyrolysis gas.
Description
Technical Field
The embodiment of the specification relates to the technical field of pyrolysis, in particular to an analysis system for pyrolysis tri-state products.
Background
The pyrolysis technology can convert solid wastes (such as medical wastes) into pyrolysis coke, pyrolysis oil and pyrolysis gas, and the pyrolysis oil gas product can be introduced into a waste incinerator to burn and recover heat, so that the coupling heat treatment of the solid wastes in a household waste incineration power plant is promoted. Therefore, the emission of pollutants can be greatly reduced, and the efficient utilization of resources is realized.
In order to better guide the actual production of the pyrolysis solid waste, it is necessary to analyze not only the yield of pyrolysis tri-state products of typical solid waste under different pyrolysis conditions, but also the composition of gas phase (i.e., pyrolysis gas) and liquid phase (i.e., pyrolysis oil) in the pyrolysis tri-state products at different pyrolysis temperature stages. However, the related art is not high in the accuracy of analysis of pyrolysis tri-state products at different pyrolysis temperature stages.
Therefore, there is a need for an analysis system for pyrolysis of tri-state products to solve the above technical problems.
Disclosure of Invention
In order to effectively improve the analysis accuracy of the pyrolysis ternary products at different pyrolysis temperature stages, the embodiment of the specification provides an analysis system of the pyrolysis ternary products.
The embodiment of the present specification provides an analysis system for pyrolysis ternary products, including:
the tabletting device is used for carrying out tabletting treatment on the solid waste to be pyrolyzed to obtain tablets to be pyrolyzed;
the infrared heating device is used for heating the tabletting to be pyrolyzed according to a preset temperature rising condition by utilizing infrared rays to obtain an oil-gas mixture and pyrolytic coke; wherein the mass of the pyrolytic coke is measured by an external balance;
the air inlet device is connected with the infrared heating device and used for providing inert gas for the infrared heating device so as to blow the oil-gas mixture out of the infrared heating device by using the inert gas; wherein the inert gas does not include nitrogen;
the cooling pipe is connected with the infrared heating device and used for cooling the temperature of the oil-gas mixture so as to reduce the secondary reaction of the oil-gas mixture;
the condensation pipe group comprises a plurality of groups of condensation pipes, each group of condensation pipes is connected with the cooling pipe, and the condensation pipes are used for condensing the cooled oil-gas mixture to obtain first pyrolysis gas and pyrolysis oil; wherein, the heating temperatures of the to-be-pyrolyzed tablets corresponding to different condensing pipes are different;
the weighing device comprises a box body, a hydraulic sensor arranged on the inner side of the bottom wall of the box body and a pressure sensor arranged on the outer side of the bottom wall of the box body, wherein a condensation pipe group is arranged in the box body, refrigerating fluid is arranged in the box body and used for providing cold energy for the condensation pipe group, and the pressure sensor is used for measuring the quality of the pyrolysis oil when a hydraulic signal detected by the hydraulic sensor is qualified;
the gas heating device is respectively connected with each group of the condensation pipes and the gas inlet device, and is used for heating the inert gas so as to heat the pyrolysis oil separated out from the condensation pipes by using the heated inert gas, so that the pyrolysis oil is heated and volatilized to form second pyrolysis gas;
and the mass spectrum analysis device is respectively connected with each group of the condensation pipes and is used for analyzing the components and the mass of the first pyrolysis gas and the components of the second pyrolysis gas.
In a possible design, infrared heating device includes the casing, set up in just be annular infrared heating pipe in the casing, set up in reactor in the infrared heating pipe, with the reactor can dismantle the flange of connection, with flange joint just stretches into support frame in the reactor, with the graphite crucible that the support frame is connected and be used for detecting the thermocouple of graphite crucible's temperature, the inert gas that air inlet unit provided lets in the reactor, the reactor is kept away from the tip of flange is the toper structure, the tip with the cooling tube is connected.
In one possible design, the infrared ray generated by the infrared heating tube is short wave infrared ray, and the outer surface of the graphite crucible is coated with a light absorbing material absorbing the short wave infrared ray.
In a possible design, the reactor further comprises a slide rail connected with the shell, the flange is connected with the slide rail, and the flange is sealed or separated from the reactor by sliding of the flange on the slide rail.
In a possible design, still include the pressure release pipeline and set up in manometer and relief valve on the pressure release pipeline, the pressure release pipeline with flange joint the flange with when the reactor is fixed, the pressure release pipeline with the inside intercommunication of reactor, the manometer is used for detecting gas pressure in the reactor, the relief valve is used for gas pressure in the reactor reaches and predetermines behind the pressure right the reactor carries out the pressure release.
In a possible design, the cooling device further comprises an air compressor connected to the cooling pipe for providing compressed air to the outer wall surface of the cooling pipe to cool the air-fuel mixture flowing through the cooling pipe.
In a possible design, the part of each set of the condensation pipes located in the box body is in a spiral structure.
In one possible design, the refrigerator further comprises a refrigerating device and a liquid discharge valve, wherein the refrigerating device is communicated with the box body, and the refrigerating liquid circularly flows along the box body and the refrigerating device;
the liquid discharge valve is arranged at the bottom of the box body, and the liquid discharge valve is opened before the gas heating device is used for heating the condensation pipe so as to discharge the refrigerating fluid in the box body.
In a possible design, the system further comprises a temperature sensor and a PI regulator, the PI regulator is respectively connected with the temperature sensor and the gas heating device, the temperature sensor is arranged on a pipeline connected between the condensation pipe group and the mass spectrometry device, and the PI regulator is used for regulating the heating temperature of the gas heating device according to the temperature detected by the temperature sensor so as to control the temperature of the pyrolysis gas entering the mass spectrometry device.
In a possible design, the pyrolysis gas analyzer further comprises an adsorption device, wherein the adsorption device is connected with the mass spectrometry device, and the adsorption device is used for adsorbing the pyrolysis gas analyzed by the mass spectrometry device.
The embodiment of the specification provides an analysis system for pyrolysis ternary products, wherein a tabletting device is used for tabletting solid waste to be pyrolyzed to obtain tablets to be pyrolyzed; the infrared heating device heats the tablet to be pyrolyzed according to a preset temperature rise condition by using infrared rays to obtain an oil-gas mixture and pyrolysis coke, and the mass of the pyrolysis coke is measured by an external balance; the air inlet device provides inert gas for the infrared heating device so as to blow the oil-gas mixture out of the infrared heating device by using the inert gas, and the inert gas does not comprise nitrogen; the cooling pipe cools the temperature of the oil-gas mixture to reduce the secondary reaction of the oil-gas mixture, so that the product analyzed by the mass spectrometry device is a nascent reaction product; the condensing tube group comprises a plurality of groups of condensing tubes, the condensing tubes condense the cooled oil-gas mixture to obtain first pyrolysis gas and pyrolysis oil, and heating temperatures of tablets to be pyrolyzed corresponding to different condensing tubes are different; the weighing device comprises a box body, a hydraulic sensor arranged on the inner side of the bottom wall of the box body and a pressure sensor arranged on the outer side of the bottom wall of the box body, a condensation pipe group is arranged in the box body, refrigerating fluid is arranged in the box body and used for providing cold energy for the condensation pipe group, and the pressure sensor is used for measuring the quality of pyrolysis oil when a hydraulic signal detected by the hydraulic sensor is qualified; the gas heating device heats the inert gas so as to heat the pyrolysis oil separated out from the condensation pipe by using the heated inert gas, so that the pyrolysis oil is heated and volatilized to form second pyrolysis gas; the mass spectrometer analyzes the composition and mass of the first pygas and the composition of the second pygas. Therefore, the scheme can effectively improve the analysis accuracy of the pyrolysis tri-state products at different pyrolysis temperature stages.
Drawings
In order to more clearly illustrate the embodiments of the present specification or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the description below are some embodiments of the present specification, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural diagram of an analysis system for pyrolysis tri-state products provided in an embodiment of the present specification.
Reference numerals are as follows:
1-a tabletting device;
2-an infrared heating device;
21-a housing;
22-infrared heating pipes;
23-a reactor;
231-end portion;
241-a flange;
242-a slide rail;
25-a support frame;
26-graphite crucible;
27-a pressure relief line;
28-pressure gauge;
29-relief valve;
3-an air intake device;
4-a cooling pipe;
41-air compressor;
5-a condensation pipe group;
51-a condenser tube;
6-a weighing device;
61-a box body;
62-a hydraulic pressure sensor;
63-a pressure sensor;
7-gas heating means;
71-a PI regulator;
8-a mass spectrometry device;
81-an adsorption device;
9-a refrigeration device;
91-a refrigerant fluid;
92-drain valve.
Detailed Description
To make the purpose, technical solutions and advantages of the embodiments of the present specification clearer and more complete, the technical solutions in the embodiments of the present specification will be described below with reference to the drawings in the embodiments of the present specification, and it is obvious that the described embodiments are part of the embodiments of the present specification, rather than all of the embodiments, and all other embodiments obtained by a person having ordinary skill in the art without making creative efforts based on the embodiments in the present specification belong to the protection scope of the present specification.
Fig. 1 is a schematic structural diagram of an analysis system for pyrolysis tri-state products provided in an embodiment of the present specification. As shown in fig. 1, the system for analyzing pyrolysis tri-state products comprises:
the tabletting device 1 is used for carrying out tabletting treatment on the solid waste to be pyrolyzed to obtain tablets to be pyrolyzed;
the infrared heating device 2 is used for heating the tabletting to be pyrolyzed by utilizing infrared rays according to a preset temperature rising condition to obtain an oil-gas mixture and pyrolytic coke; wherein the mass of the pyrolytic coke is measured by an external balance;
the air inlet device 3 is connected with the infrared heating device 2 and is used for providing inert gas for the infrared heating device 2 so as to blow the oil-gas mixture out of the infrared heating device 2 by using the inert gas; wherein the inert gas does not include nitrogen;
the cooling pipe 4 is connected with the infrared heating device 2, and the cooling pipe 4 is used for cooling the temperature of the oil-gas mixture so as to reduce the secondary reaction of the oil-gas mixture;
the condensation pipe group 5 comprises a plurality of groups of condensation pipes 51, each group of condensation pipes 51 is connected with the cooling pipe 4, and the condensation pipes 51 are used for condensing the cooled oil-gas mixture to obtain first pyrolysis gas and pyrolysis oil; wherein, the heating temperatures of the tablets to be pyrolyzed corresponding to different condensing pipes 51 are different;
the weighing device 6 comprises a box body 61, a hydraulic sensor 62 arranged on the inner side of the bottom wall of the box body 61 and a pressure sensor 63 arranged on the outer side of the bottom wall of the box body 61, wherein the condensation pipe group 5 is arranged in the box body 61, a refrigerant 91 is arranged in the box body 61, the refrigerant 91 is used for providing cold energy for the condensation pipe group 5, and the pressure sensor 63 is used for measuring the quality of pyrolysis oil when a hydraulic signal detected by the hydraulic sensor 62 is qualified;
the gas heating device 7 is respectively connected with each group of the condensation pipes 51 and the gas inlet device 3, and the gas heating device 7 is used for heating the inert gas so as to heat the pyrolysis oil separated out from the condensation pipes 51 by using the heated inert gas, so that the pyrolysis oil is heated and volatilized to form second pyrolysis gas;
and the mass spectrum analysis device 8 is respectively connected with each group of the condensation pipes 51, and the mass spectrum analysis device 8 is used for analyzing the components and the mass of the first pyrolysis gas and the components of the second pyrolysis gas.
Each of the devices will be described below.
< tableting apparatus 1>
Since the principle of heating the solid waste in the embodiment of the present specification adopts infrared rays, in order to ensure the heating efficiency, the solid waste can be subjected to tabletting treatment, that is, the solid waste to be pyrolyzed (for example, medical waste) is subjected to tabletting treatment by arranging the tabletting device 1, so as to obtain the tablet to be pyrolyzed.
In some embodiments, the resulting thickness of the tablet to be pyrolyzed is about 5mm, e.g., 4mm to 6mm.
In specific operation, the pressing device 1 comprises a tablet press and a die, the solid waste to be pyrolyzed is firstly spread in the die, then the solid waste to be pyrolyzed is put into the tablet press, and the solid waste is manually pressurized to 20Mpa, so that the tablet to be pyrolyzed can be obtained.
< Infrared heating device 2>
In the related technology, the mode of heating the to-be-pyrolyzed solid waste generally adopts resistance wire heating, and the heating rate is generally limited within 50 ℃/min. And the solid waste to be pyrolyzed has different components and qualities of pyrolysis products under the conditions of different temperature rising rates. However, the range of the temperature increase rate of the related art is small, and it is difficult to explore the intrinsic pyrolysis mechanism thereof.
In this embodiment, treat the pyrolysis preforming and heat according to predetermined intensification condition through setting up infrared heating device 2 utilizing the infrared ray, obtain oil-gas mixture and pyrolysis coke. The heating rate of the infrared heating mode can reach 6000 ℃/min at the fastest speed, pyrolysis of materials under wide heating rate can be achieved, more possibilities are provided for scientific research in the field of pyrolysis, and therefore a more comprehensive pyrolysis mechanism can be explored (namely gas generation and content change in the whole stage in the pyrolysis process are monitored, and the method is greatly helpful for analyzing the fracture mechanism of chemical bonds after solid waste to be pyrolyzed is heated).
Wherein the mass of the pyrolytic coke is measured by an external balance. That is, after the pyrolysis of the thermally decomposed pellet is completed, the yield of the pyrolytic coke is obtained by calculating the mass difference of the graphite crucible 26 before and after the pyrolysis (i.e., the mass of the graphite crucible 26 after the pyrolysis minus the mass of the blank graphite crucible 26).
In one embodiment of the present disclosure, the infrared heating device 2 includes a housing 21, an annular infrared heating pipe 22 disposed in the housing 21, a reactor 23 disposed in the infrared heating pipe 22, a flange 241 detachably connected to the reactor 23, a support 25 connected to the flange 241 and extending into the reactor 23, a graphite crucible 26 connected to the support 25, and a thermocouple for detecting a temperature of the graphite crucible 26, an inert gas provided by the gas inlet device 3 is introduced into the reactor 23, an end 231 of the reactor 23 far away from the flange 241 is in a conical structure, and the end 231 is connected to the cooling pipe 4.
In the related art, due to the structural limitation of the reactor 23 (that is, the design of abrupt change of the caliber of the pipeline is adopted at the end of the conventional reactor), a large amount of pyrolysis oil is condensed at the wall surface of the reactor in the pyrolysis experiment, so that the pyrolysis oil is not fully collected, and the yield of the pyrolysis oil is inaccurately measured.
In the present embodiment, by providing the end 231 of the reactor 23 away from the flange 241 with a tapered structure, condensation of pyrolysis oil at the end of the reactor can be greatly reduced, thereby improving the measurement of the yield of pyrolysis oil.
In one embodiment of the present specification, the infrared ray generated by the infrared heating tube 22 is a short wave infrared ray, and the outer surface of the graphite crucible 26 is coated with a light absorbing material that absorbs the short wave infrared ray.
In this embodiment, by coating the outer surface of the graphite crucible 26 with a light absorbing material that absorbs short-wave infrared rays, it is possible to achieve rapid heat transfer to the thermal preform even at 300 ℃ or less, and thus uniform heat transfer in the entire temperature range can be achieved.
In one embodiment of the present disclosure, a slide rail 242 connected to the housing 21 is further included, the flange 241 is connected to the slide rail 242, and the flange 241 is sealed or separated from the reactor 23 by sliding the flange 241 on the slide rail 242.
In this embodiment, the flange 241 is advantageously sealed or separated from the reactor 23 by providing a slide rail 242 connected to the housing 21.
In an embodiment of the present specification, the reactor further includes a pressure relief pipeline 27, and a pressure gauge 28 and a pressure relief valve 29 that are disposed on the pressure relief pipeline 27, the pressure relief pipeline 27 is connected to the flange 241, when the flange 241 is fixed to the reactor 23, the pressure relief pipeline 27 is communicated with the inside of the reactor 23, the pressure gauge 28 is configured to detect the gas pressure in the reactor 23, and the pressure relief valve 29 is configured to relieve the pressure in the reactor 23 after the gas pressure in the reactor 23 reaches a preset pressure.
In the embodiment, the pressure gauge 28 is arranged to detect the gas pressure in the reactor 23, so that the gas tightness of the whole system can be detected based on the detected gas pressure, and the gas pressure in the reactor 23 can be monitored in real time to reduce the overhigh pressure caused by blockage, thereby improving the safety coefficient; by providing the relief valve 29, it can be ensured that the gas pressure in the reactor 23 is not excessively high even if the gas pressure in the reactor 23 is increased.
Of course, the infrared heating device 2 further comprises elements such as a control panel, a temperature display, a power switch and a controller, so that the infrared heating device 2 can automatically work according to a preset program, and the convenience of the experiment is greatly improved.
< air intake device 3>
Since the mass spectrometer 8 is based on the principle of analyzing the molecular weight of the gas, nitrogen and carbon monoxide cannot be distinguished by the mass spectrometer 8, and in order to solve this problem, it is considered that the inert gas supplied from the air inlet unit 3 to the infrared heating unit 2 is argon or the like.
< Cooling tube 4>
Since the oil-gas mixture generated by pyrolysis may itself undergo secondary reactions in the heating zone, the secondary reactions are more likely to occur if the tip (i.e., the end 231) of the reactor 23 is also designed with a sharp opening. When the oil-gas mixture undergoes a secondary reaction, the product analyzed by the mass spectrometer 8 is not a nascent reaction product, which affects the trend of the overall experimental conclusion.
In order to solve this problem, it is conceivable to provide a cooling pipe 4 at the end of the reactor 23 to cool the temperature of the oil-gas mixture, so that secondary reactions of the oil-gas mixture itself can be reduced.
In some embodiments, the temperature of the cooling pipe 4 is 100-200 ℃, so that the temperature of the oil-gas mixture generated by pyrolysis can be immediately reduced to be below the temperature point of the secondary reaction after leaving the heating zone, and thus, the proportion of the pyrolysis nascent state reaction product can be increased, and the accuracy of the overall experimental conclusion can be favorably ensured.
In one embodiment of the present specification, an air compressor 41 is further included, and the air compressor 41 is connected to the cooling pipe 4 and is used for supplying compressed air to the outer wall surface of the cooling pipe 4 to cool the air-fuel mixture flowing through the cooling pipe 4.
In this embodiment, the cooling tube 4 is cooled by air cooling, since the cooling temperature of the cooling tube 4 may be lower than 100 ℃ due to the liquid cooling, and the lower than 100 ℃ may cause partial components to condense on the wall surface of the cooling tube 4, which is also disadvantageous.
< condensation tube group 5>
In one embodiment of the present disclosure, each set of condensation tubes 51 is disposed in the tank 61 in a spiral structure.
In this embodiment, the portions of the condensing pipes 51 in the box 61 are all set to be helical structures, so that some components in the oil-gas mixture can be effectively condensed.
In one embodiment of the present specification, the refrigeration device 9 and the liquid discharge valve 92 are further included, the refrigeration device 9 is communicated with the box body 61, and the refrigeration liquid 91 circularly flows along the box body 61 and the refrigeration device 9;
the drain valve 92 is provided at the bottom of the tank 61, and the drain valve 92 is opened before the gas heating device 7 heats the condenser pipe 51 to discharge the refrigerant liquid 91 in the tank 61.
In this embodiment, by providing the refrigerating device 9 and the drain valve 92, on-line analysis of the yield and composition of pyrolysis oil (i.e., weighing and analysis are performed separately without detaching the condensation tube group 5 from the system) can be realized.
Wherein, a circulating pump is arranged in the refrigerating device 9, and the refrigerant fluid 91 can circularly flow along the box body 61 and the refrigerating device 9 through the circulating pump.
To ensure that the components of the oil and gas mixture may be completely condensed, in some embodiments, the temperature of the condensate 91 may need to be controlled to be no higher than-40 ℃.
The first pyrolysis gas is noncondensable gas in the oil-gas mixture, such as nitrogen, hydrogen, carbon monoxide, carbon dioxide, and the like. The second pyrolysis gas is generated by heating and volatilizing the pyrolysis oil, most of the second pyrolysis gas is hydrocarbon, and the molecular weight of the second pyrolysis gas is usually within 5000, so that the components and the mass of the first pyrolysis gas and the components of the second pyrolysis gas can be analyzed through the mass spectrometry device 8. However, since the pyrolysis oil is inevitably free from a high molecular gas having a molecular weight of more than 5000, it is not within the analysis range of the mass spectrometer 8 provided in the examples of the present specification (of course, LC-HRMS may be provided to analyze a gas having a molecular weight of more than 5000). It is for this reason that the mass of the pyrolysis oil cannot be measured by means of the mass spectrometer 8, but by means of the weighing device 6, so that the accuracy of the analysis can be guaranteed.
Referring to fig. 1, for example, the condensation tube set 5 includes four sets of condensation tubes 51, and the temperature setting procedure of the infrared heating device 2 is to heat the initial temperature to 300 ℃ for 5min, and then to heat the initial temperature to 600 ℃ for 5min every 100 ℃. During the temperature rising stage and the heat preservation period, the valve of the corresponding condensation pipe 51 is controlled to be opened and closed by a computer. For example, in the phase of waiting for temperature rise, the computer controls to open the valve of the first condensation pipe 41 and close the valves of the other three condensation pipes 51. And during the heat preservation period at 300 ℃, the valve of the second condensation pipe is opened, the valves of the other three condensation pipes are closed, and the like. Thus, pyrolysis oil with initial temperature of 300 ℃, 300-400 ℃, 400-500 ℃ and 500-600 ℃ is collected by the four sets of condensation pipes 51 respectively at the end of pyrolysis.
In the embodiment, by designing the condensation tube group 5 by means of the concept of "step condensation", the collection of pyrolysis liquid phase products in different pyrolysis stages can be realized, and the method has important significance for the research of pyrolysis mechanisms. Further, the condensation tube group 5 can be optimized to be composed of more condensation tubes 51 (i.e. more than four groups), so that the step condensation of pyrolysis products in more temperature intervals can be realized.
< weighing apparatus 6>
In the related art, the tube bank 5 is weighed in a complicated manner by detaching it from the system and then measuring the mass difference before and after pyrolysis by using a balance, respectively. In order to realize the online measurement of the pyrolysis oil, a hydraulic sensor 62 and a pressure sensor 63 may be considered, and when a hydraulic signal detected by the hydraulic sensor 62 is qualified, the quality of the pyrolysis oil detected by the pressure sensor 63 is the accurate quality of the pyrolysis oil.
It can be understood that the initial value of the pressure sensor 63 is a stable value detected after the refrigeration cycle is turned on before pyrolysis, i.e., the value is used as a zero point for measuring the quality of the pyrolysis oil.
< gas heating apparatus 7>
The gas heating device 7 is used for heating the inert gas to heat the pyrolysis oil separated out from the condensing tube 51 by using the heated inert gas, so that the pyrolysis oil is heated and volatilized to form a second pyrolysis gas. Here, the specific configuration of the gas heating device 7 is not limited and described in detail.
In one embodiment of the present specification, a temperature sensor (not shown) and a PI regulator 71 are further included, the PI regulator 71 is connected to the temperature sensor and the gas heating device 7, the temperature sensor is disposed on a pipeline connected between the condensation tube set 5 and the mass spectrometer 8, and the PI regulator 71 is configured to adjust the heating temperature of the gas heating device 7 according to the temperature detected by the temperature sensor, so as to control the temperature of the pyrolysis gas entering the mass spectrometer 8.
In the present embodiment, since the pyrolysis gas (including the first pyrolysis gas and the second pyrolysis gas) cannot be maintained at a temperature of 100 ℃ or higher before entering the mass spectrometer 8, it is likely to cause condensation of the pyrolysis gas on the inner wall of the piping connected between the condensation tube group 5 and the mass spectrometer 8, which is disadvantageous for analysis of the composition and yield. Therefore, by providing the temperature sensor and the PI regulator 71, the temperature of the pyrolysis gas entering the mass spectrometer 8 can be controlled above a preset temperature (e.g., 100 ℃).
< Mass spectrometer 8>
In the related art, because the pyrolysis gas is usually detected by a gas chromatography device to determine the yield, the gas chromatography device has certain errors in calculating the mass of each gas. Therefore, the embodiment of the present specification considers using the mass spectrometer 8 instead of the gas chromatography device in the related art.
In an embodiment of the present specification, the apparatus further includes an adsorption device 81, the adsorption device 81 is connected to the mass spectrometer 8, and the adsorption device 81 is configured to adsorb the pyrolysis gas analyzed by the mass spectrometer 8.
In this embodiment, by providing the adsorption device 81, the environmental friendliness of the experimental environment can be effectively ensured. In some embodiments, the adsorption device 81 may be provided with activated carbon.
In summary, in the above technical solution, by using the infrared heating tube 22 and the graphite crucible 26 coated with the light absorbing material, the solid waste to be pyrolyzed can be rapidly and uniformly heated; the end 231 of the reactor 23 far away from the flange 241 is in a conical structure and is provided with the cooling pipe 4, so that the oil-gas mixture generated by pyrolysis can be rapidly cooled when leaving the heating zone, and the occurrence of secondary reaction is reduced; the system can realize the accurate measurement of the yield of the gas, liquid and solid ternary products after pyrolysis, and breaks through the limitation that the traditional pyrolysis liquid phase yield is calculated by using a differential method; the system is simple to operate, low in investment and operation cost, and capable of realizing online detection of pyrolysis gas and pyrolysis oil, so that the experiment time of scientific researchers can be greatly shortened, and the scientificity, accuracy and repeatability of experiment results are improved. Therefore, the scheme can effectively improve the analysis accuracy of the pyrolysis ternary products at different pyrolysis temperature stages.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one of 8230" does not exclude the presence of additional like elements in a process, method, article, or apparatus comprising the element.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solutions of the present specification, and not to limit them; although the present description has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the spirit and scope of the technical solutions of the embodiments of the present specification.
Claims (10)
1. An analytical system for pyrolysis of tri-state products, comprising:
the tabletting device (1) is used for carrying out tabletting treatment on solid waste to be pyrolyzed to obtain tablets to be pyrolyzed;
the infrared heating device (2) is used for heating the pressed sheet to be pyrolyzed according to a preset temperature-rising condition by utilizing infrared rays to obtain an oil-gas mixture and pyrolytic coke; wherein the mass of the pyrolytic coke is measured by an external balance;
the air inlet device (3) is connected with the infrared heating device (2) and is used for providing inert gas for the infrared heating device (2) so as to blow the oil-gas mixture out of the infrared heating device (2) by using the inert gas; wherein the inert gas does not include nitrogen;
the cooling pipe (4) is connected with the infrared heating device (2), and the cooling pipe (4) is used for cooling the temperature of the oil-gas mixture so as to reduce the occurrence of secondary reaction of the oil-gas mixture;
the condensation pipe group (5) comprises a plurality of groups of condensation pipes (51), each group of condensation pipes (51) is connected with the cooling pipe (4), and the condensation pipes (51) are used for condensing the cooled oil-gas mixture to obtain first pyrolysis gas and pyrolysis oil; wherein the heating temperatures of the tablets to be pyrolyzed corresponding to different condensing pipes (51) are different;
the weighing device (6) comprises a box body (61), a hydraulic sensor (62) arranged on the inner side of the bottom wall of the box body (61) and a pressure sensor (63) arranged on the outer side of the bottom wall of the box body (61), the condensation pipe group (5) is arranged in the box body (61), a refrigerant liquid (91) is arranged in the box body (61), the refrigerant liquid (91) is used for providing cold energy for the condensation pipe group (5), and the pressure sensor (63) is used for measuring the quality of the pyrolysis oil when a hydraulic signal detected by the hydraulic sensor (62) is qualified;
the gas heating device (7) is respectively connected with each group of the condensation pipes (51) and the gas inlet device (3), and the gas heating device (7) is used for heating the inert gas so as to heat the pyrolysis oil separated out from the condensation pipes (51) by using the heated inert gas, so that the pyrolysis oil is heated and volatilized to form second pyrolysis gas;
and the mass spectrum analysis device (8) is respectively connected with each group of the condensation pipes (51), and the mass spectrum analysis device (8) is used for analyzing the components and the mass of the first pyrolysis gas and the components of the second pyrolysis gas.
2. The analytical system for three-state products of pyrolysis according to claim 1, wherein the infrared heating device (2) comprises a housing (21), an infrared heating tube (22) arranged in the housing (21) and in a ring shape, a reactor (23) arranged in the infrared heating tube (22), a flange (241) detachably connected with the reactor (23), a support frame (25) connected with the flange (241) and extending into the reactor (23), a graphite crucible (26) connected with the support frame (25), and a thermocouple for detecting the temperature of the graphite crucible (26), wherein the inert gas provided by the gas inlet device (3) is introduced into the reactor (23), the end (231) of the reactor (23) far away from the flange (241) is in a conical structure, and the end (231) is connected with the cooling tube (4).
3. The analytical system for three-state products of pyrolysis according to claim 2, wherein the infrared ray generated by the infrared heating tube (22) is short wave infrared ray, and the outer surface of the graphite crucible (26) is coated with a light absorbing material absorbing the short wave infrared ray.
4. A system for analyzing tri-state products of pyrolysis according to claim 2, further comprising a slide rail (242) connected with the housing (21), wherein the flange (241) is connected with the slide rail (242), and the flange (241) is sealed or separated from the reactor (23) by the sliding of the flange (241) on the slide rail (242).
5. The analysis system for the three-state product of pyrolysis according to claim 2, further comprising a pressure relief pipeline (27), and a pressure gauge (28) and a pressure relief valve (29) which are arranged on the pressure relief pipeline (27), wherein the pressure relief pipeline (27) is connected with the flange (241), when the flange (241) is fixed with the reactor (23), the pressure relief pipeline (27) is communicated with the inside of the reactor (23), the pressure gauge (28) is used for detecting the gas pressure in the reactor (23), and the pressure relief valve (29) is used for relieving the pressure of the reactor (23) after the gas pressure in the reactor (23) reaches a preset pressure.
6. A system for analyzing three-state products of pyrolysis according to any one of claims 1-5, further comprising an air compressor (41), wherein the air compressor (41) is connected with the cooling pipe (4) and is used for providing compressed air to the outer wall surface of the cooling pipe (4) so as to cool the oil-gas mixture flowing through the cooling pipe (4).
7. A system for analyzing three-state products of pyrolysis according to any one of claims 1-5, characterized in that the part of each set of the condensation pipes (51) in the box body (61) is in a spiral structure.
8. The system for analyzing three-state products of pyrolysis according to any one of claims 1-5, further comprising a refrigerating device (9) and a drain valve (92), wherein the refrigerating device (9) is communicated with the box body (61), and the refrigerating fluid (91) circulates along the box body (61) and the refrigerating device (9);
the drain valve (92) is disposed at the bottom of the tank (61), and the drain valve (92) is opened before the gas heating device (7) heats the condenser tube (51) to discharge the refrigerant liquid (91) in the tank (61).
9. A system for analyzing tri-state products of pyrolysis according to any one of claims 1-5, further comprising a temperature sensor and a PI regulator (71), wherein the PI regulator (71) is connected with the temperature sensor and the gas heating device (7) respectively, the temperature sensor is arranged on a pipeline connected between the condensation pipe group (5) and the mass spectrometry device (8), and the PI regulator (71) is used for regulating the heating temperature of the gas heating device (7) according to the temperature detected by the temperature sensor so as to control the temperature of pyrolysis gas entering the mass spectrometry device (8).
10. A pyrolysis three-state product analysis system according to any one of claims 1-5, further comprising an adsorption device (81), wherein the adsorption device (81) is connected with the mass spectrometry device (8), and the adsorption device (81) is used for adsorbing the pyrolysis gas analyzed by the mass spectrometry device (8).
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