CN115326910B - Analysis system for pyrolysis tri-state products - Google Patents
Analysis system for pyrolysis tri-state products Download PDFInfo
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- CN115326910B CN115326910B CN202210793883.0A CN202210793883A CN115326910B CN 115326910 B CN115326910 B CN 115326910B CN 202210793883 A CN202210793883 A CN 202210793883A CN 115326910 B CN115326910 B CN 115326910B
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- 238000004458 analytical method Methods 0.000 title claims abstract description 30
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- 238000010438 heat treatment Methods 0.000 claims abstract description 95
- 239000000203 mixture Substances 0.000 claims abstract description 42
- 238000001816 cooling Methods 0.000 claims abstract description 39
- 239000011261 inert gas Substances 0.000 claims abstract description 28
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 21
- 239000002910 solid waste Substances 0.000 claims abstract description 19
- 238000005303 weighing Methods 0.000 claims abstract description 11
- 239000000571 coke Substances 0.000 claims abstract description 9
- 238000009833 condensation Methods 0.000 claims description 23
- 230000005494 condensation Effects 0.000 claims description 23
- 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
- 238000001179 sorption measurement Methods 0.000 claims description 11
- 239000012530 fluid Substances 0.000 claims description 10
- 238000001819 mass spectrum Methods 0.000 claims description 10
- 238000010517 secondary reaction Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000005057 refrigeration Methods 0.000 claims description 6
- 239000011358 absorbing material Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000004891 communication Methods 0.000 claims description 2
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- 238000002474 experimental method Methods 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
- 238000010586 diagram Methods 0.000 description 2
- 239000002906 medical waste Substances 0.000 description 2
- 239000010813 municipal solid waste Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000003507 refrigerant Substances 0.000 description 2
- 230000001105 regulatory effect 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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- 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
- G01N1/42—Low-temperature sample treatment, e.g. cryofixation
-
- 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
-
- 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
-
- 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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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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Abstract
The specification relates to pyrolysis technical field, especially relates to an analysis system of pyrolysis tristate product. The system comprises a tabletting device, an infrared heating device, an air inlet device, a cooling pipe, a condensing pipe group, a weighing device, a gas heating device and a mass spectrometry device, wherein the tabletting device carries out tabletting treatment on solid waste to be pyrolyzed to obtain tablets to be pyrolyzed, and the infrared heating device heats the tablets to be pyrolyzed by utilizing infrared rays to obtain an oil-gas mixture and pyrolysis coke; the air inlet device supplies inert gas to 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 so as to volatilize pyrolysis oil to form second pyrolysis gas; the mass spectrometry device analyzes the composition, mass, and composition of the first 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 waste (such as medical waste) into pyrolysis coke, pyrolysis oil and pyrolysis gas, and pyrolysis oil gas products can be introduced into a garbage incinerator to burn and recover heat, so that the coupling heat treatment of the solid waste in a household garbage incineration power plant is promoted. Thus, 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 pyrolysis solid waste, it is necessary to analyze not only the yields of pyrolysis tri-state products of typical solid waste under different pyrolysis conditions, but also the components of the gas phase (i.e., pyrolysis gas) and the liquid phase (i.e., pyrolysis oil) in the pyrolysis tri-state products at different pyrolysis temperature stages. However, the accuracy of analysis of pyrolysis tri-state products at different pyrolysis temperature stages is not high by the related art.
Accordingly, there is a need for an analysis system for pyrolysis tristate products to solve the above-mentioned problems.
Disclosure of Invention
In order to effectively improve analysis accuracy of pyrolysis tri-state products at different pyrolysis temperature stages, the embodiment of the specification provides an analysis system of pyrolysis tri-state products.
Embodiments of the present disclosure provide an analysis system for pyrolyzing a tri-state product, comprising:
the tabletting device is used for tabletting the solid waste to be pyrolyzed to obtain tablets to be pyrolyzed;
the infrared heating device is used for heating the tablet to be pyrolyzed by utilizing infrared rays according to preset heating conditions to obtain an oil-gas mixture and pyrolysis coke; wherein the mass of the pyrolytic focus is measured by an external balance;
the air inlet device is connected with the infrared heating device and is 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 is used for cooling the temperature of the oil-gas mixture so as to reduce secondary reaction of the oil-gas mixture;
the condensing tube group comprises a plurality of groups of condensing tubes, each group of condensing tubes is connected with the cooling tube, and the condensing tubes 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 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, a refrigerating fluid is arranged in the box body and is 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 is respectively connected with each group of the condensing pipes and the gas inlet device and is used for heating the inert gas so as to heat pyrolysis oil separated out from the condensing 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 condensing 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 one possible design, the infrared heating device comprises a shell, an infrared heating pipe which is arranged in the shell and is annular, a reactor which is arranged in the infrared heating pipe, a flange which is detachably connected with the reactor, a support frame which is connected with the flange and stretches into the reactor, a graphite crucible which is connected with the support frame, and a thermocouple which is used for detecting the temperature of the graphite crucible, wherein inert gas provided by the air inlet device is introduced into the reactor, the end part of the reactor, which is far away from the flange, is in a conical structure, and the end part is connected with the cooling pipe.
In one possible design, the infrared rays generated by the infrared heating tube are short-wave infrared rays, and the outer surface of the graphite crucible is coated with a light absorbing material for absorbing the short-wave infrared rays.
In one possible design, the reactor further comprises a sliding rail connected with the shell, the flange is connected with the sliding rail, and the flange is sealed or separated from the reactor through sliding of the flange on the sliding rail.
In one possible design, the pressure release device further comprises a pressure release pipeline, a pressure gauge and a pressure release valve, wherein the pressure gauge and the pressure release valve are arranged on the pressure release pipeline, the pressure release pipeline is connected with the flange, when the flange is fixed with the reactor, the pressure release pipeline is communicated with the inside of the reactor, the pressure gauge is used for detecting the gas pressure in the reactor, and the pressure release valve is used for releasing the pressure of the gas in the reactor after the gas pressure in the reactor reaches the preset pressure.
In one possible design, the cooling system further comprises an air compressor connected with the cooling pipe for supplying compressed air to the outer wall surface of the cooling pipe to cool the oil-gas mixture flowing through the cooling pipe.
In one possible design, the portion 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 is opened before the condensing tube is heated by the gas heating device so as to discharge the refrigerating fluid in the box body.
In one possible design, the device further comprises a temperature sensor and a PI regulator, wherein 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 spectrum analysis 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 pyrolysis gas entering the mass spectrum analysis device.
In one possible design, the device further comprises an adsorption device, wherein the adsorption device is connected with the mass spectrum analysis device and is used for adsorbing pyrolysis gas analyzed by the mass spectrum analysis device.
The embodiment of the specification provides an analysis system for pyrolysis tri-state products, wherein a tabletting device carries out tabletting treatment on solid waste to be pyrolyzed to obtain tablets to be pyrolyzed; the infrared heating device heats the to-be-pyrolyzed tablet by utilizing infrared rays according to preset heating conditions 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 supplies inert gas to 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 comprise nitrogen; the cooling pipe cools the temperature of the oil-gas mixture to reduce secondary reaction of the oil-gas mixture, so that the product analyzed by the mass spectrum analysis device can be ensured to be 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 to-be-pyrolyzed tablets 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, the condensing tube group is arranged in the box body, refrigerating fluid is arranged in the box body and used for providing cold energy for the condensing tube 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 pyrolysis oil separated out from the condensing tube by utilizing the heated inert gas, so that the pyrolysis oil is heated and volatilized to form second pyrolysis gas; the mass spectrometry device analyzes the composition, mass, and composition of the first pyrolysis gas. Therefore, the analysis accuracy of pyrolysis tri-state products at different pyrolysis temperature stages can be effectively improved by the scheme.
Drawings
In order to more clearly illustrate the embodiments of the present description or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are some embodiments of the present description, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an analysis system for pyrolysis tri-state products according to an embodiment of the present disclosure.
Reference numerals:
1-a tabletting device;
2-an infrared heating device;
21-a housing;
22-infrared heating pipes;
a 23-reactor;
231-end;
241-flange;
242-slide rail;
25-supporting frames;
26-graphite crucible;
27-a pressure relief pipeline;
28-pressure gauge;
29-a pressure relief valve;
3-an air intake device;
4-cooling pipes;
41-an air compressor;
5-condensing tube group;
51-a condenser tube;
6-a weighing device;
61-a box body;
62-a hydraulic sensor;
63-a pressure sensor;
7-a gas heating device;
71-PI regulator;
8-mass spectrometry;
81-an adsorption device;
9-a refrigeration device;
91-refrigerating fluid;
92-drain valve.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present specification more apparent, the technical solutions of the embodiments of the present specification will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present specification, and it is apparent that the described embodiments are some, but not all, embodiments of the present specification, and all other embodiments obtained by persons of ordinary skill in the art without making any inventive effort based on the embodiments of the present specification are within the scope of protection of the present specification.
FIG. 1 is a schematic diagram of an analysis system for pyrolysis tri-state products according to an embodiment of the present disclosure. As shown in fig. 1, the analysis system of pyrolysis tristate products comprises:
the tabletting device 1 is used for tabletting the solid waste to be pyrolyzed to obtain tablets to be pyrolyzed;
the infrared heating device 2 is used for heating the tablet to be pyrolyzed by utilizing infrared rays according to preset heating conditions to obtain an oil-gas mixture and pyrolysis coke; wherein the mass of the pyrolytic focus is measured by an external balance;
an air inlet device 3 connected with the infrared heating device 2 for providing inert gas to 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 secondary reaction of the oil-gas mixture;
the condensing tube group 5 comprises a plurality of groups of condensing tubes 51, each group of condensing tubes 51 is connected with the cooling tube 4, and the condensing tubes 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 refrigerating fluid 91 is arranged in the box body 61, the refrigerating fluid 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 condensing pipes 51 and the gas inlet device 3, and the gas heating device 7 is used for heating inert gas so as to heat pyrolysis oil separated out from the condensing pipes 51 by using the heated inert gas, so that the pyrolysis oil is heated and volatilized to form second pyrolysis gas;
and a mass spectrum analysis device 8 connected to each group of the condensation pipes 51, wherein the mass spectrum analysis device 8 is used for analyzing the components, the mass and the components of the second pyrolysis gas.
Each of the devices is described below.
< tabletting device 1>
Since the principle of heating the solid waste in the embodiment of the present specification adopts infrared rays, in order to ensure heating efficiency, it is considered to perform tabletting treatment on the solid waste, that is, to perform tabletting treatment on solid waste to be pyrolyzed (for example, medical waste) by arranging the tabletting device 1, so as to obtain tablets to be pyrolyzed.
In some embodiments, the resulting tablet to be pyrolyzed has a thickness of about 5mm, for example, 4mm to 6mm.
In a specific operation, the pressure device 1 comprises a tablet press and a die, solid waste to be pyrolyzed is firstly paved in the die, then the solid waste to be pyrolyzed is put into the tablet press, and the solid waste to be pyrolyzed is manually pressurized to 20Mpa, so that the tablet to be pyrolyzed can be obtained.
< Infrared heating device 2>
In the related art, a mode of heating solid waste to be pyrolyzed generally adopts resistance wire heating, and the heating rate is generally limited to be within 50 ℃/min. The solid waste to be pyrolyzed can generate different components and qualities of pyrolysis products under the condition of different heating rates. However, the range of the temperature rising rate of the related art is small, and it is difficult to explore the inherent pyrolysis mechanism thereof.
In the embodiment, the infrared heating device 2 is arranged to heat the to-be-pyrolyzed tablets according to the preset heating conditions by utilizing infrared rays, so as to obtain an oil-gas mixture and pyrolysis coke. The heating rate of the infrared heating mode can reach 6000 ℃/min at the highest speed, pyrolysis under the wide heating rate of materials can be realized, more possibility is provided for scientific research and research in the pyrolysis field, and therefore, a more comprehensive pyrolysis mechanism (namely monitoring gas generation and content change at all stages in the pyrolysis process and greatly helping to analyze the breaking mechanism of chemical bonds after solid waste to be pyrolyzed is heated) can be explored.
Wherein the mass of the pyrolytic focus is measured by an external balance. That is, after the completion of pyrolysis by the pyrolysis tabletting, the yield of pyrolytic coke is obtained by calculating the mass difference of the graphite crucible 26 before and after pyrolysis (i.e., the mass of the graphite crucible 26 after 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 infrared heating tube 22 disposed in the housing 21 and having a ring shape, a reactor 23 disposed in the infrared heating tube 22, a flange 241 detachably connected to the reactor 23, a support frame 25 connected to the flange 241 and extending into the reactor 23, a graphite crucible 26 connected to the support frame 25, and a thermocouple for detecting a temperature of the graphite crucible 26, an inert gas supplied from the gas inlet device 3 is introduced into the reactor 23, an end 231 of the reactor 23 remote from the flange 241 has a tapered structure, and the end 231 is connected to the cooling tube 4.
In the related art, due to the limitation of the structure of the reactor 23 (i.e., the design of abrupt change of the caliber of the pipe at the end of the conventional reactor), a large amount of pyrolysis oil is condensed at the wall of the reactor in the pyrolysis experiment, which results in insufficient collection of the pyrolysis oil and thus inaccurate measurement of the yield of the pyrolysis oil.
In the present embodiment, by disposing the end 231 of the reactor 23 remote from the flange 241 in a tapered configuration, it is possible to greatly reduce the condensation of pyrolysis oil at the end of the reactor, thereby improving the measurement of the yield of pyrolysis oil.
In one embodiment of the present disclosure, the infrared light generated by the infrared heating tube 22 is short wave infrared light, and the outer surface of the graphite crucible 26 is coated with a light absorbing material that absorbs the short wave infrared light.
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 tablet to be pyrolyzed at 300 ℃ or less, so that uniform heat transfer in the full temperature range can be achieved.
In one embodiment of the present disclosure, the apparatus further includes a sliding rail 242 connected to the housing 21, and the flange 241 is connected to the sliding rail 242, such that the flange 241 is sealed or separated from the reactor 23 by sliding the flange 241 on the sliding rail 242.
In this embodiment, sealing or separating the flange 241 from the reactor 23 is facilitated by providing a slide rail 242 connected to the housing 21.
In one embodiment of the present disclosure, the pressure release device further includes a pressure release pipeline 27, and a pressure gauge 28 and a pressure release valve 29 disposed on the pressure release pipeline 27, where the pressure release pipeline 27 is connected to the flange 241, and when the flange 241 is fixed to the reactor 23, the pressure release pipeline 27 is in communication with the interior of the reactor 23, the pressure gauge 28 is used for detecting the gas pressure in the reactor 23, and the pressure release valve 29 is used for releasing the pressure of the reactor 23 after the gas pressure in the reactor 23 reaches the 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 pressure over high caused by blockage, thereby improving the safety coefficient; by providing the relief valve 29, it is 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 a control panel, a temperature display, a power switch, a controller and other elements, so that the infrared heating device 2 automatically works according to a preset program, and the convenience of experiments is greatly improved.
< air intake device 3>
Since the mass spectrometer 8 is based on the principle of analyzing the molecular weight of a gas, nitrogen and carbon monoxide cannot be distinguished by the mass spectrometer 8, and in order to solve this problem, it is conceivable that the inert gas supplied from the gas inlet 3 to the infrared heater 2 is argon or the like.
< Cooling tube 4>
Since the pyrolysis-generated oil and gas mixture may itself undergo secondary reactions in the heating zone, the secondary reactions are more likely to occur if the end of the reactor 23 (i.e., the end 231) is also designed with abrupt openings. When the oil-gas mixture itself undergoes a secondary reaction, the product analyzed by the mass spectrometry device 8 is not a nascent reaction product, which affects the trend of the overall experimental conclusion.
In order to solve this technical problem, it is considered to provide a cooling pipe 4 at the end of the reactor 23 to cool the temperature of the oil-gas mixture, so that the secondary reaction of the oil-gas mixture itself can be reduced.
In some embodiments, the temperature of the cooling tube 4 is 100-200 ℃, so that the oil-gas mixture generated by pyrolysis can be immediately cooled to below the temperature point of secondary reaction after leaving the heating zone, the proportion of pyrolysis nascent reaction products can be improved, and the accuracy of the overall experimental conclusion is guaranteed.
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 for supplying compressed air to the outer wall surface of the cooling pipe 4 to cool the oil-gas mixture flowing through the cooling pipe 4.
In this embodiment, since the liquid cooling may cause the cooling temperature of the cooling tube 4 to be lower than 100 ℃, and the lower than 100 ℃ may cause a part of the components to condense on the wall surface of the cooling tube 4, which is also disadvantageous, the cooling tube 4 is cooled by air cooling.
< condenser tube group 5>
In one embodiment of the present disclosure, the portion of each set of condenser tubes 51 located within the housing 61 is in a helical configuration.
In the present embodiment, by arranging the portion of each group of the condensation pipes 51 located in the tank 61 in a spiral structure, it is possible to effectively condense a part of the components in the oil-gas mixture.
In one embodiment of the present disclosure, the refrigerator further includes a refrigerating device 9 and a drain valve 92, the refrigerating device 9 is communicated with the tank 61, and the refrigerating fluid 91 circulates along the tank 61 and the refrigerating device 9;
a drain valve 92 is provided at the bottom of the tank 61, and the drain valve 92 is opened before the condenser tube 51 is heated by the gas heating device 7 to drain the refrigerant 91 in the tank 61.
In this embodiment, by providing the refrigerating apparatus 9 and the drain valve 92, an on-line analysis of the yield and composition of pyrolysis oil (i.e., weighing and analysis, respectively, without removing the condensation duct set 5 from the system) can be achieved.
The refrigerating apparatus 9 is provided with a circulation pump, and the refrigerant liquid 91 can circulate along the tank 61 and the refrigerating apparatus 9 by the circulation pump.
To ensure that the components of the oil and gas mixture can be fully condensed, in some embodiments, the temperature of the condensate 91 needs to be controlled to be no higher than-40 ℃.
It should be noted that the first pyrolysis gas is non-condensable gas in the oil-gas mixture, such as nitrogen, hydrogen, carbon monoxide, carbon dioxide, and the like. The second pyrolysis gas below is a gas generated by the thermal volatilization of pyrolysis oil, and is mostly hydrocarbon, and its molecular weight is typically less than 5000, so that the components, mass and composition of the first pyrolysis gas can be analyzed by the mass spectrometry device 8. However, since pyrolysis oil inevitably has a high molecular gas having a molecular weight of more than 5000, this is not within the analysis category of the mass spectrometry device 8 provided in the embodiment of the present specification (of course, LC-HRMS may be provided to analyze a gas having a molecular weight of more than 5000). For this reason, the mass of the pyrolysis oil cannot be measured by means of the mass spectrometry device 8, but is measured by the weighing device 6, so that the accuracy of the analysis can be ensured.
With continued reference to fig. 1, for example, the condensing tube set 5 includes four condensing tubes 51, and the temperature program set by the infrared heating device 2 is to raise the initial temperature to 300 ℃ and keep the temperature for 5min, and then keep the temperature for 5min every 100 ℃ until the temperature reaches 600 ℃. During the period to be warmed up and the period to be kept warm, the valve switch of the corresponding condenser tube 51 is controlled by a computer. For example, during the warm-up phase, the computer controls to open the valve of the first condenser tube 41 and close the valves of the other three condenser tubes 51. During the incubation period at 300 ℃, the valve of the second condenser tube was opened, and the valves of the other three condenser tubes were closed, and so on. Thus, at the end of pyrolysis, the four sets of condensation pipes 51 collect pyrolysis oil at an initial temperature of 300 ℃, 300-400 ℃, 400-500 ℃ and 500-600 ℃, respectively.
In the embodiment, by designing the condensation pipe 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 mechanism. Further, the condensation duct group 5 may be continuously optimized to be composed of more condensation ducts 51 (i.e., four or more groups), so that the stepwise condensation of the pyrolysis products may be achieved in more temperature intervals.
< weighing device 6>
In the related art, the condensation tube group 5 is weighed by detaching it from the system, and then the mass difference before and after pyrolysis is measured by using a balance, which is complicated. In order to realize the on-line measurement of the pyrolysis oil, the hydraulic sensor 62 and the pressure sensor 63 may be considered to be provided, and when the hydraulic signal detected by the hydraulic sensor 62 is qualified, the pyrolysis oil quality detected by the pressure sensor 63 is the accurate pyrolysis oil quality.
It is known 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 taken as a zero point for pyrolysis oil mass measurement.
< gas heating device 7>
The gas heating device 7 is used for heating the inert gas, so as to heat the pyrolysis oil separated out from the condensation pipe 51 by using the heated inert gas, and volatilize the pyrolysis oil to form a second pyrolysis gas. The specific configuration of the gas heating device 7 is not limited and will not be described in detail here.
In one embodiment of the present disclosure, the apparatus further includes a temperature sensor (not shown in the drawing) and a PI regulator 71, wherein the PI regulator 71 is connected to the temperature sensor and the gas heating device 7, respectively, and the temperature sensor is disposed on a pipeline connected between the condensation tube set 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 the pyrolysis gas entering the mass spectrometry device 8.
In the present embodiment, since the temperature of 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 spectrometry device 8, it is likely that the pyrolysis gas is caused to condense on the inner wall of the pipe connected between the condensation pipe group 5 and the mass spectrometry device 8, which is disadvantageous for analysis of the components and the yield. Thus, by providing a temperature sensor and PI regulator 71, the temperature of the pyrolysis gas entering the mass spectrometry device 8 can be controlled above a preset temperature (e.g., 100 ℃).
< Mass Spectrometry device 8>
In the related art, since pyrolysis gas is generally detected by a gas chromatography apparatus to determine the yield, the gas chromatography apparatus may have some error in calculating various gas qualities. Accordingly, the present embodiment considers that the mass spectrometry device 8 is used instead of the gas chromatography device in the related art.
In one embodiment of the present disclosure, the apparatus further includes an adsorption device 81, where the adsorption device 81 is connected to the mass spectrometry device 8, and the adsorption device 81 is used for adsorbing the pyrolysis gas analyzed by the mass spectrometry device 8.
In this embodiment, by providing the adsorption device 81, the environmental protection of the experimental environment can be effectively ensured. In some embodiments, the adsorption device 81 may be provided with activated carbon.
In summary, the above technical solution can realize rapid and uniform heating of solid waste to be pyrolyzed by adopting the infrared heating tube 22 and the graphite crucible 26 coated with the light absorbing material; by arranging the conical structure of the end 231 of the reactor 23 far away from the flange 241 and the cooling pipe 4, the oil-gas mixture generated by pyrolysis can be rapidly cooled down when leaving the heating zone, so that the occurrence of secondary reaction is reduced; the system can accurately measure the yields of gas, liquid and solid tri-state products after pyrolysis, and breaks through the limitation that the traditional pyrolysis liquid phase yield is obtained by using a subtraction method; the system is simple to operate, low in investment and running cost, and capable of simultaneously realizing on-line detection of pyrolysis gas and pyrolysis oil, so that the experiment time of scientific research workers can be greatly reduced, and the scientificity, accuracy and repeatability of an experiment result are improved. Therefore, the scheme can effectively improve the analysis accuracy of pyrolysis tri-state products at different pyrolysis temperature stages.
It is noted that relational terms such as first and second, and the like, are 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. Moreover, 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 …" does not exclude the presence of additional identical elements in a process, method, article or apparatus that comprises the element.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present specification, and are not limiting thereof; although the present specification 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 scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present specification.
Claims (10)
1. An analysis system for pyrolysis tristate products, comprising:
the tabletting device (1) is used for tabletting the solid waste to be pyrolyzed to obtain tablets to be pyrolyzed;
the infrared heating device (2) is used for heating the tablet to be pyrolyzed by utilizing infrared rays according to preset heating conditions to obtain an oil-gas mixture and pyrolysis coke; wherein the mass of the pyrolytic focus is measured by an external balance;
an air inlet device (3) connected with the infrared heating device (2) and 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 utilizing 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 secondary reaction of the oil-gas mixture;
the condensing tube group (5) comprises a plurality of groups of condensing tubes (51), each group of condensing tubes (51) is connected with the cooling tube (4), and the condensing tubes (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 tube group (5) is arranged in the box body (61), refrigerating fluid (91) is arranged in the box body (61), the refrigerating fluid (91) is used for providing cold energy for the condensation tube 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 condensing 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 pyrolysis oil separated out from the condensing 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 condensing pipes (51), and the mass spectrum analysis device (8) is used for analyzing the components, the mass and the components of the second pyrolysis gas.
2. The analysis system of pyrolysis tristate products according to claim 1, characterized in that the infrared heating device (2) comprises a shell (21), an infrared heating pipe (22) which is arranged in the shell (21) and is annular, a reactor (23) which is arranged in the infrared heating pipe (22), a flange (241) which is detachably connected with the reactor (23), a support frame (25) which is connected with the flange (241) and stretches into the reactor (23), a graphite crucible (26) which is connected with the support frame (25) and a thermocouple which is used for detecting the temperature of the graphite crucible (26), inert gas provided by the gas inlet device (3) is introduced into the reactor (23), an end part (231) of the reactor (23) which is far away from the flange (241) is in a conical structure, and the end part (231) is connected with the cooling pipe (4).
3. The analysis system of pyrolysis tri-state products according to claim 2, characterized in that the infrared rays generated by the infrared heating tube (22) are short wave infrared rays, and the outer surface of the graphite crucible (26) is coated with a light absorbing material absorbing the short wave infrared rays.
4. The system for analyzing pyrolysis tristate products according to claim 2, further comprising a sliding rail (242) connected to the housing (21), the flange (241) being connected to the sliding rail (242), the flange (241) being sealed or separated from the reactor (23) by sliding of the flange (241) on the sliding rail (242).
5. The analysis system of pyrolysis tristate products according to claim 2, further comprising a pressure relief pipeline (27), 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), the pressure relief pipeline (27) is communicated with the inside of the reactor (23) when the flange (241) is fixed with 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. The analysis system of pyrolysis tri-state products according to any of the claims 1-5, further comprising an air compressor (41), said air compressor (41) being connected to the cooling pipe (4) for providing compressed air to the outer wall surface of the cooling pipe (4) for cooling the oil-gas mixture flowing through the cooling pipe (4).
7. The analysis system of pyrolysis tri-state products according to any of the claims 1 to 5, characterized in that the portion of each set of condensation tubes (51) located inside the tank (61) is of a spiral structure.
8. The analysis system of pyrolysis tri-state products according to any one of claims 1 to 5, further comprising a refrigeration device (9) and a drain valve (92), the refrigeration device (9) being in communication with the tank (61), the refrigeration liquid (91) circulating along the tank (61) and the refrigeration device (9);
the liquid discharge valve (92) is arranged at the bottom of the box body (61), and the liquid discharge valve (92) is opened before the condensing tube (51) is heated by the gas heating device (7) so as to discharge the refrigerating fluid (91) in the box body (61).
9. The analysis system of pyrolysis tri-state products according to any one of claims 1-5, further comprising a temperature sensor and a PI regulator (71), the PI regulator (71) being connected to the temperature sensor and the gas heating means (7), respectively, the temperature sensor being arranged on a line connected between the condensing tube group (5) and the mass spectrometry means (8), the PI regulator (71) being adapted to regulate the heating temperature of the gas heating means (7) in dependence of the temperature detected by the temperature sensor for controlling the temperature of the pyrolysis gas entering the mass spectrometry means (8).
10. The analysis system of pyrolysis tri-state products according to any of the claims 1-5, further comprising an adsorption device (81), the adsorption device (81) being connected to the mass spectrometry device (8), the adsorption device (81) being adapted to adsorb pyrolysis gas after analysis by the mass spectrometry device (8).
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