A three-phase experimental system for lubricating grease combustion / coking / carbon deposition research

CN117630103BActive Publication Date: 2026-10-30TIANJIN UNIV
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Patent Information

Application Number
CN202311622142.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-11-30
Publication Date
2026-10-30
Estimated Expiration
2043-11-30

AI Technical Summary

Technical Problem

[0006]目前,常用实验设备及其附属的制备、进样设备,尚不能满足上述需要,但具体的实验研究和工程实践已对不同温度、压力条件下润滑油脂的固、液、气三态均相反应过程,及相应的结焦和积碳过程提出了需要

Benefits of technology

[0022]本发明通过预实验设备可实现完整的预实验,以监测润滑油脂的完整沸程和反应历程,并明确所对应的温度和压力条件。

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a three-phase experimental system for lubricating grease combustion / coking / carbon deposition research, which comprises pre-experiment equipment, reactant preparation / separation equipment and a flow tube reactor group; the pre-experiment equipment comprises a jet stirring reactor, a sample inlet pipeline and an exhaust pipeline; the jet stirring reactor is internally provided with two symmetrical nozzles; the reactant preparation / separation equipment comprises a liquid-gas two-phase heating cabin, a baffle type liquid-gas separator and a gasification tank; the liquid-gas two-phase heating cabin comprises a cabinet, a top cover and a glass observation window, and the glass observation window can effectively observe a liquid-gas interface; a carrier gas inlet and an outlet are inserted into the top of the gasification tank, and the bottom of the gasification tank is connected with the flow tube reactor group. The application can prepare different phase reactants, can separate different phase reactants, and can realize pyrolysis, oxidation, coking and carbon deposition process research of different phase lubricating greases under different temperature and pressure conditions.
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Description

Technical Field

[0001] This invention belongs to the field of burners (F23D) and relates to a combination of two or more burners (F23D23 / 00). In particular, it relates to a multifunctional combustion experimental device that uses a flow tube reactor and a jet stirring reactor to study the combustion, coking, and carbon deposition processes of lubricating oil and grease under three homogeneous phases of gas, liquid, and solid. Background Technology

[0002] Combustion science aims to study the physical and chemical processes, organization, and coupling processes of fuels, oxidizers, alternative fuels, or other forms of combustible substances undergoing intense chemical reactions accompanied by heat and light emission. In recent years, combustion science has evolved from a traditional empirical science into a complex system discipline encompassing a wide range of aspects, rich in content, and considering the coupling effects of multiple factors. It involves thermodynamics, fluid mechanics, chemical reaction kinetics, heat and mass transfer, physics, and fundamental mathematics. Combustion science primarily focuses on the pyrolysis (also known as thermal cracking), oxidation, and flame processes of experimental subjects such as fuels. Experimental indicators include combustion products, ignition delay time, and flame morphology. With the deepening of reaction kinetic research, some newer studies are beginning to focus on the coking and carbon deposition processes of fuels, with corresponding measurement indicators including coke / carbon deposition quality and coke morphology.

[0003] Depending on the reaction system, combustion science studies a wide range of systems, including solid-state homogeneous reaction systems, liquid-state homogeneous reaction systems, gas-state homogeneous reaction systems, gas-liquid two-phase reaction systems, solid-liquid two-phase reaction systems, and gas-solid-liquid three-phase reaction systems. Due to limitations in experimental and detection equipment, current experimental research primarily focuses on homogeneous reaction systems, and this research is relatively in-depth. Current experimental studies generally employ wide temperature windows, ranging from over 800℃. Within such a wide temperature window, liquid and solid fuels are highly likely to have undergone phase changes. Therefore, in practical experimental research, it is often necessary to focus on the phase change process of the fuel and strictly design corresponding experimental temperature ranges and partial pressures to prevent fuel liquefaction in gaseous homogeneous experiments or undesirable vaporization and solidification processes in liquid homogeneous experiments. Different experiments require the design of targeted combustion pretreatment devices, feeding devices, and phase-compatible experimental setups to ensure the stability of fuel sample introduction, reaction, and combustion processes during the experiment. The current academic approach is basically to design according to needs, that is, to design corresponding pretreatment, feeding and experimental devices based on a single experiment. Related experimental equipment that can prepare reactants of different phases or separate reactants of different phases is still relatively rare.

[0004] Currently, commonly used combustion experimental equipment in academia and industry includes flow tube reactors, jet stirred reactors, shock tubes, and detonation tubes. Different experimental equipment is often compatible with different fuel states. For example, jet stirred reactors are commonly used for gaseous homogeneous experiments, while flow tube reactors can be used for both gaseous and liquid homogeneous experiments. Different experimental equipment has its own strengths, and in academic research, different experimental equipment is often used to study the combustion process of the same fuel to ensure the accuracy of theoretical analysis and to expand the corresponding experimental conditions. Currently, experimental setups that can simultaneously accommodate multiple reaction systems and various experimental devices are still relatively rare in relevant reports.

[0005] Lubricating grease is a collective term for lubricating oil and lubricating grease. Lubricating oil is a liquid or semi-solid lubricant used on various mechanical equipment to reduce friction and protect machinery and processed parts. Its functions include lubrication, cooling, rust prevention, cleaning, sealing, and buffering. Lubricating grease is mainly a thick, grease-like substance, primarily semi-solid, and its functions include lubrication, sealing, filling gaps, and rust prevention in mechanical equipment. Lubricating oil includes mineral base oil, synthetic base oil, and bio-based oil, with mineral base oil being the most common. It is composed of various chain hydrocarbons (including straight-chain n-alkanes, branched-chain hydrocarbons, etc.), cycloalkanes, aromatic hydrocarbons, gums, asphaltenes, and organic substances containing various heteroatoms. Lubricating grease has a more complex composition, consisting of base oil, additives, and soap base. In engineering practice, lubricating grease is often used under high-temperature conditions, accompanied by complex physical and chemical changes, such as the volatilization and combustion of lubricating oil at high temperatures, thermal oxidation and coking of lubricating oil, the gradual transformation of lubricating grease from solid to liquid, and the production of carbon deposits from the volatilization of lubricating grease. Multiple research institutions and engineering production units have reported flame, coking, and carbon deposit phenomena in lubricated components during experiments and production. These reports cover temperature conditions ranging from 200℃ to over 1000℃, and pressure conditions similarly encompassing a wide range from ultra-low pressure to supercritical states. Therefore, studying the combustion, coking, and carbon deposit processes of lubricating greases with different phases using a broad range of experimental and pressure conditions has significant research and engineering value and meets the current needs of academia and industry.

[0006] Currently, commonly used experimental equipment and its associated preparation and sample introduction equipment cannot meet the above needs. However, specific experimental research and engineering practice have raised the need for homogeneous solid-liquid-gas three-state reaction processes of lubricating greases under different temperature and pressure conditions, as well as the corresponding coking and carbon deposition processes. To meet current research needs, it is necessary to design an experimental setup capable of preparing and separating different phase reactants, and capable of studying the pyrolysis, oxidation, coking, and carbon deposition processes of lubricating greases with different phases under different temperature and pressure conditions. Summary of the Invention

[0007] To address the aforementioned existing technologies, this invention proposes a three-phase experimental system for studying the combustion, coking, and carbon deposition of lubricating greases. This system includes pre-experimental equipment for monitoring the complete boiling range and reaction process, independent heating for preparing / separating reactants to create stable gas-liquid feed streams, and a flow tube reactor for conducting homogeneous solid-liquid-gas three-phase experiments. This experimental system can monitor the complete boiling range and reaction process of lubricating greases through pre-experiments in a jet-stirred reactor. It can separate lubricating greases in multiple states through independent heating and separation devices, achieving stable gas-liquid two-phase feed. It can simultaneously perform and realize homogeneous pyrolysis, oxidation, coking, and carbon deposition experiments of lubricating greases in gas, solid, and liquid states. This three-phase experimental system is compatible with multiple reaction systems and various experimental equipment, while being safe, reliable, compact, simple to assemble and disassemble, easy to process, and not prone to clogging. It can achieve comprehensive and rigorous temperature monitoring and stable feed of lubricating greases in multiple states.

[0008] To address the aforementioned technical problems, this invention proposes a three-phase experimental system for studying the combustion, coking, and carbon deposition of lubricating greases, comprising pre-experimental equipment, reactant preparation / separation equipment, and a flow tube reactor assembly; the specific structures of each part are as follows:

[0009] The pre-experimental equipment includes a jet-stirred reactor, an inlet pipe A, and an exhaust pipe B. The shell of the jet-stirred reactor is a sphere made of fused silica. The inlet pipe A and the exhaust pipe B are coaxial and have the same diameter. One end of the inlet pipe A is connected to a first gas phase mass flow controller, and the other end of the inlet pipe A extends into the spherical shell. At the extended end, there are two forked jet nozzles symmetrical to the center of the spherical shell. Each jet nozzle is L-shaped. One end of the exhaust pipe B is connected to the spherical shell, and the other end of the exhaust pipe B is connected to the inlet of a four-way valve. The spherical shell is equipped with a sampling nozzle.

[0010] The reactant preparation / separation equipment includes a liquid-gas two-phase heating chamber, a baffle-type liquid-gas separator, and a vaporization tank. The liquid-gas two-phase heating chamber includes a housing with a top cover and a glass observation window. Both the top cover and the inner wall of the housing are electrolytically passivated. The bottom area of ​​the housing is larger than the area of ​​the top cover. The cross-section of the internal space of the housing is consistent from the bottom surface upwards to 2 / 3 of the height, and gradually decreases to the area of ​​the top cover from 2 / 3 of the height upwards. The top cover is secured by a tight seal. The glass observation window is fixed with a snap-fit; its position and size must allow at least 3 / 4 of the liquid-gas interface to be observed through it; a threaded connection hole is provided on the side wall of the housing, positioned above the grease level in the inner cavity, and a pipe C is connected between the threaded connection hole and the first gas phase mass flow controller, with a first needle valve installed on pipe C; the housing is connected to the sample inlet pipe D of the baffle-type liquid-gas separator via a threaded connection hole on the bottom plate of the housing, and a first needle valve is installed on the sample inlet pipe D. A two-needle valve; the baffle-type liquid-gas separator is cylindrical, and its interior is equipped with multiple levels of baffles, all of which are arranged inclined from the outer wall towards the center, with the length of each baffle extending beyond the central axis of the separator; a partition is located at the bottom of the separator; the surfaces of the baffles, partitions, and the inner wall of the separator are all electrolytically passivated; a gas-phase plug and a liquid-phase plug are respectively located at the bottom of the separator and on both sides of the partition. The vaporization tank is cylindrical and filled with a large number of small steel balls to promote the vaporization process. An inlet plug is located at the bottom of the vaporization tank, and a sample inlet pipeline connects the inlet plug to the gas phase plug. A gas phase outlet drain valve and a gas phase suction pump are sequentially installed on the sample inlet pipeline from the gas phase plug to the inlet plug. A carrier gas inlet and outlet are respectively inserted through two through holes at the top of the vaporization tank, and needle valves are installed on both the carrier gas inlet and outlet.

[0011] The flow tube reactor group includes a semi-solid flow tube reactor, a gas phase flow tube reactor, and a liquid phase flow tube reactor, each equipped with a front and rear inlet / outlet. The front inlet / outlet of the semi-solid flow tube reactor is equipped with a pusher plate injector. The front inlet / outlet of the gas phase flow tube reactor is connected to the gas outlet of the gasification tank, and a second gas phase mass flow controller is installed on the front inlet / outlet. The front inlet / outlet of the liquid phase flow tube reactor is connected to the liquid phase side plug at the bottom of the liquid-gas two-phase heating chamber, and a liquid phase mass flow controller is installed on the front inlet / outlet. A liquid phase suction pump is installed on the connecting pipe section between the liquid phase mass flow controller and the liquid phase side plug.

[0012] In this invention, temperature sensors are installed inside the spherical shell of the jet stirring reactor, the cavity of the baffle-type liquid-gas separator, the box of the liquid-gas two-phase heating chamber, and the gasification tank.

[0013] Furthermore, in the three-phase experimental system described in this invention:

[0014] The sampling nozzle is a thin-walled, trumpet-shaped structure made of fused silica. The sampling nozzle is a backup sampling port, which is connected to a mass spectrometer or mass spectrometry / chromatography detector when in use, and is sealed with a leak-proof gasket when not in use.

[0015] The other three ports of the four-way valve are exhaust ports, and the three exhaust ports are respectively connected to a vacuum gauge, a chromatographic injection device, and an exhaust gas treatment device.

[0016] The gasification tank insert has a carrier gas inlet connected to a carrier gas cylinder and a gas pump.

[0017] The liquid-gas two-phase heating chamber has two temperature sensors inside. One sensor is located above the liquid-gas interface to monitor the gas temperature inside the chamber, and the other sensor is located below the liquid-gas interface to monitor the liquid temperature inside the chamber.

[0018] The jet-stirred reactor is heated and kept warm by a tubular heater; the sample inlet pipe A and the exhaust pipe B are wrapped with heating tape for insulation.

[0019] The liquid-gas two-phase heating chamber, the baffle-type liquid-gas separator, and the vaporization tank are heated and insulated by a box-type heating furnace; the outer side of the gas inlet and outlet of the vaporization tank is equipped with a heating belt, which is uniformly double-wired and wound around the center line.

[0020] Heating belts are provided on the outside of the gas phase flow tube reactor, liquid phase flow tube reactor, semi-solid phase flow tube reactor and the back pipe. The heating belts are uniformly double-wired and wound around the center line. Thermocouples are inserted in the heating belts to monitor the temperature of the flow tube reactors.

[0021] Compared with the prior art, the beneficial effects of the present invention are:

[0022] This invention enables complete pre-experimentation through pre-experiment equipment to monitor the complete boiling range and reaction process of lubricating greases and to determine the corresponding temperature and pressure conditions.

[0023] The reactant preparation / separation equipment of this invention has a relatively independent heating device to independently heat the lubricating grease. Under the premise of strict temperature monitoring, it can prepare stable gas and liquid phase injection streams, realize the stable vaporization of lubricating grease, and provide a stable gas phase injection stream.

[0024] This invention is compatible with various pressure and temperature conditions and includes two or more commonly used experimental devices in combustion science, such as flow tube reactors and jet stirred reactors. The flow tube reactor group in this invention is equipped with a semi-solid flow tube reactor with a pusher plate sampler, which realizes stable sample introduction of semi-solid lubricating grease and combustion-related research.

[0025] Based on an understanding of the complete boiling range and reaction process, this invention's three-phase experimental system can simultaneously conduct homogeneous pyrolysis, oxidation, coking, and carbon deposition experiments on lubricating greases in gas, solid, and liquid states. This invention is compatible with multiple reaction systems and various experimental equipment, while being safe, reliable, compact, simple to assemble and disassemble, easy to process, and not prone to clogging. It provides rigorous temperature monitoring and a complete pump system for suction and hydrophobic functions. It enables comprehensive and precise temperature monitoring and stable sample introduction of lubricating greases in multiple phases. Attached Figure Description

[0026] Figure 1 This is a schematic diagram of the overall structure and operation of a three-phase experimental system used for the study of combustion / coking / carbon deposition of lubricating greases;

[0027] Figure 2 yes Figure 1 Enlarged view of the local structure at point I in the middle.

[0028] In the picture:

[0029] 1-Top cover 2-Fasting buckles 3-Box body

[0030] 4-Glass observation window; 5-Base screw plug; 6-Second needle valve

[0031] 7-Baffle-type liquid-gas separator; 8-Second temperature sensor; 9-Gas phase side screw plug

[0032] 10-Fourth needle valve 11-Drain valve 12-Liquid phase side plug

[0033] 13-Third needle valve 14-Liquid phase suction pump 15-Gas phase suction pump

[0034] 16-Inlet plug 17-Third temperature sensor 18-Carrier air intake duct

[0035] 19-Push-plate sampler; 20-Semi-solid flow tube reactor; 21-Gas flow tube reactor

[0036] 22-Catalyst installation mesh; 23-Post-connection pipe; 24-Liquid phase flow tube reactor.

[0037] 25-Four-way valve; 26-Jet stirred reactor; 27-Sampling nozzle

[0038] 28-First temperature sensor 29-Liquid phase mass flow controller

[0039] 30 - First and second gas phase mass flow controllers; 31 - First needle valve

[0040] 32-Side wall screw plug; 33-Air outlet; 34-Temperature sensor

[0041] 35-Liquid-Gas Two-Phase Heating Chamber; 36-Vaporization Tank; 37-Jet Nozzle

[0042] 38-partition

[0043] 39-baffle Detailed Implementation

[0044] The design concept of this invention, a three-phase experimental system for studying the combustion, coking, and carbon deposition of lubricating greases, is based on the objective needs of current combustion science research on the solid, liquid, and gaseous homogeneous reactions of lubricating greases and the macroscopic pyrolysis, oxidation, coking (including thermal cracking coking and thermal oxidation coking), and carbon deposition processes exhibited during the reaction. This system enables the preparation of reactants in different physical states / phases, the effective separation of greases in multiple physical states, and the conduct of pyrolysis, oxidation, coking, and carbon deposition experiments on lubricating greases in different physical states under different temperature, pressure, and reaction equipment conditions. The three-phase experimental system mainly includes pre-experimental equipment, reactant preparation / separation equipment, and multiple flow tube reactors equipped with mass flow controllers. Equipped with a relatively independent heating device, this invention achieves stable vaporization of lubricating oil and grease, providing a stable gas-phase feed flow for pre-experimental equipment. This facilitates monitoring the complete boiling range and reaction process of lubricating grease under different pressure conditions, clarifying the corresponding temperature and pressure conditions. On one hand, based on a clear understanding of the complete boiling range and reaction process, and under strict temperature control, it achieves liquid-gas separation of partially vaporized lubricating grease, enabling the separation of lubricating greases in different physical states using a single pretreatment and feeding device, providing a stable gas-liquid feed flow for subsequent experimental setups. On the other hand, it can be integrated with various commonly used combustion reaction devices, such as flow tube reactors and jet-stirred reactors. These reactors have well-defined and fixed temperature and pressure control strategies and methods to ensure compatibility with different pressures, temperatures, and reactor conditions. Furthermore, the three-phase experimental system of this invention includes an independent semi-solid lubricating grease experimental device to supplement experiments conducted at temperatures below 200°C where the lubricating grease is in a semi-solid state.

[0045] The present invention will be further described below with reference to the accompanying drawings and specific embodiments, but the following embodiments are by no means intended to limit the present invention.

[0046] In the description of this invention, it should be noted that the terms "upper," "lower," "left," "right," "inner," and "outer," etc., used to indicate orientation or positional relationships are based solely on the orientation or positional relationships shown in the accompanying drawings. They are used only for the convenience of describing the invention or simplifying related descriptions, and do not indicate or imply that the device or element referred to must have a specific orientation, or must have a specific structure or arrangement, or must operate in a specific arrangement. Therefore, they should not be construed as limitations on the invention. The terms "first," "second," and "third," etc., used are only to distinguish multiple components with the same structure.

[0047] In the description of this invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "provided with," "arranged," and "connected" should be interpreted broadly. For example, "connection" in the description can be a fixed connection, a detachable connection, a non-detachable weld, or a connection in an integral, one-piece manufacturing form; it can be a direct connection or an indirect connection through an intermediate medium. Those skilled in the art can understand the specific meaning of the above terms in this invention based on actual engineering needs and specific circumstances in engineering practice.

[0048] like Figure 1 As shown, the present invention proposes a three-phase experimental system for studying the combustion / coking / carbon deposition of lubricating greases, including pre-experimental equipment, reactant preparation / separation equipment, and flow tube reactor group.

[0049] The pre-experimental equipment includes a first gas phase mass flow controller 30, a jet stirred reactor 26, a four-way valve 25, and auxiliary pipelines, including an inlet pipeline A and an exhaust pipeline B.

[0050] The shell of the jet-stirred reactor 26 is a spherical shell made of fused silica. At the center of the interior of the spherical shell are two forked jet nozzles 37 symmetrically positioned about the center of the shell. Each jet nozzle 37 is L-shaped, and the tails of the two jet nozzles intersect. Figure 2As shown; the upper end of the spherical shell is provided with a sampling nozzle 27. The outer wall of the sampling nozzle 27 and the outer wall of the jet stirring reactor 26 can be connected by fusion welding or directly processed as a whole. The sampling nozzle 27 is a spare sampling port. When in use, it is connected to a mass spectrometer or a mass spectrometry / chromatography detector. When not in use, it is filled with a leak-proof gasket and locked. In this embodiment, the sampling nozzle 27 is a trumpet-shaped thin-walled structure made of fused silica. The internal cavity of the sampling nozzle 27 communicates with the sampling port machined on the spherical shell. The central axis of the sampling nozzle 27 coincides with the central axis of the sampling port on the spherical shell. The jet stirring reactor 26 has an exhaust port machined at its rear end along the injection direction. The exhaust port passes through the outer wall of the jet stirring reactor 26 and communicates with the exhaust pipe B. The central axis of the exhaust pipe B coincides with the central axis of the injection pipe A and is perpendicular to the central axis of the sampling nozzle 27. One end of the injection pipe A is connected to the first gas phase mass flow controller 30, and the other end of the injection pipe A extends into the center of the spherical shell and communicates with the intersection of the tails of the two jet nozzles 37. One end of the exhaust pipe B communicates with the spherical shell. The left end of the four-way valve 25 is the air inlet, which is connected to the exhaust pipe B. The upper, lower, and right ends are the exhaust ports. The other end of the exhaust pipe B is connected to the air inlet of the four-way valve 25. The three exhaust ports are respectively connected to a vacuum gauge, a chromatographic sample injection device, and a waste gas treatment device, used to detect the internal pressure of the jet stirring reactor 26, sample and detect reaction products, and treat combustion waste gas. A first temperature sensor 28 is inserted into the spherical shell of the jet stirring reactor 26 near the wall. A leak-proof gasket and rubber ring are provided between the end of the circuit of the first temperature sensor 28 and the opening of the mounting hole to prevent air and liquid leakage.In this embodiment, the spherical shell of the jet-stirred reactor 26 is hollow, and through holes penetrating the outer wall are machined on the left, right, and upper ends. The inner diameter of the through holes on the left and right ends should be consistent, while the inner diameter of the through hole on the upper end can be slightly adjusted according to requirements. The gaseous reactants enter the injection pipe A of the jet-stirred reactor 26 through the first gas phase mass flow controller 30. The injection pipe A extends into the inner cavity of the jet-stirred reactor 26 from the through hole on the left side, approximately at the center of the sphere of the jet-stirred reactor 26. The injection pipe A branches into two jet nozzles 37 symmetrical about the center of the jet-stirred reactor 26. The overall shape of the jet nozzles 37 is an "L" bend. After sufficient reaction, the reaction products in the jet-stirred reactor 26 are discharged through the exhaust pipe. Gas line B enters the four-way valve 25; the exhaust line B communicates with the inner cavity of the jet stirring reactor 26 through the right through hole of the jet stirring reactor 26, and the outer wall of the exhaust line B directly intersects with the outer wall of the jet stirring reactor 26; a sampling nozzle 27 is machined on the jet stirring reactor 26, which communicates with the inner cavity of the jet stirring reactor 26 through the upper through hole of the jet stirring reactor 26, and the outer wall of the sampling nozzle 27 directly intersects with the outer wall of the jet stirring reactor 26; the central axis of the left and right through holes of the jet stirring reactor 26 coincides with the central axis of the sample inlet line A and the exhaust line B; the central axis of the sampling nozzle 27 coincides with the central axis of the upper through hole of the jet stirring reactor 26, and is perpendicular to the central axis of the sample inlet line A and the exhaust line B. The left end of the four-way valve 25 is the air inlet, connected to the exhaust pipe B. The upper, lower, and right ends are exhaust ports, respectively connected to a vacuum gauge, a chromatographic sample injection device, and a waste gas treatment device, used to detect the internal pressure of the jet-stirred reactor 26, sample and detect reaction products, and treat combustion waste gas. The sampling nozzle 27 is a spare sampling port, connected as needed to a mass spectrometer, mass spectrometry / chromatography detector, or other detection equipment. When not in use, it is filled with a leak-proof gasket and locked. The jet-stirred reactor 26 is placed in a tubular furnace for heating and insulation. The external parts of the sample injection pipe A and the exhaust pipe B are uniformly double-stranded with heating tape around the center line to achieve pipe insulation and prevent liquefaction of gaseous reactants.

[0051] The reactant preparation / separation equipment includes a liquid-gas two-phase heating chamber 35, a baffle-type liquid-gas separator 7, a vaporization tank 36, and auxiliary valves and pipelines.

[0052] The liquid-gas two-phase heating chamber 35 consists of a top cover 1, a box body 3, and a glass observation window 4, which together form the internal space of the liquid-gas two-phase heating chamber. The inner walls of the top cover 1 and the box body 3 are both electrolytically passivated. The box body 3 is made of a thermally conductive alloy material, with an openable top cover 1 installed on the top and a glass observation window 4 installed on the side wall. The box body 3 and the top cover 1 of the liquid-gas two-phase heating chamber are fixed together by fastening buckles 2. The side wall of the housing 2 is machined with a threaded connection hole, which is positioned above the grease level in the inner cavity. This connection hole is connected to the sample inlet line A of the jet stirring reactor 26 via a side wall plug 32. The sample inlet line A has a thread at one end near the housing 3 for assembling the side wall plug 32. The central axes of the sample inlet line A, the side wall plug 32, and the threaded connection hole coincide. A pipe C connects the threaded connection hole to the first gas phase mass flow controller 30, and a first needle valve 31 is installed on pipe C. The baffle-type liquid-gas separator 7 is cylindrical. A sample inlet line D is located at the top of the baffle-type liquid-gas separator 7, and the top of the sample inlet line D is threaded. The bottom of the housing 3 has a threaded hole. The housing 3 is connected to the sample inlet line D via a base plug 5 and the threaded hole at the bottom. The central axes of the sample inlet line D, the base plug 5, and the threaded hole coincide. A second needle valve 6 is installed on the sample inlet line D. The liquid-gas two-phase heating chamber 35 is equipped with two temperature sensors 34 inside its housing 3. One temperature sensor 34 is positioned above the internal lubricating grease level, i.e., the liquid-gas interface, while the other temperature sensor 34 is positioned below the internal lubricating grease level, i.e., below the liquid-gas interface. These sensors are used to monitor the temperature of the gaseous and liquid substances inside the chamber, respectively. The internal temperature and pressure conditions of the liquid-gas two-phase heating chamber should ensure that the lubricating grease is a liquid-gas mixture. The two temperature sensors 34 are internally inserted and are equipped with anti-leakage gaskets and rubber rings to ensure that the device does not leak after the sensors are installed. The temperature sensor signals are directly transmitted to the computer, and the data is visible in real time.The bottom area of ​​the housing 3 is larger than the area of ​​the top cover 1. The cross-sectional area of ​​the internal space of the housing 3 is consistent from the bottom surface of the housing to 2 / 3 of its height, and gradually decreases to the area of ​​the top cover 1 from 2 / 3 of its height upwards. In this embodiment, the cross-sectional area of ​​the internal space of the liquid-gas two-phase heating chamber 35 remains constant from the bottom surface of the housing 3 to 2 / 3 of its height, and gradually decreases to the area of ​​the top cover 1 from 2 / 3 of its height. The cross-section of the internal space of the liquid-gas two-phase heating chamber is rectangular from the bottom surface of the housing 3 to the top cover 1. The top cover 1 is a short, tall, cubic shape, and its bottom area is slightly smaller than the area of ​​the top opening of the housing 3. The top cover 1 is secured with fastening clips 2 on the side. The top cover 1 can be opened after the fastening clips 2 are released. A leak-proof gasket is provided between the top cover 1 and the fastening clips 2. A window is machined into the side of the housing 3, with the upper edge of the window slightly lower than 2 / 3 of the housing height. A glass observation window 4, made of high-strength glass and shaped like a short, tall cubic shape, is installed in this window to observe the phase changes of the lubricating grease and the liquid-gas interface. A leak-proof gasket is provided between the glass observation window 4 and the housing opening. A clear liquid level should be visible through the glass observation window 4, and the position and size of the glass observation window 4 should be sufficient to observe at least 3 / 4 of the liquid-gas interface area. The liquid-gas two-phase heating chamber 35 is placed in a box-type furnace for heating and insulation.

[0053] The baffle-type liquid-gas separator 7 has multiple levels of baffles 39 inside. All baffles 39 are arranged inclined from the outer wall towards the center. The length of each baffle 39 extends beyond the central axis of the baffle-type liquid-gas separator 7. The length and number of levels of the baffles 39 should be sufficient to separate the liquid-gas mixture inside the liquid-gas two-phase heating chamber, so that the liquid-gas mixture separates due to inertia during its movement along the baffles 39. A second temperature sensor 8 is inserted inside the baffle-type liquid-gas separator 7 to monitor the internal temperature. A leak-proof gasket and rubber ring are provided between the end of the wiring of the second sensor 8 and the installed hole to prevent air and liquid leakage. A baffle 38 for liquid-gas separation is provided at the bottom of the baffle-type liquid-gas separator 7. The liquid level inside the baffle-type liquid-gas separator should not be higher than the height of the internal baffle 38 for liquid-gas separation. The bottom of the baffle-type liquid-gas separator 7, and on both sides of the partition 38, are respectively provided with a gas phase plug 9 and a liquid phase plug 12. The bottom of the baffle-type liquid-gas separator has a threaded hole on the side of the partition 38 in the direction of the inertial force of the liquid-gas mixture. The baffle-type liquid-gas separator 7 is connected to the liquid phase mass flow controller 29 through the liquid phase plug 12 and the pipeline E. The central axis of the sample inlet end of the pipeline E, the liquid phase plug, and the threaded hole coincide. The pipeline E is provided with a third needle valve 13 and a liquid phase suction pump 14. The liquid phase suction pump 14 is used to increase the liquid pressure in the pipeline E, so that the liquid quickly enters the liquid phase mass flow controller 29. The liquid phase suction pump 14 should be able to effectively increase the pressure of the liquid phase lubricating grease. The residence time of the liquid phase lubricating grease in the pipeline E should be significantly shorter than its residence time in the baffle-type liquid-gas separator 7. The inner wall surface of the baffle-type liquid-gas separator 7, including the surface of the baffle 39 and the surface of the bottom partition 38, is electrolytically passivated. The baffle-type liquid-gas separator 7 is placed in a box-type heating furnace for heating and heat preservation. The outside of the pipeline E is wrapped with heating tape in a uniform double-wire pattern around the center line to achieve pipeline heat preservation.

[0054] The vaporization vessel 36 is made of a thermally conductive alloy and has a cylindrical shape. The internal cavity is also cylindrical, and the inner wall is electrolytically passivated. The inner diameter design of the vaporization vessel 36 should significantly reduce the surface pressure of the injected reactants, thereby lowering the boiling point of the reactants and enabling them to vaporize rapidly. The vaporization vessel is filled with a large number of small steel balls that promote the vaporization process, so as to shorten the time required for the reactants to completely vaporize. The bottom of the vaporization tank 36 is provided with an inlet plug 16. A threaded hole is machined at the bottom of the baffle-type liquid-gas separator 7 on the opposite side of the inertial force direction of the liquid-gas mixture (i.e., the baffle 38; the other side). A pipe F is installed in the threaded hole. The baffle-type liquid-gas separator 7 communicates with the vaporization tank 36 through the gas phase side plug 9 and the pipe F. A thread is machined on the sample inlet pipe F near the baffle-type liquid-gas separator 7 to mate with the gas phase side plug 9. The sample inlet end of the sample inlet pipe F, the gas phase side plug 9, and the baffle-type liquid-gas separator... The central axes of the threaded holes on the opposite side of the inertial force direction of the bottom liquid-gas mixture 7 coincide; a drain valve 11 and a gas phase suction pump 15 are sequentially installed on the pipeline F between the baffle-type liquid-gas separator 7 and the vaporization tank 39, from the gas phase side plug 9 to the air inlet plug 16. The gas phase suction pump 15 should be able to effectively increase the pressure of the gas phase lubricating grease, and the residence time of the gas phase lubricating grease in the pipeline F should be significantly shorter than its residence time in the baffle-type liquid-gas separator, so that the gas can quickly enter the vaporization tank 36. The drain valve 11 is used to further separate the liquid-gas mixture. The pipeline F is externally insulated by uniformly double-wired heating tape wrapped around the center line. The top of the vaporization tank 36 has two mounting holes through which a carrier gas inlet 18 and an outlet 33 are respectively inserted. Sealing and heat-insulating gaskets are provided between the carrier gas inlet 18 and its mounting hole, and between the outlet 33 and its mounting hole. The outlet 33 is connected to a second gas phase mass flow controller 30. Needle valves are provided on both the carrier gas inlet 18 and the outlet 33. The carrier gas inlet 18 inserted into the vaporization tank 36 is externally connected to a carrier gas cylinder and a gas pump for introducing carrier gas into the vaporization tank 36 and blowing the vaporized reactants into the second gas phase mass flow controller 30. A third temperature sensor 17 is inserted inside the vaporization tank 36 to monitor the internal temperature. A leak-proof gasket and rubber ring are provided between the end of the third temperature sensor 17's wiring and the mounting hole to prevent gas and liquid leakage. The vaporization tank 36 is placed in a box-type heating furnace for heating and heat preservation. The outer surfaces of the carrier gas inlet 18 and the vaporizer outlet 33 are uniformly wrapped with heating tape around the center line in a double-line manner to achieve pipeline insulation.

[0055] The flow tube reactor group includes a semi-solid flow tube reactor 20, a gas phase flow tube reactor 21, and a liquid phase flow tube reactor 24, each equipped with a front and rear inlet pipe 23. The front inlet pipe of the semi-solid flow tube reactor 20 is equipped with a pusher plate sampler 19. The front inlet pipe of the gas phase flow tube reactor 21 is connected to the gas outlet 33 of the gasification tank 36, and a second gas phase mass flow controller 30 is installed on the front inlet pipe. The front inlet pipe of the liquid phase flow tube reactor 24 is connected to the liquid phase side plug 12 at the bottom of the liquid-gas two-phase heating chamber, and a liquid phase mass flow controller 29 is installed on the front inlet pipe. A liquid phase suction pump 14 is installed on the connecting pipe section between the liquid phase mass flow controller 29 and the liquid phase side plug 12.

[0056] In this embodiment, the flow rate of the gaseous reactants in the liquid-gas two-phase heating chamber 35 is controlled by the first gaseous mass flow controller 30, and they enter the jet-stirred reactor 26 via the sample inlet pipe A of the jet-stirred reactor 26. The flow rate of the liquid-phase reactants separated by the baffle-type liquid-gas separator 7 is controlled by the liquid-phase mass flow controller 29, and they enter the liquid-phase flow tube reactor 24 via the liquid-phase side plug 12 of the liquid-gas separator and the sample inlet pipe of the liquid-phase flow tube reactor 24. The non-pure gaseous reactants separated by the baffle-type liquid-gas separator 7 enter the vaporization tank 36 via the gaseous side plug 9 of the liquid-gas separator, the sample inlet pipe of the vaporization tank 36, and the bottom plug 16 of the vaporization tank. After being fully vaporized, their flow rate is controlled by the second gaseous mass flow controller 30, and they enter the gas-phase flow tube reactor 21 via the gas outlet 33 of the vaporization tank 36. The semi-solid grease is fed into the semi-solid flow tube reactor 20 gradually by the pusher plate sampler 19. The gas-phase flow tube reactor 21, liquid-phase flow tube reactor 24, and semi-solid-phase flow tube reactor 20 are all hollow thick-walled tubes made of corundum. A corundum tube flange is machined on the rear end face of the front tube along the sample inlet direction. The corundum tube flange and the left end flange of the corundum rear tube 23 are bolted together and equipped with a leak-proof and heat-insulating gasket. The inner diameter of the front tube and the rear tube 23 are the same and are not affected by the flange structure. After assembly, the central axes of the front tube, the rear end flange of the front tube, the rear tube 23, and the front end flange of the rear tube coincide. Catalyst mounting mesh 22 is provided near the rear end flange of each of the gas-phase flow tube reactor 21, liquid-phase flow tube reactor 24, and semi-solid-phase flow tube reactor 20 for adding catalyst as needed. The end of the rear tube 23 is connected to detection equipment such as a mass spectrometer and a chromatograph.

[0057] Heating strips are provided on the exterior of the gas-phase flow tube reactor 21, the liquid-phase flow tube reactor 24, the semi-solid-phase flow tube reactor 20, and the downstream pipe 23 to achieve pipeline heating and insulation. The heating strips are uniformly double-wired and wound around the centerline, and thermocouples are inserted inside the heating strips to monitor the temperature of the flow tube reactors.

[0058] This invention proposes a three-phase experimental system for the study of combustion, coking, and carbon deposition of lubricating greases. Based on this experimental system, homogeneous pyrolysis, oxidation, coking, and carbon deposition experiments of lubricating greases in gas, solid, and liquid states can be carried out simultaneously. It is compatible with multiple reaction systems and various experimental equipment, is safe and reliable, compact and simple, and easy to process. It effectively meets the current needs for the study of the combustion of lubricating greases and is conducive to the rapid acquisition of experimental data for a certain fuel or alternative fuel.

[0059] The pre-experimental equipment of this invention can systematically monitor the complete boiling range and reaction process of lubricating greases, clarify the corresponding temperature and pressure conditions, and provide a basis for the design and determination of subsequent experimental conditions while obtaining experimental data of the jet-stirred reactor.

[0060] The reactant preparation / separation device of the present invention combines three processes: independent heating, liquid-gas separation, and evaporation-gasification, and realizes the preparation of stable gas-phase and liquid-phase sample streams based on a single device under strict temperature monitoring.

[0061] The semi-solid flow tube reactor 20 with pusher plate sampler 19 set in this invention realizes stable sample injection of semi-solid lubricating grease, which is an effective supplement to gas phase and liquid phase research.

[0062] The components in the pre-experimental equipment, reactant preparation / separation equipment, and flow tube reactor equipment are connected by flanges, threads, or plug tubes, etc., which is simple, conforms to current experimental practices, and is easy to disassemble, repair, or replace. It is also convenient to set up, adjust, or assemble the device with commonly used experimental, control, and detection devices.

[0063] The specific operational process for conducting homogeneous phase studies of lubricating greases in their gas, solid, and liquid states using this invention is as follows:

[0064] First, a preliminary experimental phase is conducted, omitting the airtightness check procedure. The jet-stirred reactor 26 is installed in the tubular furnace, and the liquid-gas two-phase heating chamber 35, the baffle-type liquid-gas separator 7, and the vaporization tank 36 are installed in the box-type furnace. These devices are secured using heat-resistant cable ties and insulation materials. The heating elements in each pipeline are energized, all needle valves, suction pumps, and drain valves are closed, and temperature sensors are connected at all points to ensure stable and effective temperature measurements are available on the computer. Connect the three exhaust ports of the four-way valve 25 to the vacuum gauge, the chromatographic injection device, and the waste gas treatment device, respectively. Connect the sampling nozzle 27 to the time-of-flight photoionization mass spectrometer (the sampling nozzle can be directly locked if not needed). Turn on the gas phase mass flow controller 30 on the injection line of the jet stirred reactor 26 and introduce a rare gas (such as argon) into the jet stirred reactor 26 to purge impurities for about 30 minutes, until the chromatograph connected to the four-way valve 25 and the mass spectrometer connected to the sampling nozzle 27 show that the gas blown out of the jet stirred reactor 26 is basically free of impurities. Stop; stop the rare gas injection, remove the fastening buckle 2 next to the top cover 1 of the liquid-gas two-phase heating chamber, open the top cover 1 of the heating chamber, add lubricating oil (or semi-solid grease) into the inner cavity of the heating chamber until it completely covers the lower liquid-gas two-phase heating chamber temperature sensor 34, but still maintain a distance of more than 5cm from the upper liquid-gas two-phase heating chamber temperature sensor 34; observe the inner cavity of the liquid-gas two-phase heating chamber 35 to ensure that the amount added is appropriate, that there is no lubricating grease adhering to the wall, and that there is no lubricating grease contaminating the glass observation window 4; if there is no abnormality, close the top cover 1 of the liquid-gas two-phase heating chamber and install the fastening buckle 2.

[0065] Increase the temperature of the box-type heater where the liquid-gas two-phase heating chamber 35 is located; for lubricating oil, if obvious bubbles are observed escaping from the liquid through the glass observation window 4, and the temperature change measured by the temperature sensor 34 slows down or basically stops, then determine the required concentration, mix part of the protective gas through the gas phase mass flow controller 30, open the first needle valve 31, and pass the mixture of lubricating oil vapor and protective gas into the jet stirring reactor 26. If the chromatograph connected to the four-way valve 25 and the mass spectrometer connected to the sampling nozzle 27 stabilize and show a clear parent signal, it indicates that the lubricating oil has begun to vaporize. Record this temperature as the lubricating oil vaporization start temperature, gradually increase the temperature, and clarify the data such as the vaporization temperature of different components of the lubricating oil, the temperature at which the lubricating oil is completely vaporized, the pyrolysis start temperature of the main components of the lubricating oil, and the pyrolysis completion temperature of the lubricating oil. For grease, if liquefaction is observed through the glass observation window 4, this temperature is recorded as the grease liquefaction start temperature. If partial liquefaction is observed, the temperature change measured by the temperature sensor 34 slows down. At this time, the required concentration is determined, and a portion of the protective gas is mixed through the gas phase mass flow controller 30. The first needle valve 31 is opened to introduce the mixture of grease vapor and protective gas into the jet stirring reactor 26. Then, wait for the signals from the chromatograph connected to the four-way valve 25 and the mass spectrometer connected to the sampling nozzle 27 to stabilize, indicating that the residual gas and impurities in the gas path have been exhausted. If a clear parent signal is detected afterward, it indicates that the liquefied grease has begun to vaporize. This temperature is recorded as the liquefied grease vaporization start temperature. The temperature is gradually increased to determine the evaporation temperature of different components of the grease, the temperature at which the grease is completely liquefied, the temperature at which the grease is completely vaporized, the pyrolysis start temperature of the main components of the grease, and the pyrolysis completion temperature of the grease. If an oxidation experiment is required, a portion of oxygen can be introduced as needed via the gas phase mass flow controller 30; if a low-pressure experiment is required, a vacuum can be drawn via the four-way valve 25 to stably reduce the pressure in the jet-stirred reactor 26. After the preliminary experiment is completed, the first needle valve 31 is closed.

[0066] Once the required data is determined, the formal experiment can begin. If catalytic pyrolysis or oxidation experiments are required, the flange of pipe 23 should be disassembled beforehand, and the required catalyst should be installed in the catalyst installation mesh 22. For the lubricating oil experiment, adjust the temperature of the box-type heater where the liquid-gas two-phase heating chamber 35 is located so that the gas temperature measured by the temperature sensor 34 of the liquid-gas two-phase heating chamber is lower than the pyrolysis start temperature of the lubricating oil, and the measured liquid temperature is lower than the complete vaporization temperature of the lubricating oil. At this time, monitor the liquid-gas interface inside the liquid-gas two-phase heating chamber 35 through the glass observation window 4. If the height is not suitable, such as not exceeding the upper temperature sensor 34 or lower than the lower temperature sensor 34, adjust the heater temperature in time. After the temperature sensor 34 in the liquid-gas two-phase heating chamber stabilizes and the liquid-gas interface height in the inner cavity of the liquid-gas two-phase heating chamber 35 is appropriate and stable, the internal temperatures of the vaporization tank 36 and the baffle-type liquid-gas separator 7 are first set as needed to ensure that they are higher than the evaporation temperature of the substance of interest to be vaporized. The internal temperatures of the vaporization tank 36 and the baffle-type liquid-gas separator 7 are confirmed to be within the required temperature range by the second temperature sensor 8 and the third temperature sensor 17. The injection flow rate, mixed protective gas concentration, and mixed oxygen concentration (for oxidation experiments) of the liquid phase mass flow controller 29 and the gas phase mass flow controller 30 are set according to experimental requirements. The gas phase flow tube is heated by the heating belt. The internal temperatures of reactor 21, liquid flow tube reactor 24, and post-connection pipe 23 are adjusted to the required values. The internal temperature of jet-stirred reactor 26 is adjusted to the required value by adjusting the temperature of the tubular heater. The first needle valve 31, the third needle valve 13, the fourth needle valve 10, the drain valve 11, the liquid phase suction pump 14, and the gas phase suction pump 15 are opened. The second needle valve 6 is gradually turned off to ensure that the flow rate of the gas-liquid mixture entering the baffle-type liquid-gas separator 7 does not exceed the allowable value. After standing for about 10 minutes, the needle valve of the carrier gas inlet 18 and the needle valve of the gasification tank outlet 33 are opened to introduce the required flow rate of carrier gas, blowing the gas in the gasification tank 36 into the gas flow tube reactor 21. After all the feedback signals from the detection equipment stabilize, it indicates that the residual gas in the device has been exhausted. Then, the detection instruments connected to the end of the post-connection pipe 23 are used to detect the pyrolysis or oxidation products. After completing an experiment under one working condition, the temperature working condition can be changed or the pressure conditions in the flow tube can be changed through relevant equipment to conduct the experiment under the next working condition. Alternatively, the experiment can be stopped, all needle valves, suction pumps, and drain valves can be closed, and all sensors and heating devices can be disconnected. After the temperature drops to room temperature, the flow tube can be removed. If necessary, it can be blown or washed. If not, the coking and carbon deposits can be sampled, observed, or weighed directly.

[0067] For grease experiments, specifically, the temperature of the box-type furnace containing the liquid-gas two-phase heating chamber 35 is adjusted so that the gas temperature measured by the temperature sensor 34 of the liquid-gas two-phase heating chamber is lower than the grease's pyrolysis initiation temperature, and the measured liquid temperature is slightly higher than the grease's complete liquefaction temperature. At this time, the liquid-gas interface inside the liquid-gas two-phase heating chamber 35 is observed through glass to ensure that the grease has completely liquefied and to avoid clogging the pipeline. Simultaneously, a certain mass of grease sample is weighed as needed and slightly inserted into the left side of the semi-solid flow tube reactor 20. A probe is used to gently push and pull the sample to ensure it does not clog the flow tube. The internal temperature of the semi-solid flow tube reactor 20 is adjusted to the required value using the heating belt, and the feed rate of the pusher plate sampler 19 is set according to engineering or experimental needs. The remaining settings and operating procedures are basically the same as those for lubricating oil experiments.

[0068] In summary, this invention proposes a three-phase experimental system for studying the combustion, coking, and carbon deposition of lubricating greases. Its main advantages lie in its independent pre-experimental equipment, which allows for complete monitoring of the boiling range and reaction process of lubricating greases, and clarification of the corresponding temperature and pressure conditions. Based on this clarified boiling range and reaction process, it integrates reactant preparation / separation equipment for independent heating, liquid-gas separation, and evaporation / gasification processes, enabling the preparation of a stable gas-liquid two-phase feed stream and the separation of gas-liquid reactants using the same equipment. Combined with multiple sets of flow tube reactors and jet-stirred reactors, it achieves experimental research on the solid-liquid-gas homogeneous reaction process of lubricating greases under different temperature and pressure conditions. While ensuring the above advantages, it also guarantees a simple process, easy disassembly or replacement of components, and convenient setup, adjustment, or integration with commonly used experimental, control, and detection devices.

[0069] Although the present invention has been described above in conjunction with the accompanying drawings, the present invention is not limited to the specific embodiments described above. The specific embodiments described above are merely illustrative and not restrictive. Adjustments, optimizations, and modifications made to the present invention by those skilled in the art under the guidance of the present invention without departing from the spirit of the present invention, such as changing the baffle-type liquid-gas separator to a centrifugal separator, are all within the protection scope of the present invention.

Claims

1. A three-phase experimental system for studying the combustion / coking / carbon deposition of lubricating greases, comprising pre-experimental equipment, reactant preparation / separation equipment, and a flow tube reactor assembly; The pre-experimental equipment includes a jet stirring reactor (26), an inlet pipe A, and an exhaust pipe B. The shell of the jet stirring reactor (26) is a sphere made of fused silica. The inlet pipe A and the exhaust pipe B are coaxial and have the same diameter. One end of the inlet pipe A is connected to a first gas phase mass flow controller (30), and the other end of the inlet pipe A extends into the spherical shell. Two jet nozzles (37) symmetrical to the center of the spherical shell are provided at the extended end. Each jet nozzle (37) is L-shaped. One end of the exhaust pipe B is connected to the spherical shell, and the other end of the exhaust pipe B is connected to the inlet of a four-way valve (25). The spherical shell is provided with a sampling nozzle (27). The reactant preparation / separation equipment includes a liquid-gas two-phase heating chamber (35), a baffle-type liquid-gas separator (7), and a vaporization tank (36); The liquid-gas two-phase heating chamber (35) includes a box (3), which is provided with a top cover (1) and a glass observation window (4). The inner walls of the top cover (1) and the box (3) are both electrolytically passivated. The bottom area of ​​the box (3) is larger than the area of ​​the top cover (1). The cross-section of the internal space of the box (3) is consistent from the bottom of the box to 2 / 3 of the height, and gradually decreases from 2 / 3 of the height to the top cover (1) to the area of ​​the top cover (1). The top cover (1) is fixed by fastening buckles (2). The position and size of the glass observation window (4) are required to allow observation of at least 3 / 4 of the liquid-gas interface. The side wall of the box (3) is provided with a pipe thread connection hole that is higher than the oil liquid level in the inner cavity. The pipe thread connection hole is connected to the first gas phase mass flow controller (30) by a pipeline C, and a first needle valve (31) is provided on the pipeline C. The housing (3) is connected to the sample inlet pipe D of the baffle-type liquid-gas separator (7) through a pipe thread connection hole set on the bottom plate of the housing. The sample inlet pipe D is provided with a second needle valve (6). The baffle-type liquid-gas separator (7) is cylindrical. The baffle-type liquid-gas separator (7) is provided with multiple baffles (39) inside. All baffles (39) are arranged inclined from the outer wall to the center. The length of the baffle (39) exceeds the central axis of the baffle-type liquid-gas separator (7). A partition (38) is provided at the bottom of the baffle-type liquid-gas separator (7). The surfaces of the baffle (39), the partition (38) and the inner wall of the baffle-type liquid-gas separator (7) are all electrolytically passivated. A gas phase plug (9) and a liquid phase plug (12) are respectively provided at the bottom of the baffle-type liquid-gas separator (7) and on both sides of the partition (38). The vaporization tank (36) is cylindrical and filled with a large number of small steel balls to promote the vaporization process. The bottom of the vaporization tank (36) is provided with an inlet plug (16). The inlet plug (16) and the gas phase plug (9) are connected by a vaporization tank sample inlet pipeline. The vaporization tank sample inlet pipeline is provided with a gas phase outlet drain valve (11) and a gas phase suction pump (15) in sequence from the gas phase plug (9) to the inlet plug (16). The top of the vaporization tank (36) is provided with a carrier gas inlet channel (18) and an outlet channel (33) through two through holes. The carrier gas inlet channel (18) and the outlet channel (33) are respectively provided with needle valves. The flow tube reactor group includes a semi-solid flow tube reactor (20), a gas phase flow tube reactor (21), and a liquid phase flow tube reactor (24), each equipped with a front and rear inlet pipe (23). The front inlet pipe of the semi-solid flow tube reactor (20) is equipped with a push plate sampler (19). The front inlet pipe of the gas phase flow tube reactor (21) is connected to the gas outlet (33) of the gasification tank (36), and a second gas phase mass flow controller (30) is installed on the front inlet pipe. The front inlet pipe of the liquid phase flow tube reactor (24) is connected to the liquid phase side plug (12) at the bottom of the liquid-gas two-phase heating chamber, and a liquid phase mass flow controller (29) is installed on the front inlet pipe. A liquid phase suction pump (14) is installed on the connecting pipe section between the liquid phase mass flow controller (29) and the liquid phase side plug (12). Temperature sensors are installed in the spherical shell of the jet stirring reactor (26), the cavity of the baffle-type liquid-gas separator (7), the box (3) of the liquid-gas two-phase heating chamber (35), and the gasification tank (36).

2. The three-phase experimental system according to claim 1, characterized in that, All temperature sensor signals are transmitted directly to the computer, and the data is visible in real time.

3. The three-phase experimental system according to claim 1, characterized in that, The sampling nozzle (27) is a thin-walled, trumpet-shaped structure made of fused silica. The sampling nozzle (27) is a spare sampling port. When in use, it is connected to a mass spectrometer or a mass spectrometry / chromatography detector. When not in use, it is filled with a leak-proof gasket and locked.

4. The three-phase experimental system according to claim 1, characterized in that, The other three ports of the four-way valve (25) are exhaust ports, and the three exhaust ports are respectively connected to a vacuum gauge, a chromatographic injection device and an exhaust gas treatment device.

5. The three-phase experimental system according to claim 1, characterized in that, The gasification tank (36) has a carrier gas inlet (18) connected to a carrier gas cylinder and a gas pump.

6. The three-phase experimental system according to claim 1, characterized in that, The liquid-gas two-phase heating chamber (35) has two temperature sensors inside its housing (3). One sensor is located above the liquid-gas interface to monitor the gas temperature inside the chamber, and the other sensor is located below the liquid-gas interface to monitor the liquid temperature inside the chamber.

7. The three-phase experimental system according to claim 1, characterized in that, The jet-stirred reactor (26) is heated and kept warm by a tubular heater; the sample inlet pipe A and the exhaust pipe B are wrapped with heating tape for insulation.

8. The three-phase experimental system according to claim 1, characterized in that, The liquid-gas two-phase heating chamber (35), the baffle-type liquid-gas separator (7) and the vaporization tank (36) are heated and kept warm by a box-type heating furnace; the outer side of the gas inlet (18) and outlet (33) of the vaporization tank (36) is provided with a heating belt, which is uniformly double-wired and wound around the center line.

9. The three-phase experimental system according to claim 1, characterized in that, Heating belts are provided on the outside of the gas phase flow tube reactor (21), liquid phase flow tube reactor (24), semi-solid phase flow tube reactor (20) and the back pipe (23). The heating belts are uniformly double-wired and wound around the center line. Thermocouples are inserted in the heating belts to monitor the temperature of the flow tube reactors.

Citation Information

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