Liquid propellant electric heating reaction device for mass spectrum online sampling detection

Abstract

The invention relates to the technical field of mass spectrometry, in particular to a liquid propellant electric heating reaction device for mass spectrometry online sampling detection. The device comprises a frame, a propellant sample injector, a mass spectrometer sampling cone and a reaction table cylinder, the reaction table cylinder vertically penetrates through the bottom face of the frame, a heat conductor is installed at the upper end of the reaction table cylinder, the sample injection end of the propellant sample injector and the sampling end of the mass spectrometer sampling cone both correspond to a heating area on the heat conductor, and an electric heating rod is installed in the reaction table cylinder. The heating end of the electric heating rod is located in the heat conductor. A heating area on a heat conductor is rapidly heated through an electric heating rod to form a high-temperature reaction micro-area, the liquid propellant is rapidly introduced into the high-temperature reaction micro-area before physical and chemical states of the liquid propellant are changed, and a sampling end of a mass spectrum sampling cone directly extends into the high-temperature reaction micro-area; and effective online sampling and rapid detection of intermediate products in the reaction process are realized.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of mass spectrometry, in particular to a liquid propellant electric heating reaction device for mass spectrometry online sampling and detection. BACKGROUND

[0002] Liquid propellant, as a special kind of high-energy chemical substance, is a key core material for aerospace equipment. It can chemically react in the engine to produce high-temperature and high-pressure gas, convert chemical energy into heat and kinetic energy, and form a certain thrust to drive the target aircraft to complete the intended action. In recent years, green liquid propellant has become an important direction and inevitable trend of aerospace power development to replace traditional toxic hydrazine propellant, so the decomposition and combustion reaction mechanism of liquid propellant has become a research hotspot.

[0003] New green liquid propellant often contains oxidizing agent, combustion agent, solvent and additive, etc., which is a mixed ionic solution. In actual application, the propellant is introduced into the catalyst bed or high-temperature combustion chamber in the form of microdroplets, directly contacts the catalyst or high-temperature heat accumulator and rapidly decomposes and combusts to produce high-temperature and high-pressure gas and diffuse out through the tail nozzle to form thrust. The decomposition and combustion process of liquid propellant is studied by using traditional flow tube reactor. In order to make the temperature of the reaction zone reach the target value, the adjacent area is also heated to a relatively high temperature by the heating furnace. The propellant is heated to a higher temperature by the peripheral system before reaching the reaction zone, and the phase change and decomposition reaction occur in the capillary tube in advance, which cannot truly simulate the actual application conditions, and even the problem of component crystallization and plugging of capillary tube occurs.

[0004] In addition, mass spectrometry, especially advanced vacuum photoionization mass spectrometry, can detect reaction intermediates on the basis of breaking the molecular structure, and provide reliable experimental evidence for chemical reaction mechanism research. However, since the decomposition and combustion reaction of liquid propellant is a millisecond-level rapid process, the ordinary mass spectrometer cannot effectively capture the reaction intermediates due to the long time difference caused by the position difference between sampling and detection. SUMMARY

[0005] Therefore, the present application provides a liquid propellant electric heating reaction device for mass spectrometry online sampling and detection.

[0006] To this end, the present application provides the following technical solutions: The application discloses a liquid propellant electric heating reaction device for mass spectrometry online sampling and detection, which comprises a frame, a propellant sampler, a mass spectrometer sampling cone and a reaction bench cylinder body, wherein the frame is internally provided with a reaction cavity, the reaction bench cylinder body vertically penetrates the bottom surface of the frame, a heat conduction block is mounted on the upper end of the reaction bench cylinder body, an electric heating rod is mounted below the heat conduction block in the reaction bench cylinder body, the heating end of the electric heating rod is located in the heat conduction block, the propellant sampler and the mass spectrometer sampling cone are respectively located on any two different surfaces of the frame except the bottom surface, and the sampling end of the propellant sampler and the sampling end of the mass spectrometer sampling cone both correspond to the electric heating area on the heat conduction block.

[0007] Further, a thermocouple is mounted below the heat conduction block in the reaction bench cylinder body, and the temperature sensing end of the thermocouple is located in the heat conduction block.

[0008] Further, an inner lining cylinder is mounted in the reaction bench cylinder body, the electric heating rod and the thermocouple are mounted in the inner lining cylinder, a locking nut is mounted at the lower end of the reaction bench cylinder body, the lower end of the inner lining cylinder is fixed to the lower end of the reaction bench cylinder body through the same annular locking gasket, the locking gasket is embedded in the inner side of the locking nut and simultaneously abuts against the lower end surface of the inner lining cylinder and the lower end surface of the reaction bench cylinder body, and the corresponding positions of the locking nut and the reaction bench cylinder body are both provided with wire through holes, and the wires of the electric heating rod and the thermocouple sequentially penetrate the wire through holes of the two components.

[0009] Further, the reaction bench cylinder body is mounted on the bottom surface of the frame through a reaction bench butt flange, and an air inlet pipe and an air outlet pipe which are in communication with the reaction cavity are respectively mounted on the side wall of the reaction bench butt flange.

[0010] Further, a sealing locking gasket is mounted between the reaction bench butt flange and the reaction bench cylinder body, a reaction bench locking flange is threadedly mounted below the sealing locking gasket on the reaction bench cylinder body, the upper end of the reaction bench locking flange abuts against the lower end of the sealing locking gasket, and a rotating handle is mounted on the reaction bench cylinder body.

[0011] Further, a high-temperature heat accumulator is mounted above the heat conduction block at the upper end of the reaction bench cylinder body, the sampling end of the propellant sampler and the sampling end of the mass spectrometer sampling cone both correspond to the electric heating area on the heat conduction block, and the material of the high-temperature heat accumulator is alumina, graphite, stainless steel or high-temperature resistant alloy.

[0012] Further, a mass spectrometer butt flange is mounted on the surface of the frame corresponding to the mass spectrometer sampling cone, the frame is sealingly mounted on a mass spectrometry detection equipment through the mass spectrometer butt flange, and the mass spectrometer sampling cone is connected with the mass spectrometry detection equipment.

[0013] Further, two second mounting plates are mounted on the rest of the frame, glass mounting holes are arranged on the same positions of the two second mounting plates, and annular mounting grooves are formed on the opposite inner sides of the two second mounting plates outside the glass mounting holes, and optical glass is mounted in the mounting grooves, wherein the optical glass is at least one selected from high-transparency quartz glass, infrared light-transparency glass, ultraviolet light-transparency glass and laser light-transparency glass.

[0014] Further, two first mounting plates are mounted on the frame surface where the propellant sampler is mounted, sealing holes are arranged on the same positions of the two first mounting plates, and annular sealing grooves are formed on the opposite inner sides of the two first mounting plates outside the sealing holes, and sealing plates are mounted in the sealing grooves, and the propellant sampler penetrates through the sealing plates and is fixed.

[0015] Further, the propellant in the propellant sampler is at least one selected from hydrazine liquid propellant, hydrazine nitrate liquid propellant, hydroxyethyl hydrazine nitrate liquid propellant, dinitramide ammonium-based green ionic liquid propellant and hydroxylamine nitrate-based green ionic liquid propellant.

[0016] Advantages and positive effects of the present application: The heat-conducting block is heated by the electric heating rod, so that the heat-conducting block is rapidly heated to form a high-temperature reaction microzone, while the surrounding environment is still in a low-temperature state, the liquid propellant is rapidly introduced into the high-temperature reaction microzone before the physical and chemical state of the liquid propellant is changed, and the actual application high-temperature working condition reaction is simulated; and the sampling end of the mass spectrometry sampling cone is directly inserted into the high-temperature reaction microzone, so that the intermediate product in the reaction process is effectively sampled and rapidly detected on line. BRIEF DESCRIPTION OF DRAWINGS

[0017] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the drawings needed to be used in the embodiments or the prior art description will be briefly introduced below. Obviously, the drawings in the following description are some embodiments of the present application, and other drawings can also be obtained by those skilled in the art without creative labor.

[0018] Figure 1 The structure diagram of the first embodiment of the liquid propellant electric heating reaction device for mass spectrometry on-line sampling and detection provided by the present application.

[0019] Figure 2 The sectional view of the first embodiment of the liquid propellant electric heating reaction device for mass spectrometry on-line sampling and detection provided by the present application.

[0020] Figure 3 The structure diagram of the second embodiment of the liquid propellant electric heating reaction device for mass spectrometry on-line sampling and detection provided by the present application.

[0021] Figure 4 This is a cross-sectional view of a second embodiment of an electrically heated reaction device for online mass spectrometry sampling and detection of liquid propellants provided by the present invention.

[0022] In the diagram: 1. Mass spectrometer sampling cone; 2. Reaction chamber; 3. Frame; 4. Mass spectrometer docking flange; 5. Reaction stage docking flange; 6. Inlet pipe; 7. Outlet pipe; 8. Second mounting plate; 9. Optical glass; 10. First mounting plate; 11. High-temperature heat storage body; 12. Reaction stage cylinder; 13. Locking nut; 14. Sealing locking gasket; 15. Reaction stage locking flange; 16. Propellant injector; 17. Sealing plate; 18. Heat-conducting block; 19. Electric heating rod; 20. Thermocouple; 21. Inner liner; 22. Locking gasket; 23. Wire through hole; 24. Rotary handle; 25. Sealing hole; 26. Sealing groove; 27. Glass mounting hole; 28. Mounting groove. Detailed Implementation

[0023] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of the present invention.

[0024] This invention provides an electrically heated reaction device for online mass spectrometry sampling and detection of liquid propellants, such as... Figures 1-2 As shown, the system includes a frame 3, a propellant injector 16, a mass spectrometer sampling cone 1, and a reaction stage cylinder 12. The frame 3 contains a reaction chamber 2. The reaction stage cylinder 12 vertically penetrates the bottom surface of the frame 3. A heat-conducting block 18 and a high-temperature heat storage body 11 are installed at its upper end. The high-temperature heat storage body 11 is located above the heat-conducting block 18. An inner liner 21 is installed inside the reaction stage cylinder 12. An electric heating rod 19 and a thermocouple 20 are installed inside the inner liner 21 below the heat-conducting block 18. The heating end of the electric heating rod 19 and the temperature sensing end of the thermocouple 20 are both located inside the heat-conducting block 18.

[0025] The reaction bench cylinder body 12 is installed on the bottom surface of the frame 3 through the reaction bench butt flange 5, and the reaction bench butt flange 5 is provided with a gas inlet pipe 6 and a gas outlet pipe 7 which are respectively connected with the reaction cavity 2, and one or more than two of a ball valve, a safety pressure relief valve, a pressure gauge and a pressure sensor can be installed on the gas inlet pipe 6 and the gas outlet pipe 7. The sealing locking gasket 14 is installed between the reaction bench butt flange 5 and the reaction bench cylinder body 12, and the reaction bench locking flange 15 is threadedly installed below the sealing locking gasket 14 on the reaction bench cylinder body 12, and the upper end of the reaction bench locking flange 15 abuts against the lower end of the sealing locking gasket 14. The sealing locking gasket 14 can be one or more than two, and the material can be one or more than two of polytetrafluoroethylene, graphite, composite graphite and silica gel. The rotating handle 24 is installed on the reaction bench cylinder body 12. The rotating handle 24 can rotate the reaction bench cylinder body 12, and then drive the reaction bench cylinder body 12 to move up and down through the threaded transmission, so as to change the distance between the upper surface of the high-temperature heat accumulator 11 and the sampling end of the mass spectrometry sampling cone 1. The surface of the reaction bench cylinder body 12 in contact with the reaction bench sealing locking gasket 14 is a smooth surface, the reaction bench sealing locking gasket 14 is pressed by the reaction bench locking flange 15 to realize the sealing contact between the reaction bench sealing locking gasket 14 and the reaction bench cylinder body 12, and the relative movement of the reaction bench cylinder body 12 relative to the frame 3 can be realized under the condition of ensuring the sealing.

[0026] The material of the high-temperature heat accumulator 11 is alumina, graphite, stainless steel or high-temperature resistant alloy. The propellant sampler 16 can be a thin tube or a capillary tube atomizing nozzle. The propellant sampler can drop the propellant in liquid form into the high-temperature reaction zone, or can spray the propellant into the high-temperature micro-reaction zone. The propellant in the propellant sampler 16 is at least one selected from hydrazine liquid propellant, hydrazine nitrate liquid propellant, hydroxyethyl hydrazine nitrate liquid propellant, dinitramide ammonium green ionic liquid propellant and hydroxylamine nitrate green ionic liquid propellant.

[0027] The propellant sampler 16 and the mass spectrometry sampling cone 1 are respectively located on any two different surfaces of the frame 3 except the bottom surface, and the sampling end of the propellant sampler 16 and the sampling end of the mass spectrometry sampling cone 1 correspond to the electric heating area on the high-temperature heat accumulator 11.

[0028] Two first mounting plates 10 are overlapped and mounted on the surface of the frame 3 on which the propellant sampler 16 is mounted, and sealing holes 25 are arranged at the same positions of the two first mounting plates 10. The opposite inner sides of the two first mounting plates 10 form annular sealing grooves 26 outside the sealing holes 25, sealing plates 17 are installed in the sealing grooves 26, and the propellant sampler 16 penetrates through the sealing plates 17 and is fixed. The mass spectrometer butt flange 4 is installed on the surface of the frame 3 corresponding to the mass spectrometry sampling cone 1, the frame 3 is sealed and mounted on the mass spectrometry detection equipment through the mass spectrometer butt flange 4, and the mass spectrometry sampling cone 1 is connected with the mass spectrometry detection equipment.

[0029] Two second mounting plates 8 are mounted on the rest of the frame 3, and glass mounting holes 27 are arranged on the same positions of the two second mounting plates 8. The opposite inner sides of the two second mounting plates 8 form annular mounting grooves 28 outside the glass mounting holes 27. The optical glass 9 is mounted in the mounting grooves 28, and the optical glass 9 is at least one selected from high-transparency quartz glass, infrared light-transmitting glass, ultraviolet light-transmitting glass and laser light-transmitting glass.

[0030] The lower end of the reaction table cylinder 12 is provided with a laser lens, and the locking nut 13 is provided with a wire through hole 23 corresponding to the laser lens.

[0031] As shown in the first embodiment, Figures 1-2 The mass spectrum sampling cone 1 is arranged on the side of the frame 3, and the propellant sampler 16 is arranged on the top of the frame 3. The optical glass 9 includes two high-transparency quartz glasses and one infrared light-transmitting glass, which are arranged on the rest of the frame 3 respectively. The infrared thermal imager is used to monitor the temperature of the reaction zone through the infrared light-transmitting glass, and the high-speed camera is used to record the image of the reaction process through the high-transparency quartz glass.

[0032] In use, the target gas is introduced into the reaction cavity 2 through the gas inlet pipe 6 and the gas outlet pipe 7, and the internal pressure of the reaction cavity 2 is controlled to reach the target pressure. The electric heating rod 19 and the thermocouple 20 are powered, the high-temperature heat accumulator 11 absorbs the heat generated by the electric heating rod 19 through the heat conduction block 18, so that the temperature of the electric heating area of the high-temperature heat accumulator 11 quickly reaches the target temperature. Before the temperature in the reaction cavity 2 reaches the propellant phase change temperature, the propellant is introduced into the high-temperature micro-reaction zone in the form of mist droplets through the propellant sampler 16, so that the rapid high-temperature decomposition or combustion reaction of the propellant occurs. The mass spectrum sampling cone 1 is used to sample and detect the intermediate products of the propellant reaction on line. The temperature of the heat conduction block 18 is monitored by the thermocouple 20, and the output power of the electric heating rod 19 is adjusted accordingly to achieve higher accuracy.

[0033] As shown in the second embodiment, Figures 3-4 The mass spectrum sampling cone 1 is arranged on the top of the frame 3, and the propellant sampler 16 is arranged on the side of the frame 3.

[0034] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present application, and are not limited thereto. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that the technical solutions described in the foregoing embodiments can be modified, or some or all of the technical features can be replaced by equivalents. The modification or replacement does not change the essence of the corresponding technical solution, which is within the scope of the technical solutions of the embodiments of the present application.

Claims

1. A liquid propellant electrically heated reaction apparatus for on-line sampling and detection by mass spectrometry, characterised in that, The application relates to a reaction platform for a mass spectrometer, which comprises a frame (3), a propellant sample injector (16), a mass spectrometer sampling cone (1) and a reaction platform cylinder (12), wherein the frame (3) is internally provided with a reaction cavity (2), the reaction platform cylinder (12) vertically penetrates the bottom surface of the frame (3), a heat conduction block (18) is mounted on the upper end of the reaction platform cylinder (12), an electric heating rod (19) is mounted below the heat conduction block (18) in the reaction platform cylinder (12), the heating end of the electric heating rod (19) is located in the heat conduction block (18), the propellant sample injector (16) and the mass spectrometer sampling cone (1) are respectively arranged on any two different surfaces of the frame (3) except the bottom surface, and the sampling end of the propellant sample injector (16) and the sampling end of the mass spectrometer sampling cone (1) are both corresponded to the electric heating area on the heat conduction block (18).

2. The liquid propellant electrically heated reaction device for on-line sampling and detection by mass spectrometry according to claim 1, characterized in that, A thermocouple (20) is mounted below the heat conduction block (18) in the reaction platform cylinder (12), and the temperature sensing end of the thermocouple (20) is located in the heat conduction block (18).

3. The liquid propellant electrically heated reaction apparatus for on-line sampling and detection by mass spectrometry according to claim 2, wherein An inner lining cylinder (21) is mounted in the reaction platform cylinder (12), and the electric heating rod (19) and the thermocouple (20) are mounted in the inner lining cylinder (21); a locking nut (13) is mounted on the lower end of the reaction platform cylinder (12), the lower end of the inner lining cylinder (21) is fixed to the lower end of the reaction platform cylinder (12) through a same annular locking gasket (22), the locking gasket (22) is embedded in the inner side of the locking nut (13) and is simultaneously attached to the lower end surface of the inner lining cylinder (21) and the lower end surface of the reaction platform cylinder (12); lead wire through holes (23) are formed in the corresponding positions of the locking nut (13) and the reaction platform cylinder (12), and the lead wires of the electric heating rod (19) and the thermocouple (20) sequentially penetrate the lead wire through holes (23) of the two components.

4. The liquid propellant electrically heated reaction apparatus for on-line sampling and detection by mass spectrometry of claim 1, wherein, The reaction platform cylinder (12) is mounted on the bottom surface of the frame (3) through a reaction platform butt flange (5), and an air inlet pipe (6) and an air outlet pipe (7) which are communicated with the reaction cavity (2) are respectively mounted on the side wall of the reaction platform butt flange (5).

5. The liquid propellant electrically heated reaction apparatus for on-line sampling and detection by mass spectrometry of claim 4, wherein, A sealing locking gasket (14) is mounted between the reaction platform butt flange (5) and the reaction platform cylinder (12), a reaction platform locking flange (15) is threadedly mounted below the sealing locking gasket (14) on the reaction platform cylinder (12), the upper end of the reaction platform locking flange (15) is abutted against the lower end of the sealing locking gasket (14), and a rotating handle (24) is mounted on the reaction platform cylinder (12).

6. The liquid propellant electrically heated reaction apparatus for on-line sampling and detection by mass spectrometry of claim 1, wherein, A high-temperature heat accumulator (11) is mounted on the upper end of the reaction platform cylinder (12) and above the heat conduction block (18), the sampling end of the propellant sample injector (16) and the sampling end of the mass spectrometer sampling cone (1) are both corresponded to the electric heating area on the heat conduction block (18), and the material of the high-temperature heat accumulator (11) is alumina, graphite, stainless steel or high-temperature resistant alloy.

7. The liquid propellant electrically heated reaction apparatus for on-line sampling and detection by mass spectrometry of claim 1, wherein, A mass spectrometer butt flange (4) is mounted on the surface of the frame (3) corresponding to the mass spectrometer sampling cone (1), the frame (3) is sealingly mounted on a mass spectrometer detection device through the mass spectrometer butt flange (4), and the mass spectrometer sampling cone (1) is connected with the mass spectrometer detection device.

8. The liquid propellant electrically heated reaction apparatus for on-line sampling and detection by mass spectrometry of claim 1, wherein, Two second installation plates (8) are installed on the rest of the frame (3), glass installation holes (27) are arranged on the same positions of the two second installation plates (8), and annular installation grooves (28) are formed on the opposite inner sides of the two second installation plates (8) outside the glass installation holes (27), and optical glass (9) is installed in the installation grooves (28), wherein the optical glass (9) is at least one selected from high-transparency quartz glass, infrared light-transmitting glass, ultraviolet light-transmitting glass and laser light-transmitting glass.

9. The liquid propellant electrically heated reaction apparatus for on-line sampling and detection by mass spectrometry of claim 1, wherein, Two first installation plates (10) are installed on the surface of the frame (3) on which the propellant sampler (16) is installed, sealing holes (25) are arranged on the same positions of the two first installation plates (10), and annular sealing grooves (26) are formed on the opposite inner sides of the two first installation plates (10) outside the sealing holes (25), and sealing plates (17) are installed in the sealing grooves (26), and the propellant sampler (16) penetrates through the sealing plates (17) and is fixed.

10. The liquid propellant electrically heated reaction apparatus for on-line sampling and detection by mass spectrometry of claim 1, wherein, The propellant in the propellant sampler (16) is at least one selected from hydrazine liquid propellant, hydrazine nitrate liquid propellant, hydroxyethyl hydrazine nitrate liquid propellant, dinitramide ammonium green ionic liquid propellant and hydroxylamine nitrate green ionic liquid propellant.

Images