CN210022078U - Experimental device for be used for high pressure gas solid phase catalytic reaction product of normal position survey - Google Patents

Experimental device for be used for high pressure gas solid phase catalytic reaction product of normal position survey Download PDF

Info

Publication number
CN210022078U
CN210022078U CN201920293858.XU CN201920293858U CN210022078U CN 210022078 U CN210022078 U CN 210022078U CN 201920293858 U CN201920293858 U CN 201920293858U CN 210022078 U CN210022078 U CN 210022078U
Authority
CN
China
Prior art keywords
pressure
pipe
tube
reaction
quartz
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201920293858.XU
Other languages
Chinese (zh)
Inventor
杨玖重
余圣圣
文武
许鸣皋
潘洋
陆亚林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Science and Technology of China USTC
Original Assignee
University of Science and Technology of China USTC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Science and Technology of China USTC filed Critical University of Science and Technology of China USTC
Priority to CN201920293858.XU priority Critical patent/CN210022078U/en
Application granted granted Critical
Publication of CN210022078U publication Critical patent/CN210022078U/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The utility model relates to an experimental apparatus for be used for normal position to survey high pressure gas solid phase catalytic reaction result. Comprises a mass spectrometer, a high-pressure catalytic reaction mechanism, a heating mechanism and a sampling nozzle; the high-pressure catalytic reaction mechanism comprises a sleeve, a pressure-bearing pipe and a quartz reaction pipe which are coaxially arranged from outside to inside; the upper end of the pressure-bearing pipe is provided with coaxial inverted cone angle micropores; a catalyst is encapsulated in the quartz reaction tube by quartz cotton; when the reactor works, the heating mechanism heats the catalyst to a reaction temperature; gas phase reactant enters from the rear end of the quartz reaction tube, contacts with the catalyst and generates catalytic reaction, reaction product enters into the pressure bearing tube through a small hole at the front end of the quartz reaction tube, forms ultrasonic molecular beam through a reverse taper angle micropore of the pressure bearing tube, and enters into a mass spectrometer for ionization detection through a sampling port of the sampling nozzle. The device can detect unstable intermediate products of gas-solid phase catalytic reaction on line in situ in real time under the condition of industrial high pressure, avoid secondary reaction in the sampling and transmitting process and is beneficial to the understanding of the mechanism of the high-pressure gas-solid phase catalytic reaction.

Description

Experimental device for be used for high pressure gas solid phase catalytic reaction product of normal position survey
Technical Field
The utility model belongs to the technical field of gas-solid phase catalytic reaction product normal position is surveyed, concretely relates to a device that is used for normal position to survey gas-solid phase catalytic reaction product.
Background
The catalyst is widely applied in industry, is the most important reaction applied in chemical industry at present, and has important contribution to the development of national economy. Important reactions in modern chemical industry, such as synthesis ammonia reaction, methanol-to-olefin reaction, Fischer-Tropsch reaction and the like, are used gas-solid phase reactions, so that research on gas-solid phase catalytic reaction has important significance for development of modern chemical industry.
In the aspect of gas-solid phase catalytic reaction mechanism research, the reaction mechanism research is still in the preliminary stage due to the limitation of important reaction product detection technology. The method for detecting the intermediate product at the present stage mainly comprises methods such as GC-MS, in-situ infrared technology, in-situ nuclear magnetic technology and the like, but the GC-MS has secondary reaction, the product detection hysteresis is serious, and MS uses EI to bombard and ionize, so that the fragment peaks of the product are more, and the reaction species are not easy to determine; in-situ infrared spectroscopy is used for detecting vibration peaks of chemical bonds or functional groups of each molecule, the spectrogram attribution is complex, and the in-situ infrared spectroscopy can only be used as an auxiliary means for determining species at present; in-situ nuclear magnetic resonance can only detect reactive intermediate species at a certain moment, and cannot give accurate judgment on a nuclear magnetic resonance spectrogram of complex chemical substances. With the further development of the catalytic industry, people increasingly need to observe the change process of a reaction intermediate in situ, in real time and on line to deeply research the catalytic mechanism, so as to better guide the development of the catalytic industry. In the patent CN201310023135 and the patent CN201610087842, reaction intermediates of the catalytic process under normal pressure and low pressure are detected by in-situ mass spectrometry, but both are capillary sampling, and there still exists a real situation that many secondary reactions occur and the catalytic process cannot be real-time reacted online. However, the above in-situ catalytic detection devices only detect intermediates under low-pressure and normal-pressure environments, and cannot perform in-situ real-time on-line detection and analysis on catalytic processes and reaction products under high-pressure environments in the actual industrial catalytic processes.
SUMMERY OF THE UTILITY MODEL
In the research is surveyed to high-pressure gas solid phase catalytic reaction result, in order to reach the high-pressure reaction pressure the same with the industrial production condition, realize the real-time online sample of normal position of unstable midbody under the high pressure environment simultaneously to avoid the secondary reaction among the sample transmission process, the utility model provides an experimental apparatus for high-pressure gas solid phase catalytic reaction result is surveyed to normal position.
The specific technical solution is as follows:
an experimental device for in-situ detection of high-pressure gas-solid phase catalytic reaction products comprises a mass spectrometer 1 and a high-pressure catalytic reactor; the high-pressure catalytic reactor is vertically and hermetically arranged at the lower part of the mass spectrometer 1;
the high-pressure catalytic reactor comprises a high-pressure catalytic reaction mechanism 4, a heating mechanism 3 and a sampling nozzle 2;
the high-pressure catalytic reaction mechanism 4 comprises a sleeve 41, a pressure-bearing pipe 42 and a quartz reaction pipe 43 which are coaxially arranged from outside to inside; the upper part of the sleeve 41 is a circular tube, the top end of the upper part is a disc flange, two exhaust pipes 411 are symmetrically arranged on two sides of the circular tube on the upper part, and the lower part is a conical pipe; the lower end of the pressure bearing pipe 42 is open, the upper end is hemispherical, the center of the upper end is provided with a micropore 421, and the micropore 421 is a conical hole with a large outside and a small inside; the quartz reaction tube 43 is coaxially arranged inside the pressure-bearing tube 42, the front end of the quartz reaction tube 43 is adjacent to the micropores 421 of the pressure-bearing tube 42, and the rear end of the quartz reaction tube 43 extends to the outside of the pressure-bearing tube 42; small holes 434 are uniformly distributed on the front end face of the front end of the quartz reaction tube 43, and a catalyst 431 is packaged in the quartz reaction tube 43 corresponding to the front end face through quartz wool 432;
the heating mechanism 3 is sleeved outside the sleeve 41;
the rear end port of the sampling nozzle 2 is fixedly connected with the mass spectrometer 1, and the sampling port of the sampling nozzle 2 coaxially corresponds to the large-diameter end of the micropore 421 of the pressure bearing pipe 42 and is positioned in the upper part of the circular pipe of the sleeve 41;
in operation, the heating mechanism 3 heats the catalyst 431 in the quartz reaction tube 43 in the high-pressure catalytic reaction mechanism 4 to a reaction temperature; high-pressure gas-phase reactants enter from the rear end of the quartz reaction tube 43, so that a high-pressure environment is formed in the quartz reaction tube 43 and contacts with the catalyst 431 to perform catalytic reaction; the gas phase reaction product enters the pressure-bearing pipe 42 through the small hole 434 at the front end of the quartz reaction pipe 43, is ejected out through the micro hole 421 of the pressure-bearing pipe 42 to form an ultrasonic molecular beam, enters the sleeve 41, enters the mass spectrometer 1 through the sampling port of the sampling nozzle 2, and is detected by the mass spectrometer 1.
The technical scheme for further limiting is as follows:
the pressure range of the quartz reaction tube 43 during reaction is 0-4 MPa.
The aperture Φ a of the small-diameter end of the micro-holes 421 is 0.01-0.5 mm.
The aperture of the small hole at the front end of the quartz reaction tube 43 is phi 0.1-1mm, and the distance between the adjacent small holes is 0.1-1 mm.
The aperture of the sampling nozzle 2 is phi 0.05-0.5mm, and the distance d2 between the sampling opening of the sampling nozzle 2 and the micropore 421 of the pressure-bearing pipe 42 is 0.5-2 mm.
The radial clearance between the quartz reaction tube 43 and the pressure-bearing tube 42 is 0.5-2 mm.
The exhaust pipe 411 at one side is closed, and a first pressure sensor 412 is arranged at the closed end; the other side exhaust pipe 411 is connected with the outlet of the air pump 414 through an electric butterfly valve 413; the conical tube lower end of the casing tube 41 is connected with a joint seat 45 through an adapter 44, the rear end of the quartz reaction tube 43 extends into the joint seat 45 through the adapter 44, the outside of the joint seat 45 corresponding to the rear end of the quartz reaction tube 43 is communicated with a high-pressure joint outer tube 46, and the side surface of the high-pressure joint outer tube 46 is provided with a second pressure sensor 462 through a pressure measuring branch tube 461.
The upper part of the adapter 44 is sleeved on the pressure-bearing pipe 42, and the axial contact surface between the adapter 44 and the pressure-bearing pipe 42 is sealed by a first sealing ring 441; the lower part of the quartz reaction tube 43 is sleeved on the adapter 44, and the axial contact surface between the adapter 44 and the sleeve 41 is sealed by a second sealing ring 442; the adapter 44 and the connection end face of the adapter seat 45 are sealed by a third sealing ring 443, and the axial contact face of the quartz reaction tube 43 and the axial contact face of the adapter seat 45 are sealed by a fourth sealing ring 444.
The beneficial technical effects of the utility model are embodied in the following aspects:
1. the design of the micropore 421 micro inverted cone angle of the pressure bearing pipe 42 ensures that an in-situ high-pressure environment of 0-4MPa is formed in the quartz reaction pipe 43, and a high-pressure catalysis system of an industrial real system is simulated. The pressure-bearing pipe 42 has the structure that the micropores 421 are as close as possible to the quartz reaction pipe 43, and the micropores 421 are made into small holes d2= phi 0.01-0.5mm with different specifications, so that the pressure environment of 0-4MPa is adjustable.
2. By adopting the design of the micropores with inverted cone angles of the micropores 421 of the pressure-bearing pipe 42, the product can form ultrasonic molecular beams immediately after being discharged from the outlet of the high-pressure catalytic reactor, thereby greatly reducing the collision among unstable intermediates and better monitoring the catalytic reaction process in situ. Structurally, the micropores 421 of the pressure-bearing pipe 42 of the high-pressure catalytic reactor are designed and processed into a form of an inverted cone with the taper of 30-60 degrees, and the assembly distance with the sampling nozzle 2 is as close as possible to d2=0.5-2 mm.
3. The design of the quartz lining reaction tube 43 is adopted, so that the phenomenon that metal elements in stainless steel reaction tubes in most high-pressure catalytic systems have catalytic activity and influence the real catalytic performance of the catalyst is avoided. Structurally, a gap of 0.5-2mm is reserved between the quartz reaction tube 43 and the pressure-bearing tube 42 to balance pressure difference, so that the quartz reaction tube 43 with the inner lining can bear high pressure.
4. The inner wall of the pressure-bearing pipe 42 is passivated, so that the phenomenon that metal elements in a stainless steel reaction pipe in most high-pressure catalytic systems have catalytic activity and influence the real catalytic performance of the catalyst is avoided.
Drawings
FIG. 1 is a view showing a usage state of the present invention;
FIG. 2 is a cross-sectional view of a high pressure catalytic reactor body;
FIG. 3 is a schematic view of the assembly of the sleeve mechanism for support and fixation;
FIG. 4 is a schematic view of the main body of the stainless steel reaction outer tube;
FIG. 5 is an enlarged view of the stainless steel reaction outer tube round cap and the inverted cone angle micro-hole;
FIG. 6 is a structural diagram of a quartz reaction tube;
FIG. 7a is a mass spectrum of a product obtained at low pressure in a Fischer-Tropsch reaction experiment by using the experimental apparatus of the present invention;
FIG. 7b is a mass spectrum of a product obtained by the experimental apparatus of the present invention at a high pressure in a Fischer-Tropsch reaction experiment;
FIG. 8a is a graph showing the variation of signal intensity of time-resolved products at low pressure in a Fischer-Tropsch reaction experiment using the experimental apparatus of the present invention;
fig. 8b is a graph showing the signal intensity variation of the time-resolved product of the experimental apparatus of the present invention under high pressure in the fischer-tropsch reaction experiment.
Sequence numbers in the upper figure: the mass spectrometer comprises a mass spectrometer 1, a sampling nozzle 2, a heating mechanism 3, a high-pressure catalytic reactor 4, a sleeve 41, a pressure-bearing pipe 42, a quartz reaction pipe 43, a connector 44, a connector seat 45, a sealing ring 45, a high-pressure connector outer pipe 46, an exhaust pipe 411, an electric butterfly valve 413, an air suction pump 414, a micropore 421, a catalyst 431, quartz wool 432, a first sealing ring 441, a second sealing ring 442, a third sealing ring 443, a fourth sealing ring 444, a pressure-measuring branch pipe 461, a first pressure sensor 412 and a second pressure sensor 462.
Detailed Description
The invention will now be further described by way of example with reference to the accompanying drawings.
Example 1
Referring to fig. 1, an experimental apparatus for in situ detection of high pressure gas-solid phase catalytic reaction products includes a mass spectrometer 1 and a high pressure catalytic reactor. The high-pressure catalytic reactor is vertically and hermetically arranged at the lower part of an ionization chamber of the mass spectrometer 1.
The high-pressure catalytic reactor comprises a high-pressure catalytic reaction mechanism 4, a heating mechanism 3 and a sampling nozzle 2.
Referring to fig. 2, the high pressure catalytic reaction mechanism 4 includes a sleeve 41, a pressure-bearing pipe 42 and a quartz reaction pipe 43 coaxially arranged from outside to inside. The gap between the quartz reaction tube 43 and the pressure-bearing tube 42 was 0.5 mm. The upper portion of the sleeve 41 is a circular tube, the top end of the upper portion is a disc flange, two exhaust pipes 411 are symmetrically arranged on two sides of the circular tube on the upper portion, and the lower portion is a conical pipe. The exhaust pipe 411 at one side is closed, and a first pressure sensor 412 is arranged at the closed end; the other side exhaust pipe 411 is connected to the outlet of the air pump 414 via an electric butterfly valve 413. Referring to fig. 4, the lower end of the pressure-bearing pipe 42 is open, the upper end is hemispherical, a micropore 421 is arranged at the center of the top end, and the micropore 421 is a conical hole with a large outer part and a small inner part; referring to fig. 5, the aperture Φ a of the small-diameter end of the micro-hole 421 is 0.05mm, and the taper θ b is 30 °. Referring to fig. 6, small holes 434 are uniformly distributed on the front end face of the front end of the quartz reaction tube 43, the aperture of each small hole is 0.5mm, and the distance between every two adjacent small holes is 0.5 mm; the quartz reaction tube 43 is coaxially arranged inside the pressure-bearing tube 42, the front end of the quartz reaction tube 43 is adjacent to the micropores 421 of the pressure-bearing tube 42, and the rear end of the quartz reaction tube 43 extends to the outside of the pressure-bearing tube 42; the front end face of the front end of the quartz reaction tube 43 is uniformly provided with small holes 434, and the quartz reaction tube 43 corresponding to the front end face is internally packaged with a catalyst 431 through quartz wool 432.
Referring to fig. 3, the lower end of the conical tube of the casing 41 is connected to a joint base 45 through a joint 44, the rear end of the quartz reaction tube 43 extends into the joint base 45 through the joint 44, the exterior of the joint base 45 corresponding to the rear end of the quartz reaction tube 43 is communicated with a high-pressure joint outer tube 46, and a second pressure sensor 462 is installed on the side surface of the high-pressure joint outer tube 46 through a pressure measuring branch tube 461. The upper part of the adapter 44 is sleeved on the pressure-bearing pipe 42, and the axial contact surface between the adapter 44 and the pressure-bearing pipe 42 is sealed by a first sealing ring 441; the lower part of the adapter 44 is sleeved on the quartz reaction tube 43, and the axial contact surface between the adapter 44 and the quartz reaction tube 43 is sealed by a second sealing ring 442; the adapter 44 and the connection end face of the adapter seat 45 are sealed by a third sealing ring 443, and the axial contact face of the quartz reaction tube 43 and the axial contact face of the adapter seat 45 are sealed by a fourth sealing ring 444.
The rear end of the sampling nozzle 2 is fixedly connected with the mass spectrometer 1, and the sampling port of the sampling nozzle 2 coaxially corresponds to the micropore 421 of the pressure bearing pipe 42 and is positioned in the sleeve 41; the aperture of the sampling nozzle 2 is phi 0.05 mm; the spacing d2 between the sampling opening of the sampling nozzle 2 and the micro-hole 421 of the pressure-bearing pipe 42 is 0.5 mm.
In the experiment, the mass spectrometer 1, the sampling nozzle 2, the heating mechanism 3 and the high-pressure catalytic reactor 4 are sequentially installed into a whole. The pressure inside the casing 41 is controlled by a vacuum pump 414, an electric butterfly valve 413 and a first pressure sensor 412 connected to an exhaust pipe 411; the reaction pressure in the pressure-bearing pipe 42 and the quartz reaction pipe 43 is measured by the second pressure sensor 462.
The catalyst 431 used in the embodiment is a Fischer-Tropsch reaction catalyst cobalt/silicon dioxide (Co/SiO 2), the particle size is 0.6mm-0.8mm, the particle size is 30-40 meshes, the weight is 0.1g, silicon dioxide is used as a carrier, and metal cobalt is used as a load to be loaded on the carrier; the measured substance is a mixture of carbon monoxide and hydrogen (CO: H)2=2: 1), reaction pressure 1.3 MPa.
Introducing a mixture of carbon monoxide and hydrogen (CO: H) into the outer tube 46 of the high-pressure joint2=2: 1), flow rate of 200 SCCM; the opening size of the micropores 421 of the pressure-bearing pipe 42 is controlled to be phi 0.05mm, so that the catalytic reaction pressure in the pressure-bearing pipe 42 and the quartz reaction pipe 43 reaches 1.3 MPa. The heating mechanism 3 heats the catalyst 431 in the quartz reaction tube 43 in the high-pressure catalytic reaction mechanism 4 to a reaction temperature of 370 ℃; the gas to be measured passes through the high-pressure joint outer tube 46, then passes through the quartz reaction tube 43 to contact the catalyst 431 and carry out catalytic reaction, the reaction product enters the pressure-bearing tube 42 through a 0.5mm small hole at the front end of the quartz reaction tube 43, forms an ultrasonic molecular beam through a micropore 421 at the top end of the pressure-bearing tube, enters the sleeve 41, is sampled by the sampling nozzle 2 and then enters the mass spectrometer 1, and is ionized by synchronous radiation light to form ions, so that the mass-to-charge ratio of the ions of the measured product is determined.
See fig. 7a and 7b, thisThe figure is a photoionization mass spectrogram obtained when the synchrotron radiation photon energy is 11eV under the pressure of 1.3MPa, and a main product C2 =–C4 =、C5 =–C11 =、C12+Time-resolved relative intensity variation plots. From FIG. 7a, it is clear that the Fischer-Tropsch reaction products of ethylene (m/z = 28), propylene (m/z = 42), butylene (m/z = 56) are distributed in the classical AFS (Anderson-Schulz-Flor). From FIG. 7b it can be seen that at 1.3MPa, the main product C is2 =–C4 =、C5 =–C11 =、C12+The trend of signal intensity with temperature.
Example 2
The catalyst 431 used in the present embodiment is a fischer-tropsch catalyst cobalt/silica (Co/SiO 2), the particle size is 30-40 mesh, the weight is 0.1g, silica is used as a carrier, and metallic cobalt is used as a load to be loaded thereon; the measured substance is a mixture of carbon monoxide and hydrogen (CO: H)2=2: 1), reaction pressure 0.16 MPa.
Introducing a mixture of carbon monoxide and hydrogen (CO: H) into the outer tube 46 of the high-pressure joint2=2: 1), flow rate of 200 SCCM; the opening size of the micropores 421 of the pressure-bearing pipe 42 is controlled to be phi 0.10mm, so that the catalytic reaction pressure in the pressure-bearing pipe 42 and the quartz reaction pipe 43 reaches 0.16 MPa. The heating mechanism 3 heats the catalyst 431 in the quartz reaction tube 43 in the high-pressure catalytic reaction mechanism 4 to a reaction temperature of 370 ℃; the gas to be measured passes through the high-pressure joint outer tube 46, then passes through the quartz reaction tube 43 to contact the catalyst 431 and carry out catalytic reaction, the reaction product enters the pressure-bearing tube 42 through a small hole of 0.5mm at the front end of the quartz reaction tube 43, forms an ultrasonic molecular beam through the micropore 421 at the top end of the reaction product, enters the mass spectrometer 1 after being sampled by the sampling nozzle 2, and is ionized by synchronous radiation light to form ions, so that the mass-to-charge ratio of the ions of the product to be measured is determined.
Referring to FIGS. 8a and 8b, the photoionization mass spectra obtained at a synchrotron radiation photon energy of 11eV under a pressure of 0.16MPa, and the main product C2 =–C4 =、C5 =–C11 =、C12+Time-resolved relative intensity variation plots. From FIG. 8a, it is clear that the Fischer-Tropsch reaction products of ethylene (m/z = 28), propylene (m/z = 42), butylene (m/z = 56), etc. are distributed in the classical AFS (Anderson-Schulz-Flor) at 0.16 MPa. From FIG. 8b it can be seen that at 0.16MPa, the main product C is2 =–C4 =、C5 =–C11 =、C12+The trend of signal intensity with temperature.

Claims (7)

1. An experimental device for in situ detection of high pressure gas-solid phase catalytic reaction products, comprising a mass spectrometer (1), characterized in that: also includes a high pressure catalytic reactor; the high-pressure catalytic reactor is vertically and hermetically arranged at the lower part of the mass spectrometer (1);
the high-pressure catalytic reactor comprises a high-pressure catalytic reaction mechanism (4), a heating mechanism (3) and a sampling nozzle (2);
the high-pressure catalytic reaction mechanism (4) comprises a sleeve pipe (41), a pressure-bearing pipe (42) and a quartz reaction pipe (43) which are coaxially arranged from outside to inside; the upper part of the sleeve (41) is a circular tube, the top end of the upper part is a disc flange, two exhaust pipes (411) are symmetrically arranged on two sides of the circular tube on the upper part, and the lower part is a conical pipe; the lower end of the pressure-bearing pipe (42) is open, the upper end of the pressure-bearing pipe is hemispherical, the center of the upper end of the pressure-bearing pipe is provided with a micropore (421), and the micropore (421) is a conical hole with a large outer part and a small inner part; the quartz reaction tube (43) is coaxially arranged inside the pressure bearing tube (42), the front end of the quartz reaction tube (43) is adjacent to the micropores (421) of the pressure bearing tube (42), and the rear end of the quartz reaction tube (43) extends to the outside of the pressure bearing tube (42); small holes (434) are uniformly distributed on the front end face of the front end of the quartz reaction tube (43), and a catalyst (431) is packaged in the quartz reaction tube (43) corresponding to the front end face through quartz wool (432);
the heating mechanism (3) is sleeved outside the sleeve (41);
the rear end opening of the sampling nozzle (2) is fixedly connected with the mass spectrometer (1), and the sampling opening of the sampling nozzle (2) coaxially corresponds to the large-diameter end of the micropore (421) of the pressure bearing pipe (42) and is positioned in the upper part of the circular pipe of the sleeve (41).
2. The experimental apparatus for in-situ detection of high pressure gas-solid phase catalytic reaction products according to claim 1, wherein: the aperture phi a of the small-diameter end of the micropore (421) is 0.01-0.5 mm.
3. The experimental apparatus for in-situ detection of high pressure gas-solid phase catalytic reaction products according to claim 1, wherein: the aperture of the small hole at the front end of the quartz reaction tube (43) is phi 0.1-1mm, and the distance between the adjacent small holes is 0.1-1 mm.
4. The experimental apparatus for in-situ detection of high pressure gas-solid phase catalytic reaction products according to claim 1, wherein: the aperture of the sampling nozzle (2) is phi 0.05-0.5mm, and the distance d2 between the sampling opening of the sampling nozzle (2) and the micropore (421) of the pressure bearing pipe (42) is 0.5-2 mm.
5. The experimental apparatus for in-situ detection of high pressure gas-solid phase catalytic reaction products according to claim 1, wherein: the radial clearance between the quartz reaction tube (43) and the pressure bearing tube (42) is 0.5-2 mm.
6. The experimental apparatus for in-situ detection of high pressure gas-solid phase catalytic reaction products according to claim 1, wherein: the exhaust pipe (411) at one side is closed, and a first pressure sensor (412) is arranged at the closed end; the exhaust pipe (411) at the other side is connected with the outlet of the air pump (414) through an electric butterfly valve (413); the circular cone pipe lower extreme of sleeve pipe (41) is passing through adapter (44) and being connected joint seat (45), in the rear end of quartz reaction pipe (43) extended joint seat (45) through adapter (44), the outside of joint seat (45) that correspond with the rear end of quartz reaction pipe (43) is communicateing high pressure joint outer tube (46), and the side of high pressure joint outer tube (46) is equipped with second pressure sensor (462) through pressure measurement branch way pipe (461).
7. The experimental device for in-situ detection of high pressure gas-solid phase catalytic reaction products according to claim 6, wherein: the upper part of the adapter (44) is sleeved on the pressure-bearing pipe (42), and the axial contact surface between the adapter (44) and the pressure-bearing pipe (42) is sealed through a first sealing ring (441); the lower part of the quartz reaction tube (43) is sleeved on the adapter (44), and the axial contact surface between the adapter (44) and the sleeve (41) is sealed by a second sealing ring (442); the adapter (44) and the connection end face of the adapter seat (45) are sealed through a third sealing ring (443), and the axial contact surface of the quartz reaction tube (43) and the axial contact surface of the adapter seat (45) are sealed through a fourth sealing ring (444).
CN201920293858.XU 2019-03-08 2019-03-08 Experimental device for be used for high pressure gas solid phase catalytic reaction product of normal position survey Active CN210022078U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201920293858.XU CN210022078U (en) 2019-03-08 2019-03-08 Experimental device for be used for high pressure gas solid phase catalytic reaction product of normal position survey

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201920293858.XU CN210022078U (en) 2019-03-08 2019-03-08 Experimental device for be used for high pressure gas solid phase catalytic reaction product of normal position survey

Publications (1)

Publication Number Publication Date
CN210022078U true CN210022078U (en) 2020-02-07

Family

ID=69354389

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201920293858.XU Active CN210022078U (en) 2019-03-08 2019-03-08 Experimental device for be used for high pressure gas solid phase catalytic reaction product of normal position survey

Country Status (1)

Country Link
CN (1) CN210022078U (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109847655A (en) * 2019-03-08 2019-06-07 中国科学技术大学 A kind of experimental provision for in-situ investigation high pressure gas and solid phase catalyzing reaction product

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109847655A (en) * 2019-03-08 2019-06-07 中国科学技术大学 A kind of experimental provision for in-situ investigation high pressure gas and solid phase catalyzing reaction product
CN109847655B (en) * 2019-03-08 2024-01-05 中国科学技术大学 Experimental device for be used for normal position to survey high-pressure gas-solid phase catalytic reaction product

Similar Documents

Publication Publication Date Title
CN107576717B (en) A kind of in-situ detector being catalyzed reaction gas phase intermediate product for different diffusion lengths
CN210022078U (en) Experimental device for be used for high pressure gas solid phase catalytic reaction product of normal position survey
CN104713968A (en) Online analysis system and method for continuous monitoring of catalysis of ammonia synthesis reaction
CN106024572B (en) The organic matter detection means and detection method of a kind of bipolarity Proton transfer reaction mass spectrometry
CN103454125A (en) System and method for measuring hydrogen content in a sample
CN109847655B (en) Experimental device for be used for normal position to survey high-pressure gas-solid phase catalytic reaction product
CN102353799A (en) Method of evaporating sample injecting inducted by dielectric barrier discharge microplasma
CN104713938B (en) The on-line analysis system and method for a kind of continuous monitoring catalysis reduction nitrobenzene reaction
Henriksen et al. Highly sensitive silicon microreactor for catalyst testing
EP3767287B1 (en) Combination structure of uhv device interconnected in-situ reaction cell and built-in mass spectrum electric quadrupole rod
CN103084127A (en) High-temperature normal-pressure catalytic reactor suitable for mass spectrometry and application thereof
CN108160009A (en) A kind of reactor and application method of self-balancing bushing pipe external and internal pressure
WO2018210108A1 (en) Reaction control and mass spectrometry station for joint use with respect to in situ pool of x-ray expressing apparatus
Patil et al. Design, modelling, and application of a low void-volume in situ diffuse reflectance spectroscopic reaction cell for transient catalytic studies
CN109884002A (en) One kind measuring atmosphere OH and HO for chemical ionization mass spectrometry2The device and method of free radical
CN102938361B (en) A kind of mass spectrum ionization source of highly sensitive on-line analysis explosive and application thereof
CN212031360U (en) Single-channel real-time shunt rapid detection mass spectrometer and capillary sampling device
CN102938360A (en) Large-area in-situ testing explosive substance mass spectrum ionization source and application thereof
CN114563464A (en) Pressure-adjustable steady-state isotope transient fast response reaction device
CN106769346B (en) Method for analyzing hydrogen isotopes in water
CN214428596U (en) Mass spectrometry system
CN217305009U (en) Transient catalytic reaction mass spectrum detection device
CN102762022A (en) Method for generating glow discharge plasma and special device for method
CN109884168B (en) Device and method for real-time online analysis of catalytic reaction process
CN105784917B (en) Application of the mass spectrograph during detection is catalyzed reactive ion intermediate

Legal Events

Date Code Title Description
GR01 Patent grant