CN-122016887-A - Membrane catalytic in-situ reaction tank based on combination of X-ray absorption spectrum and multi-mode spectrum

CN122016887ACN 122016887 ACN122016887 ACN 122016887ACN-122016887-A

Abstract

The invention belongs to the technical field of scientific instruments and heterogeneous catalysis characterization, and discloses a membrane catalysis in-situ reaction tank based on the combination of an X-ray absorption spectrum and a multi-mode spectrum, which comprises a shell, a reaction tank body and a reaction tank, wherein an installation cavity is arranged on the shell; the device comprises a shell, a reaction platform arranged on an installation cavity of the shell, a cover body assembly arranged on the reaction platform, a window used for installing an optical window, a fluid transmission unit and a gas inlet pipe, wherein the reaction cavity is formed between the cover body assembly and the reaction platform, a sample reacts in the reaction cavity, the window used for installing the optical window is arranged on the cover body assembly, an acute angle included angle is formed between a central axis of the window and a base plane provided by the reaction platform, the optical window comprises a first group of window applicable to X-rays and a second group of window applicable to molecular spectrums, the fluid transmission unit comprises an air inlet pipe for inputting a gas reactant into the reaction cavity and an air outlet pipe for discharging the gas in the reaction cavity, the air inlet pipe is arranged on the cover body assembly, and the air outlet pipe is arranged on the reaction platform.

Inventors

LI ZHAOHUA
ZHU MINGHUI
XU ZHI
GU HAOYUAN
LEI LINFENG
SHAO FENG

Assignees

苏州实验室

Dates

Publication Date: 20260512
Application Date: 20260317

Claims (10)

1. A membrane catalytic in-situ reaction cell based on the combination of an X-ray absorption spectrum and a multimode spectrum, which is characterized by comprising: A housing (10) provided with a mounting cavity; the reaction platform (20) is arranged on the mounting cavity of the shell (10); The device comprises a reaction platform (20), a cover body assembly (30), a window (32) and a light source, wherein the cover body assembly (30) is arranged on the reaction platform (20) so that a reaction cavity is formed between the cover body assembly (30) and the reaction platform (20), and a sample reacts in the reaction cavity; The fluid transmission unit comprises an air inlet pipe (40) for inputting a gaseous reactant into the reaction cavity and an air outlet pipe (50) for discharging the gas in the reaction cavity, wherein the air inlet pipe (40) is arranged on the cover body assembly (30), and the air outlet pipe (50) is arranged on the reaction platform (20).
2. The membrane catalytic in-situ reaction cell based on the combination of the X-ray absorption spectrum and the multimode spectrum according to claim 1, wherein an acute included angle formed between a central axis of the window (32) and a base plane provided by the reaction platform (20) is 40-50 degrees.
3. The membrane-catalyzed in situ reaction cell based on the combination of X-ray absorption spectroscopy and multimode spectroscopy according to claim 1, wherein the window (32) comprises an entrance window and an exit window arranged opposite; the light path configuration of the in-situ reaction tank is configured such that incident light is horizontally incident through an incident window in the window (32), and reflected light excited by the reaction platform (20) is emitted in a direction perpendicular to the incident light through an emergent window in the window (32) and received by a detector.
4. The membrane catalytic in situ reaction cell based on the combination of X-ray absorption spectrum and multimode spectrum according to claim 3, characterized in that the window (32) comprises a first window (321) for mounting the first set of louvers and a second window (322) for mounting the second set of louvers, a first central line of the first window (321) and the exit window and a second central line of the second window (322) are distributed in a cross-shape; the intersection angle of the first central connecting line and the second central connecting line is 90 degrees.
5. The membrane catalytic in situ reaction cell based on the combination of X-ray absorption spectroscopy and multimode spectroscopy according to claim 1, wherein: the first group of optical window sheets (31) is made of one or more of diamond, beryllium, polyimide and ultrathin glass; The second set of optical panes (31) has a quality selected from one or more of the group of zinc selenide, calcium fluoride, potassium bromide, sodium chloride, magnesium fluoride, sapphire, quartz, silicon.
6. The membrane catalytic in situ reaction cell based on the combination of X-ray absorption spectroscopy and multimode spectroscopy according to claim 1, characterized in that the cover assembly (30) comprises a dome (dome) in hemispherical structure and a fastener (35) for sealing and fastening the dome (dome) on the reaction platform (20) by a sealing ring (34); In a sealed and buckled state, the fastening piece (35) is sleeved outside the dome (33) and is fixed on the shell (10) through a fastening bolt (36).
7. The membrane catalytic in-situ reaction cell based on the combination of X-ray absorption spectrum and multimode spectrum according to claim 1, wherein the reaction platform (20) comprises a bearing disc (21) provided with a circular arc-shaped groove (22) and lateral interface seats (23), and the lateral interface seats (23) are aligned and configured at two ends of the circular arc-shaped groove (22) and used for penetrating and sealing a tubular sample.
8. The membrane catalytic in-situ reaction cell based on the combination of the X-ray absorption spectrum and the multi-mode spectrum according to claim 7, wherein the lateral interface seat (23) and a tubular sample penetrating into the lateral interface seat are sealed through a flexible sealing structure, the flexible sealing structure comprises a flexible pressing ring (24) sleeved on the tubular sample and a clamping sleeve nut (25) for enabling the flexible pressing ring (24) to be tightly pressed on the tubular sample in a sealing mode, and the flexible pressing ring (24) is selected from a graphite ring, a fluororubber ring, a perfluoroether rubber ring or a metal C-shaped ring.
9. The membrane catalytic in-situ reaction tank based on the combination of the X-ray absorption spectrum and the multi-mode spectrum according to claim 7, wherein a support column (26) which can be in penetrating fit with a heating rod (27) and a thermocouple (28) is arranged at the lower part of the bearing disc (21), a central flow channel (29) penetrating through the circular arc-shaped groove (22) from the air outlet pipe (50) is arranged at the center of the support column (26), and the tail end of the thermocouple (28) extends into the circular arc-shaped groove (22) through the central flow channel (29) so as to abut against a tubular sample.
10. The membrane catalytic in-situ reaction cell based on the combination of X-ray absorption spectrum and multimode spectrum according to claim 1, characterized in that a circulating cooling water channel (11) surrounding the outside of the reaction platform (20) is arranged inside the shell (10); The materials of the shell (10) and the reaction platform (20) are selected from high temperature resistant and corrosion resistant alloys including but not limited to 316 stainless steel, 304 stainless steel, hastelloy, inconel or titanium alloy.

Description

Membrane catalytic in-situ reaction tank based on combination of X-ray absorption spectrum and multi-mode spectrum Technical Field The invention belongs to the technical field of scientific instruments and heterogeneous catalysis characterization, and particularly relates to a membrane catalysis in-situ reaction tank based on combination of an X-ray absorption spectrum and a multi-mode spectrum. Background In traditional catalytic reaction studies, the catalyst reaction process is often difficult to observe directly, especially in membrane reactor technology. The membrane reactor technology can couple the catalytic reaction and the product separation process, break thermodynamic equilibrium limit, greatly improve catalytic performance and product selectivity, and is widely applied to the processes of natural gas conversion, hydrogen purification, methanol reforming hydrogen production and the like. In-situ (In-situ) or operating (Operando) characterization is critical In order to understand the structure-activity relationship of the membrane catalyst under practical operating conditions. In recent years, X-ray absorption spectroscopy (XAS) technology has been widely used as an advanced characterization tool in research in the fields of nanomaterials and catalysts. XAS is capable of providing information about the electronic structure of the catalyst and the coordination environment, which is critical to understanding the activity and selectivity of the catalyst. Meanwhile, multimode spectrum (including infrared spectrum, raman spectrum, ultraviolet-visible spectrum, etc.) is widely used in biological and chemical research because it can provide information on molecular vibration and adsorbed species at the same time. However, existing in situ spectral characterization devices still have the following significant limitations: 1. Sample morphology limitations mainstream in situ reaction cells are often designed for powder or pellet samples and cannot effectively load, hold and seal tubular membrane catalysts (e.g., hollow fiber membranes) with curvature. 2. Single characterization limitations current in situ reaction cells are typically only amenable to single spectroscopic testing. The X-ray absorption spectrum can provide the electronic structure and fine coordination environment of the catalyst, while the infrared spectrum or raman spectrum can detect surface adsorbed species and molecular vibration information. 3. The high temperature and high pressure conflict with the light path, namely, under the working condition of high temperature and high pressure, the reaction tank needs thick-wall metal and a complex cooling system, which often can shade the light path. In particular, the fluorescent mode of XAS generally requires a detector at 90 ° to the incident light, while diffuse reflection of infrared also requires a specific angle of incidence and reflection, and arranging multiple windows in a limited space without interfering with each other is a significant engineering challenge. Disclosure of Invention In view of the above, the present invention aims to provide a membrane catalytic in-situ reaction cell based on the combination of an X-ray absorption spectrum and a multimode spectrum. In order to achieve the above purpose, the present invention provides the following technical solutions: a membrane catalytic in-situ reaction cell based on the combination of X-ray absorption spectroscopy and multimode spectroscopy, comprising: A housing provided with an installation cavity; The reaction platform is arranged on the mounting cavity of the shell; The cover body assembly is arranged on the reaction platform, so that a reaction cavity is formed between the cover body assembly and the reaction platform, and a sample reacts in the reaction cavity; the cover body component is provided with a window for installing an optical window, an acute angle is formed between the central axis of the window and a base plane provided by the reaction platform, and the optical window comprises a first group of window sheets applicable to X rays and a second group of window sheets applicable to molecular spectrums; the fluid transmission unit comprises an air inlet pipe for inputting a gaseous reactant into the reaction cavity and an air outlet pipe for discharging the gas in the reaction cavity, the air inlet pipe is arranged on the cover body assembly, and the air outlet pipe is arranged on the reaction platform. Preferably, an acute included angle formed between the central axis of the window and a base plane provided by the reaction platform is 40-50 degrees. Preferably, the window comprises an incident window and an emergent window which are oppositely arranged; The light path configuration of the in-situ reaction tank is configured such that incident light is horizontally incident through an incident window in the window, and reflected light excited by the reaction platform is emitted in a direction perpendicular to the