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CN-122016656-A - Metal mesh substrate for in-situ infrared test and preparation method and application thereof

CN122016656ACN 122016656 ACN122016656 ACN 122016656ACN-122016656-A

Abstract

The invention provides a metal mesh substrate for in-situ infrared test and a preparation method and application thereof. The invention adopts the metal net with specific materials and forms to support the sample preparation, can completely replace the traditional self-supporting sample preparation, greatly simplifies the sample preparation process, overcomes the problems that various catalysts are difficult to prepare the sample or have poor effect after sample preparation due to the physical and chemical properties of the catalysts, and makes the advanced catalysis in-situ research means of in-situ infrared characterization easier to use.

Inventors

  • HU XIAOYU
  • WANG BIN
  • JIANG JIANZHUN
  • SHI ZHAN
  • SHANG YIMEI
  • GAO SHUSHU
  • LI JING

Assignees

  • 中国石油化工股份有限公司
  • 中石化(北京)化工研究院有限公司

Dates

Publication Date
20260512
Application Date
20241112

Claims (10)

  1. 1. The metal mesh substrate for in-situ infrared test comprises a single-layer metal mesh which is subjected to fine grinding treatment by adopting a polishing solution, wherein the light transmittance of the metal mesh substrate in a middle infrared band is 25-80%.
  2. 2. The metal mesh substrate of claim 1, wherein, The mesh number of the single-layer metal mesh is 20-120 meshes, the wire diameter is 0.05-0.25 mm, and preferably, the mesh number of the single-layer metal mesh is 20-100 meshes, and the wire diameter is 0.09-0.2 mm.
  3. 3. The wire mesh substrate according to claim 1, wherein the wire mesh is made of at least one metal material selected from the group consisting of titanium, tungsten, and stainless steel.
  4. 4. A method for preparing a metal mesh substrate for in-situ infrared testing according to any one of claims 1 to 3, comprising the step of subjecting the cleaned metal mesh to fine grinding treatment by polishing liquid.
  5. 5. The preparation method according to claim 4, comprising the following steps: (1) Soaking and cleaning the metal net for the first time by adopting alkaline solution, soaking and cleaning for the second time by adopting acid solution, and drying; (2) And (3) placing the dried metal net obtained in the step (1) in a grinding polisher for fine grinding treatment, and then cleaning and drying to obtain the metal net substrate.
  6. 6. The method according to claim 5, wherein in the step (1): the alkaline compound in the alkaline solution is selected from at least one of inorganic alkaline compounds, preferably at least one of sodium hydroxide and sodium carbonate, and/or, The concentration of the alkaline compound in the alkaline solution is 0.5-10 mol/L, preferably 0.5-2 mol/L, and/or, The acidic compound in the acidic solution is selected from at least one of inorganic acids, preferably at least one of HCl, carbonic acid, nitrous acid, and/or, The concentration of the acidic compound in the acidic solution is 0.05-10 mol/L, preferably 0.1-2 mol/L.
  7. 7. The method according to claim 5, wherein in the step (1): The first soaking time is 1-12 hours, preferably 1-6 hours, and/or, The second soaking time is 1-12 hours, preferably 1-6 hours, and/or, The cleaning adopts an ultrasonic cleaning mode, preferably, the cleaning temperature is 0-45 ℃, and/or, The drying condition in the step (1) is that the drying is carried out for 0.5-2 hours at 80-120 ℃, preferably for 1-2 hours at 100-120 ℃.
  8. 8. The method according to claim 5, wherein, The conditions of the fine grinding treatment in the step (2) include: the diamond grinding sheet is adopted, preferably, the mesh number of the diamond grinding sheet is 100-800 meshes, and/or, A polyurethane polishing pad is used, and/or, The rotation speed of the polishing disk is 10-60 r/min, and/or, The polishing solution comprises hydrogen peroxide, silicon dioxide and water, preferably, the concentration of the hydrogen peroxide in the polishing solution is 1-5wt%, the concentration of the silicon dioxide is 10-30wt%, and/or, The flow rate of the polishing solution is 1-10 mL/min, preferably 1-5 mL/min, and/or, The polishing and refining time is 1-30 min, preferably 5-15 min.
  9. 9. The method according to claim 5, wherein, The step (2) adopts an ultrasonic cleaning mode, preferably the cleaning solvent is an alcohol solvent, the cleaning time is 30-180 min, and/or, The drying condition in the step (2) is that the drying is carried out for 0.5-4 hours at 80-120 ℃.
  10. 10. A method for testing a solid catalyst by in-situ infrared comprises the steps of paving a catalyst sample on a metal mesh substrate and performing in-situ infrared test after tabletting, wherein the metal mesh substrate is the metal mesh substrate for in-situ infrared test according to any one of claims 1-3 or the metal mesh substrate for in-situ infrared test obtained by the preparation method according to any one of claims 4-9, and preferably, the tabletting is carried out under the condition that the pressure is 0-4 MPa and/or the time is 10-60 s.

Description

Metal mesh substrate for in-situ infrared test and preparation method and application thereof Technical Field The invention belongs to the technical field of infrared spectrum testing, and particularly relates to a metal mesh substrate for in-situ infrared testing, and a preparation method and application thereof. Background Catalytic in-situ characterization is an advanced catalytic research method, and in-situ molecular spectroscopy, particularly in-situ infrared spectroscopy, is the most important means of in-situ research. In the catalytic in situ characterization by means of in situ infrared transmission spectroscopy, it often involves a critical process of preparing a pure solid catalyst sample into a self-supporting sheet of 13mm diameter, complete and uniform. Based on the influence of diffraction effect and the requirement of spectral transmittance, the thickness of the thin sheet should be below 100 micrometers, if the thin sheet is too thick, infrared light cannot penetrate through a sample, if the sample is incomplete, serious scattering effect can be generated, and the thin sheet of the sample must have certain strength, otherwise, in-situ measurement cannot be performed stably in the environment atmosphere of high-low temperature change, vacuum, high pressure, gas flow and the like. These demanding requirements for sample preparation increase the difficulty of implementing in-situ infrared characterization because the nature of many catalysts is not conducive to the formation of samples that meet the measurement requirements, for example, some catalysts are poorly formable and difficult to form into sheets with a certain strength, some catalysts have a certain viscosity, are very easy to adhere to tabletting dies and cannot be demolded, and strongly absorbing samples, such as dark catalysts, that have very low intrinsic transmittance must be formed into self-supporting sheets of a thinner thickness with a smaller number of samples to ensure infrared light transmission. Scientific research and experimenters are often limited by experimental technology of the in-situ infrared sample preparation process, and a great deal of time and effort are spent, but high-quality data results cannot be obtained, and even the data results are blocked from being directly beyond a threshold of in-situ infrared characterization. Disclosure of Invention In order to solve the technical problems, the invention provides a metal mesh substrate for in-situ infrared test, and a preparation method and application thereof. The invention adopts the metal net with specific material and shape as the substrate in the in-situ infrared test to support the sample preparation, can completely replace the traditional self-supporting sample preparation, and can overcome the problems that various catalysts are difficult to prepare the sample or have poor effect after the sample preparation due to the physical and chemical properties of the catalysts. The invention aims to provide a metal mesh substrate for in-situ infrared test, which comprises a single-layer metal mesh subjected to fine grinding treatment by using polishing solution, wherein the light transmittance of the metal mesh substrate in a middle infrared band (400-4000 cm -1) is 25-80%. According to the present invention, the mesh number of the single-layer metal mesh is 20 to 120 mesh (for example, the mesh number of the metal mesh may be 20, 30, 40, 50, 60, 70, 80, 90, 100, 110, 120 mesh or a value between any two of the above ranges), the wire diameter is 0.05 to 0.25mm (for example, the wire diameter of the metal mesh may be 0.05、0.06、0.07、0.08、0.09、0.1、0.11、0.12、0.13、0.14、0.15、0.16、0.17、0.18、0.19、0.2、0.21、0.22、0.23、0.24、0.25mm or a value between any two of the above ranges), and preferably, the mesh number of the single-layer metal mesh is 20 to 100 mesh, and the wire diameter is 0.09 to 0.2mm. According to the invention, the metal material adopted by the metal net is at least one selected from titanium, tungsten and stainless steel. The second objective of the present invention is to provide a method for preparing a metal mesh substrate for in-situ infrared test according to one of the objectives of the present invention, which includes a step of finely grinding the cleaned metal mesh with a polishing solution. According to the invention, the preparation method of the metal mesh substrate for in-situ infrared test specifically comprises the following steps: (1) Soaking and cleaning the metal net for the first time by adopting alkaline solution, soaking and cleaning for the second time by adopting acid solution, and drying; (2) And (3) placing the dried metal net obtained in the step (1) in a grinding polisher for fine grinding treatment, and then cleaning and drying to obtain the metal net substrate. According to the invention, in the step (1) of the preparation method of the metal mesh substrate for in-situ infrared test: The alkaline compound in the alkaline solutio