Device for evaluating gas-gas catalytic reaction activity of solid reactant

Abstract

The invention discloses a solid reactant gas-gas catalytic reaction activity evaluation device which comprises a reaction tube, a reaction gas inlet is formed in the upper end of the reaction tube, a reactant supply area, a catalytic reaction area and a product cleaning area are sequentially arranged in the reaction tube from top to bottom, and a catalyst layer is mounted in the catalytic reaction area. The catalyst layer is hermetically attached to the inner wall of the reaction tube; a reactant container I with an upper hole is arranged in the reactant supply area, a reactant container II is further arranged outside the reaction tube, the lower end of the reactant container II is communicated with the lower end of the reactant container I through a pipeline, and a sealing cover is arranged at the upper end of the reactant container II; a product collecting container is arranged in the product cleaning area, the opening end of the product collecting container is located in the product cleaning area, and the product collecting container and the product cleaning area are detachably and hermetically connected; and a heating layer is arranged on the outer wall of the reaction tube corresponding to the catalytic reaction area and the reactant supply area. According to the invention, online supply of reactants is realized, shutdown cooling and cleaning are not needed, and durability evaluation of the catalyst for more than 1000 hours can be supported.

Description

Technical Field

[0001] This invention relates to the field of catalytic performance evaluation equipment technology, and more specifically, to a device for evaluating the activity of solid reactant gas-to-gas catalytic reactions. Background Technology

[0002] In the field of catalytic material research and development, evaluating the activity and durability of catalysts is a core aspect, especially for reactants that are solid at room temperature but liquefy or vaporize upon heating to participate in the reaction (such as solid alcohols, solid organic acids, and low-melting-point organometallic compounds). The corresponding gas-to-gas catalytic reactions typically require reaction temperatures of 300-500℃. Evaluation devices for these reactions face several technical bottlenecks, such as the discontinuous nature of reactant replenishment. Existing catalytic evaluation devices (such as fixed-bed reactors) often use a single, closed reactant container, allowing only one-time loading of reactants. Once the solid reactants at room temperature liquefy and are consumed, the reactor must be shut down for cooling and the device reopened to replenish the sample. This not only interrupts the reaction process but also causes abnormal catalyst activity due to temperature fluctuations (e.g., shutdown at high temperatures can easily lead to catalyst sintering), making it impossible to obtain continuous and stable catalyst lifetime data.

[0003] Furthermore, blockage and maintenance issues at the reaction outlet are also common problems in these types of reactions. Incompletely reacted liquefied reactants or reaction products with high melting points can be carried by the gas flow to the low-temperature outlet region, where they rapidly condense into solid particles (e.g., reactions where the reactants or products are sulfur). Traditional apparatus often uses straight-pipe outlets without dedicated collection and cleaning components, leading to easy accumulation and blockage of the pipes. This can cause a sudden increase in reaction pressure, interruption of gas flow, and premature termination of the experiment. While some apparatuses have added filter components, these are often integrated with the reaction tubes, requiring disassembly of the entire reaction system for cleaning. This process is complex and time-consuming (1-2 hours per cleaning cycle), severely impacting experimental efficiency.

[0004] In summary, existing technologies cannot simultaneously meet the requirements for catalyst durability evaluation that involves "online replenishment of reactants and rapid cleaning of effluent solids." There is an urgent need for an integrated, continuous, and highly adaptable dedicated experimental device. Summary of the Invention

[0005] To address the issues of online reactant replenishment and outlet solid condensation cleanup in existing technologies, this invention provides a solid reactant gas-to-gas catalytic reaction activity evaluation device. This device enables online reactant replenishment without shutdown for cooling, solving the core problem of "interruption of experimentation due to shutdown" in traditional devices. It can support catalyst durability evaluation for more than 1000 hours.

[0006] The technical solution adopted is as follows: A device for evaluating the activity of a solid reactant gas-to-gas catalytic reaction includes a reaction tube with a reactant gas inlet at its upper end. Inside the reaction tube, from top to bottom, are a reactant supply zone, a catalytic reaction zone, and a product cleaning zone. A catalyst layer is installed in the catalytic reaction zone, and the catalyst layer is sealed to the inner wall of the reaction tube. A reactant container I with an upper opening is located in the reactant supply zone. A reactant container II is also located outside the reaction tube, with its lower end connected to the lower end of reactant container I via a pipeline. A sealing cap is provided at the upper end of reactant container II. A product collection container is located in the product cleaning zone, with its opening located within the product cleaning zone; the two are detachably and sealed together. A heating layer is provided on the outer wall of the reaction tube corresponding to the catalytic reaction zone and the reactant supply zone.

[0007] Furthermore, the outer wall of the reactant container II and the outer wall of the reaction tube corresponding to the product cleaning area are respectively provided with heat insulation layers.

[0008] Preferably, the product collection container is a cylindrical structure with an opening at the top and an air vent at the bottom. A high-temperature resistant filter layer is laid on its inner wall, and a sealing ring is provided near the outer side of the upper opening of the product collection container. The product collection container is screwed tightly sealed to the inner wall of the product cleaning area.

[0009] Preferably, a scale is provided on the reactant container II.

[0010] Preferably, the height of reactant container II is greater than or equal to the height of reactant container I.

[0011] Preferably, the catalyst layer includes a catalyst sample and fasteners, wherein the catalyst sample is fixed in the catalytic reaction zone by the fasteners.

[0012] Preferably, the reaction tube, reactant container I, and reactant container II are integrally formed.

[0013] The technical solution of the present invention has the following advantages: The device of this invention adopts a vertical integrated structure, with a reactant supply zone, a catalytic reaction zone, and a product cleaning zone set up in the reaction tube. The reactant supply zone is equipped with a reactant container I with a perforated cover and a spare reactant container II, preferably combined with a heat insulation layer to achieve online supply and stable liquefaction of solid reactants. A catalyst layer and a heating layer are installed in the catalytic reaction zone to achieve precise temperature control. A quick-release product collection container is set up in the product cleaning zone to achieve online cleaning of condensed solids at the outlet. This solves the problems of reactant supply interruption, outlet blockage, and cumbersome operation of traditional devices. It can support catalyst durability tests for long-term operation (more than 1000 hours) and has the characteristics of continuous operation, strong adaptability, high efficiency, safety and stability. It is suitable for the evaluation of gas-to-gas catalytic reactions of solids at room temperature and heated liquefied reactants. Attached Figure Description

[0014] To more clearly illustrate the specific embodiments of the present invention, the accompanying drawings used in the specific embodiments will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0015] Figure 1 This is a cross-sectional view of the overall structure of the catalytic reaction activity evaluation device provided by the present invention.

[0016] The meanings of the symbols in the image are as follows: 1-Reaction tube, 11-Reaction gas inlet 1a - Reactant supply zone, 1b - Catalytic reaction zone, 1c - Product cleanup zone 2-Catalyst Layer 21-Catalyst sample, 22-Fasteners 3-Reactant Container I 31-Cover body, 31a-Top opening 4-Reactant Container II 41-Sealing cap 5-Product collection container 51-Air outlet 6-Heating layer; 7-Insulation layer; 8-High temperature resistant filter layer; 9-Sealing ring; 10-Support. Detailed Implementation

[0017] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0018] like Figure 1 As shown, this invention provides a device for evaluating the activity of a solid reactant gas-to-gas catalytic reaction, comprising a reaction tube 1, with a reaction gas inlet 11 at the upper end of the reaction tube 1 for continuously introducing reaction gas. Inside the reaction tube 1, from top to bottom, are arranged a reactant supply zone 1a, a catalytic reaction zone 1b, and a product cleaning zone 1c. A catalyst layer 2 is installed in the catalytic reaction zone 1b, and the catalyst layer 2 is sealed to the inner wall of the reaction tube 1. Preferably, the catalyst layer 2 is located in the middle region of the reaction tube 1. The reactant supply zone 1a is provided with a reactant container 13 with an upper opening 31a, which can... A cover 31 is provided at the upper open end of the reactant container I3, and the upper opening 31a is located in the middle of the cover 31. At the same time, a reactant container II4 is provided outside the reaction tube 1. The lower end of the reactant container II4 is connected to the lower end of the reactant container I3 through a pipeline. The upper end of the reactant container II4 is provided with a sealing cover 41. The amount of reactants inside can be observed through the reactant container II4. Reactants can also be replenished through the reactant container II4 to achieve continuous feeding. Preferably, the height of the reactant container II4 is greater than or equal to the height of the reactant container I3.

[0019] To address the existing shutdown and cleaning issues, this invention also includes a product collection container 5 in the product cleaning zone 1c. The opening of the product collection container 5 is located in the product cleaning zone 1c, and the two are detachably sealed. A heating layer 6 is provided on the outer wall of the reaction tube 1 corresponding to the catalytic reaction zone 1b and the reactant supply zone 1a. By heating the reaction tube 1 at high temperature through the heating layer 6, the reactant supply zone and the catalytic reaction zone can quickly reach the predetermined temperature. The heating zone 6 can provide a reaction temperature of 300-500℃. The solid reactants in the reaction container 13 are liquefied after heating and mix with the reaction gas introduced from above to form a gas-gas reaction system, which then undergoes a catalytic reaction through the catalyst layer. The gas after the reaction is slowly cooled in the product cleaning zone, and the unreacted reactants condense into solids and adhere to the product collection container 5. The condensed solids can be quickly cleaned by rapidly disassembling the product collection container 5 without stopping the heating and catalytic reaction, greatly improving the efficiency of catalytic reaction activity evaluation.

[0020] To slowly lower the temperature of the reactants after the catalytic reaction and slow down the condensation rate of unreacted reactants, allowing them to condense completely in the product collection container, a heat insulation layer 7 is installed on the outer wall of the reaction tube 1 corresponding to the product cleaning zone 1c. This area does not have a heating zone; instead, the heat insulation layer structure is used directly to achieve a temperature of 120-150℃. The product collection container 5 used in this invention is a cylindrical structure with an open top and a vent 51 at the bottom. A high-temperature resistant filter layer 8 is laid on its inner wall. A sealing ring 9, preferably a high-temperature resistant O-ring, is provided near the outer side of the upper opening of the product collection container 5 to ensure the high-temperature sealing of the reaction tube 1. The product collection container 5 is tightly sealed to the inner wall of the product cleaning zone 1c. The lower part of the product collection container 5 extends from the lower end of the reaction tube 1. The condensed solid is captured by the high-temperature resistant filter layer 8 (preferably filter paper) and the purified gas is discharged from the particulate-free gas outlet 51. A gas chromatograph with a PDF detector can be connected to the gas outlet 51 to detect the concentration of the reaction product carbonyl sulfide.

[0021] Meanwhile, an insulation layer 7 is also wrapped around the outer wall of the reactant container II4 and the connecting pipes, so that the solid reactants placed in the reactant container II4 can be gradually heated. In conjunction with the insulation layer 7, the solid reactants can be replenished online and liquefied stably. For example, the temperature of the reactants in the reactant container II can be raised to 120-150℃, maintaining a stable temperature inside the container and allowing the solid reactants to continuously liquefy into reaction raw materials.

[0022] To facilitate observation of the amount of reactant used in reactant container II4, a scale is installed on reactant container II4. When the reactant level drops to the lowest set scale line, the sealing cap 41 on reactant container II4 needs to be opened, reactant added, and then the sealing cap 41 should be promptly placed on the upper opening of reactant container II4 to complete the online reactant replenishment.

[0023] The catalyst layer 2 used in this invention includes a catalyst sample 21 and a fastener 22. The catalyst sample 21 is fixed in the catalytic reaction zone 1b by the fastener 22. The periphery of the catalyst sample 21 and the inner wall of the reaction tube need to be completely sealed.

[0024] Of course, during the manufacturing process, a support 10 can be installed at the lower end of the reaction tube 1 to form a whole structure of the reaction tube 1, the reactant container I3 and the reactant container II4.

[0025] Example: Long-term performance evaluation of catalysts for the synthesis of carbonyl sulfide from the reaction of CO and sulfur.

[0026] Open the cap 31 at the top of reactant container I3 and add 20 grams of sulfur powder into reactant container I3. Tighten the cap 31 with holes. Open the sealing cap 41 at the top of reactant container II4 and add 20 grams of sulfur powder to reactant container II4. Tighten the sealing cap 41. Fix the integral catalyst sample 21 to the catalyst fastener 22, ensuring that there is no gap between the catalyst and the inner wall of the reaction tube 1. Insert the high-temperature resistant filter layer 8 into the product collection container 5 with a cylindrical bottom liner, install the quick-release product collection container 5 and tighten the seal. Air tightness test:

[0027] Close the vent 51 at the bottom of the product collection container 5, introduce N2 through the reaction gas inlet 11, and maintain the pressure at 0.1 MPa; check for air leaks at the temperature-resistant O-ring seal 9, quick-release port, and other parts, and discharge the inert gas after confirming that the airtightness is qualified. Catalyst reaction

[0028] Start the insulation layer 7 of the reactant container II and set its temperature to 150℃; start the heating zone of the catalytic reaction zone and raise the temperature to 450℃ at a rate of 5-10℃ / min to stabilize the device temperature.

[0029] CO reaction gas is introduced through the reaction gas inlet 11, and the gas flow rate is controlled at 100 mL / min. When the reaction gas passes through the reactant container I3, it mixes with the gasified sulfur vapor to form a gas-gas reaction system, and then undergoes a catalytic reaction through the catalyst layer. After the reaction, the gas is slowly cooled by the insulation layer of the product cleaning zone 1c. Unreacted reactants condense into solids and are captured by the high-temperature resistant filter layer (such as filter paper) laid in the product collection container. The purified gas is discharged from the particulate-free outlet 51. Online supply and cleanup

[0030] Online replenishment of reactants: Observe the sulfur liquid level in reactant container II4 using a ruler. When the liquid level drops to only 10% of the container's mark, add solid sulfur to the 75% mark, tighten the sealing cap 41, and continue the experiment without stopping the machine.

[0031] Online cleaning of solids at the outlet: When a significant decrease in the gas output rate is observed, close the particulate-free gas outlet 51 and unscrew the product collection container 5; remove the high-temperature resistant filter layer 8 (filter paper) of the inner liner, replace it with a new filter layer, reinstall the product collection container 5, and open the gas outlet 51 to resume the reaction. The entire process takes ≤5 minutes and the experiment is continuous without interruption.

[0032] This process can support long-term catalyst durability testing (over 1000 hours) while ensuring operational safety and the continuity of experimental data.

[0033] Any aspects not covered in this invention are applicable to existing technologies.

[0034] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A device for evaluating the activity of solid reactant gas-to-gas catalytic reaction, characterized in that, The device includes a reaction tube (1), with a reaction gas inlet (11) at the upper end. Inside the reaction tube (1), from top to bottom, are a reactant supply zone (1a), a catalytic reaction zone (1b), and a product cleaning zone (1c). A catalyst layer (2) is installed in the catalytic reaction zone (1b), and the catalyst layer (2) is sealed to the inner wall of the reaction tube (1). A reactant container I (3) with an upper opening is provided in the reactant supply zone (1a). A reaction vessel is also provided outside the reaction tube (1). Reactant container II (4) is connected to the lower end of reactant container I (3) by a pipeline. The upper end of reactant container II (4) is provided with a sealing cap (41). The product cleaning zone (1c) is provided with a product collection container (5). The opening end of the product collection container (5) is located in the product cleaning zone (1c). The two are detachably sealed. The outer wall of the reaction tube (1) corresponding to the catalytic reaction zone (1b) and the reactant supply zone (1a) is provided with a heating layer (6).

2. The device for evaluating the activity of solid reactant gas-to-gas catalytic reaction according to claim 1, characterized in that, The outer wall of the reactant container II (4) and the outer wall of the reaction tube (1) corresponding to the product cleaning zone (1c) are respectively provided with heat insulation layer (7).

3. The device for evaluating the activity of solid reactant gas-to-gas catalytic reaction according to claim 2, characterized in that, The product collection container (5) is a cylindrical structure with an opening at the top and an air outlet (51) at the bottom. A high-temperature resistant filter layer (8) is laid on its inner wall. A sealing ring (9) is provided near the outer side of the upper opening of the product collection container (5). The product collection container (5) and the inner wall of the product cleaning area (1c) are screwed together in a sealed manner.

4. The device for evaluating the activity of solid reactant gas-to-gas catalytic reaction according to claim 3, characterized in that, The reactant container II (4) is equipped with a scale.

5. The device for evaluating the activity of solid reactant gas-to-gas catalytic reaction according to claim 4, characterized in that, The height of reactant container II (4) is greater than or equal to the height of reactant container I (3).

6. The device for evaluating the activity of solid reactant gas-to-gas catalytic reaction according to any one of claims 1-5, characterized in that, The catalyst layer (2) includes a catalyst sample (21) and a fastener (22), wherein the catalyst sample (21) is fixed in the catalytic reaction zone (1b) by the fastener (22).

7. The device for evaluating the activity of solid reactant gas-to-gas catalytic reaction according to claim 6, characterized in that, The reaction tube (1), reactant container I (3) and reactant container II (4) are integrally formed structures.

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