CN-122017116-A - Multichannel catalyst evaluation device and evaluation method for oxygen storage amount test

CN122017116ACN 122017116 ACN122017116 ACN 122017116ACN-122017116-A

Abstract

The invention belongs to the technical field of testing, and particularly discloses a multichannel catalyst evaluation device and an evaluation method for oxygen storage test. The reaction system of the device comprises a plurality of single-channel reactors, a plurality of analysis systems respectively correspond to the single-channel reactors, a carrier gas pipeline and a basic atmosphere gas pipeline of a gas distribution system comprise a gas source I, a pressure stabilizing valve, a pressure gauge, a switching valve and a one-way valve which are sequentially connected, an outlet end of the one-way valve is divided into a plurality of branch circuits I and is provided with an MFC, a liquid supply source and an auxiliary carrier gas source are connected with a liquid evaporation tank, the pipeline is provided with the MFC, a CO gas pipeline and an O 2 gas pipeline of an OSC gas switching unit comprise a gas source II, the pressure stabilizing valve, the pressure gauge, the switching valve and the one-way valve which are sequentially connected, the outlet end of the one-way valve is divided into a plurality of branch circuits II provided with auxiliary carrier gas and is provided with the MFC and a high-speed switching valve, and the control system is electrically connected with each switching valve, each MFC, each high-speed switching valve and the reaction system and the analysis system.

Inventors

Guo lv
CHEN LI
YANG DONGXIA
LU CHAOFEN
WANG CHENGXIONG
ZHANG AIMIN
QIN QINGGAO
TAN SHUHAI
HE HONGYANG
WANG CHUNXUE
ZHAO YUNKUN

Assignees

云南贵金属实验室有限公司
昆明贵研催化剂有限责任公司
波露明（北京）科技有限公司

Dates

Publication Date: 20260512
Application Date: 20260206

Claims (10)

1. The multichannel catalyst evaluation device for the oxygen storage test is characterized by comprising a gas distribution system (1), a reaction system (2), a plurality of analysis systems (3) and a control system (4), wherein the reaction system (2) consists of a plurality of single-channel reactors (21) which are arranged in parallel, and the analysis systems (3) are respectively corresponding to the single-channel reactors (21) of the reaction system (2) and are used for detecting concentration values and air-fuel ratio changes before and after the reaction of each test component in real time; the gas distribution system (1) comprises a carrier gas pipeline (11), a basic atmosphere gas pipeline (12), a plurality of liquid raw material gas inlet pipelines (13) and an OSC gas switching unit (14), The carrier gas pipeline (11) and the basic atmosphere gas pipeline (12) comprise a gas source I, a pressure stabilizing valve (15), a pressure gauge (16), a switch valve (17) and a one-way valve (18) which are sequentially connected, the outlet ends of the one-way valves (18) corresponding to the carrier gas pipeline (11) and the basic atmosphere gas pipeline (12) are respectively divided into a plurality of branches I, a mass flow controller (19) is arranged on each branch I, and the tail end of any branch I of the basic atmosphere gas pipeline (12) is combined with the tail end of the corresponding branch I of the carrier gas pipeline (11) and then connected with the inlet end of the corresponding single-channel reactor (21); The liquid raw material air inlet pipeline (13) comprises a liquid supply source (1A), an auxiliary carrier gas source (1B) and a liquid evaporation tank (1C), wherein the liquid supply source (1A) and the auxiliary carrier gas source (1B) are respectively connected with the inlet end of the liquid evaporation tank (1C), mass flow controllers (19) are respectively arranged on pipelines connected with the inlet ends of the liquid supply source (1A) and the auxiliary carrier gas source (1B) and the liquid evaporation tank (1C), and the outlet end of the liquid evaporation tank (1C) is connected with the inlet end of a corresponding single-channel reactor (21) through the pipelines; The OSC gas switching unit (14) comprises a gas source II, a CO gas pipeline (1D) and an O 2 gas pipeline (1E), wherein the CO gas pipeline (1D) and the O 2 gas pipeline (1E) comprise a gas source II, a pressure stabilizing valve (15), a pressure gauge (16), a switch valve (17) and a one-way valve (18) which are sequentially connected, the outlet ends of the one-way valves (18) corresponding to the CO gas pipeline (1D) and the O 2 gas pipeline (1E) are respectively divided into a plurality of branches II which output CO and O 2 with different concentrations, a mass flow controller (19) and a high-speed switching valve (1F) are arranged on the branches II and are connected with the single-channel inlet ends of the reactors (21), the branches II of the CO gas pipeline (1D) and the O 2 gas pipeline (1E) are respectively provided with an auxiliary carrier gas (1G), and the mass flow controller (19) is arranged on the pipelines of the auxiliary carrier gas (1G) and the outlet ends of the auxiliary carrier gas pipeline are connected with the front ends of the pipelines of the high-speed switching valves (1F) corresponding to the branches II; The control system (4) is respectively and electrically connected with each switch valve (17), each mass flow controller (19), each high-speed switch valve (1F), each analysis system (3) and each reaction system (2) of the gas distribution system (1).
2. The multi-channel catalyst evaluation device for oxygen storage amount test according to claim 1, wherein the gas source I of the base atmosphere gas line (12) supplies at least one of carbon dioxide, nitric oxide, ammonia, methane, hydrogen, propylene and propane, and the liquid supply source (1A) supplies a volatilizable liquid including water, benzene, hydrocarbons or alcohols.
3. The multi-channel catalyst evaluation device for oxygen storage test according to claim 1 or 2, wherein the outlet ends of the check valves (18) corresponding to the CO gas pipeline (1D) and the O 2 gas pipeline (1E) are respectively divided into three branches II, the three branches II of the CO gas pipeline (1D) are respectively a CO-high gas branch, a CO-medium gas branch and a CO-low gas branch and are used for outputting three different concentrations of CO, the three branches II of the O 2 gas pipeline (1E) are respectively an O 2 -high gas branch, an O 2 -medium gas branch and an O 2 -low gas branch and are used for outputting three different concentrations of O 2 , and the three branches II of the CO gas pipeline (1D) and the O 2 gas pipeline (1E) are respectively connected with the inlet ends of the single-channel reactors (21) of the reaction system (2).
4. The multi-channel catalyst evaluation device for oxygen storage amount test according to claim 3, wherein the CO-high gas branch and the O 2 -high gas branch form an A-channel gas, the CO-low gas branch and the O 2 -low gas branch form a C-channel gas, the CO-medium gas branch and the O 2 -medium gas branch form a B-channel gas, the A-channel gas is mixed with other gas components in the gas distribution system (1) to form an oxygen-enriched atmosphere, the C-channel gas is mixed with other gas components in the gas distribution system (1) to form an oxygen-depleted atmosphere, the B-channel gas is mixed with other gas components in the gas distribution system (1) to form a stoichiometric ratio atmosphere, and the control system (4) controls the corresponding high-speed switching valve (1F) to circulate the A-channel gas, the B-channel gas and the C-channel gas into the corresponding single-channel reactor (21) according to a preset alternate cycle, or circulates the A-channel gas and the C-channel gas into the corresponding single-channel reactor (21) according to a preset alternate cycle.
5. The multi-channel catalyst evaluation device for oxygen storage test according to claim 4, wherein the reaction system (2) comprises three single-channel reactors (21) with the same structure and three heating furnaces (22) with independent temperature control corresponding to the single-channel reactors (21), the single-channel reactors (21) comprise heating areas at the upper part and reaction areas at the lower part, the heating areas of the single-channel reactors (21) are arranged in the corresponding heating furnaces (22), the reaction areas of the single-channel reactors (21) are provided with sample tubes (26) filled with catalysts (25), each gas component output by the gas distribution system (1) is introduced into the reaction areas of the single-channel reactors (21), and the heating furnaces (22) are electrically connected with the control system (4).
6. The multi-channel catalyst evaluation device for oxygen storage test according to claim 5, wherein a gas mixer (23) is arranged at the upper part of a reaction zone of the single-channel reactor (21), a plurality of gas inlet pipelines (24) penetrating through a heating zone and extending into the gas mixer (23) from the bottom end are arranged in the single-channel reactor (21), each gas component output by the gas distribution system (1) is respectively communicated with a corresponding gas inlet pipeline (24) in the single-channel reactor (21), the reaction system (2) further comprises a thermocouple detector (27) penetrating through the single-channel reactor (21) and arranged at the front end of the catalyst (25), and the thermocouple detector (27) is electrically connected with the analysis system (3).
7. The multi-channel catalyst evaluation device for oxygen storage amount test according to claim 5, wherein the analysis system (3) comprises a sampling tube, a gas analyzer (31), a front oxygen sensor (32) and a rear oxygen sensor (33), the sampling tube is divided into a front sampling tube (34) and a rear sampling tube (35), the front sampling tube (34) is provided with a first control valve, the rear sampling tube (35) is provided with a second control valve, the front sampling tube (34) and the front oxygen sensor (32) are arranged at the front end of a sample tube (26) of the single-channel reactor (21), the rear sampling tube (35) and the rear oxygen sensor (33) are arranged at the rear end of the sample tube (26) of the single-channel reactor (21), the front sampling tube (34) and the rear sampling tube (35) of each single-channel reactor (21), the front oxygen sensor (32) and the rear oxygen sensor (33) are respectively electrically connected with the gas analyzer (31), and the first control valve and the second control valve (31) are respectively electrically connected with the gas analyzer (4).
8. A multi-channel catalyst evaluation method for oxygen storage amount test is characterized in that the multi-channel catalyst evaluation device for oxygen storage amount test based on claim 7 comprises the steps of catalyst installation, atmosphere replacement, collection of data before reaction, collection of data after reaction, reaction atmosphere control, reaction temperature control and purging, and the specific contents of the steps are as follows: A. catalyst installation, namely placing sample tubes (26) filled with the same volume of catalyst (25) in the reaction areas of the single-channel reactors (21) respectively; B. The control system (4) opens each switch valve (17) corresponding to the gas distribution system (1), respectively introduces the carrier gas, the basic atmosphere, the liquid raw material and the auxiliary carrier gas (1G) of the gas distribution system (1) into each single-channel reactor (21), and simultaneously at least introduces the A-channel gas and the B-channel gas of the OSC gas switching unit (14) into two single-channel reactors (21) respectively, or introduces the A-channel gas, the B-channel gas and the C-channel gas of the OSC gas switching unit (14) into three single-channel reactors (21) respectively; C. The method comprises the steps of collecting pre-reaction data, wherein a control system (4) controls a gas analyzer (31) to start collecting data and opens a first control valve of the analysis system (3), and the gas analyzer (31) records concentration values I and air-fuel ratios I of various gas components before reaction in a single-channel reactor (21) through a front end adoption pipe (34) and a front oxygen sensor (32); D. the control system (4) closes the first control valve of the analysis system (3) and simultaneously opens the second control valve, and the gas analyzer (31) records the concentration value II and the air-fuel ratio II of each gas component after reaction in the single-channel reactor (21); E. In the step D, a control system (4) controls the opening and closing parameters of each high-speed switching valve (1F) in the OSC gas switching unit (14) to enable the gas in the A path and the gas in the B path to be respectively introduced into the two single-channel reactors (21) in a preset alternate period cycle or enable the gas in the A path, the gas in the B path and the gas in the C path to be respectively introduced into the three single-channel reactors (21) in the preset alternate period cycle; F. in the step D, the control system (4) controls the heating furnace (22) to heat each single-channel reactor (21) to the required reaction temperature at a specific heating rate according to a preset heating program and keep the temperature for a period of time, and the gas analyzer (31) records the reaction temperature detected by the thermocouple detector (27); G. The control system (4) closes the mass flow controllers (19), the switching valves (17) and the high-speed switching valves (1F) on the pipelines of the gas distribution system (1), stops heating of the heating furnace (22), keeps carrier gas to sweep the pipelines, the single-channel reactor (21) and the gas analyzer (31) for a preset time, and completes OSC test of the plurality of catalysts (25) after the completion.
9. The method for evaluating a multi-channel catalyst for oxygen storage amount testing according to claim 8, wherein the carrier gas and the auxiliary carrier gas (1G) are both nitrogen, the basic atmosphere comprises carbon dioxide, nitric oxide, propylene, propane, and the liquid raw material is liquid water.
10. The method for evaluating the multichannel catalyst for oxygen storage testing of claim 8, wherein the single-channel reactor (21) and the sample tube (26) are high-temperature resistant quartz tubes with design temperature of +/-1000 ℃, the high-speed switching valve (1F) comprises a pneumatic valve and an electromagnetic valve for controlling the pneumatic valve, the electromagnetic valve is electrically connected with the control system (4), and the response time of the high-speed switching valve (1F) is less than or equal to 100ms.

Description

Multichannel catalyst evaluation device and evaluation method for oxygen storage amount test Technical Field The invention belongs to the technical field of testing, and particularly relates to a multichannel catalyst evaluation device and an evaluation method for oxygen storage test. Background The fixed bed reactor is used as a core device for realizing gas-solid phase catalytic reaction in the fields of chemical industry, petrochemical industry, energy sources, materials and the like, and the core principle is that a solid catalyst is fixed in a bed layer, so that fluid (gas or liquid) flows through the bed layer along a specific direction and reacts with the solid phase, and the fixed bed reactor is widely applied to various catalytic reaction scenes by virtue of the characteristics of high reaction stability, mature process and the like. The multichannel fixed bed reactor effectively improves space utilization rate and experimental efficiency through the design advantage of being capable of carrying out multiple groups of reactions in parallel, and becomes a research hot spot of the fixed bed reactor in recent years. The tail gas of the motor vehicle contains various harmful substances such as carbon monoxide (CO), nitrogen oxides (NOx), hydrocarbon (THC), particulate Pollutants (PM) and the like, and the direct emission can cause serious pollution to the atmospheric environment. Along with the increasing of environmental pollution control force, the emission regulations of motor vehicles are gradually upgraded, and the standard requirements from the state I to the state VI are becoming severe, wherein the severity of the emission regulations of the state VI is far beyond the international similar standard in the same period, so that the emission of tail gas pollutants of motor vehicles is strictly controlled, and the tail gas purification efficiency is improved, and the method becomes an important subject in the current environmental protection field. The noble metal catalyst in the three-way catalyst is a core material for purifying tail gas of motor vehicles, and can effectively convert pollutants in the tail gas through catalysis, so that the pollution degree of the tail gas to the atmosphere is reduced. The oxygen storage amount (OSC) of the catalyst is a key index for measuring the performance of the catalyst, namely, the larger the oxygen storage amount (OSC) is, the stronger the activity of the catalyst is, the better the tail gas purifying effect is, and on the contrary, the smaller the oxygen storage amount (OSC) is, the weaker the activity of the catalyst is, and the severe emission requirement is difficult to meet. Therefore, the accurate measurement of the oxygen storage amount (OSC) of the catalyst is of great significance to the research and development, screening and performance optimization of the catalyst. However, the conventional test of oxygen storage of the catalyst adopts a test mode of matching a single reactor with a single atmosphere, and has the obvious limitations that on one hand, the single test can only complete the evaluation of one catalyst or a group of reaction conditions, so that the test period is long, the research and development process of the catalyst is seriously restricted, on the other hand, in the single reactor mode, part of gas is required to be directly exhausted in the gas path switching process, a great amount of gas sources are wasted, the test cost is obviously increased, and meanwhile, the conventional device is difficult to realize synchronous comparison of a plurality of groups of reaction conditions, and the optimal catalyst raw material formula and reaction parameters cannot be rapidly screened. With the rapid development of combinatorial chemistry in the catalytic field, the synthesis speed of the catalyst is greatly improved, and the requirements of high throughput, high precision and multi-condition parallelism are provided for the catalyst performance evaluation technology. Although the existing multichannel fixed bed related device solves the parallel test problem to a certain extent, the special suitability for oxygen storage amount test still has the defects that part of devices lack an accurate atmosphere switching unit, dynamic change of air-fuel ratio under real working conditions is difficult to simulate, so that deviation exists between an OSC evaluation result and actual performance, temperature control accuracy of a heating system of part of devices is insufficient, temperature distribution is uneven, accuracy of the oxygen storage amount test result is affected, and an air distribution system of some devices cannot realize accurate proportioning and synchronous supply of liquid raw materials and various gas components. Therefore, there is a need to develop a multi-channel catalyst evaluation device for oxygen storage testing, which has a compact structure, uniform heating, accurate and controllable parameters, and can realize multi