CN111983132A - Small sample evaluation method for performance of three-way catalyst - Google Patents

Small sample evaluation method for performance of three-way catalyst Download PDF

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CN111983132A
CN111983132A CN202010816637.3A CN202010816637A CN111983132A CN 111983132 A CN111983132 A CN 111983132A CN 202010816637 A CN202010816637 A CN 202010816637A CN 111983132 A CN111983132 A CN 111983132A
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atmosphere
way catalyst
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杜君臣
徐立峰
郭律
王成雄
杨冬霞
赵云昆
冯丰
覃庆高
高琨阳
张慧峰
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Kunming Sino Platinum Metals Catalyst Co ltd
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Abstract

The invention discloses a hand sample evaluation method for performance of a three-way catalyst, and particularly relates to a hand sample evaluation method for evaluating performance of a three-way catalyst by configuring two paths of O in a test system of a hand sample evaluation device2One path is O in lean combustion atmosphere calculated based on oxygen excess coefficient2The other path is O of rich combustion atmosphere calculated according to oxygen excess coefficient2And (4) flow rate. By the on-off control of the electromagnetic valve, lean burn O is ensured2Or rich combustion of O2One of the two paths of O2With HC, CO, NO, CO2、N2、H2Forming tail gas simulation mixed gas by O; by lean combustion of O2And rich combustion of O2The switching frequency of the electromagnetic valve is regulated and controlled, and the performance evaluation of the three-way catalyst under the frequent lean-rich switching dynamic atmosphere is realized. The evaluation method of the invention is the performance evaluation of the small sample on the fixed bed catalytic reactor, thus having the characteristics of low test cost and high test efficiency, in addition, the invention not only can react the low-temperature ignition activity difference of the catalyst, but also can reflect the high-temperature conversion activity difference of the catalyst, therefore, the result has better adaptabilityUsage and representativeness.

Description

Small sample evaluation method for performance of three-way catalyst
Technical Field
The invention belongs to the technical field of motor vehicle exhaust aftertreatment, relates to a method for evaluating the performance of a three-way catalyst, and particularly relates to a sample evaluation method for the performance of the three-way catalyst.
Background
Since the invention of oxygen sensing in the last 70 th century, the post-treatment technical route of closed-loop control electronic fuel injection system and three-way catalyst is CO, HC and NOxPM/PN emission control makes a great contribution. The three-way catalyst is used as a key part for controlling the automobile exhaust emission, and is the most effective technical means for controlling the automobile emission in the world at present. Therefore, the development of high performance three-way catalysts is a fundamental approach to meet increasingly stringent emission legislation requirements.
The reliability, test period, cost and the like of the performance evaluation method of the three-way catalyst directly restrict the development of the high-performance catalyst. At present, laboratory sample evaluation, engine bench experiments and finished vehicle emission performance tests are three representative methods for evaluating the performance of the three-way catalyst.
The laboratory hand sample evaluation is to load a catalyst cutting sample with a certain volume into a reaction tube, introduce automobile exhaust simulation mixed gas, and respectively determine the concentration change of gas components before and after catalytic reaction, thereby obtaining the change rule of the gas concentration along with the reaction temperature.
In the engine bench test, the exhaust of an automobile engine is used as a gas source, a full-size catalyst is adopted, and the running process of a real automobile is simulated on the engine test bench, so that the activity and the ageing resistance of the catalyst are tested.
The whole vehicle emission test is to run the vehicle on a rotary drum test platform according to the running working condition specified by relevant regulations and determine whether the automobile exhaust pollutants after the full-size catalyst is installed can meet the emission requirements specified by the relevant regulations.
Therefore, the engine rack and the whole vehicle performance test based on the rotary drum adopt a post-processing strategy of an electronic fuel injection system and a three-way catalyst under closed-loop control, can effectively represent the pollutant conversion behavior of the three-way catalyst under the frequent lean-rich switching atmosphere (rapidly fluctuating around lambda 1) in the road running process of an actual vehicle, and the traditional laboratory sample evaluation adopts the steady-state test of simulating mixed gas by automobile tail gas, so that the influence of the frequent lean-rich switching dynamic atmosphere on the storage reduction performance and the precious metal migration performance of the oxygen storage material of the three-way catalyst cannot be effectively presented, and the performance evaluation results of part of the catalysts are distorted.
Because the engine pedestal and the finished automobile emission test have the defects of high construction cost of a test platform, large danger coefficient, long test period, pretty test resources, high entrustment test cost and the like to a certain extent, in order to facilitate the rapid screening of the three-way catalyst in a laboratory, a small sample evaluation method of the three-way catalyst with high test speed, high applicability and reliable test results is urgently needed to be developed.
Disclosure of Invention
The invention aims to provide a method for evaluating the performance of a three-way catalyst under a dynamic atmosphere by realizing frequent lean-rich switching on a sample evaluation device, so as to solve the problems of poor representativeness and distorted results of the conventional sample evaluation method and meet the research requirements of the high-performance three-way catalyst.
The invention relates to a sample evaluation method for performance of a three-way catalyst, which is based on O in tail gas simulation mixed gas2The method for realizing the evaluation of the catalyst performance under the atmosphere of frequent lean-rich switching by dynamic modulation comprises the following steps:
a small sample evaluation method for the performance of three-way catalyst in small sample evaluation deviceConfiguration in test system is based on O in tail gas simulation gas mixture2The performance evaluation under the dynamic atmosphere of frequent lean burn atmosphere and rich gas atmosphere switching is realized by dynamic modulation; two paths of O are configured in the test system of the sample evaluation device2One way is lambda calculated from the oxygen excess coefficient>1 lean atmosphere of O2The other path is lambda calculated according to the oxygen excess coefficient<1 rich atmosphere of O2Flow rate; by the switch of the electromagnetic valve and the control of the switching frequency of the electromagnetic valve, the lean burn O is ensured2Or rich combustion of O2One of the two paths of O2With HC, CO, NO, CO2、N2、H2And forming tail gas simulation mixed gas by O, and realizing the performance evaluation under the frequent lean-rich switching dynamic atmosphere.
The oxygen excess coefficient is calculated by the formula:
Figure BDA0002632947940000021
wherein: lambda is the oxygen excess coefficient; c (CO) is the gas volume concentration of CO in%; c (C)nH2n) Gas volume concentration of HC in%; c (O)2) Is represented by%2The gas volume concentration of (a); c (NO) is the gas volume concentration of NO in%; n is more than or equal to 2.
The switching frequency of the electromagnetic valve is set to 10s-1。
The performance evaluation can be a continuous temperature programming performance test at 150-500 ℃ or a constant temperature conversion performance test at one or more temperature points of 200-500 ℃.
The continuous temperature programming performance test is used for recording the concentration change curves of CO, HC and NO along with the temperature from 150 ℃ to 500 ℃ at the temperature rise rate of 15 ℃/min.
The constant temperature conversion performance test of the plurality of temperature points is carried out by carrying out a hollow tube test at a constant temperature of 200, 300, 400 and 500 ℃, and then the conversion activity of the catalyst is tested at a constant temperature of 200, 300, 400 and 500.
The test system of the small sample evaluation device consists of two parts, namely hardware and software, wherein the core components of the hardware are a mass flowmeter, an electromagnetic valve, a reaction furnace, an oxygen analyzer and an online FTIR gas analyzer; the software is composed of a computer control program that controls each hardware.
The performance evaluation method of the three-way catalyst comprises the following steps: preparing a small sample, calibrating an oxygen analyzer, calibrating an online FTIR gas analyzer, checking air tightness, calibrating a mass flowmeter, testing an empty tube, testing the performance of the small sample and processing data.
The invention has the beneficial effects that:
1) the performance evaluation method of the three-way catalyst is a small sample performance evaluation on the fixed bed catalytic reactor, so the method has the characteristics of low test cost and high test efficiency.
2) The invention uses O2The dynamic modulation of the three-way catalyst realizes the evaluation of the catalyst performance under the atmosphere of frequent lean-rich combustion switching, can effectively simulate the post-treatment technical route of an electronic fuel injection system and a three-way catalyst controlled by an actual vehicle closed loop, and the frequent lean-rich combustion atmosphere switching can reflect the influence on the storage reduction performance, the noble metal migration performance, the catalyst structure and the like of the oxygen storage material of the three-way catalyst, so the three-way catalyst has the advantages of good applicability, strong representativeness and high reliability.
3) The performance evaluation result of the small catalyst sample under the mixed gas dynamic test atmosphere is consistent with the whole vehicle emission performance test result based on the rotary drum. Compared with the small sample performance evaluation under the traditional steady-state test atmosphere, the small sample performance evaluation under the dynamic test atmosphere not only can reflect the low-temperature ignition activity difference of the catalyst, but also can reflect the high-temperature conversion activity difference of the catalyst, so that the result has better applicability and representativeness.
Drawings
FIG. 1 is a schematic diagram of a method for evaluating a sample according to the present invention.
FIG. 2 is a graph comparing catalyst conversion performance under a mixed gas steady state test atmosphere.
FIG. 3 is a graph comparing the NO conversion performance of catalysts under a mixed gas dynamic test atmosphere.
FIG. 4 is a graph comparing HC conversion performance of catalysts under an atmosphere of a mixture dynamic test.
FIG. 5 is a graph comparing CO conversion performance of catalysts under a mixed gas dynamic test atmosphere.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described below with reference to specific embodiments. It should be noted that these descriptions are only illustrative and are not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known concepts, structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Referring to fig. 1, the test system of the hand sample evaluation device used in the present invention is composed of two parts, namely hardware and software, wherein the core components of the hardware are a mass flow meter, an electromagnetic valve, a reaction furnace, an oxygen analyzer and an online FTIR gas analyzer; the software is composed of a computer control program that controls each hardware.
The catalysts A and B in the implementation of the invention are three-way catalysts with 2 different technical characteristics of Kunming noble research catalyst Limited liability company, and the noble metal content of the three-way catalysts is 60g/ft3Rh 55:5, the support specification was 110 x 90mm, mesh 750cpsi, and wall thickness 2.5 mil.
The fixed bed catalytic reactor equipment for evaluating the performance of the three-way catalyst in the embodiment of the invention is nonstandard self-assembly equipment of Kunming noble research catalyst Limited liability company. The oxygen analyzer is a MEXA 7100H type high-precision oxygen analyzer, and the precision of the oxygen analyzer is 0.002%. The on-line FTIR gas analyzer is a Mutigas 6000 on-line infrared spectrum gas analyzer of MKS company, and the gas collection frequency is set to be 1s-1。
The performance evaluation method comprises the following steps: preparing a small sample, calibrating an oxygen analyzer, calibrating an online FTIR gas analyzer, checking air tightness, calibrating a mass flowmeter, testing an empty tube, testing the performance of the small sample and processing data.
In the following comparative examples and examples, the test systems and method steps of the above-described sample evaluation apparatus are prior art in the field except for the method of the present invention and the specific description thereof, and thus need not be described in detail.
Comparative example 1
The results of packaging 110 by 90 full-size catalysts a and B, carrying the packaged catalysts on kunming precious research catalyst limited commercial vehicles, and carrying out the whole vehicle emission performance test on the Shanghai AVL drum test platform according to the WLTC working condition specified by the national 6 regulation are shown in table 1. As can be seen from table 1, catalyst a and catalyst B both completely meet the regulatory emission limits, but it is evident that catalyst B has lower pollutant emissions and better catalyst performance.
TABLE 1 comparison of emissions Performance of the entire vehicle
Figure BDA0002632947940000051
Comparative example 2
Cylindrical small samples with a diameter of 1 inch and a height of 1 inch were taken from the full-size catalysts a and B of 110 × 90, and after calibration of an oxygen analyzer, an on-line FTIR gas analyzer, and a mass flow meter and gas tightness inspection of a pipeline, the temperature was raised from 150 ℃ to 500 ℃ at a temperature rise rate of 15 ℃/min in an equivalent steady-state gas distribution atmosphere of λ ═ 1 in table 2, and concentration change curves of CO, HC, and NO with the temperature were recorded, and the results are shown in fig. 2. As can be seen, the overall time-dependent change in concentration of catalyst a, whether CO, HC or NO, is at the lower left of catalyst B, indicating that at the same temperature, catalyst a catalyzes the conversion of the pollutants CO, HC, NO prior to catalyst B, i.e.: catalyst a had better activity than catalyst B.
TABLE 2 sample gas distribution under the atmosphere of steady-state test of mixed gas
Figure BDA0002632947940000052
Example 1
The test evaluation system for the small sample of the fixed bed catalytic reactor is assembled and consists of a 7-path air inlet pipeline, a mass flow meter, an electromagnetic valve, a reaction furnace, an oxygen analyzer and an online FTIR gas analyzer, and is specifically shown in figure 1.
In the above small sample evaluation deviceTwo paths of O are configured in the arranged test system2One path is O in a lean atmosphere with lambda 1.02 calculated from the oxygen excess factor2The other path is O of rich combustion atmosphere with lambda being 0.98 calculated according to oxygen excess coefficient2And (4) flow rate. The distribution concentrations of CO, HC and NO in the table 2 are calculated according to the formula
Figure BDA0002632947940000061
Calculating O of lean burn atmospheres20.94% concentration of O in a rich atmosphere2The concentration was 0.15%. The gas distribution of the dynamic test atmosphere thus composed is shown in table 3.
Cylindrical small samples of 1 inch in diameter and 1 inch in height were taken from 110 x 90 full size catalysts a and B, and the actual diameters and heights of the small samples were measured using vernier calipers to calculate the actual volumes of catalyst a and catalyst B to be 12.86mL and 12.86mL, respectively. At 30000h-1Calculating and designing NO, CO and C3H6、CO2Lean burn O2Rich combustion of O2、N2The flow rate of (B) was 3.2mL/min, 16.1mL/min, 6.4mL/min, 514.4mL/min, 60.4mL/min, 9.6mL/min, 5.2L. The heating temperature of the water was 65 ℃.
A catalyst to be tested is loaded in a small sample evaluation device, an oxygen analyzer, an online FTIR gas analyzer and a mass flowmeter are calibrated in a calibration mode, and after a pipeline is checked for air tightness, the switching frequency of an electromagnetic valve is set to be 10s-1The concentration change curves of NO, HC and CO with temperature were recorded by increasing the temperature from 150 ℃ to 500 ℃ at a temperature increase rate of 15 ℃/min with the above-mentioned volume flow of the gas distribution, and the results are shown in FIGS. 3, 4 and 5. It can be seen from the figure that the concentration fluctuation of the catalyst B in the dynamic atmosphere at the low temperature section is obviously greater than that of the catalyst A, and the whole concentration variation curve of the catalyst B along with time is positioned at the lower left of the catalyst A NO matter CO, HC or NO, which indicates that the catalyst B has better light-off conversion performance in the dynamic test atmosphere. In the high-temperature section, the concentration of pollutants such as CO and the like in the catalyst A is greater than that in the catalyst B, which shows that the high-temperature performance of the catalyst B under the dynamic test atmosphere is also better.
TABLE 3 sample gas distribution under mixed gas dynamic test atmosphere
Figure BDA0002632947940000062
Example 2
The test evaluation system for the small sample of the fixed bed catalytic reactor is assembled and consists of a 7-path air inlet pipeline, a mass flow meter, an electromagnetic valve, a reaction furnace, an oxygen analyzer and an online FTIR gas analyzer, and is specifically shown in figure 1.
Two paths of O are configured in the test system of the sample evaluation device2One path is O in a lean atmosphere with lambda 1.02 calculated from the oxygen excess factor2The other path is O of rich combustion atmosphere with lambda being 0.98 calculated according to oxygen excess coefficient2And (4) flow rate. The distribution concentrations of CO, HC and NO in the table 2 are calculated according to the formula
Figure BDA0002632947940000071
Calculating O of lean burn atmospheres20.94% concentration of O in a rich atmosphere2The concentration was 0.15%. The gas distribution of the dynamic test atmosphere thus composed is shown in table 3.
Cylindrical small samples of 1 inch in diameter and 1 inch in height were taken from 110 x 90 full size catalysts a and B, and the actual diameters and heights of the small samples were measured using vernier calipers to calculate the actual volumes of catalyst a and catalyst B to be 12.86mL and 12.86mL, respectively. At 30000h-1Calculating and designing NO, CO and C3H6、CO2Lean burn O2Rich combustion of O2、N2The flow rate of (B) was 3.2mL/min, 16.1mL/min, 6.4mL/min, 514.4mL/min, 60.4mL/min, 9.6mL/min, 5.2L. The heating temperature of the water was 65 ℃.
A catalyst to be tested is loaded in a small sample evaluation device, an oxygen analyzer, an online FTIR gas analyzer and a mass flowmeter are calibrated in a calibration mode, and after a pipeline is checked for air tightness, the switching frequency of an electromagnetic valve is set to be 10s-1Introducing the gas distribution according to the volume flow of the gas distribution, performing a hollow tube test at constant points of 200, 300, 400 and 500 ℃, and then testing the constant temperature point conversion activity of the catalysts A and B at 200, 300, 400 and 500. According to the test curveThe graph is represented by the formula:
Figure BDA0002632947940000072
Figure BDA0002632947940000073
Figure BDA0002632947940000074
the calculated conversion results for each contaminant are shown in table 4.
As can be seen from Table 4, the conversion activity of catalyst CO decreased with increasing temperature, and the conversion activity of catalyst B was better than that of catalyst A at each constant temperature.
TABLE 4 comparison of catalyst Performance under constant temperature point Mixed gas dynamic test atmosphere
Figure BDA0002632947940000081
Based on the above embodiments, the performance evaluation result of the small sample of the catalyst under the mixed gas dynamic test atmosphere is consistent with the test result of the emission performance of the whole vehicle based on the rotary drum. Compared with the small sample performance evaluation under the traditional steady-state test atmosphere, the small sample performance evaluation under the dynamic test atmosphere not only can reflect the low-temperature ignition activity difference of the catalyst, but also can reflect the high-temperature conversion activity difference of the catalyst, so that the result has better applicability and representativeness.

Claims (6)

1. A sample evaluation method for performance of a three-way catalyst is characterized by comprising the following steps:
configuration of O in tail gas-based simulated mixed gas in test system of sample evaluation device2The performance evaluation under the dynamic atmosphere of frequent lean burn atmosphere and rich gas atmosphere switching is realized by dynamic modulation;
in the sample evaluation deviceIn the test system, two paths of O are configured2One path is O in lean atmosphere2The other path is O in rich combustion atmosphere2Flow rate;
during performance evaluation under the dynamic atmosphere, lean burn O is ensured by switching on and off the electromagnetic valve and controlling the switching frequency of the electromagnetic valve2Or rich combustion of O2One of the two paths of O2With HC, CO, NO, CO2、N2、H2And the O is formed into tail gas simulation mixed gas.
2. A sample evaluation method of the performance of the three-way catalyst according to claim 1, wherein:
o of the lean atmosphere2The flow rate is calculated from the oxygen excess coefficient>1, O of the rich atmosphere2The flow rate is calculated from the oxygen excess coefficient<1；
The oxygen excess coefficient is calculated by the formula:
Figure FDA0002632947930000011
wherein: lambda is the oxygen excess coefficient; c (CO) is the gas volume concentration of CO in%; c (C)nH2n) Gas volume concentration of HC in%; c (O)2) Is represented by%2The gas volume concentration of (a); c (NO) is the gas volume concentration of NO in%; n is more than or equal to 2.
3. A sample evaluation method of the performance of the three-way catalyst according to claim 1 or 2, characterized in that:
the switching frequency of the electromagnetic valve is set to 10s-1。
4. A sample evaluation method of the performance of the three-way catalyst according to claim 3, wherein:
the performance evaluation can be a continuous temperature programming performance test at 150-500 ℃ or a constant temperature conversion performance test at one or more temperature points of 200-500 ℃.
5. A sample evaluation method of the performance of the three-way catalyst according to claim 4, wherein:
the continuous temperature programming performance test is used for recording the concentration change curves of CO, HC and NO along with the temperature from 150 ℃ to 500 ℃ at the temperature rise rate of 15 ℃/min.
6. A sample evaluation method of the performance of the three-way catalyst according to claim 4, wherein:
the constant temperature conversion performance test of the plurality of temperature points is carried out by carrying out a hollow tube test at a constant temperature of 200, 300, 400 and 500 ℃, and then the conversion activity of the catalyst is tested at a constant temperature of 200, 300, 400 and 500.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112577751A (en) * 2020-12-14 2021-03-30 东风汽车集团有限公司 Model selection method of automobile exhaust three-way catalyst
CN113567611A (en) * 2021-07-19 2021-10-29 中自环保科技股份有限公司 Evaluation device and evaluation method of LNT catalyst

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CN102590537A (en) * 2012-02-29 2012-07-18 福州大学 System for evaluating catalyst and material
CN108333137A (en) * 2017-11-27 2018-07-27 昆明贵研催化剂有限责任公司 A method of it measuring three-effect catalysis material ammonia product and generates performance

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN101634253A (en) * 2008-07-24 2010-01-27 株式会社三国 Air-fuel ratio control device of internal combustion engine and air-fuel ratio control method
CN102590537A (en) * 2012-02-29 2012-07-18 福州大学 System for evaluating catalyst and material
CN108333137A (en) * 2017-11-27 2018-07-27 昆明贵研催化剂有限责任公司 A method of it measuring three-effect catalysis material ammonia product and generates performance

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112577751A (en) * 2020-12-14 2021-03-30 东风汽车集团有限公司 Model selection method of automobile exhaust three-way catalyst
CN112577751B (en) * 2020-12-14 2022-03-15 东风汽车集团有限公司 Model selection method of automobile exhaust three-way catalyst
CN113567611A (en) * 2021-07-19 2021-10-29 中自环保科技股份有限公司 Evaluation device and evaluation method of LNT catalyst

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Application publication date: 20201124