CN113702239A - Falling rate detection method for motor vehicle exhaust treatment catalytic converter - Google Patents
Falling rate detection method for motor vehicle exhaust treatment catalytic converter Download PDFInfo
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- CN113702239A CN113702239A CN202111076039.8A CN202111076039A CN113702239A CN 113702239 A CN113702239 A CN 113702239A CN 202111076039 A CN202111076039 A CN 202111076039A CN 113702239 A CN113702239 A CN 113702239A
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 104
- 238000001514 detection method Methods 0.000 title abstract description 15
- 238000000576 coating method Methods 0.000 claims abstract description 44
- 239000011248 coating agent Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 32
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000005303 weighing Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 20
- 239000007789 gas Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 230000008569 process Effects 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000007664 blowing Methods 0.000 claims abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 3
- 238000010926 purge Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 230000035939 shock Effects 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 4
- 238000013461 design Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 14
- 239000003054 catalyst Substances 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000010791 quenching Methods 0.000 description 3
- 230000000171 quenching effect Effects 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Exhaust Gas After Treatment (AREA)
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Abstract
The invention relates to the technical field of detection of motor vehicle exhaust catalytic converters, in particular to a falling rate detection method for a motor vehicle exhaust treatment catalytic converter, which comprises the following steps of S1, weighing the catalytic converter to be detected to obtain a weight M1; s2, continuously roasting the catalytic converter at 800-950 ℃ for 50-200 hours; during roasting, introducing mixed gas into a roasting furnace, wherein the mixed gas contains 5-20% of water vapor by volume fraction, 50-200ppm of sulfur dioxide and 15-25% of oxygen by volume fraction; s3, taking out the catalytic converter, cooling to room temperature, and blowing the cooled catalytic converter by using airflow; weighing to obtain a weight M2; and S4, calculating the coating falling rate. The connecting force between the coating and between the coating and the carrier of the catalytic converter in practical application can be more perfectly evaluated, and the risk of coating falling off in the application process caused by unreasonable design of the catalytic converter is reduced, so that the risk of unqualified durability of the catalytic converter is reduced.
Description
Technical Field
The invention relates to the technical field of detection of motor vehicle tail gas catalytic converters, in particular to a falling rate detection method for a motor vehicle tail gas treatment catalytic converter.
Background
With the upgrading of emission regulations of motor vehicles (such as gasoline vehicles, natural gas vehicles and the like), the emission limit and the endurance mileage of the motor vehicles are more strict, and especially the endurance mileage is increased, so that the requirement on the durability of the exhaust purification catalytic converter is higher and higher. The catalytic converter is mainly divided into two parts, namely a coating and a carrier. The strength of the connecting force between the coatings and the carrier play a key role in the durability of the catalytic converter. When the connecting force is weak, the coating can be gradually peeled off and fall off along with the increase of the endurance mileage, so that the performance of the catalytic converter is gradually reduced, and the requirements of emission regulations can not be met in severe cases. Therefore, the bonding force between the coating layers and the carrier are generally expressed by the peeling rate, and a method for studying the peeling rate of the coating layers becomes a key point of attention.
Currently, the following methods are mainly used to measure the coating peeling rate: (1) an ultrasonic wave method, and (2) a high-temperature thermal shock method. For example, chinese patent CN201610006674.1 mentions that the catalyst has an operating temperature below 0 ℃ (cold start in winter) to above 1000 ℃, and has a large rate of temperature rise and drop (rapid cooling and heating); the space velocity is 0-100000 hours-1(ii) a variation within a range; under the condition that the working pressure is also changed in a large range, a coating can generate a large number of cracks and continuously fall off, and the durability of the catalyst is seriously influenced. The process of temperature quenching and quenching with a maximum temperature of up to 1000 c is known in the industry as a high temperature thermal shock process. This patent also mentions the use of ultrasound to detect the peeling of the catalyst coating. Ultrasonic methodThe method is used for simulating the mechanical vibration in the environment where the catalytic converter is placed so as to measure the influence of the mechanical vibration on the coating falling. The high-temperature thermal shock method is mainly used for simulating a quenching and shock heating condition in the environment where the catalytic converter is placed, so that the influence of thermal stress on coating peeling is measured.
In practice, in addition to mechanical vibration and shock cooling, the environment in which the catalytic converter is used also contains constant temperature and chemical substances (such as water vapor, sulfur dioxide, etc.), and these conditions also have the risk of potentially affecting the peeling of the coating, especially the chemical substances may react with the coating to cause cracking and peeling of the coating, which has not been studied in the above patent.
The currently adopted ultrasonic method and high-temperature thermal shock method cannot comprehensively evaluate the shedding rate of the catalytic converter, and the risk of coating shedding exists in the application process.
Disclosure of Invention
The invention aims to: aiming at the problems that the shedding rate of a catalytic converter can not be comprehensively evaluated and the coating shedding risk exists in the application process in the prior art, the shedding rate detection method for the motor vehicle exhaust treatment catalytic converter is provided. According to the method, water vapor and sulfur dioxide are introduced under a high-temperature condition, the use environment is simulated, the defects of ultrasonic and thermal shock detection methods can be overcome, and the connecting force between the coating and the carrier of the catalytic converter in practical application can be evaluated better and perfectly.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for detecting the falling rate of a catalytic converter for treating the tail gas of a motor vehicle comprises the following steps,
s1, weighing the catalytic converter to be detected to obtain a weight M1;
s2, continuously roasting the catalytic converter at 800-950 ℃ for 50-200 hours; in the roasting process, continuously introducing mixed gas into a roasting furnace, wherein the mixed gas contains 5-20% of water vapor by volume fraction, 50-200ppm of sulfur dioxide and 15-25% of oxygen by volume fraction;
s3, taking out the catalytic converter, cooling to room temperature, and blowing the cooled catalytic converter by using airflow; weighing to obtain a weight M2;
s4, calculating the peeling rate of the coating,
in a preferred embodiment of the present invention, the mixed gas is composed of air, water vapor, and sulfur dioxide gas.
As a preferable embodiment of the present invention, before step S1, the method further comprises step S0; and S0, drying the catalytic converter to be detected.
As a preferable scheme of the invention, in the step S0, the drying temperature is 120-200 ℃, and the drying time is 1-2 hours.
As a preferable aspect of the present invention, in step S3, the purged catalytic converter is dried before weighing.
As a preferable scheme of the invention, in the step S3, the drying temperature is 120-200 ℃, and the drying time is 1-2 hours.
As a preferable embodiment of the present invention, in step S3, the pressure of the purge gas flow is 0.3 to 0.6MPa, and the purge time is 10 to 120 seconds.
In a preferred embodiment of the present invention, the roasting furnace is a muffle furnace or a tube furnace.
As a preferable aspect of the present invention, before step S1 or after step S3, ultrasonic detection is performed on the catalytic converter.
As a preferable aspect of the present invention, before step S1 or after step S3, the catalytic converter is subjected to high-temperature thermal shock detection.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
the invention relates to a falling rate detection method for a catalytic converter for treating tail gas of a motor vehicle. The invention makes up the defects of the existing ultrasonic wave and thermal shock detection method, and by using the invention and combining the ultrasonic wave and thermal shock methods, the connecting force between the coating and between the coating and the carrier in the practical application of the catalytic converter can be more completely evaluated, and the risk of coating falling off in the application process caused by unreasonable design of the catalytic converter is reduced, thereby reducing the risk of unqualified durability of the catalytic converter.
Drawings
FIG. 1 is an SEM photograph of a catalytic converter A-5 in example 1 of the present invention in a post-treatment state under treatment conditions of 800 deg.C-200H-10% H2O-100ppmSO2。
FIG. 2 is an SEM image of catalytic converter A-3 in the untreated state in comparative example 3 of the present invention.
FIG. 3 is an SEM photograph of the catalytic converter A-3 of comparative example 3 of the present invention in a post-treatment state under calcination treatment conditions of 800 ℃ to 200 hours.
FIG. 4 is an SEM photograph of a catalytic converter A-4 of comparative example 4 of the present invention in a post-treatment state under treatment conditions of 800 deg.C-200H-10% H2O。
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The catalytic converter for the experiment is a catalytic converter manufactured by the company with the serial numbers of A-1, A-2, A-3, A-4, A-5, A-6, A-7 and A-8; eight catalysts used the same batch of support and coating.
Example 1
Selecting a catalytic converter A-5, and drying for 1 hour at 150 ℃; after cooling to room temperature, weighing to obtain a weight M1;
placing the catalytic converter in a tubular furnace, and introducing air containing 10% of water vapor by volume and 100ppm of sulfur dioxide; calcining the catalytic converter at 800 ℃ for 200 hours;
cooling to room temperature, taking out the catalytic converter, and purging the treated catalytic converter for 30 seconds by using air with the air pressure of 0.6 MPa; placing the purged catalytic converter in an oven for 2 hours at 120 ℃, and weighing to obtain a weight M2; and calculating the coating shedding rate (M1-M2)/M1 after purging.
Example 2
Selecting a catalytic converter A-6, and drying for 2 hours at 120 ℃; after cooling to room temperature, weighing to obtain a weight M1;
placing the catalytic converter in a muffle furnace, and introducing air containing 20% of water vapor by volume fraction and 200ppm of sulfur dioxide; the catalytic converter was calcined at 900 ℃ for 100 hours;
cooling to room temperature, taking out the catalytic converter, and purging the treated catalytic converter for 50 seconds by using air with the air pressure of 0.3 MPa; placing the purged catalytic converter in an oven for 2 hours at 120 ℃, and weighing to obtain a weight M2; and calculating the coating shedding rate (M1-M2)/M1 after purging.
Example 3
Selecting a catalytic converter A-7, and drying for 1 hour at 200 ℃; after cooling to room temperature, weighing to obtain a weight M1;
placing the catalytic converter in a tubular furnace, and introducing air containing 15% of water vapor and 150ppm of sulfur dioxide by volume; the catalytic converter was calcined at 950 ℃ for 50 hours;
cooling to room temperature, taking out the catalytic converter, and purging the treated catalytic converter for 120 seconds by using air with the air pressure of 0.4 MPa; placing the purged catalytic converter in an oven for 2 hours at 120 ℃, and weighing to obtain a weight M2; and calculating the coating shedding rate (M1-M2)/M1 after purging.
Example 4
Selecting a catalytic converter A-8, and drying for 1 hour at 140 ℃; after cooling to room temperature, weighing to obtain a weight M1;
placing the catalytic converter in a muffle furnace, and introducing air containing 5% of water vapor and 50ppm of sulfur dioxide by volume; continuously roasting the catalytic converter at 950 ℃ for 100 hours;
cooling to room temperature, taking out the catalytic converter, and purging the treated catalytic converter for 100 seconds by using air with the air pressure of 0.6 MPa; placing the purged catalytic converter in an oven for 2 hours at 150 ℃, and weighing to obtain a weight M2; and calculating the coating shedding rate (M1-M2)/M1 after purging.
Comparative example 1Ultrasonic testing
Selecting a catalytic converter A-1, and drying for 1 hour at 150 ℃; after cooling to room temperature, weighing was carried out to obtain a weight M1. Roasting in a tube furnace at 900 deg.C for 10min, cooling to room temperature, placing in an ultrasonic cleaning device, ultrasonic cleaning for 10min, and drying at 120 deg.C until the weight change is stable. Purging the treated catalytic converter for 30 seconds by using the air pressure of 0.6MPa, placing the purged catalytic converter in an oven for 2 hours at the temperature of 120 ℃, and weighing to obtain the weight M2; and calculating the coating falling rate after purging.
Comparative example 2High temperature thermal shock detection
Selecting a catalytic converter A-2, and drying for 1 hour at 150 ℃; after cooling to room temperature, weighing was carried out to obtain a weight M1. Carrying out cold and hot impact for 3 times at room temperature to 1000 ℃ in a muffle furnace, purging the treated catalytic converter for 30 seconds by using 0.6MPa air pressure, placing the purged catalytic converter in an oven for treatment for 2 hours at 120 ℃, and weighing to obtain the weight M2; and calculating the coating falling rate after purging.
Comparative example 3Calcining without introducing water vapor and sulfur dioxide
Selecting a catalytic converter A-3, and drying for 1 hour at 150 ℃; after cooling to room temperature, weighing was carried out to obtain a weight M1. Placing the mixture in a tube furnace to bake for 200 hours at 800 ℃. Moving out the catalytic converter, cooling to room temperature, purging the treated catalytic converter for 30 seconds by using 0.6MPa air pressure, placing the purged catalytic converter in an oven for treatment at 120 ℃ for 2 hours, and weighing to obtain M2; and calculating the coating falling rate after purging. FIG. 2 is an SEM image of A-3 in an untreated state. FIG. 3 is an SEM image of A-3 after 800-200 h treatment.
Comparative example 4Roasting and introducing water vapor but not sulfur dioxide
Selecting a catalytic converter A-4, and drying for 1 hour at 150 ℃; after cooling to room temperature, weighing was carried out to obtain a weight M1. The catalyst was placed in a tube furnace, 10% steam was introduced, and the catalytic converter was calcined at 800 ℃ for 200 hours. Moving out the catalytic converter, cooling to room temperature, purging the treated catalytic converter for 30 seconds by using 0.6MPa air pressure, placing the purged catalytic converter in an oven for treatment at 120 ℃ for 2 hours, and weighing to obtain M2; and calculating the coating falling rate after purging. A-4 is calcined at high temperature and treated with steam, and the SEM image is shown in FIG. 4.
The results of the coating peeling test in comparative examples 1 to 4 and examples 1 to 4 are shown in the following table.
TABLE 1 catalytic converter coating spallation rate results
| Numbering | Catalytic converter numbering | Coating peeling ratio (%) |
| Comparative example 1 | A-1 | 0.2 |
| Comparative example 2 | A-2 | 2.0 |
| Comparative example 3 | A-3 | 1.5 |
| Comparative example 4 | A-4 | 4.8 |
| Example 1 | A-5 | 9.7 |
| Example 2 | A-6 | 9.6 |
| Example 3 | A-7 | 10.0 |
| Example 4 | A-8 | 10.5 |
Remarking: in the industry, the coating falling rate index is generally controlled within 3% or 5%.
From table 1 above, it can be seen that: the values of the shedding rate obtained by different detection methods have larger difference. An increase in slip rate values under the conditions of the examples results in an increase in the performance loss of the catalytic converter; the connection force between the coating and the coating or between the coating and the carrier is greatly influenced by water vapor and sulfur dioxide under certain constant temperature conditions. The detection method of the embodiment can effectively identify the risk of the coating of the catalytic converter falling off, so that the unreasonable design of the catalytic converter is avoided, and the effective design meets the emission regulation with longer mileage.
Test example 1Electron microscope experiment
To observe the effect of water vapor and sulfur dioxide on the catalytic converter coating under constant temperature conditions, A-3 (untreated state), A-3 (800-200H) in comparative example 3, A-4 (800-200H-10% H) in comparative example 4, were measured2O), A-5 of example 1 (800 deg.C-200H-10% H)2O-100ppmSO2) SEM experiments were performed, and the results are shown in FIGS. 1 to 4.
As can be seen from SEM comparison, H2O、SO2Larger cracks between the coatings can be caused and the coating can be stripped more frequently by cracks. The method of example 1 can accurately simulate the chemical substances of the catalytic converter in the application processInteraction of the substance with the coating.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A method for detecting the falling rate of a catalytic converter for treating motor vehicle exhaust is characterized by comprising the following steps,
s1, weighing the catalytic converter to be detected to obtain a weight M1;
s2, continuously roasting the catalytic converter at 800-950 ℃ for 50-200 hours; in the roasting process, continuously introducing mixed gas into a roasting furnace, wherein the mixed gas contains 5-20% of water vapor and 50-200ppm of sulfur dioxide by volume fraction, and the mixed gas contains 15-25% of oxygen by volume fraction;
s3, taking out the catalytic converter, cooling to room temperature, and blowing the cooled catalytic converter by using airflow; weighing to obtain a weight M2;
s4, calculating the peeling rate of the coating,
2. the method of claim 1, wherein the mixed gas comprises air, water vapor, and sulfur dioxide gas.
3. The method for detecting a slip-off rate of a motor vehicle exhaust treatment catalytic converter according to claim 1, wherein before step S1, the method further comprises step S0;
and S0, drying the catalytic converter to be detected.
4. The method for detecting a slip-off rate of a catalytic converter for motor vehicle exhaust gas treatment according to claim 3, wherein the drying temperature is 120 ℃ to 200 ℃ and the drying time is 1 to 2 hours in step S0.
5. The method for detecting a shedding rate of a catalytic converter for treating motor vehicle exhaust according to claim 1, wherein in step S3, the purged catalytic converter is dried before weighing.
6. The method for detecting a slip-off rate of a catalytic converter for motor vehicle exhaust gas treatment according to claim 5, wherein the drying temperature is 120 ℃ to 200 ℃ and the drying time is 1 to 2 hours in step S3.
7. The method for detecting a slip-off rate of a catalytic converter for motor vehicle exhaust gas treatment according to claim 1, wherein in step S3, the pressure of the purge gas flow is 0.3 to 0.6Mpa, and the purge time is 10 to 120 seconds.
8. The method for detecting the shedding rate of the motor vehicle exhaust treatment catalytic converter according to claim 1, wherein the baking furnace is a muffle furnace or a tube furnace.
9. The method of claim 1, wherein the catalytic converter is ultrasonically inspected before step S1 or after step S3.
10. The method of claim 1, wherein a high temperature thermal shock test is performed on the catalytic converter before step S1 or after step S3.
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