CN113702239B - Method for detecting falling rate of catalytic converter for treating tail gas of motor vehicle - Google Patents
Method for detecting falling rate of catalytic converter for treating tail gas of motor vehicle Download PDFInfo
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 110
- 238000000034 method Methods 0.000 title claims abstract description 37
- 238000000576 coating method Methods 0.000 claims abstract description 42
- 239000011248 coating agent Substances 0.000 claims abstract description 40
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000007789 gas Substances 0.000 claims abstract description 28
- 238000010926 purge Methods 0.000 claims abstract description 26
- 238000005303 weighing Methods 0.000 claims abstract description 24
- 238000001816 cooling Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 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
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 19
- 230000035939 shock Effects 0.000 claims description 10
- 238000013461 design Methods 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 14
- 238000010791 quenching Methods 0.000 description 8
- 230000000171 quenching effect Effects 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003993 interaction 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
- 238000012545 processing Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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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)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Exhaust Gas After Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention relates to the technical field of detection of motor vehicle tail gas catalytic converters, in particular to a method for detecting the falling rate of a motor vehicle tail gas treatment catalytic converter, which comprises the following steps of S1, weighing the catalytic converter to be detected to obtain weight M1; s2, roasting the catalytic converter continuously 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, 50-200ppm of sulfur dioxide and 15-25% of oxygen by volume; s3, taking out the catalytic converter, cooling to room temperature, and purging the cooled catalytic converter by using air flow; weighing to obtain a weight M2; s4, calculating the coating falling rate. The connection force of 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 method for detecting the falling rate of 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 exhaust emission limit and the durable mileage of the motor vehicles are more severe, and particularly the durable mileage is increased, the requirement on the durability of the exhaust gas purifying catalytic converter is higher. The catalytic converter is mainly divided into two parts, namely a coating and a carrier. The strength of the connection force between the coating layers and the carrier plays 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 durable mileage, so that the performance of the catalytic converter is gradually attenuated, and the emission regulation requirement can not be met when the catalytic converter is serious. Therefore, the adhesion between the coating layers and the support is generally expressed by the falling rate, and a method for studying the falling rate of the coating layers has become a key point of interest.
At present, the following methods are mainly used for measuring the coating falling rate: (1) ultrasonic method, (2) high temperature thermal shock method. For example, chinese patent CN201610006674.1 mentions that the catalyst operating temperature is below 0 ℃ (cold start in winter) to above 1000 ℃ and the rate of temperature rise and fall is very high (quench quenching); space velocity is 0-100000 hours -1 A range of variation; under the condition that the working pressure is also wide in variation range, a large number of cracks can appear on the coating, the coating is continuously dropped, and the durability of the catalyst is seriously affected. The process of quenching and quenching at a temperature up to 1000 ℃ is known in the industry as the high temperature thermal shock process. The patent also mentions the use of ultrasound to detect the shedding of the catalyst coating. The ultrasonic method is mainly used for simulating mechanical vibration in the placement environment of the catalytic converter, so that the influence of the mechanical vibration on the falling-off of the coating is measured. The high-temperature thermal shock method is mainly used for simulating quenching and quenching conditions in the environment where the catalytic converter is placed, so that the influence of thermal stress on coating shedding is measured.
In practice, besides mechanical vibration, quenching and quenching, the application environment of the catalytic converter also contains constant temperature and chemical substances (such as water vapor, sulfur dioxide and the like), and these conditions also have risks of potentially influencing the coating detachment, especially the chemical substances can react with the coating to cause the cracking and detachment of the coating, which is not studied in the above patent.
The existing ultrasonic method and high-temperature thermal shock method cannot comprehensively evaluate the shedding rate of the catalytic converter, and the risk of shedding of the coating exists in the application process.
Disclosure of Invention
The invention aims at: aiming at the problem that the shedding rate of the catalytic converter cannot be comprehensively estimated in the prior art and the coating shedding risk exists in the application process, the method for detecting the shedding rate of the catalytic converter for treating the tail gas of the motor vehicle is provided. According to the method, steam and sulfur dioxide are introduced under the high-temperature condition, the using environment is simulated, the defects of ultrasonic waves and a thermal shock detection method can be overcome, and the connection force of the coating and the carrier of the catalytic converter in practical application can be well and perfectly estimated.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for detecting the falling rate of catalytic converter for treating tail gas of motor vehicle includes such steps as,
s1, weighing a catalytic converter to be detected to obtain a weight M1;
s2, roasting the catalytic converter continuously 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, 50-200ppm of sulfur dioxide and 15-25% of oxygen by volume;
s3, taking out the catalytic converter, cooling to room temperature, and purging the cooled catalytic converter by using air flow; weighing to obtain a weight M2;
s4, calculating the falling rate of the coating,
as a preferred embodiment of the present invention, the mixed gas is composed of air, water vapor, and sulfur dioxide gas.
As a preferred embodiment of the present invention, step S0 is further included before step S1; 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.
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 scheme of the invention, in the step S3, the pressure of the purging airflow is 0.3-0.6Mpa, and the purging time is 10-120 seconds.
As a preferable mode of the invention, the roasting furnace is a muffle furnace or a tube furnace.
As a preferred embodiment of the present invention, the catalytic converter is subjected to ultrasonic detection before step S1 or after step S3.
As a preferred embodiment of the present invention, the catalytic converter is subjected to high temperature thermal shock detection before step S1 or after step S3.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows:
the invention relates to a method for detecting the falling rate of a catalytic converter for treating tail gas of a motor vehicle. The invention overcomes 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 method, the connection force of the coating and the carrier of the catalytic converter in practical application can be more perfectly evaluated, and the risk of falling off of the coating 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 image of the treated state of the catalytic converter A-5 in example 1 of the present invention, under the treatment conditions of 800-200 h-10% H 2 O-100ppmSO 2 。
FIG. 2 is an SEM image of the untreated state of the catalytic converter A-3 of comparative example 3 of the present invention.
FIG. 3 is an SEM image of the treated state of the catalytic converter A-3 of comparative example 3 of the present invention, and the calcination treatment conditions were 800 to 200 hours.
FIG. 4 is an SEM image of the treated state of the catalytic converter A-4 of comparative example 4 under the treatment conditions of 800 to 200h to 10% H 2 O。
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The catalytic converter for experiments is selected from a self-made catalytic converter by a company, and the serial numbers of the catalytic converters are A-1, A-2, A-3, A-4, A-5, A-6, A-7 and A-8 respectively; eight catalysts used the same batch of support and coating.
Example 1
Selecting a catalytic converter A-5, and drying at 150 ℃ for 1 hour; after cooling to room temperature, weighing to obtain weight M1;
placing the catalytic converter in a tube furnace, and introducing air containing 10% of water vapor and 100ppm of sulfur dioxide by volume fraction; roasting the catalytic converter at 800 ℃ for 200 hours;
after cooling to room temperature, taking out the catalytic converter, and purging the catalytic converter for 30 seconds after treatment by using air with the air pressure of 0.6 MPa; placing the purged catalytic converter in an oven at 120 ℃ for 2 hours, and weighing to obtain weight M2; the coating shedding rate (M1-M2)/M1 after purging was calculated.
Example 2
Selecting a catalytic converter A-6, and drying at 120 ℃ for 2 hours; after cooling to room temperature, weighing to obtain weight M1;
placing the catalytic converter in a muffle furnace, and introducing air containing 20% of water vapor and 200ppm of sulfur dioxide by volume percent; roasting the catalytic converter at 900 ℃ for 100 hours;
after cooling to room temperature, taking out the catalytic converter, and purging the catalytic converter for 50 seconds after treatment by using air with the air pressure of 0.3 MPa; placing the purged catalytic converter in an oven at 120 ℃ for 2 hours, and weighing to obtain weight M2; the coating shedding rate (M1-M2)/M1 after purging was calculated.
Example 3
Selecting a catalytic converter A-7, and drying at 200 ℃ for 1 hour; after cooling to room temperature, weighing to obtain weight M1;
placing the catalytic converter in a tube furnace, and introducing air containing 15% of water vapor and 150ppm of sulfur dioxide by volume percent; roasting the catalytic converter at 950 ℃ for 50 hours;
after cooling to room temperature, taking out the catalytic converter, and purging the catalytic converter for 120 seconds after treatment by using air with the air pressure of 0.4 MPa; placing the purged catalytic converter in an oven at 120 ℃ for 2 hours, and weighing to obtain weight M2; the coating shedding rate (M1-M2)/M1 after purging was calculated.
Example 4
Selecting a catalytic converter A-8, and drying at 140 ℃ for 1 hour; after cooling to room temperature, weighing to obtain 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 percent; continuously roasting the catalytic converter for 100 hours at 950 ℃;
after cooling to room temperature, taking out the catalytic converter, and purging the catalytic converter for 100 seconds after treatment by using air with the air pressure of 0.6 MPa; placing the purged catalytic converter in an oven at 150 ℃ for 2 hours, and weighing to obtain weight M2; the coating shedding rate (M1-M2)/M1 after purging was calculated.
Comparative example 1Ultrasonic detection
Selecting a catalytic converter A-1, and drying at 150 ℃ for 1 hour; after cooling to room temperature, weight M1 was obtained by weighing. Roasting for 10min at 900 ℃ in a tube furnace, cooling to room temperature, placing in an ultrasonic cleaning device, ultrasonically cleaning for 10min, and drying at 120 ℃ 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 treatment at 120 ℃ for 2 hours, and weighing to obtain weight M2; and (5) calculating the coating falling rate after purging.
Comparative example 2High temperature thermal shock detection
Selecting a catalytic converter A-2, and drying at 150 ℃ for 1 hour; after cooling to room temperature, weight M1 was obtained by weighing. Carrying out cold and hot impact for 3 times at room temperature-1000 ℃ in a muffle furnace, purging the catalytic converter for 30 seconds by using 0.6MPa air pressure after the catalytic converter is purged, placing the catalytic converter in an oven for processing for 2 hours at 120 ℃, and weighing to obtain weight M2; and (5) calculating the coating falling rate after purging.
Comparative example 3Roasting but not introducing steam and sulfur dioxide
Selecting a catalytic converter A-3, and drying at 150 ℃ for 1 hour; after cooling to room temperature, weight M1 was obtained by weighing. Placing in a tube furnace and roasting at 800 ℃ for 200 hours. Removing the catalytic converter, cooling to room temperature, purging the catalytic converter for 30 seconds by using the air pressure of 0.6MPa, placing the catalytic converter after purging in an oven at 120 ℃ for 2 hours, and weighing to obtain the weight M2; and (5) calculating the coating falling rate after purging. FIG. 2 is an SEM image of an untreated state of A-3. FIG. 3 is an SEM image of A-3 after 800-200 h of treatment.
Comparative example 4Roasting and introducing steam but not sulfur dioxide
Selecting a catalytic converter A-4, and drying at 150 ℃ for 1 hour; after cooling to room temperature, weight M1 was obtained by weighing. Placing the mixture in a tube furnace, introducing 10% of water vapor, and roasting the catalytic converter at 800 ℃ for 200 hours. Removing the catalytic converter, cooling to room temperature, purging the catalytic converter for 30 seconds by using the air pressure of 0.6MPa, placing the catalytic converter after purging in an oven at 120 ℃ for 2 hours, and weighing to obtain the weight M2; and (5) 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 falling rate tests in comparative examples 1 to 4 and examples 1 to 4 are shown in the following table.
TABLE 1 results of the shedding Rate of catalytic converter coatings
| Numbering device | Catalytic converter numbering | Coating falling off rate (%) |
| 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 |
Remarks: 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 shedding rate values obtained by different detection methods have great difference. An increase in the slip-off value under the conditions of the examples would result in an increase in the catalytic converter performance loss; the method shows that the connection force between the coating and the coating or between the coating and the carrier is greatly affected by water vapor and sulfur dioxide under certain constant temperature conditions. The detection method of the embodiment can effectively identify the risk of falling of the coating of the catalytic converter, so that the unreasonable design of the catalytic converter is avoided, and the effective design meets the emission regulations of longer mileage.
Test example 1Electron microscope experiment
To observe the effect of water vapor and sulfur dioxide on the catalytic converter coating at constant temperature, A-3 (untreated state), A-3 (800-200 h), A-4 (800-200 h-10% H) in comparative example 3, comparative example 4 2 O), A-5 of example 1 (800-200 h-10% H 2 O-100ppmSO 2 ) SEM experiments were performed and the results are shown in FIGS. 1-4.
As can be seen from SEM comparison, H 2 O、SO 2 Larger cracks between the coatings can be caused, and the cracks can lead to larger coating falling-off rates. The method of example 1 was used to accurately simulate the interaction of chemicals with the coating during application of the catalytic converter.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (10)
1. A method for detecting the falling rate of a catalytic converter for treating motor vehicle tail gas is characterized by comprising the following steps,
s1, weighing a catalytic converter to be detected to obtain a weight M1;
s2, roasting the catalytic converter continuously 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, 50-200ppm of sulfur dioxide and 15-25% of oxygen by volume;
s3, taking out the catalytic converter, cooling to room temperature, and purging the cooled catalytic converter by using air flow; weighing to obtain a weight M2;
s4, calculating the falling rate of the coating,
2. the method for detecting the falling rate of a catalytic converter for treating motor vehicle exhaust according to claim 1, wherein the mixed gas is composed of air, water vapor, sulfur dioxide gas.
3. The method for detecting the falling-off rate of a catalytic converter for treating motor vehicle exhaust gas according to claim 1, further comprising step S0 before step S1;
s0, drying the catalytic converter to be detected.
4. The method for detecting the falling rate of a catalytic converter for treating motor vehicle exhaust gas according to claim 3, wherein in the step S0, the drying temperature is 120 ℃ to 200 ℃ and the drying time is 1 to 2 hours.
5. The method for detecting the falling-off rate of a catalytic converter for treating motor vehicle exhaust gas according to claim 1, wherein in step S3, the catalytic converter after purging is dried before weighing.
6. The method for detecting the falling off rate of a catalytic converter for treating motor vehicle exhaust according to claim 5, wherein in step S3, the drying temperature is 120 ℃ to 200 ℃ and the drying time is 1 to 2 hours.
7. The method for detecting the falling off rate of a catalytic converter for treating motor vehicle exhaust gas according to claim 1, wherein in the step S3, the pressure of the purge gas is 0.3 to 0.6Mpa, and the purge time is 10 to 120 seconds.
8. The method for detecting the falling-off rate of a catalytic converter for treating motor vehicle exhaust gas according to claim 1, wherein the roasting furnace is a muffle furnace or a tube furnace.
9. The method for detecting the falling-off rate of a catalytic converter for treating motor vehicle exhaust gas according to claim 1, wherein the catalytic converter is subjected to ultrasonic detection before step S1 or after step S3.
10. The method for detecting the falling-off rate of a catalytic converter for treating motor vehicle exhaust gas according to claim 1, wherein the catalytic converter is subjected to high-temperature thermal shock detection before step S1 or after step S3.
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