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CN112047720A - Preparation method of high-porosity particle catcher - Google Patents

Preparation method of high-porosity particle catcher Download PDF

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Publication number
CN112047720A
CN112047720A CN202010988569.9A CN202010988569A CN112047720A CN 112047720 A CN112047720 A CN 112047720A CN 202010988569 A CN202010988569 A CN 202010988569A CN 112047720 A CN112047720 A CN 112047720A
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pore
forming material
temperature
starch
sintering
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缪卫国
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Changzhou Haowei Environmental Protection Technology Co ltd
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Changzhou Haowei Environmental Protection Technology Co ltd
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    • C04B33/00Clay-wares
    • C04B33/02Preparing or treating the raw materials individually or as batches
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
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    • F01N3/00Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
    • F01N3/021Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
    • F01N3/022Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous
    • F01N3/0222Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous the structure being monolithic, e.g. honeycombs
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
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    • F01N3/00Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
    • F01N3/021Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
    • F01N3/033Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices
    • F01N3/035Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters in combination with other devices with catalytic reactors, e.g. catalysed diesel particulate filters
    • BPERFORMING OPERATIONS; TRANSPORTING
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Abstract

The invention relates to a preparation method of a high-porosity particle catcher, which comprises the following steps: mixing 10-60% of starch pore-forming material, 0.1-30% of organic matter pellet pore-forming material and 5-30% of carbon source pore-forming material to form pore-forming material; mixing 40-45% of talc, 10-20% of kaolin, 20-30% of alumina and 10-15% of silicon oxide to form an inorganic raw material; then, according to the ratio of the inorganic raw materials to the pore-forming material of 10: 2-5, adding 6-10% of binder and 1-2% of lubricant, adding 20-30% of water, and stirring; extruding the materials by an extruder; drying the honeycomb ceramic blank body by a dryer; and (3) putting the dried honeycomb ceramic blank into a sintering furnace, gradually increasing the temperature from room temperature to 1420 ℃, increasing the temperature by 30 ℃ per hour, and then keeping the temperature at 1420 ℃ for 8 hours. By utilizing the ternary pore-forming material system, the requirement of high porosity is met, and the heat accumulation during sintering is reduced by staggering the heating peaks, so that the occurrence of sintering cracking is reduced.

Description

Preparation method of high-porosity particle catcher
Technical Field
The invention relates to an automobile exhaust treatment device, in particular to a preparation method of a high-porosity particle catcher.
Background
Honeycomb ceramic particle trap technology has been widely used in the treatment of automobile and truck exhaust. In general, the honeycomb ceramic particle catcher adopts a wall-flow type filtration mode to remove particles in tail gas. The principle is that every other hole is blocked at the inlet, and the other hole is kept smooth; while at the outlet the corresponding hole remains blocked or unblocked conversely. Therefore, the honeycomb ceramic is in a chessboard type of the chess, and ensures that tail gas must pass through the wall, thereby achieving the purpose of retaining particles in the tail gas on the wall.
In application, particles (such as carbon black) in the tail gas are gathered in a channel which is not blocked at the inlet, and after a certain amount of particles is obtained, a computer system starts a regeneration process to burn off the collected carbon black, so that the back pressure of the system is reduced. Since most of such carbon blacks are small particles of micron or nanometer size, their burning speed is extremely fast, releasing a large amount of heat in a very short time (within ten or more minutes), causing a sharp rise in the internal temperature of the particle trap. If the control is not good, the particle catcher can be burnt. By computer control of the regeneration step, the risk of melting can be reduced. However, thermal stress resulting from too high and too fast a temperature rise is always present and is a major cause of particle trap cracking. Therefore, the particulate trap for a general diesel engine has a large heat capacity, and thus the temperature rising rate during regeneration is reduced. When the material is fixed, the increase of the heat capacity is realized by depending on the weight of the material, and the specific method is to increase the wall thickness.
At the same time, the material must have a certain porosity, e.g. 50-65%, in order to reduce the back pressure of the particle trap. In the case of the particle catcher, besides the pores of the material itself, the pores are formed by adding pore-forming material to increase the porosity to the expected range. Such pore-forming materials are burned off during the low temperature stage of sintering (150-. Typical pore-forming materials include carbon (graphite, activated carbon, carbon black), nutshell powder, starch, organic spheres, and the like. Although the pore-forming materials are different in types, they all have the following characteristics: exothermic upon burning off. Due to the fact that the addition amount of the pore-forming material in the formula of the particle catcher is large and the heat storage is large, the temperature of the center is increased too fast in the process, the temperature difference between the center and the periphery is increased, and sintering cracking is caused. To reduce the possibility of cracking, the temperature rise rate of the furnace is generally slowed, so that the pore-forming material slowly burns and releases heat, thereby reducing the temperature rise rate of the particle trap. For particle traps (greater than 10 inches in diameter) sintering processes, the total time is typically over 120 hours.
To meet ever more stringent exhaust emission standards, more and more catalyst is coated on the particle trap. This results in an increase in back pressure due to the pores being filled with catalyst. Therefore, for the case of high catalyst coating, high porosity materials are generally employed. The porosity of the material is more than 60%, so that the material can contain more catalyst and has good back pressure performance.
To increase porosity, more pore-forming material is typically added to the formulation. However, when the pore-forming material is contained to a certain extent, the porosity cannot be increased more by increasing the content thereof. On the other hand, excessive pore-forming material increases heat generation during sintering, thereby increasing the possibility of sintering cracking. Therefore, it is necessary to adjust the pore-forming material ratio in the formulation so as to not only meet the requirement of high porosity performance, but also avoid the possibility of sintering cracking.
Disclosure of Invention
The invention aims to provide a preparation method of a high-porosity particle catcher, which utilizes a ternary pore-forming material system to meet the requirement of high porosity and reduces heat accumulation during sintering by staggering a heating peak so as to reduce the occurrence of sintering cracking.
In order to achieve the purpose, the technical scheme of the invention is as follows: a preparation method of a high-porosity particle catcher comprises the following steps:
s1: mixing 10-60% of starch pore-forming material, 0.1-30% of organic matter pellet pore-forming material and 5-30% of carbon source pore-forming material, wherein the percentage of the formula is weight percentage, forming the pore-forming material, and analyzing exothermic peaks of various pore-forming materials by using differential scanning calorimetry;
s2: mixing 40-45% of talc, 10-20% of kaolin, 20-30% of alumina and 10-15% of silicon oxide, wherein the formula percentage is weight percentage to form inorganic raw materials;
s3: then, according to the ratio of the inorganic raw materials to the pore-forming material of 10: 2-5, adding 6-10% of binder and 1-2% of lubricant, adding 20-30% of water, and stirring to obtain a material;
s4: extruding the materials by an extruder to form a honeycomb ceramic blank;
s5: drying the honeycomb ceramic blank body by a dryer at the drying temperature of 80-120 ℃ for 20-40 minutes;
s6: and finally, sintering, namely putting the dried honeycomb ceramic blank into a sintering furnace, gradually raising the temperature from room temperature to 1420 ℃, raising the temperature at 30 ℃ per hour, keeping the temperature at 1420 ℃ for 8 hours, and finally taking out and naturally cooling.
The starch pore-forming material is one or more of corn starch, potato starch, lotus root starch and pea starch.
The organic small ball pore-forming material is a small ball-shaped thermoplastic acrylic polymer.
The carbon source pore-forming material is one or more of graphite, activated carbon and nut shell powder.
20-40% of starch pore-forming material.
0.5-5% of organic small-ball pore-forming material.
The binder is hydroxypropyl methyl cellulose, and the lubricant is potassium laurate.
After the method is adopted, the pore-forming material with different exothermic peaks is selected, so that exothermic in the sintering process can be released dispersedly, and the pore-forming material is heated slowly from normal temperature to 1420 ℃ in the heating process. Therefore, the sample is prevented from being heated up rapidly, the temperature difference between the inside and the outside of the sample is reduced, and the thermal stress is finally reduced. Experiments prove that the temperature difference can be reduced to half or less than that of a unitary pore-forming material by applying the ternary pore-forming material, so that the requirement of high porosity is met, and the heat accumulation during sintering is reduced by staggering the heating peaks, so that the occurrence of sintering cracking is reduced.
Detailed Description
The examples given below illustrate the invention in further detail.
According to the invention, three pore-forming materials are matched, the exothermic peak values of the pore-forming materials are in different temperature ranges, the three pore-forming materials are respectively 50% of starch, 20% of organic matter globules and 30% of graphite, and the pore-forming materials are formed after mixing.
Mixing 40% of talc, 20% of kaolin, 30% of alumina and 10% of silicon oxide, wherein the formula percentage is weight percentage, and forming an inorganic raw material; the proportion of the inorganic raw materials and the pore-forming materials is as follows, the invention adopts five proportions of ABCDE as comparison, see Table 1;
TABLE 1
Figure BDA0002690070680000041
Then, 4% of a binder, 1% of a lubricant, etc., and 26% of water were added to each formulation, and after mixing, the mixture was extruded into 200/12 honeycomb ceramic green bodies having a diameter of 280mm, wherein 200 means 200 cells per square inch and 12 means 12. mu. inches in wall thickness. And drying the blank body, and sintering. Drying the mixture by a dryer at 100 ℃ for 30 minutes;
s6: and finally, sintering, namely putting the dried honeycomb ceramic blank into a sintering furnace, gradually raising the temperature from room temperature to 1420 ℃, raising the temperature at 30 ℃ per hour, keeping the temperature at 1420 ℃ for 8 hours, and finally taking out and naturally cooling.
The exothermic peaks of the various pore-forming materials were analyzed by Differential Scanning Calorimetry (DSC). The exothermic peak values of the organic pellets, the starch and the graphite are respectively 280 ℃ and 182 ℃ respectively.
In order to measure the difference between the internal temperature and the external temperature during the sintering of the blank, one S-shaped thermocouple is inserted into the center of the sample, and the other S-shaped thermocouple is placed outside the sample and close to the skin. Heating from room temperature to 1420 deg.C at a rate of 30 deg.C/hr, holding at 1420 deg.C for 8 hr, and cooling. The maximum temperature difference results for the various formulations are shown in table 2.
TABLE 2
Formulation of Maximum temperature difference (. degree. C.) Maximum temperature difference corresponds to furnace temperature (DEG C)
A 185 310
B 163 308
C 120 305
D 85 300
E 83 300
As can be seen from Table 2, the furnace temperature corresponding to the maximum temperature difference is about 300-310 ℃, and the various formulas are not greatly different. However, the maximum temperature difference is very different depending on the formulation. The maximum temperature difference is reduced along with the reduction of the content of the starch substances, and the maximum temperature difference can be reduced by about half by reducing 70 percent of the starch substances. Due to the reduction of the temperature difference, the possibility of cracking can be greatly reduced, and the sintering time can be reduced.
The sintered samples were subjected to porosity tests and the results are shown in Table 3.
TABLE 3
Formulation of Porosity (%) Average pore diameter (um)
A 51.3 18.3
B 49.5 17.6
C 50.5 16.8
D 51.5 15.9
E 48.3 16.3
As can be seen from table 3, the use of two or more pore-forming materials does not have a significant effect on the porosity after sintering, and the pore size can be adjusted. For the formulation with the target of about 50% porosity, the aim can be achieved by using less than 8% of starch substances, adding 0.5-3% of organic small balls and adding proper graphite.
By combining the above results, the pore-forming materials with different exothermic peaks are purposefully selected, and the exothermic in the sintering process can be dispersedly released, so that the sample is prevented from being rapidly heated, the temperature difference between the inside and the outside of the sample is reduced, and the thermal stress is finally reduced. Experiments prove that the temperature difference can be reduced to half or less than that of a unitary pore-forming material by applying a binary or ternary pore-forming material, so that sintering cracking is effectively avoided, and the sintering time is saved. In addition, the required porosity and pore size can be achieved by proper pore-forming material proportion.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications are all within the scope of the present invention.

Claims (7)

1. A preparation method of a high-porosity particle catcher is characterized by comprising the following steps: the preparation method comprises the following steps:
s1: mixing 10-60% of starch pore-forming material, 0.1-30% of organic matter pellet pore-forming material and 5-30% of carbon source pore-forming material, wherein the percentage of the formula is weight percentage, forming the pore-forming material, and analyzing exothermic peaks of various pore-forming materials by using differential scanning calorimetry;
s2: mixing 40-45% of talc, 10-20% of kaolin, 20-30% of alumina and 10-15% of silicon oxide, wherein the formula percentage is weight percentage to form inorganic raw materials;
s3: then, according to the ratio of the inorganic raw materials to the pore-forming material of 10: 2-5, adding 6-10% of binder and 1-2% of lubricant, adding 20-30% of water, and stirring to obtain a material;
s4: extruding the materials by an extruder to form a honeycomb ceramic blank;
s5: drying the honeycomb ceramic blank body by a dryer at the drying temperature of 80-120 ℃ for 20-40 minutes;
s6: and finally, sintering, namely putting the dried honeycomb ceramic blank into a sintering furnace, gradually raising the temperature from room temperature to 1420 ℃, raising the temperature at 30 ℃ per hour, keeping the temperature at 1420 ℃ for 8 hours, and finally taking out and naturally cooling.
2. The method of making a high porosity particle trap as defined in claim 1, wherein: the starch pore-forming material is one or more of corn starch, potato starch, lotus root starch and pea starch.
3. The method of making a high porosity particle trap as defined in claim 1, wherein: the organic small ball pore-forming material is a small ball-shaped thermoplastic acrylic polymer.
4. The method of making a high porosity particle trap as defined in claim 1, wherein: the carbon source pore-forming material is one or more of graphite, activated carbon and nut shell powder.
5. The method of making a high porosity particle trap as defined in claim 1, wherein: 20-40% of starch pore-forming material.
6. The method of making a high porosity particle trap as defined in claim 3, wherein: 0.5-5% of organic small-ball pore-forming material.
7. The method of making a high porosity particle trap as defined in claim 1, wherein: the binder is hydroxypropyl methyl cellulose, and the lubricant is potassium laurate.
CN202010988569.9A 2020-09-18 2020-09-18 Preparation method of high-porosity particle catcher Pending CN112047720A (en)

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Publication number Priority date Publication date Assignee Title
WO2006006667A1 (en) * 2004-07-14 2006-01-19 Ngk Insulators, Ltd. Method for manufacturing porous honeycomb structure
US20070142208A1 (en) * 2005-12-21 2007-06-21 Addiego William P High porosity cordierite ceramic honeycomb article and method
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WO2012023617A1 (en) * 2010-08-19 2012-02-23 日立金属株式会社 Manufacturing method for ceramic honeycomb structure
CN108675826A (en) * 2018-06-29 2018-10-19 凯龙高科技股份有限公司 A kind of cordierite wall-flow honeycomb ceramic filter and preparation method thereof
CN111423248A (en) * 2020-05-14 2020-07-17 常州浩蔚环保科技有限公司 Production process of particle catcher

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006006667A1 (en) * 2004-07-14 2006-01-19 Ngk Insulators, Ltd. Method for manufacturing porous honeycomb structure
US20070142208A1 (en) * 2005-12-21 2007-06-21 Addiego William P High porosity cordierite ceramic honeycomb article and method
JP2010001184A (en) * 2008-06-20 2010-01-07 Nippon Soken Inc Method for manufacturing exhaust gas filter
WO2012023617A1 (en) * 2010-08-19 2012-02-23 日立金属株式会社 Manufacturing method for ceramic honeycomb structure
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Application publication date: 20201208