CN114956853A - Honeycomb ceramic, preparation method and application thereof, and honeycomb filter - Google Patents

Honeycomb ceramic, preparation method and application thereof, and honeycomb filter Download PDF

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Publication number
CN114956853A
CN114956853A CN202210561444.7A CN202210561444A CN114956853A CN 114956853 A CN114956853 A CN 114956853A CN 202210561444 A CN202210561444 A CN 202210561444A CN 114956853 A CN114956853 A CN 114956853A
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Prior art keywords
honeycomb ceramic
honeycomb
sintering aid
silicon carbide
aluminum oxide
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CN202210561444.7A
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Chinese (zh)
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朱恒
王建业
王键
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Shandong Sinocera Functional Material Co Ltd
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Shandong Sinocera Functional Material Co Ltd
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Priority to CN202210561444.7A priority Critical patent/CN114956853A/en
Publication of CN114956853A publication Critical patent/CN114956853A/en
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    • C04B38/0006—Honeycomb structures
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    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
    • F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
    • F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
    • F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
    • F01N3/021—Exhaust 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
    • F01N3/022—Exhaust 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
    • F01N3/0222—Exhaust 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
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
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    • F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
    • F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
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    • F01N3/2803—Construction of catalytic reactors characterised by structure, by material or by manufacturing of catalyst support
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Abstract

The invention discloses a honeycomb ceramic, a preparation method and application thereof and a honeycomb filter, and belongs to the technical field of honeycomb ceramics. The porosity of the honeycomb ceramic is 35-50%, and the bending strength is 5-15 MPa; the contact angle between silicon and silicon carbide in the honeycomb ceramic is 110-140 degrees. The raw materials for preparing the honeycomb ceramic comprise silicon carbide, metal silicon powder and a sintering aid; the sintering aid comprises aluminum oxide, strontium carbonate and magnesium hydroxide; the grain size of the aluminum oxide is 1-15um, the grain size of the strontium carbonate is 0.5-20um, and the grain size of the magnesium hydroxide is 1-15 um. The invention is applied to the aspect of tail gas treatment, solves the problem that the application range of the existing honeycomb ceramic body is limited due to low strength and porosity, and can give consideration to both high strength and moderate porosity.

Description

Honeycomb ceramic, preparation method and application thereof, and honeycomb filter
Technical Field
The invention belongs to the technical field of honeycomb ceramics, and particularly relates to honeycomb ceramics, a preparation method and application thereof, and a honeycomb filter.
Background
With the rapid development of technology, automobiles on roads are increasing, but exhaust gas from internal combustion engines such as diesel engines, various combustion apparatuses, and the like contains a large amount of particulate matter such as soot. Since these pollutants are directly discharged into the atmosphere, they cause serious environmental pollution, and therefore, it is necessary to provide a filter device for collecting particulate matter in a flow path of exhaust gas and treating the exhaust gas. In order to trap harmful substances such as nitrogen oxides (NOx) and carbon monoxide (CO) generated when exhaust gas and waste of an automobile are incinerated, and dust and other particulate substances contained therein, a honeycomb filter made of a honeycomb ceramic structure, such as a diesel particulate filter (hereinafter, also referred to as "DPF"), is used for an automobile as a catalyst carrier for purification and for trapping particulate substances in exhaust gas, and particulate substances such as soot discharged from an internal combustion engine can be effectively removed. However, many conventional ceramic honeycomb structures have a problem that the mechanical strength is low and the collection efficiency is low because the partition walls are thin and the porosity is high.
Chinese CN108386254A discloses a plugged honeycomb structure in which the cell walls are made of a material containing silicon carbide, the porosity of the cell walls measured by mercury porosimetry is 42 to 52%, the thickness of the cell walls is 0.15 to 0.36mm, the porosity of the honeycomb structure is moderate, the trapping performance is excellent, and the increase rate of pressure loss can be reduced.
However, the honeycomb ceramic body proposed in the above patent still has a problem of low strength, and thus, it cannot really overcome the problem of limited application range of the existing honeycomb ceramic body due to low strength and porosity.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve the technical problem that the application range of the existing honeycomb ceramic body is limited due to low strength and porosity, and provides a honeycomb ceramic which can give consideration to high strength and moderate porosity, a preparation method and application thereof, and a honeycomb filter.
In order to solve the technical problem, the technical scheme adopted by the invention is as follows:
on one hand, the invention provides a honeycomb ceramic, the porosity of the honeycomb ceramic is 35% -50%, and the bending strength is 5-15 MPa; the contact angle between silicon and silicon carbide in the honeycomb ceramic is 110-140 degrees.
Preferably, the raw materials for preparing the honeycomb ceramic comprise silicon carbide, metal silicon powder and a sintering aid;
the sintering aid comprises aluminum oxide, strontium carbonate and magnesium hydroxide;
the particle size of the aluminum oxide is 1-15um, the particle size of the strontium carbonate is 0.5-20um, and the particle size of the magnesium hydroxide is 1-15 um.
Preferably, the raw materials for preparing the honeycomb ceramic consist of silicon carbide, metal silicon powder and a sintering aid; the sintering aid consists of aluminum oxide, strontium carbonate and magnesium hydroxide.
Preferably, the sintering aid is prepared by a ball milling method.
Preferably, the ball milling speed is 250-400r/min, and the time duration is 25-50 min.
Preferably, the ball milling apparatus is a planetary ball mill.
Another aspect of the present invention provides a method for preparing a honeycomb ceramic according to any one of the above technical solutions, including: ball milling and pre-dispersing aluminum oxide, strontium carbonate and magnesium hydroxide, fully mixing with silicon carbide and metal silicon powder, pugging and extruding to form unit strips; drying, cutting and plugging the unit strips; then degreasing, sintering and oxidizing; and finally, splicing, grinding and skin grafting to prepare the honeycomb ceramic.
The invention also provides application of the honeycomb ceramic in any technical scheme in tail gas treatment.
The invention finally provides a honeycomb filter which is prepared from the honeycomb ceramic in any technical scheme.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides honeycomb ceramic, wherein the contact angle between silicon and silicon carbide is reduced by 20-30 degrees, and the silicon is better infiltrated among silicon carbide particles; the porosity of the honeycomb ceramic reaches 35-50%, and the bending strength reaches 5-15 MPa;
the invention also provides a preparation method of the honeycomb ceramic, which is simple, does not need to add other types of raw materials and does not need a complex processing technology, and the prepared honeycomb ceramic product has stable quality and good consistency, and the yield is more than or equal to 99 percent;
the invention also provides a honeycomb filter which has the characteristics of high strength, moderate porosity, trapping efficiency and no increase of the oil consumption of an automobile.
Detailed Description
The technical solutions in the embodiments of the present invention will be fully described in detail below. It is obvious that the described embodiments are only some specific embodiments, not all embodiments, of the general technical solution of the present invention. All other embodiments, which can be derived by a person skilled in the art from the general idea of the invention, fall within the scope of protection of the invention.
The invention provides a honeycomb ceramic, wherein the porosity of the honeycomb ceramic is 35% -50%, the bending strength is 5-15MPa, and the contact angle between silicon and silicon carbide in the honeycomb ceramic is 140 degrees. The honeycomb ceramic provided by the embodiment has the characteristics of high strength and moderate porosity, and has the characteristics of trapping efficiency and no increase of automobile oil consumption when being applied to a honeycomb filter. The porosity of the honeycomb ceramic is limited by the technical scheme, because the too high porosity can increase the volume of large pores and reduce the trapping efficiency; and if the porosity is too low, the backpressure of the silicon carbide DPF is increased, so that the oil consumption of the automobile is increased. The technical scheme further defines a contact angle between silicon and silicon carbide in the honeycomb ceramic, the contact angle is reduced by 20-30 degrees, the silicon is better infiltrated among silicon carbide particles, the mechanical property of a honeycomb ceramic structure body is enhanced, and the water absorption rate and the porosity are effectively controlled.
In a preferred embodiment, the raw materials for preparing the honeycomb ceramic comprise silicon carbide, metal silicon powder and a sintering aid; the sintering aid comprises aluminum oxide, strontium carbonate and magnesium hydroxide; the particle size of the aluminum oxide is 1-15um, the particle size of the strontium carbonate is 0.5-20um, and the particle size of the magnesium hydroxide is 1-15 um. The embodiment improves the mechanical property and porosity of the honeycomb ceramic structure unit strip by limiting the granularity of the sintering aid, thereby improving the production of the honeycomb ceramicAnd (4) performance of the product. Wherein the aluminum oxide is Al 2 O 3 Calculated as SrCO, strontium carbonate 3 In terms of Mg (OH) 2 And (6) counting. By limiting the type and particle size of the sintering aid, the sintering aid can react with silicon dioxide on the silicon surface during sintering to increase the wettability of silicon, so that silicon can be better infiltrated among silicon carbide particles to increase the mechanical strength of the honeycomb ceramic structure. Furthermore, the technical scheme of the application limits that the sintering aid comprises aluminum oxide and strontium carbonate, and the sintering aid can be matched with other components to increase the wettability of silicon, so that the silicon can be better infiltrated among silicon carbide particles, the mechanical strength of the honeycomb ceramic structure body is increased, the acid resistance of the honeycomb ceramic structure body is stronger, and the good performance can be still kept in the acidification process.
In addition, the particle sizes of alumina, strontium carbonate, and magnesium hydroxide need to be appropriately matched to obtain a sintered body having high mechanical strength. It is understood that the particle size of the aluminum oxide can also be 2um, 3um, 4um, 5um, 6um, 7um, 8um, 9um, 10um, 11um, 12um, 13um, 14um and any value within the range thereof, the particle size of the strontium carbonate can also be 1um, 2um, 3um, 4um, 5um, 6um, 7um, 8um, 9um, 10um, 11um, 12um, 13um, 14um, 15um, 16um, 17um, 18um, 19um and any value within the range thereof, and the particle size of the magnesium hydroxide can also be 2um, 3um, 4um, 5um, 6um, 7um, 8um, 9um, 10um, 11um, 12um, 13um, 14um and any value within the range thereof.
In a preferred embodiment, the mass of the sintering aid accounts for 0.5-5% of the total mass of the pug.
In a preferred embodiment, the raw materials for preparing the honeycomb ceramic comprise silicon carbide, metal silicon powder and a sintering aid; the sintering aid consists of aluminum oxide, strontium carbonate and magnesium hydroxide. The technical scheme specifically limits the types of raw materials except silicon carbide, metal silicon powder, aluminum oxide, strontium carbonate and magnesium hydroxide, does not contain other components, does not need a complex processing technology, and has low cost, low energy consumption and short production period. The mechanical property and porosity of the honeycomb ceramic structure unit strip can be obviously improved only by adding common moisture and a binding agent to carry out pretreatment on a sintering aid.
In a preferred embodiment, the sintering aid is prepared by a ball milling method. Compared with the granularity of the main raw materials of silicon carbide and metal silicon powder, the granularity of the sintering aids such as aluminum oxide, strontium carbonate and magnesium hydroxide is too small, and the pug is difficult to be fully mixed only by mixing and kneading of a mixing barrel and pugging, so that silicon cannot be well infiltrated among silicon carbide particles during sintering, the mechanical strength of the honeycomb ceramic structural body unit strip is low, the porosity is too high, the volume of large pores is increased due to too high porosity, the collection efficiency is reduced, the back pressure of the silicon carbide DPF is increased due to too low porosity, and the automobile oil consumption is increased. Therefore, the technical scheme limits that the sintering aid is prepared by a ball milling method, the viscosity of slurry particles generated after ball milling dispersion is reduced, the agglomeration among the particles is reduced, the dispersibility is good, and the difference among honeycomb ceramic products is also reduced. In a preferred embodiment, the ball milling apparatus is a planetary ball mill.
In a preferred embodiment, the ball milling speed is 250-400r/min, and the time duration is 25-50 min. If the rotating speed is too low, the ball milling of the sintering aid is insufficient, and if the time is too long, the granularity of the slurry is not uniform. It is understood that the rotational speed may also be 270r/min, 290r/min, 310r/min, 330r/min, 350r/min, 370r/min, 390r/min and any point value within the range thereof, and the time period may also be 30min, 40min, 45min and any point value within the range thereof.
Another aspect of the present invention provides a method for preparing a honeycomb ceramic according to any one of the above technical solutions, including: ball milling and pre-dispersing aluminum oxide, strontium carbonate and magnesium hydroxide, fully mixing with silicon carbide and metal silicon powder, pugging and extruding to form unit strips; drying, cutting and plugging the unit strips; then degreasing, sintering and oxidizing; and finally, splicing, grinding and skin grafting to prepare the honeycomb ceramic. The technical scheme specifically limits that the sintering aid is dispersed and then mixed with the silicon carbide and the silicon metal, and the reason is that the agglomeration of powder due to water absorption can be greatly reduced by slurry generated after the sintering aid is dispersed by ball milling, so that the dispersibility is improved. And secondly, when the silicon carbide and the metal silicon powder are mixed in the form of slurry, the sintering aid can be better mixed in the pug, and the difference between honeycomb ceramic products caused by the non-uniform pug is reduced.
The preparation method of the honeycomb ceramic is simple, other types of raw materials are not required to be added, a complex processing technology is not required, the prepared honeycomb ceramic product is stable in quality and good in consistency, and the yield is more than or equal to 99%.
The invention also provides application of the honeycomb ceramic in any technical scheme in tail gas treatment.
The invention finally provides a honeycomb filter which is prepared from the honeycomb ceramic in any technical scheme. The honeycomb filter has the characteristics of high strength, moderate porosity, trapping efficiency and no increase of the oil consumption of automobiles.
In order to more clearly and specifically describe the honeycomb ceramic, the preparation method, the application and the honeycomb filter provided by the embodiment of the invention, the following description will be made with reference to the specific embodiment.
Example 1
(I) Ball-milling and pre-dispersing the aluminum oxide, strontium carbonate and magnesium hydroxide sintering aid, then fully mixing the aluminum oxide, strontium carbonate and magnesium hydroxide sintering aid with silicon carbide and metal silicon powder, and then performing pugging and extrusion molding;
(II) drying, cutting and plugging the holes of the unit strips obtained in the step (I);
(III) degreasing, sintering and oxidizing the unit strips obtained in the step (II);
and (IV) splicing the unit strips obtained in the step (III), grinding and skin grafting, and finally preparing the honeycomb ceramic structure body.
Wherein the mass of the sintering aid accounts for 0.5-5% of the total mass of the pug, and the particle size, the ball milling rotation speed and the ball milling time of the sintering aid are defined in the table 1 and the example 1.
Example 2
The same as example 1, except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in example 2 of Table 1.
Example 3
The same as example 1, except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in example 3 of Table 1.
Example 4
The same as example 1, except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in example 4 of Table 1.
Example 5
The same as example 1, except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in example 5 of Table 1.
Example 6
The same as example 1, except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in example 6 of Table 1.
Example 7
The same as example 1, except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in example 7 of Table 1.
Example 8
The same as example 1, except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in example 8 of Table 1.
Comparative example 1
The same as example 1 except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in comparative example 1 of Table 1.
Comparative example 2
The same as example 1 except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in comparative example 2 of Table 1.
Comparative example 3
The same as example 1 except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in comparative example 3 of Table 1.
Comparative example 4
The same as example 1 except that the particle size of the sintering aid, the rotation speed of the ball mill and the time of the ball mill were as defined in comparative example 4 of Table 1.
Comparative example 5
The same as example 1 except that the particle size of the sintering aid, the ball milling rotation speed and the ball milling time were as defined in comparative example 5 of table 1.
TABLE 1 EXAMPLES 1-8 AND COMPARATIVE EXAMPLES 1-5 materials
Figure BDA0003656740750000071
Performance testing
The sintered bodies obtained in examples 1 to 8 and comparative examples 1 to 5 were subjected to the following property tests:
(1) three-point bending strength: the test method is GB-T6569-2006;
(2) porosity: the porosity was determined using a mercury porosimeter. In the measurement of the porosity, a part of the partition wall is cut out from the plugged honeycomb structure as a test piece, and the porosity is measured using the obtained test piece. The test piece was a rectangular parallelepiped having a length of about 10mm, and about 20mm, respectively. The sampling site of the test piece was near the center of the honeycomb structural portion in the axial direction.
The test results are shown in table 2.
TABLE 2 test results of the sintered bodies obtained in examples 1 to 8 and comparative examples 1 to 5
Examples Three point bending strength/MPa Porosity/% Percent of yield%
Example 1 7.8 37.4 99.1
Example 2 9.6 38.5 99.5
Example 3 10.9 40.1 99.4
Example 4 13.5 41.2 99.2
Example 5 7.2 36.1 99.6
Example 6 9.1 37.8 99.5
Example 7 11.2 39.1 99.3
Example 8 13.7 40.9 99.5
Comparative example 1 5.2 29.9 85.8
Comparative example 2 1.2 33.4 88.9
Comparative example 3 3.4 34.2 90.7
Comparative example 4 2.8 32.2 95.9
Comparative example 5 3.6 30.1 93.2
If the rotating speed is too low, the ball milling of the sintering aids is insufficient, and the particle size of each sintering aid is larger, so that the mechanical strength and the porosity of the honeycomb ceramic structure are reduced; if the time is too long, the slurry has non-uniform particle size and the slurry has non-uniform composition, which still causes the mechanical strength and porosity of the ceramic honeycomb structure to decrease.

Claims (9)

1. The honeycomb ceramic is characterized in that the porosity of the honeycomb ceramic is 35-50%, and the bending strength is 5-15 MPa; the contact angle between silicon and silicon carbide in the honeycomb ceramic is 110-140 degrees.
2. The honeycomb ceramic of claim 1, wherein raw materials for preparing the honeycomb ceramic comprise silicon carbide, metal silicon powder and a sintering aid;
the sintering aid comprises aluminum oxide, strontium carbonate and magnesium hydroxide;
the particle size of the aluminum oxide is 1-15um, the particle size of the strontium carbonate is 0.5-20um, and the particle size of the magnesium hydroxide is 1-15 um.
3. The honeycomb ceramic of claim 2, wherein the raw materials for preparing the honeycomb ceramic consist of silicon carbide, metallic silicon powder and sintering aid; the sintering aid consists of aluminum oxide, strontium carbonate and magnesium hydroxide.
4. The honeycomb ceramic of claim 2 or 3, wherein the sintering aid is prepared by a ball milling method.
5. The honeycomb ceramic of claim 4, wherein the ball milling speed is 250-400r/min and the duration is 25-50 min.
6. The honeycomb ceramic of claim 5, wherein the ball milling apparatus is a planetary ball mill.
7. The method for producing a honeycomb ceramic according to any one of claims 1 to 6, comprising: ball milling and pre-dispersing aluminum oxide, strontium carbonate and magnesium hydroxide, fully mixing with silicon carbide and metal silicon powder, pugging and extruding to form unit strips; drying, cutting and plugging the unit strips; then degreasing, sintering and oxidizing; and finally, splicing, grinding and skin grafting to prepare the honeycomb ceramic.
8. Use of a honeycomb ceramic according to any one of claims 1 to 6 for exhaust gas treatment.
9. A honeycomb filter produced from the honeycomb ceramic according to any one of claims 1 to 6.
CN202210561444.7A 2022-05-23 2022-05-23 Honeycomb ceramic, preparation method and application thereof, and honeycomb filter Pending CN114956853A (en)

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CN113443914A (en) * 2020-03-25 2021-09-28 日本碍子株式会社 Method for producing silicon carbide-containing honeycomb structure

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