CN110304937A - A kind of ceramic honeycomb filter carrier and preparation method thereof - Google Patents

A kind of ceramic honeycomb filter carrier and preparation method thereof Download PDF

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Publication number
CN110304937A
CN110304937A CN201910701890.1A CN201910701890A CN110304937A CN 110304937 A CN110304937 A CN 110304937A CN 201910701890 A CN201910701890 A CN 201910701890A CN 110304937 A CN110304937 A CN 110304937A
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parts
powder
silicon carbide
honeycomb filter
ceramic honeycomb
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李军虎
张金龙
田建刚
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Jincheng Fuji New Material Co Ltd
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Jincheng Fuji New Material Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D39/00Filtering material for liquid or gaseous fluids
    • B01D39/14Other self-supporting filtering material ; Other filtering material
    • B01D39/20Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
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Abstract

A kind of ceramic honeycomb filter carrier and preparation method thereof, the present invention relates to ceramic honey comb technical fields;It is made of precursor powder and auxiliary agent, and wherein the weight proportion of precursor powder and auxiliary agent is 85~90:10~15;Wherein, the precursor powder is made of following parts by weight ingredient: silicon carbide coarse powder A40~70 part, 15~30 parts of silicon carbide micro-powder B, 3~5 parts of kaolin, active 3~10 parts of ɑ-alumina powder, 1~5 part of silicon powder, 1~3 part of graphite, 5~15 parts of pore creating material;The auxiliary agent is made of following parts by weight ingredient: 2~8 parts of hydroxypropyl methyl cellulose, 1~4 part of stearate, 2~6 parts of glycerol, 5~15 parts of nano aluminum sol liquid, 25~30 parts of pure water.Using the thermal conductivity of mullite superior thermal stability and silicon carbide, the filtering of vehicle exhaust carbon soot particles can be met and used.

Description

A kind of ceramic honeycomb filter carrier and preparation method thereof
Technical field
The present invention relates to ceramic honey comb technical fields, and in particular to a kind of ceramic honeycomb filter carrier and its preparation side Method.
Background technique
Currently, China's atmosphere pollution is very serious, motor vehicle exhaust emission pollution has accounted for 70% of atmosphere pollution or more.Mesh Before, the country has enforced National V emission standard, some areas VI standard of state of enforcement.Therefore it is required that automobile engine manufacturer is in tail gas Catalytic treatment is carried out to tail gas before discharge.
Ceramic honey comb is a kind of porous functional material, and ceramic honey comb has high specific surface area and good physico Stability is learned, in addition also there is low-density, high permeability, good energy absorption and high temperature resistant, corrosion-resistant, chemical steady The various features such as qualitative and dimensional stability is high, is easy to regenerate.
The material of honeycomb ceramic carrier is prepared in addition to current widely used cordierite, there are also aluminium titanates, silicon carbide, Mullite etc. can satisfy performance although wherein its thermal expansion coefficient of carbofrax material is relatively higher to a certain extent It is required that while also having intensity height, high temperature resistant, corrosion-resistant, wear-resistant, high-specific surface area, height than the series of advantages such as strong.
The prior art prepares silicon carbide ceramic honey comb wall flow particulate filters (DPF) using recrystallized silicon carbide, but Recrystallized silicon carbide preparation is needed using 2450 DEG C of high temperature sinterings of vacuum atmosphere oven, and raw material need high-purity silicon carbide raw material, greatly The price of silicon carbide honeycomb ceramics is increased greatly.Therefore the higher product of cost performance occur be the industry an important technology difficulty Topic.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of structure is simple, design rationally, make With convenient ceramic honeycomb filter carrier and preparation method thereof, the thermally conductive of the superior thermal stability of mullite and silicon carbide is utilized Property, the filtering of vehicle exhaust carbon soot particles can be met and used.
To achieve the above object, ceramic honeycomb filter carrier of the present invention, it is by precursor powder and auxiliary agent group At wherein the weight proportion of precursor powder and auxiliary agent is 85~90:10~15;Wherein, the precursor powder is by as follows Parts by weight ingredient composition: 40~70 parts of silicon carbide coarse powder A, 15~30 parts of silicon carbide micro-powder B, 3~5 parts of kaolin, activity ɑ- 3~10 parts of alumina powder, 1~5 part of silicon powder, 1~3 part of graphite, 5~15 parts of pore creating material;The auxiliary agent is by following weight Part at being grouped as: 2~8 parts of hydroxypropyl methyl cellulose, 1~4 part of stearate, 2~6 parts of glycerol, nano aluminum sol liquid 5~ 15 parts, 25~30 parts of pure water.
Further, the silicon carbide coarse powder A be SIC >=98.5, partial size D50=30~50 μm, FeO content≤ 0.1%.
Further, the silicon carbide micro-powder B be SIC >=98.5, partial size D50=10~14 μm, FeO content≤ 0.1%.
Further, partial size D50=1~2 μm of the active ɑ-alumina powder, Na2O content≤0.1%.
Further, kaolinic partial size D50=1~4 μm.
Further, partial size D50=1~3 μm of the silicon powder, SiO2>=99%.
Further, partial size D50=1~5 μm of the graphite.
Further, the pore creating material is one of organic crylic acid bead, starch, active carbon, partial size D50=30 ~80 μm.
Further, the hydroxypropyl methyl cellulose is 6000mpa.s.
The preparation method of heretofore described ceramic honeycomb filter carrier, operating procedure are as follows:
1, by silicon carbide coarse powder A, silicon carbide micro-powder B, kaolin, active ɑ-alumina powder, silicon powder, graphite, pore-creating Agent carries out sieving processing respectively, then adds hydroxypropyl methyl cellulose and stearate, and mixed at high speed stirring obtains mixture;
2, continue to add glycerol, nano aluminum sol liquid and pure water into said mixture, then mediated, pugging, Aging, last extrusion molding forms blank;
3, above-mentioned blank being subjected to microwave drying, cutting, firing, firing temperature is 1500-1600 DEG C, then is kept the temperature, In insulating process, real time temperature measurement is carried out to each temperature measuring point, is individually adjusted, guarantees that the control of different location temperature is at 0~5 DEG C in furnace Within, soaking time is 4-10 hours, and reducing atmosphere obtains honeycomb ceramic carrier;
4, above-mentioned honeycomb ceramic carrier is subjected to two-sided intersection plug-hole, closes the one face open face of hole in same duct, Multiple honeycomb ceramic carriers are spliced again, a new carrier is constituted, round carrier is machined to peripheral milling, in circle Carrier surface is made skin graft, and carries out double sintering after skin-grafting, and 1200-1300 DEG C of firing temperature.
Further, splicing material used by splicing in the step 4 is consistent with skin-grafting material used by skin-grafting, by Following mass percent is at being grouped as: silicon carbide 80-90%, cellucotton 5-10%%, aluminium oxide 10%, hydroxypropyl methyl fiber Element 2%.
After adopting the above structure, the invention has the following beneficial effects:
1, the present invention is by the research to automotive emission feature, and sold DPF carrier property test in the market, mesh Preceding DPF carrier sold in the market is essentially recrystallized silicon carbide and cordierite, the use of temperature is respectively 1600 DEG C, 1300 DEG C; The present invention is to develop a kind of a kind of new material carrier to fall between using temperature, and material is that silicon carbide compound is not come Shi Zhi can meet the filtering of vehicle exhaust carbon soot particles and use using the thermal conductivity of mullite superior thermal stability and silicon carbide;
2, it is excellent to have that elevated temperature strength is high, thermal shock resistance is good, heating conduction is high, does not shrink under high temperature etc. for the silicon carbide in the present invention Point, the present invention use thickness silicon carbide for aggregate, while wrapping up nano aluminum sol liquid, active oxidation on the surface of silicon carbide Aluminium, kaolin, SILICA FUME promote the activated alumina, the height that are wrapped in silicon carbide using the high temperature active of nanometer Aluminum sol Ridge soil, SILICA FUME, in-situ preparation mullite at high temperature, it is good, thermal shock resistance is good using mullite elevated temperature strength the advantages that, be coated on Between silicon-carbide particle, silicon carbide compound mullite material is formed it into, while adding pore creating material, graphite generation aperture, convenient for crowded Out, to form honeycomb ceramic carrier (DPF);
3, heretofore described ceramic honeycomb filter carrier index is as follows: carborundum content: 85~90%, anti-thermal shock Property: 550 degree, aperture: 8~20 μm, porosity: >=45%, compression strength: >=7MPa, carbon soot particles capture rate: >=95%, make With temperature: 1500 DEG C, refractoriness under load: 1650 DEG C.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art To obtain other drawings based on these drawings.
Fig. 1 is the product index figure of embodiment.
Specific embodiment
The present invention will be further described below with reference to the drawings.
Referring to as shown in Figure 1, present embodiment (embodiment one) the technical solution adopted is that:
1, by 60 parts of silicon carbide coarse powder A, 25 parts of silicon carbide micro-powder B, active 9 parts of ɑ-alumina powder, 5 parts of kaolin, 2 parts of SILICA FUME, 1 part of graphite, 10 parts of pore creating material, 5 parts of hydroxypropyl methyl cellulose, 1 part of stearate, 2 parts of glycerol, 25 parts of pure water Formula weighs each raw material, then by silicon carbide coarse powder A, silicon carbide micro-powder B, active ɑ-alumina powder, kaolin, SILICA FUME, Graphite, the screening of pore creating material raw material, then add hydroxypropyl methyl cellulose, stearate, mixed at high speed obtains mixture;
2, continue to add glycerol, nanometer Aluminum sol, pure water in said mixture, then mediated, is pugging, aging, 40*40mm, 300 mesh, the blank that wall thickness is 0.3mm is made in extrusion molding again;
3, above-mentioned blank is subjected to microwave drying, cutting, firing, firing temperature is 1500 DEG C, is then kept the temperature, is kept the temperature In the process, to each temperature measuring point carry out real time temperature measurement, individually adjust, guarantee furnace in different location temperature control 0~5 DEG C with Interior, soaking time is 4 hours, and reducing atmosphere obtains honeycomb ceramic carrier;
4, the honeycomb ceramic carrier of 40*40mm is subjected to two-sided intersection plug-hole, makes the one face open face of hole in same duct Closing, multiple honeycomb ceramic carriers of 40*40mm are spliced, the carrier of 160*160mm is spliced into, is machined with peripheral milling The round carrier for being 144mm at outer diameter, makes skin graft in circular carrier surface, double sintering, firing temperature is carried out after skin-grafting 1200℃;Wherein, used splicing material is consistent with skin-grafting material, is made of following weight percent composition: silicon carbide 80%, Cellucotton 10%%, aluminium oxide 10%, hydroxypropyl methyl cellulose 2%.
Further, the granularity of the silicon carbide coarse powder A in the step 1 is D50=50 μm, silicon carbide micro-powder B granularity It is D50=11 μm, active ɑ-alumina powder granularity is D50=2 μm, and kaolinite soil granularity is D50=5 μm, and SILICA FUME granularity is D50=1 μm, graphite particle size is D50=5 μm, and pore creating material is acrylic acid bead, and granularity is 50 μm, and hydroxypropyl methyl cellulose is 6000mpa.s。
Further, nano aluminum aerosol particle size is 10nm in the step 2.
Embodiment two
The preparation method of silicon carbide compound mullite ceramic honey comb DPF carrier, includes the following steps: in the present invention
1, by 60 parts of silicon carbide coarse powder A, 30 parts of silicon carbide micro-powder B, active 6 parts of ɑ-alumina powder, kaolin 3.2 Part, 1.5 parts of SILICA FUME, 2 parts of graphite, it is 15 parts of pore creating material, 8 parts of hydroxypropyl methyl cellulose, 3 parts of stearate, 4 parts of glycerol, pure 30 parts of water formulas weigh each raw material, then by silicon carbide coarse powder A, silicon carbide micro-powder B, active ɑ-alumina powder, kaolin, micro- Silicon powder, graphite, the screening of pore creating material raw material, then add hydroxypropyl methyl cellulose, stearate, mixed at high speed must mix Object;
2, continue to add glycerol, nanometer Aluminum sol, pure water in said mixture, then mediated, is pugging, aging, 40*40mm, 300 mesh, the blank that wall thickness is 0.25mm is made in extrusion molding again;
3, above-mentioned blank is subjected to microwave drying, cutting, firing, firing temperature is 1550 DEG C, is then kept the temperature, is kept the temperature In the process, to each temperature measuring point carry out real time temperature measurement, individually adjust, guarantee furnace in different location temperature control 0~5 DEG C with Interior, soaking time is 8 hours, and reducing atmosphere obtains honeycomb ceramic carrier;
4, the honeycomb ceramic carrier of 40*40mm is subjected to two-sided intersection plug-hole, makes the one face open face of hole in same duct Closing, multiple honeycomb ceramic carriers of 40*40mm are spliced, the carrier of 320*320mm is spliced into, is machined with peripheral milling The round carrier for being 305mm at outer diameter, makes skin graft in circular carrier surface, double sintering, firing temperature is carried out after skin-grafting 1300℃;Wherein, used splicing material is consistent with skin-grafting material, is made of following weight percent composition: silicon carbide 85%, Cellucotton 5%%, aluminium oxide 10%, hydroxypropyl methyl cellulose 2%.
Further, the granularity of the silicon carbide coarse powder A in the step 1 is D50=40 μm, silicon carbide micro-powder B granularity It is D50=14 μm, active ɑ-alumina powder granularity is D50=2 μm, and kaolinite soil granularity is D50=3 μm, and SILICA FUME granularity is D50=2 μm, graphite particle size is D50=3 μm, and pore creating material is active carbon particle, and granularity is 70 μm, and hydroxypropyl methyl cellulose is 6000mpa.s。
Further, nano aluminum aerosol particle size is 15nm in the step 2.
The above is only used to illustrate the technical scheme of the present invention and not to limit it, and those of ordinary skill in the art are to this hair The other modifications or equivalent replacement that bright technical solution is made, as long as it does not depart from the spirit and scope of the technical scheme of the present invention, It is intended to be within the scope of the claims of the invention.

Claims (10)

1. a kind of ceramic honeycomb filter carrier, it is characterised in that: it is made of precursor powder and auxiliary agent, wherein precursor The weight proportion of end and auxiliary agent is 85~90:10~15;Wherein, the precursor powder is made of following parts by weight ingredient: Silicon carbide coarse powder A40~70 part, silicon carbide micro-powder B15~30 part, 3~5 parts of kaolin, active 3~10 parts of ɑ-alumina powder, 1~5 part of silicon powder, 1~3 part of graphite, 5~15 parts of pore creating material;The auxiliary agent is made of following parts by weight ingredient: hydroxypropyl first 2~8 parts of base cellulose, 1~4 part of stearate, 2~6 parts of glycerol, 5~15 parts of nano aluminum sol liquid, 25~30 parts of pure water.
2. a kind of ceramic honeycomb filter carrier according to claim 1, it is characterised in that: the silicon carbide coarse powder A For SIC >=98.5, partial size D50=30~50 μm, FeO content≤0.1%.
3. a kind of ceramic honeycomb filter carrier according to claim 1, it is characterised in that: the silicon carbide micro-powder B For SIC >=98.5, partial size D50=10~14 μm, FeO content≤0.1%.
4. a kind of ceramic honeycomb filter carrier according to claim 1, it is characterised in that: the active ɑ-aluminium oxide Partial size D50=1~2 μm of micro mist, Na2O content≤0.1%.
5. a kind of ceramic honeycomb filter carrier according to claim 1, it is characterised in that: the kaolinic partial size D50=1~4 μm.
6. a kind of ceramic honeycomb filter carrier according to claim 1, it is characterised in that: the partial size of the silicon powder D50=1~3 μm, SiO2>=99%.
7. a kind of ceramic honeycomb filter carrier according to claim 1, it is characterised in that: the partial size of the graphite D50=1~5 μm.
8. a kind of ceramic honeycomb filter carrier according to claim 1, it is characterised in that: the pore creating material is organic One of acrylic acid bead, starch, active carbon, partial size D50=30~80 μm.
9. a kind of preparation method of ceramic honeycomb filter carrier, it is characterised in that: its operating procedure is as follows:
(1), by silicon carbide coarse powder A, silicon carbide micro-powder B, kaolin, active ɑ-alumina powder, silicon powder, graphite, pore creating material Sieving processing is carried out respectively, then adds hydroxypropyl methyl cellulose and stearate, and mixed at high speed stirring obtains mixture;
(2), continue to add glycerol, nano aluminum sol liquid and pure water into said mixture, then mediated, is pugging, old Corruption, last extrusion molding form blank;
(3), above-mentioned blank is subjected to microwave drying, cutting, firing, firing temperature is 1500-1600 DEG C, then is kept the temperature, and is protected During temperature, to each temperature measuring point carry out real time temperature measurement, individually adjust, guarantee furnace in different location temperature control 0~5 DEG C with Interior, soaking time is 4-10 hours, and reducing atmosphere obtains honeycomb ceramic carrier;
(4), above-mentioned honeycomb ceramic carrier is subjected to two-sided intersection plug-hole, closes the one face open face of hole in same duct, then Multiple honeycomb ceramic carriers are spliced, a new carrier is constituted, is machined to round carrier with peripheral milling, are carried in circle Body surface face is made skin graft, and carries out double sintering after skin-grafting, and 1200-1300 DEG C of firing temperature.
10. a kind of preparation method of ceramic honeycomb filter carrier according to claim 9, it is characterised in that: described Splicing material used by splicing in step (4) is consistent with skin-grafting material used by skin-grafting, by following mass percent at grouping At: silicon carbide 80-90%, cellucotton 5-10%%, aluminium oxide 10%, hydroxypropyl methyl cellulose 2%.
CN201910701890.1A 2019-07-31 2019-07-31 A kind of ceramic honeycomb filter carrier and preparation method thereof Pending CN110304937A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111299547A (en) * 2020-03-18 2020-06-19 安徽华德电力技术工程有限公司 High-temperature-resistant composite material and preparation method and application thereof
CN114524675A (en) * 2022-02-22 2022-05-24 山东奥福环保科技股份有限公司 Silicon-bonded silicon carbide diesel particulate filter and preparation method thereof
CN115536427A (en) * 2022-10-21 2022-12-30 昆明理工大学 Porous ceramic material for silicon carbide-based solid-liquid-gas separation and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111299547A (en) * 2020-03-18 2020-06-19 安徽华德电力技术工程有限公司 High-temperature-resistant composite material and preparation method and application thereof
CN114524675A (en) * 2022-02-22 2022-05-24 山东奥福环保科技股份有限公司 Silicon-bonded silicon carbide diesel particulate filter and preparation method thereof
CN115536427A (en) * 2022-10-21 2022-12-30 昆明理工大学 Porous ceramic material for silicon carbide-based solid-liquid-gas separation and preparation method thereof

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