CN108675826A - A kind of cordierite wall-flow honeycomb ceramic filter and preparation method thereof - Google Patents
A kind of cordierite wall-flow honeycomb ceramic filter and preparation method thereof Download PDFInfo
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- CN108675826A CN108675826A CN201810714435.0A CN201810714435A CN108675826A CN 108675826 A CN108675826 A CN 108675826A CN 201810714435 A CN201810714435 A CN 201810714435A CN 108675826 A CN108675826 A CN 108675826A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
- C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
- C04B35/195—Alkaline earth aluminosilicates, e.g. cordierite or anorthite
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- C04B38/0006—Honeycomb structures
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- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
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Abstract
The present invention provides a kind of cordierite wall-flow honeycomb ceramic filters and preparation method thereof.The cordierite wall-flow honeycomb ceramic filter of the present invention, by weight, including following component:100 parts of cordierite base raw material, 2~8 parts of organic resin microcapsules, 2~8 parts of graphite powder.The cordierite wall-flow honeycomb ceramic filter of the present invention has the characteristics that intensity is high, the porosity is high, coefficient of thermal expansion is low and aperture is adjustable, can be used for the trapping to automotive diesel carbon soot particles under varying environment;The stable preparation process of inventive cordierite matter wall-flow honeycomb ceramic filter is reliable, and easily controllable, the prices of raw materials are cheap, it is easy to accomplish.
Description
Technical field
The invention belongs to tail gas clean-up technical field, it is related to a kind of cordierite wall-flow honeycomb ceramic filter and its system
Preparation Method.
Background technology
Diesel engine obtains more and more in recent years due to having many advantages, such as that the thermal efficiency is high, fuel economy is good, service life is long
It is widely applied.But diesel engine can discharge a large amount of particle (PM) in use, they can for a long time suspend in the air, sternly
Heavily contaminated environment influences the health of the mankind.Therefore, world many countries have successively formulated the method for limitation small particle emission of diesel car
Rule, and emission limit is lower and lower.
Micro particle catching technology is to realize that diesel particulate emission controls one of maximally efficient and simple technology, wherein wall
Streaming honeycomb ceramic filter body is current most common grain catcher (abbreviation DPF), and principle is the duct using filter
Replace blocking technology before and after import and adjacent outlets, exhaust is made to be passed through from wall surface and achieve the purpose that filter particle.Currently, violet is green
Stone has the characteristics that raw material extensively and cheap and technical equipment requires the low making material for being widely used as DPF, comprehensive performance
Excellent cordierite DPF is always the project of domestic each enterprise and the research of ceramic honey comb R&D institution.
CN101612499A discloses a kind of preparation method of wall-flow honeycomb ceramic filter, using cordierite honeycomb
Ceramic material is combined with carbon particle or the special pore creating material of organic resin particles, the ingredient of honeycomb ceramic filter body blank stock,
Mass parts and grain size are as follows:Kaolin (Al2O3·2SiO2·2H2O) 35~45 parts, average grain diameter≤5 μm;Talcum (3MgO
4SiO2·H2O) 20~30 parts, average grain diameter be 15 μm;4~9 parts of Alpha-alumina, average grain diameter≤2 μm;Carbon particle or/with have
Totally 5~15 parts of the pore creating material of machine polymeric particles composition, average grain diameter are 10~20 μm;3~7 parts of binder;By mentioned component
It is uniformly mixed with blank with 20~30 parts of warps of water;Blank is after 0.09MPa or less vacuum outgas white silk is made 2~3 times in vacuum degree
It completes to change to plastic mud material, be squeezed out by the mold of extruder after the aging 24 ± 8h of plastic mud material, mold hole density is 100~
250 holes/square inch;Pug cuts into the wet green body of certain length after squeezing out, dry body body is obtained after microwave drying, then to dry
Green body intersects plug-hole, drying, skin-grafting and deburring, and product most is made through firing process afterwards.Wall-flow honeycomb made from the invention is made pottery
Porcelain filtering body product porosity is 50%~52%, and micropore average pore size is 8~13 μm, but its coefficient of thermal expansion is higher, is resisted
Compressive Strength is relatively low.
CN105833620A discloses half general formula ceramic honey comb particulate filter of one kind and preparation method thereof, and raw material is with matter
The group of amount part becomes:Schistose kaolinite 25~30, alumina powder 15~20, foliated talc 37~40, fused quartz powder 6~10,
Pore creating material 8~20, water-soluble binder 3~10 and suitable water;Its preparation process:By the abundant mechanical mixture of raw material, kneading, make
It is uniform;Mixture aging 20~40h after being made 2~3 times by vacuum white silk under vacuum degree is 90~95KPa, obtains plasticity mud
Material;It squeezes out to obtain the honeycomb ceramic blank of certain specification by mold;It is modified by 8~12Kw microwave dryings 2h, cutting
To dry body body;By being fired into semi-finished product under temperature programming high temperature;The irregular outer wall of green body is by mechanically pulling off again to lay equal stress on
Finished product is obtained after new skin-grafting, microwave drying, single-ended transpostion interval plug-hole, microwave drying.Pore creating material used in the invention is day
Right fiber or polyvinyl chloride or polyvinyl alcohol or methyl methacrylate or starch etc..Half general formula honeycomb made from the invention
Ceramic particle object filter main performance index is:Porosity is 40%~65%, and micropore average pore size is 8~20 μm, resistance to compression
Intensity is more than 18MPa, and coefficient of thermal expansion is less than 1.0 × 10-6/ DEG C, still, the firing process of the invention is more difficult to control, therefore into
Row large-scale production has larger difficulty.
CN105294145A discloses a kind of use for diesel engine wall flow particulate trap ceramic filtering body preparation method, carries
The ceramic filtering body of waveform air intake passage, this method is first with the stone for inside selective laser sintering and moulding including skeleton
Then black mold in aqueous-based ceramic slurry cast to graphite jig, will wait for that ceramic slurry curing is molded, obtain ceramic body, warp
Freeze-drying, ablation graphite jig, high temperature sintering processing are crossed, wall flow particulate trap ceramic filtering body is finally obtained.But this
Method complex manufacturing technology, in actual production with larger difficulty.
Invention content
In view of the deficiencies of the prior art, one of the objects of the present invention is to provide a kind of cordierite honeycomb ceramic filters
Filtering body has the characteristics that intensity is high, the porosity is high, coefficient of thermal expansion is low and aperture is adjustable.
For this purpose, the present invention uses following technical scheme:
A kind of cordierite wall-flow honeycomb ceramic filter, by weight, including following component:
100 parts of cordierite base raw material, 2~8 parts of organic resin microcapsules, 2~8 parts of graphite powder.
The present invention is original using the compound pore creating material that obtains of organic resin microcapsules and graphite powder using cordierite as primary raw material
Material prepares cordierite wall-flow honeycomb ceramic filter.The pore creating material of the present invention is Organic-inorganic composite pore creating material, and this
Organic material described in invention is organic resin microcapsules, and inorganic material is graphite powder.Wherein, organic resin microcapsules are being burnt
At will produce heat in the process, additive amount, which crosses conference, makes filtering body be cracked because of thermal stress, and organic resin microcapsules
For hollow structure, with different degrees of scuffing and destruction are had in aggregate raw particles mixed process, cause under pore-creating effect
Drop is unable to get the porosity corresponding with its additive amount institute and aperture.Therefore, single to obtain height from a small amount of addition microcapsules
The purpose of pore-creating effect is difficult to realize;Graphite powder is as inorganic pore creating material, and ignition temperature is different from organic microcapsules, therefore two
Person will not generate amount of heat in same temperature range in sintering process and filtering body is caused to crack;The two acts synergistically, can
Keep pore creating material good fluidity intensity obtained high, pore-creating is uniform, and pore-size distribution is reasonable, and pore-creating effect is good, available to be added with it
The matched porosity of amount institute and aperture.
Pore creating material made from ratio of the present invention by both Reasonable Regulation And Control organic resin microcapsules and graphite powder can get
The cordierite wall-flow honeycomb ceramic filter of different porosities and aperture.It is with the cordierite base parts by weight of raw materials
The parts by weight of 100 parts of meters, the organic resin microcapsules are 2~8 parts, such as the parts by weight of the organic resin microcapsules are 2
Part, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, the parts by weight of the graphite powder are 2~8 parts, for example, the graphite powder parts by weight
It is 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts.
Organic resin microcapsules of the present invention refer to the hollow-particle that organic resin is constituted, and formation mechenism is as follows:
Using thermoplastic resin as shell, the microballon of liquid low-boiling compound is included, after heating, shell softening, liquid carbon therein
Hydrogen compound becomes gas, and capsule body is expanded because of the pressure of generation.From volume, original 50~100 times can be expanded as,
Therefore also referred to as thermal expansivity microcapsules.The shell of microcapsules is mostly used AN analog copolymers at present.
To ensure that filtering body has high porosity and suitable pore-size distribution, the average grain diameter of the organic resin microcapsules
Be 20~80 μm, for example, the organic resin microcapsules average grain diameter be 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80
μm.The graphite powder is the spheroidal particle that circularity is 0.8~1, for example, the graphite powder be circularity be 0.8,0.85,0.9,
0.95、1.Preferably, the average grain diameter of the graphite powder be 20~60 μm, such as the graphite powder average grain diameter be 20 μm,
30μm、40μm、50μm、60μm。
Heretofore described " circularity " expression is when planar observation raw particles, extent of deviation of the shape from positive round
Index, refer to using flow-type particle image analysis device, after the projected area S and the perimeter L that measure raw particles, be based on down
State the calculated circularity SD of formula (1).The index is, positive round is indicated when circularity is 1, be worth it is smaller illustrate it is inclined from positive round
Difference is bigger.
SD=4 π S/L2 (1)
In formula, SD is circularity;S is projected area;L is perimeter.
Cordierite is a kind of silicate mineral, and chemical composition is the silicate rich in iron, magnesium, aluminium, and the magnesium in ingredient can quilt
Iron or manganese are replaced, and partial aluminium can also be replaced by iron, and usually there is light blue or lilac, glassy lustre to be clear to half
It is transparent.Cordierite also has there are one feature, has apparent pleochroism (trichroism), sends out different colours in a different direction
Light.The cordierite of the excellent color U.S. of product is taken as jewel, and in addition to this, cordierite is existing since fire resistance is good, expanded by heating rate is low
Generally using as the honeycomb support material of vehicle purifier.
In the present invention, a kind of cordierite wall-flow honeycomb ceramic filter, including cordierite base raw material, and with institute
It is 100 parts of meters to state cordierite base parts by weight of raw materials,
4~16 parts of pore creating material, for example, pore creating material parts by weight be 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts,
12 parts, 13 parts, 14 parts, 15 parts, 16 parts.
3~8 parts of methylcellulose, such as the parts by weight of methylcellulose are 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts.
3~8 parts of glycerine, such as the parts by weight of glycerine are 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts.
25~35 parts of water, for example, water parts by weight be 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33
Part, 34 parts, 35 parts.
Wherein, by weight, the cordierite base raw material includes following components:
Preferably, by weight, the cordierite base raw material includes following components:
20~30 parts of talcum, for example, talcum parts by weight be 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27
Part, 28 parts, 29 parts, 30 parts.
30~45 parts of kaolin, for example, kaolinic parts by weight be 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, 36
Part, 37 parts, 38 parts, 39 parts, 40 parts, 41 parts, 42 parts, 43 parts, 44 parts, 45 parts.
15~35 parts of aluminium oxide, for example, aluminium oxide parts by weight be 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, 21
Part, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts.
5~10 parts of silicon powder, such as the parts by weight of silicon powder are 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts.
The second object of the present invention is to provide a kind of preparation method of cordierite wall-flow honeycomb ceramic filter, this
The manufacturing process of invention is simple, easily controllable, and the prices of raw materials are cheap, it is easy to accomplish, the preparation method includes the following steps:
It is in terms of 100 parts by the cordierite base parts by weight of raw materials, it is original to take 2~8 parts of organic resin microcapsules and 2~8 parts of graphite powders
The cordierite wall-flow honeycomb ceramic filter is prepared after mixing, pore-creating in material.
Preferably, a kind of preparation method of cordierite wall-flow honeycomb ceramic filter, includes the following steps:
1) by weight, by 100 parts of cordierite base raw material, 2~8 parts of organic resin microcapsules, 2~8 parts
Graphite powder and the mixing of 3~8 parts of methylcellulose, obtain powder mixture;
2) 3~8 parts of glycerine and 25~35 parts of water by weight, are added to the powder mixture that step 1) obtains
It mediates, obtains pug;
3) pug for obtaining step 2) through be kneaded, it is aging after, obtain plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake that step 3) obtains is formed into cellular moulded pottery not yet put in a kiln to bake, dryness finalization under the guiding of mold through squeezing;
It 5) will be through the cellular moulded pottery not yet put in a kiln to bake sealing of hole after step 4) dryness finalization;
6) the cordierite wall-flow honeycomb will be obtained through the moulded pottery not yet put in a kiln to bake high temperature sintering after step 5) sealing pores, cooling
Ceramic filtering body.
In step 1), the mixing carries out in batch mixer, and the time of the mixing is 40~80min, such as institute
The time for stating mixing is 40min, 50min, 60min, 70min, 80min.
In step 2), time of the kneading is 40~80min, for example, the kneading time be 40min, 50min,
60min、70min、80min。
Preferably, in step 2), the temperature of the kneading is 30 DEG C or less.
Preferably, in step 3), the mixing carries out in vacuum kneading machine, and the number of the mixing is 2~3
Secondary, the vacuum degree of the vacuum kneading machine is 0.09MPa or less.
Preferably, in step 3), the aging time be 20~25h, such as the aging time be 20h, 21h,
22h、23h、24h、25h。
In step 6), the detailed process of the high temperature sintering is:Cellular moulded pottery not yet put in a kiln to bake after step 5) dryness finalization is put
Enter in high temperature sintering furnace, when being heated to 1400~1450 DEG C with 5 DEG C/min of heating rate, and keep the temperature 6~10h, such as keeping the temperature
Between be 6h, 7h, 8h, 9h, 10h.
As the preferred embodiment of the present invention, the preparation method of the cordierite wall-flow honeycomb ceramic filter includes such as
Lower step:
1) by weight, by 100 parts of cordierite base raw material, 2~8 parts of organic resin microcapsules, 2~8 parts
Graphite powder and 3~8 parts of methylcellulose, which are added in batch mixer, mixes 40~80min, obtains powder mixture;
2) 3~8 parts of glycerine and 25~35 parts of water by weight, are added to the powder mixture that step 1) obtains
It mediates, the temperature for controlling kneading is 30 DEG C hereinafter, obtaining pug;
3) pug for obtaining step 2) is kneaded 2~3 times in vacuum degree is 0.09MPa vacuum kneading machines below, old
After 20~25h of corruption, plasticity moulded pottery not yet put in a kiln to bake is obtained;
4) the plasticity moulded pottery not yet put in a kiln to bake that step 3) obtains is put into extruder, cellular mud is formed through squeezing under the guiding of mold
Base, wherein mold hole density is 200~400 holes/square inch;Pug cuts into wet green body after squeezing out, and is put into microwave drying oven
Interior dryness finalization;
5) will through the cellular moulded pottery not yet put in a kiln to bake after step 4) dryness finalization after ends cutting is smooth transpostion interval plug-hole, after dry
Carry out deburring and skin-grafting;
6) moulded pottery not yet put in a kiln to bake after step 5) sealing pores is put into high temperature sintering furnace, is heated with 5 DEG C/min of heating rate
It to 1400~1450 DEG C, and keeps the temperature 6~10h and carries out high temperature sintering, naturally cool to 100 DEG C, obtain the cordierite wall stream
Formula honeycomb ceramic filter body.
Compared with prior art, beneficial effects of the present invention are:
(1) cordierite wall-flow honeycomb ceramic filter of the invention, have good mechanical strength, high temperature resistant, it is anticorrosive,
The feature that the porosity is high, micropore is uniform and distribution is good, aperture is adjustable, wherein cordierite honeycomb ceramic filter obtained
The filtering body porosity is 49~60%, and average pore size is 12~17.5 μm, and the ginseng of organic resin microcapsules and graphite powder is adjusted
Number carrys out the size of adjustment aperture;The intensity of cordierite wall-flow honeycomb ceramic filter is high, wherein and A axis compression strength is 4~
9.8MPa, B axle compression strength are 2~5.2MPa, and C axis compression strength is 0.25~0.5MPa;Meanwhile cordierite wall-flow type bee
Nest ceramic filter isolator CTE is low, and coefficient of thermal expansion is 0.658 × 10-6~0.957 × 10-6/℃。
(2) arresting efficiency of cordierite wall-flow honeycomb ceramic filter of the invention is high, and arresting efficiency reaches 85%
More than;Thermal shock resistance is good, and product does not crack room temperature~550 DEG C cycle three times.
(3) manufacturing process of cordierite wall-flow honeycomb ceramic filter of the invention is simple, easily controllable, raw material
It is cheap, it is easy to accomplish, it can be used for the trapping to automotive diesel carbon soot particles under varying environment, conducive to promoting and answering
With.
Specific implementation mode
The technical solution further illustrated the present invention below by specific implementation mode.
Unless specific instructions, various raw materials of the invention are commercially available buys, or is prepared according to the conventional method of this field
It obtains.
Embodiment 1
A kind of cordierite wall-flow honeycomb ceramic filter provided by the invention, cordierite base raw material group become:
It is in terms of 100 parts by above-mentioned basic material parts by weight, pore creating material group becomes:
20 μm 8 parts of organic resin microcapsules average grain diameter
40 μm of graphite powder average grain diameter, 0.8 2 parts of circularity
The present embodiment separately adds 6 parts of methylcellulose, 6 parts of glycerine, 30 parts of water.
The preparation method of the above-mentioned cordierite wall-flow honeycomb ceramic filter of the present embodiment, includes the following steps:
1) powders such as talcum, kaolin, aluminium oxide, silicon powder, pore creating material, methylcellulose original is weighed by above-mentioned formula
Material, is added to batch mixer mixing 60min;
2) glycerine and water are added to kneading 60min in powder mixture and obtain uniform pug, kneading process will control mud
Material temperature degree is at 30 DEG C or less;
3) above-mentioned pug is put into vacuum deairing machine and is kneaded 2 times (vacuum degree 0.09MPa or less), it is then aging to be formed for 24 hours
Plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake is put into extruder, forms cellular moulded pottery not yet put in a kiln to bake under the guiding of mold, mold hole density is
300 holes/square inch;Pug cuts into the wet green body of certain altitude after squeezing out, be put into drying and shaping in microwave drying oven;
5) by the smooth rear transpostion interval plug-hole of dry green body end face cutting, deburring and skin-grafting are carried out after dry;
6) above-mentioned filtering body moulded pottery not yet put in a kiln to bake is put into high temperature sintering furnace, 1410 DEG C is heated to 5 DEG C/min of heating rate,
And 8 hours are kept the temperature, it then naturally cools to 100 DEG C and cordierite wall-flow honeycomb ceramic filter is prepared.
The performance indicator of the cordierite wall-flow honeycomb ceramic filter of the present embodiment is as follows:The porosity 59.5% is put down
Equal 17.5 μm of aperture, A axis compression strength 4MPa, B axle compression strength 2.5MPa, C axis compression strength 0.25MPa, coefficient of thermal expansion
0.957×10-6/℃。
Embodiment 2
A kind of cordierite wall-flow honeycomb ceramic filter provided by the invention, cordierite base raw material group become:
It is in terms of 100 parts by above-mentioned basic material parts by weight, pore creating material group becomes:
40 μm 6 parts of organic resin microcapsules average grain diameter
30 μm of graphite powder average grain diameter, 0.9 2 parts of circularity
The present embodiment separately adds 6 parts of methylcellulose, 6 parts of glycerine, 30 parts of water.
The preparation method of the above-mentioned cordierite wall-flow honeycomb ceramic filter of the present embodiment, includes the following steps:
1) powders such as talcum, kaolin, aluminium oxide, silicon powder, pore creating material, methylcellulose original is weighed by above-mentioned formula
Material, is added to batch mixer mixing 60min;
2) glycerine and water are added to kneading 60min in powder mixture and obtain uniform pug, kneading process will control mud
Material temperature degree is at 30 DEG C or less;
3) above-mentioned pug is put into vacuum deairing machine and is kneaded 2 times (vacuum degree 0.09MPa or less), it is then aging to be formed for 24 hours
Plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake is put into extruder, forms cellular moulded pottery not yet put in a kiln to bake under the guiding of mold, mold hole density is
300 holes/square inch;Pug cuts into the wet green body of certain altitude after squeezing out, be put into drying and shaping in microwave drying oven;
5) by the smooth rear transpostion interval plug-hole of dry green body end face cutting, deburring and skin-grafting are carried out after dry;
6) above-mentioned filtering body moulded pottery not yet put in a kiln to bake is put into high temperature sintering furnace, 1410 DEG C is heated to 5 DEG C/min of heating rate,
And 8 hours are kept the temperature, it then naturally cools to 100 DEG C and is prepared into cordierite wall-flow honeycomb ceramic filter.
The performance indicator of the present embodiment cordierite wall-flow honeycomb ceramic filter is as follows:The porosity 56.8% is averaged
16.8 μm of aperture, A axis compression strength 5.6MPa, B axle compression strength 3MPa, C axis compression strength 0.3MPa, coefficient of thermal expansion
0.859×10-6/℃。
Embodiment 3
A kind of cordierite wall-flow honeycomb ceramic filter provided by the invention, cordierite base raw material group become:
It is in terms of 100 parts by above-mentioned basic material parts by weight, pore creating material group becomes:
60 μm 4 parts of organic resin microcapsules average grain diameter
20 μm of graphite powder average grain diameter, 13 parts of circularity
The present embodiment separately adds 6 parts of methylcellulose, 6 parts of glycerine, 30 parts of water.
The preparation method of the above-mentioned cordierite wall-flow honeycomb ceramic filter of the present embodiment, includes the following steps:
1) powders such as talcum, kaolin, aluminium oxide, silicon powder, pore creating material, methylcellulose original is weighed by above-mentioned formula
Material, is added to batch mixer mixing 60min;
2) glycerine and water are added to kneading 60min in powder mixture and obtain uniform pug, kneading process will control mud
Material temperature degree is at 30 DEG C or less;
3) above-mentioned pug is put into vacuum deairing machine and is kneaded 2 times (vacuum degree 0.09MPa or less), it is then aging to be formed for 24 hours
Plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake is put into extruder, forms cellular moulded pottery not yet put in a kiln to bake under the guiding of mold, mold hole density is
300 holes/square inch;Pug cuts into the wet green body of certain altitude after squeezing out, be put into drying and shaping in microwave drying oven;
5) by the smooth rear transpostion interval plug-hole of dry green body end face cutting, deburring and skin-grafting are carried out after dry;
6) above-mentioned filtering body moulded pottery not yet put in a kiln to bake is put into high temperature sintering furnace, 1410 DEG C is heated to 5 DEG C/min of heating rate,
And 8 hours are kept the temperature, it then naturally cools to 100 DEG C and is prepared into cordierite wall-flow honeycomb ceramic filter.
The performance indicator of the present embodiment cordierite wall-flow honeycomb ceramic filter is as follows:The porosity 54.3% is averaged
14.5 μm of aperture, A axis compression strength 6.5MPa, B axle compression strength 3.5MPa, C axis compression strength 0.35MPa, coefficient of thermal expansion
0.745×10-6/℃。
Embodiment 4
A kind of cordierite wall-flow honeycomb ceramic filter provided by the invention, cordierite base raw material group become:
It is in terms of 100 parts by above-mentioned basic material parts by weight, pore creating material group becomes:
80 μm 2 parts of organic resin microcapsules average grain diameter
60 μm of graphite powder average grain diameter, 0.8 4 parts of circularity
The present embodiment separately adds 6 parts of methylcellulose, 6 parts of glycerine, 30 parts of water.
The preparation method of the above-mentioned cordierite wall-flow honeycomb ceramic filter of the present embodiment, includes the following steps:
1) powders such as talcum, kaolin, aluminium oxide, silicon powder, pore creating material, methylcellulose original is weighed by above-mentioned formula
Material, is added to batch mixer mixing 60min;
2) glycerine and water are added to kneading 60min in powder mixture and obtain uniform pug, kneading process will control mud
Material temperature degree is at 30 DEG C or less;
3) above-mentioned pug is put into vacuum deairing machine and is kneaded 2 times (vacuum degree 0.09MPa or less), it is then aging to be formed for 24 hours
Plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake is put into extruder, forms cellular moulded pottery not yet put in a kiln to bake under the guiding of mold, mold hole density is
300 holes/square inch;Pug cuts into the wet green body of certain altitude after squeezing out, be put into drying and shaping in microwave drying oven;
5) by the smooth rear transpostion interval plug-hole of dry green body end face cutting, deburring and skin-grafting are carried out after dry;
6) above-mentioned filtering body moulded pottery not yet put in a kiln to bake is put into high temperature sintering furnace, 1410 DEG C is heated to 5 DEG C/min of heating rate,
And 8 hours are kept the temperature, it then naturally cools to 100 DEG C and is prepared into cordierite wall-flow honeycomb ceramic filter.
The performance indicator of the present embodiment cordierite wall-flow honeycomb ceramic filter is as follows:The porosity 52.5% is averaged
13.4 μm of aperture, A axis compression strength 7.2MPa, B axle compression strength 4.1MPa, C axis compression strength 0.4MPa, coefficient of thermal expansion
0.658×10-6/℃。
Embodiment 5
A kind of cordierite wall-flow honeycomb ceramic filter provided by the invention, cordierite base raw material group become:
It is in terms of 100 parts by above-mentioned basic material parts by weight, pore creating material group becomes:
60 μm 2 parts of organic resin microcapsules average grain diameter
40 μm of graphite powder average grain diameter, 0.9 2 parts of circularity
The present embodiment separately adds 6 parts of methylcellulose, 6 parts of glycerine, 30 parts of water.
The preparation method of the above-mentioned cordierite wall-flow honeycomb ceramic filter of the present embodiment, includes the following steps:
1) powders such as talcum, kaolin, aluminium oxide, silicon powder, pore creating material, methylcellulose original is weighed by above-mentioned formula
Material, is added to batch mixer mixing 60min;
2) glycerine and water are added to kneading 60min in powder mixture and obtain uniform pug, kneading process will control mud
Material temperature degree is at 30 DEG C or less;
3) above-mentioned pug is put into vacuum deairing machine and is kneaded 2 times (vacuum degree 0.09MPa or less), it is then aging to be formed for 24 hours
Plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake is put into extruder, forms cellular moulded pottery not yet put in a kiln to bake under the guiding of mold, mold hole density is
300 holes/square inch;Pug cuts into the wet green body of certain altitude after squeezing out, be put into drying and shaping in microwave drying oven;
5) by the smooth rear transpostion interval plug-hole of dry green body end face cutting, deburring and skin-grafting are carried out after dry;
6) above-mentioned filtering body moulded pottery not yet put in a kiln to bake is put into high temperature sintering furnace, 1410 DEG C is heated to 5 DEG C/min of heating rate,
And 8 hours are kept the temperature, it then naturally cools to 100 DEG C and is prepared into cordierite wall-flow honeycomb ceramic filter.
The performance indicator of the present embodiment cordierite wall-flow honeycomb ceramic filter is as follows:The porosity 49.8% is averaged
12.7 μm of aperture, A axis compression strength 9.8MPa, B axle compression strength 5.2MPa, C axis compression strength 0.5MPa, coefficient of thermal expansion
0.721×10-6/℃。
Comparative example 1
A kind of cordierite wall-flow honeycomb ceramic filter that the comparative example provides, cordierite base raw material group become:
It is in terms of 100 parts by above-mentioned basic material parts by weight, pore creating material group becomes:
60 μm 10 parts of organic resin microcapsules average grain diameter
This comparative example separately adds 6 parts of methylcellulose, 6 parts of glycerine, 30 parts of water.
The preparation method of the above-mentioned cordierite wall-flow honeycomb ceramic filter of this comparative example, includes the following steps:
1) powders such as talcum, kaolin, aluminium oxide, silicon powder, pore creating material, methylcellulose original is weighed by above-mentioned formula
Material, is added to batch mixer mixing 60min;
2) glycerine and water are added to kneading 60min in powder mixture and obtain uniform pug, kneading process will control mud
Material temperature degree is at 30 DEG C or less;
3) above-mentioned pug is put into vacuum deairing machine and is kneaded 2 times (vacuum degree 0.09MPa or less), it is then aging to be formed for 24 hours
Plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake is put into extruder, forms cellular moulded pottery not yet put in a kiln to bake under the guiding of mold, mold hole density is
300 holes/square inch;Pug cuts into the wet green body of certain altitude after squeezing out, be put into drying and shaping in microwave drying oven;
5) by the smooth rear transpostion interval plug-hole of dry green body end face cutting, deburring and skin-grafting are carried out after dry;
6) above-mentioned filtering body moulded pottery not yet put in a kiln to bake is put into high temperature sintering furnace, 1410 DEG C is heated to 5 DEG C/min of heating rate,
And 8 hours are kept the temperature, it then naturally cools to 100 DEG C and is prepared into cordierite wall-flow honeycomb ceramic filter.
The performance indicator of this comparative example cordierite wall-flow honeycomb ceramic filter is as follows:The porosity 61.5% is averaged
9.8 μm of aperture, A axis compression strength 3.5MPa, B axle compression strength 1.6MPa, C axis compression strength 0.15MPa, coefficient of thermal expansion
1.56×10-6/ DEG C, sintering qualified rate is low, and 40% product is cracking.
Comparative example 2
A kind of cordierite wall-flow honeycomb ceramic filter that this comparative example provides, cordierite base raw material group become:
It is in terms of 100 parts by above-mentioned basic material parts by weight, pore creating material group becomes:
60 μm of graphite powder average grain diameter, 0.9 10 parts of circularity
This comparative example separately adds 6 parts of methylcellulose, 6 parts of glycerine, 30 parts of water.
The preparation method of the above-mentioned cordierite wall-flow honeycomb ceramic filter of this comparative example, includes the following steps:
1) powders such as talcum, kaolin, aluminium oxide, silicon powder, pore creating material, methylcellulose original is weighed by above-mentioned formula
Material, is added to batch mixer mixing 60min;
2) glycerine and water are added to kneading 60min in powder mixture and obtain uniform pug, kneading process will control mud
Material temperature degree is at 30 DEG C or less;
3) above-mentioned pug is put into vacuum deairing machine and is kneaded 2 times (vacuum degree 0.09MPa or less), it is then aging to be formed for 24 hours
Plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake is put into extruder, forms cellular moulded pottery not yet put in a kiln to bake under the guiding of mold, mold hole density is
300 holes/square inch;Pug cuts into the wet green body of certain altitude after squeezing out, be put into drying and shaping in microwave drying oven;
5) by the smooth rear transpostion interval plug-hole of dry green body end face cutting, deburring and skin-grafting are carried out after dry;
6) above-mentioned filtering body moulded pottery not yet put in a kiln to bake is put into high temperature sintering furnace, 1410 DEG C is heated to 5 DEG C/min of heating rate,
And 8 hours are kept the temperature, it then naturally cools to 100 DEG C and is prepared into cordierite wall-flow honeycomb ceramic filter.
The performance indicator of this comparative example cordierite wall-flow honeycomb ceramic filter is as follows:The porosity 52.6% is averaged
8.9 μm of aperture, A axis compression strength 4.2MPa, B axle compression strength 2.4MPa, C axis compression strength 0.23MPa, coefficient of thermal expansion
1.49×10-6/ DEG C, sintering qualified rate is low, and 35% product is cracking.
Comparative example 3
A kind of cordierite wall-flow honeycomb ceramic filter that this comparative example provides, cordierite base raw material group become:
It is in terms of 100 parts by above-mentioned basic material parts by weight, pore creating material group becomes:
80 μm 1.5 parts of organic resin microcapsules average grain diameter
60 μm of graphite powder average grain diameter, 0.9 1.5 parts of circularity
This comparative example separately adds 6 parts of methylcellulose, 6 parts of glycerine, 30 parts of water.
The preparation method of the above-mentioned cordierite wall-flow honeycomb ceramic filter of this comparative example, includes the following steps:
1) powders such as talcum, kaolin, aluminium oxide, silicon powder, pore creating material, methylcellulose original is weighed by above-mentioned formula
Material, is added to batch mixer mixing 60min;
2) glycerine and water are added to kneading 60min in powder mixture and obtain uniform pug, kneading process will control mud
Material temperature degree is at 30 DEG C or less;
3) above-mentioned pug is put into vacuum deairing machine and is kneaded 2 times (vacuum degree 0.09MPa or less), it is then aging to be formed for 24 hours
Plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake is put into extruder, forms cellular moulded pottery not yet put in a kiln to bake under the guiding of mold, mold hole density is
300 holes/square inch;Pug cuts into the wet green body of certain altitude after squeezing out, be put into drying and shaping in microwave drying oven;
5) by the smooth rear transpostion interval plug-hole of dry green body end face cutting, deburring and skin-grafting are carried out after dry;
6) above-mentioned filtering body moulded pottery not yet put in a kiln to bake is put into high temperature sintering furnace, 1410 DEG C is heated to 5 DEG C/min of heating rate,
And 8 hours are kept the temperature, it then naturally cools to 100 DEG C and is prepared into cordierite wall-flow honeycomb ceramic filter.
The dosage of the pore creating material of this comparative example is 3 parts, the performance of cordierite wall-flow honeycomb ceramic filter obtained
Index is as follows:The porosity 45.5%, 7.5 μm of average pore size, A axis compression strength 10.2MPa, B axle compression strength 4.9MPa, C axis
Compression strength 0.45MPa, coefficient of thermal expansion 1.25 × 10-6/℃。
Comparative example 4
A kind of cordierite wall-flow honeycomb ceramic filter that this comparative example provides, cordierite base raw material group become:
It is in terms of 100 parts by above-mentioned basic material parts by weight, pore creating material group becomes:
80 μm 9 parts of organic resin microcapsules average grain diameter
60 μm of graphite powder average grain diameter, 0.9 9 parts of circularity
This comparative example separately adds 6 parts of methylcellulose, 6 parts of glycerine, 30 parts of water.
The preparation method of the above-mentioned cordierite wall-flow honeycomb ceramic filter of this comparative example, includes the following steps:
1) powders such as talcum, kaolin, aluminium oxide, silicon powder, pore creating material, methylcellulose original is weighed by above-mentioned formula
Material, is added to batch mixer mixing 60min;
2) glycerine and water are added to kneading 60min in powder mixture and obtain uniform pug, kneading process will control mud
Material temperature degree is at 30 DEG C or less;
3) above-mentioned pug is put into vacuum deairing machine and is kneaded 2 times (vacuum degree 0.09MPa or less), it is then aging to be formed for 24 hours
Plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake is put into extruder, forms cellular moulded pottery not yet put in a kiln to bake under the guiding of mold, mold hole density is
300 holes/square inch;Pug cuts into the wet green body of certain altitude after squeezing out, be put into drying and shaping in microwave drying oven;
5) by the smooth rear transpostion interval plug-hole of dry green body end face cutting, deburring and skin-grafting are carried out after dry;
6) above-mentioned filtering body moulded pottery not yet put in a kiln to bake is put into high temperature sintering furnace, 1410 DEG C is heated to 5 DEG C/min of heating rate,
And 8 hours are kept the temperature, it then naturally cools to 100 DEG C and is prepared into cordierite wall-flow honeycomb ceramic filter.
Pore creating material dosage is 18 parts in this comparative example, and the performance of cordierite wall-flow honeycomb ceramic filter obtained refers to
Mark is as follows:The porosity 71.2%, 24.3 μm of average pore size, A axis compression strength 1.5MPa, B axle compression strength 0.8MPa, C axis are anti-
Compressive Strength 0.04MPa, coefficient of thermal expansion 1.36 × 10-6/ DEG C, sintering qualified rate is low, and 50% product is cracking.
To sum up, cordierite wall-flow honeycomb ceramic filter of the invention, which has high intensity, porosity height, thermally expands, is
The low and adjustable aperture feature of number, can be used for the trapping to automotive diesel carbon soot particles, arresting efficiency under varying environment and reaches
To 85% or more;Thermal shock resistance is good, and product does not crack room temperature~550 DEG C cycle three times;Inventive cordierite matter wall-flow type bee
The stable preparation process of nest ceramic filtering body is reliable, easily controllable, and the prices of raw materials are cheap, it is easy to accomplish.
The present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment, but the present invention is not
It is confined to above-mentioned detailed process equipment and technological process, that is, does not mean that the present invention has to rely on above-mentioned detailed process equipment and work
Skill flow could be implemented.Person of ordinary skill in the field is it will be clearly understood that any improvement in the present invention, to product of the present invention
The equivalence replacement of each raw material and the addition of auxiliary element, the selection of concrete mode etc., all fall within protection scope of the present invention and public affairs
Within the scope of opening.
Claims (10)
1. a kind of cordierite wall-flow honeycomb ceramic filter, which is characterized in that by weight, including following component:
100 parts of cordierite base raw material
2~8 parts of organic resin microcapsules
2~8 parts of graphite powder.
2. cordierite wall-flow honeycomb ceramic filter according to claim 1, which is characterized in that the organic resin
The average grain diameter of microcapsules is 20~80 μm.
3. cordierite wall-flow honeycomb ceramic filter according to claim 1 or 2, which is characterized in that the graphite
Powder is the spheroidal particle that circularity is 0.8~1;
Preferably, the average grain diameter of the graphite powder is 20~60 μm.
4. the cordierite wall-flow honeycomb ceramic filter according to one of claim 1-3, which is characterized in that and with
The cordierite base parts by weight of raw materials is 100 parts of meters, further includes:
3~8 parts of methylcellulose
3~8 parts of glycerine
25~35 parts of water.
5. the cordierite wall-flow honeycomb ceramic filter according to one of claim 1-4, which is characterized in that by weight
Part meter, the cordierite base raw material includes following components:
6. a kind of preparation method of cordierite wall-flow honeycomb ceramic filter as described in any one in claim 1-5,
It is characterized in that, the preparation method includes the following steps:It is to take 2~8 in terms of 100 parts by the cordierite base parts by weight of raw materials
Part organic resin microcapsules and 2~8 parts of graphite powders are raw material, and the cordierite wall-flow type is prepared after mixing, pore-creating
Honeycomb ceramic filter body.
7. preparation method according to claim 6, which is characterized in that the preparation method includes the following steps:
1) by weight, by 100 parts of cordierite base raw material, 2~8 parts of organic resin microcapsules, 2~8 parts of graphite
Powder and the mixing of 3~8 parts of methylcellulose, obtain powder mixture;
2) 3~8 parts of glycerine and 25~35 parts of water by weight, are added to the powder mixture that step 1) obtains to pinch
It closes, obtains pug;
3) pug for obtaining step 2) through be kneaded, it is aging after, obtain plasticity moulded pottery not yet put in a kiln to bake;
4) the plasticity moulded pottery not yet put in a kiln to bake that step 3) obtains is formed into cellular moulded pottery not yet put in a kiln to bake, dryness finalization under the guiding of mold through squeezing;
It 5) will be through the cellular moulded pottery not yet put in a kiln to bake sealing of hole after step 4) dryness finalization;
6) the cordierite honeycomb ceramic filter will be obtained through the moulded pottery not yet put in a kiln to bake high temperature sintering after step 5) sealing pores, cooling
Filtering body.
8. the preparation method described according to claim 6 or 7, which is characterized in that in step 1), the mixing is in batch mixer
It carries out, the time of the mixing is 40~80min;
Preferably, in step 2), the time of the kneading is 40~80min;
Preferably, in step 2), the temperature of the kneading is 30 DEG C or less;
Preferably, in step 3), the mixing carries out in vacuum kneading machine, and the number of the mixing is 2~3 times, institute
The vacuum degree for stating vacuum kneading machine is 0.09MPa or less;
Preferably, in step 3), the aging time is 20~25h.
9. according to the preparation method described in one of claim 6-8, which is characterized in that in step 6), the tool of the high temperature sintering
Body process is:Cellular moulded pottery not yet put in a kiln to bake after step 5) dryness finalization is put into high temperature sintering furnace, with 5 DEG C/min of heating speed
Rate is heated to 1400~1450 DEG C, and keeps the temperature 6~10h.
10. according to the preparation method described in one of claim 6-9, which is characterized in that the preparation method includes the following steps:
1) by weight, by 100 parts of cordierite base raw material, 2~8 parts of organic resin microcapsules, 2~8 parts of graphite
Powder and 3~8 parts of methylcellulose, which are added in batch mixer, mixes 40~80min, obtains powder mixture;
2) 3~8 parts of glycerine and 25~35 parts of water by weight, are added to the powder mixture that step 1) obtains to pinch
It closes, the temperature for controlling kneading is 30 DEG C hereinafter, obtaining pug;
3) pug for obtaining step 2) is kneaded 2~3 times in vacuum degree is 0.09MPa vacuum kneading machines below, and aging 20
After~25h, plasticity moulded pottery not yet put in a kiln to bake is obtained;
4) the plasticity moulded pottery not yet put in a kiln to bake that step 3) obtains is put into extruder, cellular moulded pottery not yet put in a kiln to bake is formed through squeezing under the guiding of mold,
In, mold hole density is 200~400 holes/square inch;Pug cuts into wet green body after squeezing out, and is put into microwave drying oven and does
Dry sizing;
5) will through the cellular moulded pottery not yet put in a kiln to bake after step 4) dryness finalization after ends cutting is smooth transpostion interval plug-hole, carried out after dry
Deburring and skin-grafting;
6) moulded pottery not yet put in a kiln to bake after step 5) sealing pores is put into high temperature sintering furnace, is heated to 5 DEG C/min of heating rate
1400~1450 DEG C, and keep the temperature 6~10h and carry out high temperature sintering, 100 DEG C are naturally cooled to, the cordierite wall-flow type is obtained
Honeycomb ceramic filter body.
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