CN116063093B - DPF honeycomb ceramic based on flaked kaolin and preparation method thereof - Google Patents
DPF honeycomb ceramic based on flaked kaolin and preparation method thereof Download PDFInfo
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000005995 Aluminium silicate Substances 0.000 title claims abstract description 65
- 235000012211 aluminium silicate Nutrition 0.000 title claims abstract description 65
- 239000000919 ceramic Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 35
- 239000000203 mixture Substances 0.000 claims abstract description 31
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 239000013078 crystal Substances 0.000 claims abstract description 23
- 239000011230 binding agent Substances 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000000454 talc Substances 0.000 claims abstract description 19
- 229910052623 talc Inorganic materials 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 11
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 9
- 230000002776 aggregation Effects 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims description 35
- 238000002156 mixing Methods 0.000 claims description 32
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 26
- 229920003023 plastic Polymers 0.000 claims description 20
- 239000004033 plastic Substances 0.000 claims description 20
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 18
- 235000012222 talc Nutrition 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 230000032683 aging Effects 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 239000000314 lubricant Substances 0.000 claims description 15
- 238000001125 extrusion Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000000465 moulding Methods 0.000 claims description 10
- 238000007873 sieving Methods 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 7
- 229910052783 alkali metal Inorganic materials 0.000 claims description 6
- 150000001340 alkali metals Chemical group 0.000 claims description 6
- 238000005054 agglomeration Methods 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 2
- 239000008158 vegetable oil Substances 0.000 claims description 2
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 claims description 2
- 229910052878 cordierite Inorganic materials 0.000 abstract description 35
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 abstract description 32
- 230000035939 shock Effects 0.000 abstract description 10
- 229910010293 ceramic material Inorganic materials 0.000 abstract description 7
- 238000004220 aggregation Methods 0.000 abstract description 2
- 238000005336 cracking Methods 0.000 abstract description 2
- 230000002068 genetic effect Effects 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 239000002356 single layer Substances 0.000 abstract description 2
- 239000000758 substrate Substances 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract 1
- 235000011187 glycerol Nutrition 0.000 description 8
- 238000007603 infrared drying Methods 0.000 description 7
- 229910052622 kaolinite Inorganic materials 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000012764 semi-quantitative analysis Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- 241000276425 Xiphophorus maculatus Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910000272 alkali metal oxide Inorganic materials 0.000 description 1
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229910052903 pyrophyllite Inorganic materials 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0006—Honeycomb structures
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/04—Clay; Kaolin
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- 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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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/349—Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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Abstract
The invention discloses DPF honeycomb ceramic based on flaked kaolin and a preparation method thereof. The DPF honeycomb ceramic based on the flaked kaolin comprises the following raw materials of a spare material, a crystal nucleus agent and a binder; wherein the standby materials consist of the following raw materials: flaked kaolin, talc, gamma-Al 2 O 3 . Compared with water washing kaolin and calcined kaolin, the invention selects the flaked kaolin, has less aggregation degree of the lamellar structure of the raw materials, most particles are dispersed, single-layer lamellar materials are used as substrates, and are in situ compounded with other two lamellar raw materials, and the composition phase cordierite with the genetic relationship of lamellar structures is relied on, so that the low thermal expansion coefficient is realized, the thermal expansion performance of the material is obviously reduced, the cordierite ceramic can resist the thermal shock circulation for 30 times at 25-1000 ℃ without deformation and cracking, and the service life of the DPF honeycomb ceramic material is greatly prolonged.
Description
Technical Field
The invention relates to the technical field of new ceramic materials, in particular to DPF honeycomb ceramic based on peeled kaolin and a preparation method thereof.
Background
The honeycomb ceramic material is used for purifying and filtering the tail gas and particles of diesel automobile to make the pollutant discharge meet the national standard (namely CO is less than or equal to 500mg/km, NO) X Less than or equal to 35mg/km, PM less than or equal to 3 mg/km). When Chai Youqi car runs, the temperature of the exhaust port of internal combustion engine is 800-1000 deg.C, and the instantaneous temp. of flameout is suddenly reduced to about 100 deg.C. The DPF honeycomb ceramics should have a low thermal expansion coefficient and a good thermal shock resistance so as not to break during use, thereby affecting the purifying treatment effect.
Currently, DPF honeycomb ceramics are generally made of cordierite, which is synthesized from kaolin, talc, alumina, and the like. Such as: chinese characterThe invention patent CN105016718A discloses a cordierite honeycomb ceramic for a diesel vehicle exhaust catalytic cleaner and a preparation method thereof, wherein kaolinite powder, talcum powder, aluminum hydroxide powder and pyrophyllite powder are used for preparing DPF cordierite ceramic honeycomb, and the CTE is 0.75X10 -6 ℃ -1 (25 ℃ C. To 800 ℃ C.); chinese patent CN106588066a discloses a cordierite closed-flow honeycomb ceramic filter for trapping soot particles of diesel engine and its preparation method, which uses kaolin, cordierite powder and talcum to prepare DPF cordierite honeycomb ceramic with CTE of 1.51×10 -6 ℃ -1 (25℃～800℃)。
However, the cordierite honeycomb ceramics prepared by the method have poor thermal expansion and thermal shock cycling resistance, and the performance has important negative effects on the service life of the DPF cordierite honeycomb ceramics.
Disclosure of Invention
The invention aims to overcome the technical defects, and provides DPF honeycomb ceramic based on peeled kaolin and a preparation method thereof, which solve the technical problems of poor thermal expansion and poor thermal shock resistance circulation capability of the DPF honeycomb ceramic in the prior art.
In a first aspect, the invention provides a DPF honeycomb ceramic based on exfoliated kaolin, the raw materials of which comprise a spare material, a crystal nucleus agent and a binder; wherein,
the standby materials consist of the following raw materials in percentage by mass: 47.88 to 52.64 weight percent of flaked kaolin, 36.65 to 41.41 weight percent of talcum powder and gamma-Al 2 O 3 10.71wt％～15.47wt％。
In a second aspect, the invention provides a preparation method of DPF honeycomb ceramics based on peeled kaolin, which comprises the following steps:
mixing the raw materials: stripping kaolin, talcum powder and gamma-Al 2 O 3 The binder and the crystal nucleus agent are subjected to ball milling and sieving independently and then are uniformly mixed according to the mass ratio to obtain a mixture;
granulating and aging: adding water into the mixture for granulating, and ageing to obtain a blank;
mixing: adding a lubricant into the blank, and then performing vacuum pugging to discharge air in the blank and mixing to obtain a plastic blank;
extrusion molding: extruding and molding the prepared plastic blank to obtain a honeycomb green body;
and (3) drying: drying the formed green body to obtain a green body;
firing: and firing the dried green body to obtain the DPF honeycomb ceramic based on the flaked kaolin.
Compared with the prior art, the invention has the beneficial effects that:
(1) The DPF honeycomb ceramic prepared by the invention has lower CTE. Compared with water-washed kaolin and calcined kaolin, the invention selects the flaked kaolin, has less aggregation degree of the lamellar structure of the raw materials, most particles are dispersed, single-layer lamellar raw materials are used as a substrate, and are subjected to in-situ compounding with other two lamellar raw materials, and the occurrence of defects in grains is reduced by virtue of the composition phase cordierite (the content is 95-99 wt%) of the genetic relationship of lamellar structures, so that the grains are complete in growth, uniform voids are generated, and a high Wen Jin cordierite phase with a complete crystal form and a low expansion coefficient is generated, thereby realizing lower CTE (coefficient of thermal expansion), and obviously reducing the thermal expansion performance of the material.
(2) The DPF ceramic honeycomb prepared by the invention has better high-temperature quenching circulation resistance. Compared with the use of water-washed kaolin and calcined kaolin, the use of exfoliated kaolin allows the synthesis of complete high temperature stable cordierite crystals with firm bonding between the grains and close alignment oriented along the extrusion direction, thus breaking in the manner of through-grain breakage. Because of the low expansion characteristics of the cordierite crystalline phase and the presence of more porosity, the smaller thermal stress concentrations counteract the structural characteristics of the material itself, enabling the cordierite body ceramic to withstand 30 thermal shock cycles from 25 ℃ to 1000 ℃ without deformation and cracking. Meanwhile, the ceramic material has a crystal phase and a structure of cordierite, so that the ceramic material can withstand high temperature exceeding 1000 ℃ (the ceramic material can stably exist at the high temperature of 1420 ℃), and the porosity is 20-30%, so that the service life of the DPF honeycomb ceramic material is greatly prolonged.
Drawings
FIG. 1 is an X-ray diffraction pattern of exfoliated kaolin, with a predominant crystalline phase of kaolinite, content of 90wt%;
FIG. 2 is a scanning electron micrograph of exfoliated kaolin at 2000 Xmagnification, with the microstructure being a exfoliated lamellar structure;
FIG. 3 is an X-ray diffraction pattern of talc;
FIG. 4 is a scanning electron micrograph of alumina with a microstructure of mostly lamellar structure;
FIG. 5 is an X-ray diffraction chart of the cordierite ceramic obtained in example 3, with a main crystal phase of α -cordierite, in an amount of 95% by weight or more;
FIG. 6 is a graph of the microtopography of the example 3 cordierite ceramic at 5000 times magnification;
FIG. 7 is a back-scattered electron image of a sample of example 3 at 1000 Xmagnification for 30 thermal shocks.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
In a first aspect, the invention provides a DPF honeycomb ceramic based on exfoliated kaolin, the raw materials of which comprise a spare material, a crystal nucleus agent and a binder; wherein,
the standby materials consist of the following raw materials in percentage by mass: 47.88 to 52.64 weight percent of flaked kaolin, 36.65 to 41.41 weight percent of talcum powder and gamma-Al 2 O 3 10.71wt％～15.47wt％。
Industrial kaolin is classified into water-washed kaolin, calcined kaolin and flaked kaolin. The ceramic field is mostly selected from water-washed kaolin, namely paste or lump materials of raw ore stacked by physically crushed layers, and flaky objects with the diameter of more than 5 mu m, wherein the thickness of the flaky objects is unevenly distributed. At present, laminated kaolin is adopted for preparing DPF cordierite honeycomb ceramics, and the DPF cordierite honeycomb ceramics contain more impurities. The kaolin flakes are formed by layering or chemically processing the stacked structure into individual flat hexagonal flakes having a diameter of less than 2 μm, which are about 1/10 of their diameter, which develop well and reduce the coloration of impurities, and which are commonly used in the paper and paint industries; and the kaolin has low content of alkaline earth metal and alkali metal oxide, so the kaolin is rarely used in ceramic industry. The inventor has found by accident in the test process that the adoption of the flaked kaolin as the raw material of the DPF honeycomb ceramic can lead the obtained DPF cordierite honeycomb ceramic to have extremely low thermal expansion coefficient and excellent thermal shock resistance and circulation capacity, so the invention is proposed.
In the embodiment, the weight of the kaolin Dan Hanliang in the flaked kaolin is more than or equal to 90 percent, R 2 O is less than or equal to 1wt%, wherein R represents alkali metal, and D is the length and width of the lamellar sheet 50 The thickness of the lamellar sheet is only about one tenth of the width or the length between 1 and 1.5 mu m, and no obvious agglomeration exists among particles.
In the embodiment, the MgO content in the talcum powder is more than or equal to 30 weight percent, R 2 O is less than or equal to 0.5wt%, wherein R represents alkali metal; the powder without calcination is the optimal raw material, so raw talcum powder is selected, and the mineral talcum in the talcum powder is more than or equal to 80wt percent, D 50 Is 2-5 μm (laser particle size analyzer), and the specific surface area is 2m 2 /g～3m 2 And/g, the morphological index is 0.65-0.85.
In the present embodiment, γ -Al 2 O 3 Is of a sheet-like structure, al 2 O 3 The content is more than or equal to 99 weight percent, D 50 Is 2-5 mu m, R 2 O is less than or equal to 0.5wt%, wherein R represents alkali metal.
In this embodiment, the nucleating agent is yttria-stabilized zirconia; further, the molar fraction of yttrium oxide was 5mol% (5Y-ZrO 2 ) The method comprises the steps of carrying out a first treatment on the surface of the The addition amount of the crystal nucleus agent is 2-4wt% of the standby material, and further 3wt%.
In this embodiment, the binder is polyvinyl alcohol, and the amount of the binder added is 4 to 7wt% of the spare material.
In this embodiment, the raw materials of the DPF honeycomb ceramic based on the exfoliated kaolin further include: and (3) water.
Further, the addition amount of water is 5-8 wt% of the total mass of the standby material, the binder and the crystal nucleus agent.
In this embodiment, the raw materials of the DPF honeycomb ceramic based on the exfoliated kaolin further include: and (3) a lubricant.
Further, the lubricant is at least one selected from glycerin and vegetable oil, and the addition amount is 2-4wt% of the standby material, and further 3wt%.
In a second aspect, the invention provides a preparation method of DPF honeycomb ceramics based on peeled kaolin, which comprises the following steps:
s1, mixing raw materials: stripping kaolin, talcum powder and gamma-Al 2 O 3 The binder and the crystal nucleus agent are subjected to ball milling and sieving independently and then are uniformly mixed according to the mass ratio to obtain a mixture; wherein, in the process of single ball milling, the ball mill is a planetary ball mill, the ball milling time is 20-24 hours, the ball mass ratio is 1 (2-3), and the rotating speed is 200-400 rpm; the mesh number of the screen is 250-320 meshes; the components are uniformly mixed in a ball milling mode, the ball milling is a planetary ball milling machine, the ball milling time is 1-2 h, the ball mass ratio is 1 (2-3), and the rotating speed is 200-400 r/min.
S2, granulating and aging: adding water into the mixture for granulating, and ageing to obtain a blank; wherein the ageing time is 24-36 h.
S3, mixing: adding a lubricant into the blank, and then performing vacuum pugging to discharge air in the blank and mixing to obtain a plastic blank; wherein, the mixing time is 20-40 min;
s4, extrusion molding: extruding and molding the prepared plastic blank by adopting a honeycomb extruder (vacuum pressure system) to obtain a honeycomb green body; wherein the vacuum degree is 5×10 2 Pa～7×10 2 Pa, the extrusion pressure is 600-800 kN.
S5, drying: drying the formed green body to obtain a green body; wherein the drying temperature is 100-150 ℃ and the drying time is 10-12 h.
S6, sintering: firing the dried green body to obtain DPF honeycomb ceramic based on the flaked kaolin; wherein, the firing conditions are as follows: heating to 1380-1400 ℃ at the speed of 3-5 ℃/min, and preserving heat for 2-2.5 h at the highest temperature point; in some embodiments of the invention, the temperature is raised at a temperature of less than 1000 ℃ at a temperature raising rate of 5 ℃/min for 0.5-1 h at a full-hundred temperature point, and at a temperature of more than or equal to 1000 ℃ at a temperature raising rate of 3 ℃/min for 0.8-1..2 h at the full-hundred temperature point.
In the following examples and comparative examples of the present invention, some raw materials are summarized as follows:
the chemical compositions of the exfoliated kaolin used in examples 1 to 4 are shown in table 1.XRD semi-quantitative analysis, kaolin Dan Hanliang of which is more than or equal to 90wt percent, SEM microstructure analysis and D of lamellar length and width 50 In the range of 1-1.5 μm, the thickness of the sheet is only about one tenth of the width or length, and no obvious agglomeration exists between particles, as shown in figures 1 and 2.
TABLE 1 chemical composition of kaolin (wt%)
The talcum powder used in the invention is D 50 =2 to 5 μm (laser particle size analyzer), morphology index is first described in U.S. patent No.5141686, which is a measure of the degree of flakiness of talc, a typical procedure for determining morphology index is to place a sample in a clamp, maximize the orientation of flaky talc in the plane of the sample clamp, and then determine the XRD of the oriented talc, morphology index M being calculated semi-quantitatively from the XRD peak intensities as in formula 1-1 by the following equation, which expresses the degree of flakiness characteristic of talc:
wherein I is x Is the intensity of the peak of (004), I y Is the intensity of the (020) reflection peak.
I.e., talc having a morphology index of between about 0.65 and about 0.85, the platy talc can reduce the coefficient of thermal expansion of the product without substantially reducing the strength of the product too much.
I of Talc powder used in the patent of the invention x (004)＝90％，I y (020) =11.25%, calculated morphology index was 0.80,mineral phase talcum in talcum powder is more than or equal to 80wt%, mgO content is more than or equal to 30wt%, R 2 O is less than or equal to 0.5wt%. As shown in FIG. 3, D 50 Is 2-5 μm and is sheet-shaped with a specific surface area of 2m 2 /g～3m 2 /g。
gamma-Al used in the present invention 2 O 3 Is of a sheet-like structure, al 2 O 3 The content is 99wt%, D 50 Is 2 μm, R 2 O≤0.5wt％。
Comparative example 1
1) D of particles in raw kaolin ores 50 ＝15μm，R 2 The weight percentage of O is 5 percent, the microstructures are all pipe rods and are interwoven with the lamination structure, the content of kaolinite is 75 percent by weight (+ -2 percent by weight), and 50.27 percent by weight of crude kaolinite ore, 38.48 percent by weight of talcum powder and gamma-Al are weighed according to the mass ratio 2 O 3 11.25% by weight of a spare material, 5% by weight of polyvinyl alcohol as a binder, 3% by weight of 5Y-ZrO 2 Respectively ball-milling for 24 hours by using a planetary ball mill as a crystal nucleus agent, sieving with a 250-mesh sieve, and mixing and ball-milling the raw materials by using the planetary ball mill for 1 hour to obtain a mixture; in the ball milling process, the mass ratio of the balls is 1:2.5, and the rotating speed is 300 rpm;
2) Adding water accounting for 5wt% of the mixture into the mixture obtained in the step 1), uniformly mixing, granulating, and aging for 24 hours to obtain a standby blank;
3) Adding glycerol accounting for 3wt% of the standby material into the standby blank obtained in the step 2) to serve as a lubricant, and mixing for 0.5h in a pugging machine to obtain a plastic blank;
4) Extruding and molding the plastic blank prepared in the step 3) by adopting a honeycomb extruder (vacuum pressure system) to obtain a honeycomb green body, wherein the vacuum degree is 5.5x10 2 20Pa, and an extrusion pressure of 650+ -10 kN;
5) Placing the green body formed in the step 4) in a far infrared drying oven, and drying for 12 hours at 100 ℃ to obtain a green body;
6) And 5) putting the dried blank in the step 5) into an electric furnace to be sintered at 1380 ℃, wherein the heating rate is 5 ℃/min (less than 1000 ℃), the whole hundred temperature point is kept for 0.5h, the 3 ℃/min (more than or equal to 1000 ℃), the whole hundred temperature point is kept for 1h, and the highest temperature point is kept for 2h, so that the cordierite honeycomb ceramic body is obtained.
Comparative example 2
1) D of particles in washed Kaolin 50 ＝10μm，R 2 The O is 4wt%, the microstructure is lamination structure, the kaolinite content is 80wt% + -2wt%, 50.27wt%, talcum 38.48wt% and gamma-Al are weighed according to the mass ratio 2 O 3 11.25% by weight of a spare material, 5% by weight of polyvinyl alcohol as a binder, 3% by weight of 5Y-ZrO 2 Respectively ball-milling for 24 hours by using a planetary ball mill as a crystal nucleus agent, sieving with a 250-mesh sieve, and mixing and ball-milling the raw materials by using the planetary ball mill for 1 hour to obtain a mixture; in the ball milling process, the mass ratio of the balls is 1:2.5, and the rotating speed is 300 rpm;
2) Adding water accounting for 5wt% of the mixture into the mixture obtained in the step 1), uniformly mixing, granulating, and aging for 24 hours to obtain a standby blank;
3) Adding glycerol accounting for 3wt% of the standby material into the standby blank obtained in the step 2) to serve as a lubricant, and mixing for 0.5h in a pugging machine to obtain a plastic blank;
4) Extruding and molding the plastic blank prepared in the step 3) by adopting a honeycomb extruder (vacuum pressure system) to obtain a honeycomb green body, wherein the vacuum degree is 5.5x10 2 20Pa, and an extrusion pressure of 650+ -10 kN;
5) Placing the green body formed in the step 4) in a far infrared drying oven, and drying for 12 hours at 100 ℃ to obtain a green body;
6) And 5) putting the dried blank in the step 5) into an electric furnace to be sintered at 1380 ℃, wherein the heating rate is 5 ℃/min (less than 1000 ℃), the whole hundred temperature point is kept for 0.5h, the 3 ℃/min (more than or equal to 1000 ℃), the whole hundred temperature point is kept for 1h, and the highest temperature point is kept for 2h, so that the cordierite honeycomb ceramic body is obtained.
Comparative example 3
1) Calcined kaolin D 50 ＝10μm，R 2 The O is 4wt%, the microstructure is a laminated structure, the kaolinite content is 85wt% +/-2 wt%, 50.27wt% of kaolinite, 38.48wt% of talcum and gamma-Al are weighed according to the mass ratio 2 O 3 11.25% by weight of a spare material, 5% by weight of polyvinyl alcohol as a binder, 3% by weight of 5Y-ZrO 2 Respectively ball-milling for 24 hours by using a planetary ball mill as a crystal nucleus agent, sieving with a 250-mesh sieve, and mixing and ball-milling the raw materials by using the planetary ball mill for 1 hour to obtain a mixture; in the ball milling process, the mass ratio of the balls is 1:2.5, and the rotating speed is 300 rpm;
2) Adding water accounting for 5wt% of the mixture into the mixture obtained in the step 1), uniformly mixing, granulating, and aging for 24 hours to obtain a standby blank;
3) Adding glycerol accounting for 3wt% of the standby material into the standby blank obtained in the step 2) to serve as a lubricant, and mixing for 0.5h in a pugging machine to obtain a plastic blank;
4) Extruding and molding the plastic blank prepared in the step 3) by adopting a honeycomb extruder (vacuum pressure system) to obtain a honeycomb green body, wherein the vacuum degree is 5.5x10 2 20Pa, and an extrusion pressure of 650+ -10 kN;
5) Placing the green body formed in the step 4) in a far infrared drying oven, and drying for 12 hours at 100 ℃ to obtain a green body;
6) And 5) putting the dried blank in the step 5) into an electric furnace to be sintered at 1380 ℃, wherein the heating rate is 5 ℃/min (less than 1000 ℃), the whole hundred temperature point is kept for 0.5h, the 3 ℃/min (more than or equal to 1000 ℃), the whole hundred temperature point is kept for 1h, and the highest temperature point is kept for 2h, so that the cordierite honeycomb ceramic body is obtained.
Example 1
1) 50.27 weight percent of kaolin, 38.48 weight percent of talcum and gamma-Al are weighed according to the mass ratio 2 O 3 11.25% by weight of a spare material, 5% by weight of polyvinyl alcohol as a binder, 3% by weight of 5Y-ZrO 2 Respectively ball-milling for 24 hours by using a planetary ball mill as a crystal nucleus agent, sieving with a 250-mesh sieve, and mixing and ball-milling the raw materials by using the planetary ball mill for 1 hour to obtain a mixture; in the ball milling process, the mass ratio of the balls is 1:2.5, and the rotating speed is 300 rpm;
2) Adding water accounting for 5wt% of the mixture into the mixture obtained in the step 1), uniformly mixing, granulating, and aging for 24 hours to obtain a standby blank;
3) Adding glycerol accounting for 3wt% of the standby material into the standby blank obtained in the step 2) to serve as a lubricant, and mixing for 0.5h in a pugging machine to obtain a plastic blank;
4)extruding and molding the plastic blank prepared in the step 3) by adopting a honeycomb extruder (vacuum pressure system) to obtain a honeycomb green body, wherein the vacuum degree is 5.5x10 2 20Pa, and an extrusion pressure of 650+ -10 kN;
5) Placing the green body formed in the step 4) in a far infrared drying oven, and drying for 12 hours at 100 ℃ to obtain a green body;
6) And 5) putting the dried blank in the step 5) into an electric furnace to be sintered at 1400 ℃, wherein the heating rate is 5 ℃/min (less than 1000 ℃), the whole temperature point is kept for 0.5h, the 3 ℃/min (more than or equal to 1000 ℃), the whole temperature point is kept for 1h, and the highest temperature point is kept for 2h, so that the cordierite honeycomb ceramic body is obtained.
Example 2
1) Weighing 47.88wt% of flaked kaolin, 36.65wt% of talcum and gamma-Al according to the mass ratio 2 O 3 15.47% by weight of a spare material, 5% by weight of polyvinyl alcohol as a binder, 3% by weight of 5Y-ZrO 2 Respectively ball-milling for 24 hours by using a planetary ball mill as a crystal nucleus agent, sieving with a 250-mesh sieve, and mixing and ball-milling the raw materials by using the planetary ball mill for 1 hour to obtain a mixture; in the ball milling process, the mass ratio of the balls is 1:2.5, and the rotating speed is 300 rpm;
2) Adding water accounting for 5wt% of the mixture into the mixture obtained in the step 1), uniformly mixing, granulating, and aging for 24 hours to obtain a standby blank;
3) Adding glycerol accounting for 3wt% of the standby material into the standby blank obtained in the step 2) to serve as a lubricant, and mixing for 0.5h in a pugging machine to obtain a plastic blank;
4) Extruding and molding the plastic blank prepared in the step 3) by adopting a honeycomb extruder (vacuum pressure system) to obtain a honeycomb green body, wherein the vacuum degree is 5.5x10 2 20Pa, and an extrusion pressure of 650+ -10 kN;
5) Placing the green body formed in the step 4) in a far infrared drying oven, and drying for 12 hours at 100 ℃ to obtain a green body;
6) And 5) putting the dried blank in the step 5) into an electric furnace to be sintered at 1400 ℃, wherein the heating rate is 5 ℃/min (less than 1000 ℃), the whole temperature point is kept for 0.5h, the 3 ℃/min (more than or equal to 1000 ℃), the whole temperature point is kept for 1h, and the highest temperature point is kept for 2h, so that the cordierite honeycomb ceramic body is obtained.
Example 3
1) Weighing 47.88wt% of flaked kaolin, 41.41wt% of talcum and gamma-Al according to the mass ratio 2 O 3 10.71wt% of the spare material, 5wt% of polyvinyl alcohol as binder, 3wt% of 5Y-ZrO 2 Respectively ball-milling for 24 hours by using a planetary ball mill as a crystal nucleus agent, sieving with a 250-mesh sieve, and mixing and ball-milling the raw materials by using the planetary ball mill for 1 hour to obtain a mixture; in the ball milling process, the mass ratio of the balls is 1:2.5, and the rotating speed is 300 rpm;
2) Adding water accounting for 5wt% of the mixture into the mixture obtained in the step 1), uniformly mixing, granulating, and aging for 24 hours to obtain a standby blank;
3) Adding glycerol accounting for 3wt% of the standby material into the standby blank obtained in the step 2) to serve as a lubricant, and mixing for 0.5h in a pugging machine to obtain a plastic blank;
4) Extruding and molding the plastic blank prepared in the step 3) by adopting a honeycomb extruder (vacuum pressure system) to obtain a honeycomb green body, wherein the vacuum degree is 5.5x10 2 20Pa, and an extrusion pressure of 650+ -10 kN;
5) Placing the green body formed in the step 4) in a far infrared drying oven, and drying for 12 hours at 100 ℃ to obtain a green body;
6) And 5) putting the dried blank in the step 5) into an electric furnace to be sintered at 1400 ℃, wherein the heating rate is 5 ℃/min (less than 1000 ℃), the whole temperature point is kept for 0.5h, the 3 ℃/min (more than or equal to 1000 ℃), the whole temperature point is kept for 1h, and the highest temperature point is kept for 2h, so that the cordierite honeycomb ceramic body is obtained.
The XRD patterns of the different cordierite were observed to differ at diffraction peaks (131), (511) and (421) according to Miyashiro, and a distortion index was proposed as shown in the formulas 1-2:
wherein: angle, degree of appearance of theta-diffraction peak;
delta-distortion index, °.
From XRD and SEM analysis results, Δ= 0, so the cordierite type synthesized in example 3 is α -cordierite (high temperature stable phase), semi-quantitative analysis results: the content of alpha-cordierite (high-temperature stable phase) is more than or equal to 95wt%.
Example 4
1) According to the mass proportion, 52.64 weight percent of the flaked kaolin, 36.65 weight percent of talcum and gamma-Al are weighed 2 O 3 10.71wt% of the spare material, 5wt% of polyvinyl alcohol as binder, 3wt% of 5Y-ZrO 2 Respectively ball-milling for 24 hours by using a planetary ball mill as a crystal nucleus agent, sieving with a 250-mesh sieve, and mixing and ball-milling the raw materials by using the planetary ball mill for 1 hour to obtain a mixture; the method comprises the steps of carrying out a first treatment on the surface of the In the ball milling process, the mass ratio of the balls is 1:2.5, and the rotating speed is 300 rpm;
2) Adding water accounting for 5wt% of the mixture into the mixture obtained in the step 1), uniformly mixing, granulating, and aging for 24 hours to obtain a standby blank;
3) Adding glycerol accounting for 3wt% of the standby material into the standby blank obtained in the step 2) to serve as a lubricant, and mixing for 0.5h in a pugging machine to obtain a plastic blank;
4) Extruding and molding the plastic blank prepared in the step 3) by adopting a honeycomb extruder (vacuum pressure system) to obtain a honeycomb green body, wherein the vacuum degree is 5.5x10 2 20Pa, and extrusion pressure of 650+ -10 kN;
5) Placing the green body formed in the step 4) in a far infrared drying oven, and drying for 12 hours at 100 ℃ to obtain a green body;
6) And 5) putting the dried blank in the step 5) into an electric furnace to be sintered at 1400 ℃, wherein the heating rate is 5 ℃/min (less than 1000 ℃), the whole temperature point is kept for 0.5h, the 3 ℃/min (more than or equal to 1000 ℃), the whole temperature point is kept for 1h, and the highest temperature point is kept for 2h, so that the cordierite honeycomb ceramic body is obtained.
TABLE 2
(note: the variables in the comparative examples are that the raw materials in step 1) in the examples were compared using a general laminated raw material. )
As can be seen from Table 2 and FIGS. 5 to 7, the DPF honeycomb ceramics of the invention adopts a comprehensive thermal expansion instrument, the heating rate is 10 ℃/min, and the thermal expansion coefficient is measured to be as low as 0.2 multiplied by 10 -6 ℃ -1 (25 ℃ C. To 800 ℃ C.); adopting a high-temperature thermal shock furnace, and circulating the thermal shock resistance for 30 times (25-1000 ℃, air cooling and no crack on the appearance); the porosity is measured to be 20-30% by adopting a vacuum water absorption meter, in addition, the pressurization rate is 5mm/min by adopting a universal pressure tester, the A (B) axis compressive strength is more than or equal to 1.5MPa, the C axis compressive strength (parallel to the hole wall direction) is more than or equal to 8.5MPa, and the A (B) axis compressive strength is more than or equal to the relevant performance requirements in wall flow type honeycomb ceramics for diesel particulate traps (JC/T2396-2017), which indicates that the DPF honeycomb ceramics can be used as a catalyst carrier and can enable the national six standards of heavy diesel vehicle pollutant emission.
Further, as is clear from the comparison with comparative examples 1 to 3, the cordierite honeycomb ceramics synthesized from the laminar kaolin have a lower thermal expansion coefficient and excellent thermal shock resistance, and are superior in performance to the conventional kaolin synthesized cordierite ceramic body.
The above-described embodiments of the present invention do not limit the scope of the present invention. Any other corresponding changes and modifications made in accordance with the technical idea of the present invention shall be included in the scope of the claims of the present invention.
Claims (6)
1. DPF honeycomb ceramic based on the flaked kaolin is characterized in that the raw materials comprise a spare material, a crystal nucleus agent and a binder; wherein,
the standby materials consist of the following raw materials in percentage by mass: kaolin 47.88-52.64 wt%, talcum powder 36.65-wt-41.41-wt%, gamma-Al 2 O 3 10.71wt% -15.47 wt%; the weight of kaolin Dan Hanliang in the flaked kaolin is more than or equal to 90 percent, R 2 O is less than or equal to 1wt%, wherein R represents alkali metal, and D is the length and width of the lamellar sheet 50 No obvious agglomeration exists between particles at 1-1.5 mu m; the talcum powder is raw talcum powder; the MgO content in the talcum powder is more than or equal to 30 weight percent, R 2 O is less than or equal to 0.5wt%, wherein R represents alkali metal;the mineral phase talcum in the talcum powder is more than or equal to 80 weight percent, D 50 Is 2-5 mu m, and the specific surface area is 2m 2 /g～3m 2 /g, morphology index is 0.65-0.85; the gamma-Al 2 O 3 Is of a sheet-like structure, al 2 O 3 The content is more than or equal to 99 weight percent, D 50 Is 2-5 mu m, R 2 O is less than or equal to 0.5wt%, wherein R represents alkali metal;
the crystal nucleus agent is yttria-stabilized zirconia, and the addition amount of the crystal nucleus agent is 2-4wt% of the standby material; the binder is polyvinyl alcohol, and the addition amount of the binder is 4-7wt% of the standby material.
2. The delaminated kaolin based DPF honeycomb ceramic according to claim 1, wherein the raw materials of the delaminated kaolin based DPF honeycomb ceramic further comprise: water and a lubricant; wherein,
the addition amount of the water is 5-8 wt% of the total mass of the standby material, the binder and the crystal nucleus agent;
the lubricant is at least one of glycerol or vegetable oil, and the addition amount of the lubricant is 2-4 wt% of the standby material.
3. A method for preparing a DPF honeycomb ceramic based on exfoliated kaolin according to any one of claims 1 to 2, characterized by comprising the following steps:
mixing the raw materials: stripping kaolin, talcum powder and gamma-Al 2 O 3 The binder and the crystal nucleus agent are subjected to ball milling and sieving independently and then are uniformly mixed according to the mass ratio to obtain a mixture; wherein,
granulating and aging: adding water into the mixture for granulating, and ageing to obtain a blank;
mixing: adding a lubricant into the blank, and then performing vacuum pugging to discharge air in the blank and mixing to obtain a plastic blank;
extrusion molding: extruding and molding the prepared plastic blank to obtain a honeycomb green body;
and (3) drying: drying the formed green body to obtain a green body;
firing: and firing the dried green body to obtain the DPF honeycomb ceramic based on the flaked kaolin.
4. The preparation method of the DPF honeycomb ceramic based on the flaked kaolin is characterized in that the components are uniformly mixed in a ball milling mode, the ball mill is a planetary ball mill in the processes of single ball milling and mixed ball milling, the single ball milling time is 20-24 hours, the mixed ball milling time is 1-2 hours, the ball mass ratio is 1 (2-3), and the rotating speed is 200-400 r/min; the mesh number of the screen is 250-320 meshes.
5. The method for preparing the DPF honeycomb ceramic based on the flaked kaolin according to claim 3, wherein the aging time is 24-36 h, and the mixing time is 20-40 min.
6. The method for preparing the DPF honeycomb ceramic based on the flaked kaolin according to claim 3, wherein the firing conditions are as follows: heating to 1380-1400 deg.c at the speed of 3-5 deg.c/min and maintaining at the highest temperature for 2-2.5 hr.
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