CN115043667A - Preparation method of cordierite honeycomb ceramic carrier with porosity of more than 60 percent - Google Patents
Preparation method of cordierite honeycomb ceramic carrier with porosity of more than 60 percent Download PDFInfo
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- CN115043667A CN115043667A CN202210816601.4A CN202210816601A CN115043667A CN 115043667 A CN115043667 A CN 115043667A CN 202210816601 A CN202210816601 A CN 202210816601A CN 115043667 A CN115043667 A CN 115043667A
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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
- C04B38/0675—Vegetable refuse; Cellulosic materials, e.g. wood chips, cork, peat, paper
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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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract
The invention discloses a preparation method of a cordierite honeycomb ceramic carrier with porosity of more than 60%, which comprises the steps of raw material inspection, screening and preparation; mixing materials; kneading mud in a mud kneading machine, coarsely refining and sieving, ageing, refining and sieving; extruding and molding to obtain a honeycomb ceramic carrier green body; drying and shaping the honeycomb ceramic carrier green body; cutting and firing the dried carrier to obtain a cordierite honeycomb ceramic carrier; the firing adopts the heating rate of 10-50 ℃ to heat up, and the firing is carried out for 12 hours at 1410 +/-5 ℃; and (5) coating a film, dotting holes, scraping mud, drying and obtaining a finished product. According to the invention, specific raw materials are adopted to combine with a special preparation process, so that the product porosity and the median pore diameter are effectively improved while the product yield, the isostatic strength, the thermal shock resistance and other performances are ensured, the prepared product porosity is 60-70%, the median pore diameter is 15-20 μm, and the use requirements of national six-emission standards of gasoline vehicles can be met.
Description
Technical Field
The invention relates to the technical field of honeycomb ceramic carrier preparation, in particular to a preparation method of a cordierite honeycomb ceramic carrier with porosity of more than 60%.
Background
The honeycomb ceramic is a porous industrial ceramic, has the characteristics of large specific surface area, small airflow resistance, low thermal expansion, thermal shock resistance and the like, is widely used for a carrier of an automobile exhaust purification catalyst and a heat accumulator for high-temperature combustion, and can change harmful components such as HC, CO, NO and the like in exhaust into harmless components to be discharged. The catalyst is widely applied to diesel automobiles, urban buses, heavy trucks, mine operation vehicles and forklifts, and is the best choice for filtering and catalyst carriers of the existing gasoline engine tail gas purification system.
In order to meet the requirement of high porosity, the conventional cordierite honeycomb ceramic carrier usually adopts expensive pore-forming agents such as organic materials and plastic balls for pore-forming, although the porosity of the product can be effectively improved, the cordierite honeycomb ceramic carrier cannot be widely accepted by users due to high manufacturing cost, and meanwhile, the porosity of the cordierite honeycomb ceramic carrier cannot reach the optimal level.
Disclosure of Invention
Aiming at the problems in the prior art, the technical problem to be solved by the application is to provide the preparation method of the cordierite honeycomb ceramic carrier with the porosity of more than 60%, so that the porosity of the product is effectively improved, the manufacturing cost is reduced, and the use requirement of the national six-emission standard of gasoline engines can be met.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a method for preparing a cordierite honeycomb ceramic carrier with porosity of more than 60% comprises the following specific steps:
1) inspecting, screening and preparing the preparation raw materials; wherein the talc has a median particle size of 20-30 μm, the alumina has a median particle size of 5-10 μm, the silica has a median particle size of 15-25 μm, the kaolin has a median particle size of 3-10 μm, and the aluminum hydroxide has a median particle size of 2-5 μm; the content of impurities by weight percent requires: CaO is less than or equal to 0.5 percent, Na 2 O+K 2 O is less than or equal to 0.5 percent; the preparation raw materials comprise 38-42 parts of talc, 18-20 parts of alumina, 18-20 parts of silicon dioxide, 8-12 parts of kaolin and 10-12 parts of aluminum hydroxide; adding 5-7 parts by weight of binder and 38-45 parts by weight of pore-forming agent into 100 parts by weight of talc, alumina, silicon dioxide, kaolin and aluminum hydroxide;
2) mixing talc, alumina, kaolin, aluminum hydroxide and silicon dioxide, adding a binder and a pore-forming agent, continuously mixing, adding water, and mixing;
3) kneading mud in a mud kneading machine, coarsely refining and sieving, ageing, refining and sieving to obtain pug;
4) feeding the refined and sieved pug into an extruder for extrusion molding to obtain a honeycomb ceramic carrier green body;
5) drying and shaping the honeycomb ceramic carrier green body;
6) cutting and firing the dried honeycomb ceramic carrier green body to obtain a cordierite honeycomb ceramic carrier; the firing is carried out for 12 hours at 1410 +/-5 ℃ by adopting the temperature rise rate of 10-50 ℃/h;
7) and (5) coating a film, dotting holes, scraping mud, drying and obtaining a finished product.
The preparation method of the cordierite honeycomb ceramic carrier with the porosity of more than 60 percent comprises the following steps of: firing at the temperature of 180 ℃ and 230 ℃ for 10h in an anaerobic environment.
The preparation method of the cordierite honeycomb ceramic carrier with the porosity of more than 60 percent comprises the steps of using hydroxypropyl methyl cellulose as the binder and ensuring the viscosity to be more than 20000 Pa.S.
According to the preparation method of the cordierite honeycomb ceramic carrier with the porosity of more than 60%, the adding amount of water is 20-22% of the total weight of the raw materials.
According to the preparation method of the cordierite honeycomb ceramic carrier with the porosity of more than 60%, the screen mesh adopted for coarse smelting and sieving is an 80-mesh screen mesh, mud is kneaded for 15-20 minutes and aged for 12-16 hours, and the screen mesh adopted for fine smelting and sieving is a 120-mesh screen mesh.
According to the preparation method of the cordierite honeycomb ceramic carrier with the porosity of more than 60%, the prepared honeycomb ceramic carrier green body has the wall thickness of 0.2-0.3 mm, the pore density of 200-300 meshes, the diameter of 100-150 mm and the length of 100-200 mm.
According to the preparation method of the cordierite honeycomb ceramic carrier with the porosity of more than 60%, the weight water content of the dried honeycomb ceramic carrier green body is less than 1.0%;
the preparation method of the cordierite honeycomb ceramic carrier with the porosity of more than 60% adopts microwave drying and shaping of the honeycomb ceramic carrier green body.
The preparation method of the cordierite honeycomb ceramic carrier with the porosity of more than 60% adopts a temperature rise rate of 15 ℃/h to rise within the range of 200-800 ℃ during firing, and adopts a temperature rise rate of 50 ℃/h to rise within other temperature ranges.
Has the advantages that: compared with the prior art, the invention adopts specific raw material composition and a special preparation process, effectively improves the porosity and the median pore diameter of the product while ensuring the performances of the finished product rate, the isostatic strength, the thermal shock resistance and the like, ensures that the porosity of the prepared product is 60-70 percent, has the median pore diameter of 15-20 mu m, and can meet the use requirement of national emission standard of gasoline engines.
Drawings
FIG. 1 is a scanning electron micrograph of a wall cross-section of a high porosity honeycomb ceramic support.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
Cordierite honeycomb ceramic carriers having a porosity of 60% or more were prepared according to the raw material amounts shown in table 2, and the specific steps of the preparation were as follows:
1) inspecting, screening and preparing raw materials; specifically, it is shown in Table 1
Wherein, the pore-forming agent: the modified wood chip powder is selected from wood chip powder or modified wood chip powder, and the modification method of the modified wood chip powder comprises the following steps: firing at the temperature of 180 ℃ and 230 ℃ for 10h in an anaerobic environment. The binder is hydroxypropyl methylcellulose, and the viscosity of the binder is 20000-25000 Pa.S (in the embodiment, 60TY which is a product sold by Shandong-one New Material science and technology Co., Ltd.) is adopted.
2) Firstly, mixing talc, alumina, kaolin, aluminum hydroxide and silicon dioxide, then adding a binder and a pore-forming agent for continuous mixing, and then adding 21% water of the sum of the inorganic material, the binder and the pore-forming agent by weight for continuous mixing;
3) kneading mud in a mud kneading machine (coarse milling and sieving, 80-mesh sieve) for 15 minutes, ageing for 12 hours, and refining and sieving (120-mesh sieve);
4) feeding the refined and sieved pug into an extruder for extrusion molding to prepare a honeycomb ceramic carrier green body, wherein the wall thickness is 0.2-0.3 mm, the pore density is 200-300 meshes, the diameter is 100-150 mm, and the length is 100-200 mm;
5) sequentially drying and shaping the green bodies of the honeycomb ceramic carrier; the water content of the dried green body of the honeycomb ceramic carrier is less than 1.0 percent (weight percentage);
6) cutting and firing the dried carrier to obtain a cordierite honeycomb ceramic carrier; the firing is carried out for 12 hours at 1410 +/-5 ℃ by adopting the temperature rise rate of 10-50 ℃/h; wherein, during firing, the temperature is raised at the temperature of 200-800 ℃ by adopting the temperature raising rate of 15 ℃/h, and the temperature is raised at the temperature of 50 ℃/h in other temperature ranges;
7) and (5) coating a film, dotting holes, scraping mud, drying and obtaining a finished product.
TABLE 2 recipe and test results (parts per unit)
| Composition (I) | Product 1 | Product 2 | Product 3 | Product 4 | Comparative example 1 | Comparative example 2 | Comparison 3 |
| Talc | 38 | 40 | 41 | 42 | 40 | 40 | 40 |
| |
20 | 18 | 19 | 20 | 18 | 18 | 18 |
| Kaolin clay | 12 | 11 | 10 | 8 | 11 | 11 | 11 |
| |
20 | 19 | 18 | 18 | 19 | 19 | 19 |
| Aluminum hydroxide | 10 | 12 | 12 | 12 | 12 | 12 | 12 |
| Binder | 5 | 6 | 6 | 7 | 3 | 6 | 10 |
| Pore-forming agent | 38 | 40 | 43 | 45 | 30 | 60 | 60 |
| Number of cracks in product | 3 | 2 | 2 | 8 | 1 | 20 | 22 |
| Number of qualified products | 97 | 98 | 99 | 92 | 99 | 80 | 78 |
| Percent pass (%) | 97 | 98 | 99 | 92 | 99 | 80 | 78 |
| Porosity (%) | 60.4 | 63.3 | 65.4 | 70.1 | 52.6 | 76.4 | 78.7 |
| Median pore diameter (mum) | 17.4 | 17.6 | 17.5 | 17.7 | 17.5 | 17.5 | 17.4 |
| Isostatic strength (MPa) | 1.7 | 1.6 | 1.5 | 1.6 | 2.4 | 0.6 | 0.5 |
| Thermal shock resistance (. degree. C.) | 650 | 650 | 650 | 650 | 650 | 650 | 650 |
The pore-forming agents of the products 2 and 3 are modified wood chip powder, the pore-forming agents of the products 1 and 4 are wood chip powder as pore-forming agents, the pore-forming agent of the comparison 1 is polymethyl methacrylate (PMMA, loss rate of 99% at 1000 ℃ and particle size of 35-45 μm, KBspherer 40PMMA, Suzhoujiyi microsphere science and technology Limited, in this embodiment), the pore-forming agents of the comparison 2 and 3 are plastic microspheres (loss rate of 99% at 1000 ℃ and particle size of 35-45 μm, Suzhoujiyi microsphere science and technology Limited, KBspherer 40ps, in this embodiment).
The porosity and the median pore diameter are tested by a mercury intrusion method (GB/T21650.1-2008/ISO 15901-1:2005, the test parameters are set as that the mercury contact angle is 130 degrees and the mercury surface tension is 0.485 N.m -1 (ii) a Mercury density (20 ℃)13.5335 g/mL; acquiring pressure data in a stepping mode, wherein the pressure balance time is 10 s; no pretreatment). Thermal shock resistance (no cracking after three cycles) was determined by honeycomb ceramic GB/T25994-.
The isostatic pressing test method comprises the following steps: the prepared sample piece is put into a proper sealing rubber sleeve (the rubber sleeve has certain elasticity); and placing the sealed sample piece in a liquid medium of an isostatic pressure tester to enable the sample piece to be positioned below the liquid level, closing an isostatic pressure liquid cylinder cover, and pressurizing liquid in the cylinder. Testing parameters, wherein the pressurizing rate is 0.1 MPa/min; the test range is 0-10 MPa. The sonar monitoring system monitors whether a sample piece in the liquid cylinder is broken or not in the boosting process, and when the sample piece is broken and makes a sound, the current pressure is the isostatic pressure intensity of the sample piece.
Fig. 1 is a scanning electron microscope image of a wall section of a high-porosity honeycomb ceramic carrier, and as can be seen by combining the results in table 2, a reasonable inorganic material formula is the basis for satisfying the basic performance of the honeycomb ceramic carrier, while the selection of raw materials, particularly the particle size and the impurity content, are one of important factors for determining the product performance, and the porosity and the median pore diameter of the product can be effectively improved by reasonably proportioning a pore-forming agent and a binder.
Example 2
The formulation and preparation of product 3 were the same as in example 1, except that different ramp rates were used during firing, and the results are shown in Table 3.
TABLE 3 product results for different temperature ramping processes
Claims (9)
1. A method for preparing a cordierite honeycomb ceramic carrier with porosity of more than 60 percent is characterized by comprising the following specific steps:
1) inspecting, screening and preparing the preparation raw materials; wherein the talc has a median particle size of 20-30 μm, the alumina has a median particle size of 5-10 μm, the silica has a median particle size of 15-25 μm, the kaolin has a median particle size of 3-10 μm, and the aluminum hydroxide has a median particle size of 2-5 μm; the content of impurities by weight percent requires: CaO is less than or equal to 0.5 percent and Na 2 O+K 2 O is less than or equal to 0.5 percent; the preparation raw materials comprise 38-42 parts of talc, 18-20 parts of alumina, 18-20 parts of silicon dioxide, 8-12 parts of kaolin and 10-12 parts of aluminum hydroxide; adding 5-7 parts by weight of binder and 38-45 parts by weight of pore-forming agent into 100 parts by weight of talc, alumina, silicon dioxide, kaolin and aluminum hydroxide;
2) mixing talc, alumina, kaolin, aluminum hydroxide and silicon dioxide, adding a binder and a pore-forming agent, continuously mixing, and adding water for mixing;
3) kneading mud in a mud kneading machine, coarsely refining and sieving, ageing, refining and sieving to obtain pug;
4) feeding the refined and sieved pug into an extruder for extrusion molding to obtain a honeycomb ceramic carrier green body;
5) drying and shaping the honeycomb ceramic carrier green body;
6) cutting and firing the dried honeycomb ceramic carrier green body to obtain a cordierite honeycomb ceramic carrier; the firing is carried out for 12 hours at 1410 +/-5 ℃ by adopting the temperature rise rate of 10-50 ℃/h;
7) and (5) coating a film, dotting holes, scraping mud, drying and obtaining a finished product.
2. The method for preparing a cordierite honeycomb ceramic carrier having a porosity of 60% or more according to claim 1, wherein the pore former is modified wood dust, and the modification method of the modified wood dust is: firing at the temperature of 180 ℃ and 230 ℃ for 10h in an anaerobic environment.
3. The method of claim 1, wherein the binder is hydroxypropyl methylcellulose and has a viscosity of > 20000 Pa-S.
4. The method for producing a cordierite honeycomb ceramic carrier having a porosity of 60% or more according to claim 1, wherein the amount of water added is 20 to 22% based on the total weight of the raw materials for production.
5. The method for preparing a cordierite honeycomb ceramic carrier with porosity of 60% or more according to claim 1, wherein the screen used for the rough refining and sieving is an 80-mesh screen, the pug is kneaded for 15-20 minutes, the aging lasts for 12-16 hours, and the screen used for the refining and sieving is a 120-mesh screen.
6. The method for preparing a cordierite honeycomb ceramic carrier with a porosity of 60% or more according to claim 1, wherein the prepared green honeycomb ceramic carrier has a wall thickness of 0.2 to 0.3mm, a cell density of 200 to 300 mesh, a diameter of 100 to 150mm and a length of 100 to 200 mm.
7. The method of claim 1, wherein the green dried honeycomb ceramic substrate has a moisture content of less than 1.0% by weight.
8. The method of claim 1 wherein the green honeycomb ceramic support is shaped by microwave drying.
9. The method for producing a cordierite honeycomb ceramic carrier having a porosity of 60% or more according to claim 1, wherein the temperature is raised at a temperature rise rate of 15 ℃/h in a range of 200 ℃ to 800 ℃ and at a temperature rise rate of 50 ℃/h in other temperature ranges during firing.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116063095A (en) * | 2023-03-06 | 2023-05-05 | 山东奥福环保科技股份有限公司 | Thin-wall cordierite honeycomb ceramic filter with large median pore diameter and preparation method and application thereof |
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| US20090295007A1 (en) * | 2008-05-30 | 2009-12-03 | William Peter Addiego | High Porosity Cordierite Honeycomb Articles |
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| CN116063095A (en) * | 2023-03-06 | 2023-05-05 | 山东奥福环保科技股份有限公司 | Thin-wall cordierite honeycomb ceramic filter with large median pore diameter and preparation method and application thereof |
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