CN115073135B - Preparation method of large-size high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier - Google Patents
Preparation method of large-size high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier Download PDFInfo
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Abstract
The invention discloses a preparation method of a large-size high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier, which comprises the following raw materials in percentage by weight: 25-42% of talc, 5-10% of non-active alumina, 12-16% of silicon dioxide, 20-30% of kaolin, 5-10% of active alumina, 0.2-0.5% of surfactant, 2-6% of binder and 1-3% of lubricant, wherein the sum of the components is 100%. The method adopts specific raw material types and specifications, matches reasonable usage and combines an improved preparation process, and can prepare the large-specification thin-wall cordierite honeycomb ceramic carrier with the diameter of more than or equal to 177mm and the wall thickness of 4mil, the thin-wall cracking rate of the product is lower than 5 percent, and the yield is high; in addition, the product also has good mechanical properties, wherein the compressive strength in the A direction is not less than 12MPa, the compressive strength in the B direction is not less than 4MPa, and the compressive strength in the C direction is not less than 0.3MPa.
Description
Technical Field
The invention relates to the technical field of honeycomb ceramic carrier preparation, in particular to a preparation method of a large-specification high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier.
Background
The large-size cordierite honeycomb ceramic carrier for purifying the tail gas of the diesel engine has the diameter generally larger than 177mm, adopts a honeycomb-shaped structure and comprises a plurality of independent pore channels separated by pore channel walls, and the density of the pore channels is more than 280 per inch 2 The wall thickness of the conventional pore canal is more than or equal to 0.17mm, and for thin-wall products, the wall thickness is generally in the mil level.
The existing thin-wall cordierite honeycomb ceramic carrier is mostly synthesized in situ by cordierite, the adopted raw materials comprise components such as talc, alumina, silica, kaolin, additives and the like, and due to different physical and chemical characteristics of the materials, thin-wall cracking can be generated in the preparation process of the product, so that defects are generated, and meanwhile, due to the thin wall, the pressure resistance of the product is reduced, and the tail gas purification effect of a diesel engine is further influenced.
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 large-specification high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier, reduce thin-wall cracking, effectively improve the pressure resistance of the product and meet the use requirement of the national six-emission standard of diesel vehicles.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a method for preparing a large-size high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier comprises the following raw materials in percentage by weight: 25-42% of talc, 5-10% of non-active alumina, 12-16% of silicon dioxide, 20-30% of kaolin, 5-10% of active alumina, 0.2-0.5% of surfactant, 2-6% of binder and 1-3% of lubricant, wherein the sum of the components is 100%; the method comprises the following specific steps:
1) Mixing talc, non-activated alumina, kaolin, activated alumina, silicon dioxide and a binder, adding a surfactant, continuously mixing, and finally mixing with a lubricant;
2) Fully pugging in a pug mill;
3) Molding in a molding machine for one time, and controlling the temperature to be not more than 38 ℃;
4) Calcining in a kiln, and carrying out temperature programming to 1400 +/-20 ℃ according to the temperature of 15-30 ℃/h, and keeping the temperature for not less than 8h;
5) Performing fine grinding size processing and skin grafting to obtain a finished product;
wherein, the diameter of the large specification is more than 177mm, the wall thickness of the thin wall is 4mil, the high pressure bearing is that the compressive strength in the A direction is not less than 12MPa, the compressive strength in the B direction is not less than 4MPa, and the compressive strength in the C direction is not less than 0.3MPa.
In the preparation method of the large-specification high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier, the particle size range of the talc is 6-14 mu m; mgO accounts for more than 30% of the weight of the talc, and CaO and K in the talc 2 O and Na 2 The weight ratio of the sum of O is less than 0.5 percent.
The preparation method of the large-specification high-pressure thin-wall cordierite honeycomb ceramic carrier has the advantages that the particle size range of inactive alumina is 2-8 mu m, and the purity is more than 99 percent.
The preparation method of the large-specification high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier has the advantages that the particle size range of silicon dioxide is 2-8 mu m, and the purity is more than 99 percent.
The preparation method of the large-specification high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier has the advantages that the particle size range of kaolin is 1-5 mu m, and Al in the kaolin 2 O 3 Weight ratio is more than 35 percent, and SiO 2 The weight ratio is more than 45 percent.
The preparation method of the large-specification high-pressure thin-wall cordierite honeycomb ceramic carrier comprises the steps of preparing active alumina with Al 2 O 3 Weight ratio is more than 65%, caO + K 2 O+Na 2 The weight ratio of O is less than 0.5 percent, and the specific surface area of the activated alumina is 150-350 m 2 /g。
The preparation method of the large-size high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier comprises the step 4), the temperature is programmed to 1400 +/-20 ℃ according to the temperature of 15-20 ℃/h, and the temperature is kept for 8-10h.
Has the advantages that: compared with the prior art, the invention has the technical advantages that:
1) The method adopts specific raw material types and specifications, matches reasonable usage and combines an improved preparation process, and can prepare the large-specification thin-wall cordierite honeycomb ceramic carrier with the diameter of more than or equal to 177mm and the wall thickness of 4mil, the thin-wall cracking rate of the product is lower than 5 percent, and the yield is high.
2) On the basis of high yield, the product can be ensured to have good mechanical property, wherein the compressive strength in the A direction is not lower than 12MPa, the cracking rate of the thin wall of the product is less than 5 percent, the yield is very high, and the use requirement can be met.
Drawings
FIG. 1 is a scanning electron microscope image of a thin-wall structure of a large-size high-pressure-bearing thin-wall honeycomb ceramic carrier.
Detailed Description
The present invention will now be described in detail with reference to the following examples.
The raw material requirements used in the following examples are shown in table 1.
Table 1 raw material specification table
Example 1
Preparing large-specification high-pressure-bearing thin-wall honeycomb ceramic carriers according to the raw material dosage of Table 2, wherein the large specification is more than 177mm in diameter, and typical dimensions comprise 330mm,305mm,267mm,228mm,190mm and 177.8mm; the thin wall was 4mil thick. The product prepared in this example (cylindrical product) had a diameter of 330mm and a thin wall thickness of 4mil.
The preparation method comprises the following specific steps:
1) Mixing talc, inactive alumina, kaolin, active alumina, silicon dioxide and a binder, adding a surfactant for continuous mixing, and finally mixing with a lubricant;
2) Fully pugging in a pug mill;
3) Molding in a molding machine at one time, controlling the temperature not to exceed 38 ℃ (the molding cannot be carried out when the temperature exceeds 38 ℃);
3) Calcining in a kiln, and carrying out temperature programming to 1400 +/-20 ℃ at the speed of 20 ℃/h, and keeping the temperature for not less than 8h.
4) And (4) performing fine grinding size processing and skin grafting (according to a conventional method, CN105777194A is referred to), and obtaining a finished product.
TABLE 2 Components and amounts (in parts) of the product and test results
In table 2, the surfactant can be tall oil, lauric acid, acrylic emulsion, and this time the product was prepared with acrylic emulsion (shenzhen jitian chemical limited, with 44% solid content). The binder was methyl cellulose (commercially available, luzhou 4000). The lubricant may be a soap solution or a polyalphaolefin, which is used this time (commercially available, model numbers PAO2, PAO3, PAO 4). The non-activated alumina is the conventional commercial alumina product. And (4) directly and visually detecting the cracking of the thin wall.
The compression strength is detected by adopting the national standard (GB/T25994-2010), the product is circular, and the load application rate is 1.5MPa/s, and the unit is MPa.
The porosity was tested by mercury intrusion method (GB/T21650.1-2008/ISO 15901-1) with the test parameters set as: contact angle of mercury is130 °; mercury surface tension 0.485 N.m -1 (ii) a Mercury density (20 ℃) 13.5335g/mL; acquiring pressure data in a stepping mode, wherein the pressure balance time is 10s; no pretreatment.
As can be seen from table 2, the specifications of the raw materials, the specific components of the product and their reasonable amounts are one of the main factors determining whether the product cracks and the strength of the product, and the products 3 and 4 in this example are most effective compared to other products.
Example 2
The preparation of product 3 according to the method of example 1 is different in that in step 3), the kiln is fired, and when the temperature is programmed to 200-600 ℃, the temperature is programmed to 1400 ± 20 ℃ at 15 ℃/h,20 ℃/h and 25 ℃/h, respectively, and the temperature is maintained for not less than 6-20h. The number of cracks of the product was measured, and the results are shown in table 3.
TABLE 3 test results of products
As can be seen from Table 3, the temperature rise rate is controlled within the range of 200-600 ℃ under the condition that the product composition is fixed, which is beneficial to improving the qualification rate of the product. The reasonable heat preservation time is the main basis for ensuring other performance parameters such as product strength, porosity and the like, and the reasonable production energy consumption is mainly considered.
Claims (1)
1. The preparation method of the large-size high-pressure-bearing thin-wall cordierite honeycomb ceramic carrier is characterized in that the preparation raw material consists of the following components in percentage by weight: 25-42% of talc, 5-10% of non-active alumina, 12-16% of silicon dioxide, 20-30% of kaolin, 5-10% of active alumina, 0.2-0.5% of surfactant, 2-6% of binder and 1-3% of lubricant, wherein the sum of the components is 100%; the method comprises the following specific steps:
1) Mixing talc, inactive alumina, kaolin, active alumina, silicon dioxide and a binder, adding a surfactant for continuous mixing, and finally mixing with a lubricant;
2) Fully pugging in a pug mill;
3) Molding in a molding machine at one time, and controlling the temperature to be not more than 38 ℃;
4) Calcining in a kiln, carrying out temperature programming according to the speed of 15-20 ℃/h to 1400 +/-20 ℃, and carrying out heat preservation for 8-10h;
5) Performing fine grinding size processing and skin grafting to obtain a finished product;
wherein the diameter of the large specification is more than 177mm, the wall thickness of the thin wall is 4mil, the high pressure bearing is that the compressive strength in the A direction is not less than 12MPa, the compressive strength in the B direction is not less than 4MPa, and the compressive strength in the C direction is not less than 0.3MPa;
the grain size of the talc is 6-14 μm, the weight ratio of MgO in the talc is more than 30%, and CaO and K in the talc 2 O and Na 2 The weight ratio of the sum of O is less than 0.5 percent; the particle size range of the inactive alumina is 2-8 μm, and the purity is more than 99%; the particle size range of the silicon dioxide is 2-8 mu m, and the purity is more than 99 percent; the particle size of the kaolin is 1-5 μm, and Al in the kaolin 2 O 3 The weight ratio is more than 35 percent, and the weight ratio of SiO2 is more than 45 percent; in activated alumina, al 2 O 3 Weight ratio is more than 65%, caO + K 2 O+Na 2 The weight ratio of O is less than 0.5 percent, and the specific surface area of the activated alumina is 150-350 m 2 /g。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1197819C (en) * | 1999-09-01 | 2005-04-20 | 康宁股份有限公司 | Fabrication of ultra-thinwall cordierite structures |
| WO2002053512A1 (en) * | 2000-12-29 | 2002-07-11 | Corning Incorporated | Fabrication of ultra-thinwall cordierite structures |
| CN102424569B (en) * | 2011-09-23 | 2013-03-13 | 江苏省宜兴非金属化工机械厂有限公司 | Thermal shock resistant thin-walled cordierite honeycomb ceramics and preparation method thereof |
| CN105777181B (en) * | 2016-03-11 | 2018-08-14 | 江苏省宜兴非金属化工机械厂有限公司 | A kind of big specification cordierite honeycomb ceramic carrier of use for diesel engine |
| CN106045551A (en) * | 2016-05-24 | 2016-10-26 | 南京柯瑞特种陶瓷股份有限公司 | Method for preparing large-diameter thin-wall honeycomb ceramic carrier |
| CN111036187B (en) * | 2019-12-23 | 2021-03-30 | 中国科学院过程工程研究所 | Honeycomb carrier and preparation method and application thereof |
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