CN111018560B - Multi-scale pore honeycomb ceramic and preparation method thereof - Google Patents
Multi-scale pore honeycomb ceramic and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of comprehensive utilization of solid waste resources and the field of preparation of inorganic non-metallic materials, in particular to a multi-scale pore honeycomb ceramic and a preparation method thereof; the raw materials of the multi-scale pore honeycomb ceramic comprise: fly ash, additive and pore-forming agent; the pore-forming agent consists of a foaming agent and a pore-forming agent, wherein the foaming agent is silicon carbide, and the pore-forming agent is nano silicon carbide; the preparation method of the multi-scale pore honeycomb ceramic comprises the following steps: (1) mixing the fly ash, the additive and the pore-making agent, and then performing ball milling, ageing and secondary pugging to obtain pug; (2) extruding and molding the pug by an extruder to obtain a honeycomb ceramic blank; (3) and drying the honeycomb ceramic blank, and sintering. The invention realizes the high-value utilization of the solid waste fly ash, increases the additional value of the fly ash, simultaneously reduces the manufacturing cost of the multi-scale pore honeycomb ceramic and further improves the performance of the multi-scale pore honeycomb ceramic.
Description
Technical Field
The invention relates to the field of comprehensive utilization of solid waste resources and the field of preparation of inorganic non-metallic materials, in particular to a multi-scale pore honeycomb ceramic and a preparation method thereof.
Background
Coal-fired power generation is the most main mode of coal utilization, and at the present stage, coal in a thermal power plant is mainly utilized by spraying pulverized coal as fuel into a boiler for combustion utilization. The temperature in the high-temperature furnace can reach 1200-1600 ℃, pulverized coal is in the high-temperature process, combustible substances are combusted, inorganic components and a small amount of unburned carbon are finally left, due to the existence of high-temperature airflow in the furnace and the suction force of a draught fan on the top of the furnace, after solid components are sequentially treated by a heater, a reheater and an economizer along a pipeline, part of coarse particle dust is deposited, in addition, the rest fine dust powder is collected, and the part of dust is pulverized fuel ash.
The honeycomb ceramic is a novel ceramic product with a structure similar to a honeycomb shape, is used in tail gas purification of small automobiles at first, is widely applied to industries such as chemical industry, electric power, metallurgy, petroleum, electronic and electric appliances, machinery and the like, is more and more extensive, and has considerable development prospect. CN104436868A discloses a honeycomb ceramic, which mainly takes a plate-shaped structure as a main part, and a plurality of filter holes are arranged in the main part, so that the solvent/water filtered by the honeycomb ceramic can be better collected; CN102875128A discloses a fly ash-based heat storage honeycomb ceramic and a preparation method thereof, and particularly provides a honeycomb ceramic prepared from fly ash, a sintering aid, a binder, a plasticizer, a surfactant and water, wherein the addition amount of the fly ash can reach 45%, and the honeycomb ceramic is mainly used in the field of heat storage materials. However, the existing honeycomb ceramics still have many problems such as high preparation cost, shortage of raw materials and limited practical application, and therefore, further research is still needed for the replacement of the raw materials for preparing the honeycomb ceramics and the improvement of the performance.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
In order to solve the technical problems, the invention provides the multi-scale pore honeycomb ceramic, which takes solid waste fly ash as a main raw material, greatly reduces the raw material cost of the honeycomb ceramic, and realizes high-value utilization of the solid waste.
Specifically, the raw materials of the multi-scale pore honeycomb ceramic comprise: fly ash, additive and pore-forming agent; the pore-forming agent consists of a foaming agent and a pore-forming agent, wherein the foaming agent is silicon carbide (SiC), and the pore-forming agent is nano silicon carbide (SiC).
The multi-scale pore honeycomb ceramic taking the fly ash as the main raw material can greatly reduce the cost of the honeycomb ceramic, but also puts higher requirements on other additives in the raw material; the invention discovers that the addition of the pore-forming agent into the raw materials is helpful for obtaining the multi-scale honeycomb ceramic with good performance and shape.
Preferably, the pore-making agent accounts for 1-5% of the total weight of the multi-scale pore honeycomb ceramic; the mass ratio of the foaming agent to the pore-forming agent is 8-10: 1.
preferably, the raw materials comprise the following components in percentage by weight based on the total weight of the multi-scale pore honeycomb ceramic:
60-90% of fly ash
9 to 37 percent of additive
1-5% of a pore-forming agent.
Preferably, the additive comprises clay, feldspar, magnesite.
As a better scheme of the invention, the raw materials comprise the following components in percentage by weight based on the total weight of the multi-scale pore honeycomb ceramic:
the invention takes the fly ash as the main raw material to be compounded with clay, feldspar, magnesite, silicon carbide and nano silicon carbide, thereby realizing the waste utilization of solid waste (fly ash) and preparing the multi-scale pore honeycomb ceramic with excellent performance.
The invention also provides a preparation method of the multi-scale pore honeycomb ceramic, which comprises the following steps:
(1) mixing the fly ash, the additive and the pore-making agent, and then performing ball milling, ageing and secondary pugging to obtain pug;
(2) extruding and molding the pug by an extruder to obtain a honeycomb ceramic blank;
(3) and drying the honeycomb ceramic blank, and sintering.
In order to further optimize the performance of the multi-scale pore honeycomb ceramic, the invention optimizes the process parameters of the preparation method (the optimal technical scheme of the invention can be obtained by combining the optimal schemes), and concretely, the following steps are carried out
Preferably, the extrusion pressure of the extruder is 8-12 MPa.
Preferably, the drying is carried out in a continuous microwave drying in a tunnel microwave oven.
Preferably, the sintering treatment temperature is 1100-1300 ℃, and the time is 1-4 h.
The technological parameters of the preparation method of the multi-scale pore honeycomb ceramic directly influence the performance of a final product, particularly the temperature and time of sintering treatment; sintering under specific conditions, wherein the surface of the prepared multi-scale pore honeycomb ceramic has uniform and consistent large-scale pores (0.2-0.5 cm), and the inside of the prepared multi-scale pore honeycomb ceramic has medium-scale pores (100-500 mu m) and small-scale pores (10-100 nm).
As a preferred scheme of the invention, the preparation method comprises the following steps:
(1) mixing the fly ash, the additive and the pore-making agent, and then performing ball milling, ageing and secondary pugging to obtain pug;
(2) extruding and molding the pug by an extruder under 8-12 MPa to obtain a honeycomb ceramic blank;
(3) and (3) carrying out continuous microwave drying on the honeycomb ceramic blank in a tunnel microwave oven, and sintering at 1100-1300 ℃ for 1-4 h.
The honeycomb ceramic prepared by the preparation method is formed by coupling multi-scale pore structures, so that the performance of the honeycomb ceramic is greatly enhanced, the application range of the honeycomb ceramic is widened, the market competitiveness of honeycomb ceramic products is increased, and the win-win of economic benefits and environmental benefits is realized.
The invention has the beneficial effects that:
(1) the preparation method of the multi-scale pore honeycomb ceramic comprises the steps of mixing and stirring fly ash, an additive and a pore-forming agent according to a certain mass percentage, extruding and molding the obtained pug under a certain pressure to prepare a honeycomb ceramic blank, drying the honeycomb ceramic blank, and sintering at a high temperature under a specific condition to obtain the multi-scale pore honeycomb ceramic; the method adopts a fully-mechanized and fully-automatic control mode, not only can fully utilize the fly ash, but also greatly improves the added value of the fly ash, realizes the recycling of solid wastes, reduces the occupied field resources due to landfill, reduces the raw material cost of the honeycomb ceramics, and relieves the current situation of shortage of ceramic raw materials.
(2) The multi-scale pore honeycomb ceramic has the advantages of high strength, high porosity, multi-scale pore coupling and the like, and can be applied to the fields of sewage treatment, gas purification, catalytic carriers, heat storage materials and the like; meanwhile, the current situations of insufficient utilization of the fly ash and environmental pollution are solved, the popularization in practice is facilitated, and the method has important economic, social and ecological environmental protection significance.
Drawings
FIG. 1 is a schematic view of a multi-scale porous honeycomb ceramic.
Fig. 2 is a sample diagram of a multi-scale pore honeycomb ceramic.
FIG. 3 is a flow chart of a process for preparing a multi-scale porous honeycomb ceramic.
Fig. 4 is a photograph of a multi-scale porous honeycomb ceramic.
Fig. 5 is an SEM image of a multi-scale porous honeycomb ceramic.
Fig. 6 is an SEM image of a multi-scale porous honeycomb ceramic.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
This example provides a multi-scale porous honeycomb ceramic (as shown in fig. 1 and 2), which is prepared from the following raw materials in percentage by weight, based on the total weight of the multi-scale porous honeycomb ceramic:
the preparation method of the multi-scale pore honeycomb ceramic is as follows (as shown in figure 3):
(1) mixing fly ash, clay, feldspar, magnesite, silicon carbide and nano silicon carbide, and then carrying out ball milling, ageing and secondary pugging to obtain pug;
(2) extruding and molding the pug by an extruder under 8Mpa to prepare a honeycomb ceramic blank;
(3) and (3) carrying out continuous microwave drying on the honeycomb ceramic blank in a tunnel microwave oven, and sintering at 1100 ℃ for 4 h.
Example 2
This example provides a multi-scale porous honeycomb ceramic (see fig. 4, 5, and 6), which is prepared from the following raw materials, by weight:
the preparation method of the multi-scale pore honeycomb ceramic is the same as that of the embodiment 1.
The preparation method of the multi-scale pore honeycomb ceramic is as follows (as shown in figure 3):
(1) mixing fly ash, clay, feldspar, magnesite, silicon carbide and nano silicon carbide, and then carrying out ball milling, ageing and secondary pugging to obtain pug;
(2) extruding and molding the pug at 10Mpa by an extruder to obtain a honeycomb ceramic blank;
(3) and (3) carrying out continuous microwave drying on the honeycomb ceramic blank in a tunnel microwave oven, and sintering at 1200 ℃ for 3 h.
Example 3
The embodiment provides a multi-scale pore honeycomb ceramic, which is prepared from the following raw materials in percentage by weight based on the total weight of the multi-scale pore honeycomb ceramic:
the preparation method of the multi-scale pore honeycomb ceramic is the same as that of the embodiment 1.
The preparation method of the multi-scale pore honeycomb ceramic is as follows (as shown in figure 3):
(1) mixing fly ash, clay, feldspar, magnesite, silicon carbide and nano silicon carbide, and then carrying out ball milling, ageing and secondary pugging to obtain pug;
(2) extruding and molding the pug by an extruder under 12Mpa to prepare a honeycomb ceramic blank;
(3) and (3) carrying out continuous microwave drying on the honeycomb ceramic blank in a tunnel microwave oven, and sintering at 1300 ℃ for 1 h.
Comparative example 1
This comparative example provides a multi-scale porous honeycomb ceramic differing from example 1 only in that: based on the total weight of the multi-scale pore honeycomb ceramic, the raw materials comprise the following components in percentage by weight:
comparative example 2
This comparative example provides a multi-scale porous honeycomb ceramic differing from example 1 only in that: the silicon carbide is replaced by calcium carbonate, and the nano silicon carbide is replaced by nano calcium carbonate.
Comparative example 3
This comparative example provides a multi-scale porous honeycomb ceramic differing from example 1 only in that: the preparation method comprises the step (3) of sintering treatment at 1000 ℃ for 4 hours.
Test example 1
The test example detects the multi-scale pore honeycomb ceramics obtained in the examples 1-3 and the comparative examples 1-3, and the results are shown in table 1;
table 1 detection and analysis results of multi-scale pore honeycomb ceramics obtained in examples 1 to 3 and comparative examples 1 to 3
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (6)
2. the method of making the multi-scale porous honeycomb ceramic of claim 1, comprising the steps of:
(1) mixing the fly ash, the additive and the pore-making agent, and then performing ball milling, ageing and secondary pugging to obtain pug; the additives are clay, feldspar and magnesite; the pore-making agent is silicon carbide and nano silicon carbide;
(2) extruding and molding the pug by an extruder to obtain a honeycomb ceramic blank;
(3) and drying the honeycomb ceramic blank, and sintering.
3. The method according to claim 2, wherein the extruder has an extrusion pressure of 8 to 12 MPa.
4. The method of claim 2, wherein the drying is performed in a continuous microwave drying in a tunnel microwave oven.
5. The preparation method according to claim 2, wherein the sintering treatment is carried out at 1100-1300 ℃ for 1-4 h.
6. The method according to any one of claims 2 to 5, comprising the steps of:
(1) mixing the fly ash, the additive and the pore-making agent, and then performing ball milling, ageing and secondary pugging to obtain pug; the additives are clay, feldspar and magnesite; the pore-making agent is silicon carbide and nano silicon carbide;
(2) extruding and molding the pug by an extruder under 8-12 MPa to obtain a honeycomb ceramic blank;
(3) and (3) carrying out continuous microwave drying on the honeycomb ceramic blank in a tunnel microwave oven, and sintering at 1100-1300 ℃ for 1-4 h.
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DE3314796A1 (en) * | 1983-04-23 | 1984-10-25 | Mayer-Reiland, geb.Reiland, Eva-Maria, 6710 Frankenthal | Premix for the preparation of high-melting foam ceramic, and process for the preparation thereof |
CN106747316A (en) * | 2016-11-21 | 2017-05-31 | 武汉理工大学 | A kind of method that utilization flyash and shale prepare thermo store honeycomb ceramic |
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DE3314796A1 (en) * | 1983-04-23 | 1984-10-25 | Mayer-Reiland, geb.Reiland, Eva-Maria, 6710 Frankenthal | Premix for the preparation of high-melting foam ceramic, and process for the preparation thereof |
CN106747316A (en) * | 2016-11-21 | 2017-05-31 | 武汉理工大学 | A kind of method that utilization flyash and shale prepare thermo store honeycomb ceramic |
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