CN113387725B - Modified zirconia corundum slurry for honeycomb ceramic heat accumulator surface and pulping method and application thereof - Google Patents
Modified zirconia corundum slurry for honeycomb ceramic heat accumulator surface and pulping method and application thereof Download PDFInfo
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- CN113387725B CN113387725B CN202110733297.2A CN202110733297A CN113387725B CN 113387725 B CN113387725 B CN 113387725B CN 202110733297 A CN202110733297 A CN 202110733297A CN 113387725 B CN113387725 B CN 113387725B
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/87—Ceramics
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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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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/5025—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with ceramic materials
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Abstract
The invention discloses a zirconia-corundum slurry for surface modification of a honeycomb ceramic heat accumulator and a pulping method. The slurry formulation includes at least one dispersant, at least one binder, at least one thickener, and a defoamer. The modified coating formed by dipping and coating the slurry on the surface of the honeycomb ceramic heat accumulator has the advantages of uniform dispersion, high slurry coating rate, tight combination, low shedding rate and excellent slag resistance.
Description
Technical Field
The invention belongs to the technical field of ceramic surface modification, relates to preparation of modified slurry, and particularly relates to modified zirconia-corundum slurry for the surface of a honeycomb ceramic heat accumulator, and a pulping method and application thereof.
Background
The honeycomb ceramic heat accumulator is a heat accumulator with a reasonable structure and high heat exchange efficiency in the heat storage materials used at present, and has the advantages of small honeycomb volume, good heat exchange and energy-saving effects, convenience in realizing automatic control, simple matching equipment and the like, wherein the heat accumulator with a square lattice structure is most widely applied. However, in actual production, the problems of ash accumulation and blockage of the lattice holes of the heat accumulator, melting and deformation of the lattice holes, cracking and crushing of through holes and the like commonly exist, so that the service life of the heat accumulator is short, and the comprehensive use performance of the honeycomb heat accumulator and the energy-saving effect of heat accumulation type combustion are seriously influenced [ Wangfang, et al, 2020; Zhu-Li He, et al,2015 ]. At present, according to the analysis of the damage reason of the heat accumulator and the related reports at home and abroad [ Al-Harbi O A, et Al,2015], the following improvement measures for delaying the damage of the honeycomb heat accumulator and prolonging the service life of the heat accumulator are summarized: (1) the air-fuel ratio is reasonably controlled, the proper atmosphere and temperature in the furnace are ensured, the generation amount of iron oxide scales is reduced as much as possible, and the generation of low-melting-point substances generated by the reaction of the heat accumulator at the high-temperature section and the iron oxide is slowed down, so that the ash accumulation and blockage of the heat accumulator are delayed. (2) The quality control of the coal gas is enhanced, and the dust and water content in the coal gas are reduced; a shaking type ash filtering net is added in the coal gas heat accumulation chamber. (3) And (4) blocking flash seams at the upper part of the honeycomb heat accumulator by using refractory mortar. The refractory slurry mixed with the high-temperature refractory fiber is adopted for plugging, so that the heat storage box can be used for a long time, and the bias flow or short circuit of the heat exchange gas in the heat storage box is avoided. (4) The honeycomb heat accumulators with different materials and specifications are used in the heating furnace segment and the heat accumulation box layer by layer or the high-performance honeycomb heat accumulator is developed. (5) Due to the characteristics of blast furnace gas, the blockage of the heat accumulator and the reduction of the heat storage capacity are almost inevitable, and the heat accumulator is replaced regularly according to the influence degree (production reduction and energy consumption increase) on the production after the heat accumulator is blocked.
The method can solve the problem that the service life of the honeycomb ceramic heat accumulator is influenced by the ash deposition and blockage of the grid holes, the fusion deformation of the grid holes, the cracking and the breakage of the through holes and the like, but the report that the existing product is replaced by the novel honeycomb ceramic heat accumulator with the characteristics of excellent slag resistance, good thermal stability, long service life and the like is almost absent. Therefore, the development of a novel honeycomb ceramic heat accumulator with long service life has important research significance.
Mullite honeycomb ceramic heat accumulator for hot blast stove in metallurgical industry mainly comprises Al2O3And SiO2Because of the existence of the hot blast stove, when the smoke passes through the heat accumulator, FeO and Fe exist in the smoke2O3Easily react with the honeycomb ceramics to generate eutectic substances which are attached to the surfaces of the holes, are easy to block the holes after long-term accumulation, and have shadowService time of sound heat accumulator Chen A N, et al,2019]. In order to solve the problem of short service life caused by the fact that the surface of the honeycomb ceramic heat accumulator is easy to corrode, the invention comprehensively utilizes a dispersing agent, a bonding agent and a thickening agent, and provides a pulping formula and a corresponding coating method for surface modification of the honeycomb ceramic heat accumulator.
Disclosure of Invention
The invention aims to provide a preparation method of modified zirconia-corundum slurry for the surface of a honeycomb ceramic heat accumulator, which has the advantages of excellent rheological property, excellent slag resistance of a modified sample and simple preparation process.
In order to achieve the purpose, the invention adopts the technical scheme that:
1. the composite material comprises the following components in percentage by mass: 30-40% of zirconia corundum micropowder (the grain diameter is less than or equal to 0.074 mu m), 0.1-0.5% of dispersant, 0.5-3% of binder, 1.0-1.6% of thickening agent, 0.1-0.5% of defoamer and the balance of deionized water.
2. The dispersing agent is at least one of high molecular polymer polyacrylamide, polycarboxylate, polyacrylic acid and sodium salt thereof, hydroxymethyl cellulose and polyvinyl alcohol.
3. The binding agent is at least one of high molecular polymer lignosulfonate, sodium tripolyphosphate, sodium hexametaphosphate and ammonium lignosulfonate.
4. The thickener is at least one of water-soluble cellulose methyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose and sodium carboxymethyl cellulose.
5. The modified slurry of claim 1, wherein: the defoaming agent is at least one of polyether and polyether modified silicon defoaming agent.
6. The preparation method of the modified slurry comprises the following steps: (1) uniformly dissolving the organic additive with the formula ratio into deionized water, stirring and heating until the organic additive is completely dissolved to obtain a mixed solution; (2) adding the formula amount of the zirconia-corundum micropowder and the defoamer into the mixed solution in turn, preheating a magnetic stirrer to 30-50 ℃, and stirring for 20-40r/min for 20-40min to prepare the zirconia-corundum slurry; (3) and dipping and coating the slurry on a honeycomb ceramic heat accumulator for surface modification.
7. The method for coating the slurry is characterized in that: the green honeycomb ceramic test piece was dipped in the prepared zirconia corundum slurry, taken out and left to stand, the residual slurry in the pores was removed, repeated 2-5 times, placed in an oven at 80-100 ℃ for drying for 1-3h, and calcined in a laboratory box electric furnace at 1300-1400 ℃ for 1-4 h.
In order to explore the slag resistance of the honeycomb ceramic heat accumulator after the surface modification of the prepared zirconia-corundum slurry, the method comprises the following steps:
(1) processing a sample to be tested into a crucible sample with the external dimension of 60mm multiplied by 90mm and the internal diameter dimension of D30mm multiplied by 40 mm;
(2) adding a proper amount of pre-prepared experimental slag into a crucible sample, placing the crucible sample into a graphite crucible, then placing the crucible into a mullite sagger, and filling graphite powder around the mullite sagger;
(3) the saggars with the samples are put into a box-type resistance furnace in sequence, heated to 1350 ℃ and 1400 ℃ and preserved for 1-3 h.
(4) And cutting the corroded sample along the radial direction, and comparing and analyzing the corrosion resistance of the sample according to the microstructure of the sample after the slag resistance experiment before and after modification.
Compared with the prior art, the invention has the following characteristics:
1. after the zirconia corundum slurry prepared by the invention is used for surface modification of the honeycomb ceramic heat accumulator, the slurry coating rate is 14-20 wt%, the peeling rate of the modified coating is less than 0.08%, the modified coating is compact, the slag resistance of the modified sample is excellent, and the purpose of prolonging the service life of the honeycomb ceramic heat accumulator is easy to realize.
2. The modified slurry is prepared by adopting the zirconia-corundum micro powder as the raw material and adding a small amount of additives which are widely applied in industry, and the modified slurry has rich raw material reserves and low economic cost.
3. The honeycomb ceramic heat accumulator is subjected to surface modification by adopting a simple and easy dip coating method, the whole preparation process is finished at room temperature, heating is not needed, energy is saved, the whole preparation process is very simple and quick, special equipment is not needed, the process repeatability is good, and the large-scale preparation is favorably realized.
The synthesis time is short, and other compounds are not required to be added.
Drawings
FIG. 1 is a rheological chart of a zirconia corundum slurry obtained in example 1 according to an embodiment of the present invention;
FIG. 2 is a scanning electron microscope image of the surface of a sample modified with a zirconia-corundum slurry obtained in example 2 according to an embodiment of the present invention;
FIG. 3 is a scanning electron microscope image of a cross section of a sample modified with a zirconia alumina slurry obtained in example 2 according to an embodiment of the present invention.
Detailed Description
To highlight the implementation objects, technical solutions and structural advantages of the present invention, the following detailed description is made with reference to the accompanying drawings and technical solutions in the examples of the present invention, which are some examples of the present invention, but not all examples. All other examples, which can be obtained by a person skilled in the art without making any creative effort based on the examples in the present invention, belong to the protection scope of the present invention.
The specific implementation mode is as follows:
the present invention will be described in detail with reference to examples.
Example 1
Ball milling and screening the zirconia-corundum micro powder to obtain powder with the particle size less than or equal to 0.074 mu m. The raw materials, the admixture and distilled water were weighed according to the formulation of table 1 and placed in a beaker, the magnetic stirrer was preheated to 30 ℃, stirred at a rotational speed of 30r/min for 30min, and the rheological properties thereof were tested. (FIG. 1: rheological diagram of zirconia corundum slurry of optimum formulation).
Table 1 rheology test sample formulation (wt%)
Example 2
The green honeycomb ceramic sample was immersed in the prepared zirconia corundum slurry, taken out, and left to stand, with the residual slurry in the pores being removed, 2-5 times repeated, and the mass of the sample before and after immersion was measured and recorded as m1 and m2, respectively, and the slurry pick-up was calculated as [ (m2-m1)/m1 ]. 100%. Drying the mixture in an oven at the temperature of 80-100 ℃ for 1-3 h; the dried green test specimens were calcined in a 1300-1400 ℃ laboratory box furnace for 1-4 h. And observing the microstructure of the modified sample surface coating under a scanning electron microscope. (FIG. 2 is a scanning electron microscope image of the surface of a sample after the zirconia corundum slurry is modified; FIG. 3 is a scanning electron microscope image of the cross section of a sample after the zirconia corundum slurry is modified; the slurry coating rate of a green body sample and a product after the zirconia corundum slurry is dipped is shown in Table 2
TABLE 2
Example 3
The mass of the surface-modified calcined sample was measured as M1, the sample was placed in a beaker, distilled water was added to the beaker to the extent that the sample was immersed in the ultrasonic cleaner for 30min, the sample was taken out and dried at 80-100 ℃ for 12-24 h, the mass of the sample was measured as M2, and the peeling ratio of the modified coating was calculated as (M1-M2)/M1: 100%. Table 2: the shedding rate of the green body sample and the product surface modified coating after dipping with the zirconia corundum slurry is shown in table 3 below.
TABLE 3
The zirconia-corundum slurry prepared by the method has the advantages of good rheological property, high slurry hanging rate, rich raw material reserves, low economic cost, simple and quick preparation process, no need of special equipment, good process repeatability and easy realization of large-scale preparation. In addition, the research shows that the slurry coating rate is 14-20 wt% after the zirconia-corundum slurry is dipped and coated on the surface of the honeycomb ceramic heat accumulator for modification, the shedding rate of the modified coating is less than 0.08%, the modified coating is compact, the slag resistance of the modified sample is excellent, the purpose of prolonging the service life of the honeycomb ceramic heat accumulator is easy to realize, and the practicability is wide.
The last statement is: the above detailed description is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. It should be noted that, within the scope of the concept of the present invention, a person skilled in the art may make several changes and modifications, or may make relevant substitutions for some technical features, all of which fall within the scope of the present invention. The scope of protection of the above patent shall be indicated finally by the appended claims: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A zirconia corundum slurry used for surface modification of a honeycomb ceramic heat accumulator is characterized in that: the coating comprises the following components in percentage by mass: 30-40% of corundum-zirconia micropowder, 0.1-0.5% of dispersant, 0.5-3% of binder, 1.0-1.6% of thickener, 0.1-0.5% of defoamer and the balance of deionized water, wherein the grain diameter of the corundum-zirconia micropowder is not more than 0.074 μm.
2. The surface-modified zirconia corundum slurry for honeycomb ceramic heat accumulator of claim 1, wherein: the dispersing agent is at least one of high molecular polymer polyacrylamide, polycarboxylate, polyacrylic acid and sodium salt thereof, hydroxymethyl cellulose and polyvinyl alcohol.
3. The surface-modified zirconia corundum slurry for honeycomb ceramic heat accumulator of claim 1, wherein: the binding agent is at least one of high molecular polymer lignosulfonate, sodium tripolyphosphate and sodium hexametaphosphate.
4. The zirconia corundum slurry for the surface modification of the honeycomb ceramic heat accumulator of claim 1, which is characterized in that: the thickener is at least one of water-soluble cellulose methyl cellulose, hydroxyethyl cellulose, hydroxypropyl methyl cellulose and sodium carboxymethyl cellulose.
5. The zirconia corundum slurry for the surface modification of the honeycomb ceramic heat accumulator of claim 1, which is characterized in that: the defoaming agent is at least one of polyether and polyether modified silicon defoaming agent.
6. A preparation method for preparing the surface modified zirconia corundum slurry for the honeycomb ceramic heat accumulator of any one of claims 1 to 5 is characterized by comprising the following steps: comprises the following steps: (1) uniformly dissolving the dispersant, the binder and the thickener in the formula ratio into deionized water, stirring and heating until the components are completely dissolved to obtain a mixed solution; (2) sequentially adding the zirconia-corundum micro powder and the defoaming agent in the formula ratio into the mixed solution, preheating a magnetic stirrer to 30-50 ℃, and stirring for 20-40min at a speed of 20-40r/min to obtain zirconia-corundum slurry; (3) and dipping and coating the slurry on a honeycomb ceramic heat accumulator for surface modification.
7. The method of claim 6, wherein: dipping the honeycomb ceramic green body sample in the prepared zirconia-corundum slurry, taking out, standing, removing residual slurry in the holes, repeating for 2-5 times, drying in an oven at 80-100 ℃ for 1-3h, and calcining in a 1300-1400 ℃ laboratory box type electric furnace for 1-4 h.
8. The use of the surface-modified zirconia-corundum slurry for honeycomb ceramic heat accumulators according to claim 1, characterized in that: the zirconia corundum slurry is used for surface modification of honeycomb ceramic heat accumulator and is applied to heat accumulator of industrial hot blast stove.
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