CN112624776A - Zirconia-alumina fiber composite wet module and preparation method thereof - Google Patents

Zirconia-alumina fiber composite wet module and preparation method thereof Download PDF

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CN112624776A
CN112624776A CN202011554161.7A CN202011554161A CN112624776A CN 112624776 A CN112624776 A CN 112624776A CN 202011554161 A CN202011554161 A CN 202011554161A CN 112624776 A CN112624776 A CN 112624776A
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fiber
zirconia
slurry
alumina
mass ratio
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CN112624776B (en
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傅超
徐营
邢桃芬
赵瑞禄
鹿明
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Shandong Luyang Hot High Technology Ceramic Fiber Co
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Shandong Luyang Hot High Technology Ceramic Fiber Co
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    • 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
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Abstract

The invention provides a zirconia-alumina fiber composite wet module and a preparation method thereof. In the preparation method provided by the invention, alumina fiber is dispersed to form fiber dispersion liquid, and then the fiber dispersion liquid is mixed with certain inorganic binder, alum solution and flocculating agent to obtain alumina fiber slurry; carrying out the same treatment on the zirconia fiber to form zirconia fiber slurry; and then sequentially injecting the two kinds of slurry into a forming die for forming, and then drying to obtain the alumina-zirconia composite fiber module. The preparation method can effectively improve the heat insulation property of the material, the heated integrity of the material shape and the strength after firing.

Description

Zirconia-alumina fiber composite wet module and preparation method thereof
Technical Field
The invention relates to the field of heat insulation materials, in particular to a zirconia-alumina fiber composite wet module and a preparation method thereof.
Background
In the field of ultrahigh temperature, the temperature-resistant, heat-insulating and energy-saving material is always an important factor influencing and even restricting the development of the field. Most of the heat insulating layers applied at ultrahigh temperature are large-density rigid products pressed by ceramic powder or particles, but the heat insulating performance is limited to a certain extent due to large density and large heat capacity of the heat insulating layers.
The zirconia fiber has good heat insulation performance, and particularly can be used for manufacturing ultra-high temperature industrial kilns, ultra-high temperature experimental electric furnaces, other ultra-high temperature heating devices and the like with the temperature of more than 1500 ℃ to 2200 ℃, and is used in various industrial and scientific research fields such as ceramic sintering, metal smelting, pyrolysis, semiconductor manufacturing, quartz melting, crystal growth, experimental research and the like. The ultra-high temperature industrial kiln at above 1500 ℃ up to 2200 ℃ needs a high temperature resistant light module to replace the heavy mullite brick. Zirconia fiber modules are the preferred product.
However, in the process of manufacturing a fiber module using zirconia fibers, it is difficult to achieve the heat insulation, heat shrinkage, strength after firing, and other properties of the fiber module due to various influences of raw materials, processes, and the like.
Disclosure of Invention
In view of the above, the present invention provides a zirconia-alumina fiber composite wet module and a method for preparing the same. The composite fiber module prepared by the invention can effectively improve the heat insulation property of the material, the heated integrity of the material form and the strength after firing.
The invention provides a preparation method of a zirconia-alumina fiber composite wet module, which comprises the following steps:
a) mixing alumina fiber, water and a dispersing agent to obtain alumina fiber dispersion liquid;
mixing the alumina fiber dispersion liquid with an inorganic binder, an alum solution and a flocculating agent to obtain alumina fiber slurry;
b) mixing zirconia fiber, water and a dispersing agent to obtain zirconia fiber dispersion liquid;
mixing the zirconia fiber dispersion liquid with an inorganic binder, an alum solution and a flocculating agent to obtain zirconia fiber slurry;
c) injecting the bottom layer fiber slurry into a forming mold, carrying out vacuum suction filtration, then injecting the upper layer fiber slurry, and carrying out vacuum suction filtration to obtain a composite wet blank;
d) drying the composite wet blank to obtain a zirconium oxide-aluminum oxide fiber composite wet module;
the bottom layer fiber slurry is the alumina fiber slurry obtained in the step a), and the upper layer fiber slurry is the zirconia fiber slurry obtained in the step b);
or
The bottom layer fiber slurry is the zirconia fiber slurry obtained in the step b), and the upper layer fiber slurry is the alumina fiber slurry obtained in the step a);
the step a) and the step b) are not limited in order.
Preferably, the alumina fiber has the following specifications: the fiber diameter is 4-6 μm, and the crystal phase is mullite crystal phase; the fiber index is more than or equal to 70 percent, the fiber length is 200-500 mu m, and the slag ball content with the length more than 212 mu m is less than or equal to 0.10wt percent;
the specifications of the zirconia fiber are as follows: the diameter of the fiber is 3-5 μm, the index of the fiber is more than or equal to 70%, the length of the fiber is 100-300 μm, and the content of slag balls with the length more than 212 μm is less than or equal to 0.15 wt%.
Preferably, the inorganic binder is low-sodium silica sol;
the specification of the low-sodium silica sol is as follows: the content of sodium oxide is less than 0.1%, the granularity is 10-20 nm, the solid content is 20-30%, and the pH value is 8-9;
in the step a), the mass ratio of the inorganic bonding agent to the alumina fiber is 3-6%;
in the step b), the mass ratio of the inorganic binder to the zirconia fiber is 5-10%.
Preferably, the mass concentration of the alum solution in the step a) and the mass concentration of the alum solution in the step b) are respectively and independently 5-15%;
the mass ratio of the alum in the alum solution in the step a) and the solid content in the inorganic binder in the step b) is respectively and independently 1: 9-15.
Preferably, the dispersant is epichlorohydrin;
in the step a), the mass ratio of the dispersing agent to the alumina fiber is 0.1-0.5%;
in the step a), the mass ratio of the dispersing agent to the zirconia fiber is 0.1-0.4%.
Preferably, the flocculant is a cationic amide;
in the step a), the mass ratio of the flocculating agent to the alumina fiber is 0.2-0.3%;
in the step b), the mass ratio of the flocculating agent to the zirconia fiber is 0.2-0.3%.
Preferably, in the step a), the mass ratio of the alumina fiber to the water is 5-20%;
in the step b), the mass ratio of the zirconia fiber to the water is 5-20%.
Preferably, in the step c), the conditions for vacuum suction filtering of the bottom layer fiber slurry are as follows: the vacuum degree is 0.04-0.075 MPa, and the pressure is 0-0.2 MPa;
the conditions for vacuum suction filtration of the upper fiber pulp are as follows: the vacuum degree is 0.08-0.095 MPa, and the pressure is 1-4 MPa;
the thickness ratio of a bottom layer wet fiber blank formed after the bottom layer fiber slurry is subjected to vacuum suction filtration to an upper layer wet fiber blank obtained after the upper layer fiber slurry is subjected to vacuum suction filtration is (0.8-2) to 1.
Preferably, in the step d), the drying temperature is 105-150 ℃ and the drying time is 4-10 h.
The invention also provides a zirconia-alumina fiber composite wet module prepared by the preparation method in the technical scheme.
In the preparation method provided by the invention, alumina fiber is dispersed to form fiber dispersion liquid, and then the fiber dispersion liquid is mixed with certain inorganic binder, alum solution and flocculating agent to obtain alumina fiber slurry; carrying out the same treatment on the zirconia fiber to form zirconia fiber slurry; and then sequentially injecting the two kinds of slurry into a forming die for forming, and then drying to obtain the alumina-zirconia composite fiber module. The preparation method can effectively improve the heat insulation property of the material, the heated integrity of the material shape and the strength after firing.
The experimental result shows that after the temperature is 1800 ℃, the back temperature of the composite module is below 85 ℃, and the composite module shows good heat insulation performance; meanwhile, the heated surface is kept intact without shrinkage after heating; the compressive strength before firing is more than 0.160MPa, the compressive strength after firing reaches more than 0.170MPa, and the high-temperature-resistant high-strength concrete has good compressive mechanical properties.
Detailed Description
The invention provides a preparation method of a zirconia-alumina fiber composite wet module, which comprises the following steps:
a) mixing alumina fiber, water and a dispersing agent to obtain alumina fiber dispersion liquid;
mixing the alumina fiber dispersion liquid with an inorganic binder, an alum solution and a flocculating agent to obtain alumina fiber slurry;
b) mixing zirconia fiber, water and a dispersing agent to obtain zirconia fiber dispersion liquid;
mixing the zirconia fiber dispersion liquid with an inorganic binder, an alum solution and a flocculating agent to obtain zirconia fiber slurry;
c) injecting the bottom layer fiber slurry into a forming mold, carrying out vacuum suction filtration, then injecting the upper layer fiber slurry, and carrying out vacuum suction filtration to obtain a composite wet blank;
d) drying the composite wet blank to obtain a zirconium oxide-aluminum oxide fiber composite wet module;
the bottom layer fiber slurry is the alumina fiber slurry obtained in the step a), and the upper layer fiber slurry is the zirconia fiber slurry obtained in the step b);
or
The bottom layer fiber slurry is the zirconia fiber slurry obtained in the step b), and the upper layer fiber slurry is the alumina fiber slurry obtained in the step a);
the step a) and the step b) are not limited in order.
In the preparation method provided by the invention, alumina fiber is dispersed to form fiber dispersion liquid, and then the fiber dispersion liquid is mixed with certain inorganic binder, alum solution and flocculating agent to obtain alumina fiber slurry; carrying out the same treatment on the zirconia fiber to form zirconia fiber slurry; and then sequentially injecting the two kinds of slurry into a forming die for forming, and then drying to obtain the alumina-zirconia composite fiber module. The preparation method can effectively improve the heat insulation property of the material, the heated integrity of the material shape and the strength after firing.
With respect to step a): mixing alumina fiber, water and a dispersing agent to obtain alumina fiber dispersion liquid; and mixing the alumina fiber dispersion liquid with an inorganic binder, an alum solution and a flocculating agent to obtain alumina fiber slurry.
In the present invention, the diameter of the alumina fiber is preferably 4 to 6 μm. The crystalline phase of the alumina fiber is a mullite crystalline phase. In the present invention, the alumina fiber is preferably pretreated before the mixing. The pretreatment includes breaking up and deslagging. The fiber index of the alumina fiber is more than or equal to 70 percent through pretreatment, the fiber length is 200-500 mu m, and the slag ball content with the length more than 212 mu m is less than or equal to 0.10wt percent.
In the invention, the mass ratio of the alumina fiber to the water is preferably 5-20%; in some embodiments of the invention, the mass ratio is 5% or 20%.
In the present invention, the dispersant is preferably epichlorohydrin. In the present invention, the mass ratio of the dispersant to the alumina fiber is preferably 0.1% to 0.5%. The mixing mode is not particularly limited, and the materials can be uniformly mixed and dispersed. After mixing, the alumina fiber dispersion liquid is obtained.
In the present invention, the inorganic binder is preferably a low sodium silica sol (NaO content < 0.1%). The specification types of the low-sodium silica sol are preferably as follows: sodium oxide content less than 0.1%, particle size of 10-20 nm, SiO2The solid content is 20-30% (preferably 30%), and the pH is 8-9. The low-sodium silica sol is adopted, the sodium content is low, the low co-melting is not facilitated, the higher use temperature working condition is facilitated, the damage of the proper pH value to the fiber strength is small, and the strength performance of the product after high-temperature burning is facilitated to be ensured.
In the present invention, preferably, the mass ratio of the inorganic binder to the alumina fiber is preferably 3% to 6%; in some embodiments of the invention, the mass ratio is 3% or 5%.
In the invention, the mass ratio of the alum in the alum solution to the solid content in the inorganic binder is preferably 1 to (9-15); in some embodiments of the invention, the mass ratio is 1: 10 or 1: 15. In the present invention, the alum solution is an alum aqueous solution, and the mass concentration of the alum solution is preferably 5% to 15%.
In the present invention, the flocculant is preferably a cationic amide; in some embodiments of the invention, the flocculant is a cationic amide model TPCP1040, offered by Ketao Environment. In the present invention, the mass ratio of the flocculant to the alumina fiber is preferably 0.2% to 0.3%.
In the present invention, the mixing sequence in the above steps is preferably: firstly, mixing the alumina fiber dispersion liquid with the inorganic binder and the alum solution, and then adding the flocculating agent for flocculation to obtain the fiber slurry. More preferably, the inorganic binder and the alum solution are sequentially added to the alumina fiber dispersion liquid to be mixed, and finally, the flocculant is added to perform flocculation, thereby obtaining the fiber slurry. The temperature of the mixing is not particularly limited, and the mixing can be carried out at room temperature, and specifically can be 7-37 ℃. And mixing to obtain the alumina fiber slurry.
With respect to step b): mixing zirconia fiber, water and a dispersing agent to obtain zirconia fiber dispersion liquid; and mixing the zirconium oxide fiber dispersion liquid with an inorganic binder, an alum solution and a flocculating agent to obtain zirconium oxide fiber slurry.
In the present invention, the diameter of the zirconia fiber is preferably 3 to 5 μm. In the present invention, the zirconia fiber is preferably pretreated before the mixing. The pretreatment includes breaking up and deslagging. Through pretreatment, the fiber index of the zirconia fiber is more than or equal to 70 percent, the fiber length is 100-300 mu m, and the slag ball content with the length more than 212 mu m is less than or equal to 0.15 percent by weight.
In the invention, the mass ratio of the zirconia fiber to water is preferably 5-20%; in some embodiments of the invention, the mass ratio is 5% or 20%.
In the present invention, the dispersant is preferably epichlorohydrin. In the present invention, the mass ratio of the dispersant to the zirconia fiber is preferably 0.1% to 0.4%. The mixing mode is not particularly limited, and the materials can be uniformly mixed and dispersed. After mixing, a zirconia fiber dispersion is obtained.
In the present invention, the inorganic binder is preferably a low sodium silica sol (NaO content < 0.1%). The specification types of the low-sodium silica sol are preferably as follows: sodium oxide content less than 0.1%, particle size of 10-20 nm, SiO2The solid content is 20-30% (preferably 30%), and the pH is 8-9. The low-sodium silica sol is adopted, the sodium content is low, the low co-melting is not facilitated, the higher use temperature working condition is facilitated, the damage of the proper pH value to the fiber strength is small, and the strength performance of the product after high-temperature burning is facilitated to be ensured.
In the present invention, preferably, the mass ratio of the inorganic binder to the zirconia fiber is preferably 5% to 10%; in some embodiments of the invention, the mass ratio is 5.5% or 10%.
In the invention, the mass ratio of the alum in the alum solution to the solid content in the inorganic binder is preferably 1 to (9-15); in some embodiments of the invention, the mass ratio is 1: 10 or 1: 15. In the present invention, the alum solution is an alum aqueous solution, and the mass concentration of the alum solution is preferably 5% to 15%.
In the present invention, the flocculant is preferably a cationic amide; in some embodiments of the invention, the flocculant is a cationic amide model TPCP1040, offered by Ketao Environment. In the present invention, the mass ratio of the flocculant to the zirconia fiber is preferably 0.2% to 0.3%.
In the present invention, the mixing sequence in the above steps is preferably: firstly, mixing the zirconium oxide fiber dispersion liquid with an inorganic binder and an alum solution, and then adding a flocculating agent for flocculation to obtain fiber slurry. More preferably, an inorganic binder and an alum solution are sequentially added to the zirconia fiber dispersion liquid to be mixed, and finally, a flocculant is added to perform flocculation, thereby obtaining a fiber slurry. The temperature of the mixing is not particularly limited, and the mixing can be carried out at room temperature, and specifically can be 7-37 ℃. And mixing to obtain zirconia fiber slurry.
The present invention is not particularly limited to the order of the above-mentioned step a) and step b).
With respect to step c): and injecting the bottom layer fiber slurry into a forming mold, carrying out vacuum suction filtration, then injecting the upper layer fiber slurry, and carrying out vacuum suction filtration to obtain a composite wet blank.
In the invention, the bottom layer fiber slurry is the alumina fiber slurry obtained in the step a), and the upper layer fiber slurry is the zirconia fiber slurry obtained in the step b); or, the bottom layer fiber slurry is the zirconia fiber slurry obtained in the step b), and the upper layer fiber slurry is the alumina fiber slurry obtained in the step a). The alumina fiber slurry can be injected first and then the zirconia fiber slurry, or the zirconia fiber slurry can be injected first and then the alumina fiber slurry.
In the present invention, the conditions for vacuum suction filtration of the bottom layer fiber slurry are preferably as follows: the vacuum degree is 0.04-0.075 MPa, and the pressure is 0-0.2 MPa. The conditions for vacuum suction filtration of the upper layer fiber slurry are preferably as follows: the vacuum degree is 0.08-0.095 MPa, and the pressure is 1-4 MPa. The invention controls the vacuum suction filtration pressure of the bottom layer slurry to be smaller than that of the upper layer slurry, thereby preventing the over-compact combination of the bottom layer slurry and being not beneficial to the suction filtration combination of the upper layer slurry and the combination between the two layers of slurry during the secondary suction filtration.
In the invention, the thickness ratio of the bottom layer wet fiber blank formed after the bottom layer fiber slurry is subjected to vacuum suction filtration to the upper layer wet fiber blank obtained after the upper layer fiber slurry is subjected to vacuum suction filtration is preferably (0.8-2) to 1. Through the treatment, the composite wet blank formed by combining the alumina wet blank and the zirconia wet blank is obtained.
With respect to step d): and drying the composite wet blank to obtain the zirconia-alumina fiber composite wet module.
In the invention, the drying temperature is preferably 105-150 ℃, and the drying time is preferablyPreferably 4-10 h. In the present invention, after the drying, it is preferable to further perform cutting to obtain a zirconia-alumina fiber composite module having a predetermined size. In the present invention, the specification of the composite module is preferably: a bulk density of 200 to 500kg/m3The thickness is 200 to 500 mm.
The invention also provides a zirconia-alumina fiber composite wet module prepared by the preparation method in the technical scheme.
Compared with the prior art, the zirconia-alumina fiber composite wet module prepared by the invention has the following beneficial effects:
1. roasting is not needed in the preparation process, and a specific binding agent and other materials are introduced in the pulping process, so that the product has higher strength after roasting in the using process.
2. The invention cuts the fiber by a wet process, screens out the fiber with proper length, prepares the fiber into a wet composite module, and is beneficial to improving the heat insulation performance of the module compared with a dry needling re-extrusion module.
3. The requirement of the ultrahigh-temperature furnace lining material is met, the weight is light, and the heat preservation and insulation effect is better.
4. The fiber blanket is formed in one step, the fiber blanket product does not need to be extruded for the second time, a protection sheet is not used for clamping, and the installation is convenient.
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In the following examples, the alumina fiber is a mullite crystal phase with a diameter of 4 to 6 μm. The diameter of the zirconia fiber is 3-5 μm. The specification of the low-sodium silica sol is as follows: the content of sodium oxide is less than 0.1%, the granularity is 10-20 nm, the solid content is 30%, and the pH value is 8-9. The flocculant is an environmentally friendly TPCP1040 cationic amide.
Example 1
S1 preparation of alumina fiber slurry
Crushing and deslagging the alumina fiber; the pretreated fiber is obtained, the fiber index is 75 percent, the fiber length is 250 mu m, and the slag ball content of the fiber length more than 212 mu m is 0.089 percent.
And adding the pretreated fibers into clear water for dispersion, adding a dispersant epichlorohydrin, and uniformly mixing to obtain an alumina fiber dispersion liquid. Wherein the mass ratio of the alumina fiber to the water is 5%, and the mass ratio of the dispersant to the alumina fiber is 0.15%.
And sequentially adding the low-sodium silica sol and the alum solution into the alumina fiber dispersion liquid, and uniformly mixing. Wherein, the low-sodium silica sol accounts for 5 percent of the mass of the alumina fiber; the concentration of alum solution is 10%, wherein the alum and SiO in the low-sodium silica sol2The mass ratio of the solids is 1: 10.
And adding cationic amide accounting for 0.25 percent of the mass of the alumina fiber into the system for flocculation to obtain alumina fiber slurry.
S2 preparation of zirconia fiber slurry
Crushing and deslagging the zirconia fiber; the pretreated fiber is obtained, the fiber index is 72 percent, the fiber length is 180 mu m, and the slag ball content of the fiber length more than 212 mu m is 0.092 percent.
And adding the pretreated fiber into clear water for dispersion, adding a dispersant epichlorohydrin, and uniformly mixing to obtain a zirconium oxide fiber dispersion liquid. Wherein the mass ratio of the zirconia fiber to the water is 5%, and the mass ratio of the dispersant to the zirconia fiber is 0.15%.
And sequentially adding the low-sodium silica sol and the alum solution into the zirconium oxide fiber dispersion liquid, and uniformly mixing. Wherein, the using amount of the low-sodium silica sol accounts for 5.5 percent of the mass of the zirconia fiber; the concentration of alum solution is 10%, wherein the alum and SiO in the low-sodium silica sol2The mass ratio of the solids is 1: 10.
And adding cationic amide accounting for 0.25 percent of the mass of the zirconia fiber into the system for flocculation to obtain zirconia fiber slurry.
S3, molding
Injecting the alumina fiber slurry into a forming mold, and performing vacuum suction filtration, wherein the vacuum degree is 0.09MPa, and the pressure is 0.2 MPa; and injecting the zirconia slurry into a forming die, locating the zirconia slurry on the upper layer of the alumina slurry, and performing vacuum suction filtration, wherein the vacuum degree is 0.095MPa, and the pressure is 2 MPa. After vacuum suction filtration and pressing, the thickness of the zirconia fiber layer to the alumina fiber layer was 1 (300 kg/m calculated according to the size of the mold)3Material addition of volume weight product).
S4, drying
And drying the obtained module at 120 ℃ for 6 h. Then, the cut product was made to the following specifications: a volume weight of 300kg/m3And the dimensions are 300mm by 300 mm.
Example 2
S1 preparation of alumina fiber slurry
Crushing and deslagging the alumina fiber; the pretreated fiber is obtained, the fiber index is 75 percent, the fiber length is 250 mu m, and the slag ball content of the fiber length more than 212 mu m is 0.089 percent.
And adding the pretreated fibers into clear water for dispersion, adding a dispersant epichlorohydrin, and uniformly mixing to obtain an alumina fiber dispersion liquid. Wherein the mass ratio of the alumina fiber to the water is 5%, and the mass ratio of the dispersant to the alumina fiber is 0.15%.
And sequentially adding the low-sodium silica sol and the alum solution into the alumina fiber dispersion liquid, and uniformly mixing. Wherein, the low-sodium silica sol accounts for 5 percent of the mass of the alumina fiber; the concentration of alum solution is 10%, wherein the alum and SiO in the low-sodium silica sol2The mass ratio of the solids is 1: 10.
And adding cationic amide accounting for 0.25 percent of the mass of the alumina fiber into the system for flocculation to obtain alumina fiber slurry.
S2 preparation of zirconia fiber slurry
Crushing and deslagging the zirconia fiber; the pretreated fiber is obtained, the fiber index is 72 percent, the fiber length is 180 mu m, and the slag ball content of the fiber length more than 212 mu m is 0.092 percent.
And adding the pretreated fiber into clear water for dispersion, adding a dispersant epichlorohydrin, and uniformly mixing to obtain a zirconium oxide fiber dispersion liquid. Wherein the mass ratio of the zirconia fiber to the water is 5%, and the mass ratio of the dispersant to the zirconia fiber is 0.15%.
And sequentially adding the low-sodium silica sol and the alum solution into the zirconium oxide fiber dispersion liquid, and uniformly mixing. Wherein, the using amount of the low-sodium silica sol accounts for 5.5 percent of the mass of the zirconia fiber; the concentration of alum solution is 10%, wherein the alum and SiO in the low-sodium silica sol2The mass ratio of the solids is 1: 10.
And adding cationic amide accounting for 0.25 percent of the mass of the zirconia fiber into the system for flocculation to obtain zirconia fiber slurry.
S3, molding
Injecting the alumina fiber slurry into a forming mold, and performing vacuum suction filtration, wherein the vacuum degree is 0.09MPa, and the pressure is 0.2 MPa; and injecting the zirconia slurry into a forming die, locating the zirconia slurry on the upper layer of the alumina slurry, and performing vacuum suction filtration, wherein the vacuum degree is 0.095MPa, and the pressure is 2 MPa. After vacuum suction filtration and pressing, the thickness of the zirconia fiber layer to the alumina fiber layer was 2 (300 kg/m calculated according to the size of the mold)3Material addition of volume weight product).
S4, drying
And drying the obtained module at 120 ℃ for 6 h. Then, the cut product was made to the following specifications: a volume weight of 300kg/m3And the dimensions are 300mm by 300 mm.
Example 3
S1 preparation of alumina fiber slurry
Crushing and deslagging the alumina fiber; the pretreated fiber is obtained, the fiber index is 75 percent, the fiber length is 250 mu m, and the slag ball content of the fiber length more than 212 mu m is 0.089 percent.
And adding the pretreated fibers into clear water for dispersion, adding a dispersant epichlorohydrin, and uniformly mixing to obtain an alumina fiber dispersion liquid. Wherein the mass ratio of the alumina fiber to the water is 20%, and the mass ratio of the dispersant to the alumina fiber is 0.5%.
And sequentially adding the low-sodium silica sol and the alum solution into the alumina fiber dispersion liquid, and uniformly mixing. Among them, low sodium siliconThe amount of the sol accounts for 3 percent of the mass of the alumina fiber; the concentration of alum solution is 10%, wherein the alum and SiO in the low-sodium silica sol2The mass ratio of the solids is 1: 15.
And adding cationic amide accounting for 0.25 percent of the mass of the alumina fiber into the system for flocculation to obtain alumina fiber slurry.
S2 preparation of zirconia fiber slurry
Crushing and deslagging the zirconia fiber; the pretreated fiber is obtained, the fiber index is 72 percent, the fiber length is 180 mu m, and the slag ball content of the fiber length more than 212 mu m is 0.092 percent.
And adding the pretreated fiber into clear water for dispersion, adding a dispersant epichlorohydrin, and uniformly mixing to obtain a zirconium oxide fiber dispersion liquid. Wherein the mass ratio of the zirconia fiber to the water is 20%, and the mass ratio of the dispersant to the zirconia fiber is 0.4%.
And sequentially adding the low-sodium silica sol and the alum solution into the zirconium oxide fiber dispersion liquid, and uniformly mixing. Wherein the low-sodium silica sol accounts for 10% of the mass of the zirconia fiber; the concentration of alum solution is 10%, wherein the alum and SiO in the low-sodium silica sol2The mass ratio of the solids is 1: 15.
And adding cationic amide accounting for 0.25 percent of the mass of the zirconia fiber into the system for flocculation to obtain zirconia fiber slurry.
S3, molding
Injecting the alumina fiber slurry into a forming mold, and performing vacuum suction filtration, wherein the vacuum degree is 0.09MPa, and the pressure is 0.2 MPa; and injecting the zirconia slurry into a forming die, locating the zirconia slurry on the upper layer of the alumina slurry, and performing vacuum suction filtration, wherein the vacuum degree is 0.095MPa, and the pressure is 2 MPa. After vacuum suction filtration and pressing, the thickness of the zirconia fiber layer to the alumina fiber layer was 1 (300 kg/m calculated according to the size of the mold)3Material addition of volume weight product).
S4, drying
And drying the obtained module at 120 ℃ for 6 h. Then, the cut product was made to the following specifications: a volume weight of 300kg/m3And the dimensions are 300mm by 300 mm.
Comparative example 1
The procedure of example 1 was followed, except that the zirconia fiber layer was not prepared, and only an alumina fiber module was formed. The specific process is as follows:
s1 preparation of alumina fiber slurry
Crushing and deslagging the alumina fiber; the pretreated fiber is obtained, the fiber index is 75 percent, the fiber length is 250 mu m, and the slag ball content of the fiber length more than 212 mu m is 0.089 percent.
And adding the pretreated fibers into clear water for dispersion, adding a dispersant epichlorohydrin, and uniformly mixing to obtain an alumina fiber dispersion liquid. Wherein the mass ratio of the alumina fiber to the water is 5%, and the mass ratio of the dispersant to the alumina fiber is 0.15%.
And sequentially adding the low-sodium silica sol and the alum solution into the alumina fiber dispersion liquid, and uniformly mixing. Wherein, the low-sodium silica sol accounts for 5 percent of the mass of the alumina fiber; the concentration of alum solution is 10%, wherein the alum and SiO in the low-sodium silica sol2The mass ratio of the solids is 1: 10.
And adding cationic amide accounting for 0.25 percent of the mass of the alumina fiber into the system for flocculation to obtain alumina fiber slurry.
S3, molding
Injecting the alumina fiber slurry into a forming mold, and performing vacuum suction filtration, wherein the vacuum degree is 0.09MPa, and the pressure is 2MPa (calculated according to the size of the mold, 300 kg/m)3Material addition of volume weight product).
S4, drying
And drying the obtained module at 120 ℃ for 6 h. Then, the cut product was made to the following specifications: a volume weight of 300kg/m3And the dimensions are 300mm by 300 mm.
Comparative example 2
The procedure of example 1 was followed except that the index of the two fibers was changed. The specific process is as follows:
s1 preparation of alumina fiber slurry
Crushing and deslagging the alumina fiber; the pretreated fiber is obtained, the fiber index is 65%, the fiber length is 550 mu m, and the slag ball content of the fiber length larger than 212 mu m is 0.15%.
And adding the pretreated fibers into clear water for dispersion, adding a dispersant epichlorohydrin, and uniformly mixing to obtain an alumina fiber dispersion liquid. Wherein the mass ratio of the alumina fiber to the water is 5%, and the mass ratio of the dispersant to the alumina fiber is 0.15%.
And sequentially adding the low-sodium silica sol and the alum solution into the alumina fiber dispersion liquid, and uniformly mixing. Wherein, the low-sodium silica sol accounts for 5 percent of the mass of the alumina fiber; the concentration of alum solution is 10%, wherein the alum and SiO in the low-sodium silica sol2The mass ratio of the solids is 1: 10.
And adding cationic amide accounting for 0.25 percent of the mass of the alumina fiber into the system for flocculation to obtain alumina fiber slurry.
S2 preparation of zirconia fiber slurry
Crushing and deslagging the zirconia fiber; the pretreated fiber is obtained, the fiber index is 60 percent, the fiber length is 90 mu m, and the slag ball content with the length more than 212 mu m is 0.12 percent.
And adding the pretreated fiber into clear water for dispersion, adding a dispersant epichlorohydrin, and uniformly mixing to obtain a zirconium oxide fiber dispersion liquid. Wherein the mass ratio of the zirconia fiber to the water is 5%, and the mass ratio of the dispersant to the zirconia fiber is 0.15%.
And sequentially adding the low-sodium silica sol and the alum solution into the zirconium oxide fiber dispersion liquid, and uniformly mixing. Wherein, the using amount of the low-sodium silica sol accounts for 5.5 percent of the mass of the zirconia fiber; the concentration of alum solution is 10%, wherein the alum and SiO in the low-sodium silica sol2The mass ratio of the solids is 1: 10.
And adding cationic amide accounting for 0.25 percent of the mass of the zirconia fiber into the system for flocculation to obtain zirconia fiber slurry.
S3, molding
Injecting the alumina fiber slurry into a forming mold, and performing vacuum suction filtration, wherein the vacuum degree is 0.09MPa, and the pressure is 0.2 MPa; then injecting the zirconia slurry into a forming die, and positioning the forming die on the upper layer of the alumina slurry for processingVacuum suction filtration is carried out, the vacuum degree is 0.095MPa, and the pressure is 2 MPa. After vacuum suction filtration and pressing, the thickness of the zirconia fiber layer to the alumina fiber layer was 1 (300 kg/m calculated according to the size of the mold)3Material addition of volume weight product).
S4, drying
And drying the obtained module at 120 ℃ for 6 h. Then, the cut product was made to the following specifications: a volume weight of 300kg/m3And the dimensions are 300mm by 300 mm.
Comparative example 3
The procedure of example 1 was followed except that the vacuum degree and pressure of the vacuum suction filtration were changed. The specific process is as follows:
s1, preparing alumina fiber slurry: the same as in example 1.
S2, preparing zirconia fiber slurry: the same as in example 1.
S3, molding
Injecting the alumina fiber slurry into a forming mold, and performing vacuum suction filtration, wherein the vacuum degree is 0.09MPa, and the pressure is 0.2 MPa; and then injecting the zirconia slurry into a forming die, locating the zirconia slurry on the upper layer of the alumina slurry, and carrying out vacuum suction filtration, wherein the vacuum degree is 0.055MPa and the pressure is 0.5 MPa. After vacuum suction filtration and pressing, the thickness of the zirconia fiber layer to the alumina fiber layer was 1 (300 kg/m calculated according to the size of the mold)3Material addition of volume weight product).
S4, drying
And drying the obtained module at 120 ℃ for 6 h. Then, the cut product was made to the following specifications: a volume weight of 210kg/m3And the dimensions are 300mm by 300 mm. The product has no weight loss, and the heat-insulating property and the compressive strength are both reduced.
Example 4
The fiber module products obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to the following performance tests:
(1) the zirconia fiber face of the fiber module was heated at 1800 ℃ to achieve heat transfer equilibrium, and the temperature of the alumina fiber face (i.e., the back temperature) was tested. Only comparative example 1 was where the alumina fiber side was subjected to the above heat treatment.
(2) And observing whether the form of the heating surface of the module is kept intact after heating, and testing thermal shrinkage.
(3) The compressive strength of the product before and after heating was tested.
The test results are shown in table 1:
TABLE 1 Properties of the products obtained in examples 1 to 3 and comparative examples 1 to 3
Figure BDA0002858476350000131
Figure BDA0002858476350000141
The test results show that the composite module prepared by the invention has good heat insulation performance; meanwhile, after being heated at high temperature, the product can keep complete shape and does not shrink; moreover, higher compressive strength can be produced after high-temperature firing. Compared with the effect of the comparative example 1, the composite module adopting the alumina fiber and the zirconia fiber can effectively reduce the back temperature and improve the heat insulation property; meanwhile, the thermal integrity and the mechanical property after burning can be improved. Compared with the effects of comparative examples 2-3, the invention proves that the specifications of the two fibers and the forming process are controlled, so that the back temperature of the composite module is effectively reduced, the heat insulation performance is improved, and the mechanical property after sintering is improved.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. The preparation method of the zirconia-alumina fiber composite wet module is characterized by comprising the following steps of:
a) mixing alumina fiber, water and a dispersing agent to obtain alumina fiber dispersion liquid;
mixing the alumina fiber dispersion liquid with an inorganic binder, an alum solution and a flocculating agent to obtain alumina fiber slurry;
b) mixing zirconia fiber, water and a dispersing agent to obtain zirconia fiber dispersion liquid;
mixing the zirconia fiber dispersion liquid with an inorganic binder, an alum solution and a flocculating agent to obtain zirconia fiber slurry;
c) injecting the bottom layer fiber slurry into a forming mold, carrying out vacuum suction filtration, then injecting the upper layer fiber slurry, and carrying out vacuum suction filtration to obtain a composite wet blank;
d) drying the composite wet blank to obtain a zirconium oxide-aluminum oxide fiber composite wet module;
the bottom layer fiber slurry is the alumina fiber slurry obtained in the step a), and the upper layer fiber slurry is the zirconia fiber slurry obtained in the step b);
or
The bottom layer fiber slurry is the zirconia fiber slurry obtained in the step b), and the upper layer fiber slurry is the alumina fiber slurry obtained in the step a);
the step a) and the step b) are not limited in order.
2. The method according to claim 1, wherein the alumina fiber has a specification of: the fiber diameter is 4-6 μm, and the crystal phase is mullite crystal phase; the fiber index is more than or equal to 70 percent, the fiber length is 200-500 mu m, and the slag ball content with the length more than 212 mu m is less than or equal to 0.10wt percent;
the specifications of the zirconia fiber are as follows: the diameter of the fiber is 3-5 μm, the index of the fiber is more than or equal to 70%, the length of the fiber is 100-300 μm, and the content of slag balls with the length more than 212 μm is less than or equal to 0.15 wt%.
3. The method of claim 1, wherein the inorganic binder is a low sodium silica sol;
the specification of the low-sodium silica sol is as follows: the content of sodium oxide is less than 0.1%, the granularity is 10-20 nm, the solid content is 20-30%, and the pH value is 8-9;
in the step a), the mass ratio of the inorganic bonding agent to the alumina fiber is 3-6%;
in the step b), the mass ratio of the inorganic binder to the zirconia fiber is 5-10%.
4. The preparation method according to claim 1, wherein the mass concentration of the alum solution in the step a) and the step b) is respectively and independently 5-15%;
the mass ratio of the alum in the alum solution in the step a) and the solid content in the inorganic binder in the step b) is respectively and independently 1: 9-15.
5. The process according to claim 1, characterized in that the dispersant is epichlorohydrin;
in the step a), the mass ratio of the dispersing agent to the alumina fiber is 0.1-0.5%;
in the step a), the mass ratio of the dispersing agent to the zirconia fiber is 0.1-0.4%.
6. The method of claim 1, wherein the flocculant is a cationic amide;
in the step a), the mass ratio of the flocculating agent to the alumina fiber is 0.2-0.3%;
in the step b), the mass ratio of the flocculating agent to the zirconia fiber is 0.2-0.3%.
7. The preparation method according to claim 1, wherein in the step a), the mass ratio of the alumina fiber to the water is 5-20%;
in the step b), the mass ratio of the zirconia fiber to the water is 5-20%.
8. The method as claimed in claim 1, wherein in the step c), the conditions for vacuum suction filtering of the bottom layer fiber slurry are as follows: the vacuum degree is 0.04-0.075 MPa, and the pressure is 0-0.2 MPa;
the conditions for vacuum suction filtration of the upper fiber pulp are as follows: the vacuum degree is 0.08-0.095 MPa, and the pressure is 1-4 MPa;
the thickness ratio of a bottom layer wet fiber blank formed after the bottom layer fiber slurry is subjected to vacuum suction filtration to an upper layer wet fiber blank obtained after the upper layer fiber slurry is subjected to vacuum suction filtration is (0.8-2) to 1.
9. The method according to claim 1, wherein the drying temperature in step d) is 105-150 ℃ for 4-10 h.
10. A zirconia-alumina fiber composite wet module prepared by the preparation method of any one of claims 1 to 9.
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