CN114195550A - Anorthite refractory material with closed pore structure and preparation method thereof - Google Patents
Anorthite refractory material with closed pore structure and preparation method thereof Download PDFInfo
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- CN114195550A CN114195550A CN202010986824.6A CN202010986824A CN114195550A CN 114195550 A CN114195550 A CN 114195550A CN 202010986824 A CN202010986824 A CN 202010986824A CN 114195550 A CN114195550 A CN 114195550A
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- GWWPLLOVYSCJIO-UHFFFAOYSA-N dialuminum;calcium;disilicate Chemical compound [Al+3].[Al+3].[Ca+2].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] GWWPLLOVYSCJIO-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910052661 anorthite Inorganic materials 0.000 title claims abstract description 98
- 239000011148 porous material Substances 0.000 title claims abstract description 46
- 239000011819 refractory material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 28
- 238000005266 casting Methods 0.000 claims abstract description 17
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 13
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 20
- 238000010304 firing Methods 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 19
- 229910052903 pyrophyllite Inorganic materials 0.000 claims description 17
- 239000004568 cement Substances 0.000 claims description 16
- 238000000465 moulding Methods 0.000 claims description 16
- INJRKJPEYSAMPD-UHFFFAOYSA-N aluminum;silicic acid;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O INJRKJPEYSAMPD-UHFFFAOYSA-N 0.000 claims description 15
- 229910052850 kyanite Inorganic materials 0.000 claims description 15
- 239000010443 kyanite Substances 0.000 claims description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 13
- 239000004927 clay Substances 0.000 claims description 13
- 239000003245 coal Substances 0.000 claims description 12
- 239000004088 foaming agent Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000012752 auxiliary agent Substances 0.000 claims description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 230000009970 fire resistant effect Effects 0.000 claims description 2
- 229910010293 ceramic material Inorganic materials 0.000 claims 1
- 229910052593 corundum Inorganic materials 0.000 claims 1
- 229910001845 yogo sapphire Inorganic materials 0.000 claims 1
- 239000011449 brick Substances 0.000 abstract description 40
- 239000002131 composite material Substances 0.000 abstract description 6
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000004020 conductor Substances 0.000 abstract description 3
- 239000012071 phase Substances 0.000 description 42
- 239000002994 raw material Substances 0.000 description 12
- 238000003756 stirring Methods 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 238000000498 ball milling Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 230000006835 compression Effects 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000001354 calcination Methods 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 239000010433 feldspar Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000003746 solid phase reaction Methods 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052851 sillimanite Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
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Abstract
The invention provides an anorthite refractory material with a closed pore structure and a preparation method thereof, the light anorthite refractory material, in particular to an anorthite casting brick, has a specific microstructure, has an anorthite and mullite composite crystalline phase, takes the anorthite phase as a main crystalline phase, and the crystalline phase accounts for more than 90%; the porous material has a closed pore structure, the pore size distribution is uniform, the porous material has a specific pore size distribution range (the pore size is 500-: more than 80 percent; has anorthite and mullite composite crystal phase, the volume density of which is controllable, andthe volume density is low; meanwhile, the high-strength heat-conducting material has better compressive strength and excellent heat-conducting property. The experimental result shows that the bulk density is 0.48g/cm3About 2.0MPa or more in compressive strength, 0.18W/(m.K) or less in thermal conductivity, and 1100 to 1230 ℃.
Description
Technical Field
The invention belongs to the technical field of refractory materials, and particularly relates to an anorthite refractory material with a closed-cell structure and a preparation method thereof.
Background
The anorthite brick has high porosity, low volume density and good heat insulation performance, and is widely applied to heat insulation filling materials of spaces between refractory bricks and a barrel body in various industrial kilns. So as to reduce the heat loss of the kiln and obtain high energy utilization efficiency. The anorthite has the melting point of 1550 ℃, has the characteristics of small density, small thermal expansion coefficient, low thermal conductivity, stable existence in reducing atmosphere and the like, can partially replace clay, silicon and high-alumina refractory materials with the working temperature of 1000-1300 ℃, and realizes energy conservation and emission reduction.
The existing anorthite series light refractory materials, particularly refractory bricks, have low strength, are easy to deform and crack in the transportation process or the use process, and the heat insulation performance needs to be improved.
Disclosure of Invention
The invention aims to provide an anorthite refractory material with a closed-cell structure and a preparation method thereof.
The invention provides a preparation method of an anorthite refractory material with a closed pore structure, which comprises the following steps:
A) mixing 48-55 wt% of coal gangue, 3-6 wt% of kyanite, 4.5-6.5 wt% of pyrophyllite, 10-14.5 wt% of refractory clay, 9.5-15.5 wt% of calcium carbonate, 5-10 wt% of high-alumina cement and 3-8 wt% of an auxiliary agent (additionally) to obtain a castable;
B) pouring and molding the casting material, demolding and drying to obtain a dried blank;
C) and firing the dried blank to obtain the anorthite refractory material with a closed pore structure.
Preferably, the content of alumina in the kyanite is more than 45 wt%, and the content of silica in the pyrophyllite is more than 80 wt%.
Preferably, Al in the high-alumina cement2O3The content is 67-69 wt%.
Preferably, the auxiliary agent comprises one or more of a fire-resistant accelerator and a foaming agent.
Preferably, the casting temperature is 25-29 ℃; the pouring time is 10-16 min.
Preferably, the drying temperature is 100-150 ℃, and the drying time is 12-36 hours.
Preferably, the firing temperature is 1240-1280 ℃; the firing time is 45-50 hours.
The invention provides an anorthite refractory material with a closed pore structure, which is prepared by the preparation method, wherein Al in the anorthite refractory material2O3The content of (A) is 36-40 wt%; SiO 22The content of (A) is 38-45 wt%; the content of CaO is 10-15 wt%;
the anorthite refractory material has a closed pore structure, and the pore diameter is 500-700 mu m.
Preferably, the anorthite refractory material has an anorthite phase as a main crystal phase, the content of the anorthite phase is more than 90%, and the rest crystal phases are a mullite phase and a cristobalite phase.
Preferably, the anorthite refractory has an internal porosity of 80% or more.
The invention provides a preparation method of an anorthite refractory material with a closed pore structure, which comprises the following steps: A) mixing 48-55 wt% of coal gangue, 3-6 wt% of kyanite, 4.5-6.5 wt% of pyrophyllite, 10-14.5 wt% of refractory clay, 9.5-15.5 wt% of calcium carbonate, 5-10 wt% of high-alumina cement and 3-8 wt% of an auxiliary agent (additionally) to obtain a castable; B) pouring and molding the casting material, demolding and drying to obtain a dried blank; C) and firing the dried blank to obtain the anorthite refractory material with a closed pore structure. The lightweight anorthite refractory material, in particular to an anorthite casting brick, has a specific microstructure, has an anorthite and mullite composite crystalline phase, takes the anorthite phase as a main crystalline phase, and the crystalline phase accounts for more than 90 percent; the porous material has a closed pore structure, the pore size distribution is uniform, the porous material has a specific pore size distribution range (the pore size is 500-: more than 80 percent; has a composite crystalline phase of anorthite and mullite,the volume density of the material is controllable and is lower; meanwhile, the high-strength heat-conducting material has better compressive strength and excellent heat-conducting property. The experimental result shows that the bulk density is 0.48g/cm3About 2.0MPa or more in compressive strength, 0.18W/(m.K) or less in thermal conductivity, and 1100 to 1230 ℃.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is an XRD pattern of a calc feldspar brick in example 1 of the present invention;
FIG. 2 is an XRD pattern of a prior art Callicate brick;
FIG. 3 is an SEM photograph of a Calcite brick of example 1 of the present invention;
fig. 4 is an SEM image of a prior art caldolite brick.
Detailed Description
The invention provides a preparation method of an anorthite refractory material with a closed pore structure, which comprises the following steps:
A) mixing 48-55 wt% of coal gangue, 3-6 wt% of kyanite, 4.5-6.5 wt% of pyrophyllite, 10-14.5 wt% of refractory clay, 9.5-15.5 wt% of calcium carbonate, 5-10 wt% of high-alumina cement and 3-8 wt% of an auxiliary agent (additionally) to obtain a castable;
B) pouring and molding the casting material, demolding and drying to obtain a dried blank;
C) and firing the dried blank to obtain the anorthite refractory material with a closed pore structure.
In the invention, the mass fraction of the coal gangue is preferably 48-55 wt%, more preferably 49-54 wt%, most preferably 52-54 wt%, and specifically, in an embodiment of the invention, 54 wt% may be used.
In the present invention, the kyanite provides an aluminum source, preferably having an alumina content above 45 wt%, and the kyanite self-expands during firing to counteract shrinkage during firing, but the amount of kyanite added in the present formulation is not so great as to cause deformation of the anorthite refractory after firing. The mass fraction of the kyanite is preferably 3 to 6 wt%, more preferably 4 to 5 wt%, and specifically, in an embodiment of the present invention, may be 5 wt%.
In the invention, the pyrophyllite is used as a silicon source to provide silicon dioxide, an anorthite phase and mullite are formed in the firing process, and the components except the silicon source in the pyrophyllite can play a role in enhancing the strength of the green brick. In the present invention, the content of silica in the pyrophyllite is preferably 80 wt% or more; the mass fraction of the pyrophyllite is preferably 4.5-6.5 wt%, more preferably 5-6 wt%, and specifically, in the embodiment of the present invention, may be 5.5 wt%.
In the present invention, the fire clay is capable of polymerizing other powders during the molding of the wet green to enhance the strength of the wet green. The mass fraction of the refractory clay is preferably 10 to 14.5 wt%, more preferably 11 to 14 wt%, most preferably 12 to 13 wt%, and specifically, in an embodiment of the present invention, may be 12.5 wt%.
In the invention, the calcium carbonate is used as a calcium source to generate calcium oxide under the action of high temperature, and an anorthite phase is formed. The mass fraction of the calcium carbonate is preferably 9.5 to 15.5 wt%, more preferably 10 to 15 wt%, most preferably 11 to 14 wt%, and specifically, in an embodiment of the present invention, may be 13 wt%.
In the invention, the high-alumina cement can increase the strength of a wet blank in the process of forming the wet blank. Al in the high-alumina cement2O3The content is preferably 67 to 69 wt%, and the mass fraction of the high-alumina cement is preferably 5 to 10 wt%, more preferably 6 to 9 wt%, most preferably 7 to 8 wt%, and specifically, in an embodiment of the present invention, may be 10 wt%.
In the invention, the anorthite refractory material comprises auxiliary components brought by raw material adjustment, such as a refractory coagulant, a foaming agent and the like, besides the main components, and the content of the auxiliary additional components accounts for 3-8 wt% of the main materials, preferably about 5% of the main materials, based on the total mass of the main materials, such as coal gangue, kyanite, pyrophyllite, refractory clay, calcium carbonate and high-alumina cement, but the addition of the auxiliary additional components is not suitable, and the wet blank solidification speed and the volume density are not controllable due to the excessive addition of the auxiliary additional components.
In the present invention, the refractory set accelerator (in addition) increases the wet-green setting speed during the forming process; the foaming agent (plus) is added to the slurry to form a pore structure by mechanical foaming during the forming process.
The raw materials are mixed according to a proportion and then are subjected to ball milling to obtain a mixture.
In the invention, the particle size of the mixture after ball milling is 1200 meshes preferably
According to the invention, the mixture is preferably mixed with auxiliary agents such as foaming agent and the like and then stirred to obtain the castable, and the obtained castable is cast and molded in a mold to obtain a blank.
In the invention, the casting time is preferably 10-16 min, more preferably 11-15 min, and most preferably 12-14 min, specifically, in the embodiment of the invention, 15 min; the casting temperature is preferably 25-29 ℃, more preferably 26-28 ℃, and specifically, in the embodiment of the invention, may be 26 ℃.
After a blank is obtained, the obtained blank is kept stand and maintained until the slurry is completely solidified to meet the requirement of demoulding;
and after demolding, drying the blank to obtain a dried blank.
In the invention, the drying temperature is preferably 100-150 ℃, more preferably 110-140 ℃, and most preferably 120-130 ℃, specifically, in the embodiment of the invention, 120 ℃; the drying time is preferably 12 to 36 hours, and more preferably 24 hours. The drying in the present invention may be oven drying.
The dried blank is fired to obtain the anorthite refractory material with a closed pore structure.
In the invention, the firing temperature is preferably 1240-1280 ℃, and more preferably 1260 ℃; the firing time is preferably 45 to 50 hours, more preferably 46 to 49 hours, and specifically, in an embodiment of the present invention, 48 hours may be used.
The invention also provides an anorthite refractory material with a closed pore structure, which is prepared according to the preparation method, wherein Al in the anorthite refractory material is2O3The content of (A) is 36-40 wt%; SiO 22The content of (A) is 38-45 wt%; the content of CaO is 10-15 wt%;
the anorthite refractory material has a closed pore structure, and the pore diameter is 500-700 mu m.
In the invention, the anorthite refractory material has an anorthite phase as a main crystal phase, the content of the anorthite phase is more than 90%, and the rest crystal phases are a mullite phase and a cristobalite phase. Specifically, in the examples of the present invention, the content of anorthite phase in the anorthite refractory was 91%, and the content of mullite phase and cristobalite phase was 9%.
In the invention, the anorthite refractory material has a closed-cell structure, the closed-cell material corresponds to the open-cell material, the closed-cell material has an independent cell structure, the inner cells are separated from each other by the wall membrane and are not connected with each other, the cells of the open-cell material are connected with each other or are completely connected, and gas or liquid can pass through the cells in single dimension or three dimensions. Generally, the porosity of the closed-cell material is lower than that of the open-cell material, but the anorthite refractory material has a closed-cell structure which is close to a circular structure and is uniformly distributed, the internal true porosity is more than 80%, and the pore diameter is 500-700 μm, preferably about 600 μm.
The anorthite refractory material has the microscopic pore structure, so that the anorthite refractory material can obtain higher compressive strength and better heat insulation performance.
Furthermore, the invention also provides an anorthite refractory brick with a closed pore structure, and the anorthite refractory brick with the closed pore structure can be directly obtained by using a brick making mold in the preparation method of the anorthite refractory material.
The invention provides a preparation method of an anorthite refractory material with a closed pore structure, which comprises the following steps: A) mixing 48-55 wt% of coal gangue, 3-6 wt% of kyanite, 4.5-6.5 wt% of pyrophyllite, 10-14.5 wt% of refractory clay, 9.5-15.5 wt% of calcium carbonate, 5-10 wt% of high-alumina cement and 3-8 wt% of an auxiliary agent (additionally) to obtain a castable; B) pouring and molding the casting material, demolding and drying to obtain a dried blank; C) and firing the dried blank to obtain the anorthite refractory material with a closed pore structure. The lightweight anorthite refractory material, in particular to an anorthite casting brick, has a specific microstructure, has an anorthite and mullite composite crystalline phase, takes the anorthite phase as a main crystalline phase, and the crystalline phase accounts for more than 90 percent; the porous material has a closed pore structure, the pore size distribution is uniform, the porous material has a specific pore size distribution range (the pore size is 500-: more than 80 percent; the crystal has anorthite and mullite composite crystal phase, and the volume density of the crystal is controllable and lower; meanwhile, the high-strength heat-conducting material has better compressive strength and excellent heat-conducting property. The experimental result shows that the bulk density is 0.48g/cm3About 2.0MPa or more in compressive strength, 0.18W/(m.K) or less in thermal conductivity, and 1100 to 1230 ℃.
In order to further illustrate the present invention, the following examples are provided to describe an anorthite refractory material with a closed cell structure and a method for preparing the same in detail, but should not be construed as limiting the scope of the present invention.
Example 1:
through formula adjustment, the raw material components of the anorthite brick are adjusted to 54 percent of coal gangue, 5 percent of kyanite, 5.5 percent of pyrophyllite and 13 percent of calcium carbonate.
(1) Mixing the main raw materials, performing ball milling, and uniformly stirring;
(2) adding auxiliary components such as 12.5% of refractory clay, 10% of high-alumina cement, 3% of additional foaming agent and the like into the mixture obtained in the step (1), and stirring to obtain a castable;
(3) pouring and molding the castable to obtain a blank, wherein the pouring time is 15min, and the indoor temperature is controlled at 26 ℃;
(4) standing and maintaining the blank obtained by casting molding until the slurry is completely solidified to meet the demolding requirement;
(5) demolding the blank after standing and maintaining, and then drying at the drying temperature of 120 ℃ for 24 hours;
(6) and firing the dried green body at 1260 ℃ for 48 h.
The anorthite brick prepared by the method has the compression strength of 2.1MPa, the average heat conductivity coefficient of 0.084W/(m.K) at 200 ℃, the average temperature of 0.11W/(m.K) at 400 ℃ and the average temperature of 0.13W/(m.K) at 600 ℃; the change of the re-burning line is-0.18 percent and the breaking strength is 1.2 MPa.
Example 2:
through formula adjustment, raw material components of the anorthite brick are adjusted to 55% of coal gangue, 6% of kyanite and 4.5% of pyrophyllite.
(1) Mixing the main raw materials, performing ball milling, and uniformly stirring;
(2) adding 14.5% of refractory clay, 15% of calcium carbonate, 5% of high-alumina cement, 3% of foaming agent and other auxiliary components into the mixture obtained in the step (1), and stirring to obtain a castable;
(3) pouring and molding the castable to obtain a blank, wherein the pouring time is 13min, and the indoor temperature is controlled at 26 ℃;
(4) standing and maintaining the blank obtained by casting molding until the slurry is completely solidified to meet the demolding requirement;
(5) demolding the blank after standing and maintaining, and then drying at the drying temperature of 120 ℃ for 24 hours;
(6) and firing the dried green body at 1280 ℃ for 48 h.
The anorthite brick prepared by the method has the compression strength of 2.34MPa, the average heat conductivity coefficient of 0.086W/(m.K) at 200 ℃, the average temperature of 400 ℃ of 0.104W/(m.K) and the average temperature of 600 ℃ of 0.126W/(m.K); the change of the re-burning line is-0.17 percent and the breaking strength is 1.1 MPa.
Comparative example 1:
through formula adjustment, the raw material components of the anorthite brick are adjusted to 54 percent of coal gangue, 5 percent of sillimanite, 5.5 percent of pyrophyllite, 12.5 percent of refractory clay, 13 percent of calcium carbonate and 10 percent of high-alumina cement.
(1) Mixing the main raw materials, performing ball milling, and uniformly stirring;
(2) adding auxiliary components such as foaming agent and the like into the mixed material in the step (1) and stirring to obtain a castable;
(3) pouring and molding the castable to obtain a blank, wherein the pouring time is 15min, and the indoor temperature is controlled at 26 ℃;
(4) standing and maintaining the blank obtained by casting molding until the slurry is completely solidified to meet the demolding requirement;
(5) demolding the blank after standing and maintaining, and then drying at the drying temperature of 120 ℃ for 24 hours;
(6) and firing the dried green body at 1260 ℃ for 48h, wherein the heat preservation time is 5 h.
The anorthite brick prepared by the method has the compression strength of 1.1MPa, the average heat conductivity coefficient of 0.091W/(m.K) at 200 ℃, the average temperature of 400 ℃ of 0.128W/(m.K) and the average temperature of 600 ℃ of 0.136W/(m.K); the change of the re-burning line is-0.3 percent and the breaking strength is 0.8 MPa.
Fig. 1 is an XRD pattern of the anorthite brick of example 1 of the present invention, fig. 2 is an XRD pattern of the anorthite brick of the prior art, fig. 3 is an SEM image of the anorthite brick of example 1 of the present invention, and fig. 4 is an SEM image of the anorthite brick of the prior art.
In the XRD (X-ray diffraction pattern) analysis of the anorthite brick of the prior art (fig. 2), the peak height at each position is low, and the anorthite brick is only about 4300 when the diffraction angle θ is 28. The peak heights at all positions are reduced to different degrees, which shows that the system has high content of high-temperature components, insufficient calcination temperature and incomplete crystalline phase conversion. The crystallinity of the anorthite brick is poor, the crystal grains are small, the defects are more, and a firm skeleton of crystal grain groups is not formed. The high-temperature solid-phase reaction of the anorthite brick is poor, the crystal phase conversion is incomplete, and the method has the advantages of low reaction temperature, high reaction temperature, and high reaction temperature, and high reaction temperature, and high reaction temperature, high reactionIs also one of the reasons for the poor thermal shock resistance of anorthite bricks. As can be seen from fig. 4, the light weight anorthite-based refractory material, especially refractory brick, has anorthite as the main crystal phase, and the main crystal phase is irregular, the crystal is not completely precipitated, the size and boundary of the crystal grain are fuzzy, the crystal grain is irregular, and no firm framework of crystal grain group is formed, and the irregular crystal phase structure results in lower compressive strength of the refractory brick and reduces the refractory insulation performance of the refractory brick. And the pore structure is mostly open pore structure, on one hand, the strength of the anorthite refractory material is low, and deformation and fracture are easy to occur in the transportation process or the use process; on the other hand, the volume density and the heat conductivity coefficient of the anorthite refractory material are influenced, so that the volume density is generally 0.48g/cm3The thermal conductivity is generally 0.2W/(mK) or more.
When the anorthite brick is analyzed by XRD (X-ray diffraction pattern) (figure 1), the peak value of each crystalline phase is obviously increased from the position of the main peak, and the peak value of anorthite phase reaches about 7000, which indicates that the crystalline phase is completely converted. And the main crystal phase is anorthite phase, and also contains a small amount of mullite and cristobalite phase. The solid phase reaction in the self-made calcium feldspar brick system is basically finished, and the calcining temperature and the calcining time basically meet the requirements.
As can be seen from fig. 1, the content of anorthite phase, which is a main crystal phase, is 91%, and the content of mullite phase and cristobalite phase is 9%.
Fig. 3 is a microscopic structure view of anorthite brick at a magnification of 5000 times, and it can be seen that: the size and the boundary of the crystal and the crystal grain of the prepared anorthite brick are clearly visible, the crystal is complete, the crystal is in a sheet shape, the diameter range of the crystal grain is mostly between 1 and 3 mu m, and a firmer framework structure of a crystal grain group is formed.
Comparative example 2:
through formula adjustment, the raw material components of the anorthite brick are adjusted to 55 percent of coal gangue, 6.5 percent of pyrophyllite, 13.5 percent of refractory clay, 14 percent of calcium carbonate and 11 percent of high-alumina cement.
(1) Mixing the main raw materials, performing ball milling, and uniformly stirring;
(2) adding auxiliary components such as foaming agent and the like into the mixed material in the step (1) and stirring to obtain a castable;
(3) pouring and molding the castable to obtain a blank, wherein the pouring time is 15min, and the indoor temperature is controlled at 26 ℃;
(4) standing and maintaining the blank obtained by casting molding until the slurry is completely solidified to meet the demolding requirement;
(5) demolding the blank after standing and maintaining, and then drying at the drying temperature of 120 ℃ for 24 hours;
(6) and firing the dried green body at 1260 ℃ for 48h, wherein the heat preservation time is 5 h.
The anorthite brick prepared by the method has the compression strength of 0.9MPa, the average heat conductivity coefficient of 0.12W/(mK) at 200 ℃, the average temperature of 400 ℃ of 0.126W/(mK) and the average temperature of 600 ℃ of 0.139W/(mK); the change of the re-burning line is-0.45 percent and the breaking strength is 0.6 MPa.
Comparative example 3:
through formula adjustment, the raw material components of the anorthite brick are adjusted to 56.5 percent of coal gangue, 7.5 percent of kyanite, 8 percent of pyrophyllite, 15.5 percent of calcium carbonate and 12.5 percent of high-alumina cement.
(1) Mixing the main raw materials, performing ball milling, and uniformly stirring;
(2) adding auxiliary components such as foaming agent and the like into the mixed material in the step (1) and stirring to obtain a castable;
(3) pouring and molding the castable to obtain a blank, wherein the pouring time is 15min, and the indoor temperature is controlled at 26 ℃;
(4) standing and maintaining the blank obtained by casting molding until the slurry is completely solidified to meet the demolding requirement;
(5) demolding the blank after standing and maintaining, and then drying at the drying temperature of 120 ℃ for 24 hours;
(6) and firing the dried green body at 1260 ℃ for 48h, wherein the heat preservation time is 5 h.
The anorthite brick prepared by the method has the compression strength of 0.8MPa, the average thermal conductivity of 0.093W/(m.K) at 200 ℃, the average temperature of 0.119W/(m.K) at 400 ℃ and the average temperature of 0.139W/(m.K) at 600 ℃; the change of the re-burning line is-0.21 percent and the breaking strength is 0.5 MPa.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of an anorthite refractory material with a closed cell structure comprises the following steps:
A) mixing 48-55 wt% of coal gangue, 3-6 wt% of kyanite, 4.5-6.5 wt% of pyrophyllite, 10-14.5 wt% of refractory clay, 9.5-15.5 wt% of calcium carbonate, 5-10 wt% of high-alumina cement and 3-8 wt% of an auxiliary agent to obtain a castable;
B) pouring and molding the casting material, demolding and drying to obtain a dried blank;
C) and firing the dried blank to obtain the anorthite refractory material with a closed pore structure.
2. The method according to claim 1, wherein the kyanite contains alumina at 45 wt% or more and the pyrophyllite contains silica at 80 wt% or more.
3. The method of claim 1, wherein the aluminous cement contains Al2O3The content is 67-69 wt%.
4. The method of claim 1, wherein the auxiliary agent comprises one or more of a fire-resistant accelerator and a foaming agent.
5. The preparation method according to claim 1, wherein the casting temperature is 25-29 ℃; the pouring time is 10-16 min.
6. The method according to claim 1, wherein the drying temperature is 100 to 150 ℃ and the drying time is 12 to 36 hours.
7. The method for preparing the ceramic material according to claim 1, wherein the firing temperature is 1240 to 1280 ℃; the firing time is 45-50 hours.
8. Closed-cell anorthite refractory material prepared by the preparation method of any one of claims 1 to 7, wherein Al in the anorthite refractory material2O3The content of (A) is 36-40 wt%; SiO 22The content of (A) is 38-45 wt%; the content of CaO is 10-15 wt%;
the anorthite refractory material has a closed pore structure, and the pore diameter is 500-700 mu m.
9. The anorthite refractory according to claim 8, wherein the anorthite refractory has an anorthite phase as a main crystal phase, the content of the anorthite phase is 90% or more, and the remaining crystal phases are a mullite phase and a cristobalite phase.
10. The anorthite refractory according to claim 8, wherein the anorthite refractory has an internal porosity of 80% or more.
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