CN112592189A - Three-stage porous ceramic and preparation method and application thereof - Google Patents
Three-stage porous ceramic and preparation method and application thereof Download PDFInfo
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- CN112592189A CN112592189A CN202011574931.4A CN202011574931A CN112592189A CN 112592189 A CN112592189 A CN 112592189A CN 202011574931 A CN202011574931 A CN 202011574931A CN 112592189 A CN112592189 A CN 112592189A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 50
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 21
- 239000011230 binding agent Substances 0.000 claims abstract description 16
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003546 flue gas Substances 0.000 claims abstract description 13
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 11
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims description 30
- 239000003054 catalyst Substances 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 10
- 235000015895 biscuits Nutrition 0.000 claims description 10
- 238000006477 desulfuration reaction Methods 0.000 claims description 10
- 230000023556 desulfurization Effects 0.000 claims description 10
- 239000011812 mixed powder Substances 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000006060 molten glass Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000004005 microsphere Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 235000007164 Oryza sativa Nutrition 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 3
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 3
- 235000009566 rice Nutrition 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 229920002472 Starch Polymers 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 239000008107 starch Substances 0.000 claims description 2
- 235000019698 starch Nutrition 0.000 claims description 2
- 240000007594 Oryza sativa Species 0.000 claims 1
- 229910010293 ceramic material Inorganic materials 0.000 claims 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims 1
- 229910001928 zirconium oxide Inorganic materials 0.000 claims 1
- 239000011521 glass Substances 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract description 2
- 230000008018 melting Effects 0.000 abstract description 2
- 239000011148 porous material Substances 0.000 description 11
- 239000000428 dust Substances 0.000 description 5
- 150000004767 nitrides Chemical class 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 150000003568 thioethers Chemical class 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0027—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions
- B01D46/0036—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours with additional separating or treating functions by adsorption or absorption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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Abstract
A three-stage porous ceramic is obtained by sintering 50-80 parts of silicon nitride, 5-10 parts of sintering aid, 30-60 parts of binder, 2-15 parts of pore-forming agent and 2-15 parts of low-temperature melting glass powder according to parts by weight, wherein the pore-forming agent adopts three specifications, including 60-100 mu m, 30-50 mu m and 1-10 mu m, as pore-forming agent for a first stage, a second stage and a third stage respectively, and the first stage, the second stage and the third stage jointly form the three-stage porous ceramic; the sintering conditions are as follows: heating to 400 ℃ at a heating rate of 2-3 ℃/min, keeping the temperature for 0.5-2 hours, continuing to heat to 650 ℃ at 550 ℃ for 2-4 hours, heating to 900 ℃ at a heating rate of 1-2 ℃/min, keeping the temperature for 2-6 hours, and naturally cooling to room temperature. The invention also discloses a preparation method of the three-stage porous ceramic and application of the three-stage porous ceramic in a flue gas filtering device.
Description
Technical Field
The invention belongs to the field of porous ceramics, and particularly relates to three-stage porous ceramics and a preparation method and application thereof.
Background
In the traditional process, the treatment of the flue gas comprises denitration, dust removal and desulfurization, the three steps are mutually independent, the flue gas needs to enter a denitration device for treatment, then enters a dust removal device and finally enters a desulfurization device, the multi-step operation increases the cost and wastes energy, and therefore a novel technology that a single device can complete the denitration, dust removal and desulfurization processes is required to be developed.
The porous ceramic has the advantages of high porosity, high strength and good physical and chemical stability, and is characterized in that a plurality of uniform and controllable pores including open pores and closed pores are distributed in a structure body. The catalyst can be combined with the porous ceramic by loading the catalyst on the surface of the porous ceramic or sintering the catalyst and the porous ceramic together, and the method is widely applied to the field of flue gas filtration. The catalyst obtained by the method has good catalytic effect and high filtering precision.
Disclosure of Invention
In order to solve the problems of increasing cost and wasting energy due to multi-step operation of flue gas treatment in the prior art, the invention provides a three-stage porous ceramic and a preparation method and application thereof.
The scheme adopted by the invention is as follows:
a three-stage porous ceramic is obtained by sintering 50-80 parts of silicon nitride, 5-10 parts of sintering aid, 30-60 parts of binder, 2-15 parts of pore-forming agent and 2-15 parts of low-temperature melting glass powder according to parts by weight, wherein the pore-forming agent adopts three specifications, including 60-100 mu m, 30-50 mu m and 1-10 mu m, as pore-forming agent for a first stage, a second stage and a third stage respectively, and the first stage, the second stage and the third stage jointly form the three-stage porous ceramic;
the sintering conditions are as follows: heating to 400 ℃ at a heating rate of 2-3 ℃/min, keeping the temperature for 0.5-2 hours, continuing to heat to 650 ℃ at 550 ℃ for 2-4 hours, heating to 900 ℃ at a heating rate of 1-2 ℃/min, keeping the temperature for 2-6 hours, and naturally cooling to room temperature.
As a preferable technical scheme of the invention, the sintering aid is one or combination of any of alumina, magnesia, zirconia and yttria.
In a preferred embodiment of the present invention, the binder comprises a PVA solution or a PVB solution.
As a preferred technical scheme of the invention, the pore-forming agent is graphite, rice hulls, PMMA microspheres, starch or polystyrene microspheres.
As a preferred technical solution of the present invention, the arrangement order of the first stage, the second stage and the third stage is the first stage, the second stage, the third stage or the first stage, the third stage, the second stage or the second stage, the first stage and the third stage.
A preparation method of three-stage porous ceramic comprises the following steps:
A. mixing 50-80 parts of silicon nitride, 5-10 parts of sintering aid, 30-60 parts of binder, 2-15 parts of pore-forming agent and 2-15 parts of low-temperature molten glass powder according to the parts by mass, adding the mixture into a ball milling tank, adding a solvent which is 1.5-2 times of the total mass of the raw materials to obtain first-stage slurry, wherein the specification of the pore-forming agent is 60-100 mu m, preparing second-stage slurry and third-stage slurry according to the same mass ratio, except that the specification of the pore-forming agent in the second-stage slurry is 30-50 mu m, and the specification of the pore-forming agent in the third-stage slurry is 1-10 mu m;
B. b, ball-milling the three parts of slurry obtained in the step A for 8-16 hours, taking out, drying and grinding at the temperature of 60-100 ℃ to obtain three parts of powder;
C. arranging the three powder materials obtained in the step B in a container according to the sequence of a first stage, a second stage and a third stage, wherein the first stage and the second stage are partially mixed at the junction, and the second stage and the third stage are partially mixed at the junction;
D. c, ultrasonically vibrating the mixed powder obtained in the step C for 5-30 minutes;
E. d, pressing and forming the mixed powder obtained in the step D to obtain a biscuit;
F. and E, sintering the biscuit obtained in the step E according to the following conditions: heating to 400 ℃ at the heating rate of 2-3 ℃/min, keeping the temperature for 0.5-2 hours, continuing to heat to 650 ℃ at 550 ℃ for 2-4 hours, heating to 900 ℃ at the heating rate of 1-2 ℃/min, keeping the temperature for 2-6 hours, and naturally cooling to room temperature to obtain the three-stage porous ceramic.
As a preferred technical scheme of the invention, the solvent in the step A is one or a mixture of deionized water, methanol, ethanol and acetone.
As a preferable technical solution of the present invention, the compression molding manner in step E is dry compression molding or extrusion molding.
As a preferred technical scheme of the invention, 1-10 parts of desulfurization or denitrification catalyst is also added in the step A.
An application of three-stage porous ceramic in a flue gas filtering device.
Compared with the prior art, the invention has the following beneficial effects:
(1) providing porous ceramic with three-level pore distribution and a preparation method thereof;
(2) different catalysts can be loaded on the three-stage porous ceramics in different grades, so that the application of the porous ceramics in the field of catalyst carriers is widened;
(3) the denitration and desulfurization catalysts are respectively loaded on different levels of the three-level porous ceramic, and the adsorption effect of the porous ceramic on smoke dust is combined, so that the integration of desulfurization, denitration and dust removal of the smoke is achieved, the energy consumption is reduced, and the production cost is reduced.
Drawings
FIG. 1 is a schematic view of a three-stage porous ceramic structure in which a first stage, a second stage, and a third stage are arranged in this order.
Detailed Description
The present invention is further described with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the claims, and other alternatives which may occur to those skilled in the art are also within the scope of the claims.
FIG. 1 is a schematic view of a three-stage porous ceramic structure arranged in the order of a first stage, a second stage, and a third stage. The pore diameter of the first level is maximum, the second level is minimum, and the third level is minimum, and the part of the juncture of the first level and the second level has certain coincidence and blending, and the area simultaneously comprises the maximum pore of the first level and the second larger pore, and similarly, the juncture of the second level and the third level also has certain coincidence and blending, and the juncture simultaneously comprises the second larger pore and the third level minimum pore.
Example 1
A three-stage porous ceramic is obtained by sintering 50 parts of silicon nitride, 5 parts of sintering aid, 30 parts of binder, 2 parts of pore-forming agent and 2 parts of low-temperature molten glass powder in parts by mass, wherein the pore-forming agent adopts three specifications including 60-100 mu m, 30-50 mu m and 1-10 mu m and is respectively used as the pore-forming agent of a first stage, a second stage and a third stage, and the first stage, the second stage and the third stage jointly form the three-stage porous ceramic;
the sintering conditions are as follows: heating to 300 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 0.5 hour, continuously heating to 550 ℃, keeping the temperature for 2 hours, heating to 700 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 2 hours, and then naturally cooling to the room temperature.
Specifically, the sintering aid is alumina.
In particular, the binder is a PVA solution.
Specifically, the pore former is graphite.
Specifically, the first stage, the second stage and the third stage are arranged in the order of the first stage, the second stage and the third stage.
The preparation method of the three-stage porous ceramic comprises the following steps:
A. mixing 50 parts of silicon nitride, 5 parts of sintering aid, 30 parts of binder, 2 parts of pore-forming agent and 2 parts of low-temperature molten glass powder according to the mass parts, adding the mixture into a ball milling tank, adding a solvent which is 1.5 times of the total mass of the raw materials to obtain first-stage slurry, wherein the specification of the pore-forming agent is 60-100 mu m, and preparing second-stage slurry and third-stage slurry according to the same mass ratio, wherein the difference is that the specification of the pore-forming agent in the second-stage slurry is 30-50 mu m, and the specification of the pore-forming agent in the third-stage slurry is 1-10 mu m;
B. b, ball-milling the three parts of slurry obtained in the step A for 8 hours, taking out, drying and grinding at the temperature of 60 ℃ to obtain three parts of powder;
C. arranging the three powder materials obtained in the step B in a container according to the sequence of a first stage, a second stage and a third stage, wherein the first stage and the second stage are partially mixed at the junction, and the second stage and the third stage are partially mixed at the junction;
D. c, ultrasonically vibrating the mixed powder obtained in the step C for 5 minutes;
E. d, pressing and forming the mixed powder obtained in the step D to obtain a biscuit;
F. and E, sintering the biscuit obtained in the step E according to the following conditions: heating to 300 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 0.5 hour, continuously heating to 550 ℃, keeping the temperature for 2 hours, heating to 700 ℃ at the heating rate of 1 ℃/min, keeping the temperature for 2 hours, and naturally cooling to room temperature to obtain the three-stage porous ceramic.
Specifically, the solvent in step A is ethanol.
Specifically, the press forming manner in the step E is dry press forming.
And a desulfurization and denitrification catalyst is loaded on the three-stage porous ceramic prepared by the preparation method, and the three-stage porous ceramic is arranged in a flue gas filtering device and used for catalytically oxidizing nitrides or sulfides in the flue gas.
Example 2
A three-stage porous ceramic is obtained by sintering 80 parts of silicon nitride, 10 parts of sintering aid, 60 parts of binder, 15 parts of pore-forming agent and 15 parts of low-temperature molten glass powder in parts by mass, wherein the pore-forming agent adopts three specifications including 60-100 mu m, 30-50 mu m and 1-10 mu m and is respectively used as the pore-forming agent of a first stage, a second stage and a third stage, and the first stage, the second stage and the third stage jointly form the three-stage porous ceramic;
the sintering conditions are as follows: heating to 400 ℃ at the heating rate of 3 ℃/min, keeping the temperature for 2 hours, continuously heating to 650 ℃, keeping the temperature for 4 hours, heating to 900 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 6 hours, and then naturally cooling to the room temperature.
Specifically, the sintering aid is yttria.
In particular, the binder is a PVA solution.
Specifically, the pore former is rice hulls.
Specifically, the first stage, the second stage and the third stage are arranged in the order of the second stage, the first stage and the third stage.
The preparation method of the three-stage porous ceramic comprises the following steps:
A. mixing 80 parts of silicon nitride, 10 parts of sintering aid, 60 parts of binder, 15 parts of pore-forming agent and 15 parts of low-temperature molten glass powder according to the mass parts, adding the mixture into a ball milling tank, adding a solvent which is 2 times of the total mass of the raw materials to obtain a first-stage slurry, wherein the specification of the pore-forming agent is 60-100 mu m, and preparing a second-stage slurry and a third-stage slurry according to the same mass ratio, wherein the difference is that the specification of the pore-forming agent in the second-stage slurry is 30-50 mu m, and the specification of the pore-forming agent in the third-stage slurry is 1-10 mu m;
B. b, ball-milling the three parts of slurry obtained in the step A for 16 hours, taking out, drying and grinding at the temperature of 100 ℃ to obtain three parts of powder;
C. arranging the three powder materials obtained in the step B in a container according to the sequence of a first stage, a second stage and a third stage, wherein the first stage and the second stage are partially mixed at the junction, and the second stage and the third stage are partially mixed at the junction;
D. c, ultrasonically vibrating the mixed powder obtained in the step C for 30 minutes;
E. d, pressing and forming the mixed powder obtained in the step D to obtain a biscuit;
F. and E, sintering the biscuit obtained in the step E according to the following conditions: heating to 400 ℃ at the heating rate of 3 ℃/min, keeping the temperature for 2 hours, continuously heating to 650 ℃, keeping the temperature for 4 hours, heating to 900 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 6 hours, and naturally cooling to room temperature to obtain the three-stage porous ceramic.
Specifically, the solvent in step a is deionized water.
Specifically, the press forming manner in the step E is dry press forming.
And a desulfurization and denitrification catalyst is loaded on the three-stage porous ceramic prepared by the preparation method, and the three-stage porous ceramic is arranged in a flue gas filtering device and used for catalytically oxidizing nitrides or sulfides in the flue gas.
Example 3
A three-stage porous ceramic is obtained by sintering 70 parts of silicon nitride, 8 parts of sintering aid, 50 parts of binder, 8 parts of pore-forming agent and 8 parts of low-temperature molten glass powder in parts by mass, wherein the pore-forming agent adopts three specifications including 60-100 mu m, 30-50 mu m and 1-10 mu m and is respectively used as the pore-forming agent of a first stage, a second stage and a third stage, and the first stage, the second stage and the third stage jointly form the three-stage porous ceramic;
the sintering conditions are as follows: heating to 350 deg.C at a heating rate of 2 deg.C/min, maintaining for 1 hr, heating to 600 deg.C, maintaining for 3 hr, heating to 800 deg.C at a heating rate of 2 deg.C/min, maintaining for 4 hr, and naturally cooling to room temperature.
Specifically, the sintering aid is magnesium oxide.
In particular, the binder is a PVB solution.
Specifically, the pore-forming agent is PMMA microspheres.
Specifically, the first stage, the second stage and the third stage are arranged in the order of the first stage, the third stage and the second stage.
The preparation method of the three-stage porous ceramic comprises the following steps:
A. mixing 70 parts of silicon nitride, 8 parts of sintering aid, 50 parts of binder, 8 parts of pore-forming agent and 8 parts of low-temperature molten glass powder according to the mass parts, adding the mixture into a ball milling tank, adding a solvent which is 2 times of the total mass of the raw materials to obtain a first-stage slurry, wherein the specification of the pore-forming agent is 60-100 mu m, and preparing a second-stage slurry and a third-stage slurry according to the same mass ratio, wherein the difference is that the specification of the pore-forming agent in the second-stage slurry is 30-50 mu m, and the specification of the pore-forming agent in the third-stage slurry is 1-10 mu m;
B. b, ball-milling the three parts of slurry obtained in the step A for 10 hours, taking out, drying and grinding at the temperature of 80 ℃ to obtain three parts of powder;
C. arranging the three powder materials obtained in the step B in a container according to the sequence of a first stage, a second stage and a third stage, wherein the first stage and the second stage are partially mixed at the junction, and the second stage and the third stage are partially mixed at the junction;
D. c, ultrasonically vibrating the mixed powder obtained in the step C for 20 minutes;
E. d, pressing and forming the mixed powder obtained in the step D to obtain a biscuit;
F. and E, sintering the biscuit obtained in the step E according to the following conditions: heating to 350 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 1 hour, continuously heating to 600 ℃ and keeping the temperature for 3 hours, heating to 800 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 4 hours, and naturally cooling to room temperature to obtain the three-stage porous ceramic.
Specifically, the solvent in step A is ethanol.
Specifically, the press forming manner in the step E is dry press forming.
And a desulfurization and denitrification catalyst is loaded on the three-stage porous ceramic prepared by the preparation method, and the three-stage porous ceramic is arranged in a flue gas filtering device and used for catalytically oxidizing nitrides or sulfides in the flue gas.
The above examples are merely illustrative for clarity and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A three-stage porous ceramic, characterized in that: the ceramic material is prepared by sintering 50-80 parts of silicon nitride, 5-10 parts of sintering aid, 30-60 parts of binder, 2-15 parts of pore-forming agent and 2-15 parts of low-temperature molten glass powder according to parts by mass, wherein the pore-forming agent adopts three specifications including 60-100 mu m, 30-50 mu m and 1-10 mu m, and is respectively used as pore-forming agents of a first stage, a second stage and a third stage, and the first stage, the second stage and the third stage jointly form three-stage porous ceramic;
the sintering conditions are as follows: heating to 400 ℃ at a heating rate of 2-3 ℃/min, keeping the temperature for 0.5-2 hours, continuing to heat to 650 ℃ at 550 ℃ for 2-4 hours, heating to 900 ℃ at a heating rate of 1-2 ℃/min, keeping the temperature for 2-6 hours, and naturally cooling to room temperature.
2. The three-stage porous ceramic of claim 1, wherein: the sintering aid is one or combination of any more of aluminum oxide, magnesium oxide, zirconium oxide or yttrium oxide.
3. The three-stage porous ceramic of claim 1, wherein: the binder comprises a PVA solution or a PVB solution.
4. The three-stage porous ceramic of claim 1, wherein: the pore-forming agent is graphite, rice hulls, PMMA microspheres, starch or polystyrene microspheres.
5. The three-stage porous ceramic of claim 1, wherein: the arrangement sequence of the first stage, the second stage and the third stage is the first stage, the second stage and the third stage or the first stage, the third stage, the second stage or the second stage, the first stage and the third stage.
6. A method for preparing a three-stage porous ceramic according to claim 1, wherein: the method comprises the following steps:
A. mixing 50-80 parts of silicon nitride, 5-10 parts of sintering aid, 30-60 parts of binder, 2-15 parts of pore-forming agent and 2-15 parts of low-temperature molten glass powder according to the parts by mass, adding the mixture into a ball milling tank, adding a solvent which is 1.5-2 times of the total mass of the raw materials to obtain first-stage slurry, wherein the specification of the pore-forming agent is 60-100 mu m, and preparing second-stage slurry and third-stage slurry according to the same mass ratio, wherein the difference is that the specification of the pore-forming agent in the second-stage slurry is 30-50 mu m, and the specification of the pore-forming agent in the third-stage slurry is 1-10 mu m;
B. b, ball-milling the three parts of slurry obtained in the step A for 8-16 hours, taking out, drying and grinding at the temperature of 60-100 ℃ to obtain three parts of powder;
C. arranging the three powder materials obtained in the step B in a container according to the sequence of a first stage, a second stage and a third stage, wherein the first stage and the second stage are partially mixed at the junction, and the second stage and the third stage are partially mixed at the junction;
D. c, ultrasonically vibrating the mixed powder obtained in the step C for 5-30 minutes;
E. d, pressing and forming the mixed powder obtained in the step D to obtain a biscuit;
F. and E, sintering the biscuit obtained in the step E according to the following conditions: heating to 400 ℃ at the heating rate of 2-3 ℃/min, keeping the temperature for 0.5-2 hours, continuing to heat to 650 ℃ at 550 ℃ for 2-4 hours, heating to 900 ℃ at the heating rate of 1-2 ℃/min, keeping the temperature for 2-6 hours, and naturally cooling to room temperature to obtain the three-stage porous ceramic.
7. The method for preparing a three-stage porous ceramic according to claim 6, wherein: the solvent in the step A is one or more of deionized water, methanol, ethanol and acetone.
8. The method for preparing a three-stage porous ceramic according to claim 6, wherein: and E, performing dry pressing or extrusion molding.
9. The method for preparing a three-stage porous ceramic according to claim 6, wherein: and step A, 1-10 parts of desulfurization or denitrification catalyst is also added.
10. Use of the tertiary porous ceramic of claim 1 in a flue gas filtration unit.
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| CN115974559A (en) * | 2022-12-23 | 2023-04-18 | 衡阳凯新特种材料科技有限公司 | Low-thermal-conductivity silicon nitride wave-transparent ceramic material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040247855A1 (en) * | 2003-06-06 | 2004-12-09 | National Inst. Of Adv. Industrial Sci. And Tech. | Grading porous structure and its process |
| CN102701778A (en) * | 2012-06-01 | 2012-10-03 | 清华大学 | Preparation method for ceramic film with hierarchical pore structure |
| CN107445626A (en) * | 2017-06-20 | 2017-12-08 | 上海极率科技有限公司 | A kind of porous SiN ceramic preparation method of bore diameter gradient distribution |
| CN111099919A (en) * | 2020-01-14 | 2020-05-05 | 中国人民解放军国防科技大学 | Silicon nitride ceramic with hierarchical pore structure and preparation method thereof |
| CN111362705A (en) * | 2020-03-19 | 2020-07-03 | 江苏禾吉新材料科技有限公司 | Porous silicon nitride ceramic and preparation method thereof |
-
2020
- 2020-12-28 CN CN202011574931.4A patent/CN112592189A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040247855A1 (en) * | 2003-06-06 | 2004-12-09 | National Inst. Of Adv. Industrial Sci. And Tech. | Grading porous structure and its process |
| CN102701778A (en) * | 2012-06-01 | 2012-10-03 | 清华大学 | Preparation method for ceramic film with hierarchical pore structure |
| CN107445626A (en) * | 2017-06-20 | 2017-12-08 | 上海极率科技有限公司 | A kind of porous SiN ceramic preparation method of bore diameter gradient distribution |
| CN111099919A (en) * | 2020-01-14 | 2020-05-05 | 中国人民解放军国防科技大学 | Silicon nitride ceramic with hierarchical pore structure and preparation method thereof |
| CN111362705A (en) * | 2020-03-19 | 2020-07-03 | 江苏禾吉新材料科技有限公司 | Porous silicon nitride ceramic and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115974559A (en) * | 2022-12-23 | 2023-04-18 | 衡阳凯新特种材料科技有限公司 | Low-thermal-conductivity silicon nitride wave-transparent ceramic material |
| CN115974559B (en) * | 2022-12-23 | 2023-11-21 | 衡阳凯新特种材料科技有限公司 | Low-thermal-conductivity silicon nitride wave-transparent ceramic material |
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