CN101053720A - Desulphurizing and dust-removing integral gradient porous ceramic filter element preparing technology - Google Patents
Desulphurizing and dust-removing integral gradient porous ceramic filter element preparing technology Download PDFInfo
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- CN101053720A CN101053720A CN 200710013608 CN200710013608A CN101053720A CN 101053720 A CN101053720 A CN 101053720A CN 200710013608 CN200710013608 CN 200710013608 CN 200710013608 A CN200710013608 A CN 200710013608A CN 101053720 A CN101053720 A CN 101053720A
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- dust
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Abstract
The invention provides a preparation process for a desulfurization and dust removal integration gradient hole ceramics filter unit, comprising the process of batching, moulding and sintering, and being characterized in that: the gradient hole ceramics filter unit has inner and outer layers, wherein the fine material of inner layer is composed of Al2O3 with granularity between 80 to 150 mu m, high temperature anchoring agent, forming anchoring agent, hole-increasing agent and water, and that of outer layer comprises desulfurizer except the compositions of inner layer and the Al2O3 granularity of outer layer is 20-70 mu m less than that of inner layer. When moulding, the fine material of inner layer is loaded into the die after sieved, isostatic pressing at the pressure of 100-200MPa, then the fine material of outer layer is loaded, isostatic pressing at the pressure of 130-250MPa, and the rough is prepared. The rough is dried at room temperature and then send to high-temperature furnace to get the desulfurization and dust removal integration gradient hole ceramics filter unit with the temperature rising to 1150-1250 degree C and holding 1-3h. The invention uses the isostatic pressing technology, has a simple process, a short production cycle, a controlled aperture and an excellent property.
Description
Affiliated technical field
The invention provides a kind of preparation technology of desulphurizing and dust-removing integral gradient porous ceramic filter element, belong to the preparing technical field of porous ceramics.
Background technology
Porous ceramics is a kind of pore function ceramics, wherein contains a large amount of openings and connects pore, thereby have characteristics such as the huge porosity, pore surface area and adjustable pore shape, the three-dimensional distribution of pore, connection.Thereby it is more and more extensive to utilize porous ceramics to remove the method range of application of granule foreign and harmful and noxious substance.China starts late in this field, we can say for the preparation technology of porous ceramics and application and only to be in trial-production or trial period, only the Drinking Water clarifier input of being made up of candle is produced in batches, also is not used in the purification of the heating gas of IGCC power plant.High temperature coal gas purification mainly comprises desulfurization and dedusting two parts, and according to the process for purifying of routine, desulfurization and dedusting are unit operations independently, must be respectively through independent device filter and desulfurization reactor are finished separately.Existing at present about making the technology report of porous ceramics, as: 1, the patent No. is that 03112045.8 " preparation method of gradient porous ceramic filter element " adopts isostatic pressing method to prepare gradient porous ceramic filter element, has the high-temperature dust removal effect, shortcoming is that its ceramic filter element does not have desulfidation, and goes out the aggregate that is adopted for the ease of the mould pull-up, must in colloidal sol, fully mix, mist projection granulating then improves the flowability of aggregate, makes complicated process of preparation; 2, the patent No. is that " Hot Gas Cleaning Using For Refractory Ceramics Filter Element and preparation method thereof " shortcoming of 200410023972.9 is that ceramic filter element does not have desulfidation; 3, the patent No. is that 200310114505.2 " preparation technology with ceramic filter element of desulfidation " adopts slip casting method to prepare ceramic component, then zinc ferrite colloidal sol is filmed on ceramic filter element, shortcoming is to use the gypsum mold moulding, be subjected to the influence of the diversion of gypsum, the tube wall of element is thin, causes ceramic component intensity low; Be subjected to the influence of slip syneresis, cause the ceramic component pipe range short; Desulfurizing agent is a zinc ferrite, is coated on the ceramic component surface with solation, and desulfurizing agent content is few, and desulfurization amount is limited.
Summary of the invention
The purpose of this invention is to provide a kind ofly can overcome above-mentioned defective, technology is simple, with short production cycle, cost is low, the preparation technology of the desulphurizing and dust-removing integral gradient porous ceramic filter element of product excellent working performance, its technical scheme is:
Comprise batching, blank forming and sintering process, it is characterized in that: gradient porous ceramic filter element divides inside and outside two-layer, and the composition of internal layer is that granularity is the Al of 80～150 μ m
2O
3, high temperature adhesives, moulding bond and pore forming agent, its weight ratio is: 70～80: 5～10: 2～5: 10～20, add 1～6% water of above-mentioned gross weight mixed the internal layer powder, outer powder is on the basis of interior layer component, other adds 10～20% desulfurizing agent of internal layer gross weight, and outer Al
2O
3Grain graininess is less than internal layer Al
2O
3Grain graininess 20～70 μ m, during moulding, earlier with proportioning good in, after stirring in batch mixer respectively, outer powder sieves, again the internal layer powder is packed in the mould, isostatic compaction, its briquetting pressure are 100～200MPa, and mould is taken out in release, open the mould top cover, the outer powder of packing into, isostatic compaction, its briquetting pressure is 130～250MPa, prepare and have double-deck ceramic filter element base substrate, with base substrate drying at room temperature 1～3 day, put into high temperature furnace then, be warming up to 1150～1250 ℃, insulation 1～3h promptly makes desulphurizing and dust-removing integral gradient porous ceramic filter element.
The preparation technology of described desulphurizing and dust-removing integral gradient porous ceramic filter element, each mass percent of forming of high temperature adhesives is that cordierite accounts for 60～70%, mullite accounts for 30～40%;
The preparation technology of described desulphurizing and dust-removing integral gradient porous ceramic filter element, pore forming agent is a kind of in carbon dust, the charcoal or both any mixture, its granularity is 80～150 μ m.
The preparation technology of described desulphurizing and dust-removing integral gradient porous ceramic filter element, the moulding bond is a cellulose.
The preparation technology of described desulphurizing and dust-removing integral gradient porous ceramic filter element, desulfurizing agent is Fe
2O
3Or ZnFe
2O
4A kind of.
The preparation technology of described desulphurizing and dust-removing integral gradient porous ceramic filter element, floor height 20～50MPa in the outer pressure ratio of isostatic compaction.
The preparation technology of described desulphurizing and dust-removing integral gradient porous ceramic filter element, during sintering, the programming rate of high temperature furnace furnace temperature is 5～10 ℃/min.
The present invention compared with prior art has following advantage:
1, the present invention is with Al
2O
3Be aggregate, non-oxidizability is strong, and shaking property of heat resistanceheat resistant is good, the through-hole rate height.
2, the present invention adopts the cordierite mullite composite material as high-temperature agglomerant, generate cordierite mutually with mullite mutually, improved the intensity of ceramic filter element.
3, the present invention is owing to added desulfurizing agent in outer raw material, and the gradient porous ceramic filter element that makes has the dust-removal and desulfurizing effect concurrently, has simplified high temperature coal gas purification technology;
The outer aperture of the gradient porous ceramic filter element that 4, makes helps the dedusting effect less than internal layer aperture 5～20 μ m;
5, the present invention adopts equal pressing forming technology, and technology is simple, and is with short production cycle, and cost is low, and the product aperture is controlled, porosity height, and the intensity height, thermal shock resistance is good, is applicable to the filtration of high temperature coal (cigarette) gas.
The specific embodiment
Embodiment 1
1, batching: gradient porous ceramic filter element divides inside and outside two-layer, and the internal layer powder is the Al of 7000 grams, 100 μ m
2O
3, 600 the gram 50 μ m cordierites, 400 the gram 50 μ m mullites, 300 the gram celluloses, 1700 the gram 100 μ m carbon dusts, 300 the gram water mixture, outer powder be 7000 the gram 80 μ m Al
2O
3, 600 grams, 50 μ m cordierites, 400 grams, 50 μ m mullites, 300 gram celluloses, 1700 grams, 100 μ m carbon dusts, 1030 gram desulfurizing agent Fe
2O
3, 300 gram water mixture, sieve after the inside and outside layer powder that proportioning is good stirs in batch mixer respectively;
2, blank forming: isostatic compaction in the mould of earlier the internal layer powder being packed into, briquetting pressure is 140Mpa, mould is taken out in release, open the mould top cover, reinstall outer powder, isostatic compaction, briquetting pressure is 160Mpa, prepares to have double-deck ceramic filter element base substrate;
3, sintering: with base substrate drying at room temperature 3 days, put into high temperature furnace then, be warming up to 1250 ℃ with the speed of 5 ℃/min, insulation 3h promptly makes desulphurizing and dust-removing integral gradient porous ceramic filter element.
After tested, the performance indications of gained gradient porous ceramic filter element are as follows: the porosity＞40%, and internal layer average pore size 25 μ m, outer average pore size 20 μ m, filtering accuracy is about 1 μ m, the removal efficiency of sulphur＞95%, the compression strength＞15MPa of element.
Embodiment 2
1, batching: gradient porous ceramic filter element divides inside and outside two-layer, and the internal layer powder is the Al of 8000 grams, 120 μ m
2O
3, 300 the gram 20 μ m cordierites, 200 the gram 20 μ m mullites, 500 the gram celluloses, 1000 the gram 120 μ m charcoals, 300 the gram water mixture, outer powder be 8000 the gram 80 μ m Al
2O
3, 300 grams, 20 μ m cordierites, 200 grams, 20 μ m mullites, 500 gram celluloses, 1000 grams, 80 μ m charcoals, 2030 gram desulfurizing agent Fe
2O
3, 300 gram water mixture, sieve after the inside and outside layer powder that proportioning is good stirs in batch mixer respectively;
2, blank forming: isostatic compaction in the mould of earlier the internal layer powder being packed into, briquetting pressure is 120Mpa, mould is taken out in release, open the mould top cover, reinstall outer powder, isostatic compaction, briquetting pressure is 160Mpa, prepares to have double-deck ceramic filter element base substrate;
3, sintering: with base substrate drying at room temperature 3 days, put into high temperature furnace then, be warming up to 1200 ℃ with the speed of 10 ℃/min, insulation 2h promptly makes desulphurizing and dust-removing integral gradient porous ceramic filter element.
After tested, the performance indications of gained gradient porous ceramic filter element are as follows: the porosity＞40%, and internal layer average pore size 30 μ m, outer average pore size 20 μ m, filtering accuracy is about 1 μ m, the removal efficiency of sulphur＞95%, the compression strength＞15MPa of element.
Embodiment 3
1, batching: gradient porous ceramic filter element divides inside and outside two-layer, and the internal layer powder is the Al of 7500 grams, 120 μ m
2O
3, 700 the gram 10 μ m cordierites, 300 the gram 10 μ m mullites, 400 the gram celluloses, 1100 the gram 120 μ m carbon dusts, 600 the gram water mixture, outer powder be 7500 the gram 60 μ m Al
2O
3, 700 grams, 10 μ m cordierites, 300 grams, 10 μ m mullites, 400 gram celluloses, 1600 grams, 80 μ m carbon dusts, 1500 gram desulfurizing agent ZnFe
2O
4, 600 gram water mixture, sieve after the inside and outside layer powder that proportioning is good stirs in batch mixer respectively;
2, blank forming: isostatic compaction in the mould of earlier the internal layer powder being packed into, briquetting pressure is 140Mpa, mould is taken out in release, open the mould top cover, reinstall outer powder, isostatic compaction, briquetting pressure is 160Mpa, prepares to have double-deck ceramic filter element base substrate;
3, sintering: with base substrate drying at room temperature 1 day, put into high temperature furnace then, be warming up to 1180 ℃ with the speed of 10 ℃/min, insulation 2h promptly makes desulphurizing and dust-removing integral gradient porous ceramic filter element.
After tested, the performance indications of gained gradient porous ceramic filter element are as follows: the porosity＞40%, and internal layer average pore size 30 μ m, outer average pore size 15 μ m, filtering accuracy is about 1 μ m, the removal efficiency of sulphur＞95%, the compression strength＞15MPa of element.
Embodiment 4
1, batching: gradient porous ceramic filter element divides inside and outside two-layer, and the internal layer powder is the Al of 7800 grams, 150 μ m
2O
3, 560 the gram 10 μ m cordierites, 240 the gram 10 μ m mullites, 300 the gram celluloses, 500 the gram 150 μ m charcoals, 600 the gram 100 μ m carbon dusts, 500 the gram water mixture, outer powder be 7800 the gram 80 μ m Al
2O
3, 560 grams, 10 μ m cordierites, the charcoals of 240 grams, 10 μ m mullites, 300 gram celluloses, 500 grams, 100 μ m, 600 grams, 100 μ m carbon dusts, 1500 gram desulfurizing agent ZnFe
2O
4, 600 gram water mixture, sieve after the inside and outside layer powder that proportioning is good stirs in batch mixer respectively;
2, blank forming: isostatic compaction in the mould of earlier the internal layer powder being packed into, briquetting pressure is 160Mpa, mould is taken out in release, open the mould top cover, reinstall outer powder, isostatic compaction, briquetting pressure is 200Mpa, prepares to have double-deck ceramic filter element base substrate;
3, sintering: with base substrate drying at room temperature 1 day, put into high temperature furnace then, be warming up to 1180 ℃ with the speed of 10 ℃/min, insulation 2h promptly makes desulphurizing and dust-removing integral gradient porous ceramic filter element.
After tested, the performance indications of gained gradient porous ceramic filter element are as follows: the porosity＞40%, and internal layer average pore size 37 μ m, outer average pore size 20 μ m, filtering accuracy is about 1 μ m, the removal efficiency of sulphur＞95%, the compression strength＞15MPa of element.
Claims (7)
1, a kind of preparation technology of desulphurizing and dust-removing integral gradient porous ceramic filter element comprises batching, blank forming and sintering process, it is characterized in that: gradient porous ceramic filter element divides inside and outside two-layer, and the composition of internal layer is that granularity is the Al of 80～150 μ m
2O
3, high temperature adhesives, moulding bond and pore forming agent, its weight ratio is: 70～80: 5～10: 2～5: 10～20, add 1～6% water of above-mentioned gross weight mixed the internal layer powder, outer powder is on the basis of interior layer component, other adds 10～20% desulfurizing agent of internal layer gross weight, and outer Al
2O
3Grain graininess is less than internal layer Al
2O
3Grain graininess 20～70 μ m, during moulding, earlier with proportioning good in, after stirring in batch mixer respectively, outer powder sieves, again the internal layer powder is packed in the mould, isostatic compaction, its briquetting pressure are 100～200MPa, and mould is taken out in release, open the mould top cover, the outer powder of packing into, isostatic compaction, its briquetting pressure is 130～250MPa, prepare and have double-deck ceramic filter element base substrate, with base substrate drying at room temperature 1～3 day, put into high temperature furnace then, be warming up to 1150～1250 ℃, insulation 1～3h promptly makes desulphurizing and dust-removing integral gradient porous ceramic filter element.
2, the preparation technology of desulphurizing and dust-removing integral gradient porous ceramic filter element as claimed in claim 1 is characterized in that: each mass percent of forming of high temperature adhesives is that cordierite accounts for 60～70%, and mullite accounts for 30～40%.
3, the preparation technology of desulphurizing and dust-removing integral gradient porous ceramic filter element as claimed in claim 1 is characterized in that: pore forming agent is a kind of in carbon dust, the charcoal or both any mixture, and its granularity is 80～150 μ m.
4, the preparation technology of desulphurizing and dust-removing integral gradient porous ceramic filter element as claimed in claim 1 is characterized in that: the moulding bond is a cellulose.
5, the preparation technology of desulphurizing and dust-removing integral gradient porous ceramic filter element as claimed in claim 1 is characterized in that: desulfurizing agent is Fe
2O
3Or ZnFe
2O
4A kind of.
6, the preparation technology of desulphurizing and dust-removing integral gradient porous ceramic filter element as claimed in claim 1 is characterized in that: floor height 20～50MPa in the outer pressure ratio of isostatic compaction.
7, the preparation technology of desulphurizing and dust-removing integral gradient porous ceramic filter element as claimed in claim 1 is characterized in that: during sintering, the programming rate of high temperature furnace furnace temperature is 5～10 ℃/min.
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| CNB2007100136088A CN100409922C (en) | 2007-02-07 | 2007-02-07 | Desulphurizing and dust-removing integral gradient porous ceramic filter element preparing technology |
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| CNB2007100136088A CN100409922C (en) | 2007-02-07 | 2007-02-07 | Desulphurizing and dust-removing integral gradient porous ceramic filter element preparing technology |
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| CN101053720A true CN101053720A (en) | 2007-10-17 |
| CN100409922C CN100409922C (en) | 2008-08-13 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344300A (en) * | 2011-06-30 | 2012-02-08 | 山东理工大学 | Isostatic pressing method for preparing ceramic filtering element for high temperature gas purification |
| CN102580404A (en) * | 2012-02-06 | 2012-07-18 | 江苏云才材料有限公司 | Method for preparing asymmetric stainless steel filter disc |
| CN109053214A (en) * | 2018-11-15 | 2018-12-21 | 广东金意陶陶瓷集团有限公司 | A kind of technique and foamed ceramic material of layering system material cloth production foamed ceramic |
| CN115196976A (en) * | 2022-06-30 | 2022-10-18 | 山东工业陶瓷研究设计院有限公司 | Gradient porous ceramic and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02290211A (en) * | 1989-04-28 | 1990-11-30 | Kanebo Ltd | Ceramic filter and manufacture thereof |
| CN1108906C (en) * | 2000-06-30 | 2003-05-21 | 隋贤栋 | Gradient ceramic-film tube and its preparation |
| US6918941B2 (en) * | 2002-08-05 | 2005-07-19 | Battelle Energy Alliance, Llc | Cermet materials, self-cleaning cermet filters, apparatus and systems employing same |
| CN1253413C (en) * | 2003-12-18 | 2006-04-26 | 山东理工大学 | Method for preparing porous ceramic by polycrystalline Al#-[2]O#-[3] fiber preforming method |
-
2007
- 2007-02-07 CN CNB2007100136088A patent/CN100409922C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102344300A (en) * | 2011-06-30 | 2012-02-08 | 山东理工大学 | Isostatic pressing method for preparing ceramic filtering element for high temperature gas purification |
| CN102580404A (en) * | 2012-02-06 | 2012-07-18 | 江苏云才材料有限公司 | Method for preparing asymmetric stainless steel filter disc |
| CN102580404B (en) * | 2012-02-06 | 2014-05-28 | 江苏云才材料有限公司 | Method for preparing asymmetric stainless steel filter disc |
| CN109053214A (en) * | 2018-11-15 | 2018-12-21 | 广东金意陶陶瓷集团有限公司 | A kind of technique and foamed ceramic material of layering system material cloth production foamed ceramic |
| CN109053214B (en) * | 2018-11-15 | 2019-03-15 | 广东金意陶陶瓷集团有限公司 | A kind of technique and foamed ceramic material of layering system material cloth production foamed ceramic |
| CN115196976A (en) * | 2022-06-30 | 2022-10-18 | 山东工业陶瓷研究设计院有限公司 | Gradient porous ceramic and preparation method thereof |
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| CN100409922C (en) | 2008-08-13 |
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Application publication date: 20071017 Assignee: Zibo Yonghua Filters Make Co., Ltd. Assignor: Shandong University of Technology Contract record no.: 2010370000080 Denomination of invention: Desulphurizing and dust-removing integral gradient porous ceramic filter element preparing technology Granted publication date: 20080813 License type: Exclusive License Record date: 20100311 |
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