CN101053721A - Desulphurizing and dust-removing integral gradient porous ceramic filter element preparing method - Google Patents

Desulphurizing and dust-removing integral gradient porous ceramic filter element preparing method Download PDF

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Publication number
CN101053721A
CN101053721A CN 200710013609 CN200710013609A CN101053721A CN 101053721 A CN101053721 A CN 101053721A CN 200710013609 CN200710013609 CN 200710013609 CN 200710013609 A CN200710013609 A CN 200710013609A CN 101053721 A CN101053721 A CN 101053721A
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filter element
ceramic filter
dust
porous ceramic
desulphurizing
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CN100423810C (en
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魏春城
田贵山
唐竹兴
孟凡涛
许珂敬
牛俊粉
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Shandong University of Technology
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Shandong University of Technology
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Abstract

The invention provides a preparation process for a desulfurization and dust removal integration gradient hole ceramics filter unit, comprising 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 SiC 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 SiC 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

The preparation method of desulphurizing and dust-removing integral gradient porous ceramic filter element
Affiliated technical field
The invention provides a kind of preparation method 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, yield rate is high, with short production cycle, cost is low, the preparation method 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, it is characterized in that: gradient porous ceramic filter element divides inside and outside two-layer, the composition of internal layer is that granularity is the SiC of 80~150 μ m, 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 SiC grain graininess is less than internal layer SiC grain 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 is 100~200MPa, 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, prepares to 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 method of described desulphurizing and dust-removing integral gradient porous ceramic filter element, each mass percent of forming of high temperature adhesives is that feldspar accounts for 20~60%, and kaolin accounts for 20~60%, and bentonite accounts for 20~60%.
The preparation method 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 method of described desulphurizing and dust-removing integral gradient porous ceramic filter element, the moulding bond is a cellulose.
The preparation method 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 method 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 method 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 aggregate with SiC, and the product deformation rate is low, the yield rate height;
2, 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 3, makes helps the dedusting effect less than internal layer aperture 5~20 μ m;
4, 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, the internal layer powder is that SiC, 600 grams, 10 μ m feldspars, 200 grams, 10 μ m kaolins, 200 grams, the 10 μ m bentonites, 300 of 7000 grams, 100 μ m restrain the carbon dust of celluloses, 1700 grams, 100 μ m, the mixture of 300 gram water, outer powder is SiC, 600 grams, 10 μ m feldspars, 200 grams, 10 μ m kaolins, 200 grams, 10 μ m bentonites, 300 gram celluloses, 1700 grams, the 100 μ m carbon dusts of 7000 grams, 80 μ m, 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 23 μ m, outer average pore size 18 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, the internal layer powder is that SiC, 250 grams, 10 μ m feldspars, 125 grams, 10 μ m kaolins, 125 grams, the 10 μ m bentonites, 500 of 8000 grams, 120 μ m restrain the charcoal of celluloses, 1000 grams, 120 μ m, the mixture of 300 gram water, outer powder is SiC, 250 grams, 10 μ m feldspars, 125 grams, 10 μ m kaolins, 125 grams, 10 μ m bentonites, 500 gram celluloses, 1000 grams, the 80 μ m charcoals of 8000 grams, 80 μ m, 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 28 μ m, outer average pore size 18 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, the internal layer powder is that SiC, 400 grams, 10 μ m feldspars, 300 grams, 10 μ m kaolins, 300 grams, the 10 μ m bentonites, 400 of 7500 grams, 120 μ m restrain the carbon dust of celluloses, 1100 grams, 120 μ m, the mixture of 600 gram water, outer powder is SiC, 400 grams, 10 μ m feldspars, 300 grams, 10 μ m kaolins, 300 grams, 10 μ m bentonites, 400 gram celluloses, 1600 grams, the 80 μ m carbon dusts of 7500 grams, 60 μ m, 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 28 μ m, outer average pore size 13 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, the internal layer powder is that SiC, 400 grams, the 10 μ m feldspars, 200 of 7800 grams, 150 μ m restrain 10 μ m kaolins, 200 grams, 10 μ m bentonites, 300 restrain the charcoal of celluloses, 500 grams, 150 μ m, the mixture that 600 grams, 100 μ m carbon dusts, 500 restrain water, outer powder is SiC, 400 grams, 10 μ m feldspars, 200 grams, 10 μ m kaolins, 200 grams, 10 μ m bentonites, 300 gram celluloses, the charcoal of 500 grams, 100 μ m, 600 grams, the 100 μ m carbon dusts of 7800 grams, 80 μ m, 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 35 μ m, outer average pore size 18 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 method of desulphurizing and dust-removing integral gradient porous ceramic filter element, comprise batching, blank forming and sintering, it is characterized in that: gradient porous ceramic filter element divides inside and outside two-layer, the composition of internal layer is that granularity is the SiC of 80~150 μ m, 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 SiC grain graininess is less than internal layer SiC grain 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 is 100~200MPa, 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 method 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 feldspar accounts for 20~60%, and kaolin accounts for 20~60%, and bentonite accounts for 20~60%.
3, the preparation method 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 method 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 method 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 method 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 method 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.
CNB2007100136092A 2007-02-07 2007-02-07 Desulphurizing and dust-removing integral gradient porous ceramic filter element preparing method Expired - Fee Related CN100423810C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
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CN102417366A (en) * 2011-08-30 2012-04-18 北京理工大学 Pore gradient silicon carbide porous ceramic and preparation method thereof
CN102718494A (en) * 2012-06-21 2012-10-10 海南大学 Preparation method of composite silicon carbide ceramic filter membrane material
CN105879553A (en) * 2016-05-26 2016-08-24 张锐 Desulphurization equipment
CN112811911A (en) * 2021-01-07 2021-05-18 盐城工学院 Dust removal and desulfurization integrated silicon nitride porous ceramic and preparation method thereof

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1057711C (en) * 1998-03-15 2000-10-25 江苏省宜兴非金属化工机械厂 Ceramic filtering board for separating solid from liquid and preparing process
JP2003010616A (en) * 2001-06-29 2003-01-14 Ngk Insulators Ltd Honeycomb structure body
US6918941B2 (en) * 2002-08-05 2005-07-19 Battelle Energy Alliance, Llc Cermet materials, self-cleaning cermet filters, apparatus and systems employing same
CN1187291C (en) * 2003-04-11 2005-02-02 中国科学院上海硅酸盐研究所 Preparation method of silicon carbide porous ceramic using yeast powder as pore forming agent

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102417366A (en) * 2011-08-30 2012-04-18 北京理工大学 Pore gradient silicon carbide porous ceramic and preparation method thereof
CN102417366B (en) * 2011-08-30 2013-08-07 北京理工大学 Pore gradient silicon carbide porous ceramic and preparation method thereof
CN102718494A (en) * 2012-06-21 2012-10-10 海南大学 Preparation method of composite silicon carbide ceramic filter membrane material
CN105879553A (en) * 2016-05-26 2016-08-24 张锐 Desulphurization equipment
CN105879553B (en) * 2016-05-26 2018-12-21 新疆金禾山能源科技有限公司 A kind of desulphurization plant
CN112811911A (en) * 2021-01-07 2021-05-18 盐城工学院 Dust removal and desulfurization integrated silicon nitride porous ceramic and preparation method thereof

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