CN102351558A - Gelcasting based method for preparing ceramic filtering element for high temperature gas purification - Google Patents

Gelcasting based method for preparing ceramic filtering element for high temperature gas purification Download PDF

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Publication number
CN102351558A
CN102351558A CN2011101821740A CN201110182174A CN102351558A CN 102351558 A CN102351558 A CN 102351558A CN 2011101821740 A CN2011101821740 A CN 2011101821740A CN 201110182174 A CN201110182174 A CN 201110182174A CN 102351558 A CN102351558 A CN 102351558A
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high temperature
gram
filter element
ceramic filter
powder
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CN2011101821740A
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魏春城
张艳平
郑明文
于萧
田贵山
冯柳
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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 gelcasting based method for preparing a ceramic filtering element for high temperature gas purification. The method comprises steps that (1) batching: the ceramic filtering element comprises an upper layer, a middle layer and a lower layer; the lower layer contains powders of aggregate with a granularity of 100-150 mum, high temperature binder and pore-forming agent; the middle layer comprises powders of aggregate with a granularity of 40-100 mum and high temperature binder; the upper layer comprises powders of aggregate with a granularity of 10-40 mum and high temperature binder; three layers of powders are respectively dispersed in organic solutions, stirred uniformly in vacuum to form mixed liquids; (2) body formation: three mixed liquids are respectively added with an initiator and a catalyst to mix into three gels; the lower layer gel is first poured into a die for solidification, then the middle layer gel is solidified, finally the upper layer gel is solidified; a ceramic filtering element body is obtained after demoulding; (3) sintering: the body is dried at room temperature and sintered to obtain the ceramic filtering element. The ceramic filtering element prepared by the method of the invention has high boss compactness, strong strength and long service life.

Description

The notes type that congeals into prepares the method for high temperature gas cleaning with ceramic filter element
Technical field
The present invention provides a kind of notes type that congeals into to prepare the method for high temperature gas cleaning with ceramic filter element, belongs to the preparing technical field of porous ceramics.
Background technology
High temperature gas cleaning requires use temperature high (use temperature is greater than 300 ℃) with ceramic filter element; Void content high (void content>45%); Filtering accuracy reaches 1 μ m; Pore size distribution is narrow; Flexural strength>15MPa; Long service life, suitable high-temperature gas filter use be of a size of ф 60mm * 10mm *>15000mm has the ceramic filter element of ф 80mm * 20mm boss.Because ceramic filter element length is above 1.5 meters; Flexural strength is low; In working order down; Be easy to fracture; Damage; Particularly near the boss position; Because stress concentration ruptures more easily, and change ceramic filter element length consuming time, maintenance is inconvenient, and (general two overlap or overlap more the porcelain filter parallel connection uses; Every cover porcelain filter has up to a hundred of ceramic filter elements); And because the filtering element porous, void content is high, surface irregularity; Therefore the airtight difficulty in boss position improves the work-ing life that the compactness at boss position can improve ceramic filter element.
Summary of the invention
The boss compactness that the purpose of this invention is to provide a kind of ceramic filter element that can overcome above-mentioned defective, preparation is high, intensity is big, notes long service life congeal into, and type prepares the method for high temperature gas cleaning with ceramic filter element.Its technical scheme is:
A kind of notes type that congeals into prepares the method for high temperature gas cleaning with ceramic filter element; Comprise batching, blank forming and sintering; It is characterized in that: (1) batching; Ceramic filter element is a gradient up and down; The number of plies is 3 layers, and the composition of lower floor's powder is that granularity is aggregate, high temperature adhesives and the pore forming agent of 100~150 μ m, and weight ratio is: 80~90: 10~20: 0~5; High temperature adhesives is made up of wilkinite and talcum, and both mass percents are 40~60: 40~60; Middle level length is 50~100mm, and it is that granularity is aggregate and the high temperature adhesives of 40~100 μ m that powder is formed, and weight ratio is: 80~90: 10~20; The upper strata is a boss, and it is that granularity is aggregate and the high temperature adhesives of 10~40 μ m that powder is formed, and weight ratio is: 80~90: 10~20; 3 layers of powder that proportioning is good are dispersed in respectively that vacuum stirring evenly forms mixed solution in the organic solution; Organic solution consist of organic monomer, linking agent, dispersion agent and water, add-on is 3~5%, 0.1~2%, 0.1~5% and 30~50% of each layer powder gross weight; (2) blank forming; 0.1~0.5% initiator and 0.1~0.5% catalyzer that in three kinds of mixed solutions, add each layer powder gross weight respectively; Be mixed into three kinds of gels; Earlier pour into lower floor's gel in the mould, 60~80 ℃ of curing; Pour 60~80 ℃ of curing of middle level gel again into; Pour 60~80 ℃ of curing of upper strata gel at last into, obtain the ceramic filter element base substrate after the demoulding; (3) sintering with base substrate drying at room temperature 1~3 day, is put into High Temperature Furnaces Heating Apparatus then, is warming up to 1150~1300 ℃ of insulation 1~8h, promptly makes ceramic filter element.
The described notes type that congeals into prepares the method for high temperature gas cleaning with ceramic filter element; Organic monomer is an acrylamide; Linking agent is N; N '-methylene-bisacrylamide; Dispersion agent is a kind of in poly amic acid, polyoxyethylene glycol or the polyvinyl alcohol; Initiator is an ammonium persulphate, and catalyzer is a Tetramethyl Ethylene Diamine.
The described notes type that congeals into prepares the method for high temperature gas cleaning with ceramic filter element, and aggregate is aluminum oxide or silicon carbide; Pore forming agent is a kind of in carbon black, the charcoal or both any mixture, and its granularity is 100~150 μ m.
The present invention compared with prior art has following advantage:
1, the particles of aggregates of the ceramic filter element boss of the present invention's preparation is tiny, makes sintering after-filtration element boss surface smooth, and intensity is high, helps the sealing of ceramic filter element, and has strengthened the anti-breaking tenacity of ceramic filter element;
2, the present invention adopts talcum as high temperature adhesives, when moulding, because the steatitic oilness helps the green compact demoulding, improves yield rate;
3, gradient about the ceramic filter element of the present invention's preparation, the product controllable aperture, interfacial bonding property is good;
4, the present invention adopts gel injection molding and forming technology, and technology is simple, and equipment requirements is low, and production efficiency is high, and yield rate is high, helps suitability for industrialized production.
Embodiment
Embodiment 1
1, batching: during ceramic filter element divide to be gone up following 3 layers; The carbon black of the aluminum oxide that consists of 800 grams, 100 μ m of lower floor's powder, 100 gram talcums, 80 gram wilkinites and 20 grams, 100 μ m; Organic solution is 30 gram acrylamides, 1 gram N; The mixture of N '-methylene-bisacrylamide, 10 gram poly amic acids and 300 gram water; Organic solution is added vacuum stirring 120min in lower floor's powder, get lower floor's mixed solution; The aluminum oxide that consists of 800 grams, 40 μ m of middle level powder, 100 gram talcums and 100 gram wilkinites; Organic solution is 40 gram acrylamides, 5 gram N; The mixture of N '-methylene-bisacrylamide, 40 gram poly amic acids and 500 gram water; Organic solution is added vacuum stirring 120min in the powder of middle level, get the middle level mixed solution; The aluminum oxide that consists of 800 grams, 10 μ m of upper strata powder, 100 gram talcums and 100 gram wilkinites; Organic solution is 40 gram acrylamides, 20 gram N; The mixture of N '-methylene-bisacrylamide, 40 gram poly amic acids and 500 gram water; Organic solution is added vacuum stirring 120min in the powder of upper strata, get the upper strata mixed solution;
2, blank forming: in three kinds of mixed solutions, add 1 gram ammonium persulphate and 5 gram Tetramethyl Ethylene Diamines respectively; Mix and form lower floor, middle level and upper strata gel; In mould, pour earlier lower floor's gel into and solidify 0.5h for 60 ℃; Pour the middle level gel again into and solidify 1h for 60 ℃; Pour the upper strata gel at last into and solidify 10h for 60 ℃, obtain the ceramic filter element base substrate after the demoulding;
3, sintering: with base substrate drying at room temperature 3 days, put into High Temperature Furnaces Heating Apparatus then, be warming up to 1250 ℃ of insulation 4h, promptly make ceramic filter element.
Embodiment 2
1, batching: during ceramic filter element divide to be gone up following 3 layers; The carbon black of the aluminum oxide that consists of 800 grams, 150 μ m of lower floor's powder, 80 gram talcums, 80 gram wilkinites, 20 grams, 80 μ m and the charcoal of 20 grams, 80 μ m; Organic solution is 40 gram acrylamides, 5 gram N; The mixture of N '-methylene-bisacrylamide, 50 gram polyoxyethylene glycol and 500 gram water; Organic solution is added vacuum stirring 60min in lower floor's powder, get lower floor's mixed solution; The aluminum oxide that consists of 800 grams, 100 μ m of middle level powder, 100 gram talcums and 100 gram wilkinites; Organic solution is 40 gram acrylamides, 5 gram N; The mixture of N '-methylene-bisacrylamide, 40 gram polyoxyethylene glycol and 500 gram water; Organic solution is added vacuum stirring 60min in the powder of middle level, get the middle level mixed solution; The aluminum oxide that consists of 900 grams, 40 μ m of upper strata powder, 60 gram talcums and 40 gram wilkinites; Organic solution is 40 gram acrylamides, 5 gram N; The mixture of N '-methylene-bisacrylamide, 40 gram polyoxyethylene glycol and 500 gram water; Organic solution is added vacuum stirring 60min in the powder of upper strata, get the upper strata mixed solution;
2, blank forming: add in lower floor's mixed solution and add 2 gram ammonium persulphates and 3 gram Tetramethyl Ethylene Diamines in 1 gram ammonium persulphate and 5 gram Tetramethyl Ethylene Diamines, the middle level mixed solution; Add 3 gram ammonium persulphates and 3 gram Tetramethyl Ethylene Diamines in the mixed solution of upper strata; Mix and form lower floor, middle level and upper strata gel; In mould, pour earlier lower floor's gel into and solidify 1h for 60 ℃; Pour the middle level gel again into and solidify 1h for 60 ℃; Pour the upper strata gel at last into and solidify 10h for 60 ℃, obtain the ceramic filter element base substrate after the demoulding;
3, sintering: with base substrate drying at room temperature 3 days, put into High Temperature Furnaces Heating Apparatus then, be warming up to 1300 ℃ of insulation 4h, promptly make ceramic filter element.
Embodiment 3
1, batching: during ceramic filter element divide to be gone up following 3 layers; The silicon carbide that consists of 900 grams, 120 μ m of lower floor's powder, 60 gram talcums, 40 gram wilkinites; Organic solution is 50 gram acrylamides, 20 gram N; The mixture of N '-methylene-bisacrylamide, 50 gram poly amic acids and 500 gram water; Organic solution is added vacuum stirring 120min in lower floor's powder, get lower floor's mixed solution; The silicon carbide that consists of 900 grams, 80 μ m of middle level powder, 50 gram talcums and 50 gram wilkinites; Organic solution is 40 gram acrylamides, 10 gram N; The mixture of N '-methylene-bisacrylamide, 40 gram poly amic acids and 400 gram water; Organic solution is added vacuum stirring 120min in the powder of middle level, get the middle level mixed solution; The silicon carbide that consists of 800 grams, 30 μ m of upper strata powder, 100 gram talcums and 100 gram wilkinites; Organic solution is 40 gram acrylamides, 5 gram N; The mixture of N '-methylene-bisacrylamide, 40 gram poly amic acids and 500 gram water; Organic solution is added vacuum stirring 120min in the powder of upper strata, get the upper strata mixed solution;
2, blank forming: in three kinds of mixed solutions, add 5 gram ammonium persulphates and 5 gram Tetramethyl Ethylene Diamines respectively; Mix and form lower floor, middle level and upper strata gel; In mould, pour earlier lower floor's gel into and solidify 2h for 60 ℃; Pour the middle level gel again into and solidify 2h for 60 ℃; Pour the upper strata gel at last into and solidify 8h for 60 ℃, obtain the ceramic filter element base substrate after the demoulding;
3, sintering: with base substrate drying at room temperature 3 days, put into High Temperature Furnaces Heating Apparatus then, be warming up to 1150 ℃ of insulation 1h, promptly make ceramic filter element.
Embodiment 4
1, batching: during ceramic filter element divide to be gone up following 3 layers; The charcoal of the silicon carbide that consists of 850 grams, 150 μ m of lower floor's powder, 50 gram talcums, 50 gram wilkinites and 50 grams, 150 μ m; Organic solution is 40 gram acrylamides, 5 gram N; The mixture of N '-methylene-bisacrylamide, 50 gram polyvinyl alcohol and 500 gram water; Organic solution is added vacuum stirring 120min in lower floor's powder, get lower floor's mixed solution; The silicon carbide that consists of 850 grams, 100 μ m of middle level powder, 75 gram talcums and 75 gram wilkinites; Organic solution is 40 gram acrylamides, 5 gram N; The mixture of N '-methylene-bisacrylamide, 40 gram polyvinyl alcohol and 500 gram water; Organic solution is added vacuum stirring 120min in the powder of middle level, get the middle level mixed solution; The silicon carbide that consists of 850 grams, 40 μ m of upper strata powder, 75 gram talcums and 75 gram wilkinites; Organic solution is 40 gram acrylamides, 5 gram N; The mixture of N '-methylene-bisacrylamide, 40 gram polyvinyl alcohol and 500 gram water; Organic solution is added vacuum stirring 120min in the powder of upper strata, get the upper strata mixed solution;
2, blank forming: add in lower floor's mixed solution and add 2 gram ammonium persulphates and 3 gram Tetramethyl Ethylene Diamines in 1 gram ammonium persulphate and 5 gram Tetramethyl Ethylene Diamines, the middle level mixed solution; Add 3 gram ammonium persulphates and 3 gram Tetramethyl Ethylene Diamines in the mixed solution of upper strata; Mix and form lower floor, middle level and upper strata gel; In mould, pour earlier lower floor's gel into and solidify 1h for 60 ℃; Pour the middle level gel again into and solidify 1h for 60 ℃; Pour the upper strata gel at last into and solidify 10h for 60 ℃, obtain the ceramic filter element base substrate after the demoulding;
3, sintering: with base substrate drying at room temperature 3 days, put into High Temperature Furnaces Heating Apparatus then, be warming up to 1200 ℃ of insulation 1h, promptly make ceramic filter element.

Claims (4)

1. the notes type that congeals into prepares the method for high temperature gas cleaning with ceramic filter element; Comprise batching, blank forming and sintering; It is characterized in that: (1) batching; Ceramic filter element is a gradient up and down; The number of plies is 3 layers, and the composition of lower floor's powder is that granularity is aggregate, high temperature adhesives and the pore forming agent of 100~150 μ m, and weight ratio is: 80~90: 10~20: 0~5; High temperature adhesives is made up of wilkinite and talcum, and both mass percents are 40~60: 40~60; Middle level length is 50~100mm, and it is that granularity is aggregate and the high temperature adhesives of 40~100 μ m that powder is formed, and weight ratio is: 80~90: 10~20; The upper strata is a boss, and it is that granularity is aggregate and the high temperature adhesives of 10~40 μ m that powder is formed, and weight ratio is: 80~90: 10~20; 3 layers of powder that proportioning is good are dispersed in respectively that vacuum stirring evenly forms mixed solution in the organic solution; Organic solution consist of organic monomer, linking agent, dispersion agent and water, add-on is 3~5%, 0.1~2%, 0.1~5% and 30~50% of each layer powder gross weight; (2) blank forming; 0.1~0.5% initiator and 0.1~0.5% catalyzer that in three kinds of mixed solutions, add each layer powder gross weight respectively; Be mixed into three kinds of gels; Earlier pour into lower floor's gel in the mould, 60~80 ℃ of curing; Pour 60~80 ℃ of curing of middle level gel again into; Pour 60~80 ℃ of curing of upper strata gel at last into, obtain the ceramic filter element base substrate after the demoulding; (3) sintering with base substrate drying at room temperature 1~3 day, is put into High Temperature Furnaces Heating Apparatus then, is warming up to 1150~1300 ℃ of insulation 1~8h, promptly makes ceramic filter element.
2. the notes as claimed in claim 1 type that congeals into prepares the method for high temperature gas cleaning with ceramic filter element; It is characterized in that: organic monomer is an acrylamide; Linking agent is N; N '-methylene-bisacrylamide; Dispersion agent is a kind of in poly amic acid, polyoxyethylene glycol or the polyvinyl alcohol; Initiator is an ammonium persulphate, and catalyzer is a Tetramethyl Ethylene Diamine.
3. the notes as claimed in claim 1 type that congeals into prepares the method for high temperature gas cleaning with ceramic filter element, and it is characterized in that: aggregate is aluminum oxide or silicon carbide.
4. the notes as claimed in claim 1 type that congeals into prepares the method for high temperature gas cleaning with ceramic filter element, it is characterized in that: pore forming agent is a kind of in carbon black, the charcoal or both any mixture, and its granularity is 100~150 μ m.
CN2011101821740A 2011-06-30 2011-06-30 Gelcasting based method for preparing ceramic filtering element for high temperature gas purification Pending CN102351558A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103342544A (en) * 2013-07-03 2013-10-09 镇江市江南矿山机电设备有限公司 Method for preparing porous alumina ceramic
CN114349519A (en) * 2022-01-19 2022-04-15 江苏宝利金材科技有限公司 Slurry formula and production process of gel-casting ceramic filter

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02192479A (en) * 1989-01-19 1990-07-30 Idemitsu Kosan Co Ltd Production of ceramic foamed product having fine pores
US5087277A (en) * 1991-03-28 1992-02-11 Virginia Polytechnic Institute High temperature ceramic particulate filter
JP2004195396A (en) * 2002-12-19 2004-07-15 Asahi Glass Co Ltd Ceramic filter and its manufacturing method
CN1532170A (en) * 2003-03-25 2004-09-29 山东理工大学 Process for preparing gradient porous ceramic filter element
CN101696110A (en) * 2009-10-23 2010-04-21 山东理工大学 Preparation method of two-layer ceramic filtering element with desulfurizing performance

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02192479A (en) * 1989-01-19 1990-07-30 Idemitsu Kosan Co Ltd Production of ceramic foamed product having fine pores
US5087277A (en) * 1991-03-28 1992-02-11 Virginia Polytechnic Institute High temperature ceramic particulate filter
JP2004195396A (en) * 2002-12-19 2004-07-15 Asahi Glass Co Ltd Ceramic filter and its manufacturing method
CN1532170A (en) * 2003-03-25 2004-09-29 山东理工大学 Process for preparing gradient porous ceramic filter element
CN101696110A (en) * 2009-10-23 2010-04-21 山东理工大学 Preparation method of two-layer ceramic filtering element with desulfurizing performance

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103342544A (en) * 2013-07-03 2013-10-09 镇江市江南矿山机电设备有限公司 Method for preparing porous alumina ceramic
CN114349519A (en) * 2022-01-19 2022-04-15 江苏宝利金材科技有限公司 Slurry formula and production process of gel-casting ceramic filter

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Application publication date: 20120215