CN1714909A - Method for preparing ceramic filter tube for purifying high temperature gas - Google Patents
Method for preparing ceramic filter tube for purifying high temperature gas Download PDFInfo
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- CN1714909A CN1714909A CNA2005100208918A CN200510020891A CN1714909A CN 1714909 A CN1714909 A CN 1714909A CN A2005100208918 A CNA2005100208918 A CN A2005100208918A CN 200510020891 A CN200510020891 A CN 200510020891A CN 1714909 A CN1714909 A CN 1714909A
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Abstract
The present invention relates to a kind of method for preparing ceramic filter tube, specifically relate to a kind of ceramic filter tube for purifying high temperature gas and preparation method who is used for coal gasifying electricity generation field.The present invention is achieved by following technical proposals: ceramic filter tube for purifying high temperature gas preparation flow of the present invention is: making oxide liquid-phase sintering agent → making is that the ceramic filter tube → making mullite fiber film → film → sintering of main microstructure carrier makes ceramic filter tube with the SiC particle.The present invention has following beneficial effect: the space of gas passage when the present invention utilizes oxide formation particle joint portion to use as screen pipe in addition, there is not unnecessary sintering aid in the pore, and pore guarantees to have the space of gas percent of pass; Can keep mechanical strength, hear resistance, chemical stability in conjunction with phase, liquid phase forms easily, and film strength of the present invention, air penetrability and integrality all meet the requirements.Clean gas high-temperature ceramic filter pipe of the present invention preparation easily, cost is low, can be widely used in the gas filtration of the temperature high performance high of aspect such as coal gasifying electricity generation.
Description
Technical field
The present invention relates to a kind of preparation method of pottery, specifically relate to a kind of method for preparing ceramic filter tube for purifying high temperature gas that is used for coal gasifying electricity generation field.
Background technology
Ceramic filter tube is that porous matter has the filtration that hear resistance, chemical stability and high-intensity characteristic are used for coal gas under the high temperature environment such as coal gasifying electricity generation simultaneously because of its structure.The preparation of ceramic filter tube is a principal component with the SiC particle mostly, uses natural materials such as clay, talcum to connect the SiC particle as bond; Because the powder dust particle that screen pipe will be caught is small-sized, at this moment will use film, always the raw material of film use ceramic to make slurry, and it being coated on the SiC particle is the screen pipe surface of carrier again, film forming, dry back sintering.Always the screen pipe carrier is made and is adopted natural materials such as mixing kaolin clay, talcum, calcium carbonate as bond, but its screen pipe carrier of making lacks the chemical stability under the high temperature, and mechanical strength is also poor; And the forming technology for preparing ceramic filter tube is usually taked extrusion molding or dry type press molding, sintering is taked solid-phase sintering or liquid-phase sintering, but extrusion molding and dry type press molding method can not effectively utilize liquid phase surface tension force to form pore space in addition, abundant SiC particle joint portion, air is bigger by the pressure loss that produces, and its bending strength is less; The material translational speed is little during solid-phase sintering, can not too much form pore space in addition, support particle joint portion, air is bigger by the pressure loss that produces simultaneously, particularly adopts casting to make long size ceramic filter tube, and its intensity and air all are difficult to guarantee by the pressure loss that produces; The firing the conditional request film and must have certain intensity, air penetrability and integrality of film, but since during sintering the shrinkage factor of film and ceramic filter tube prime modulus differ, cause be full of cracks easily.At present, about making the technical scheme of satisfactory long size ceramic filter tube of intensity and film, yet there are no record.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiency that prior art exists, and providing a kind of is principal component with the SiC particle, with Al
2O
3Deng oxide is the liquid phase oxidation thing of bond, and the liquid-phase sintering process preparation of the long size casting forming of employing has the ceramic filter tube of the clean gas temperature high performance high of hear resistance, chemical stability and good air permeability.
The present invention is achieved by following technical proposals: ceramic filter tube for purifying high temperature gas preparation flow of the present invention is: making oxide liquid-phase sintering agent → making is that the ceramic filter tube → making mullite fiber film → film → sintering of main microstructure supporter makes ceramic filter tube with the SiC particle.
The ceramic filter tube of clean gas temperature high performance high of the present invention and preparation method have following beneficial effect compared with prior art: because the present invention utilizes liquid phase to connect the principal component particle, can form beyond the particle joint portion space of gas passage when using as screen pipe, do not have unnecessary sintering aid in the pore, pore guarantees to have the space of gas percent of pass; The present invention has adopted with Al
2O
3Oxidation liquid phase bond for principal component can keep mechanical strength, hear resistance, chemical stability in conjunction with phase, accessory ingredient SiO
2, CaO, MgO effect be that liquid phase forms agent, accessory ingredient Y
2O
3, ZrO
2Can improve the alkali resistance of liquid phase, accessory ingredient TiO
2, B
2O
3Can reduce the temperature that liquid phase generates.Film strength, air penetrability and integrality that the inventive method is made all meet the requirements.Clean gas high-temperature ceramic filter pipe of the present invention preparation easily, cost is low, can be widely used in the gas filtration of the temperature high performance high of aspect such as coal gasifying electricity generation.
The specific embodiment
Below in conjunction with embodiment the present invention is further described.
Method for preparing ceramic filter tube for purifying high temperature gas of the present invention is characterised in that preparation flow is: making oxide liquid-phase sintering agent → making is that the ceramic filter tube → making mullite fiber film → film → sintering of main microstructure carrier makes ceramic filter tube with the SiC particle, and described preparation oxide liquid-phase sintering agent is the principal component Al that can keep mechanical strength, hear resistance, chemical stability
2O
370~90%, the 2nd composition SiO that liquid phase is formed
23.5~4.5%, CaO1.5~3%, MgO0.5~2%, can improve alkali-proof the 3rd composition Y of liquid phase
2O
30~1.5%, ZrO
20~1.5%, can reduce the 4th composition B that liquid phase generates temperature
2O
30~1.5%, TiO
20~1.5% mixes, and adding distil water mixes, pulverized 24 hours in ball mill, slurry is cast on the plaster mold after the taking-up to be dried, with 1350 ℃~1450 ℃ temperature sintering 2 hours in air, oxide liquid-phase sintering agent; Described preparation SiC is that the ceramic filter tube of main microstructure carrier is to be that 250~350 microns SiC particle 35~45%, 1000 purpose SiC powder 3.5~4.5%, oxide liquid phase forms agent 3.5~4.5% potato powder 0.5~1.5%, ion exchange water 35~45% is mixed and made into slurry with particle diameter, be poured into behind the plaster mold dryly, make length and be 1~1.5 meter, the tubulose shaping carrier of 55~65 millimeters of external diameters, 8~12 millimeter one end sealing of wall thickness; Described many crystallizations of preparation mullite fiber outer membrane is to be that 3.5-4.5 micron, long 20~40 microns many crystallizations mullite fiber 8~10%, oxide liquid-phase sintering agent 0.5~1.5%, dispersant 0.01%, ion exchange water 85~95% are mixed into slurry with particle diameter; Described filming is that the many crystallizations mullite slurry that will make is coated in the ceramic filter tube carrier outer surface that makes; Described sintering is that the long size screen pipe with drying vertically places on the liftable brace table, insert with 250 millimeters speed per hour and to be incubated in advance in 1350 ℃~1450 ℃ electric furnace, adopt the region-type sintering process to carry out sintering, make the silicon carbide porous body ceramic filter tube.
Described preparation oxide liquid-phase sintering agent can also be with principal component Al
2O
3The 77~89%, the 2nd composition SiO
23.8 CaO~4.2%,
2~2.5%, MgO1~1.5%, the 3rd composition Y
2O
30.8 ZrO~1.2%,
20.8 the~1.2%, the 4th composition B
2O
30.8 TiO~1.2%,
20.8~1.2% mixes; Described preparation silicon carbide porous body ceramic filter tube can also be to be that 280~320 microns SiC particle 38~42%, 1000 purpose SiC powder 3.8~4.2%, oxide liquid phase form agent 3.8~4.2%, potato powder 0.8~1.2%, ion exchange water 38~42%, clay 6~10%, calcium carbonate 4~8%, talcum 2~6% and are mixed and made into slurry with particle diameter, be poured into behind the plaster mold dryly, make length and be 1~1.5 meter, the tubulose shaping carrier of the end sealing of 55~65 millimeters of external diameters, 9~10 millimeters of wall thickness; Described many crystallizations of preparation mullite fiber outer membrane is to be that 3.8~4.2 microns, many crystallizations mullite fiber 9~10% of long 30~35 microns, oxide liquid-phase sintering agent 0.8~1.2%, dispersant 0.01%, the ion exchange water 89~92% that has made are mixed into slurry with particle diameter; Described sintering is that the long size screen pipe with drying vertically places on the liftable brace table, insert with 250 millimeters speed per hour and to be incubated in advance in 1380 ℃~1420 ℃ electric furnace, adopt the region-type sintering process to carry out sintering, make the silicon carbide porous body ceramic filter tube.
Described potato powder is to be dissolved in advance that to make concentration in 40 ℃~60 ℃ the hot water be 10% the aqueous solution.
Described coating thickness is 100~300 microns.
The microstructure of described ceramic filter tube is by containing 80~89%Al
2O
3Oxide liquid-phase sintering agent air calcination under 1400 ℃ of temperature oxide of generating liquid phase earthenware principal component carborundum crystals is coupled together the formation porous body; The microstructure of described mullite fiber film is to mix and be coated in ceramic filter tube prime modulus outer surface and air calcination generates liquid phase under 1400 ℃ of temperature oxide couples together the porous body that constitutes with many crystallizations mullite fiber crystal by containing many crystallizations mullite fiber 8~10%, oxide liquid-phase sintering agent 0.8~1%, dispersant 0.01%, ion exchange water 89~92%.
The ceramic filter tube slurry of described casting forming is in the dry solidification process, moisture in the slurry moves to SiC particle binding site drying under capillary effect, it is condensing that sintering aid micro mist and moisture move to binding site together, forms pore space in addition, SiC particle joint portion.This space is exactly the passage of gas when using as screen pipe.
Ceramic filter tube after the described shaping carries out liquid-phase sintering, because of the sintering temperature sintering aid generates liquid, flow of matter is good, sintering aid all can cover the SiC particle surface, move to the binding site of SiC particle, form pore space in addition, Sic particle joint portion, and do not have unnecessary sintering aid in the pore, pore has the space of guaranteeing the gas percent of pass.
Embodiment 1.
(1) produces oxide liquid-phase sintering agent: the Al that gets low Na
2O
377 parts in powder, kaolin (SiO
263%, Al
2O
336%) 10 parts, 8 parts in calcium carbonate (CaO56%), talcum (SiO
260%, MgO30%, Al
2O
36%, CaO1%) 8 parts.
Be added into Y
2O
3, ZrO
2, B
2O
3, TiO
2Each 1 part, pulverize mixing 24 hours with distilled water with ball milling.
The slurry that obtains is poured on the plasterboard, and take out dry back, with 1350 ℃, in air sintering 2 hours, making density is 3.55g/cm
3, bending strength is the oxide liquid-phase sintering agent of 174Mpa.
(2) produce the ceramic filter tube carrier: be averaged 100 parts on the SiC particle of 300 microns of particle diameters, 10 parts in 1000 purpose SiC powder, 10 parts of oxide liquid-phase sintering agent, 2 parts in potato powder, 100 parts of ion exchange waters.The potato powder is dissolved in 50 ℃ hot water in advance, and to make concentration be 10% the aqueous solution, above-mentioned raw materials mixed make slurry, and this slurry is cast in and makes long 1 meter, the ceramic filter tube of 55 millimeters of external diameters, 8 millimeter one end sealing of wall thickness on the plaster mold;
(3) produce many crystallizations mullite fiber outer membrane: getting particle diameter is that many crystallizations mullite fiber 8% of 3.5 microns, long 20 microns, oxide liquid-phase sintering agent 0.5%, dispersant 0.01%, the ion exchange water 85% that employing has made are mixed into slurry;
(4) film: many crystallizations mullite slurry that will make is coated in the ceramic filter tube carrier outer surface that makes, and film thickness is 100 microns;
(5) sintering: the long size screen pipe of drying is vertically placed on the liftable brace table, insert with 250 millimeters speed per hour and be incubated in advance in 1350 ℃ electric furnace, adopt the region-type sintering process to carry out sintering, make the silicon carbide porous body ceramic filter tube.
The ceramic filter tube flexibility that present embodiment makes is 4.5 millimeters.
Embodiment 2.
(1) produces oxide liquid-phase sintering agent: the Al that gets low Na
2O
379 parts in powder, kaolin (SiO
263%, Al
2O
336%) 10 parts, 6 parts in calcium carbonate (CaO56%), talcum (SiO
260%, MgO30%, Al
2O
36%, CaO1%) 6 parts.
Be added into Y
2O
3, ZrO
2, B
2O
3, TiO
2Each 0.8 part, pulverize mixing 24 hours with distilled water with ball milling.
The slurry that obtains is poured on the plasterboard, dry back with 1380 ℃, in air sintering 2 hours, making density is 3.60g/cm
3, bending strength is the oxide liquid-phase sintering agent of 275Mpa.
(2) produce the ceramic filter tube carrier: be averaged 100 parts on the SiC particle of 300 microns of particle diameters, 10 parts in 1000 purpose SiC powder, 10 parts of oxide liquid-phase sintering agent, 2 parts in potato powder, 100 parts of ion exchange waters.The potato powder is dissolved in 55 ℃ hot water in advance, and to make concentration be 10% the aqueous solution, above-mentioned raw materials mixed make slurry, this slurry is cast in dry back taking-up on the plaster mold, makes the ceramic filter tube of 1.2 meters of length, 60 millimeters of external diameters, 10 millimeter one end sealing of wall thickness.
(3) produce many crystallizations mullite fiber outer membrane: getting particle diameter is that many crystallizations mullite fiber 9% of 4 microns, long 30 microns, oxide liquid-phase sintering agent 0.8%, dispersant 0.01%, the ion exchange water 90% that employing has made are mixed into slurry;
(4) film: many crystallizations mullite slurry that will make is coated in the ceramic filter tube carrier outer surface that makes, and film thickness is 150 microns;
(5) sintering: the long size screen pipe of drying is vertically placed on the liftable brace table, insert with 250 millimeters speed per hour and be incubated in advance in 1380 ℃ electric furnace, adopt the region-type sintering process to carry out sintering, make the silicon carbide porous body ceramic filter tube.
The ceramic filter tube flexibility that present embodiment makes is 2.5 millimeters.
Embodiment 3.
(1) produces oxide liquid-phase sintering agent: the Al that gets low Na
2O
382 parts in powder, kaolin (SiO
263%, Al
2O
336%) 6 parts, 4 parts in calcium carbonate (CaO56%), talcum (SiO
260%, MgO30%, Al
2O
36%, CaO1%) 4 parts.
Be added into Y
2O
3, ZrO
2, B
2O
3, TiO
2Each 1 part, pulverize mixing 24 hours with distilled water with ball milling.
The slurry that obtains is poured on the plasterboard, dry back with 1400 ℃, in air sintering 2 hours, making density is 3.60g/cm
3, bending strength is the oxide liquid-phase sintering agent of 280Mpa.
(2) produce the ceramic filter tube carrier: be averaged 100 parts on the SiC particle of 300 microns of particle diameters, 10 parts in 1000 purpose SiC powder, 10 parts of oxide liquid-phase sintering agent, 2 parts in potato powder, 100 parts of ion exchange waters.The potato powder is dissolved in 60 ℃ hot water in advance, and to make concentration be 10% the aqueous solution, above-mentioned raw materials mixed make slurry, this slurry is cast in dry back taking-up on the plaster mold, makes the ceramic filter tube of 1.3 meters of length, 65 millimeters of external diameters, 10 millimeter one end sealing of wall thickness.
(3) produce many crystallizations mullite fiber outer membrane: getting particle diameter is that many crystallizations mullite fiber 10% of 4.5 microns, long 35 microns, oxide liquid-phase sintering agent 1.2%, dispersant 0.01%, the ion exchange water 90% that employing has made are mixed into slurry;
(4) film: many crystallizations mullite slurry that will make is coated in the ceramic filter tube carrier outer surface that makes, and film thickness is 200 microns;
(5) sintering: the long size screen pipe of drying is vertically placed on the liftable brace table, insert with 250 millimeters speed per hour and be incubated in advance in 1400 ℃ electric furnace, adopt the region-type sintering process to carry out sintering, make the silicon carbide porous body ceramic filter tube.
The ceramic filter tube flexibility that present embodiment makes is 0.6 millimeter.
Embodiment 4.
(1) produces oxide liquid-phase sintering agent: the Al that gets low Na
2O
389 parts in powder, kaolin (SiO
263%, Al
2O
336%) 5 parts, 3 parts in calcium carbonate (CaO56%), talcum (SiO
260%, MgO30%, Al
2O
36%, CaO1%) 3 parts.
Be added into Y
2O
3, ZrO
2, B
2O
3, TiO
2Each 1 part, pulverize mixing 24 hours with distilled water with ball milling.
The slurry that obtains is poured on the plasterboard, dry back with 1450 ℃, in air sintering 2 hours, making density is 3.62g/cm
3, bending strength is the oxide liquid-phase sintering agent of 285Mpa.
(2) produce the ceramic filter tube carrier: be averaged 100 parts on the SiC particle of 300 microns of particle diameters, 10 parts in 1000 purpose SiC powder, 10 parts of oxide liquid-phase sintering agent, 2 parts in potato powder, 100 parts of ion exchange waters.The potato powder is dissolved in 55 ℃ hot water in advance, and to make concentration be 10% the aqueous solution, above-mentioned raw materials mixed make slurry, and this slurry is cast in and makes long 1.5 meters, the ceramic filter tube of 60 millimeters of external diameters, 10 millimeter one end sealing of wall thickness on the plaster mold.
(3) produce many crystallizations mullite fiber outer membrane: getting particle diameter is that many crystallizations mullite fiber 10% of 4 microns, long 40 microns, oxide liquid-phase sintering agent 1.5%, dispersant 0.01%, the ion exchange water 95% that employing has made are mixed into slurry;
(4) film: many crystallizations mullite slurry that will make is coated in the ceramic filter tube carrier outer surface that makes, and film thickness is 150 microns;
(5) sintering: the long size screen pipe of drying is vertically placed on the liftable brace table, insert with 250 millimeters speed per hour and be incubated in advance in 1450 ℃ electric furnace, adopt the region-type sintering process to carry out sintering, make the silicon carbide porous body ceramic filter tube.
The ceramic filter tube flexibility that present embodiment makes is 0.5 millimeter.
Claims (5)
1, a kind of method for preparing ceramic filter tube for purifying high temperature gas, it is characterized in that preparation flow is: making oxide liquid-phase sintering agent → making is that the ceramic filter tube → making mullite fiber film → film → sintering of main microstructure carrier makes ceramic filter tube with the SiC particle, and described preparation oxide liquid-phase sintering agent is the principal component Al that can keep mechanical strength, hear resistance, chemical stability
2O
370~90%, the 2nd composition SiO that liquid phase is formed
23.5~4.5%, CaO1.5~3%, MgO0.5~2%, can improve alkali-proof the 3rd composition Y of liquid phase
2O
30~1.5%, ZrO
20~1.5%, can reduce the 4th composition B that liquid phase generates temperature
2O
30~1.5%, TiO
20~1.5% mixes, and adding distil water mixes, pulverized 24 hours in ball mill, slurry is cast on the plaster mold back to be dried takes out, with 1350 ℃~1450 ℃ temperature sintering 2 hours in air, oxide liquid-phase sintering agent; Described preparation SiC is that the ceramic filter tube of main microstructure carrier is to be that 250~350 microns SiC particle 35~45%, 1000 purpose SiC powder 3.5~4.5%, oxide liquid phase forms agent 3.5~4.5%, potato powder 0.5~1.5%, ion exchange water 35~45% and be mixed and made into slurry with particle diameter, be poured into behind the plaster mold dryly, make length and be 1~1.5 meter, the tubulose shaping carrier of 55~65 millimeters of external diameters, 8~12 millimeter one end sealing of wall thickness; Described many crystallizations of preparation mullite fiber outer membrane is to be that 3.5-4.5 micron, many crystallizations mullite fiber 8~10% of long 20~40 microns, oxide liquid-phase sintering agent 0.5~1.5%, dispersant 0.01%, the ion exchange water 85~95% that has made are mixed into slurry with particle diameter; Described filming is that the many crystallizations mullite slurry that will make is coated in the ceramic filter tube carrier outer surface that makes; Described sintering is that the long size tubular carrier with drying vertically places on the liftable brace table, insert with 250 millimeters speed per hour and to be incubated in advance in 1350 ℃~1450 ℃ electric furnace, adopt the region-type sintering process to carry out sintering, make the silicon carbide porous body ceramic filter tube.
2, method for preparing ceramic filter tube for purifying high temperature gas as claimed in claim 1 is characterized in that: described preparation oxide liquid-phase sintering agent can also be with principal component Al
2O
3The 77~89%, the 2nd composition SiO
23.8~4.2%, CaO2~2.5%, MgO1~1.5%, the 3rd composition Y
2O
30.8 ZrO~1.2%,
20.8 the~1.2%, the 4th composition B
2O
30.8 TiO~1.2%,
20.8%~1.2 mixes; Described preparation silicon carbide porous body ceramic filter tube can also be to be that 280~320 microns SiC particle 38~42%, 1000 purpose SiC powder 3.8~4.2%, oxide liquid phase form agent 3.8~4.2%, potato powder 0.8~1.2%, ion exchange water 38~42%, clay 6~10%, calcium carbonate 4~8%, talcum 2~6% and are mixed and made into slurry with particle diameter, be poured into behind the plaster mold dryly, make length and be 1~1.5 meter, the tubulose shaping carrier of the end sealing of 55~65 millimeters of external diameters, 9~10 millimeters of wall thickness; Described many crystallizations of preparation mullite fiber outer membrane is to be that 3.8~4.2 microns, many crystallizations mullite fiber 9~10% of long 30~35 microns, oxide liquid-phase sintering agent 0.8~1.2%, dispersant 0.01%, the ion exchange water 89~92% that has made are mixed into slurry with particle diameter; Described sintering is that the long size tubular carrier with drying vertically places on the liftable brace table, insert with 250 millimeters speed per hour and to be incubated in advance in 1380 ℃~1420 ℃ electric furnace, adopt the region-type sintering process to carry out sintering, make the silicon carbide porous body ceramic filter tube.
3, ceramic filter tube for purifying high temperature gas as claimed in claim 1 or 2 is characterized in that: described potato powder is to be dissolved in advance that to make concentration in 40 ℃~60 ℃ the hot water be 10% the aqueous solution.
4, ceramic filter tube for purifying high temperature gas as claimed in claim 1 or 2 is characterized in that: described coating thickness is 100~300 microns.
5, ceramic filter tube for purifying high temperature gas as claimed in claim 1 is characterized in that: the microstructure of described ceramic filter tube is by containing 80~89%Al
2O
3Oxide liquid-phase sintering agent air calcination under 1400 ℃ of temperature oxide of generating liquid phase earthenware principal component carborundum crystals is coupled together the formation porous body; The microstructure of described mullite fiber film is to mix and be coated in ceramic filter tube carrier outer surface and air calcination generates liquid phase under 1400 ℃ of temperature oxide couples together the porous body that constitutes with many crystallizations mullite fiber crystal by containing many crystallizations mullite fiber 8~10%, oxide liquid-phase sintering agent 0.8~1%, dispersant 0.01%, ion exchange water 89~92%.
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