CN1350996A - High-strength refractory catalytic cleaning ceramic filter and its preparing process - Google Patents
High-strength refractory catalytic cleaning ceramic filter and its preparing process Download PDFInfo
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Abstract
A high-strength refractory ceramic filter for catalytic cleaning is composed of supporting body and surficial layer of carrier-catalytic active components. It is prepared through such steps as breaking alumina (50-70%), zircon (20-35%) and aluminium fluoride (10-15%), mixing with aqueous solution of polyvinyl alcohol, shaping supporting body, calcining, preparing solution of Al sol from AlCl2 (28-32%), absolute alcohol, water and nitric acid, adding nitrates of Mg, Cu, Mn, Co, Pd, La Si and K, reflowing, concentrating, immersing the supporting body in the solution, drying, and calcining.
Description
Technical field
The present invention relates to a kind of high-strength refractory catalytic cleaning ceramic filter and production method of using at aspects such as waste-gas cleaning and molten steel filtrations thereof.
Background technology
Traditional catalytic purification strainer generally is made up of porous ceramic support, support of the catalyst and catalytic activity component three parts.The supporter of catalytic purification strainer adopts porous cordierite ceramics to make more, this material has advantages such as low price, wide material sources, but also there is fusing point low (1400 ℃), often undergo phase transition during in temperature near 1000 ℃, shortcomings such as easy sintering, result of use is not good under hot conditions.The function of support of the catalyst mainly is to keep active substance that big as far as possible surface-area and inhibition sintering are arranged, and its selection always is most important, also is the most difficult.At present, the main both at home and abroad carrier that adopts active gamma-alumina as high temperature catalyst, but the phase transformation of γ → α will take place in gamma-alumina between 1000 ℃~1200 ℃, cause a large amount of losses of surface-area.As for the catalytic activity component, usually adopt precious metals such as palladium, platinum both at home and abroad, traditional viewpoint thinks that the catalytic activity of precious metal is than base metal height, in fact the low-temperature catalytic activity of precious metal is better than base metal really, but its high-temperature catalytic activity is good unlike base metal.This mainly is because precious metal at high temperature volatilizees and sintering easily, therefore, surpasses under 1000 ℃ the condition in temperature, should not adopt precious metal directly as active constituent.In a word, no matter traditional catalytic purification strainer is supporter, carrier, or the catalytic activity component, all exist the easy agglomerating problem of high temperature.For this reason, people have carried out many improvement, and the most representative adds rare earth, basic metal and rare-earth oxide exactly in active constituent, to strengthen its anti-agglutinatting property.But the technology more complicated of this method, and the result of use under hot conditions is also undesirable, therefore, no matter from economic angle or technical standpoint a kind of gratifying method of all can not saying so.
Summary of the invention
The technical problem to be solved in the present invention is, overcome the problem of conventional catalyst polishing filter easy sintering, resistance to elevated temperatures difference under hot conditions, provide good, the anti-caking power of a kind of high high-temp stability strong high-strength refractory catalytic cleaning ceramic filter and production method thereof.
High-strength refractory catalytic cleaning ceramic filter of the present invention is made up of supporter, support of the catalyst and catalytic active component, described supporter is that spontaneous mullite fiber strengthens zircon corundum-mullite ceramic base composite material supporter, the two unites two into one described support of the catalyst and catalytic activity component, is carrier-catalytic activity component shell;
The each component ratio that described spontaneous mullite fiber strengthens zircon corundum-mullite ceramic base composite material supporter is: aluminum oxide: 50~70%, zircon: 20~35%, aluminum fluoride: 10~15%, and above-mentioned content all is weight percentage;
The each component ratio of described carrier-catalytic activity component shell is: Al
2O
3: 28~32%, MgO:18~24%, CuO:13~15%, MnO:12~15%, CoO:5~6.5%, PdO:0.1~1.0%, La
2O
3: 1~2%, SiO
2: 1.5~3.5%, K
2O:4~6.5%, above-mentioned content all is weight percentage.
In above-mentioned carrier-catalytic activity component shell, also contain CeO:5~8% (weight percent).The production method of above-mentioned strainer is:
1, press aluminum oxide: 50~70%, zircon: 20~35%, aluminum fluoride: 10~15% batchings (weight percent) again through ball mill pulverizing, are ground into granularity and are 0.04~0.15 millimeter powder;
2, press powder: the mixed of polyvinyl alcohol water solution=1: 0.35~0.85, and the prefabricated material of mixing one-tenth;
3, Polyurethane flex foam mold is immersed in the prefabricated material, flood into honeycomb type porous ceramic support base substrate, perhaps use the through-type porous ceramic support base substrate of mold injects method moulding;
4, dried supporter base substrate is put into the stove sintering, heat-up rate is 150~270 ℃/h, and sintering temperature is 1600 ℃, and sintering time is 2~6 hours, furnace cooling promptly becomes spontaneous mullite fiber and strengthens zircon corundum-mullite ceramic base composite material supporter to room temperature;
5, get AlCl
3In reactor, slowly drip AlCl
3The warp that quality is 20 times-20 ℃ refrigerated dehydrated alcohol, the room temperature ice-water bath refluxed 6~8 hours, added AlCl under 80 ℃~90 ℃ backflows in batches
3The dehydrated alcohol that quality is 80 times, 80 ℃ distill out superfluous ethanol, and excess gets aluminum ethylate in 30 ℃ of oven dry;
6, by aluminum ethylate: water: nitric acid=1: 100: 0.07 (mol ratio) is got aluminum ethylate, adds water according to quantity, and when being warming up to 85 ℃, the limit drips nitric acid, and refluxing 2 hours in the limit, is condensed into transparent aluminium sol solution;
7, get the aluminium sol solution, press MgO, CuO, MnO, CoO, PdO, La
2O
3, SiO
2, K
2The ratio of O in carrier-catalytic activity component shell adds the nitrate of Mg, Cu, Mn, Co, Pd, La, Si, K respectively, wherein, Pd is a palladium chloride solution, Si is a silicon sol, refluxes 80 ℃ of colloidal solution that are concentrated into certain viscosity 16 hours at 90 ℃~100 ℃;
8, spontaneous mullite fiber is strengthened zircon corundum-mullite ceramic base composite material supporter after 500 ℃ of pre-calcinations, immersed in the above-mentioned colloidal solution 5~10 minutes, take out, at room temperature heavyization is 2 hours, in 40 ℃ air-dry 6 hours, 120 ℃ of dryings 5 hours;
9, put it in the stove, from 100 ℃, be warming up to 900 ℃ with the speed of 10 ℃/h, constant temperature 30 hours is reduced to room temperature with stove;
10, with it at 550 ℃, with the logical purity oxygen of 50ml/min 30 minutes, carry out pre-oxidation treatment, at 500 ℃,, carry out prereduction and handle with the logical pure hydrogen of 70ml/min 60 minutes, promptly become the high-strength refractory catalytic cleaning ceramic filter finished product.
The present invention adopts to has very the spontaneous mullite fiber of low thermal coefficient of expansion, superior heat resistance and strengthens zircon corundum-mullite ceramic based composites and make the supporter of strainer, improved the resistance to elevated temperatures of supporter, and, it also has very high chemical stability, mechanical property and physicals, satisfied the requirement of under hot conditions, using, be suitable at high temperature using.
The two unites two into one with support of the catalyst and catalytic activity component in the present invention, and adopts chemical process, is 2850 ℃ with fusing point, has the magnesium oxide and the major ingredient of aluminum oxide while as carrier of high thermal stability, thereby, improved the thermostability of carrier; When making carrier, Mn-Co-Cu-Pd-O introduces in the lump with the catalytic activity component, wherein, though the low temperature active of base metal oxide Mn-Co-Cu-O is not as palladium, but their thermotolerance is stronger than palladium, the this point specific activity is more important, at cold zone, the palladium catalyzed reaction is in the high-temperature zone, the Mn-Co-Cu-O catalyzed reaction that resistance toheat is good, base metal plays a role in different temperature ranges with precious metal, has complementary advantages, therefore, Pd-O and Mn-Co-Cu-O are combined the Applicable temperature scope that has just enlarged active constituent, simultaneously, also adopted pre-oxidation treatment and prereduction treatment process, preoxidation helps improving the high temperature oxidation activity, prereduction helps improving low-temperature oxidation activity, thereby has further improved the catalytic activity of catalyzer; For thermostability and the anti-caking power that increases carrier substance and catalytic active substance, also added thermo-stabilizer La-Si-K-O, make catalyst support material and catalytic activity component form homogeneous, resistant to elevated temperatures, have the active entity of higher high-temperature catalytic, thereby make its overall performance obtain further raising.
Adopt catalyst converter of the present invention, at the catalytic purification of vehicle exhaust, the catalyticcombustion aspect of steam turbine, gas combustion apparatus, the transformation efficiency of CH and CO all reaches 99%; Aspect the catalyticcombustion of liquid metal, for ferrite base spheroidal graphite cast iron, tensile strength improves 17.5%, and elongation improves 10%, and impelling strength improves 42.9%; For cast steel ZG45, tensile strength improves 13.9%, and elongation improves 39.3%, and impelling strength improves 32.8%.
Embodiment
Embodiment 1:
1.1, press aluminum oxide: 50kg, zircon: 35kg, aluminum fluoride: 15kg batching, again through ball mill pulverizing, be ground into granularity and be 0.04~0.15 millimeter powder;
1.2, press powder: the mixed of polyvinyl alcohol water solution=1: 0.35, and the prefabricated material of mixing one-tenth;
1.3, Polyurethane flex foam mold is immersed in the prefabricated material, flood into honeycomb type porous ceramic support base substrate;
1.4, dried supporter base substrate is put into the stove sintering, heat-up rate is 150 ℃/h, and sintering temperature is 1600 ℃, and sintering time is 2 hours, furnace cooling promptly becomes spontaneous mullite fiber and strengthens zircon corundum-mullite ceramic base composite material supporter to room temperature;
1.5, get AlCl
3In reactor, slowly drip AlCl
3The warp that quality is 20 times-20 ℃ refrigerated dehydrated alcohol, the room temperature ice-water bath refluxed 6 hours, added AlCl under 90 ℃ of backflows in batches
3The dehydrated alcohol that quality is 80 times, 80 ℃ distill out superfluous ethanol, and excess gets aluminum ethylate in 30 ℃ of oven dry;
1.6, by aluminum ethylate: water: nitric acid=1: 100: 0.07 (mol ratio) is got aluminum ethylate, adds water according to quantity, and when being warming up to 85 ℃, the limit drips nitric acid, and refluxing 2 hours in the limit, is condensed into transparent aluminium sol solution;
1.7, get aluminium sol solution 98kg, press MgO, CuO, MnO, CoO, PdO, La
2O
3, SiO
2, K
2The ratio of O in carrier-catalytic activity component shell adds purity respectively and is 99% Mg (NO
3)
276kg, purity are 99% Cu (NO
3)
23H
2O 45kg, purity are 50% Mn (NO
3)
232kg, purity are 99% Co (NO
3)
26H
2O 24.5kg, purity are 99% Pd C1
22H
2O 9kg, purity are 99% La (NO
3)
21.3kg, purity is that 27% silicon sol 10kg, purity are 99% KNO
311.5kg, refluxed 80 ℃ of colloidal solution that are concentrated into certain viscosity 16 hours at 100 ℃;
1.8, spontaneous mullite fiber is strengthened zircon corundum-mullite ceramic base composite material supporter after 500 ℃ of pre-calcinations, immersed in the above-mentioned colloidal solution 5 minutes, take out, at room temperature heavyization is 2 hours, in 40 ℃ air-dry 6 hours, 120 ℃ of dryings 5 hours;
1.9, put it in the stove, from 100 ℃, be warming up to 900 ℃ with the speed of 10 ℃/h, constant temperature 30 hours is reduced to room temperature with stove;
1.10, with it at 550 ℃, with the logical purity oxygen of 50ml/min 30 minutes, carry out pre-oxidation treatment, at 500 ℃,, carry out prereduction and handle with the logical pure hydrogen of 70ml/min 60 minutes, promptly become the high-strength refractory catalytic cleaning ceramic filter finished product.
Embodiment 2:
2.1, press aluminum oxide: 70kg, zircon: 20kg, aluminum fluoride: 10kg batching, again through ball mill pulverizing, be ground into granularity and be 0.04~0.15 millimeter powder;
2.2, press powder: the mixed of polyvinyl alcohol water solution=1: 0.5, and the prefabricated material of mixing one-tenth;
2.3, with prefabricated material with the through-type porous ceramic support base substrate of mold injects method moulding;
2.4, dried supporter base substrate is put into the stove sintering, heat-up rate is 200 ℃/h, and sintering temperature is 1600 ℃, and sintering time is 4 hours, furnace cooling promptly becomes spontaneous mullite fiber and strengthens zircon corundum-mullite ceramic base composite material supporter to room temperature;
2.5, get AlCl
3In reactor, slowly drip AlCl
3The warp that quality is 20 times-20 ℃ refrigerated dehydrated alcohol, the room temperature ice-water bath refluxed 7 hours, added AlCl under 85 ℃ of backflows in batches
3The dehydrated alcohol that quality is 80 times, 80 ℃ distill out superfluous ethanol, and excess gets aluminum ethylate in 30 ℃ of oven dry;
2.6, by aluminum ethylate: water: nitric acid=1: 100: 0.07 (mol ratio) is got aluminum ethylate, adds water according to quantity, and when being warming up to 85 ℃, the limit drips nitric acid, and refluxing 2 hours in the limit, is condensed into transparent aluminium sol solution;
2.7, get aluminium sol solution 100kg, press MgO, CuO, MnO, CoO, PdO, La
2O
3, SiO
2, K
2The ratio of O in carrier-catalytic activity component shell adds purity respectively and is 99% Mg (NO
3)
272kg, purity are 99% Cu (NO
3)
23H
2O 42kg, purity are 50% Mn (NO
3)
227kg, purity are 99% Co (NO
3)
26H
2O 22kg, purity are 99% Pd Cl
22H
2O 7.5kg, purity are 99% La (NO
3)
21.0kg, purity is that 27% silicon sol 7.0kg, purity are 99% KNO
310kg adds purity and is 99% Ce (NO again
3)
36H
2O 14.5kg refluxed 80 ℃ of colloidal solution that are concentrated into certain viscosity 16 hours at 95 ℃;
2.8, spontaneous mullite fiber is strengthened zircon corundum-mullite ceramic base composite material supporter after 500 ℃ of pre-calcinations, immersed in the above-mentioned colloidal solution 10 minutes, take out, at room temperature heavyization is 2 hours, in 40 ℃ air-dry 6 hours, 120 ℃ of dryings 5 hours;
2.9, put it in the stove, from 100 ℃, be warming up to 900 ℃ with the speed of 10 ℃/h, constant temperature 30 hours is reduced to room temperature with stove;
2.10, with it at 550 ℃, with the logical purity oxygen of 50ml/min 30 minutes, carry out pre-oxidation treatment, at 500 ℃,, carry out prereduction and handle with the logical pure hydrogen of 70ml/min 60 minutes, promptly become the high-strength refractory catalytic cleaning ceramic filter finished product.
Embodiment 3:
3.1, press aluminum oxide: 60kg, zircon: 28kg, aluminum fluoride: 12kg batching, again through ball mill pulverizing, be ground into granularity and be 0.04~0.15 millimeter powder;
3.2, press powder: the mixed of polyvinyl alcohol water solution=1: 0.85, and the prefabricated material of mixing one-tenth;
3.3, Polyurethane flex foam mold is immersed in the prefabricated material, flood into honeycomb type porous ceramic support base substrate;
3.4, dried supporter base substrate is put into the stove sintering, heat-up rate is 270 ℃/h, and sintering temperature is 1600 ℃, and sintering time is 6 hours, furnace cooling promptly becomes spontaneous mullite fiber and strengthens zircon corundum-mullite ceramic base composite material supporter to room temperature;
3.5, get AlCl
3In reactor, slowly drip AlCl
3The warp that quality is 20 times-20 ℃ refrigerated dehydrated alcohol, the room temperature ice-water bath refluxed 8 hours, added AlCl under 80 ℃ of backflows in batches
3The dehydrated alcohol that quality is 80 times, 80 ℃ distill out superfluous ethanol, and excess gets aluminum ethylate in 30 ℃ of oven dry;
3.6, by aluminum ethylate: water: nitric acid=1: 100: 0.07 (mol ratio) is got aluminum ethylate, adds water according to quantity, and when being warming up to 85 ℃, the limit drips nitric acid, and refluxing 2 hours in the limit, is condensed into transparent aluminium sol solution;
3.7, get aluminium sol solution 97kg, press MgO, CuO, MnO, CoO, PdO, La
2O
3, SiO
2, K
2The ratio of O in carrier-catalytic activity component shell adds purity respectively and is 99% Mg (NO
3)
277kg, purity are 99% Cu (NO
3)
23H
2O 43kg, purity are 50% Mn (NO
3)
229kg, purity are 99% Co (NO
3)
26H
2O 23kg, purity are 99% PdCl
22H
2O 0.8kg, purity are 99% La (NO
3)
22.6kg, purity is that 27% silicon sol 11kg, purity are 99% KNO
312kg adds purity and is 99% Ce (NO again
3)
36H
2O 20kg refluxed 80 ℃ of colloidal solution that are concentrated into certain viscosity 16 hours at 90 ℃;
3.8, spontaneous mullite fiber is strengthened zircon corundum-mullite ceramic base composite material supporter after 500 ℃ of pre-calcinations, immersed in the above-mentioned colloidal solution 8 minutes, take out, at room temperature heavyization is 2 hours, in 40 ℃ air-dry 6 hours, 120 ℃ of dryings 5 hours;
3.9, put it in the stove, from 100 ℃, be warming up to 900 ℃ with the speed of 10 ℃/h, constant temperature 30 hours is reduced to room temperature with stove;
3.10, with it at 550 ℃, with the logical purity oxygen of 50ml/min 30 minutes, carry out pre-oxidation treatment, at 500 ℃,, carry out prereduction and handle with the logical pure hydrogen of 70ml/min 60 minutes, promptly become the high-strength refractory catalytic cleaning ceramic filter finished product.
Embodiment 4:
4.1, press aluminum oxide: 65kg, zircon: 25kg, aluminum fluoride: 10kg batching, again through ball mill pulverizing, be ground into granularity and be 0.04~0.15 millimeter powder;
4.2, press powder: the mixed of polyvinyl alcohol water solution=1: 0.8, and the prefabricated material of mixing one-tenth;
4.3, Polyurethane flex foam mold is immersed in the prefabricated material, flood into honeycomb type porous ceramic support base substrate;
4.4, dried supporter base substrate is put into the stove sintering, heat-up rate is 250 ℃/h, and sintering temperature is 1600 ℃, and sintering time is 5 hours, furnace cooling promptly becomes spontaneous mullite fiber and strengthens zircon corundum-mullite ceramic base composite material supporter to room temperature;
4.5, get AlCl
3In reactor, slowly drip AlCl
3The warp that quality is 20 times-20 ℃ refrigerated dehydrated alcohol, the room temperature ice-water bath refluxed 6 hours, added AlCl under 85 ℃ of backflows in batches
3The dehydrated alcohol that quality is 80 times, 80 ℃ distill out superfluous ethanol, and excess gets aluminum ethylate in 30 ℃ of oven dry;
4.6, by aluminum ethylate: water: nitric acid=1: 100: 0.07 (mol ratio) is got aluminum ethylate, adds water according to quantity, and when being warming up to 85 ℃, the limit drips nitric acid, and refluxing 2 hours in the limit, is condensed into transparent aluminium sol solution;
4.7, get aluminium sol solution 90kg, press MgO, CuO, MnO, CoO, PdO, La
2O
3, SiO
2, K
2The ratio of O in carrier-catalytic activity component shell adds purity respectively and is 99% Mg (NO
3)
267kg, purity are 99% Cu (NO
3)
23H
2O 40kg, purity are 50% Mn (NO
3)
224kg, purity are 99% Co (NO
3)
26H
2O 19kg, purity are 99% PdCl
22H
2O 0.2kg, purity are 99% La (NO
3)
22.5kg, purity is that 27% silicon sol 6kg, purity are 99% KNO
38kg adds purity and is 99% Ce (NO again
3)
36H
2O 14kg refluxed 80 ℃ of colloidal solution that are concentrated into certain viscosity 16 hours at 95 ℃;
4.8, spontaneous mullite fiber is strengthened zircon corundum-mullite ceramic base composite material supporter after 500 ℃ of pre-calcinations, immersed in the above-mentioned colloidal solution 7 minutes, take out, at room temperature heavyization is 2 hours, in 40 ℃ air-dry 6 hours, 120 ℃ of dryings 5 hours;
4.9, put it in the stove, from 100 ℃, be warming up to 900 ℃ with the speed of 10 ℃/h, constant temperature 30 hours is reduced to room temperature with stove;
4.10, with it at 550 ℃, with the logical purity oxygen of 50ml/min 30 minutes, carry out pre-oxidation treatment, at 500 ℃,, carry out prereduction and handle with the logical pure hydrogen of 70ml/min 60 minutes, promptly become the high-strength refractory catalytic cleaning ceramic filter finished product.
Claims (3)
1, a kind of high-strength refractory catalytic cleaning ceramic filter, it is made up of supporter, support of the catalyst and catalytic active component, it is characterized in that, described supporter is that spontaneous mullite fiber strengthens zircon corundum-mullite ceramic base composite material supporter, the two unites two into one described support of the catalyst and catalytic activity component, is carrier-catalytic activity component shell;
The each component ratio that described spontaneous mullite fiber strengthens zircon corundum-mullite ceramic base composite material supporter is: aluminum oxide: 50~70%, zircon: 20~35%, aluminum fluoride: 10~15%, and above-mentioned content all is weight percentage;
The each component ratio of described carrier-catalytic activity component shell is: Al
2O
3: 28~32%, MgO:18~24%, CuO:13~15%, MnO:12~15%, CoO:5~6.5%, PdO:0.1~1.0%, La
2O
3: 1~2%, SiO
2: 1.5~3.5%, K
2O:4~6.5%, above-mentioned content all is weight percentage.
2, high-strength refractory catalytic cleaning ceramic filter according to claim 1 is characterized in that, also contains CeO:5~8% (weight percent) in above-mentioned carrier-catalytic activity component shell.
3, a kind of production method of high-strength refractory catalytic cleaning ceramic filter is characterized in that:
3.1, press aluminum oxide: 50~70%, zircon: 20~35%, aluminum fluoride: 10~15% batchings (weight percent) again through ball mill pulverizing, are ground into granularity and are 0.04~0.15 millimeter powder;
3.2, press powder: the mixed of polyvinyl alcohol water solution=1: 0.35~0.85, and the prefabricated material of mixing one-tenth;
3.3, Polyurethane flex foam mold is immersed in the prefabricated material, flood into honeycomb type porous ceramic support base substrate, perhaps use the through-type porous ceramic support base substrate of mold injects method moulding;
3.4, dried supporter base substrate is put into the stove sintering, heat-up rate is 150~270 ℃/h, and sintering temperature is 1600 ℃, and sintering time is 2~6 hours, furnace cooling promptly becomes spontaneous mullite fiber and strengthens zircon corundum-mullite ceramic base composite material supporter to room temperature;
3.5, get AlCl
3In reactor, slowly drip AlCl
3The warp that quality is 20 times-20 ℃ refrigerated dehydrated alcohol, the room temperature ice-water bath refluxed 6~8 hours, added AlCl under 80 ℃~90 ℃ backflows in batches
3The dehydrated alcohol that quality is 80 times, 80 ℃ distill out superfluous ethanol, and excess gets aluminum ethylate in 30 ℃ of oven dry;
3.6, by aluminum ethylate: water: nitric acid=1: 100: 0.07 (mol ratio) is got aluminum ethylate, adds water according to quantity, and when being warming up to 85 ℃, the limit drips nitric acid, and refluxing 2 hours in the limit, is condensed into transparent aluminium sol solution;
3.7, get the aluminium sol solution, press MgO, CuO, MnO, CoO, PdO, La
2O
3, SiO
2, K
2The ratio of O in carrier-catalytic activity component shell adds the nitrate of Mg, Cu, Mn, Co, Pd, La, Si, K respectively, wherein, Pd is a palladium chloride solution, Si is a silicon sol, refluxes 80 ℃ of colloidal solution that are concentrated into certain viscosity 16 hours at 90 ℃~100 ℃;
3.8, spontaneous mullite fiber is strengthened zircon corundum-mullite ceramic base composite material supporter after 500 ℃ of pre-calcinations, immersed in the above-mentioned colloidal solution 5~10 minutes, take out, at room temperature heavyization is 2 hours, in 40 ℃ air-dry 6 hours, 120 ℃ of dryings 5 hours;
3.9, put it in the stove, from 100 ℃, be warming up to 900 ℃ with the speed of 10 ℃/h, constant temperature 30 hours is reduced to room temperature with stove;
3.10, with it at 550 ℃, with the logical purity oxygen of 50ml/min 30 minutes, carry out pre-oxidation treatment, at 500 ℃,, carry out prereduction and handle with the logical pure hydrogen of 70ml/min 60 minutes, promptly become the high-strength refractory catalytic cleaning ceramic filter finished product.
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- 2001-10-08 CN CNB011282584A patent/CN1140344C/en not_active Expired - Fee Related
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