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 PDF

Info

Publication number
CN1350996A
CN1350996A CN 01128258 CN01128258A CN1350996A CN 1350996 A CN1350996 A CN 1350996A CN 01128258 CN01128258 CN 01128258 CN 01128258 A CN01128258 A CN 01128258A CN 1350996 A CN1350996 A CN 1350996A
Authority
CN
China
Prior art keywords
hours
supporter
mullite
catalytic
catalytic activity
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN 01128258
Other languages
Chinese (zh)
Other versions
CN1140344C (en
Inventor
穆柏春
刘伟
吴宪龙
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CNB011282584A priority Critical patent/CN1140344C/en
Publication of CN1350996A publication Critical patent/CN1350996A/en
Application granted granted Critical
Publication of CN1140344C publication Critical patent/CN1140344C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Landscapes

  • Catalysts (AREA)

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

A kind of high-strength refractory catalytic cleaning ceramic filter and production method thereof
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.
CNB011282584A 2001-10-08 2001-10-08 High-strength refractory catalytic cleaning ceramic filter and its preparing process Expired - Fee Related CN1140344C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB011282584A CN1140344C (en) 2001-10-08 2001-10-08 High-strength refractory catalytic cleaning ceramic filter and its preparing process

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB011282584A CN1140344C (en) 2001-10-08 2001-10-08 High-strength refractory catalytic cleaning ceramic filter and its preparing process

Publications (2)

Publication Number Publication Date
CN1350996A true CN1350996A (en) 2002-05-29
CN1140344C CN1140344C (en) 2004-03-03

Family

ID=4668134

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB011282584A Expired - Fee Related CN1140344C (en) 2001-10-08 2001-10-08 High-strength refractory catalytic cleaning ceramic filter and its preparing process

Country Status (1)

Country Link
CN (1) CN1140344C (en)

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101607158B (en) * 2008-06-21 2011-06-15 淄博鑫拓耐火材料有限公司 Silicon carbide porous ceramic filter and manufacturing method thereof
CN104193310A (en) * 2014-08-29 2014-12-10 潮州三环(集团)股份有限公司 Ceramic material and preparation method thereof
CN105837241A (en) * 2015-01-16 2016-08-10 济南圣泉倍进陶瓷过滤器有限公司 Foam ceramic filter for cast steel and high temperature alloy and manufacturing method thereof
CN106431442A (en) * 2016-10-20 2017-02-22 郑州丽福爱生物技术有限公司 High-temperature-resistant ceramic and preparation method thereof
CN107010964A (en) * 2017-05-18 2017-08-04 清华大学 It is a kind of to strengthen the method for ultralight foamed ceramics blank strength
CN107626200A (en) * 2016-07-18 2018-01-26 康宁股份有限公司 Mixed-metal oxides Formaldehyde decomposition catalyst filter and its manufacture method
CN107857580A (en) * 2017-12-16 2018-03-30 李炫颖 A kind of preparation method of resistance to acid attack type porous ceramic film support material
CN107903080A (en) * 2017-12-12 2018-04-13 武汉钢铁有限公司 A kind of preparation method of zirconia/mullite high porosity ceramic material
CN107986812A (en) * 2017-12-12 2018-05-04 武汉钢铁有限公司 A kind of preparation method of in-situ self-toughening zirconia-mullite composite diphase material

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100444925C (en) * 2006-12-22 2008-12-24 北京佳康尔水处理技术有限公司 Filter core for removing fluorine from drinking water and preparation method thereof

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101607158B (en) * 2008-06-21 2011-06-15 淄博鑫拓耐火材料有限公司 Silicon carbide porous ceramic filter and manufacturing method thereof
CN104193310A (en) * 2014-08-29 2014-12-10 潮州三环(集团)股份有限公司 Ceramic material and preparation method thereof
CN105837241A (en) * 2015-01-16 2016-08-10 济南圣泉倍进陶瓷过滤器有限公司 Foam ceramic filter for cast steel and high temperature alloy and manufacturing method thereof
CN105837241B (en) * 2015-01-16 2018-12-14 济南圣泉倍进陶瓷过滤器有限公司 Cast steel and high temperature alloy ceramic foam filter and its manufacturing method
CN107626200A (en) * 2016-07-18 2018-01-26 康宁股份有限公司 Mixed-metal oxides Formaldehyde decomposition catalyst filter and its manufacture method
CN106431442A (en) * 2016-10-20 2017-02-22 郑州丽福爱生物技术有限公司 High-temperature-resistant ceramic and preparation method thereof
CN107010964A (en) * 2017-05-18 2017-08-04 清华大学 It is a kind of to strengthen the method for ultralight foamed ceramics blank strength
CN107010964B (en) * 2017-05-18 2020-01-21 清华大学 Method for enhancing strength of ultra-light foamed ceramic body
CN107903080A (en) * 2017-12-12 2018-04-13 武汉钢铁有限公司 A kind of preparation method of zirconia/mullite high porosity ceramic material
CN107986812A (en) * 2017-12-12 2018-05-04 武汉钢铁有限公司 A kind of preparation method of in-situ self-toughening zirconia-mullite composite diphase material
CN107903080B (en) * 2017-12-12 2020-12-29 武汉钢铁有限公司 Preparation method of zirconia-mullite high-porosity ceramic material
CN107857580A (en) * 2017-12-16 2018-03-30 李炫颖 A kind of preparation method of resistance to acid attack type porous ceramic film support material

Also Published As

Publication number Publication date
CN1140344C (en) 2004-03-03

Similar Documents

Publication Publication Date Title
CN1140344C (en) High-strength refractory catalytic cleaning ceramic filter and its preparing process
CN101879448B (en) Ordered structure catalyst for hydrogenation of oxalic ester for preparing ethylene glycol and preparation method thereof
CN111499387A (en) High-strength silicon nitride composite silicon carbide ceramic and preparation method and application thereof
CN101143326A (en) Preparation method and application of a compound carrier metal nanometer catalyst
CN104475138A (en) Vanadium-phosphorus-zirconium-titanium composite oxide catalyst for synthesising acrylic acid (ester) as well as preparation method and application of vanadium-phosphorus-zirconium-titanium composite oxide catalyst
CN102773091B (en) Composite-carrier honeycomb monolithic denitration catalyst and preparing method thereof
CN106800420A (en) A kind of silicon carbide whisker in-situ composite corindon high-temperature ceramic materials and preparation method thereof
CN106378135A (en) Iron-based catalyst used in preparation of low-carbon olefin from synthetic gas, and preparation method and application thereof
CN113289663B (en) Methanation catalyst preparation method for isothermal fixed bed
CN102936678B (en) Vanadium-nitrogen alloy production method
CN100430321C (en) Method for preparing modified aluminium titanate material
CN1410393A (en) Preparation method of special foamed ceramic filter for magnesium alloy
CN101805201A (en) Preparation method of porous silicon carbide ceramics with high thermal shock resistance
CN100465132C (en) Preparation method of carborundum composite-phase ceramic
CN106565250A (en) High-strength alkali-resistant sialon-corundum composite refractory material and preparation method thereof
CN102188983B (en) Fibrous nano porous V2O5-K2SO4 / composite carrier catalyst and application thereof
CN101531527B (en) Producing method of sintering coarse granule silicon carbide products by one reaction
CN102011021A (en) Method for reduction preparation of Mg-Li-Sr alloy by vacuum heat
CN113731422A (en) Preparation method of slurry bed methane synthesis catalyst
CN1242954C (en) Iolite-base composite ceramic with oxygen-storage function and preparing method thereof
CN117696099B (en) Catalyst, process for producing the same, process for producing ethylenically unsaturated acid or ester thereof
CN118835142A (en) Aluminum-silicon alloy ceramic composite shaping phase-change heat storage material and preparation method thereof
CN114345363B (en) Preparation method of isothermal fixed bed methanation catalyst
CN115463650B (en) Isobutane-CO 2 Catalyst for dehydrogenation reaction and preparation method thereof
CN117401987A (en) Unfired Al-SiC refractory material for blast furnace and preparation method thereof

Legal Events

Date Code Title Description
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C06 Publication
PB01 Publication
C14 Grant of patent or utility model
GR01 Patent grant
C19 Lapse of patent right due to non-payment of the annual fee
CF01 Termination of patent right due to non-payment of annual fee