CN1178750C - Method for coating active component on cellular carrier - Google Patents
Method for coating active component on cellular carrier Download PDFInfo
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- CN1178750C CN1178750C CNB021207763A CN02120776A CN1178750C CN 1178750 C CN1178750 C CN 1178750C CN B021207763 A CNB021207763 A CN B021207763A CN 02120776 A CN02120776 A CN 02120776A CN 1178750 C CN1178750 C CN 1178750C
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Abstract
The present invention relates to a method for coating active components on cellular carriers, which comprise: the first end of a cellular carrier is soaked in serous fluid containing active components, vacuum is applied to the second end, so the serous fluid flows into a hole passage of the carrier. Subsequently, the second end of the cellular carrier is soaked in the serous fluid containing the active components, vacuum is applied to the first end, so the serous fluid flows into a hole passage of the carrier. The carrier coated with the serous fluid is dried, wherein the cellular carrier has a particle catching function, the system pressure is from 0 to 85 KPa through the applied vacuum, and the total volume of the serous fluid entering the hole passage of the carrier is from 20 to 98% of carrier volume when the vacuum is applied. With the method is used for coating the carrier, the coating of the carrier is more uniform.
Description
Technical field
The invention relates to a kind of method at coating active component cellular carrier.
Background technology
The diesel car tail gas refining catalyst is to handle modern exhaust gas from diesel vehicle, makes its discharging reach the important means of environmental requirement.The something in common of this catalyst and cleaning catalyst for tail gases of automobiles is to form by a kind of honeycomb substrate and the active component that is coated on the carrier, and described honeycomb substrate all contains numerous parallel ducts.Difference is, the duct both ends open that contains on the honeycomb substrate of cleaning catalyst for tail gases of automobiles, on the cross section hole density be the 46.5-186.0 hole/centimetre
2, the sectional area 0.91-1.72 millimeter in each hole
2And all there is the outlet of an end in each duct that the honeycomb substrate of diesel car tail gas refining catalyst contains by shutoff, on the cross section density 12.4-31.0 hole, hole/centimetre
2, the sectional area 16.0-24.1 millimeter in each hole
2, because each duct is not straight-through, the wall that gas can passing hole channel flows into another duct from a duct, solid particle then can not pass the wall in duct.Therefore, when purifying tail gas of diesel vehicles, force tail gas to pass from the wall in duct, the particle in the exhaust gas from diesel vehicle then is left in the duct of catalyst, thereby both reached control hydrocarbon, carbon monoxide and discharged nitrous oxides, and can control the purpose of solid particle discharging again.Therefore, being used for diesel car tail gas refining catalyst and other each duct that contains the solid particle exhaust gas purifying catalyst all has an end to be known as the honeycomb substrate with particle capture function by the honeycomb substrate of shutoff.
US6,149,973 disclose a kind of method that applies a kind of cylindrical monolithic honeycomb substrate with the coating disperse system, described carrier has discharge orifice vertically, described discharge orifice on cross section with net distribution, above described carrier has one and a bottom surface, this method comprises the steps: that (1) install carrier in vertical direction, and the direction of discharge orifice that makes carrier is for vertically; (2) with the coating disperse system that surpasses about 10% volume of discharge orifice volume from the described discharge orifice of bottom surface filling, make that filling is finished after, the upper section of carrier is flooded by described coating disperse system; (3) above described carrier, remove unnecessary coating disperse system; (4) extract motive force out by one and find time and remove discharge orifice, described extraction motive force comes from through one extracts the vavuum pump that pipe links to each other with the bottom surface of catalyst carrier out.The coating procedure of this method is to adopt siphon principle, makes the slurry carrier that contains active component, thereby reach active component is coated to purpose on the carrier.Adopt this method, even the honeycomb substrate of duct both ends open is applied, the bubble in the slurries also forms vapour lock easily, and slurries can not enter in some duct, cause the coating in the carrier duct inhomogeneous.And when the honeycomb substrate with particle capture function being applied with this method, because having each duct of the honeycomb substrate of particle capture function all is that an end is by shutoff, slurries can not in depth enter the duct of carrier more, therefore, adopt this method can not the honeycomb substrate with particle capture function to be applied effectively at all.
US4,609,563 disclose a kind of method that the catalyst-coated of scheduled volume is arrived a kind of inner surface of hollow matrix, this method comprises that the catalyst slurry with scheduled volume joins in the cavity with the dipping tank at the bottom of, the hollow matrix that will have first, second open end and desire coat internal surfaces reduces, make the end of first opening be arranged in the cavity of dipping tank, and be completely infused in the slurries; This matrix keeps certain height, makes first open end be positioned at distance predetermined and the bottom dipping tank cavity; On second open end of matrix, apply vacuum with a vacuum source, the slurries in all dipping tanks all are inhaled in the matrix, inner surface is applied; Within the predetermined time, second open end in matrix applies vacuum continuously, and all slurries in dipping tank are sucked out and enter in the matrix, the dry coating that forms on matrix.This method is used the method for quantitative adsorption slurry, the volume that is used slurries is identical with the water hole volume of carrier, the shortcoming of this method is, in coating procedure, slurries climb along the duct of carrier, because the effect of the adsorption property of carrier inner surface, the end absorption that slurries are introduced into and the slurries of adhesion are more, the other end is then less, so just caused the inhomogeneous absorption of slurries on carrier, cause coating in the duct of carrier, to form a thickness gradient, make that the catalytic performance of catalyst is not good.This method also can adopt the method for two ends absorption, and the end with carrier is immersed in the slurries earlier, vacuumizes at an other end, after the part in the absorption scheduled volume slurries, rotating carrier is immersed in the other end of carrier in the remaining slurries, repeats the step that vacuumizes and adsorb.Yet even adopt the method for two ends absorption, the absorption of slurries in the duct is also inhomogeneous, and in this case, slurries are more the absorption of carrier two ends, and fewer in the middle adsorbance in duct, therefore, the two ends coating is than thick middle.In addition, this method at remain coating to cleaning catalyst for tail gases of automobiles honeycomb substrate with two openings, because having each duct of the honeycomb substrate of particle capture function all is that an end is by shutoff, quantitatively the method for absorption makes the dispersion of slurries in carrier more inhomogeneous, therefore, this method honeycomb substrate of also being not suitable for being used for to having the particle capture function applies.
Summary of the invention
The objective of the invention is to overcome the uneven shortcoming of prior art coating, provide a kind of coating uniform more method at coating active component cellular carrier.
Method provided by the invention comprises that first end with honeycomb substrate is immersed in the slurries that contain active component, apply vacuum at second end, make slurries enter the duct of carrier, second end with honeycomb substrate is immersed in the slurries that contain active component then, apply vacuum at first end, make slurries enter the duct of carrier, the dry carrier that applies sizing liquor, wherein, described honeycomb substrate is the honeycomb substrate with particle capture function, the vacuum that applies makes system pressure reach 0 to 85 kPa, and the cumulative volume that the time chien shih slurries that apply vacuum enter the carrier duct is the 20-98% of carrier bulk.
The advantage of method provided by the invention is that coating is more even on the catalyst that obtains.For example, the catalyst that method provided by the invention is obtained longitudinally cuts, and with the distribution situation that the method for range estimation is observed catalyst duct floating coat, finds that the coating in the duct is even, does not have the not coated inner surface that occupies.And adopt US4, and the catalyst of the method preparation of 609,563 disclosed employing two ends absorption has some not had coating to be coated near the plug in the duct of shutoff, and coating is inhomogeneous.
Description of drawings
Fig. 1 is the schematic flow sheet of method provided by the invention.
The specific embodiment
According to method provided by the invention, the vacuum that applies makes final system pressure reach 0 to 85 kPa, is preferably 20-80 kPa.The cumulative volume that the time chien shih slurries that apply vacuum enter the carrier duct is the 20-98% of carrier bulk, is preferably 30-80%.
According to embodiment preferred of the present invention, making the slurry volume that enters the carrier duct from first end and second end respectively in the time that second and first end applies vacuum is the 10-49% of carrier inner surface apertures volume, is preferably 15-40%.
The dry condition that applies the carrier of sizing liquor is conventionally known to one of skill in the art, can be 90-300 ℃ as baking temperature, is preferably 100-200 ℃.
According to method provided by the invention, described active component comprises the active component that various exhaust gas purifying catalyst contained of using the honeycomb substrate with particle capture function, and the kind of these components and the content in catalyst are conventionally known to one of skill in the art.
With the diesel car tail gas refining catalyst is example, the active component that the diesel car tail gas refining catalyst contains comprises a kind of heat-resistant inorganic oxide as matrix, the oxide and/or the hydroxide of IVB family element, the oxide of the oxide of the noble metal of group VIII, hydroxide and/or simple substance and rare earth element and/or hydroxide.Total amount with catalyst coat is a benchmark, the content of heat-resistant inorganic oxide is the heavy % of 50-96, be preferably the heavy % of 70-90, the content of the oxide of IVB family element is the heavy % of 1-10, be preferably the heavy % of 4-10, the content of rare earth oxide is the heavy % of 1-30, is preferably the heavy % of 4-20, the content of group VIII noble metals oxide is the heavy % of 0.1-30, is preferably the heavy % of 0.1-20.
Wherein, the described scope that can select as the heat-resistant inorganic oxide of matrix is conventionally known to one of skill in the art, and heat-resistant inorganic oxide can be selected from a kind of in aluminium oxide, silica, silica-alumina, silica-cobalt oxide, aluminium oxide-magnesia, the silica-magnesia as described.Wherein, preferred aluminium oxide, silica or silica-alumina.Aluminium oxide more preferably.
Described IVB family element is selected from titanium and/or zirconium.
Described group VIII noble metals is selected from one or more in ruthenium, rhodium, palladium, osmium, iridium, the platinum, is preferably in rhodium, palladium, the platinum one or more.
Described rare earth element is selected from one or more in lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, the lutetium, is preferably lanthanum, cerium, lanthanum rich mischmetal or cerium-rich mischmetal.
The content of active component is determined according to the content of active component in carrier water hole volume and the final catalyst in the described slurries that contain active component.The total amount of the active component that is in the catalyst to be contained equals the amount of the active component that contained in the slurries with water hole volume equal volume.The described solid content that contains the slurries of active component is the heavy % of 5-30, is preferably the heavy % of 8-20.
Carrier bulk described in the present invention is that the spatial overall of carrier is long-pending, for example, supposes that carrier is a cylinder, and carrier bulk is that cylindrical floor space multiply by cylindrical height.The water hole volume of carrier refers to the volume of the saturated adsorbed water of carrier.
Describe method provided by the present invention in detail below in conjunction with accompanying drawing.
As shown in Figure 1, the honeycomb substrate with particle capture function 1 that will be had anchor clamps 2 clampings of sealing property descends, first end of carrier 1 is soaked in the slurries 4 that are placed in the dipping tank 3, the space of carrier 1 second end is airtight, open vavuum pump 8, air enters buffer 6 along pipeline 5, and discharge from vavuum pump 8 through pipeline 7, because action of pressure, slurries 4 enter the duct of carrier 1, when system pressure reaches greater than 0 to 85 kPa, in the time of preferred 20-80 kPa, and the volume that makes the slurries that enter carrier reaches the 10-49% of carrier bulk, during preferred 15-40%, stops to vacuumize, and open through pipeline 9 and be connected valve 10 on the buffer 6, carrier 1 is promoted from slurries 4 (or do not open valve 10, and directly carrier 1 is promoted from slurries 4), carrier 1 first end no longer is soaked in the slurries 4.With carrier 1 Rotate 180 degree, carrier 1 is descended, second end of carrier 1 is soaked in the slurries 4 that are placed in the dipping tank 3, the space of carrier 1 first end is airtight, open vavuum pump 8, air enters buffer 6 along pipeline 5, and discharge from vavuum pump 8 through pipeline 7, because action of pressure, slurries 4 enter the duct of carrier 1, when system pressure reaches greater than 0 to 85 kPa, in the time of preferred 20-80 kPa, and the volume that makes the slurries that enter carrier reaches the 10-49% of carrier bulk, during preferred 15-40%, stops to vacuumize, and open through pipeline 9 and be connected valve 10 on the buffer 6, carrier 1 is promoted from slurries 4 (or do not open valve 10, and directly carrier 1 is promoted from slurries 4), carrier 1 second end no longer is soaked in the slurries 4.Unload carrier 1 from anchor clamps 2, drying obtains catalyst.Wherein, the slurries 4 in the dipping tank 3 can be by holding vessel 12 through pipeline 11 continuous or interruption supplies.
The following examples will the present invention is described further, but therefore do not limit the present invention.
Example 1
This example illustrates method provided by the invention.
As shown in Figure 1, in dipping tank 3, add a kind of slurries 4.These slurries 4 are with boehmite (salic 32 heavy %, the Shandong catalyst plant is produced), zirconium oxychloride (ZrOCl
28H
2O, Beijing Chemical Plant's product), rare earth chloride (contains and mixes rare earth oxide 44 heavy %, wherein, lanthana accounts for 40 heavy % of mixed rare-earth oxide, cerium oxide accounts for 53 heavy % of mixed rare-earth oxide, and other rare earth oxide accounts for 7 heavy % of mixed rare-earth oxide), the rhodium chloride solution of the platinum acid chloride solution of platiniferous 0.02082 grams per milliliter, rhodium-containing 0.0041 grams per milliliter and deionized water be mixed with and form.Contain aluminium oxide 7.5 heavy % in these slurries 4, zirconia 0.5 heavy %, (wherein lanthana 0.6 weighs % to rare earth oxide 1.5 heavy %, cerium oxide 0.8 heavy %, other rare earth oxide 0.1 heavy %), platinum 0.25 heavy %, rhodium 0.25 heavy %, water 90 heavy %, the solid content of slurries are 10 heavy %.
To be descended by the honeycomb substrate with particle capture function 1 that rubber clamp 2 clamps, first end of carrier 1 is soaked in the slurries 4 that are placed in the dipping tank 3, the space of carrier 1 second end is airtight.Described carrier 1 is the cylindrical ceramic carrier, and weight is 1312 grams, and cross-sectional area is 162.24 centimetres
2, be 15.24 centimetres highly, the stomatal number on the cross section be 15.5 holes/centimetre
2, pore is the square pore of 4 millimeters of the length of sides, the pore sectional area is 16.0 millimeters
2, carrier bulk is 2473 milliliters, and all there is an end ripple shutoff in each duct, and the water hole volume of carrier is 494.6 milliliters.
Open vavuum pump 8, air enters buffer 6 along pipeline 5, and discharge from vavuum pump 8 through pipeline 7, when system pressure reaches 70 kPas, keep this pressure, reach 20% of carrier bulk until the volume that enters the slurries in carrier duct from first end, the volume of slurries that enters the carrier duct is by placing the title under the dipping tank to measure weight and become volume to record by density conversion.Open through pipeline 9 and be connected valve 10 on the buffer 6, carrier 1 is promoted from slurries 4, carrier 1 first end no longer is soaked in the slurries 4.With carrier 1 Rotate 180 degree, carrier 1 is descended, second end of carrier 1 is soaked in the slurries 4 that are placed in the dipping tank 3, the space of carrier 1 first end is airtight, opens vavuum pump 8, and air enters buffer 6 along pipeline 5, and discharge from vavuum pump 8 through pipeline 7, when system pressure reaches 70 kPas, keep this pressure, reach 20% of carrier bulk until the volume that enters the slurries in carrier duct from second end.Stop to vacuumize, and open through pipeline 9 and be connected valve 10 on the buffer 6, carrier 1 is promoted from slurries 4, carrier 1 second end no longer is soaked in the slurries 4.Unload 1,130 ℃ of oven dry of carrier from anchor clamps 2, obtain catalyst C1.Longitudinally cut catalyst C1, observe the uniformity coefficient of coating, find that coating is very even, and the inner surface in all ducts is all coated covers.Coating consists of aluminium oxide 75 heavy %, zirconia 5 heavy %, rare earth oxide 15 heavy % (wherein lanthana 6 weighs %, cerium oxide 8 heavy %, other rare earth oxide 1 heavy %), platinum 2.5 heavy %, rhodium 2.5 heavy %.Coating is formed by calculating.
Comparative Examples 1
This Comparative Examples explanation art methods.
According to US4,609,563 disclosed methods apply the honeycomb substrate with particle capture function.As Fig. 1, will be descended by the honeycomb substrate with particle capture function 1 (with example 1) that rubber clamp 2 clamps, first end of carrier 1 is soaked in the 494.6 milliliters of slurries 4 (with example 1) that are placed in the dipping tank 3, the space of carrier 1 second end is airtight.
Example 2
This example illustrates method provided by the invention.
As shown in Figure 1, in dipping tank 3, add a kind of slurries 4 (with example 1), to be descended by the honeycomb substrate with particle capture function 1 (with example 1) that rubber clamp 2 clamps, first end of carrier 1 is soaked in the slurries 4 that are placed in the dipping tank 3, the space of carrier 1 second end is airtight.
Open vavuum pump 8, air enters buffer 6 along pipeline 5, and discharge from vavuum pump 8 through pipeline 7, when system pressure reaches 50 kPas, keep this pressure, reach 30% of carrier bulk until the volume that enters the slurries in carrier duct from first end, the volume of slurries that enters the carrier duct is by placing the title under the dipping tank to measure weight and become volume to record by density conversion.Directly carrier 1 is promoted from slurries 4, carrier 1 first end no longer is soaked in the slurries 4.
With carrier 1 Rotate 180 degree, carrier 1 is descended, second end of carrier 1 is soaked in the slurries 4 that are placed in the dipping tank 3, the space of carrier 1 first end is airtight, opens vavuum pump 8, and air enters buffer 6 along pipeline 5, and discharge from vavuum pump 8 through pipeline 7, when system pressure reaches 50 kPas, keep this pressure, reach 30% of carrier bulk until the volume that enters the slurries in carrier duct from second end.Stop to vacuumize, directly carrier 1 is promoted from slurries 4, carrier 1 second end no longer is soaked in the slurries 4.Unload 1,130 ℃ of oven dry of carrier from anchor clamps 2, obtain catalyst C2.Longitudinally cut catalyst C2, observe the uniformity coefficient of coating, find that coating is very even, and the inner surface in all ducts is all coated covers.Coating is formed aluminium oxide 75 heavy %, zirconia 5 heavy %, rare earth oxide 15 heavy % (wherein lanthana 6 weighs %, cerium oxide 8 heavy %, other rare earth oxide 1 heavy %), platinum 2.5 heavy %, rhodium 2.5 heavy %.
Claims (14)
1. method at coating active component cellular carrier, this method comprises that first end with honeycomb substrate is immersed in the slurries that contain active component, apply vacuum at second end, make slurries enter the duct of carrier, second end with honeycomb substrate is immersed in the slurries that contain active component then, apply vacuum at first end, make slurries enter the duct of carrier, the dry carrier that applies sizing liquor, it is characterized in that, described honeycomb substrate is the honeycomb substrate with particle capture function, and the vacuum that applies makes system pressure reach 0 to 85 kPa, and the cumulative volume that the time chien shih slurries that apply vacuum enter the carrier duct is the 20-98% of carrier bulk.
2. method according to claim 1 is characterized in that, the vacuum that applies makes final system pressure reach 20-80 kPa, and the cumulative volume that the time chien shih slurries that apply vacuum enter the carrier duct is the 30-80% of carrier bulk.
3. method according to claim 1 is characterized in that, making the slurry volume that enters the carrier duct from first end and second end respectively in the time that second and first end applies vacuum is the 10-49% of carrier bulk.
4. method according to claim 3 is characterized in that, making the slurry volume that enters the carrier duct from first end and second end respectively in the time that second and first end applies vacuum is the 15-40% of carrier bulk.
5. method according to claim 1, it is characterized in that, described active component comprises a kind of heat-resistant inorganic oxide as matrix, the oxide and/or the hydroxide of IVB family element, the oxide of the noble metal of group VIII, the oxide of hydroxide and/or simple substance and rare earth element and/or hydroxide, total amount with catalyst coat is a benchmark, the content of heat-resistant inorganic oxide is the heavy % of 50-96, the content of the oxide of IVB family element is the heavy % of 1-10, the content of rare earth oxide is the heavy % of 1-30, and the content of group VIII noble metals oxide is the heavy % of 0.1-30.
6. method according to claim 5, it is characterized in that the content of heat-resistant inorganic oxide is the heavy % of 70-90, the content of the oxide of IVB family element is the heavy % of 4-10, the content of rare earth oxide is the heavy % of 4-20, and the content of group VIII noble metals oxide is the heavy % of 0.1-20.
7. according to claim 5 or 6 described methods, it is characterized in that described heat-resistant inorganic oxide is selected from a kind of in aluminium oxide, silica, silica-alumina, silica-cobalt oxide, aluminium oxide-magnesia, the silica-magnesia.
8. method according to claim 7 is characterized in that described heat-resistant inorganic oxide is selected from aluminium oxide, silica or silica-alumina.
9. method according to claim 8 is characterized in that described heat-resistant inorganic oxide refers to aluminium oxide.
10. according to claim 5 or 6 described methods, it is characterized in that described IVB family element is selected from titanium and/or zirconium.
11., it is characterized in that one or more in described group VIII noble metals selected from rhodium, palladium, the platinum according to claim 5 or 6 described methods.
12., it is characterized in that described rare earth element is selected from lanthanum, cerium, lanthanum rich mischmetal or cerium-rich mischmetal according to claim 5 or 6 described methods.
13. method according to claim 1 is characterized in that, the described solid content that contains the slurries of active component is the heavy % of 5-30.
14. method according to claim 13 is characterized in that, the described solid content that contains the slurries of active component is the heavy % of 8-20.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021207763A CN1178750C (en) | 2002-05-31 | 2002-05-31 | Method for coating active component on cellular carrier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021207763A CN1178750C (en) | 2002-05-31 | 2002-05-31 | Method for coating active component on cellular carrier |
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| Publication Number | Publication Date |
|---|---|
| CN1461674A CN1461674A (en) | 2003-12-17 |
| CN1178750C true CN1178750C (en) | 2004-12-08 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021207763A Expired - Lifetime CN1178750C (en) | 2002-05-31 | 2002-05-31 | Method for coating active component on cellular carrier |
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- 2002-05-31 CN CNB021207763A patent/CN1178750C/en not_active Expired - Lifetime
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