CN1010382B - Method of impregnating ceramic monolithic structures with predetermined amounts of catalyst - Google Patents
Method of impregnating ceramic monolithic structures with predetermined amounts of catalystInfo
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- CN1010382B CN1010382B CN 85101134 CN85101134A CN1010382B CN 1010382 B CN1010382 B CN 1010382B CN 85101134 CN85101134 CN 85101134 CN 85101134 A CN85101134 A CN 85101134A CN 1010382 B CN1010382 B CN 1010382B
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- building block
- coating
- slurries
- vacuum
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Abstract
The present invention discloses a method for impregnating the internal skeleton structure of a carrier by slurry containing catalysts. In the processes, the catalyst slurry quantified in advance is poured in a container quantitively to be in contact with one end surface of the carrier, and a cover is placed on the edge of the second end surface opposite to the first end surface and is sealed by a sealing ring. The space between the cover and the adjacent second end surface is defined to be a vacuum, the catalyst slurry is sucked in the skeleton structure from a bottom end surface after a vacuum is applied to the cover, and therefore, the internal skeleton structure (on the wall surfaces of an internal passage) is uniformly impregnated by the catalyst slurry.
Description
The present invention relates to dipping, particularly with giving earlier quantitative catalyst soakage carrier about the monolithic ceramic catalyst carrier.
Toxic substance in the current well-known elimination Vehicular exhaust or to change it into harmless composition be as a kind of method that overcomes atmosphere pollution, people more and more know clearly simultaneously, now and all must partly load onto catalytic reactor device from now at vehicle exhaust, about this respect, the catalyst that promptly provides in reactor is a kind of skeleton structure of the integral body that scribbles catalyst firmly, or honey comb like member, it is the garden cylindricality or avette usually.For surface as much as possible is provided, a lot of vertical passages are arranged in the inside of member in member.
Hard, the skeleton structure of monoblock is to be made by pottery, this class pottery is made up of fire-resistant crystalline material, for example: sillimanite (Al
2SiO
5), magnesium silicate, zircon (ZrSiO
4), petalite (LiAlSi
4O
10), spodumene, cordierite, alumina silicate, mullite (Al
6Si
2O
18) or their composition.It has been generally acknowledged that the surface that this class material has porous,, be recommended in usually before the impregnated catalyst in order to improve the Surface Permeability of skeleton face, earlier on skeleton structure the highly porous alumina layer of coated one deck to increase effective surface area.These monoblocks, existing narration in the whole skeleton carrier patent documentation before this of actual catalytically inactive.For example Keith(translates: base is thought) wait the U.S.Patent(United States Patent (USP)) its patent No. is 3,331,787 and 3,565,830, here just be not described in detail.
Than typical method, at this measure one example, catalyst component includes I B family in the one or more periodic table of elements, V B family, the noble metal of VII B family and VIII family, base metal and metal oxide, be meant copper, vanadium, chromium, magnesium, iron, cobalt, nickel, platinum, palladium, rhodium and calcium especially, catalyst metals can be a single variety, also can be that it follows one or more other reactive metals to use with.
In the literature in Ji Zai the whole bag of tricks, cited is with high-temperature resistant coating aluminium oxide and come coated monoblock carrier with for example noble metal catalyst coating such as platinum, palladium and rhodium for example, these methods consider it is totally unfavorable from the cost viewpoint, thereby dwindled applying of coating greatly, Ang Gui precious metal particularly with catalytic activity, for example on high surface area surface codeposition with platinum, palladium and the rhodium of refractory metal.
So U.S.3,565,830 have introduced the monoblock skeleton structure have been soaked in being coated with slip, stir simultaneously, make slurry go deep into inner duct fully, later on the method for vibrations with gently remove outer surface and starch with the excessive amount of being coated with that is blocked in the internal channel with air blowing.U.S.P.3,873,350Dwyer etc. have narrated in patent the monoblock carrier have been soaked in being coated with slip, later, take out the carrier coated slurry, vibration venting redundant sizing agent, and when blowing air and dredge passage, carrier is constantly made horizontal axis rotate.
Soaking like this, coating technology, the one, many times of change expense, and also has another disadvantage, be that slurry is coated on the whole object, both comprised wherein that the inner skeleton works also comprised exterior circumferential surface, when using the conduct of noble metal catalyst salt precious metal to be coated with the component of slip, since normal when using the catalyst block member vehicle exhaust with the building block appearance contact that is contained in the catalytic reactor, thereby just in vain the waste of that part precious metal of coated on the outer surface.
At U.S.4,039,482, someone proposes with the coating slurries ceramic monolithic carrier to be carried out vacuum impregnation to accelerate the coated process, for example platinum or platinum catalytically-active metals carry out coated to the ceramic monolith structure part with aluminium oxide and those in order, earlier member is placed in the pressure vessel, hold to fill in the structure and be coated with slip, then with the member application of vacuum, use the slurry dipping members, after the vacuum impregnation, slurry emits from container, then compressed air is blown over container and is removed excessive slurry, carries out high temperature drying after this.
At U.S.4, in 208,454 too with the slurry ceramic block member that soaks, the pasting in the member skeleton passage is removed in application of vacuum then, and application of vacuum will constantly be carried out, so that air enters in the member passage in rapid succession, with thorough removing blocking channel and redundant sizing agent, U.S.4,039,482 and U.S.4,208,454 two pieces of patent contents all are with the excessive pasting ceramic monolithic structure of soaking, excessive greatly pasting always has loss, loss be expensive catalyst metals.U.S.4,038, the 482 vacuum-impregnated method of introducing of ceramic component, still similar previous dipping is coated with the method for slurry, thus still exist the member external surface deposited some costliness but inoperative coating.
U.S.4,039,482 and U.S.4,208, used excessive coating in 454 the technical process, thereby at U.S.4,039, added the step that to use the unnecessary coating of air scavenging in 482, U.S.4 simultaneously, 039,482 and U.S.4, during setting forth, 028,454 two piece of patent all requires the step that ceaselessly vacuumizes.
These steps all are both to take time undoubtedly, have increased the cost in the technical process again.Therefore at the catalyst of ceramic integral impregnated catalyst substantially, requirement provides a kind of method, and it can accurately control the quantity of aluminium oxide and metallic catalyst coating, to reduce the coating excess quantity, can reach the efficient that had both improved process work like this, reduce the purpose of paint loss simultaneously again.
The present invention can meet following requirement, be high-temperature resistant coating slurry or the catalyst metals that vacuum covering ceramic monolith member uses a kind of method is provided, reach accurately to control to give and determine good coating quantity earlier, and metering ground coated goes to support element, this has just removed from need be with the excess coating material member that soaks, also removed simultaneously the additional step of from member, removing excess coating material that brings by the process of soaking from, according to process of the present invention, can be by the high-temperature-resistant layer of needed concentration preparation and a kind of uniform coating of catalytic metal component, no longer need to manage to remove unnecessary amount component surface there in the coated process and remove in the inner skeleton that part of coating content in the blocking channel.
In the method for the invention, a following end of the ceramic monolithic structures of exotic material that will flood or catalytic metal composition or all two kinds of materials is placed in a jar or the container, is placed with in the middle of its and gives earlier quantitative pasting by the needed coating of skeleton passage of coated monoblock support element.A tubaeform lid is placed on the other end of ceramic monolithic structures.
Seal between lid and ceramic component.Vacuumize (promptly being lower than atmospheric pressure) at the building block other end.
Coating is inhaled under the effect of vacuum in the inner skeleton passage of ceramic monolithic structures up to all coating in container by extinction, then, vacuum breaker, open the coverage rate of bulk ceramics member, take out the good member of coated, according to practice of the present invention, in the integrated member coated to just within it on portion's skeleton channel wall, thereby there is no need from monolithic structures to get rid of and to clean excessive coating, simultaneously also unnecessaryly carry out any application of vacuum step of giving, and from monolithic structures, give the step of draining air earlier, the ceramic integral member carries out surperficial coated by giving quantitative coating earlier, through a drying device or heat treatment occasion coating is carried out high-temperature maturing then.
A reasonable detailed process that has some strong point among the present invention is with vacuum on the termination of ceramic component, carrying out the vacuum suction is coated with, elder generation carries out vacuum impregnation with the pasting that a part accounts for total amount 50% to 85% greatly, then turn around, carry out the vacuum suction is coated with from the other end of ceramic component, find such process, can accelerate dipping process, improved the distributing homogeneity of coating on the inner frame channel wall greatly.
Fig. 1 is the hasty profile that carries out coated ceramic monolithic skeleton carrier member according to the present invention.Our idea is the technology place that can give prominence to this patent in conjunction with referring to sketch and more detailed explanation, makes the reader can well understand the features and advantages of the present invention.
As indicated in the figure, be suitable at present actual device system preferably.
First comprises that an open containers or plate 10 the insides load onto coating slurries 11, slurry face indicated altitude is with reference to 11a, on Pan10Bi, open flatly, access port pipe 13, charging valve 13a suitably is loaded in 13 pipelines, as the operation valve that is arranged in dish 10 outsides, valve 13a operation can be manual, also can be automatic.
Second portion is the top that is positioned at first, and the tubaeform cover 14 of a hollow is arranged, the bottom of cover 14 be one to the tubaeform circle 14a that extends out out.Cover 14 open tops connect conduit 15, and the last suitable valve of string (not drawing in the picture) is connected to the vavuum pump of mentioning (not drawing among the figure) in the conduit 15.
The inside of member 18 has many from a vertical passage that extends to the other end, in order to express clearly, among the figure represented support element be drawn as square, but be actually the garden cylindricality or avette.Fix (not drawing among the figure) with a suitable way in the monolithic structures 18 coating slurries, it can be a kind of anchor clamps, and as a kind of mechanical grip device, best this anchor clamps can rotate 180 degree in coating slurries 11.
During operation, building block 18 ships from storehouse, be fixed on the dish 10 above, leave the face of trying to get to the heart of a matter 16 certain distances, open valve 13 yield quantitative slurries 11 usefulness pumps squeeze into the dish 10, the liquid level 11a of the coating slurries of control injection dish 10 is to certain altitude, locating below case like this is building block lower surface 18a, and it is in floodage, compresses after sandwiching sealing ring 20 between cover limit 14a and the building block upper end 18b, valve in conduit 15 is adjusted then, and space 21 and vavuum pump are interconnected.After vacuum is connected in space 21, owing to use negative pressure, the coating slurries just flood part and up are sucked into building block 18 from plate 10, arrow 22 expression slurries flow to and are sucked into 18a under the building block that is flooding, arrow 23 expression vacuum are used pumping direction, 21 will keep the suction that can stably make progress of slip liquid that the vacuum time enough floods part with retaining member piece 18 to be coated onto the inner passage of building block in the space, form the very big dope layer of surface area, and/or form that to make the poisonous vehicle exhaust of conversion be the catalyst layer of non-toxic gas.
In dish 10 after being coated with slip and having aspirated of ormal weight, the vacuum at 21 places is abolished in the space, pressure returns to atmospheric pressure, cover 14 is still upwards mentioned from building block limit, upper end (18b) then, after then taking building block apart anchor clamps from plate 10 tops, directly take away, be put in the drying box and (do not draw among the figure), coating in the building block inner passage in drying box is dried, if need, molten roasting more once because by the coating of controlled quentity controlled variable coated in the member body, the necessity of mentioning in the former document of problem of these states of draining unnecessary amount coating and getting rid of the obstruction of inner surface in the coated operation has not just existed.
In practical application of the present invention, contain high temperature resistant solid part of the high surface of suspended state in the coating slurries.For example, gamma (gamma or γ) aluminium oxide or have catalytically-active metals, for example platinum and palladium; The salt of aqueous solution state is as chloroplatinic acid and palladium bichloride; They can be with similar slurry with high temperature resistant solid codeposition together.
Want the amount of coated coating slurries and in dish, measure 11, when being easy to calculate in the metering between the coated building block successively, the foundation of calculating is to want the internal surface area of the skeleton piece of coated, can calculate by following formula according to the weight that needs coated to calculate required coating slurries in the solid coating amount of member body inner channel walls after the building block drying:
The weight of filling (wet amount)=(matrix volume (cubic feet per inch) * do amount (gram/cubic feet per inch))/(solid content percentage/100 in the slurries)
Herein
" wet as to measure "-amount of slurry, gram gives quantitatively at the inner passage of building block coated, and weighing is wanted in plate 10.
The inner volume of wanting coated of " matrix volume "-building block.
" do amount "-behind the building block bone dry, remain in solid-state coating compound amount in inner passage, i.e. exotic material or catalyst weight, perhaps both.
The representative property of the coating slurries that the present invention uses in practice: be a kind of catalyst platinum-rhodium/aluminum slurry below the example.
The better scope of character general range
Viscosity-centipoise 15～300 17～17
% contains amount of solid 35～52 45～50
Contain aluminium oxide % 50 in the amount of solid～99.9 65～99
The application of paint slurries carry out vacuum to building block and are coated with suction actually, its vacuum 0.5 English inch water column to 20.0 English inch water columns or more than.
Real process to the more normal employing of the present invention, being in when back sealing at the limit, upper end of building block 18a with cover 14 one after the other has and sequentially increases negative pressure the suction that is coated with of member, the range of viscosities of more suitable for this reason coating slurries is 45-50 centipoises, quite low vacuum is incorporated on the monolithic structures such as 0.5 to 0.7 English inch water column, 1 to 8 second time, give quantitative wet slurry dipping members piece with about 50% to 85%.
Beginning applies building block with what pointed out than low vacuum, and the inner passage of building block can be flooded equably, and " going out thorn " phenomenon is seldom arranged on the building block inner channel walls.
Because it is higher in initial vacuum often " to go out to sting " generation of this phenomenon, slurry fails to aspirate equably, topped on the inner channel walls of carrier, rise than the high 2 English inch of channel part at some part slurry face in the centre, projecting surface is called as thorn in these pipelines; After this, than higher vacuum, higher 5 to 10 times such as vacuum than the vacuum of bringing into use, i.e. 3 to 20 English inch water columns, the suction coated that under this vacuum building block is carried out 10-30 time second the inner passage of the remainder coated building block of coating slurries on.If give the higher at the beginning vacuum of building block in the suction coated stage, be vacuum 6 to 8 English inch water columns, though the time that needs of coated material coating slurries can shorten fully, but measured, using high initial vacuum floods and has caused the upper end of scurrying the member body on a part of slurry and the loss slurry, also have higher vacuum to cause that big material coating goes out thorn, and causing in the member body inner passage the inhomogeneous of heavy stain, this uneven coating impregnation state directly reduces in the automobile exhaust system function with the building block of toxic gas catalyzed conversion function.To mentioning that as preceding by the viscosity that is coated with slip 15 to 300 centipoises of present practical application of the present invention, preferable is 17 to 70 centipoises.The coating slurries are drawn in the inner passage of member body, in this range of viscosities, help the coating slurries to rest on the conduit wall, when slurry viscosity increases, for slurries are up aspirated, vacuum also must be done accordingly to adjusted, when the coating slurry viscosity is lower than 15 centipoises when a lot, suction coating can go wrong.The vital point that the present invention of Practical significance-be coated with slip vacuum impregnation process arranged is for when building block is fixed in the container, part is submerged in the slurries, the lower surface 18a of building block is placed in the container, before building block is carried out application of vacuum, between the bottom surface 16 of the base of building block and plate 10 slit is arranged, size is to become with the size of member body and shape.Carry out the coating dipping for special member, the break joint distance that fits in the needs most is easy to determine by experiment.
Such as to 3.18 * 6.68 * 6.3(English inch) the avette stone building block of size, best clearance distance records it by experiment and is approximately 0.040 English inch, when this slit near this give first regulation apart from the time, carry out vacuum impregnation according to the present invention, so, on the inner channel walls of member body, will reach the satisfied evenly coating of heavy stain.If the slit is during greater or less than the numerical value of being determined by experiment of the best, the coating that discovery obtains is inhomogeneous, such as when slit during greater than optimum value, the coating that is immersed in the member body concentrates on the intercooler core position of member body, and the coating that is immersed in the member body during less than optimum value when the slit concentrates on the outer annular ring of member body.Usually to member block structured number range, to 6.3 English inch, under this size range, the clearance distance that suitable coated process is used is from 0.020 to 0.125 English inch approximately from about 2.5 English inch for fixed its height.By the present invention, in actual application, also used another method, it is when carrying out the vacuum impregnation step, when building block to give quantitative 50% by weight to 85%() after the coating slurries finish dipping, return to normal pressure, then building block is fallen turnback, then continue vacuum impregnation, can see that this method has been improved the uniformity of coating on the internal channel wall from opposite that end.
Impregnated building block, slough the moisture content of its inside through the drying equipment building block drying that coated is good there, general building block baking temperature is 125～250 ℃, can guarantee to remove the moisture content of all the inside blendings like this, and coating can firmly adhere on the inner road wall, dry back is controlled it to the good building block of coated and is made it cooling, and can directly can take with hand without the carrier protective gloves up to operating personnel is as the criterion.
According to process of the present invention, what the patent application of this effective building block coating and process thereof was used is meticulous, the controllable quantitative coating of elder generation that gives, reduced the quantity in stock of coating in the dipping process, reduce the possible problem in the actual treatment, thereby also reduced the cost of paying owing to the loss expensive catalyst material of slipping up and carelessness causes.
Can give quantitative coating slurries with fast speeds according to process of the present invention floods building block inside coated, there is example to show that its cycle was less than 1 minute, with dripping the processing method be coated with or spray by comparison, these out-of-date methods not only slowly but also time-consuming with those.
Process of the present invention is to have done improvedly to proposing vacuum impregnation technology in the previous document, and it does not have the heavy stain of excessive coating on the outer surface of building block; Eliminated the air blowing step; And the expensive coating of loss therefrom because in the inner passage of building block, there is not excessive coating deposition, in the previous document in vacuum impregnation coating process required cleaning step also eliminated.
Process of the present invention also can in seconds be flooded fast, does not outgas, and gives uniform coating slurry coating.
Hereinafter will explain with regard to the practical process of the present invention, the building block of catalytic can carry out coated by required coating slurries at an easy rate accurately, and this slurries consumption can be calculated earlier before dipping process, and it is irrelevant with the minimum weight of member.
Be deposited on the coating content of building block one by one, the amount on every is identical basically.The deviation of their each interblocks is very low, and only positive and negative 0.5%.
In the vacuum impregnation process of the present invention, use accurate weight of coated paint, after aspiration procedure is finished, the adsorbance that remains in the dish seldom we can say almost do not have, this has just eliminated the potential of the loss amount of being coated with may, analyzed by the coating material balance that is used for by process of the present invention, 99.7% coating slurries are heavy have been steeped on building block.
From impregnated in the result of cordierite building block.Basically be to be deposited on the member entirely, measure that 0.1%(weight meter of explanation) the coating slurries are the filtration place 0.2%(weight meters of being caught to combine in vacuum system) coating (in solid) remain in the plate 10.
In order to further specify process of the present invention, enumerate following several example about actual dipping process to the ceramic component piece.
Example 1
" long avette ceramic monolithic structures has honeycomb briquette shape internal structure, and interior surface thereof is long-pending to be 110.3 cubic feet per inch, by granular cordierite (2MgO2Al in 3.18 " * 6.68 " * 6.3 that 9 of series give weighing earlier
2O
35SiO
2) entitling that makes is the universal ceramic monolithic structure of M-20, with viscosity is 49 centipoises, contain amount of solid and be the 45.1%(66.5%(weight meter of amount of solid wherein by weight) what be left for aluminium oxide is platinum and rhodium, weight ratio is that 10: 1 catalyst mixture and being coated with in the slip of some base metal oxides is coated with.
By the requirement of this specification, the coating compounds of 253.61 grams are deposited on have equably made on the building block inner passage profile of above-mentioned size because the used cat ceramic piece of catalytic reactor in the automobile, as the slip amount that is coated with of the required usefulness of deposition of solid promptly with the formula calculating that proposed with the front:
Wet that amount=(110.3 cubic feet per inch * 25.91 gram/cubic feet per inch)/(45.1/100)=563 restrain
Sketch has been introduced the style that the building block inner passage is coated with a kind of equipment that the dipping of slip uses, when each module component of 9 one group of dipping, elder generation coils in 10 with 1/2nd be added to with being coated with about 281～282 gram meterings of slip, the bottom of building block is dipped into and is coated with in the slip, and vertically fix the position, 0.04 English inch is adjusted in slit between the bottom surface 16 of building block bottom 18a and plate 10, be lowered under tubaeform cover 14 blows slowly from top to bottom building block upper end limit 18b and 14 sealings of cover are adjacent to, the top of building block applies the vacuum of the water column of 0.625 English inch according to priority, time remaining 5 seconds, 50% the quantitative coating slurries that give charge in the building block, then increase vacuum, draw up 15 seconds of air (containing 9 English inch water columns) time remaining of 200SCFM to Danone, at this moment finished half has been coated with the work that slip is impregnated into building block, remove vacuum then, join in the dish to the coating slurries metering of second half scheduled volume, building block is fallen turnback, be about to be originally that the upper end of building block now is positioned in the plate, the slit still is adjusted into 0.040 English inch, the operation in tandem of repeating vacuum, i.e. 5 seconds of 0.625 English inch water column, 9 English inch water column vacuum remained the dipping of 50% piece table area in 15 seconds then.
Claim the weight of the member body of coating slurry, detect its wet feed and must measure that then that coated is good member is weighed about 120 ℃ of dryings one hour again, and number is recorded in the following table 1.
Carry out the building block coated by this process, the letter character that entitling is used is AI-19.
After 1-99 module component piece coated is finished, with give the plate that claimed earlier 10 and be bound up on cover 14 ground in the middle of the vacuum-pump line filter 4 dryings and weigh, the weightening finish gram number of plate is 3.5 grams after measured, 0.073% this scale that just accounts for total deposition in the building block shows the coating content that remains in the dish, just one of them part that loses in the coated process.The gram number that records in filter is 38.4 grams or accounts for 0.81% of deposition on the building block, these part expression coating slurries fail to be deposited on the inner passage of building block through building block in aspiration procedure, and conclusion we can say that the part that the coating slurries go less in the coated process only accounts for 1%(weight meter) below.
Will be according to the good drying of example 1 dipping three sections of horizontal one-tenth in branch ground such as building block.Measure the infiltration sample degree uniformity of coating at the building block inner surface.
Point out that through checking these strippings and slicings coating is to be evenly distributed on the whole inner passage of building block really.
Come comparison with the monolithic structures with identical originally the run into method of soaking, its practical measurement shows that clearly the osmotic gradient value is to have improved really.
Table 1
Originally heavily wet restitution is heavy+do heavily dried must measuring
Sample Ke Kekeke
A-1 768.5 504.5
B-2 766.5 508.5
C-3 766.5 506.5
D-4 761.0 516.0 1014.7 253.7
E-5 762.0 511.0
F-6 761.5 521.5 1016.0 254.5
G-7 761.5 512.5
H-8 761.5 513.0
I-9 760.5 510.0 1013.6 253.1
Example 2
Basically repeat the process of example 1, different is to building block sequentially earlier with vacuum be 0.625 English inch water column flood for 5 seconds 85% give quantitative coating slurries on building block, vacuum is that 9 English inch water columns make the coating slurries of suction inner passage are fully flooded its inner passage 20 seconds then.Subsequently, building block is fallen turnback, soaked now at dish 10 in the upper end of former building block, apply 15 seconds of negative pressure of the vacuum of 9 English inch water columns then, give quantitative slurry with remaining 15% and go to be impregnated in the inner passage with original reverse suction.
The data record of this process is in table II, the member coated entitling English alphabet J-1 of this process.
The osmotic gradient testing surface determines to have reached heavy uniformly stain and infiltration on the wall of whole member piece inner passage.
The table II
Original weight is wet that amount restitution weight+dry weight is done heavyly
Sample Ke Kekeke
J-1 765.0 510.0
K-2 768.0 529.0
L-3 767.5 509.0
M-4 760.5 510.5
N-5 765.0 507.0 1019.9 254.9
O-6 762.0 513.0 1015.9 253.9
P-7 759.0 514.0
S-8 762.5 514.0
T-9 762.0 515.0 1015.6 253.6
The example III
Repeat routine I process, different is,
6 avette building blocks 3.18 " * 6.68 " * 6.3 "
Contain valuable slurries with 614 grams, its materials consist of 80% aluminium oxide (Al
2O
3), 1.8% precious metal (platinum: rhodium=5: 1) and 18.2% base metal oxide viscosity be 55 centipoises, solid content 47.09%.
Building block is immersed in the slurry in that bottom surface and plate that the slit is 0.075 English inch at the end.
Method that need not sequential change vacuum, but took out foot 2 minutes with the first half amounts of 614 grams; the first half slurry in 614 grams is drawn into the building block the inside; and after drawing into uniform deposition on portion's skeleton surface channel within it; remove vacuum; building block is fallen turnback; the face on will former building block before this now places dish to be submerged in slurries in order to the negative pressure of 200SCfm air (promptly 9 " water column), clearance distance is with original the same, add level of vacuum also with original the same, promptly 9 English inch water columns, have gone so back half material of 614 grams is drawn in the building block that has deposited coating more equably at 2 minutes time.
Building block 200 ℃ of dryings 13 hours, dry building block after measured, precious metal solid impregnating layer has been evenly distributed in the building block, the solid adhesion amount of six module component pieces, point out that by analysis its total variation of coated building block is positive and negative 1.4% in order.
Show to have pointed out fully in the III result that obtains below
The table III
The attached slurry of the heavy solid of sample vacuum draw building block
The product slurry is restraining to be measured
Number gram original weight dry weight gram %
The suction for the second time of suction for the first time
1 307.5 306.5 767 1069 302 49
2 306.5 306 765 1066 301 49
3 306.5 306 763 1065 302 49
4 306 306 761 1064 303 49
5 306.5 306.5 765 1068 303 49
6 306.5 306.5 763 1068 305 49
Dry 200 ℃ average 302 49%
L＝±1.4%
The example IV
Repeat the process of routine III, different is: test is all given quantitative coating slurries and is drawn in the building block by the lower end of building block, and test is no longer carried out building block and fallen the step of turnback.From building block lower end suction coating slurries 614 grams, enter in the building block, keep enough vacuum, be 200SCfm air (i.e. 9 English inch water columns) experience 5 minutes, from measuring building block, though noble metal solid part is to be evenly distributed in its inner passage, its Σ variation of solid adhesion amount of analyzing 6 is 8.5%, significantly makes mistakes from data if reject sample NO8(sample NO8) the Σ variation of five samples is positive and negative 4.3%.These results show in the table IV fully:
The table IV
Sample number suction coating building block weight solid adhesion amount % slurries
Slurries (vehicle weight) gram
NO restrains former dried gram
7 613 768 1052 284 46
8 613 765 1031 266 43
9 613 765 1043 278 45
10 613 763 1050 287 47
11 612 762 1049 287 47
12 612 765 1063 288 47
Average 281 46%
Σ±8.5
Front of the present invention has been narrated all processes, and has further lifted routine the explanation inner skeleton structure of ceramic monolithic structures is carried out coated and dipping.
When considering simple vacuum deposition apparatus, be actually used in improvement of the present invention, imagination is to change the feed mode, the coating slurries are downward by the upper end of building block, be on one side of the lower end of building block and add vacuum, with such layout, during practical operation according to method of the present invention, efficient is lower as a result though finish each coated, brings very big operational issue simultaneously, can obtain satisfied result.
For example, in following direction aspirator, it is immersed in the coating slurries with building block, has the lower surface of the building block that the tray of containers bottom surface of slurry stands away the slightly vacuum draw process that makes progress to come comparison in leaving simultaneously, needs excessive 50% coating slurries.
Change into down like this to the vacuum impregnation process, before adding vacuum,, must will cover a distributor in the upper end of member, as paper or cloth filter, breather cloth and wire netting for even dispersion paints slurries on the ceramic monolithic carrier.Place an airtight container and be close to its periphery on module component, enter container with giving earlier quantitative coating slurries through a pipe metering ground, tubaeform lid is attached under the monoblock support element on the end periphery, seals each other.Between the following and cover of this monoblock support element our said vacuum chambers, after vacuumizing, quantitative in advance coating slurries enter into the inner skeleton member by monolithic structures upper end.Measured already, the coating slurries of continuous application, its appropriate viscosity is at 20 to 50 centipoises, and vacuum can satisfy the 200SCfm air, takes out 5-15 second continuously at every turn, needs 304 gram coating slurries suctions downwards to enter the inner skeleton structure altogether.
Claims (15)
1, with the method for a kind of coating slurries to the inner skeleton structure dipping of ceramic integral member, this coating is suspended in the volatile liquid component by the solid coating material and constitutes, and the method for dipping comprises following step:
Predetermined amounts is supplied with first end face contact with the monoblock carrier structure of coating slurries, and the weight of required coating slurries can be calculated by following formula:
(matrix volume (cubic feet per inch) * do amount (gram/cubic feet per inch))/(percent solids in the slurries/100)
The matrix volume is that the interior cross-sectional area of building block multiply by height, does to such an extent that amount is the solid-state coating compound amount that remains in the inner passage behind the building block bone dry.
Settle a cover that seals mutually with member above the other end of monoblock support element, contiguous support element upper end formation one vacuum chamber is followed at this place,
On cover, vacuumize, slurries aspirated the into inner skeleton structure of member by the other end of monoblock support element, with in the member equably dipping coat slurries,
First end face of described building block is the low side of en-block construction, and the low side of this building block partly is immersed in the coating slurries in the container, and the building block low side is immersed in and is coated with in the slip, and leaving container interior bottom surface has a spacer segment.
2, by the method for claim 1, it is characterized in that, the slit of one from 0.020 to 0.125 English inch being arranged between the low side of building block and container interior bottom surface promptly at the interval,
3, by the method for claim 2, it is characterized in that the slit is about 0.040 English inch.
4, by the method for claim 1, it is characterized in that the viscosity of coating slurries is from 15 to 300 centipoises approximately.
5, by the method for claim 1, it is characterized in that this place is evacuated to rare two steps of joining, wherein second step vacuum high during of being added in building block than first step.
6, by the method for claim 5, it is characterized in that the first step vacuum in two steps is 0.5 to 0.7 English inch water column, is 3.0 to 20.0 English inch water columns in the second step vacuum.
By the method for claim 6, it is characterized in that 7, the continuous time is from 1 to 8 second when being added on first step vacuum, and from 10 to the 30 seconds approximately second step duration.
8, by the method for claim 5, it is characterized in that the coating slurries have range of viscosities from 17 to 70 centipoises approximately, the vacuum that second step is added in building block is approximately and is added in 5 on the first step to 10 times.
9, press the method for claim 1, it is characterized in that, give after first of quantitative coating slurries are sucked the lower end of monoblock support element on partly, building block is fallen turnback, then proceed vacuum draw, the residue of coating slurries is partly aspirated into original upper surface of building block.
10, by the method for claim 9, it is characterized in that the quantitative slurries that give of nearly 50% to 85% weight at first upwards are drawn into, the lower end of building block is then with 15%(weight) the coating slurries upwards be pumped into the former upper surface of reversing building block later.
By the method for claim 1, it is characterized in that 11, wherein the coating slurries of scheduled volume are with the upper surface contact of building block, the lower surface of building block is in vacuum.
12, by the method for claim 1, it is characterized in that, wherein be coated with feed liquid form in solid content be about 35% to 52%(weight).
13, by the method for claim 1, it is characterized in that, contain the aluminium oxide of high surface area values in the coating solid.
14, by the method for claim 1, it is characterized in that, contain noble metal in the coating solid, noble metal is from platinum, and palladium is selected in the gang that rhodium is formed.
By the method for claim 1, it is characterized in that 15, coating slurries solid constituent is the aluminium oxide of a high surface area values and from platinum, palladium, the mixture of the noble metal of selecting in the rhodium family.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85101134 CN1010382B (en) | 1984-04-05 | 1985-04-01 | Method of impregnating ceramic monolithic structures with predetermined amounts of catalyst |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US06/596,993 US4550034A (en) | 1984-04-05 | 1984-04-05 | Method of impregnating ceramic monolithic structures with predetermined amounts of catalyst |
| CN 85101134 CN1010382B (en) | 1984-04-05 | 1985-04-01 | Method of impregnating ceramic monolithic structures with predetermined amounts of catalyst |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85101134A CN85101134A (en) | 1987-01-17 |
| CN1010382B true CN1010382B (en) | 1990-11-14 |
Family
ID=25741353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 85101134 Expired CN1010382B (en) | 1984-04-05 | 1985-04-01 | Method of impregnating ceramic monolithic structures with predetermined amounts of catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1010382B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101271434B1 (en) * | 2011-09-29 | 2013-06-10 | 희성촉매 주식회사 | Metered weight coater for precise PM control |
| CN111644344B (en) * | 2020-05-23 | 2021-09-03 | 东南大学 | Quartz glass tube protective film coating system for high-power ultraviolet germicidal lamp |
-
1985
- 1985-04-01 CN CN 85101134 patent/CN1010382B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN85101134A (en) | 1987-01-17 |
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