CN105032456B - Surface is modified application of the cordierite in soot conversion is realized - Google Patents
Surface is modified application of the cordierite in soot conversion is realized Download PDFInfo
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- CN105032456B CN105032456B CN201510411867.0A CN201510411867A CN105032456B CN 105032456 B CN105032456 B CN 105032456B CN 201510411867 A CN201510411867 A CN 201510411867A CN 105032456 B CN105032456 B CN 105032456B
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Abstract
The invention discloses a kind of surfaces to be modified application of the cordierite in soot conversion is realized, cordierite dielectric surface is made to wrap up one layer of SiOC presoma first with sol impregnation method, then it is crosslinked using polystyrene microsphere prepared by emulsion polymerization and cordierite sample, finally composite crosslinking body is pyrolyzed, obtaining surface has the cordierite of nanometer porous structure.Technical scheme of the present invention overcomes the defects of main passive regeneration process temperature of existing particulate matter filtering body is excessively high, nano level pore space structure reduces the ignition point of carbon black, the conversion ratio of carbon black is improved, is conducive to particulate matter filtering body for being regenerated in diesel engine vent gas processing procedure.
Description
The application is application No. is 201310358768.1, and the applying date is August in 2013 15 days, entitled " a kind of
The divisional application of cordierite that surface is modified and its preparation method and application ".
Technical field
The invention belongs to be catalyzed carbon-smoke combustion technical field, more particularly, it is related to a kind of made on cordierite surface and receives
The porous preparation method and applications of meter level.
Background technology
Diesel car occupies increasing share by feat of good mobility and economy in automotive field, still
As various countries put into effect stringenter emission regulation in succession, exhaust emissions of diesel engine has become restriction diesel engine and further develops
Bottleneck factor.And particulate matter (PM) especially PM2.5 in diesel engine vent gas has human body stronger carcinogenesis.At present,
Particulate matter filtering body (DPF) is one of most effective post-processing technology for reducing diesel particulate discharge generally acknowledged at present.But
With the deposition of soot particulate, pressure drop raising leads to the reduction of engine power and fuel economy, it is necessary to which DPF is carried out
Regeneration.There are mainly two types of modes for the regeneration of DPF：One kind is initiative regeneration, i.e., dpf temperature is made to reach particulate matter by external energy
Ignition point, be deposited on filtering body dielectric surface particulate matter burning；Another kind is passive regeneration, i.e., relatively low
Under Tail Pipe Temperature, the oxidation of particulate matter is realized.Since temperature is higher during initiative regeneration, lead to DPF in regenerative process
Crackle is susceptible to, damages the performance of DPF；Therefore, passive regeneration becomes the main side of particulate matter filtering body (DPF) regeneration research
To.The ignition point for being deposited on the particulate matter of DPF dielectric surfaces is related with two factors：Macroscopic view and the microcosmic physicochemical property of particulate matter
With DPF dielectric surfaces and the exposure level of particulate matter.Therefore, as can the pattern for changing DPF dielectric surfaces is allowed to and particulate matter ruler
It is very little match reach close contact, just can significantly reduce the ignition point of particulate matter, be conducive to the passive regeneration of DPF.
Invention content
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, it is main to overcome existing particulate matter filtering body (DPF)
The defects of passive regeneration process temperature is excessively high provides a kind of preparation method for the cordierite that surface is modified.It is modified by surface
Cordierite can significantly reduce the ignition point of soot, be conducive to DPF for being regenerated in diesel engine vent gas processing procedure.
The technical purpose of the present invention is achieved by following technical proposals：
Cordierite that a kind of surface is modified and preparation method thereof, carries out as steps described below：
Step 1, the crosslinked colloidal sol that polystyrene microsphere (PS) and SiOC presomas are uniformly mixed is prepared
Weigh the hydrogen containing siloxane (PHMS) and 1 of identical mass fraction, 3,5,7- tetramethyls -1,3,5,7- tetravinyls
Cyclotetrasiloxane (D4Vi it) is mixed, then adds in methyl vinyl silicone coordination platinum catalyst thereto, then thereto
The polystyrene microsphere (PS) of 0.1-1 mass fractions is added in, is uniformly dispersed.
In above-mentioned preparation process, ultrasonic disperse mode is selected to disperse system.
In above-mentioned preparation process, the coordination platinum catalyst selects methyl vinyl silicone coordination platinum catalyst (platinum
Content：300ppm) purchased from Shenzhen platinum complex Co., Ltd, chemical formula is as follows：
Catalyst charge is 1%-the 3% of hydrogen containing siloxane and t etram-ethyltetravinylcyclotetrasiloxane gross mass,
How much main speed for influencing cross-linking reaction and carrying out of its addition.
The polystyrene microsphere (PS) selects the polystyrene microsphere often selected in method for preparing template, such as utilizes lotion
Polymerization prepares polystyrene (PS) microballoon, but needs the particle diameter distribution of polystyrene microsphere selected uniform, more single, example
Such as the PS microballoons that emulsion polymerization synthesizes, grain size 200nm, and favorable dispersibility.According to volume ratio distilled water：Absolute ethyl alcohol
=100:30 prepare ethanol water, adjust the PH of ethanol water with the NaOH solution of a concentration of 0.1-0.3mol/L, make molten
The PH of liquid>7, then the butyl titanate ethanol solution that mass fraction is 4-8% is added in above-mentioned ethanol water,
40min is stirred to react at 30-40 DEG C, obtains stable TiO 2 sol；Obtained TiO 2 sol is transferred to four mouthfuls
In flask, it is passed through protective gas nitrogen (N2), then successively into four-hole boiling flask add in dodecyl sodium sulfate (emulsifier),
Stupid ethylene, ammonium persulfate (initiator), 60-75 DEG C of constant temperature are stirred to react 8-10h, obtain polystyrene microsphere lotion.Use quality
A concentration of 5% NaOH solution is demulsified to lotion, and system is filtered, is washed, dry at 60 DEG C to obtain PS microballoons for 24 hours
Powder (photonic crystal of opals structure of Tang Rongnian, PS/TiO2 composite material prepares and characterization, electronic component and material, and 2003
Year).
Step 2, cordierite dielectric surface is made to wrap up polystyrene microsphere (PS) and SiOC presomas using sol impregnation method
Uniformly mixed crosslinked colloidal sol
When being impregnated, cordierite medium is impregnated in crosslinked colloidal sol, dip time (impregnating) is at least
30min, preferably 2-4h.
Before being impregnated, select to anticipate cordierite dielectric surface：Cordierite is cut into length：It is wide：It is high
=8-10mm：8-10mm：15-17mm is put into the mixed solution that volume ratio acetone/ethanol is 3 and impregnates 3-5h, is then placed in 60
Dry 2-3h in DEG C baking oven；Dried sample is soaked in the nitric acid (HNO of a concentration of 0.5-1mol/L3) 3-5h in solution,
Sample after immersion is put into drying for standby in drying box after being cleaned with deionized water.
After the infusion has taken place, air blast through-hole after taking-up makes the upper PS of cordierite dielectric surface attachment and SiOC presomas
Crosslinked colloidal sol is subsequently placed in constant temperature 4h at 50 DEG C, obtains the composite crosslinking body of cordierite, PS microballoons and SiOC presomas.
Step 3, the composite crosslinking body prepared in step 2 is pyrolyzed, obtaining surface has nanometer porous structure
Cordierite
It is pyrolyzed in inert environments first：It is warming up to for 20-25 DEG C from room temperature according to the heating rate of 1-2 DEG C/min
700~900 DEG C, then 1-2h of constant temperature drops to room temperature 20-25 with the cooling rate of 3~6 DEG C/min in inert gas shielding
DEG C, the composite crosslinking body after being pyrolyzed in atmosphere of inert gases is pyrolyzed, again in air according to the liter of 1-2 DEG C/min
Warm speed is warming up to 700~900 DEG C for 20-25 DEG C from room temperature, then constant temperature 1h is down to the cooling rate with 3~6 DEG C/min
20-25 DEG C of room temperature；
The inert environments selection inert gas is achieved, and is first passed through inert gas to exclude in high temperature process furnances stove
Continue to be passed through inert gas after air, such as be first passed through inert gas 4-6min, throughput is controlled in 200-400sccm, is drained
After air in stove, continue to be passed through gas；The inert gas selection argon gas, nitrogen or helium.
There is nanoscale Hierarchical porosity structure by modified cordierite dielectric surface, pore size distribution$ is more uniform,
Pore diameter range concentrates on 100-150nm, and pore structure thickness is 2-4 PS microballoon layer；Modified cordierite makes the conversion of carbon black
Rate significantly improves.The scanning electron microscope of 1-4 displays (uses Hitachi, Japan X-650 scanning electron microscopies with reference to the accompanying drawings
Mirror) photo it is found that PS microballoons be in orderly close-packed structure, show using emulsion polymerization prepare PS microballoons have shape rule
Then, size structure is uniform, and diameter range integrated distribution is in 170-200nm；Composite crosslinking body through in argon gas, air be sintered after,
The micro-sphere crosslinked parts of PS have been formed in situ pore space structure, and orderly closely packed pattern obtains PS microballoons in cordierite dielectric surface
The duplication of height.PS microballoons and hole diameter in attached drawing are compared, it is found that the hole diameter after the completion of sintering is slightly less than PS microballoons, this
It is since the frame of empty structure is SiOC, a degree of contraction can occurs during SiOC is sintered by SiOC presomas
It is caused.
By doing EDX energy spectrum analysis to the cordierite dielectric surface after the completion of sintering, show modified dielectric surface
Elemental composition is for Si, O, C and also containing a small amount of La, the atomic ratio shared by them：[Si]=24.4%, [O]=
58.84%, [C]=15.27%；Therefore dielectric surface ingredient is after the completion of can tentatively judging sintering：Si1.6O3.85C。
The cordierite (embodiment 1,4 and 5) of surface texture modification has been investigated to carbon black particle using thermogravimetry (TGA)
Catalytic oxidation performance.To simplify experimentation, using the carbon black diesel oil substitute of German goldschmidt chemical corporation (DegussaAG)
Dry carbon cigarette in machine discharge carbon soot particles, the two main component is identical, and crystal grain is similar with specific surface area.Laboratory apparatus is the U.S.
Perkin-Elmer companies Pyris Diamond thermal analyzers, it is 30-800 DEG C to measure temperature range, air atmosphere, gas stream
Fast 20.0ml/min, 10 DEG C/min of heating rate.By thermogravimetric curve be converted into soot conversion ratio can obtain one it is smooth continuous
Different temperatures under to the curve of soot conversion ratio, from attached drawing 5 it is found that the cordierite that is modified for ordered porous structural of surface is (real
Apply example 5) unmodified cordierite is substantially better than at the very start to the conversion ratio of carbon black, (the initiation temperature of pure carbon black at 500 DEG C
Ti), surface reaches 75% for the cordierite that ordered porous structural is modified to the conversion ratio of carbon black, without by any modification
Cordierite only has 30% to the conversion ratio of carbon black, this shows that nano level pore space structure reduces the ignition point of carbon black, improves
The conversion ratio of carbon black.Embodiment 4 fails to show to be substantially better than embodiment 1 to the conversion ratio of carbon black in attached drawing 5, this is because real
The pore space structure applied in example 4 is unevenly distributed, and is not multilayered structure, fails to show to charcoal under the action of systematic error
The raising of black conversion ratio.It can be seen that the surface that technical solution obtains according to the present invention, which is modified cordierite, is realizing soot conversion
Middle to realize application, the temperature for realizing soot conversion is 30-800 DEG C, preferably 300-800 DEG C.
Description of the drawings
Fig. 1 is the SEM figures of the polystyrene microsphere of orderly accumulation.
Fig. 2 is that surface unmodified cordierite inner surface SEM schemes.
Fig. 3 is that the modified cordierite inner surface SEM in surface schemes (1).
Fig. 4 is that the modified cordierite inner surface SEM in surface schemes (2).
Fig. 5 is conversion ratio activity curve of the cordierite sample to carbon black.
Specific embodiment
The technical solution further illustrated the present invention with reference to specific embodiment, wherein containing hydrogen silicone oil (PHMS, analysis
It is pure) purchased from Jilin Huafeng Organic Silicon Co., Ltd.；1,3,5,7-tetramethyl 1,3,5,7-tetravinyl cyclotetrasiloxane
(D4Vi, analysis are pure) purchased from thousand rainbow Industrial Co., Ltd.s of Zhejiang San Men；Methyl vinyl silicone coordination platinum catalyst (Pt%=
3000ppm) purchased from Shenzhen platinum complex Co., Ltd.
Embodiment 1
Cordierite is cut into length：It is wide：Height=10mm：10mm：5mm, in mixed solution of the acetone/ethanol volume ratio for 3
After impregnating 4h, the dry 4h at 60 DEG C；Then dried cordierite is placed in the HNO of a concentration of 1mol/L3It is impregnated in solution
4h, after being rinsed repeatedly with distilled water, dry 12h is spare at 100 DEG C.It is 1 according to mass ratio：1 weighs hydrogen containing siloxane
(PHMS) and 1,3,5,7-tetramethyl 1,3,5,7-tetravinyl cyclotetrasiloxane (D4Vi) each 1g is mixed in beaker, excusing from death
10min is vibrated, is sufficiently mixed the two, instills the methyl vinyl silicone coordination platinum of an a concentration of 3000ppm of drop thereto
Continue excusing from death vibration 10min after catalyst, obtain SiOC precursor solutions.The cordierite of above-mentioned pretreatment is put into SiOC solution
Air blast through-hole after middle immersion 30min, makes cordierite dielectric surface adhere to last layer SiOC precursor solutions, is then done at 60 DEG C
Dry 4-6h prepares the sample in cordierite dielectric surface package SiOC presomas.
Above-mentioned cordierite sample is to be pyrolyzed under the argon gas flowed, is first passed through 5min argon gas to drain furnace air, gas
Flow is 300sccm, continues to be passed through argon gas, and 440 DEG C of constant temperature 1h are risen to first, in accordance with the heating rate of 1 DEG C/min, then with 1 DEG C/
The heating rate of min rises to 800 DEG C, and constant temperature 1h cools to room temperature with the furnace；Then by the crosslinked being pyrolyzed in argon gas in air
Pyrolysis rises to 800 DEG C from room temperature according to the heating rate of 1 DEG C/min, after constant temperature 1h, cools to room temperature with the furnace, prepare surface
Wrap up the cordierite sample of one layer of SiOC：SiOC@cordierites.
Embodiment 2
Cordierite is cut into length：It is wide：Height=10mm：10mm：5mm, in mixed solution of the acetone/ethanol volume ratio for 3
After impregnating 4h, the dry 4h at 60 DEG C；Then dried cordierite is placed in the HNO of a concentration of 1mol/L3It is impregnated in solution
4h, after being rinsed repeatedly with distilled water, dry 12h is spare at 100 DEG C.It is 1 according to mass ratio：1 weighs hydrogen containing siloxane
(PHMS) and 1,3,5,7-tetramethyl 1,3,5,7-tetravinyl cyclotetrasiloxane (D4Vi it) is mixed in beaker, excusing from death vibration
10min is sufficiently mixed the two, continues excusing from death after one drop methyl vinyl silicone coordination platinum catalyst of instillation thereto and vibrates
10min obtains SiOC precursor solutions.The cordierite of above-mentioned pretreatment is put into air blast after impregnating 30min in SiOC solution to lead to
Hole makes cordierite dielectric surface adhere to last layer SiOC precursor solutions, and then the dry 4-6h at 60 DEG C, is prepared in violet blueness
Stone dielectric surface wraps up the sample of SiOC presomas.
100ml distilled water and 30ml absolute ethyl alcohols are taken in 250ml beakers, with a concentration of after room temperature magnetic agitation 10min
The NaOH solution of 0.1mol/L adjusts the PH ≈ 9 of ethanol water, and obtained ethanol water is transferred to 250ml four-hole boiling flasks
In；The butyl titanate ethanol solution that 10ml mass fractions are 4% is added in into four-hole boiling flask, is stirred to react at 40 DEG C
40min obtains stable titania gel；0.2g dodecyl sodium sulfates (emulsifier) are added in into four-hole boiling flask successively,
It is passed through protective gas N2, 5ml styrene and 0.2g ammonium persulfates (initiator) are added in, then the isothermal reaction 8h at 75 DEG C,
Obtain polystyrene microsphere (PS) lotion of the uniform monodispersity of size structure.It is demulsified with a concentration of 5% NaOH solution, to body
System is filtered, washs, 60 DEG C of dryings are spare for 24 hours.
Weigh hydrogen containing siloxane (PHMS) and 1,3,5,7- tetramethyls -1,3,5,7- tetravinyl cyclotetrasiloxanes
(D4Vi) in 8ml beakers, excusing from death vibration 10min is sufficiently mixed the two, a concentration of 3000ppm is instilled into beaker each 1g
Methyl vinyl silicone coordination platinum catalyst one drip, continue ultrasonic vibration 10min, obtain SiOC precursor solutions；Forward
Polystyrene microsphere (PS) the ultrasonic disperse 2h afterwards that 0.1g is added in liquid solution is driven, obtains the PS suspension of polymolecularity.It will be upper
It states the cordierite sample by pretreatment to be transferred in PS suspension, after impregnating 4h, air blast through-hole after taking-up is subsequently placed in 50 DEG C
Lower constant temperature 4h, obtains composite crosslinking body.
Complex crosslinked under the argon gas of flowing is pyrolyzed, is first passed through 5min argon gas to drain furnace air, throughput
For 300sccm, continue to be passed through argon gas, 440 DEG C of constant temperature 1h are risen to, then with 1 DEG C/min's first, in accordance with the heating rate of 1 DEG C/min
Heating rate rises to 800 DEG C, and constant temperature 1h cools to room temperature with the furnace；Then it is the crosslinked being pyrolyzed in argon gas is warm in air
Solution rises to 800 DEG C from room temperature according to the heating rate of 1 DEG C/min, after constant temperature 1h, cools to room temperature with the furnace, obtains inner surface tool
There is the cordierite of nano micropore structure.
Embodiment 3
Preparation, the SiOC forerunner of the pre-treatment of cordierite, surface SiOC presomas package and PS microballoons in the present embodiment
The preparation of liquid solution with embodiment 2, unlike：The ultrasonic disperse after the PS microballoons of addition 0.4g into SiOC precursor solutions
2h obtains the PS suspension of polymolecularity.The above-mentioned cordierite sample by pretreatment is transferred in PS suspension, impregnates 4h
Afterwards, air blast through-hole after taking-up is subsequently placed in constant temperature 4h at 50 DEG C, obtains composite crosslinking body.
Complex crosslinked first under the argon gas of flowing is pyrolyzed, passes first into 5min argon gas to drain furnace air, gas
Flow is 300sccm, continues to be passed through argon gas, and 440 DEG C of constant temperature 1h are risen to first, in accordance with the heating rate of 1 DEG C/min, then with 1 DEG C/
The heating rate of min rises to 800 DEG C, and constant temperature 1h cools to room temperature with the furnace；Then by the crosslinked being pyrolyzed in argon gas in air
The crosslinked of pyrolysis is placed in Muffle furnace by middle pyrolysis, rises to 800 DEG C from room temperature according to the heating rate of 1 DEG C/min, constant temperature 1h
Afterwards, room temperature is cooled to the furnace, obtaining inner surface has the cordierite of nano micropore structure.
Embodiment 4
Preparation, the SiOC presomas at the preceding place of cordierite, surface SiOC presomas package and PS microballoons in the present embodiment
The preparation of solution with embodiment 2, unlike：The ultrasonic disperse 2h after the PS microballoons of addition 0.8g into SiOC precursor solutions,
Obtain the PS suspension of polymolecularity.The above-mentioned cordierite sample by pretreatment is transferred in PS suspension, after impregnating 4h,
Air blast through-hole after taking-up is subsequently placed in constant temperature 4h at 50 DEG C, obtains composite crosslinking body.
Complex crosslinked first under the argon gas of flowing is pyrolyzed, passes first into 5min argon gas to drain furnace air, gas
Flow is 300sccm, continues to be passed through argon gas, and 440 DEG C of constant temperature 1h are risen to first, in accordance with the heating rate of 1 DEG C/min, then with 1 DEG C/
The heating rate of min rises to 800 DEG C, and constant temperature 1h cools to room temperature with the furnace；Then by the crosslinked being pyrolyzed in argon gas in air
The crosslinked of pyrolysis is placed in Muffle furnace by middle pyrolysis, rises to 800 DEG C from room temperature according to the heating rate of 1 DEG C/min, constant temperature 1h
Afterwards, room temperature is cooled to the furnace, obtaining inner surface has the cordierite of nano micropore structure.
Embodiment 5
The preparation of the pre-treatment of cordierite, surface SiOC presomas package and PS microballoon lotions is the same as implementation in the present embodiment
Example 2, unlike：It is not demulsified to PS microballoon lotions, but SiOC presomas will be wrapped up by pre-treatment and surface
Cordierite sample and 100ml polystyrene microspheres (PS) lotion liquid are transferred in centrifuge tube, rotating speed under 4000r/min from
The heart for 24 hours, obtains the complex of polystyrene microsphere (PS) and cordierite, and by obtained complex, dry 72h is spare at 60 DEG C.
Weigh methyl hydrogen polysiloxanes (PHMS) and 1,3,5,7- tetramethyls -1,3,5,7- tetravinyl cyclotetrasiloxanes
(D4Vi) in 8ml beakers, excusing from death vibration 10min is sufficiently mixed the two, a concentration of 3000ppm is instilled into beaker each 2g
Methyl vinyl silicone coordination platinum catalyst one drip, continue ultrasonic vibration 10min, obtain SiOC precursor solutions；It will be dry
Complex after dry is placed in SiOC precursor solutions, filters 2h repeatedly through vacuum pump at room temperature, is emptied in PS microballoons gap
Air, sample is then placed in constant temperature 4h at 50 DEG C, obtains the crosslinked of complex.
The crosslinked of complex under the argon gas of flowing is pyrolyzed, is first passed through 5min argon gas to drain furnace air, air-flow
It measures as 300sccm, continues to be passed through argon gas, 440 DEG C of constant temperature 1h are risen to, then with 1 DEG C/min first, in accordance with the heating rate of 1 DEG C/min
Heating rate rise to 800 DEG C, constant temperature 1h cools to room temperature with the furnace；Then by the crosslinked being pyrolyzed in argon gas in air
Pyrolysis, the crosslinked of pyrolysis is placed in Muffle furnace, rises to 800 DEG C from room temperature according to the heating rate of 1 DEG C/min, constant temperature 1h
Afterwards, it cools to room temperature with the furnace, after through-hole processing is carried out to the sample after the completion of sintering, obtains inner surface with nano ordered
The cordierite of more hollow structures.
Illustrative description has been done to the present invention above, it should explanation, in the situation for the core for not departing from the present invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (1)
1. surface is modified application of the cordierite in soot conversion is realized, which is characterized in that passes through modified cordierite medium
Ingredient is Si1.6O3.85C, surface have nanoscale Hierarchical porosity structure, and pore size distribution$ is more uniform, and pore diameter range concentrates on
100-150nm, surface are modified cordierite and carry out as steps described below：
Cordierite is cut into length：It is wide：Height=10mm：10mm：5mm impregnates in mixed solution of the acetone/ethanol volume ratio for 3
After 4h, the dry 4h at 60 DEG C；Then dried cordierite is placed in the HNO of a concentration of 1mol/L34h is impregnated in solution, is used
After distilled water rinses repeatedly, dry 12h is spare at 100 DEG C, is 1 according to mass ratio：1 weigh hydrogen containing siloxane (PHMS) and
1,3,5,7-tetramethyl 1,3,5,7-tetravinyl cyclotetrasiloxane (D4Vi it) is mixed in beaker, ultrasonic vibration 10min makes
The two is sufficiently mixed, and continues ultrasonic vibration 10min after instilling a drop methyl vinyl silicone coordination platinum catalyst thereto,
SiOC precursor solutions are obtained, the cordierite of above-mentioned pretreatment is put into SiOC solution air blast through-hole after immersion 30min, makes violet
Green stone dielectric surface adheres to last layer SiOC precursor solutions, and then the dry 4-6h at 60 DEG C, is prepared in cordierite medium
Wrap up the sample of SiOC presomas in surface；
100ml distilled water and 30ml absolute ethyl alcohols are taken in 250ml beakers, with a concentration of after room temperature magnetic agitation 10min
The NaOH solution of 0.1mol/L adjusts the p H ≈ 9 of ethanol water, and obtained ethanol water is transferred to tetra- mouthfuls of burnings of 250ml
In bottle；The butyl titanate ethanol solution that 10ml mass fractions are 4% is added in into four-hole boiling flask, is stirred to react at 40 DEG C
40min obtains stable titania gel；0.2g dodecyl sodium sulfates are added in into four-hole boiling flask successively, are passed through protection
Property gas N2, 5ml styrene and 0.2g ammonium persulfates are added in, then the isothermal reaction 8h at 75 DEG C, it is uniform to obtain size structure
The polystyrene microsphere lotion of monodispersity；
It will be by pre-treatment and the cordierite sample of surface package SiOC presomas and the transfer of 100ml polystyrene microsphere lotions liquid
Into centrifuge tube, the complex for for 24 hours, obtaining polystyrene microsphere and cordierite is centrifuged in the case where rotating speed is 4000r/min, will
The complex arrived dry 72h at 60 DEG C is spare；
Weigh methyl hydrogen polysiloxanes (PHMS) and 1,3,5,7- tetramethyls -1,3,5,7- tetravinyl cyclotetrasiloxanes
(D4Vi) each 2g is in 8ml beakers, ultrasonic vibration 10min, is sufficiently mixed the two, a concentration of 3000ppm is instilled into beaker
Methyl vinyl silicone coordination platinum catalyst one drip, continue ultrasonic vibration 10min, obtain SiOC precursor solutions；It will be dry
Complex after dry is placed in SiOC precursor solutions, filters 2h repeatedly through vacuum pump at room temperature, is emptied in PS microballoons gap
Air, sample is then placed in constant temperature 4h at 50 DEG C, obtains the crosslinked of complex；
The crosslinked of complex under the argon gas of flowing is pyrolyzed, is first passed through 5min argon gas to drain furnace air, throughput is
300sccm continues to be passed through argon gas, and 440 DEG C of constant temperature 1h, then the liter with 1 DEG C/min are risen to first, in accordance with the heating rate of 1 DEG C/min
Warm rate rises to 800 DEG C, and constant temperature 1h cools to room temperature with the furnace；Then the crosslinked being pyrolyzed in argon gas is pyrolyzed in air,
The crosslinked of pyrolysis is placed in Muffle furnace, 800 DEG C are risen to from room temperature according to the heating rate of 1 DEG C/min, after constant temperature 1h, with stove
It is cooled to room temperature, after through-hole processing is carried out to the sample after the completion of sintering, obtains inner surface with nano ordered porous knot
The cordierite of structure.
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| CN111485976A (en) * | 2019-01-28 | 2020-08-04 | 华中师范大学 | Diesel particulate trap loaded with macroporous perovskite oxide and application thereof |
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| CN105032458B (en) | 2017-06-06 |
| CN103433063B (en) | 2016-08-17 |
| CN105032458A (en) | 2015-11-11 |
| CN105032456A (en) | 2015-11-11 |
| CN103433063A (en) | 2013-12-11 |
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