CN102441379A - Catalytic combustion catalyst and preparing method thereof - Google Patents
Catalytic combustion catalyst and preparing method thereof Download PDFInfo
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- CN102441379A CN102441379A CN2010105109996A CN201010510999A CN102441379A CN 102441379 A CN102441379 A CN 102441379A CN 2010105109996 A CN2010105109996 A CN 2010105109996A CN 201010510999 A CN201010510999 A CN 201010510999A CN 102441379 A CN102441379 A CN 102441379A
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Abstract
The invention discloses a catalytic combustion catalyst and a preparing method thereof. Such catalytic combustion catalyst takes honeycomb ceramics as the carrier, and the surface of the honeycomb ceramics is respectively provided with a SiO2 coating and a CeO2 coating. Counted by the total weight of the coatings, the coatings contain 80wt%-95wt% of activated SiO2 and 5wt%-20wt% of CeO2. The surface of the coatings is loaded with activated components of metallic elements including Pt, Zr and La, in which the molar ratio of the metallic elements Pt, Zr and La is 0.1-1:1, 5-4.5:1.5-4. The carrying amount of activated component of precious metal Pt is 0.2-3.5g for each litre of catalyst. A method for preparing catalytic combustion catalyst, comprising the steps of preprocessing the carrier, preparing the sol, coating the carrier sol and loading the metal activated components. The catalytic combustion catalyst provided by the invention has very high coating firmness and high-temperature activity as well as stability in the process of catalyzing and combusting the organic waste gas; moreover, such catalytic combustion catalyst has good treatment effect for the waste gas with different high temperature and high air speed.
Description
Technical field
The present invention relates to a kind of catalyst for catalytic combustion and preparation method thereof, specifically relate to catalyst for catalytic combustion of a kind of high-activity stable property and preparation method thereof.
Background technology
Volatile organic matter (VOCs) results from petroleum refining industry and electronics, printing, coating, paint process industry.The organic exhaust gas of a large amount of dischargings is contaminated environment not only, also the serious harm human beings'health.The Along with people's growth in the living standard, also increasingly high to the requirement of living environment, effective processing of this kind gas has caused people's extensive concern.In the technology of handling VOCs, Production by Catalytic Combustion Process has efficiently, the characteristics of low temperature, obtains more and more general application.In order to guarantee the circulation of waste gas, reduce droop loss, catalytic combustion mostly adopts the resistant to elevated temperatures loaded catalyst of porous, and this catalyst generally passes through at the porous carrier face coat, the method for load active component preparation then.
CN88100589 discloses a kind of catalyst that is used for purifying exhaust air; Comprise the honeycomb support of en-block construction and be deposited on the coating on the honeycomb support; This coating is to form with a kind of carbon monoxide-olefin polymeric that contains with the refractory inorganic oxide of average particulate diameter in 0.5 to 20 micrometer range, on refractory inorganic oxide, has platinum and/or palladium and rhodium with the high concentration deposition.This kind catalyst is to apply honeycomb support through the moisture thin pulp that employing contains carbon monoxide-olefin polymeric to produce with the carrier that calcining applies.Patent CN1415410A discloses a kind of catalyst for catalytic combustion and preparation method thereof.Solved in the prior art noble metal component utilization rate of catalyst for catalytic combustion low, disperse uneven problem.It is active component that this catalyst adopts precious metals pt, and the mode through the organic acid competitive Adsorption is distributed in the honeycomb ceramic carrier surface, and wherein the noble metal loading is every liter of 0.5～4gPt, carrier coating consist of active A l
2O
320%～80%, TiO
210%～40%, CeO
25%～30%, ZrO
25%～20%.CN1488435 discloses a kind of catalyst for catalytic combustion that organic waste-gas purification is handled that is used for, and is made up of honeycomb ceramic carrier skeleton and the coating and the noble metal active component that apply on it of bulk.The coating of catalyst is by Al
2O
3, SiO
2Form with the common composite oxides that form of one or more alkaline earth oxides.
Above-described organic waste gas catalytic combustion catalyst mostly adopts the method preparation of honeycomb substrate, slurry coating and noble metal dipping; Noble metal has active high advantage as the catalyst for catalytic combustion of active component; Common organic exhaust gas is had very high clearance, and still, there is poor stability in above-mentioned catalyst; When handling the organic exhaust gas of high temperature high-speed activity low, be prone to inactivation and to the shortcoming and defect such as bad adaptability of different organic exhaust gas; The catalyst for catalytic combustion that particularly adopts the mode of slurry coating to prepare can't adapt to the acute variation of tolerance and because the exhaust gas concentration fluctuation causes the temperature acute variation, and at this moment, catalyst coat can be owing to agingly occur coming off; Thereby influence the effect of catalyst, and then reduce even forfeiture organic waste gas catalytic combustion disposal ability.Therefore, develop and combine the extensive catalyst for catalytic combustion of firm high-activity stable property and adaptability significant.
Summary of the invention
Deficiency to prior art; The present invention provides a kind of catalyst for catalytic combustion and preparation method thereof, and this catalyst has very high coating firmness and with high temperature active stability and to different high temperature high-speed waste gas the good treatment effect arranged all in handling the Catalytic Combustion of Organic Exhaust Gases process.
Catalyst for catalytic combustion of the present invention is a carrier with the ceramic honey comb, and the honeycomb ceramic carrier surface has SiO successively
2Coating and CeO
2Coating by the gross weight of coating, contains weight percentage and is 80%～95% active SiO in the coating
2, 5%～20% CeO
2, in the coating surface load Pt, Zr, La metallic element active component being arranged, Pt, Zr, La metallic element mol ratio are 0.1～1: 1.5～4.5: 1.5～4, the loading of precious metals pt active component is every liter of catalyst 0.2～3.5g.
Generally to select cordierite for use be that raw material is processed to honeycomb ceramic carrier among the present invention; SiO
2Coating is introduced by Ludox, CeO
2Coating is introduced by cerium colloidal sol.
The preparation method of a kind of catalyst for catalytic combustion of the present invention comprises process for preparation, carrier collosol coating process, the metal active constituent loading process of carrier preprocessing process, Ludox and cerium colloidal sol.
It is to soak 1～6 hour in 0.5%～2% the watery hydrochloric acid that described honeycomb ceramic carrier preprocessing process at first is positioned over mass concentration with honeycomb substrate; Place the ultrasonic cleaning machine to clean 0.5～4 hour in carrier and liquid, take out the back and dried by the fire 0.5～6 hour down at 60 ℃～150 ℃; Carrier after oven dry roasting again obtained the carrier of clean dry in 5 hours.
Described Ludox and cerium colloidal sol layoutprocedure, wherein Ludox is non-sodium cation Ludox, preferred ammonia cationic colloidal silica, SiO in the Ludox
2Weight percentage is 15～35%, and the Ludox average grain diameter is 10～200nm; The compound method of cerium colloidal sol is various; Preferably be solvent with distilled water, add cerous nitrate and citric acid, making cerous nitrate solution concentration is 0.1～0.3mol/L; The pH value is 2～6; Stirred 4～16 hours down at 50 ℃～90 ℃, regulating the pH value through slow adding ammoniacal liquor is 7～9, and it is subsequent use to process stable cerium colloidal sol.
Described carrier coating process places Ludox to take out after 5～60 minutes in pretreated carrier, blows the liquid in the most space with compressed air, dries 3～16 hours down at 60 ℃～160 ℃, and roasting is 3～16 hours under air ambient, promptly makes to have SiO
2The honeycomb type ceramic monolith of coating; Then, place cerium colloidal sol to take out after 5～60 minutes in above-mentioned carrier, blow the liquid in the most space with compressed air, dried 3～16 hours down at 60 ℃～160 ℃, roasting obtained having CeO in 3～16 hours under air ambient
2Honeycomb ceramic carrier,
It is the nitrate solution of 0.5～2% Pt, Zr and La that the carrier of described active constituent loading process after with coating places metallic element quality percentage composition; Pt, Zr, La metallic element mol ratio are 0.1～1: 1.5～4.5 in the solution: 1.5～4; Stop after 3～60 minutes and take out; Dried 3～16 hours down at 60 ℃～160 ℃, roasting is 3～16 hours under air ambient, makes catalyst for catalytic combustion.
Compared with prior art, the present invention has following advantage:
1, the carrier surface of catalyst for catalytic combustion of the present invention has SiO successively
2Coating and CeO
2Coating; Coating surface carried noble metal and base metal active component; Promote the interaction between the metal active constituent, improved the interaction of catalyst activity component and coating and the active force on coating and honeycomb type ceramic monolith surface, effectively prevented coating shedding and loss of active component; Improve activity of such catalysts stability, advantages such as that the catalyst for catalytic combustion that makes has is high temperature resistant, anti-high-speed.
2, carrier coating adopts the mode of Ludox and cerium colloidal sol to introduce among the preparation method of catalyst for catalytic combustion of the present invention; Adopt colloidal sol that carrier is carried out coating; Colloidal particle can be securely attached to carrier surface; Combine between colloidal particle closely and coating is evenly distributed, improved the fastness and the coating specific area of carrier coating.
3, preferred colloidal particle is the ammonia cationic colloidal silica of 10-200nm in the inventive method, avoids the detrimental effect of Na ion pair reaction in the catalytic process, and the catalyst of preparation has that cohesive force is strong, high temperature resistant, the characteristics of high-specific surface area.
4, catalyst for catalytic combustion of the present invention is strong to VOCs treatment of waste gas adaptability, can efficiently handle the VOCs waste gas of multiple complicacy, and preparation method and equipment are simple, easy operating and suitability for industrialized production.
The specific embodiment
Further specify effect of the present invention and effect below in conjunction with embodiment, but said embodiment should not be construed as the restriction of the scope of the invention.
Embodiment 1
With specification is that to put into mass concentration be that 1% watery hydrochloric acid soaks 2h for the honeycomb ceramic carrier of 100mm * 100mm * 50mm; With carrier and diluted acid liquid after cleaning 2h under the microwave; Dry up after the taking-up; And placing 100 ℃ baking oven 6 hours, the honeycomb type ceramic monolith that the carrier roasting of gained was obtained clean dry in 5 hours is subsequent use.
Is the cerous nitrate solution of 0.3mol/L with distilled water for the solvent configuration concentration, and adding an amount of citric acid, to make the pH of solution be 4, stirred 6 hours down at 70 ℃, uses ammoniacal liquor to regulate the pH value 7.9, and it is subsequent use to process stable cerium colloidal sol.
Choosing average grain diameter is 10～200nm, SiO
2Content is 25% ammonia cationic colloidal silica, pretreated carrier is put into Ludox take out after 30 minutes, blows the slurries in the most duct with compressed air, dries 6 hours down at 160 ℃, and roasting is 5 hours under air ambient, applies CeO with same method again
2Colloidal sol obtains having uniform SiO
2And CeO
2The carrier of coating is subsequent use.
With distilled water is solvent, adds Pt (NO at 1: 4: 4 by metal element mol ratio
3)
4Powder, Zr (NO
3)
4Powder, La (NO
3)
3.6H
2The O crystalline particle; Preparing metal element quality percentage composition is 1.2% composite reactive component nitrate solution; The carrier that has applied coating is put into this solution dipping to be taken out after 10 minutes; Place 160 ℃ baking oven 6 hours, catalyst for catalytic combustion was promptly processed in roasting in 5 hours again, and wherein the loading of Pt is every liter of catalyst 1.0g.
Embodiment 2
With specification is that to put into mass concentration be that 2% watery hydrochloric acid soaks 2h for the honeycomb ceramic carrier of 100mm * 100mm * 50mm; With carrier and diluted acid liquid after cleaning 2h under the microwave; Dry up after the taking-up; And placing 110 ℃ baking oven 4 hours, the honeycomb type ceramic monolith that the carrier roasting of gained was obtained clean dry in 5 hours is subsequent use.
Is the cerous nitrate solution of 0.15mol/L with distilled water for the solvent configuration concentration, and adding an amount of citric acid, to make the pH of solution be 5, stirred 4 hours down at 90 ℃, uses ammoniacal liquor to regulate pH value 8.5, and the formation stable sols is subsequent use.
Choosing average grain diameter is 10～200nm, SiO
2Content is 30% decationizing Ludox, pretreated carrier is put into Ludox take out after 15 minutes, blows the slurries in the most duct with compressed air, dries 4 hours down at 110 ℃, and roasting is 5 hours under air ambient, applies CeO with same method again
2Colloidal sol obtains having uniform SiO
2And CeO
2The carrier of coating is subsequent use.
With distilled water is solvent, presses metal element mol ratio and adds Pt (NO at 1: 4: 3
3)
4Powder, Zr (NO
3)
4Powder, La (NO
3)
3.6H
2The O crystalline particle; Preparing metal element quality percentage composition is 1.8% composite reactive component nitrate solution; The carrier that has applied coating is put into this solution dipping to be taken out after 30 minutes; Place 110 ℃ baking oven 6 hours, catalyst for catalytic combustion was promptly processed in roasting in 5 hours again, and wherein the loading of Pt is every liter of catalyst 1.2g.
Embodiment 3
With specification is that to put into mass concentration be that 1% watery hydrochloric acid soaks 6h for the honeycomb ceramic carrier of 100mm * 100mm * 50mm; With carrier and diluted acid liquid after cleaning 4h under the microwave; Dry up after the taking-up; And placing 70 ℃ baking oven 6 hours, the honeycomb type ceramic monolith that the carrier roasting of gained was obtained clean dry in 5 hours is subsequent use.
Is the cerous nitrate solution of 0.1mol/L with distilled water for the solvent configuration concentration, and adding an amount of citric acid, to make the pH of solution be 5, stirred 12 hours down at 110 ℃, uses ammoniacal liquor to regulate pH value 7.5, and the formation stable sols is subsequent use.
Choosing average grain diameter is 10～200nm, SiO
2Content is 20% sodium cation Ludox, pretreated carrier is put into Ludox take out after 40 minutes, blows the slurries in the most duct with compressed air, dries 4 hours down at 70 ℃, and roasting is 5 hours under air ambient, applies CeO with same method again
2Colloidal sol obtains having uniform SiO
2And CeO
2The carrier of coating is subsequent use.
With distilled water is solvent, 1: 2: 4 in molar ratio adding Pt (NO
3)
4Powder, Zr (NO
3)
4Powder, La (NO
3)
3.6H
2The O crystalline particle; Preparing metal element quality percentage composition is 0.8% composite reactive component nitrate solution; The carrier that has applied coating is put into this solution dipping to be taken out after 30 minutes; Place 70 ℃ baking oven 6 hours, catalyst for catalytic combustion was promptly processed in roasting in 5 hours again, and wherein the loading of Pt is every liter of catalyst 0.8g.
Comparative example
By the method for patent CN1488435, measuring 100mL concentration is 50gAl
2O
3Al (the NO of/100mL solution
3)
3The aqueous solution, the weak aqua ammonia that under agitation slowly adds 20% (V/V) are to pH=7.0, and adding 2mL concentration is 50gAl
2O
3Al (the NO of/100mL solution
3)
3The aqueous solution continued to stir after 10 minutes, and adding 133mL concentration is 30gSiO
2The Ludox of/100mL solution, adding 100mL concentration again is the Mg (NO of 10gMgO/100mL solution
3)
2The aqueous solution, adding water purification to moisture thin pulp cumulative volume is 1000mL, is stirred to evenly, with the coating liquid of this moisture thin pulp as honeycomb ceramic carrier coating.
The honeycomb ceramic carrier that will be of a size of 72 * 72 * 50mm is immersed in the above-mentioned moisture thin pulp; Submergence was taken out after 10 minutes, removed the residual slurries in the hole with compressed air, and then 60 ℃ of dryings 15 hours in the air; 550 ℃ of roastings are 2 hours in the air, promptly get the honeycomb ceramic carrier with coating.
Compound concentration is the H of 0.4Pt/100mL solution
2PtCl
6Aqueous solution 1000mL floods night as the noble metal active component; To apply cated honeycomb ceramic carrier and in this maceration extract, flood taking-up after 20 minutes; Blow away raffinate in the hole with compressed air, and then 120 ℃ of dryings 10 hours in the air, 500 ℃ of roastings are 5 hours in the air; Promptly get catalyst for catalytic combustion, wherein the loading of active component Pt is every liter of catalyst 1.2g.。
In order to estimate the treatment effect of each catalyst to the sulfur-bearing organic exhaust gas, respectively with the VOCs of sewage treatment plant waste gas and oil refinery dry gas to the catalyst evaluation that experimentizes:
Estimate as process object with certain sewage treatment plant's VOCs waste gas, the total hydrocarbon concentration of this waste gas is 4000mg/m
3, contain H
2About 5～the 15ppm of S, reaction velocity are 30000h
-1, 300 ℃ of bed inlet temperatures.The 24h evaluation result is seen table 1.
With oil refinery dry gas (CH
4, ethane, ethene, propane, propylene, H
2Deng) estimate for process object, the waste gas total hydrocarbon concentration is 2200mg/m
3, reaction velocity is 20000h
-1, H
2The volume fraction of S is 0.1%, 450 ℃ of bed inlet temperatures.The 24h evaluation result is seen table 2.
Can find out that by table 1 and table 2 catalyst has active preferably and higher organic removal rate.
The long running of the catalyst of embodiment 2 mades is estimated situation (VOCs of sewage treatment plant waste gas is process object), and clearance remains on more than 97% always.20 little hourly space velocities in running later stage are by 20000h
-1Bring up to 50000h
-1, running finishes back microscopically comparative catalyst surface abrasion situation, and nothing significantly chaps and comes off, and the made catalyst of Comparative Examples can be observed be full of cracks and obscission at microscopically.。
This shows that catalyst of the present invention has the good treatment effect to VOCs waste gas, and guaranteed activity stability and the fastness of coating under the hot conditions.
Table 1 catalyst is to the purified treatment effect of the VOCs of sewage treatment plant waste gas
Table 2 catalyst is to the purified treatment effect of oil refinery dry gas
The experimental evaluation of table 3 catalyst long running
| The duration of runs/hour | Inlet total hydrocarbon mg/m 3 | Outlet total hydrocarbon mg/m 3 | Clearance % |
| 24 | 4110 | 22.7 | 99.4 |
| 96 | 4222 | 36.2 | 99.1 |
| 168 | 4100 | 30.8 | 99.2 |
| 240 | 4100 | 41.2 | 99.0 |
| 272 | 4014 | 44.2 | 98.9 |
| 340 | 4128 | 80.5 | 98.0 |
| 350 | 4080 | 88.2 | 97.8 |
| 360 | 4008 | 86.5 | 97.8 |
Claims (9)
1. a catalyst for catalytic combustion is a carrier with the ceramic honey comb, and the honeycomb ceramic carrier surface has SiO successively
2Coating and CeO
2Coating by the gross weight of coating, contains weight percentage and is 80%～95% active SiO in the coating
2, 5%～20% CeO
2, in the coating surface load Pt, Zr, La metallic element active component being arranged, Pt, Zr, La metallic element mol ratio are 0.1～1: 1.5～4.5: 1.5～4, the loading of precious metals pt active component is every liter of catalyst 0.2～3.5g.
2. catalyst according to claim 1 is characterized in that SiO
2Coating is introduced by Ludox, CeO
2Coating is introduced by cerium colloidal sol.
3. the preparation method of the described catalyst for catalytic combustion of claim 1 comprises process for preparation, carrier collosol coating process, the metal active constituent loading process of carrier preprocessing process, Ludox and cerium colloidal sol.
4. method according to claim 3; It is characterized in that it is to soak 1～6 hour in 0.5%～2% the watery hydrochloric acid that the honeycomb ceramic carrier preprocessing process at first is positioned over mass concentration with honeycomb substrate; Place the ultrasonic cleaning machine to clean 0.5～4 hour in carrier and liquid, take out the back and dried by the fire 0.5～6 hour down at 60 ℃～150 ℃; Carrier after oven dry roasting again obtained the carrier of clean dry in 5 hours.
5. method according to claim 3 is characterized in that Ludox is non-sodium cation Ludox, SiO in the Ludox
2Weight percentage is 15～35%, and the Ludox average grain diameter is 10～200nm.
6. according to claim 3 or 5 described methods, it is characterized in that Ludox is the ammonia cationic colloidal silica.
7. method according to claim 3; The preparation that it is characterized in that cerium colloidal sol is solvent with distilled water, adds cerous nitrate and citric acid, and making cerous nitrate solution concentration is 0.1～0.3mol/L; The pH value is 2～6; Stirred 4～16 hours down at 50 ℃～90 ℃, regulating the pH value through slow adding ammoniacal liquor is 7～9, and it is subsequent use to process stable cerium colloidal sol.
8. method according to claim 3; It is characterized in that the carrier coating process places Ludox to take out after 5～60 minutes in pretreated carrier; Blow the liquid in the most space with compressed air; Dried 3～16 hours down at 60 ℃～160 ℃, roasting is 3～16 hours under air ambient, promptly makes to have SiO
2The honeycomb type ceramic monolith of coating; Then, place cerium colloidal sol to take out after 5～60 minutes in above-mentioned carrier, blow the liquid in the most space with compressed air, dried 3～16 hours down at 60 ℃～160 ℃, roasting obtained having CeO in 3～16 hours under air ambient
2Honeycomb ceramic carrier,
9. method according to claim 3; It is characterized in that it is the nitrate solution of 0.5～2% Pt, Zr and La that carrier after the active constituent loading process is with coating places metallic element quality percentage composition; Pt, Zr, La metallic element mol ratio are 0.1～1: 1.5～4.5 in the solution: 1.5～4, and stop after 3～60 minutes and take out, dried 3～16 hours down at 60 ℃～160 ℃; Roasting is 3～16 hours under air ambient, makes catalyst for catalytic combustion.
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|---|---|---|---|
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|---|---|---|---|
| CN 201010510999 CN102441379B (en) | 2010-10-12 | 2010-10-12 | Catalytic combustion catalyst and preparing method thereof |
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| CN102441379B CN102441379B (en) | 2013-06-19 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106238041A (en) * | 2016-07-28 | 2016-12-21 | 天津大学 | The preparation method of the catalyst that volatile organic matter ozonisation is decomposed it is catalyzed under a kind of room temperature |
| CN111266100A (en) * | 2018-12-04 | 2020-06-12 | 大连凯特利催化工程技术有限公司 | Ethane catalytic combustion monolithic catalyst and preparation method thereof |
| CN112295554A (en) * | 2020-11-13 | 2021-02-02 | 中国科学技术大学 | Catalytic combustion catalyst, preparation method and application thereof |
| CN113634249A (en) * | 2021-07-23 | 2021-11-12 | 浙江大学杭州国际科创中心 | High-temperature stable catalytic combustion catalyst and preparation method thereof |
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| CN1277892A (en) * | 2000-06-21 | 2000-12-27 | 中国科学院兰州化学物理研究所 | Catalyst for use in waste gas purification |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1277892A (en) * | 2000-06-21 | 2000-12-27 | 中国科学院兰州化学物理研究所 | Catalyst for use in waste gas purification |
Non-Patent Citations (1)
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| 陈玉香等: "WSH-1催化燃烧催化剂在炼油厂污水场废气治理中的应用", 《石油炼制与化工》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106238041A (en) * | 2016-07-28 | 2016-12-21 | 天津大学 | The preparation method of the catalyst that volatile organic matter ozonisation is decomposed it is catalyzed under a kind of room temperature |
| CN111266100A (en) * | 2018-12-04 | 2020-06-12 | 大连凯特利催化工程技术有限公司 | Ethane catalytic combustion monolithic catalyst and preparation method thereof |
| CN111266100B (en) * | 2018-12-04 | 2022-10-28 | 大连凯特利催化工程技术有限公司 | Ethane catalytic combustion monolithic catalyst and preparation method thereof |
| CN112295554A (en) * | 2020-11-13 | 2021-02-02 | 中国科学技术大学 | Catalytic combustion catalyst, preparation method and application thereof |
| CN112295554B (en) * | 2020-11-13 | 2022-03-01 | 中国科学技术大学 | Catalytic combustion catalyst, preparation method and application thereof |
| CN113634249A (en) * | 2021-07-23 | 2021-11-12 | 浙江大学杭州国际科创中心 | High-temperature stable catalytic combustion catalyst and preparation method thereof |
| CN113634249B (en) * | 2021-07-23 | 2022-07-05 | 浙江大学杭州国际科创中心 | High-temperature stable catalytic combustion catalyst and preparation method thereof |
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|---|---|
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