CN102441379B - Catalytic combustion catalyst and preparing method thereof - Google Patents
Catalytic combustion catalyst and preparing method thereof Download PDFInfo
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- CN102441379B CN102441379B CN 201010510999 CN201010510999A CN102441379B CN 102441379 B CN102441379 B CN 102441379B CN 201010510999 CN201010510999 CN 201010510999 CN 201010510999 A CN201010510999 A CN 201010510999A CN 102441379 B CN102441379 B CN 102441379B
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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 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 discharges is contaminated environment not only, also the serious harm mankind's health.Along with the raising of people's living standard, also more and more higher to the requirement of living environment, effective processing of this kind gas has caused people's extensive concern.In the technology of processing 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 then method of load active component preparation.
CN88100589 discloses a kind of catalyst for purifying exhaust air, comprise the honeycomb support of en-block construction and be deposited on the coating on honeycomb support, this coating is to form with a kind of carbon monoxide-olefin polymeric that contains the refractory inorganic oxide in 0.5 to 20 micrometer range with average particulate diameter, has platinum and/or palladium and rhodium with the high concentration deposition on refractory inorganic oxide.This kind of catalyst is that the moisture thin pulp that contains carbon monoxide-olefin polymeric by employing applies the carrier that honeycomb support and calcining apply and produces.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 inhomogeneous problem.It is active component that this catalyst adopts precious metals pt, and the mode by 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 of processing for organic waste-gas purification, block honeycomb ceramic carrier skeleton and the coating and the noble metal active component that apply on it, consists of.The coating of catalyst is by Al
2o
3, SiO
2with the common composite oxides that form of one or more alkaline earth oxides, form.
Above-described organic waste gas catalytic combustion catalyst mostly adopts honeycomb substrate, the method preparation of slurry coating and noble metal dipping, noble metal has advantages of active high as the catalyst for catalytic combustion of active component, common organic exhaust gas is had to very high clearance, but, above-mentioned catalyst existence and stability is poor, while processing the organic exhaust gas of high temperature high-speed, activity is low, easy inactivation and to the shortcoming and defect such as bad adaptability of different organic exhaust gas, particularly adopt catalyst for catalytic combustion prepared by the mode of slurry coating can't adapt to the acute variation of tolerance and because the exhaust gas concentration fluctuation causes the temperature acute variation, now, catalyst coat can come off due to aging the appearance, thereby affect the effect of catalyst, and then reduce and even lose the organic waste gas catalytic combustion disposal ability.Therefore, develop in conjunction with high-activity stable firmly and the extensive catalyst for catalytic combustion of adaptability significant.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of catalyst for catalytic combustion and preparation method thereof, this catalyst has very high coating firmness and high temperature active stability and different high temperature high-speed waste gas is all had to good treatment effect in the catalyticing combustion process of processing organic exhaust gas.
Catalyst for catalytic combustion of the present invention, take ceramic honey comb as carrier, and the honeycomb ceramic carrier surface has SiO successively
2coating and CeO
2coating, by the gross weight of coating, contain weight percentage and be 80%～95% active SiO in 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.
In the present invention, generally to select cordierite be that raw material is made to honeycomb ceramic carrier; 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, comprise process for preparation, carrier collosol coating process, the metal active constituent loading process of carrier preprocessing process, Ludox and cerium colloidal sol.
At first described honeycomb ceramic carrier preprocessing process is positioned over honeycomb substrate in the watery hydrochloric acid that mass concentration is 0.5%～2% and soaks 1～6 hour, carrier and liquid are placed in to supersonic cleaning machine and clean 0.5～4 hour, dry 0.5～6 hour under 60 ℃～150 ℃ after taking-up; Carrier after oven dry roasting again obtains clean dry carrier in 5 hours.
Described Ludox and cerium colloidal sol layoutprocedure, wherein Ludox is non-sodium cation Ludox, preferred ammonia cationic colloidal silica, SiO in 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 take distilled water as solvent, add cerous nitrate and citric acid, making cerous nitrate solution concentration is 0.1～0.3mol/L, the pH value is 2～6, under 50 ℃～90 ℃, stirring 4～16 hours, is 7～9 by slowly adding ammoniacal liquor to regulate the pH value, makes stable cerium colloidal sol standby.
Described carrier coating process is placed in Ludox by pretreated carrier and takes out after 5～60 minutes, with compressed air, blows the liquid in space, under 60 ℃～160 ℃, dries 3～16 hours, and under air ambient, roasting is 3～16 hours, makes and has SiO
2the honeycomb type ceramic monolith of coating; Then, above-mentioned carrier is placed in to cerium colloidal sol and takes out after 5～60 minutes, with compressed air, blow the liquid in space, dry 3～16 hours under 60 ℃～160 ℃, under air ambient, roasting obtains having CeO in 3～16 hours
2honeycomb ceramic carrier,
Described active constituent loading process is placed in Pt, Zr that metallic element quality percentage composition is 0.5～2% and the nitrate solution of La by the carrier after coating, in solution, Pt, Zr, La metallic element mol ratio are 0.1～1: 1.5～4.5: 1.5～4, stop after 3～60 minutes and take out, under 60 ℃～160 ℃, dry 3～16 hours, under air ambient, roasting is 3～16 hours, 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, promoted the interaction between metal active constituent, the interaction of catalyst activity component and coating and the active force on coating and honeycomb type ceramic monolith surface have been improved, effectively prevent coating shedding and loss of active component, improve the activity stability of catalyst, the advantages such as that the catalyst for catalytic combustion made has is high temperature resistant, anti-high-speed.
2, in the preparation method of catalyst for catalytic combustion of the present invention, carrier coating adopts the mode of Ludox and cerium colloidal sol to introduce, adopt colloidal sol to carry out coating to carrier, colloidal particle can be attached to carrier surface securely, be evenly distributed in conjunction with tight and coating between colloidal particle, improved fastness and the coating specific area of carrier coating.
3, the ammonia cationic colloidal silica that in the inventive method, preferred colloidal particle is 10-200nm, avoid the detrimental effect of Na ion pair reaction in catalytic process, the catalyst of preparation to have that cohesive force is strong, high temperature resistant, the characteristics of high-specific surface area.
4, the processing strong adaptability of catalyst for catalytic combustion of the present invention to VOCs waste gas, can efficiently process the VOCs waste gas of Various Complex, and the preparation method and equipment simple, easy operating and suitability for industrialized production.
The specific embodiment
Further illustrate effect of the present invention and effect below in conjunction with embodiment, but described embodiment should not be construed as the restriction of the scope of the invention.
Embodiment 1
The honeycomb ceramic carrier that is 100mm * 100mm * 50mm by specification is put into the watery hydrochloric acid that mass concentration is 1% and is soaked 2h, after carrier and diluted acid liquid are cleaned to 2h under microwave, after taking-up, dry up, and be placed in the baking oven 6 hours of 100 ℃, the carrier roasting of gained is obtained to clean dry honeycomb type ceramic monolith in 5 hours standby.
The cerous nitrate solution that the distilled water of take is 0.3mol/L as the solvent configuration concentration, and to add appropriate citric acid to make the pH of solution be 4, under 70 ℃, stirs 6 hours, uses ammoniacal liquor to regulate the pH value 7.9, makes stable cerium colloidal sol standby.
Choosing average grain diameter is 10～200nm, SiO
2the ammonia cationic colloidal silica that content is 25%, put into Ludox by pretreated carrier and take out after 30 minutes, with compressed air, blows the slurries in duct, under 160 ℃, dries 6 hours, and under air ambient, roasting is 5 hours, then apply CeO with same method
2colloidal sol, obtain having uniform SiO
2and CeO
2the carrier of coating is standby.
Take distilled water as solvent, by metal element mol ratio, add Pt (NO at 1: 4: 4
3)
4powder, Zr (NO
3)
4powder, La (NO
3)
3.6H
2the O crystalline particle, the composite reactive component nitrate solution that preparing metal element quality percentage composition is 1.2%, the carrier that has applied coating is put into to this solution dipping to be taken out after 10 minutes, be placed in the baking oven 6 hours of 160 ℃, roasting makes catalyst for catalytic combustion in 5 hours again, and wherein the loading of Pt is every liter of catalyst 1.0g.
Embodiment 2
The honeycomb ceramic carrier that is 100mm * 100mm * 50mm by specification is put into the watery hydrochloric acid that mass concentration is 2% and is soaked 2h, after carrier and diluted acid liquid are cleaned to 2h under microwave, after taking-up, dry up, and be placed in the baking oven 4 hours of 110 ℃, the carrier roasting of gained is obtained to clean dry honeycomb type ceramic monolith in 5 hours standby.
The cerous nitrate solution that the distilled water of take is 0.15mol/L as the solvent configuration concentration, and to add appropriate citric acid to make the pH of solution be 5, under 90 ℃, stirs 4 hours, uses ammoniacal liquor to regulate the pH value 8.5, forms stable colloidal sol standby.
Choosing average grain diameter is 10～200nm, SiO
2the decationizing Ludox that content is 30%, put into Ludox by pretreated carrier and take out after 15 minutes, with compressed air, blows the slurries in duct, under 110 ℃, dries 4 hours, and under air ambient, roasting is 5 hours, then apply CeO with same method
2colloidal sol, obtain having uniform SiO
2and CeO
2the carrier of coating is standby.
Take distilled water as solvent, by metal element mol ratio, add Pt (NO at 1: 4: 3
3)
4powder, Zr (NO
3)
4powder, La (NO
3)
3.6H
2the O crystalline particle, the composite reactive component nitrate solution that preparing metal element quality percentage composition is 1.8%, the carrier that has applied coating is put into to this solution dipping to be taken out after 30 minutes, be placed in the baking oven 6 hours of 110 ℃, roasting makes catalyst for catalytic combustion in 5 hours again, and wherein the loading of Pt is every liter of catalyst 1.2g.
Embodiment 3
The honeycomb ceramic carrier that is 100mm * 100mm * 50mm by specification is put into the watery hydrochloric acid that mass concentration is 1% and is soaked 6h, after carrier and diluted acid liquid are cleaned to 4h under microwave, after taking-up, dry up, and be placed in the baking oven 6 hours of 70 ℃, the carrier roasting of gained is obtained to clean dry honeycomb type ceramic monolith in 5 hours standby.
The cerous nitrate solution that the distilled water of take is 0.1mol/L as the solvent configuration concentration, and to add appropriate citric acid to make the pH of solution be 5, under 110 ℃, stirs 12 hours, uses ammoniacal liquor to regulate the pH value 7.5, forms stable colloidal sol standby.
Choosing average grain diameter is 10～200nm, SiO
2the sodium cation Ludox that content is 20%, put into Ludox by pretreated carrier and take out after 40 minutes, with compressed air, blows the slurries in duct, under 70 ℃, dries 4 hours, and under air ambient, roasting is 5 hours, then apply CeO with same method
2colloidal sol, obtain having uniform SiO
2and CeO
2the carrier of coating is standby.
Take distilled water as solvent, within 1: 2: 4 in molar ratio, add Pt (NO
3)
4powder, Zr (NO
3)
4powder, La (NO
3)
3.6H
2the O crystalline particle, the composite reactive component nitrate solution that preparing metal element quality percentage composition is 0.8%, the carrier that has applied coating is put into to this solution dipping to be taken out after 30 minutes, be placed in the baking oven 6 hours of 70 ℃, roasting makes catalyst for catalytic combustion 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, under agitation slowly add the weak aqua ammonia of 20% (V/V) to pH=7.0, and adding 2mL concentration is 50gAl
2o
3al (the NO of/100mL solution
3)
3the aqueous solution, continue to stir after 10 minutes, and adding 133mL concentration is 30gSiO
2the Ludox of/100mL solution, then add the Mg (NO that 100mL concentration is 10gMgO/100mL solution
3)
2the aqueous solution, adding water purification to moisture thin pulp cumulative volume is 1000mL, is stirred to evenly, usings 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 above-mentioned moisture thin pulp, submergence was taken out after 10 minutes, with compressed air, removed the residual slurries in hole, and then 60 ℃ of dryings 15 hours in air, in air, 550 ℃ of roastings are 2 hours, obtain the cated honeycomb ceramic carrier of tool.
The H that compound concentration is 0.4Pt/100mL solution
2ptCl
6aqueous solution 1000mL floods night as the noble metal active component, to apply cated honeycomb ceramic carrier and flood taking-up after 20 minutes in this maceration extract, blow away raffinate in hole with compressed air, and then 120 ℃ of dryings 10 hours in air, in air, 500 ℃ of roastings are 5 hours, obtain 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 sulfur-containing organic waste gas, with the VOCs of sewage treatment plant waste gas and oil refinery dry gas, catalyst is carried out to experimental evaluation respectively:
Usining certain VOCs of sewage treatment plant waste gas is estimated as processing object, and the total hydrocarbon concentration of this waste gas is 4000mg/m
3, containing H
2s is 5～15ppm approximately, and reaction velocity is 30000h
-1, 300 ℃ of bed inlet temperatures.The 24h evaluation result is in Table 1.
With oil refinery dry gas (CH
4, ethane, ethene, propane, propylene, H
2deng) for processing object, estimated, 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 in Table 2.
By table 1 and table 2, can be found out, catalyst has active and higher organic removal rate preferably.
The long running of the catalyst of embodiment 2 mades is estimated situation (VOCs of sewage treatment plant waste gas is for processing 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, comparative catalyst's surface abrasion situation under microscope after running finishes, without significantly chapping and coming off, the made catalyst of Comparative Examples can be observed be full of cracks and obscission under the microscope.。
As can be seen here, catalyst of the present invention has good treatment effect to VOCs waste gas, and has guaranteed activity stability under the hot conditions and the fastness of coating.
The purified treatment effect of table 1 catalyst to the VOCs of sewage treatment plant waste gas
The purified treatment effect of table 2 catalyst to oil refinery dry gas
The experimental evaluation of table 3 catalyst long running
| The duration of runs/hour | Entrance 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 (2)
1. the preparation method of a catalyst for catalytic combustion, the process for preparation, carrier collosol coating process, the metal active constituent loading process that comprise carrier preprocessing process, Ludox and cerium colloidal sol, it is characterized in that at first the honeycomb ceramic carrier preprocessing process is positioned over honeycomb ceramic carrier in the watery hydrochloric acid that mass concentration is 0.5%～2% and soaks 1～6 hour, carrier and liquid are placed in to supersonic cleaning machine and clean 0.5～4 hour, dry 0.5～6 hour under 60 ℃～150 ℃ after taking-up, carrier after oven dry roasting again obtains clean dry carrier in 5 hours, and Ludox is non-sodium cation Ludox, SiO in Ludox
2weight percentage is 15～35%, the Ludox average grain diameter is 10～200nm, the preparation of cerium colloidal sol be take distilled water as solvent, add cerous nitrate and citric acid, making cerous nitrate solution concentration is 0.1～0.3mol/L, the pH value is 2～6, under 50 ℃～90 ℃, stir 4～16 hours, by slowly adding ammoniacal liquor to regulate the pH value, be 7～9, make stable cerium colloidal sol standby, the carrier coating process is placed in Ludox by pretreated carrier and takes out after 5～60 minutes, blow the liquid in space with compressed air, under 60 ℃～160 ℃, dry 3～16 hours, under air ambient, roasting is 3～16 hours, make and there is SiO
2the honeycomb ceramic carrier of coating, then, above-mentioned carrier is placed in to cerium colloidal sol and takes out after 5～60 minutes, with compressed air, blow the liquid in space, dry 3～16 hours under 60 ℃～160 ℃, under air ambient, roasting obtains having CeO in 3～16 hours
2honeycomb ceramic carrier, the active constituent loading process is placed in Pt, Zr that metallic element quality percentage composition is 0.5～2% and the nitrate solution of La by the carrier after coating, in solution, Pt, Zr, La metallic element mol ratio are 0.1～1: 1.5～4.5: 1.5～4, stop after 3～60 minutes and take out, under 60 ℃～160 ℃, dry 3～16 hours, under air ambient, roasting is 3～16 hours, make catalyst for catalytic combustion, this catalyst be take ceramic honey comb as carrier, and the honeycomb ceramic carrier surface has SiO successively
2coating and CeO
2coating, by the gross weight of coating, contain weight percentage and be 80%～95% active SiO in 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. method according to claim 1, is characterized in that Ludox is the ammonia cationic colloidal silica.
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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 true CN102441379B (en) | 2013-06-19 |
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| 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 |
| 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 |
| CN112295554B (en) * | 2020-11-13 | 2022-03-01 | 中国科学技术大学 | Catalytic combustion catalyst, preparation method and application 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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2010
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (2)
| Title |
|---|
| WSH-1催化燃烧催化剂在炼油厂污水场废气治理中的应用;陈玉香等;《石油炼制与化工》;20090228;第40卷(第2期);第45～48页 * |
| 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》.2009,第40卷(第2期),第45～48页. |
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