CN102441404B - Sulfur-resistant catalytic combustion catalyst and preparation method thereof - Google Patents
Sulfur-resistant catalytic combustion catalyst and preparation method thereof Download PDFInfo
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- CN102441404B CN102441404B CN 201010510998 CN201010510998A CN102441404B CN 102441404 B CN102441404 B CN 102441404B CN 201010510998 CN201010510998 CN 201010510998 CN 201010510998 A CN201010510998 A CN 201010510998A CN 102441404 B CN102441404 B CN 102441404B
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Abstract
The invention discloses a sulfur-resistant catalytic combustion catalyst and a preparation method thereof. The catalytic combustion catalyst adopts honeycomb ceramic as a carrier, the surface of the honeycomb ceramic carrier is provided with coating, whereinich by metering according to the total weight, the coating contains 40 to 85 percent by weight of active Al2O3, 5 to 50 percent by weight of TiO2, 5 to 15 percent by weight of CeO2, 2 to 10 percent by weight of La2O3 and 3 to 15 percent by weight of one or more of CuO, MnO2, NiO and Fe2O3, the coating is loaded with precious metal active components Pt or Pt and Pd, the molar ratio of Pt to Pd is 1:1 to 3:1, and the amount of the loaded precious metal active components is 0.2g to 3.5g per liter of the catalyst. The preparation method for the catalytic combustion catalyst includes a coating slurry preparation process, a carrier-preprocessing process and a carrier-coating and precious metal active component-loading process. The catalyst has high activity and stability in the process of catalytic combustion for treating sulfurous organic flue gas, the preparation method is simple, and the catalyst is suitable for industrial application.
Description
Technical field
The invention belongs to the sulfur-containing organic waste gas field of purification, be specifically related to a kind of catalyst for catalytic combustion with anti-sulphur and preparation method thereof.
Background technology
Along with developing rapidly of industrial trade, a lot of enterprises discharge organic exhaust gas in a large number, particularly in petroleum refining industry and electronics, printing, coating, paint process industry.A large amount of dischargings of organic exhaust gas have had a strong impact on people's normal life, and the health of harm humans has serious harm to people's eye, respiratory tract and nervous system.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.Production by Catalytic Combustion Process to the processing of volatile organic matter have efficiently, the characteristics of low temperature, but generally sulfur-containing organic waste gas is produced poisoning phenomenon, affect the activity stability of catalyst.How to develop and have sulfur resistance, at a low price, effectively catalyst for catalytic combustion becomes the emphasis of research.
Patent CN1415410A discloses a kind of catalyst for catalytic combustion and preparation method thereof.Solved the problem that in the prior art, the noble metal component utilization rate of catalyst for catalytic combustion is low, dispersion is inhomogeneous.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, active A l
2O
320%～80%, TiO
210%～40%, CeO
25%～30%, ZrO
25%～20%.CN02133123.5 discloses a kind of catalyst for catalytic combustion, is comprised of the honeycomb ceramic carrier skeleton of bulk and coating and the noble metal active component that applies on it.This catalyst has the advantages that coating difficult drop-off, resistance to elevated temperatures are good, noble metal active component effective rate of utilization is high.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, between coating and honeycomb ceramic carrier skeleton in conjunction with firm, use procedure floating coat difficult drop-off.Above-described catalyst for catalytic combustion can be adapted to the catalytic combustion of the organic exhaust gas of multiple low concentration, but the deficiency that exists is that this catalyst does not have tolerance to sulphur, and the catalytic combustion that can't adapt to sulfur-containing organic waste gas is processed.
At present, organic waste gas catalytic combustion catalyst mostly adopts noble metal as active component, noble metal has advantages of active high as the catalyst for catalytic combustion of active component, common organic exhaust gas had very high clearance, but when having a certain amount of sulfide in waste gas, the noble metal active component of this catalyst is easy to sulfide and interacts and inactivation, even loses the organic waste gas catalytic combustion treatment effect thereby reduce.Therefore, develop the noble metal with anti-sulphur significant as the catalyst for catalytic combustion of active component.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of catalyst for catalytic combustion and preparation method who processes sulfur-containing organic waste gas, this catalyst has high-activity stable in the catalyticing combustion process of processing sulfur-containing organic waste gas.
Catalyst for catalytic combustion of the present invention is take ceramic honey comb as carrier, there is coating on the honeycomb ceramic carrier surface, on coating, noble metal active component Pt or mol ratio are arranged is Pt and the Pd of 1: 1～3: 1 in load, the loading of noble metal active component is every liter of catalyst 0.2～3.5g, by the gross weight of coating, contain weight percentage in coating and be 40%～85% active A l
2O
3, 5%～50% TiO
2, 5%～15% CeO
2, 2%～10% La
2O
3, 3%～15% CuO, MnO
2, NiO, Fe
2O
3In one or more.
In the present invention, generally to select cordierite be that raw material is made to honeycomb ceramic carrier; Al used in coating
2O
3Can be various crystalline forms, preferred crystal formation is γ-Al
2O
3TiO
2Can be various other TiO of level
2Powder, preferred Nano grade.
In the present invention, the preparation process of catalyst for catalytic combustion comprises: coating slurries process for preparation, carrier preprocessing process, carrier coating and noble metal active component loading process.
Described coating slurry configurations process adds appropriate Al take distilled water as solvent
2O
3Powder, TiO
2Powder, CeO
2Powder, La
2O
3The nitrate of powder and one or more copper, manganese, iron, nickel grinds to form with the equally distributed slurries of water standbyly, makes in the catalyst of preparation by the gross weight of coating, contains weight percentage in coating and be 40%～85% active A l
2O
3, 5%～50% TiO
2, 5%～15% CeO
2, 2%～10% La
2O
3, 3%～15% CuO, MnO
2, NiO, Fe
2O
3In one or more.The TiO that adds
2Powder is nanoscale.
At first described honeycomb ceramic carrier preprocessing process is positioned over honeycomb substrate mass concentration is to soak 1～6 hour in 0.5%～2% watery hydrochloric acid, carrier and liquid are placed in supersonic cleaning machine cleaned 0.5～4 hour, dried by the fire 0.5～6 hour under 60 ℃～150 ℃ after taking out; Carrier after oven dry roasting again obtained cleaning dry carrier in 5 hours.
Described carrier coating and active constituent loading process are placed in pretreated carrier the coating slurries of preparing and take out after 5～60 minutes, blow slurries in the space with compressed air, dried 3～16 hours under 60 ℃～160 ℃, roasting is 3～16 hours under air ambient, namely makes the cated honeycomb type ceramic monolith of tool; Then, it is 0.5～2% Pt or Pt and Pd precious metal salt solution that above-mentioned carrier is placed in mass concentration, if the mixed solution of Pt and Pd, wherein mol ratio Pt: Pd is 1: 1～3: 1, stop after 3～60 minutes and take out, dried 3～16 hours under 60 ℃～160 ℃, roasting is 3～16 hours under air ambient, makes anti-sulfur catalysis combustion catalyst.
Compared with prior art, the present invention has following advantage:
1, CuO, MnO have been added in the coating of catalyst for catalytic combustion of the present invention
2, NiO, Fe
2O
3Deng composition, reduced the interaction of noble metal active component in sulphur-containing substance and catalyst in the sulfur-containing organic waste gas, improved the stability of catalyst treatment sulfur-containing organic waste gas in catalyticing combustion process, make the catalyst have stronger sulfur resistance.
2, the nanoscale TiO that adds in catalyst coat of the present invention
2Can effectively improve the structure of coating, each component in coating is mixed, make the noble metal active component of catalyst cupport be uniformly distributed in coating surface, improved the active force on the interaction of catalyst activity component and coating and coating and honeycomb type ceramic monolith surface, effectively prevent coating shedding and loss of active component, improve the activity stability of catalyst.
3, manufacture craft of the present invention and equipment are 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
Take distilled water as solvent, add appropriate Al
2O
3Powder, nanoscale TiO
2Powder, CeO
2Powder, La
2O
3Powder and copper nitrate grind to form with the equally distributed slurries of water standby, make in the catalyst of preparation by the gross weight of coating, contain active A l in coating
2O
361%, TiO
225%, CeO
28.3%, La
2O
32.3%, CuO3.4%.
It is that 1% watery hydrochloric acid soaks 2h that the specification honeycomb ceramic carrier that is 100mm * 100mm * 50mm is put into mass concentration, with carrier and diluted acid liquid after cleaning 2h under microwave, dry up after taking-up, and be placed in the baking oven 6 hours of 100 ℃, the carrier roasting of gained was obtained cleaning dry honeycomb type ceramic monolith in 5 hours standby.
Dry support is placed in slurries takes out after 25 minutes, blow slurries in the duct with compressed air, oven dry is 6 hours under 100 ℃, and roasting is 5 hours under air ambient.It is that 0.55% solution dipping took out after 10 minutes that the carrier of gained is placed in the Pt mass concentration, be placed in the baking oven 6 hours of 100 ℃, more anti-sulfur catalysis combustion catalyst is namely made in roasting in 5 hours.
Embodiment 2
Take distilled water as solvent, add appropriate Al
2O
3Powder, TiO
2Powder, CeO
2Powder, La
2O
3Powder, copper nitrate and manganese nitrate grind to form with the equally distributed slurries of water standby, make in the catalyst of preparation by the gross weight of coating, contain Al in coating
2O
370%, TiO
217%, CeO
25.6%, La
2O
31.8%, CuO3.2%, MnO
22.4%.
It is that 1% watery hydrochloric acid soaks 2h that the specification honeycomb ceramic carrier that is 100mm * 100mm * 50mm is put into mass concentration, with carrier and diluted acid liquid after cleaning 2h under microwave, dry up after taking-up, and be placed in the baking oven 4 hours of 120 ℃, the carrier roasting of gained was obtained cleaning dry honeycomb type ceramic monolith in 5 hours standby.
Dry support is placed in slurries takes out after 25 minutes, blow slurries in the duct with compressed air, oven dry is 4 hours under 120 ℃, and roasting is 5 hours under air ambient.It is that 0.55% solution dipping took out after 10 minutes that the carrier of gained is placed in the Pt mass concentration, be placed in the baking oven 6 hours of 120 ℃, more anti-sulfur catalysis combustion catalyst is namely made in roasting in 5 hours.
Embodiment 3
Take distilled water as solvent, add appropriate Al
2O
3Powder, nano-TiO
2Powder, CeO
2Powder, La
2O
3Powder, copper nitrate, manganese nitrate, ferric nitrate and nickel nitrate grind to form with the equally distributed slurries of water standby, make in the catalyst of preparation by the gross weight of coating, contain active A l in coating
2O
370%, TiO
211%, CeO
211%, La
2O
32%, CuO2%, MnO
22%, Fe
2O
31.2%, NiO0.8%.
It is that 1% watery hydrochloric acid soaks 2h that the specification honeycomb ceramic carrier that is 100mm * 100mm * 50mm is put into mass concentration, with carrier and diluted acid liquid after cleaning 2h under microwave, dry up after taking-up, and be placed in the baking oven 6 hours of 100 ℃, the carrier roasting of gained was obtained cleaning dry honeycomb type ceramic monolith in 5 hours standby.
Dry support is placed in slurries takes out after 40 minutes, blow slurries in the duct with compressed air, oven dry is 6 hours under 100 ℃, and roasting is 5 hours under air ambient.It is that 1.2% solution dipping took out after 10 minutes that the carrier of gained is placed in Pt and Pd mass concentration, and the mol ratio of Pt and Pd is 2: 1, be placed in the baking oven 6 hours of 100 ℃, more anti-sulfur catalysis combustion catalyst is namely made in roasting in 5 hours.
Embodiment 4
Take distilled water as solvent, add appropriate Al
2O
3Powder, nano-TiO
2Powder, CeO
2Powder, La
2O
3Powder, copper nitrate, manganese nitrate, ferric nitrate and nickel nitrate grind to form with the equally distributed slurries of water standby, make in the catalyst of preparation by the gross weight of coating, contain active A l in coating
2O
340%, TiO
225%, CeO
214%, La
2O
38%, CuO5%, MnO
24%, Fe
2O
33%, NiO1%.
It is that 2% watery hydrochloric acid soaks 6h that the specification honeycomb substrate that is 100mm * 100mm * 50mm is put into mass concentration, with carrier and diluted acid liquid after cleaning 4h under microwave, dry up after taking-up, and be placed in the baking oven 6 hours of 110 ℃, the carrier roasting of gained was obtained cleaning dry honeycomb type ceramic monolith in 5 hours standby.
Dry support is placed in slurries takes out after 40 minutes, blow slurries in the duct with compressed air, oven dry is 6 hours under 110 ℃, and roasting is 5 hours under air ambient.It is that 1.5% solution dipping took out after 10 minutes that the carrier of gained is placed in the Pt mass concentration, be placed in the baking oven 6 hours of 100 ℃, more anti-sulfur catalysis combustion catalyst is namely made in roasting in 5 hours.
Comparative example
According to the method for patent CN1415410A, take 70g gama-alumina powder, 14g Detitanium-ore-type TiO
2Powder, 10gCeO
2Powder, 6gZrO
2Powder adds 1.4L distilled water after mixing, grind to form moisture even thin pulp.Be that 100mm * 100mm * 50mm honeycomb ceramic body takes out after submergence 30min in above-mentioned moisture thin pulp with specification, blow raffinate with compress wind, 120 ℃ of air dryings 12 hours, the cated honeycomb substrate of tool was made in 550 ℃ of lower roastings 3 hours.Then, it is 1.5% that carrier is put into the Pt mass concentration, and in the aqueous solution of acetic acid concentration 0.05mol/L, dipping takes out after 60min, and 120 ℃ of air dryings 20 hours, roasting namely made catalyst for catalytic combustion in 3 hours in 550 ℃ of air.This catalyst coat forms: active A l
2O
370%, TiO
214%, ZrO6%, CeO
210%.
In order to estimate each catalyst to the treatment effect of sulfur-containing organic waste gas, catalyst is carried out experimental evaluation.
Organic exhaust gas with the sulfur-bearing 600ppm of certain oil-refining chemical factory discharging is estimated as processing object, and the total hydrocarbon concentration of this waste gas is 4000mg/m
3, reaction velocity is 30000h
-1, 300 ℃ of bed inlet temperatures.Evaluation result sees Table 1.
As can be seen from Table 1, catalyst of the present invention has anti-sulphur and higher organic removal rate preferably.
Table 2 is that the long running of the catalyst of embodiment 3 mades is estimated situation, and clearance remains on more than 97% always.The prepared catalyst of comparative example continuous operation after 50 hours organic removal rate drop to 84.7%, obvious sulfur poisoning phenomenon has occured.
The purified treatment effect of table 1 catalyst to sulfur-containing organic waste gas
The experimental evaluation of table 2 catalyst long running
| The duration of runs/hour | Entrance total hydrocarbon mg/m 3 | Outlet total hydrocarbon mg/m 3 | Clearance % |
| 24 | 4100 | 22.7 | 99.4 |
| 48 | 4080 | 23.5 | 99.4 |
| 72 | 3980 | 30.6 | 99.2 |
| 96 | 4112 | 78.2 | 98.1 |
| 120 | 4082 | 66.5 | 98.4 |
| 144 | 3996 | 45.3 | 98.9 |
| 168 | 4112 | 44.2 | 98.9 |
| 192 | 4012 | 70.1 | 98.3 |
| 216 | 4026 | 55.6 | 98.6 |
| 240 | 4105 | 65.8 | 98.4 |
| 264 | 3911 | 70.2 | 98.2 |
| 288 | 3890 | 69.8 | 98.2 |
| 272 | 4004 | 80.2 | 98.0 |
| 312 | 3966 | 81.7 | 97.9 |
| 336 | 4111 | 79.6 | 98.1 |
| 360 | 4068 | 90.2 | 97.8 |
Claims (4)
1. the preparation method of an anti-sulfur catalysis combustion catalyst, it is characterized in that: comprise coating slurries process for preparation, carrier preprocessing process, carrier coating and noble metal active component loading process, described coating slurry configurations process adds appropriate Al take distilled water as solvent
2O
3Powder, TiO
2Powder, CeO
2Powder, La
2O
3The nitrate of powder and one or more copper, manganese, iron, nickel grinds to form with the equally distributed slurries of water standbyly, makes in the catalyst of preparation by the gross weight of coating, contains weight percentage in coating and be 40%～85% active A l
2O
3, 5%～50% TiO
2, 5%～15% CeO
2, 2%～10% La
2O
3, 3%～15% CuO, MnO
2, NiO, Fe
2O
3In one or more, the anti-sulfur catalysis combustion catalyst of preparing is take ceramic honey comb as carrier, there is coating on the honeycomb ceramic carrier surface, on coating, noble metal active component Pt or mol ratio are arranged is Pt and the Pd of 1: 1～3: 1 in load, and the loading of noble metal active component is every liter of catalyst 0.2～3.5g.
2. it is characterized in that in accordance with the method for claim 1: the TiO that adds
2Powder is nanoscale.
3. in accordance with the method for claim 1, it is characterized in that: at first described honeycomb ceramic carrier preprocessing process is positioned over honeycomb substrate mass concentration is to soak 1～6 hour in 0.5%～2% watery hydrochloric acid, carrier and liquid are placed in supersonic cleaning machine cleaned 0.5～4 hour, dried by the fire 0.5～6 hour under 60 ℃～150 ℃ after taking out; Carrier after oven dry roasting again obtained cleaning dry carrier in 5 hours.
4. in accordance with the method for claim 1, it is characterized in that: described carrier coating and noble metal active component loading process are placed in pretreated carrier the coating slurries of preparing and take out after 5～60 minutes, blow slurries in the space with compressed air, dried 3～16 hours under 60 ℃～160 ℃, roasting is 3～16 hours under air ambient, namely makes the cated honeycomb type ceramic monolith of tool; Then, it is 0.5～2% Pt or the precious metal salt solution of Pt and Pd that above-mentioned carrier is placed in mass concentration, if the mixed solution of Pt and Pd, wherein mol ratio Pt: Pd is 1: 1～3: 1, stop after 3～60 minutes and take out, dried 3～16 hours under 60 ℃～160 ℃, roasting is 3～16 hours under air ambient, makes anti-sulfur catalysis combustion catalyst.
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| CN102441404B true CN102441404B (en) | 2013-06-19 |
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| CN105008046B (en) * | 2013-02-25 | 2017-09-01 | 优美科触媒日本有限公司 | Exhaust gas purification catalyst and the exhaust gas purifying method using the exhaust gas purification catalyst |
| CN104549529B (en) * | 2013-10-22 | 2016-08-17 | 中国石油化工股份有限公司 | A kind of high firmness honeycomb ceramic carrier and preparation method thereof |
| CN105964255A (en) * | 2016-06-24 | 2016-09-28 | 浙江恒荣环保科技有限公司 | Preparation method of high-sulfur-resistance catalytic combustion catalyst |
| CN106040259A (en) * | 2016-06-24 | 2016-10-26 | 浙江恒荣环保科技有限公司 | Catalyst for catalytic combustion of VOCs and preparation method of catalyst |
| WO2018096385A1 (en) | 2016-11-23 | 2018-05-31 | Qatar University | Palladium catalyst for oxidation of methane and method of preparation and use thereof |
| CN107308954A (en) * | 2017-06-22 | 2017-11-03 | 浙江工业大学 | A kind of monoblock type combustion catalyst with dynamics model |
| CN108126710A (en) * | 2017-12-26 | 2018-06-08 | 河北旭阳焦化有限公司 | A kind of sulfur resistive removes the preparation and application of naphthalene catalyst |
| CN110327938B (en) * | 2019-07-30 | 2022-05-13 | 苏州卡泰里环保能源有限公司 | Catalytic combustion catalyst with core-shell structure and preparation method thereof |
| CN110743545A (en) * | 2019-09-29 | 2020-02-04 | 浙江工业大学 | Ethylene oxide double-active-site combustion catalyst and preparation and application thereof |
| CN110961142A (en) * | 2019-12-17 | 2020-04-07 | 珂黎艾净化技术江苏有限公司 | NSC (non-catalytic cracking) purification catalyst of tail gas emission control purifier for internal combustion engine |
| CN112403490A (en) * | 2020-10-27 | 2021-02-26 | 福建龙新三维阵列科技有限公司 | Sulfur-resistant catalyst, preparation method and application |
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