CN101439286A - Oxiadition catalyst for eliminating harmful accessory substances containing rare-earth metal in catalytic purification process of nitrous oxides - Google Patents
Oxiadition catalyst for eliminating harmful accessory substances containing rare-earth metal in catalytic purification process of nitrous oxides Download PDFInfo
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- CN101439286A CN101439286A CNA2007101779978A CN200710177997A CN101439286A CN 101439286 A CN101439286 A CN 101439286A CN A2007101779978 A CNA2007101779978 A CN A2007101779978A CN 200710177997 A CN200710177997 A CN 200710177997A CN 101439286 A CN101439286 A CN 101439286A
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Abstract
The invention provides an oxidation catalyst used for eliminating the byproducts like carbon monoxide and hydrocarbon generated during the catalytic purification process of a nitrogen oxide. The conversion rate of the oxidation catalyst to CO approaches to 100 percent under the temperature of 270 DEG C, in the exhaust temperature range of a diesel engine (200 to 500 DEG C), the carbon monoxide, hydrocarbon, residual carbon and hydrogen and oxygen containing organisms in tail gas can be completely oxidized and eliminated. The oxidization capacity of the catalyst is proper and can not affect the activity of the cleaning catalyst of the nitrogen oxide when being combined and used with the cleaning catalyst of the nitrogen oxide. The catalyst is formed by taking copper as an active component, taking the rare earth of cerium as an addition agent component and loading the two components on the carrier of an inorganic oxide. The oxidation catalyst is characterized in that the active component can be at least one from the following copper compounds; the addition agent component can be at least one from the following cerium compounds; the inorganic oxide can be at least one from the following inorganic oxides. The copper compounds comprise copper nitrate, bluestone and cupric acetate; the compounds of copper-cerium chloride comprise cerium nitrate, cerous sulfate and cerous phosphate; the inorganic oxide of cerium acetate comprises silicon dioxide, gamma-aluminium oxide, zirconia, lanthana, zinc oxide and titanium dioxide.
Description
Technical field
The present invention is a kind of oxidation catalyst, is used for eliminating accessory substances such as carbon monoxide that catalyst for purification of nitrogen oxides produces in the purifying nitrogen oxide process and residual carbon hydrogen compound.It is characterized in that this catalyst as active component,, loads on both copper on the inorganic oxide carrier with infusion process and to constitute as adjuvant component with the rare earth cerium.This oxidation catalyst, in the time of 270 ℃ to the conversion ratio of CO near 100%, in the scope of diesel exhaust gas temperature (200 ℃～500 ℃), can be with the carbon monoxide in the tail gas, hydrocarbon and oxygen-bearing organic matter complete oxidation are eliminated.This catalyst activity component is a common metal, oxidability is moderate, and the catalytic efficiency height is when uniting use with catalyst for purification of nitrogen oxides, neither can influence activity, can effectively remove accessory substances such as carbon monoxide, hydrocarbon and oxygen-bearing organic matter again catalyst for purification of nitrogen oxides.
Technical background
Diesel engine has good dynamic property and economy, is a main flow direction of following motor vehicle development.The noxious pollutant that diesel engine produces in combustion process also can not be ignored but simultaneously.Wherein, particle and nitrogen oxide are two big pollutants of diesel engine.The silver components that we develop loads on the catalyst for purification of nitrogen oxides on the porous inorganic oxide carrier, can be in very wide temperature range, with hydrocarbon or oxygen-bearing organic matter is reducing agent, and well purifying nitrogen oxide makes it to be converted into harmless nitrogen.But we notice in the process of purifying nitrogen oxide, have a large amount of carbon monoxide to produce, and in the lower temperature range of catalyst for purification of nitrogen oxides conversion ratio, a certain amount of residue reducing agent is arranged in the gas.More perfect for the purification that makes diesel engine vent gas, be necessary the harmful side product that produces in the purifying nitrogen oxide process is handled.
At present, be used for eliminating the diesel oxidation catalyst of diesel engine vent gas carbon monoxide and hydrocarbon, generally use noble metal to be active component, cost is higher.And the precious metal oxidation catalyst oxidability is too high, and is not suitable for to place and eliminates carbon monoxide and residue reducing agent behind the catalyst for purification of nitrogen oxides.Studies show that, after commercial precious metal oxidation catalyst places catalyst for purification of nitrogen oxides, when eliminating carbon monoxide and hydrocarbon, the transformation efficiency of nitrogen oxide is reduced greatly.What we needed is the moderate oxidation catalyst of a kind of oxidability, when it and catalyst for purification of nitrogen oxides coupling, both can promptly eliminate accessory substance carbon monoxide and hydrocarbon fully at lower temperature, can not influence the catalytic purification efficient of nitrogen oxide again.In addition, in order to alleviate the burden of tail gas catalytic purification system, the efficient of this kind catalyst should be very high, and requirement should be much smaller than catalyst for purification of nitrogen oxides, and this kind catalyst and nitrogen oxide catalyst should keep compound mode the most closely.
Summary of the invention
The invention provides and a kind ofly be used for eliminating catalyst for purification of nitrogen oxides in the purifying nitrogen oxide process, the oxidation catalyst of the carbon monoxide of generation and residual carbon hydrogen compound.It is characterized in that this catalyst, as adjuvant component, is loaded on both on the inorganic oxide carrier with infusion process and to constitute with the rare earth cerium as active component by copper.Active component is carried on the inorganic oxide carrier by infusion process by the copper of metallic element weight scaled value 1-15%.Adjuvant component is carried on the inorganic oxide carrier by infusion process by the rare earth cerium of metallic element weight scaled value 5-50%.Inorganic oxide is silica, γ-alundum (Al, zirconia, lanthana, zinc oxide, titanium dioxide one or more hopcalites wherein.This catalyst uses copper to be active component, and the rare earth cerium of wide material sources is as adjuvant component, be simple and easy to inorganic porous property material be carrier.The preparation method is simple, takes the infusion process of generally using.The present invention is on the achievement in research basis that fully takes into account in the past, has carried out the result of big quantity research.The catalyst that is provided is in the diesel engine vent gas temperature range, volume is three of a catalyst for purification of nitrogen oxides/for the moment, transformed carbon monoxide and the hydrocarbon in the gas fully, and do not influence the catalytic purification efficient of nitrogen oxide, reach the purpose of eliminating the diesel engine gas pollutant fully.
Catalyst of the present invention is main active component with copper, is adjuvant component with the rare earth cerium, two components is loaded on the inorganic oxide carrier of certain form to constitute.Aforementioned active component is obtained by the mixture of at least one or more than one in the compound of following copper: copper nitrate, copper sulphate, copper acetate, copper chloride.Aforementioned adjuvant component is obtained by the mixture of at least one or more than one in the compound of following rare earth cerium: cerous nitrate, cerous sulfate, cerous phosphate, cerous acetate.Aforementioned inorganic oxide carrier can be silica, γ-alundum (Al, zirconia, lanthana, zinc oxide, the mixture of at least a or more than one inorganic oxides in the titanium dioxide.The inorganic oxide carrier specific area is at least greater than 20 meters squared per gram, and inorganic oxide carrier is a powder.
According to the present invention, the adjuvant component cerium can pass through the certain density metal soluble compound aqueous solution, tells inorganic oxide carrier before loading on well-known infusion process.Active ingredient copper can be passed through the aqueous solution with certain density metal soluble compound, tells on the inorganic oxide carrier before loading on infusion process.For example, select infusion process for use, the inorganic oxide powder carrier is slowly poured in the certain density cerous nitrate aqueous solution under constantly stirring, continue then to stir 1-2 hour, remove moisture at 60 ℃, spend the night 120 ℃ of bakings again with Rotary Evaporators.The above-mentioned inorganic oxide carrier that has added the adjuvant component cerium in air atmosphere, with the programming rate of 10 ℃ of per minutes, is warmed up to 500 ℃ or 550 ℃ from 50 ℃, 500 ℃ or 550 ℃ of calcinings 4-5 hour.Further, select infusion process for use, the above-mentioned inorganic oxide powder carrier that has added the adjuvant component cerium is slowly poured in the certain density copper nitrate aqueous solution under constantly stirring, continue then to stir 1-2 hour, remove moisture with Rotary Evaporators at 60 ℃, spend the night 120 ℃ of bakings again.Above-mentioned dried catalyst in air atmosphere, with the programming rate of 10 ℃ of per minutes, is warmed up to 500 ℃ or 550 ℃ from 50 ℃, 500 ℃ or 550 ℃ of calcinings 4-5 hour.The catalyst screening that makes is the particle of certain order number.
Aforesaid catalyst according to different needs, can be made various structures, and catalyst can be coated in the form of coating on the wall surface of the pottery or the circulation passage of metal honeycomb, or catalyst is made spherical or tabular.
Preparation process of the present invention is simple, and is easy to operate.Compare with existing commercial diesel oxidation catalyst, the present invention has following advantage:
(1) to select common metal copper for use be active component to catalyst of the present invention, and the rare earth cerium is an adjuvant component, and inorganic porous property material is a carrier, and raw material is cheap is easy to get in preparation, wide material sources, and the preparation method is simple.
(2) catalyst of the present invention is in the time of 270 ℃, to the transformation efficiency of carbon monoxide near 100%.
When (3) catalyst of the present invention is used for behind the catalyst for purification of nitrogen oxides, significantly improves the integer catalyzer system and removed CO and residual hydrocarbon activity, and do not influenced the transformation efficiency of nitrogen oxide.
(4) catalyst of the present invention only need be equivalent to 1/3 of catalyst for purification of nitrogen oxides consumption, keep the compactest arrangement mode with catalyst for purification of nitrogen oxides, just can satisfy the requirement of in the diesel engine exhaust temperature range, eliminating carbon monoxide and hydrocarbon fully.
The specific embodiment
In order to be illustrated more clearly in the present invention, enumerate following examples, but it there is not any restriction to the scope of application of the present invention.
Embodiment 1
Get 10 gram γ-alundum (Al powder, under constantly stirring, slowly pour in 200 milliliters of aqueous solution that dissolve 15.4132 gram cerous nitrates.Stir after 1 hour, use the Rotary Evaporators evaporating water, put into the ceramic evaporation ware, 120 ℃ of bakings are spent the night.Composite oxide carrier after the oven dry in air atmosphere, with the programming rate of 10 ℃ of per minutes, is warmed up to 500 ℃ from 50 ℃, 500 ℃ of calcinings 4 hours.Get the oxide carrier powder that 10 grams have added the adjuvant component cerium, under constantly stirring, slowly pour in 200 milliliters of aqueous solution that dissolve 1.8875 gram copper nitrates.Stir after 1 hour, use the Rotary Evaporators evaporating water, put into the ceramic evaporation ware, 120 ℃ of bakings are spent the night.Catalyst after the oven dry in air atmosphere, with the programming rate of 10 ℃ of per minutes, is warmed up to 500 ℃ from 50 ℃, and 500 ℃ of calcinings 4 hours, obtaining chemical composition was 5%Cu/Ce (30%)/Al
2O
3Oxidation catalyst.Sieve is that 40～60 order particles are standby.
Embodiment 2
Get 10 gram SiO 2 powders, under constantly stirring, slowly pour in 200 milliliters of aqueous solution that dissolve 15.4132 gram cerous nitrates.Stir after 1 hour, use the Rotary Evaporators evaporating water, put into the ceramic evaporation ware, 120 ℃ of bakings are spent the night.All the other preparation processes are described with embodiment 1.Preparing chemical composition is 5%Cu/Ce (30%)/SiO
2Oxidation catalyst.
Embodiment 3
Measure the catalyst of 0.8 milliliter of embodiment 1, be positioned in the tubular fixed-bed reactor and react.Reacting gas consists of: the mist total flow is 2000 milliliters of per minutes, wherein, oxygen 10%, carbon monoxide 1000ppm, nitrogen are balanced gas.Reaction velocity (GHSV) is 150,000/ hours to the catalyst of embodiment 2.The reaction temperature interval is from 90 ℃ to 300 ℃.Carbon monoxide and carbon dioxide utilize gas chromatograph for determination.Reaction result shows that in this temperature range, behind catalyst system, the carbon monoxide conversion ratio is near 100%.The result as shown in Table 1.Embodiment 1 oxidation catalyst can be removed CO effectively, and the CO clearance has reached 100% in the time of 130 ℃.
The CO oxidation efficiency is with variation of temperature on table one oxidation catalyst
| Reaction temperature/℃ | 90 | 120 | 130 | 150 | 200 | 250 | 300 |
| CO conversion ratio/% | 65 | 92 | 100 | 100 | 100 | 100 | 100 |
Embodiment 4
The catalyst of measuring 2.4 milliliters of catalyst for purification of nitrogen oxides and 0.8 milliliter of embodiment 1 is positioned in the tubular fixed-bed reactor and reacts, and place front and back, as Fig. 1.
Reacting gas is the simulation diesel engine vent gas.Gas composition: the mist total flow is 2000 milliliters of per minutes, wherein, oxygen 10%, nitric oxide 800ppm, carbon monoxide 600ppm, propylene 1714ppm, nitrogen are balanced gas.Reaction velocity (GHSV) is 50,000/ hours to catalyst for purification of nitrogen oxides, is 150,000/ hours to oxidation catalyst.The reaction temperature interval is from 200 ℃ to 600 ℃.Nitrous oxides concentration utilizes chemiluminescent NOx analyzer to measure, and carbon monoxide utilizes gas Chromatographic Determination.Reaction result as shown in Table 2.200 ℃ of CO oxygenation efficiency of embodiment 1 oxidation catalyst have reached 79%, 250 ℃ and have eliminated CO fully, and do not have influence substantially for the NOx conversion ratio.
Table two propylene is that CO and NOx transform situation on the SCR reacting middle catalyst of reducing agent
Embodiment 5
The catalyst of measuring 2.4 milliliters of catalyst for purification of nitrogen oxides and 0.8 milliliter of embodiment 1 is positioned in the tubular fixed-bed reactor and reacts, and place front and back, as Fig. 1.
Reacting gas is the simulation diesel engine vent gas.Gas composition: the mist total flow is 2000 milliliters of per minutes, wherein, oxygen 10%, moisture 10%, nitric oxide 800ppm, carbon monoxide 600ppm, ethanol 1565ppm, nitrogen are balanced gas.Reaction velocity (GHSV) is 50,000/ hours to catalyst for purification of nitrogen oxides, is 150,000/ hours to oxidation catalyst.The reaction temperature interval is from 200 ℃ to 600 ℃.Nitrous oxides concentration utilizes chemiluminescent NOx analyzer to measure, and carbon monoxide, acetaldehyde concentration of alcohol utilize gas chromatograph for determination.Reaction result as shown in Table 3.Oxidation catalyst CO conversion ratio in the time of 270 ℃ reaches 100%, and ethanol acetaldehyde is removed fully, and the NOx conversion ratio is not had influence substantially.
Table three ethanol is that pollutant transformed situation during the SCR of reducing agent reacted
Comparative Examples 1
Measure 2.4 milliliters of catalyst for purification of nitrogen oxides, be positioned in the tubular fixed-bed reactor and react.
Reacting gas is the simulation diesel engine vent gas.Gas composition: the mist total flow is 2000 milliliters of per minutes, wherein, oxygen 10%, moisture 10%, nitric oxide 800ppm, carbon monoxide 600ppm, ethanol 1565ppm, nitrogen are balanced gas.Reaction velocity (GHSV) is 50,000/ hours to catalyst for purification of nitrogen oxides, and the reaction temperature interval is from 200 ℃ to 600 ℃.Nitrous oxides concentration utilizes chemiluminescent NOx analyzer to measure, and carbonomonoxide concentration is utilized gas chromatograph for determination.Reaction result as shown in Table 4.Catalyst for purification of nitrogen oxides has NOx conversion ratio efficiently, but has produced a large amount of CO and imperfect combustion ethanol acetaldehyde in the process.
The table tetraethoxide is pollutant conversion situation contrast on the SCR reacting middle catalyst of reducing agent
Comparative Examples 2
Measure the commercial precious metal oxidation catalyst of 2.4 milliliters of catalyst for purification of nitrogen oxides and 0.8 milliliter, be positioned in the tubular fixed-bed reactor and react, place front and back, as Fig. 1.
Reacting gas is the simulation diesel engine vent gas.Gas composition: the mist total flow is 2000 milliliters of per minutes, wherein, oxygen 10%, moisture 10%, nitric oxide 800ppm, carbon monoxide 600ppm, ethanol 1565ppm, nitrogen are balanced gas.Reaction velocity (GHSV) is 50,000/ hours to catalyst for purification of nitrogen oxides, is 150,000/ hours to oxidation catalyst.The reaction temperature interval is from 200 ℃ to 600 ℃.Nitrous oxides concentration utilizes chemiluminescent NOx analyzer to measure, and carbon monoxide, acetaldehyde concentration of alcohol utilize gas chromatograph for determination.Reaction result as shown in Table 5.Rearmounted precious metal oxidation catalyst complete oxidation CO temperature is reduced to 150 ℃, but greatly reduces transformation efficiency of the oxides of nitrogen.As embodiment 4 reaction results, embodiment 1 rearmounted oxidation catalyst can complete oxidation CO and do not influence transformation efficiency of the oxides of nitrogen at 270 ℃.Therefore embodiment 1 oxidation catalyst has more moderate oxidation activity with respect to precious metal oxidation catalyst, is the catalyst that is more suitable for eliminating the accessory substance of purification of nitrogen oxides process.
Table five ethanol is pollutant conversion situation contrast on the SCR reacting middle catalyst of reducing agent
Description of drawings
Fig. 1 oxidation catalyst is that 3:1 is positioned over catalyst for purification of nitrogen oxides schematic diagram afterwards with the volume ratio
Claims (6)
1. one kind is used for eliminating carbon monoxide, the OXIDATION OF HYDROCARBONS catalyst that the catalytic purification of nitroxide process produces, it is characterized in that this catalyst by copper as active component,, two components are loaded on the inorganic oxide carrier with infusion process constitute as adjuvant component with the rare earth cerium.
2. the described catalyst of claim 1 as described above, it is characterized in that, the copper that active component is counted 1-15% by metallic element weight scaled value is carried on the inorganic oxide carrier by infusion process, active component is obtained by the mixture of at least one or more than one in the compound of following copper: copper nitrate, copper sulphate, copper acetate, copper chloride.
3. the described catalyst of claim 1 as described above, it is characterized in that the rare earth cerium that adjuvant component is counted 5-50% by metallic element weight scaled value is carried on the inorganic oxide carrier by infusion process, adjuvant component is obtained by the mixture of at least one or more than one in the compound of following cerium: cerous nitrate, cerous sulfate, cerous phosphate, cerous acetate.
4. the described catalyst of claim 1 as described above, it is characterized in that, inorganic oxide is silica, γ-alundum (Al, zirconia, lanthana, zinc oxide, titanium dioxide one or more hopcalites wherein, the inorganic oxide carrier specific area has 20 meters squared per gram or bigger specific area, and inorganic oxide carrier is Powdered.
5. the described catalyst of claim 1-4 as described above is characterized in that catalyst is coated in the form of coating on the wall surface of circulation passage of pottery or metal honeycomb, or catalyst is made spherical or tabular.
6. the described Application of Catalyst of claim 1-5 as described above, it is characterized in that, when being applied to eliminate carbon monoxide that catalyst for purification of nitrogen oxides produces and residual hydrocarbon in the purifying nitrogen oxide process, can not influence the transformation efficiency of nitrogen oxide.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101862655A (en) * | 2010-06-28 | 2010-10-20 | 济南大学 | ZrO2 loaded copper catalyst and preparation method and application thereof |
| CN102821850A (en) * | 2010-03-25 | 2012-12-12 | Toto株式会社 | Photocatalyst-coated body and photocatalyst coating liquid |
| CN108187685A (en) * | 2017-12-30 | 2018-06-22 | 宁波高新区州致科技有限公司 | A kind of application of carbon monoxide-olefin polymeric in nitrogen oxides in effluent discharge is inhibited |
| CN114160152A (en) * | 2021-12-09 | 2022-03-11 | 山东爱亿普环保科技股份有限公司 | Denitration and decarburization double-effect catalyst and preparation method thereof |
| CN114917895A (en) * | 2022-07-21 | 2022-08-19 | 山东天璨环保科技有限公司 | Preparation method of rare earth denitration catalyst |
| CN116673047A (en) * | 2023-04-07 | 2023-09-01 | 浙江大学 | Catalyst capable of cooperatively removing nitrogen oxides and CO, and preparation method and application thereof |
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2007
- 2007-11-23 CN CNA2007101779978A patent/CN101439286A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102821850A (en) * | 2010-03-25 | 2012-12-12 | Toto株式会社 | Photocatalyst-coated body and photocatalyst coating liquid |
| CN102821850B (en) * | 2010-03-25 | 2016-01-27 | Toto株式会社 | Light catalyst loating body and photocatalyst masking liquid |
| CN101862655A (en) * | 2010-06-28 | 2010-10-20 | 济南大学 | ZrO2 loaded copper catalyst and preparation method and application thereof |
| CN108187685A (en) * | 2017-12-30 | 2018-06-22 | 宁波高新区州致科技有限公司 | A kind of application of carbon monoxide-olefin polymeric in nitrogen oxides in effluent discharge is inhibited |
| CN114160152A (en) * | 2021-12-09 | 2022-03-11 | 山东爱亿普环保科技股份有限公司 | Denitration and decarburization double-effect catalyst and preparation method thereof |
| CN114160152B (en) * | 2021-12-09 | 2022-07-22 | 山东爱亿普环保科技股份有限公司 | Denitration and decarburization double-effect catalyst and preparation method thereof |
| CN114917895A (en) * | 2022-07-21 | 2022-08-19 | 山东天璨环保科技有限公司 | Preparation method of rare earth denitration catalyst |
| CN114917895B (en) * | 2022-07-21 | 2022-09-16 | 山东天璨环保科技有限公司 | Preparation method of rare earth denitration catalyst |
| CN116673047A (en) * | 2023-04-07 | 2023-09-01 | 浙江大学 | Catalyst capable of cooperatively removing nitrogen oxides and CO, and preparation method and application thereof |
| CN116673047B (en) * | 2023-04-07 | 2024-04-12 | 浙江大学 | Catalyst capable of cooperatively removing nitrogen oxides and CO, and preparation method and application thereof |
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Open date: 20090527 |