CN102068988A - Supported nano-spinel composite oxide catalytic material and preparation method thereof - Google Patents

Supported nano-spinel composite oxide catalytic material and preparation method thereof Download PDF

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Publication number
CN102068988A
CN102068988A CN2010105845519A CN201010584551A CN102068988A CN 102068988 A CN102068988 A CN 102068988A CN 2010105845519 A CN2010105845519 A CN 2010105845519A CN 201010584551 A CN201010584551 A CN 201010584551A CN 102068988 A CN102068988 A CN 102068988A
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nitrate
catalysis material
nano spinel
preparation
complex oxide
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周洁
姚炜
刘洋
张豪杰
眭艳辉
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Abstract

The invention discloses a supported nano-spinel composite oxide catalytic material used in automobile exhaust purification and a preparation method thereof. In the preparation method, cordierite honeycomb ceramic is taken as a carrier, and gamma-Al2O3 is taken as an active coating; and then a nano-spinel composite oxide is supported to form the catalytic material, wherein, the components of the catalytic material based on mass percentage are as follows: the gamma-Al2O3 accounts for 10-25% of the weight of the cordierite honeycomb ceramic, and the nano-spinel composite oxide accounts for 10-30% of the weight of the gamma-Al2O3. With the space velocity of 15,000h-1 and at the temperature of 250-500 DEG C, the supported nano-spinel composite oxide catalytic material prepared by the method can achieve the CO purification rate up to 92.4% and the nitrogen oxide conversion rate up to 80.3%. The preparation method has the advantages of rich raw material source and simple preparation process; and the obtained catalytic material has good catalytic performance and good stability in automobile exhaust purification, and the catalyst contains no noble metal, thus having lower cost.

Description

Loaded nano spinel complex oxide catalysis material and preparation method
Technical field
The present invention relates to a kind of catalysis material and preparation method, particularly relate to a kind of loaded nano spinel complex oxide catalysis material and preparation method.
Background technology
Motor vehicle exhaust emission is the primary pollution source of modern big and medium-sized cities atmosphere pollution, and the major pollutants of motor vehicle emission have: carbon monoxide (CO), hydrocarbon (HC), nitrogen oxide (NOx), sulfide and graininess dust etc.Nitrogen oxide is the general name of various oxynitrides, in engine emission, mainly is nitric oxide and nitrogen dioxide, accounts for 99% of nitrogen oxide total amount as nitric oxide in the gasoline engine exhaust.Nitrogen oxide can serious harm human beings'health, simultaneously to environment also have harmfulness, it can cause great environmental problem such as acid rain, photochemical fog, greenhouse effects.At present, remove nitric oxide production method and can be divided into on-catalytic method and catalysis method two big classes.The on-catalytic method often exists that equipment is huge, expense is high, secondary pollution problems is arranged, so catalysis method is adopted in the purification of vehicle exhaust usually.
Cleaning catalyst for tail gases of automobiles is the effective means that reduces that motor vehicle exhaust emission pollutes.The catalyst type that is used for purifying vehicle exhaust is a lot, and early stage automobile exhaust purifier uses common metal (Cu, Cr, Mn etc.), and its abundant raw material, cost are low, but poor catalytic activity, initiation temperature height, easily poisons, and has not used now.Afterwards, people use noble metal (Pd, Pt, Rh etc.) to make catalyst, have advantages such as catalytic activity height, life-span length, anti-sulphur and phosphorus ability are good, but the noble metal scarcity of resources costs an arm and a leg, the purifying and catalyzing apparatus cost is higher, therefore be difficult to extensively promote, and for preventing the noble metal catalyst lead poisoning, automobile need use unleaded gas.In the catalytic cleaning of car tail gas field, the catalysis material of high catalytic activity and lower cost is paid close attention to by everybody more and more.The spinel complex oxide Stability Analysis of Structures, heat-resisting good, have higher oxidation activity, and have certain reducing activity, therefore CO and the NO in the purifying automobile tail gas obtained extensive studies simultaneously.
Spinelle is a kind of crystal structure of uniqueness, and general formula is AB 2O 4, have good redox characteristic, mainly be because at spinel-type AB 2O 4In, A and B can be under the prerequisites that does not change its lattice position, and utilizing appraises at the current rate realizes the electronics transmission.Spinelle at high temperature can keep stable crystal structure and big specific area, and reason is A, as long as B is a cation. and satisfying the charge number sum is eight. and ionic radius satisfies the needs of crystal structure again simultaneously, just can form various spinelles.At present, the method for preparing such spinel type composite metal oxide material mainly contains the precipitation method, sol-gel process, citric acid complex firing method, hydrothermal synthesis method, polymer complex method etc.
Find that through the retrieval to prior art document discloses spinel complex oxide of a kind of catalytic purification of motor vehicle tail gas and preparation method thereof, the chemical formula of this oxide is: CuNi 2-xMn xO 4X=0-2 wherein, the metal nitrate of cupric, nickel, manganese is made into mixed solution with certain stoichiometric proportion and citric acid, after agitating heating, concentrated ashing, grinding roasting, make the composite oxide power that contains spinel structure again, though preparation technology is simple for this catalyst, cost is lower, but has only provided initiation temperature, to the DeGrain of tail gas clean-up.
Document discloses and has been used for catalyst and the preparation method that vehicle exhaust is handled, and it is a complex carrier with original position synthesis of molecular sieve on the cordierite carrier, and carried metal Cu, Cu-La or Ag active component are made, and this catalyst is at air speed 11000h -1Conversion ratio to the NOx in the lean-combustion engine tail gas reaches as high as 74.4%.
Summary of the invention
The object of the present invention is to provide a kind of loaded nano spinel complex oxide Catalysts and its preparation method that is used for purifying vehicle exhaust.The present invention is achieved by the following technical solutions:
The invention provides a kind of loaded nano spinel complex oxide catalysis material, it is characterized in that, this catalysis material is carrier with the cordierite honeycomb ceramic, γ-alundum (Al is an active coating, the loaded with nano spinel complex oxide is prepared from, its mass percent is: γ-alundum (Al accounts for 10~25% of cordierite honeycomb ceramic carrier weight, and the nano spinel composite oxides account for 10~30% of γ-alundum (Al weight.
The chemical formula of described nano spinel composite oxides is: AAl 2O 4, wherein A is iron or cobalt or nickel or copper, or copper and mickel.
The invention provides a kind of preparation method of loaded nano spinel complex oxide catalysis material, it is characterized in that may further comprise the steps:
The first step, be 1: 2 according to mol ratio, dissolve in the deionized water, be made into nitrate mixed solution, prepare the aqueous solution of a certain amount of alkalescent precipitating reagent metal nitrate and aluminum nitrate;
Second the step, under agitation slowly be added drop-wise to nitrate solution in the aqueous solution of precipitating reagent, perhaps inverted sequence drips, and keeping the pH of solution is 9, drips the back and continues to stir, placed 60~80 ℃ of water-baths aging 2 hours, and spent deionised water and be filtered to filtrate pH=7;
The 3rd the step, with the gained filter residue 100~120 ℃ of bakings, 600~800 ℃ of roastings get the nano spinel composite oxide powder;
The 4th step, with the nano spinel composite oxide powder, boehmite, ethylene glycol, deionized water were with mass ratio 3: 10: 2: 100 mix making beating makes slurry, is 2.5~4 with rare nitric acid adjusting slurry pH value;
The 5th the step, with the cordierite ceramic carrier impregnation in slurry, purge ceramic monolith surface redundant sizing agent by pressure-air then, at last with ceramic monolith in 80~100 ℃ of oven dry, 750~800 ℃ of roastings make loaded nano spinel complex oxide catalysis material.
Described metal nitrate is or nickel nitrate or ferric nitrate or cobalt nitrate or copper nitrate or nickel nitrate and copper nitrate.
Tail gas was tested after the present invention adopted FGA-4100A five component automobile exhaust analyzers to reaction gas and catalysis.Vehicle exhaust with cyclinder gas CO content be 10%, NO (content 2000ppm), 0 2Content is 2%, N 2For balance gas is simulated.Catalysis material adopts normal pressure fixed catalytic bed to the purifying property evaluation of vehicle exhaust, carry out in φ 16mm crystal reaction tube, the catalysis material consumption is φ 15 * 30mm, the electric tube furnace heating, AI temperature controller control temperature, reaction gas gas volume air speed (GHSV) is 10000~30000h -1, temperature is 250~500 ℃.
Compared with prior art, the present invention adopts coprecipitation to prepare the nano spinel composite oxides, it is loaded on prepare loaded nano spinel complex oxide catalysis material on the cordierite honeycomb ceramic carrier again.The present invention has the following advantages: as a kind of novel cleaning catalyst for tail gases of automobiles that is used for, can purify CO and NO simultaneously, be 10000~30000h in air speed -1The time, has good purifying property, purifying rate to CO under 250~500 ℃ is up to 92.4%, transformation efficiency of the oxides of nitrogen is up to 80.3%, the raw material source of being adopted is abundant, preparation technology is simple, and the prepared loaded nano spinel complex oxide catalyst that goes out has good catalytic performance, stablizes purifying vehicle exhaust, and catalyst not contain the noble metal cost lower.
The specific embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1 blank sample
With 5 gram boehmites, 1 gram ethylene glycol, 50 gram deionized waters mix making beating and make slurry, and regulating slurry pH value with rare nitric acid is 3; With cordierite ceramic carrier impregnation in slurry 5 minutes, purge ceramic monolith surface redundant sizing agent by pressure-air then, at last with ceramic monolith in 100 ℃ of bakings 2 hours, 750 ℃ of roastings 2 hours make blank sample.
Made blank sample is carried out catalytic performance test according to the afore-mentioned test condition, and blank sample is respectively 12.6% and 6.7% to the conversion ratio of CO and NOx.
Embodiment 2
Is 1: 2 with ferric nitrate and aluminum nitrate according to mol ratio, dissolves in the deionized water, is made into nitrate mixed solution, under agitation slowly is added drop-wise in the urea liquid, keeps the pH of solution to be about 9; Drip the back and continue to stir 1.5 hours h, place 80 ℃ of water-baths, the 2 hours h that wear out, spend deionised water and be filtered to filtrate pH=7; 120 ℃ of bakings 4 hours, 600 ℃ of roasting 2h got the nanometer hercynite with the gained filter residue.With 1.5 gram nanometer hercynite powders, 5 gram boehmites, 1 gram ethylene glycol, 50 gram deionized waters mix making beating and make slurry, and regulating slurry pH value with rare nitric acid is 3; With cordierite ceramic carrier impregnation in slurry 5 minutes, purge ceramic monolith surface redundant sizing agent by pressure-air then, at last with ceramic monolith in 100 ℃ of bakings 2 hours, 750 ℃ of roastings 2 hours make loaded nano hercynite catalysis material.
Made catalysis material is carried out catalytic performance test according to the afore-mentioned test condition, and catalysis material is respectively 63.9% and 37.8% to the conversion ratio of CO and NOx.
Embodiment 3
Is 1: 2 with cobalt nitrate and aluminum nitrate according to mol ratio, dissolves in the deionized water, is made into nitrate mixed solution, under agitation slowly is added drop-wise in the urea liquid, keeps the p H of solution to be about 9; Drip the back and continue to stir 1.5 hours, place 80 ℃ of water-baths 2h that wears out, spend deionised water and be filtered to filtrate pH=7; 120 ℃ of bakings 4 hours, 600 ℃ of roastings got the nanometer cobalt aluminate in 2 hours with the gained filter residue.With 1.5 gram nanometer cobalt aluminate powders, 5 gram boehmites, 1 gram ethylene glycol, 50 gram deionized waters mix making beating and make slurry, and regulating slurry pH value with rare nitric acid is 3; With cordierite ceramic carrier impregnation in slurry 5 minutes, purge ceramic monolith surface redundant sizing agent by pressure-air then, at last with ceramic monolith in 100 ℃ of bakings 2 hours, 750 ℃ of roastings 2 hours make loaded nano cobalt aluminate catalysis material.
Made catalysis material is carried out catalytic performance test according to the afore-mentioned test condition, and catalysis material is respectively 92.4% and 76.2% to the conversion ratio of CO and NOx.
Embodiment 4
Is 1: 2 with copper nitrate and aluminum nitrate according to mol ratio, dissolves in the deionized water, is made into nitrate mixed solution, under agitation slowly is added drop-wise in the urea liquid, keeps the p H of solution to be about 9; Drip the back and continue to stir 1.5 hours, placed 80 ℃ of water-baths aging 2 hours, spend deionised water and be filtered to filtrate pH=7; 120 ℃ of bakings 4 hours, 600 ℃ of roasting 2h got nanometer copper aluminate with the gained filter residue.With 1.5 gram nanometer copper aluminate powders, 5 gram boehmites, 1 gram ethylene glycol, 50 gram deionized waters mix making beating and make slurry, and regulating slurry pH value with rare nitric acid is 3; With cordierite ceramic carrier impregnation in slurry 5 minutes, purge ceramic monolith surface redundant sizing agent by pressure-air then, at last with ceramic monolith in 100 ℃ of bakings 2 hours, 750 ℃ of roastings 2 hours make loaded nano-copper aluminate catalysis material.
Made catalysis material is carried out catalytic performance test according to the afore-mentioned test condition, and catalysis material is respectively 87.1% and 69.4% to the conversion ratio of CO and NOx.
Embodiment 5
Is 1: 2 with nickel nitrate and aluminum nitrate according to mol ratio, dissolves in the deionized water, is made into nitrate mixed solution, under agitation slowly is added drop-wise in the urea liquid, keeps the p H of solution to be about 9; Drip the back and continue to stir 1.5 hours, placed 80 ℃ of water-baths aging 2 hours, spend deionised water and be filtered to filtrate pH=7; 120 ℃ of bakings 4 hours, 600 ℃ of roastings got the nanometer nickel aluminate in 2 hours with the gained filter residue.With 1.5 gram nanometer nickel aluminate powders, 5 gram boehmites, 1 gram ethylene glycol, 50 gram deionized waters mix making beating and make slurry, and regulating slurry pH value with rare nitric acid is 3; With cordierite ceramic carrier impregnation in slurry 5 minutes, purge ceramic monolith surface redundant sizing agent by pressure-air then, at last with ceramic monolith in 100 ℃ of bakings 2 hours, 750 ℃ of roastings 2 hours make loaded nano nickel aluminate catalysis material.
Made catalysis material is carried out catalytic performance test according to the afore-mentioned test condition, and catalysis material is respectively 90.8% and 73.9% to the conversion ratio of CO and NOx.
Embodiment 6
Is 1: 2 with copper nitrate, nickel nitrate and aluminum nitrate according to mol ratio, dissolves in the deionized water, is made into nitrate mixed solution, under agitation slowly is added drop-wise in the urea liquid, keeps the pH of solution to be about 9; Drip the back and continue to stir 1.5 hours, placed 80 ℃ of water-baths aging 2 hours, spend deionised water and be filtered to filtrate pH=7; 120 ℃ of bakings 4 hours, 600 ℃ of roastings got the nanometer copper nickel aluminate in 2 hours with the gained filter residue.With 1.5 gram nanometer copper nickel aluminate powders, 5 gram boehmites, 1 gram ethylene glycol, 50 gram deionized waters mix making beating and make slurry, and regulating slurry pH value with rare nitric acid is 3; With cordierite ceramic carrier impregnation in slurry 5 minutes, purge ceramic monolith surface redundant sizing agent by pressure-air then, at last with ceramic monolith in 100 ℃ of bakings 2 hours, 750 ℃ of roastings 2 hours make loaded nano-copper nickel aluminate catalysis material.
Made catalysis material is carried out catalytic performance test according to the afore-mentioned test condition, and catalysis material is respectively 91.7% and 80.3% to the conversion ratio of CO and NOx.

Claims (4)

1. loaded nano spinel complex oxide catalysis material, it is characterized in that, this catalysis material is carrier with the cordierite honeycomb ceramic, γ-alundum (Al is an active coating, the loaded with nano spinel complex oxide is prepared from, its mass percent is: γ-alundum (Al accounts for 10~25% of cordierite honeycomb ceramic carrier weight, and the nano spinel composite oxides account for 10~30% of γ-alundum (Al weight.
2. loaded nano spinel complex oxide catalysis material according to claim 1 is characterized in that the chemical formula of described nano spinel composite oxides is: AAl 2O 4, wherein A is iron or cobalt or nickel or copper, or copper and mickel.
3. the preparation method of loaded nano spinel complex oxide catalysis material according to claim 1 is characterized in that may further comprise the steps:
The first step, be 1: 2 according to mol ratio, dissolve in the deionized water, be made into nitrate mixed solution, prepare the aqueous solution of a certain amount of alkalescent precipitating reagent metal nitrate and aluminum nitrate;
Second the step, under agitation slowly be added drop-wise to nitrate solution in the aqueous solution of precipitating reagent, perhaps inverted sequence drips, and keeping the pH of solution is 9, drips the back and continues to stir, placed 60~80 ℃ of water-baths aging 2 hours, and spent deionised water and be filtered to filtrate pH=7;
The 3rd the step, with the gained filter residue 100~120 ℃ of bakings, 600~800 ℃ of roastings get the nano spinel composite oxide powder;
The 4th step, with the nano spinel composite oxide powder, boehmite, ethylene glycol, deionized water were with mass ratio 3: 10: 2: 100 mix making beating makes slurry, is 2.5~4 with rare nitric acid adjusting slurry pH value;
The 5th the step, with the cordierite ceramic carrier impregnation in slurry, purge ceramic monolith surface redundant sizing agent by pressure-air then, at last with ceramic monolith in 80~100 ℃ of oven dry, 750~800 ℃ of roastings make loaded nano spinel complex oxide catalysis material.
4. the preparation method of loaded nano spinel complex oxide catalysis material according to claim 3 is characterized in that described metal nitrate is or nickel nitrate or ferric nitrate or cobalt nitrate or copper nitrate, or nickel nitrate and copper nitrate.
CN2010105845519A 2010-12-11 2010-12-11 Supported nano-spinel composite oxide catalytic material and preparation method thereof Pending CN102068988A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105536793A (en) * 2015-12-10 2016-05-04 中国科学院生态环境研究中心 Iron-aluminum composite metal oxide micro-nano material and preparation method thereof, and degradation method for polybrominated diphenyl ethers
CN106179395A (en) * 2016-07-11 2016-12-07 广西大学 The oxidation of a kind of high-performance CO and NOx eliminate the preparation method of hydrogen-storing material
CN106423184A (en) * 2016-10-10 2017-02-22 华北电力大学 Catalyst capable of removing N2O, NO and NO2 simultaneously and preparation method
US9688703B2 (en) 2013-11-12 2017-06-27 Dow Corning Corporation Method for preparing a halosilane
CN108889301A (en) * 2018-08-07 2018-11-27 太原理工大学 A kind of spinel-type catalyst and preparation method thereof
CN111644182A (en) * 2020-03-05 2020-09-11 王金波 Honeycomb ceramic monolithic catalyst for rapidly catalyzing and oxidizing CO under high airspeed condition and preparation method thereof
CN112547076A (en) * 2020-12-23 2021-03-26 浙江盛旺环境工程有限公司 Prestressed SCR denitration catalyst and preparation method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9688703B2 (en) 2013-11-12 2017-06-27 Dow Corning Corporation Method for preparing a halosilane
CN105536793A (en) * 2015-12-10 2016-05-04 中国科学院生态环境研究中心 Iron-aluminum composite metal oxide micro-nano material and preparation method thereof, and degradation method for polybrominated diphenyl ethers
CN105536793B (en) * 2015-12-10 2018-03-06 中国科学院生态环境研究中心 Iron aluminum composite metal oxide micro Nano material and preparation method, PBDE biodegrading process
CN106179395A (en) * 2016-07-11 2016-12-07 广西大学 The oxidation of a kind of high-performance CO and NOx eliminate the preparation method of hydrogen-storing material
CN106179395B (en) * 2016-07-11 2018-11-20 广西大学 A kind of preparation method of high-performance CO oxidation and NOx elimination hydrogen-storing material
CN106423184A (en) * 2016-10-10 2017-02-22 华北电力大学 Catalyst capable of removing N2O, NO and NO2 simultaneously and preparation method
CN108889301A (en) * 2018-08-07 2018-11-27 太原理工大学 A kind of spinel-type catalyst and preparation method thereof
CN108889301B (en) * 2018-08-07 2021-09-14 太原理工大学 Spinel type catalyst and preparation method thereof
CN111644182A (en) * 2020-03-05 2020-09-11 王金波 Honeycomb ceramic monolithic catalyst for rapidly catalyzing and oxidizing CO under high airspeed condition and preparation method thereof
CN112547076A (en) * 2020-12-23 2021-03-26 浙江盛旺环境工程有限公司 Prestressed SCR denitration catalyst and preparation method thereof

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Application publication date: 20110525